JP2692139B2 - Manufacturing method of sputtering target - Google Patents

Description

TECHNICAL FIELD The present invention relates to the structure and composition of a rare earth-transition metal alloy sputtering target, and a manufacturing method.

[Conventional technology]

Conventionally, sputtering targets for forming rare-earth transition metal-based magneto-optical recording films include casting, sintering, and semi-melting methods. The casting method here is to use the cast ingot as a target by directly processing the outer diameter, and the sintering method is to crush the cast ingot once and form the target shape by sintering. Is. Further, the semi-melting method is disclosed in JP-A-61-95788.
And JP-A-61-99640.

[Problems to be solved by the invention]

However, the above-mentioned sintering method essentially contains a large amount of oxygen (2000 ppm is the limit) and is not suitable for a rare earth transition metal system which is easily oxidized. On the other hand, the casting method is preferable because it has a small amount of oxygen (about 500 ppm), but has a problem that a composition distribution occurs in the film formation surface.

In addition, the target produced by the semi-melting method is characterized in that the composition distribution does not easily occur in the substrate surface, but since the semi-melting method is also basically manufactured by sintering, the target is in a completely dense state. However, voids are continuously connected to the inside of the target, and when left in the atmosphere, oxygen progresses from the surface of the target toward the inside, and the oxide layer becomes so large that it cannot be cleaned by pre-sputtering. Will end up.

Therefore, the present invention solves such a problem,
The purpose is to overcome the drawbacks of the conventional cast alloy target that the composition distribution occurs in the film formation surface, and to overcome the drawback of the semi-melting and sintering targets that they are easily oxidized. It is to provide various targets and manufacturing methods thereof.

[Means for solving the problem]

1. a step of heating and melting a rare earth metal and a transition metal to form a molten alloy, and adjusting the temperature of the molten alloy to a first temperature, and then adding a rare earth metal powder and a transition metal powder to the molten alloy And a step of introducing the sputtering target, wherein the first temperature is lower than a melting point of the rare earth metal powder and lower than a melting point of the transition metal powder. And

2. A step of putting a transition metal powder having a first melting point and a porosity of 30 to 80% into a container, and a rare earth having a second melting point lower than the first melting point above the transition metal powder. The step of placing the transition metal alloy ingot, heating the transition metal powder and the rare earth transition metal alloy ingot to a temperature between the first melting point and the second melting point, the transition metal powder to the transition metal powder. The method is characterized by including a step of forming a compact through a step of impregnating a rare earth transition metal alloy, and a step of heat-treating the compact.

3. The rare earth metal includes at least one or more rare earth metal elements selected from Sm, Nb, Pr, Ce, Tb, and Dy, and the transition metal includes at least one transition metal element selected from Fe and Co. It is characterized by including.

4. The average particle size of the transition metal powder is 10 μm to 3.0 mm.

[Action]

In the case of the composite target method that deposits a rare earth metal (RE) chip on a transition metal (TM) target that has been conventionally used in the laboratory, the composition distribution in the substrate surface is opposite to that of the cast alloy target. Shows the tendency of.

In other words, in the case of a compound target, there are more REs just above the target and more TMs on the sides. On the other hand, the cast alloy target has more TM as it goes directly above the target and more RE as it goes to the side. It can be seen that there is a complementary relationship between the flying directions of sputtered particles of RE and TM in the cast alloy target and the composite target. In other words, if a target in which the RE single phase and the TM single phase and the RE-TM alloy phase are appropriately mixed can be formed, it is possible to form a uniform film having no composition distribution in the substrate surface.

The following two methods are mainly conceivable as a manufacturing method for producing a target having a packing density of 100% that is difficult to oxidize.

One is a method in which RE particles and TM particles are put into a RE-TM alloy bath having a low melting point and mixed to prepare. The other one is RE when it solidifies
This is a method of dispersing TM powder (sheet) in a RE-TE alloy bath in which a single phase appears. What can be said to be common to both is that the powder or sheet is completely surrounded by the RE-TM alloy bath water, and the formed body does not have the fine pores found in the sintered product. The pores of the product of the present invention are like the cavities found in the cast product even if they exist, the pores themselves are not connected, and the surface oxidation does not proceed to the inside.

[Example 1-1] First, an Nd Dy ingot with Nd ₂₃ Dy ₇₇ at% was made as a raw material,
NdDy powder is made by crushing the ingot so that the average particle size becomes about 500 μm. Then, a FeCo ingot with Fe _80.5 Co _19.5 at% was made, and the ingot was crushed to have an average particle size of 200 μm.
o Make powder.

Next, Nd, Dy, Fe, and Co are added to the crucible so that Nd _10.0 Dy _35.0 Fe _44.0 Co _11.0 at% is reached, the temperature is raised to 1550 ° C once to completely melt, and then lowered to 1200 ° C. Then, FeCo powder as the above-mentioned NdDy powder was put into the crucible in this NdDyFeCo molten alloy. Since NdDy has a melting point of 1400 ° C. and FeCo is 1530 ° C., it does not dissolve in 1200 ° C. hot water, so NdDy and FeCo exist as powders. The amounts of NdDyFeCo, NdDy, and FeCo are as follows.

(NdDyFeCo) _A ((NdDy) _C (FeCo) _D ) _B A: B = 25: 75 wt% C: D = 28: 72 at% (NdDyFeCo)-(NdDy)-(FeC
o) The molten metal is cast into a mold, the finished cast alloy is processed, and a schematic diagram of the surface structure of a 4 ″ φ × 6t sputtering target is shown in FIG. 1. The phase 1 is (NdDy) ₃₃
(FeCo) ₆₇ at% composition phase, this phase is FeCo composition phase,
3 is the NdDy composition phase. In other words, NdDy RE single phase and FeCo
It can be seen that it consists of three phases, a TM simple substance phase of No.2 and a RE-TM alloy phase of NdDyFeCo.

This NdDyFeCo target was attached to a sputtering apparatus as shown in FIG. 2, a film was formed, and its magnetic characteristics and composition distribution were examined. Reference numeral 21 in FIG. 2 is a sputtering target, and 22 is a substrate holder (300φ). Film formation conditions are Ar pressure 2.5 mTorr, initial vacuum degree 3 × 10 ^-7 Torr, input power DC
It was performed at 1.0A 340V using a power supply. FIG. 3 is a composition distribution and magnetic characteristic distribution diagram in a substrate holder using the target of the present invention. As shown in this figure, the composition is 28.0 to 28.5 at RE.
%, The magnetic properties are also uniform at Hc of 9.7 to 10.5 KOe. Almost almost uniform film can be formed in the substrate holder. Naturally, this target was a cast alloy, so the amount of oxygen was small and was 350 ppm.

A magneto-optical recording medium was produced by sputtering using the target of the present invention. A structural drawing of the medium is shown in FIG.
351 is a polycarbonate substrate, 352 is an AlSiN dielectric film, 353 is an NdDyFeCo film made with the target of the present invention, 354
Is an AlSiN dielectric film. This medium has a linear velocity of 5.7m / sec, Do
With a main length of 1.4 μm, a very high value of C / N 59 dB was obtained.
Even in the reliability test, under constant temperature and humidity of 90 ° C and 90% RH, 3000
No pitting corrosion occurred for a long time.

On the other hand, for comparison, an NdDyFeCo target was prepared by a conventional manufacturing method. That is, the entire composition of NdDyFeCo was melted in a crucible at 1500 ° C., and then poured into a mold to form an ingot.
Thereafter, the ingot was cut and polished to prepare a 4 ″ φ × 6t NdDyFeCo target. A schematic view of the surface structure of this target is shown in FIG.

41 is a (Nd _0.12 Dy _0.88 ) ₂₅ (Fe _0.8 Co _0.2 ) ₇₅ at% composition phase, and 42 is a (Nd _0.3 Dy _0.7 ) _33.3 (Fe _0.8 Co _0.2 ) _66.7 at% composition phase. That is, both phases are NdDyFeCo alloy phases.
The overall composition was Nd _6.5 Dy _21.5 Fe ₅₈ Co ₁₄ at%. A film was formed on this target with the sputtering apparatus shown in FIG. Figure 5 shows the cast alloy Nd produced by this conventional manufacturing method.
The composition distribution and magnetic characteristic distribution map in the substrate holder using the DyFeCo target are shown. As shown in this figure, the composition of RE is 2
At 9.8 to 26.8 at%, the more RE toward the center of the substrate holder, the less RE toward the outer periphery of the holder. The magnetic properties of Hc are 12 to 6 KOe, and Hc increases toward the center of the holder. This agrees with the composition distribution.

A magneto-optical recording medium was prepared by sputtering using this conventional target. The structure of the medium is the same as that of FIG. 35, and the magneto-optical recording layer is sandwiched by AlSiN dielectric films. This medium has a linear velocity of 5.7 m / sec and a domain length of 1.4 μm.
The value was a little lower, C / N 55 dB. This is an effect of the composition distribution in the medium. 90 ° C 90% RH in reliability test
No pitting corrosion occurred even after 3000 hours under constant temperature and humidity.

Further, for comparison, JP-A-61-957788 and JP-A-61-957788
An NdDyFeCo target was manufactured by the semi-melting method shown in No. 99640 and the film formation was evaluated. The target composition is Nd _6.5 Dy _21.5 Fe
₅₈ Co ₁₄ at%, and the amounts of NdDy, NdDyFeCo, and FeCo are the same as described above. The oxygen content of this target was 1500 ppm.
This target was attached to the sputtering device shown in FIG.
Pre-sputtering was sufficiently performed to form a film after the target surface was in a sufficiently clean state. The film forming conditions are the same as described above. FIG. 6 shows the composition distribution and magnetic characteristic distribution diagram in the substrate holder using the semi-molten NdDyFeCo target. The composition distribution is similar to that of the target of the present invention shown in FIG. 3, but the magnetic characteristic distribution is the coercive force (Hc)
It can be seen that is shifted in the smaller direction. This is a phenomenon caused by the fact that the semi-molten target has a larger amount of oxygen than the target of the present invention because it is sintered, and the rare earth metal is partially oxidized by oxygen.

Using this semi-molten target, a magneto-optical recording medium was created by sputtering. The structure of the medium is the same as that of FIG. 35, and the magneto-optical recording layer is sandwiched by AlSiN dielectric films. This medium has a linear velocity of 5.7 m / sec and a domain length of 1.4 μ.
It was C / N 57 dB at m, which was a little low value. This is because oxygen in the target was also taken into the film. In the reliability test, pitting corrosion started to occur from the 200th hour under constant temperature and humidity of 90 ℃ and 90% RH, and the Error Rate started to deteriorate. This is also because oxygen in the target was taken into the film.

The aforementioned NdDyFeCo target of the present invention and semi-molten NdDyFeCo
The target was removed after the sputtering was completed, and both targets were left in the atmosphere for 24 hours. After that, both targets were mounted on the sputtering apparatus shown in FIG. 2 again to attempt film formation. Table 1 shows the discharge state during sputtering.

As shown in the table above, the target of the present invention remained at DC sputtering Ar pressure of 2.5 mTorr from the initial stage and the discharge was very stable, but the semi-molten target could not perform DC sputtering at the initial stage. This is because the surface of the semi-molten target became a complete insulator after being left in the atmosphere for a long time. After 1 hour, DC sputtering was possible, but the Ar pressure had to be 10 mTorr, and after 7 hours, DC sputtering was finally possible at 2.5 mTorr.

FIG. 7 shows the relationship between the sputtering time and the magnetic characteristics of the film for both targets after being left in the atmosphere. 71 is a target according to the present invention, and 72 is a target according to the semi-melting method. As is clear from this figure, the target according to the present invention exhibits stable film characteristics immediately after sputtering even when exposed to the atmosphere for a long time. On the other hand, when the target by the semi-melting method is exposed to the air for a long time, the sputtering itself becomes very difficult at the beginning, and even after performing the long-time pre-sputtering, the film properties are not stable at all, and the film properties are not stable. It will be about the time when the number of targets decreases and the number of targets stabilizes. The magnetic properties of the films shown in these are bounded by the compensation composition,
Since the composition (characteristics) is on the TMrich side, the larger the coercive force (Hc), the better the film characteristics.

Next, it was investigated how the target by the semi-melting method affects the film characteristics when exposed to the atmosphere. The target was thoroughly cleaned by pre-sputtering, and the film characteristics were stable.
It was left for minutes, 30 minutes, 1 hour, 5 hours, 10 hours. After that, an experiment similar to that shown in FIG. 7 was performed, and the dependence of the magnetic properties of the film on the sputtering time was observed. Figure 8 shows that. 81 is 10 minutes left in the atmosphere, 82 is 30 minutes left in the atmosphere, 83 is 1 hour left in the atmosphere, 84 is 5 hours left in the atmosphere, and 83 is 10 hours left in the atmosphere. As is clear from the figure, when the target obtained by the semi-melting method is left in the atmosphere for 10 minutes, surface oxidation of the target occurs and the film magnetic characteristics are affected. Further, it can be seen that the longer the standing time in the air is, the more the oxidation from the target surface progresses and the more serious the influence on the magnetic properties of the film becomes.

The fact that leaving them in the atmosphere has a serious problem in terms of yield cost when mass-producing magneto-optical recording media. The target according to the present invention also has a great effect in this respect.

Although the substrate used was a PC and AlSiN was used for the derivative film, the medium created could be PMMA, APO, glass, etc. in addition to the PC substrate.
In addition to iN, the effects of the present invention existed with any derivative film such as SiN, Si ₃ N ₄ , SiO, AlSiNO, ZnS.

Example 1-2] Next make Pr ₂₃ Tb ₇₇ at% to become PrTb ingot as a raw material,
PrTb powder is prepared in the same manner as in Example 1-1. And similarly Fe
_80.5 Co _19.5 at% Make powder.

Further, each element is put into the crucible so as to be Pr ₁₀ Tb ₃₅ Fe ₄₄ Co ₁₁ at%, the temperature is once raised to 1550 ° C. and completely melted, and then lowered to 1200 ° C. Then, the PrTbFeCo molten alloy was charged with the PrTb powder and the FeCo powder described above in a crucible. Since this PrTb has a melting point of 1370 ° C and FeCo is 1530 ° C, it does not dissolve in hot water at 1200 ° C, so PrTb powder, Fe
It will exist as Co powder. And these Pr
The amounts of TbFeCo, PrTb, and FeCo are as follows.

(PrTbFeCo) _E ((PrTb) _G (FeCo) _H ) _F E: F = 25: 75 wt% G: H = 28: 72 at% Thus formed (PrTbFeCo)-(PrTb)-(FeC
o) As a result of evaluating the composition distribution and the magnetic property distribution in the substrate holder with the same film forming apparatus and film forming method as in Example 1-1 using the cast alloy target, RE was 28.0 to 28.5 at% and Hc was
It was uniform at 18.0 to 19.0 KOe. Also, the amount of oxygen was as small as 380 PPM, the sputtering discharge was stable from the beginning even after being left in the air for 24 hours, and the magnetic properties of the film were also stable from the beginning.

 The effect of the present invention was confirmed even with the PrTbFeCo composition.

[Example 1-3] Next, an SmGd ingot having an Sm ₂₃ Gd of ₇₇ at% is made, and an SmGd powder is made. And in the same way, make Fe ₉₀ Co ₁₀ at% powder. Furthermore Sm
Put each element into the crucible so that ₁₀ Gd ₃₅ Fe _49.5 Co _5.5 at%, raise the temperature to 1550 ° C once to completely dissolve it, and then lower it to 1200 ° C. Then, this SmGdFeCo molten alloy was charged with the above SmGd powder and FeCo powder in a crucible. Since this SmGd has a melting point of 1270 ° C and FeCo of 1530 ° C, it does not dissolve in 1200 ° C hot water, so SmGd powder, FeCo
It will exist as a powder. And these SmGdFe
The amounts of Co, SmGd, and FeCo are as follows.

(SmGdFeCo) _I ((SmGd) _K (FeCo) _L ) _J I: J = 25: 75wt% K: L = 28: 72at% Thus formed (SmGdFeCo)-(SmGd)-(FeC
o) The cast alloy target was a target capable of forming a film having no composition distribution or magnetic property distribution in the substrate holder as in the case of Examples 1-1 and 1-2. Hc is 5 to 5.5 KO
The e and RE were uniform at 28-28.5 at%. Oxygen amount is 300ppm
The sputtering discharge was stable from the beginning even after being left in the atmosphere for 24 hours, and the film magnetic characteristics were also stable from the beginning.

 The effect of the present invention was confirmed even with the SmGdFeCo composition.

[Example 1-4] Next, a CePrDy ingot with Ce _11.5 Pr _11.5 Dy ₇₇ at% was prepared.
Make CePrDy powder. Then, prepare Fe _80.5 Co _19.5 at% powder in the same manner, and further add each element into the crucible so that Ce _5.0 Pr _5.0 Dy _35.0 Fe _44.0 Co _11.0 at%, raise the temperature once to 1550 ° C and completely melt. And then lower to 1200 ℃. Then, the CePrDyCo molten alloy was mixed with the above CePrDy powder and FeCo.
The powder was placed in a crucible. This CePrDy has a melting point of 1350 ° C.
Since FeCo is 1530 ° C and is not dissolved in hot water at 1200 ° C, it exists as CePrDy, FeCo powder as it is. The CePrDyFeCo, CePrDy and FeCo amounts are in the following proportions.

((CePrDyFeCo) _M ((CePrDy) _P (FeCo) _Q ) _N M: N = 25: 75wt% P: Q = 28: 72at% Thus formed (CePrDyFeCo)-(CePrDy)-
The (FeCo) cast alloy target was manufactured according to Examples 1-1, 1-2, 1-
As with No. 3, it was a target capable of forming a film without composition distribution in the substrate holder. The oxygen content was 420 ppm, and the sputtering discharge was stable from the beginning even after being left in the air for 24 hours, and the magnetic properties of the film were also stable from the beginning.

 The effect of the present invention was confirmed with respect to the CePrDyFeCo composition.

In addition to the composition systems shown in these Examples 1-1, 1-2, 1-3, 1-4, NdTbFeCo, NdGdFeCo, NdDbCo, NdTbGdFe, NdTbGdFeC
o, NdDyGdFeCo, NdDyGdTbFeCo, PrDyFeCo, PrGdFeCo, NdPrDy
FeCo, NdCeDyFeCo, NdTbCo, NdPrCeDyFeCo, NdSmDyFeCo, CeS
Sm, Nd, such as mPrDyFeCo, CePrNdDyTbFeCo, CeNdPrDyGdFeCo, etc.
At least one light rare earth element of Pr and Ce and Gd, Tb, Dy
It has been confirmed that the effect of the present invention is present in all the composition systems containing at least one or more heavy rare earths and at least one or more transition metals of Fe and Co.

Next, if the target composition does not include light rare earth metals,
That is, an example in which a heavy rare earth metal (HR) and a transition metal (TM) are contained will be described.

Example 2-1 First, as a raw material, Tb powder having an average particle size of about 300 μm was prepared, and an FeCo ingot having an Fe ₉₃ Co of ₇ at% had an average particle size of 150 μm.
Grind to a certain size to make FeCo powder.

Next, the crucible was put into a crucible in a vacuum so as to have Tb ₄₅ Fe ₅₁ Co ₄ at%, the temperature was once raised to 1650 ° C to completely dissolve it, and then lowered to 1200 ° C. And in this TbFeCo molten alloy,
The above Tb powder and FeCo powder were put into a crucible. Since Tb has a melting point of 1450 ° C. and FeCo is 1530 ° C., it does not dissolve in 1200 ° C. hot water, so Tb and FeCo powders remain as they are. Then, the amounts of these TbFeCo, Tb, and FeCo are as follows.

(TbFeCo) _A (Tb _C (FeCo) _D ) _B A: B = 25: 75 wt% C: D = 22: 78 at% The (TbFeCo) -Tb- (FeCo) molten metal thus formed is cast into a mold, After that, the finished casting alloy is processed,
A 4 ″ φ × 6t sputtering target was created. The surface texture of the resulting target was the same as in the case of Fig. 1. The RE-TM alloy phase of TbFeCo, the RE simple phase of Tb, and the TM simple phase of FeCo were prepared. It was three phases.

This TbFeCo target according to the present invention was mounted on the same sputtering apparatus as shown in FIG. 2 to form a film, and its magnetic characteristics and composition distribution were examined. The film forming conditions are Ar pressure of 2.5 mTorr, initial vacuum degree of 3 × 10 ^-7 Torr, and input power of 1.0 A using a DC power source, 34
It was done at 0V. FIG. 9 is a composition distribution and magnetic characteristic distribution diagram in a substrate holder using the target of the present invention. As shown in this figure, the composition of RE is uniform at 22.0 to 22.5 at%, and the magnetic properties are also uniform at Hc of 14.7 to 15.5 KOe. Almost almost uniform film can be formed in the substrate holder. Naturally, this target was a cast alloy, so it had a low oxygen content of 350 ppm.

The magneto-optical recording medium prepared using the target of the present invention had a very high value of C / N 60 dB at a linear velocity of 5.7 / sec and a domain length of 1.4 μm. Also in the reliability test, 90 ℃ 90% RH
No pitting corrosion was observed even after 3000 hours under constant temperature and humidity.
There was also no increase in ror rate.

On the other hand, a TbFeCo target was prepared by a conventional manufacturing method for comparison. That is, the total composition of TbFeCo is Tb ₂₂ Fe ₇₃ Co ₅ at
It was melted in a crucible at 1650 ° C. so that it would be 100%, and then poured into a mold to make an ingot. Then, this ingot was cut and polished to prepare a 4 ″ φ × 6t TbFeCo target. Fig. 10 is a composition distribution and magnetic characteristic distribution diagram in the substrate holder using the cast alloy TbFeCo target by this conventional manufacturing method. As shown in this figure, the composition is 22.8 to 19.8 at% RE,
There is more RE toward the center of the substrate holder, and conversely less RE toward the outside of the holder. Also, the magnetic characteristics
Hc increases from 17 to 11 KOe and goes into the holder. This agrees with the composition distribution. In other words, in the cast alloy TbFeCo target manufactured by the conventional manufacturing method, TM (transition metal) is more likely to jump in the upper direction of the target,
RE exhibits a property of easily jumping, which causes a composition distribution in the substrate holder.

The magneto-optical recording medium created using this target is
The linear velocity was 5.7 m / sec, the domain length was 1.4 μm, and the C / N was 57 dB, which was a little low value. This is an effect of composition distribution in the medium.
In the reliability test, 3000 at 90 ° C and 90% RH under constant temperature and humidity.
No pitting occurred after the time.

Further, for comparison, JP-A-61-95788 and JP-A-61-9
A TbFeCo target was manufactured by the semi-melting method shown in No. 9640 and the film formation was evaluated. The target composition is Tb ₂₂ Fe ₇₃ Co ₅ at%, and the amounts of Tb, TbFeCo, and FeCo are the same as described above. The oxygen content of this target was 1300 ppm. This target was also mounted on the sputtering apparatus shown in FIG. 2 and pre-sputtering was sufficiently performed to form a film after the target surface was in a sufficiently clean state. The film forming conditions are the same as described above. Fig. 11 shows the composition distribution and magnetic property distribution diagram in the substrate holder using the semi-melted TbFeCo target. Although the composition distribution is about the same as that of the target of the present invention shown in FIG. 9, it can be seen that the magnetic characteristic distribution is shifted in the direction in which the coercive force (Hc) is small overall. This is a phenomenon caused by the partial melting of the rare earth metal by oxygen because the semi-melting method target is more sintered than the target of the present invention because it is sintered.

The magneto-optical recording medium created using this target is
At a linear velocity of 5.7 m / sec and a domain length of 1.4 μm, the C / N was 58 dB, which was a little low value. This is because oxygen in the target was also taken into the film. In the reliability test, 90 ℃ 90
Pitting corrosion occurs from the 200th hour under constant temperature and humidity of% RH.
Rate started to deteriorate. This is also because oxygen in the target was taken into the film.

Further, the above-mentioned TbFeCo target of the present invention and the semi-molten TbFe target
After the sputtering, the Co target was removed and both targets were left in the atmosphere for 24 hours. After that, both targets were mounted on the sputtering apparatus shown in FIG. 2 again to attempt film formation. Table 2 shows the discharge state during sputtering.

As shown in the above table, the target of the present invention was very stable in the discharge with the DC sputtering Ar pressure of 2.5 mTorr from the initial stage, but the semi-molten target could not perform the DC sputtering in the initial stage. Since this was left in the atmosphere for a long time, semi-molten Tb
This is because the surface of the FeCo target is completely an insulator. After 1 hour, DC sputtering was possible, but the Ar pressure had to be 8 mTorr, and after 5 hours, DC sputtering was finally possible at 2.5 mTorr.

FIG. 12 shows the relationship between the sputtering time and the magnetic properties of the film for both targets after being left in the atmosphere. 121 is the target according to the present invention, and 122 is the target according to the semi-melting method. As is clear from this figure, the target according to the present invention exhibits stable film characteristics immediately after sputtering even when exposed to the atmosphere for a long time. On the other hand, when the target by the semi-melting method is exposed to the air for a long time, the sputtering itself becomes very difficult at the beginning, and the film characteristics are not stable even after performing the long-time pre-sputtering, and the film characteristics are not stable. By the time it stabilizes, there will be no more targets left. The magnetic properties of the films shown in these are bounded by the compensation composition,
Since the composition (characteristics) is on the TMrich side, the larger the coercive force (Hc), the better the film characteristics.

Next, it was investigated how the semi-melting method target affects the film characteristics when left in the atmosphere. The target was thoroughly cleaned by pre-sputtering, and the film characteristics were stable.
It was left for 3 minutes, 30 minutes, 1 hour, and 3 hours. After that, the same experiment as in Fig. 12 was performed, and the dependence of the magnetic properties of the film on the sputtering time was observed. Fig. 13 shows this, 131 for 10 minutes in the atmosphere, 132 for 30 minutes in the atmosphere, 133 for 1 hour in the atmosphere, and 134 for 3 hours in the atmosphere. As is clear from the figure, when the target obtained by the semi-melting method is left in the atmosphere for 10 minutes, surface oxidation of the target occurs and the film magnetic characteristics are affected. And, the longer it is left in the air, the more the oxidation from the target surface progresses,
It can be seen that the degree of influence that affects the magnetic properties of the film becomes severe.

The effect of the present invention was confirmed even with TbFeCo containing no light rare earth metal.

[Example 2-2] Next, as a raw material, Dy powder having an average particle diameter of about 300 µm was prepared, and an FeCo ingot having an Fe ₉₃ Co of ₇ at% was formed to have an average particle diameter of 150 µm.
Grind to a certain size to make FeCo powder.

Next, the crucible is put into a crucible so that it becomes Dy ₄₅ Fe ₅₁ Co ₄ at%, the temperature is once raised to 1650 ° C to completely melt it, and then it is lowered to 1200 ° C. And in this DyFeCo molten alloy,
The above Dy powder and FeCo powder were put into a crucible. Since Dy has a melting point of 1450 ° C. and FeCo is 1530 ° C., it does not dissolve in 1200 ° C. hot water, so the Dy, FeCo powder remains as a powder. The amounts of DyFeCo and DyFeCo are as follows.

(DyFeCo) _E (Dy _G (FeCo) _H ) _F D: F = 25: 75wt% G: H = 22: 78at% The (DyFeCo) -Dy- (FeCo) molten metal thus formed is cast into a mold. After that, the finished cast alloy was processed, and the composition distribution and magnetic property distribution in the substrate holder were evaluated by the same film forming apparatus and film forming method as in Example 2-1, using a 4 ″ φ × 6t sputtering target. RE is 22.0
~ 22.5at%, uniform, magnetic properties Hc is 12.0 ~ 13.0KO
It was uniform in e. The amount of oxygen was as low as 350 ppm. or,
Even after being left in the air for 24 hours, the sputtering discharge was stable from the beginning and the film magnetic characteristics were also stable from the beginning.

 The effect of the present invention on the DyFeCo composition was confirmed.

As Example 2-3] Next feedstock, make GdTb ingot becomes Tb ₅₀ Gd ₅₀ at%, making GdTb powder. And in the same way, make Fe ₉₃ Co ₇ at% powder. Further, each element is put into the crucible so as to have Gd _22.5 Tb _22.5 Fe ₅₁ Co ₄ at%, the temperature is once raised to 1650 ° C to completely dissolve it, and then it is lowered to 1200 ° C. And this GdTb
The above-mentioned GdTb powder and FeCo powder were put into a crucible in an FeCo molten alloy. This GdTb powder has a melting point of 1400 ° C,
Since it is 1530 ℃, it does not dissolve in 1200 ℃ hot water, so
The GdTb and FeCo powders remain as powders. The amounts of GdTbFeCo, GdTb and FeCo are as follows.

(GdTdFeCo) _I ((GdTb) _K (FeCo) _L ) _J I: J = 25: 75wt% K: L = 22: 78at% Thus formed (GdTbFeCo)-(GdTb)-(FeC
o) The cast alloy target was a target capable of forming a film with no composition distribution or magnetic property distribution in the substrate holder as in the case of Examples 2-1 and 2-2. Hc is 11 ~ 13KOe, R
E was uniform at 22 to 22.5 at%. The amount of oxygen was 300 ppm.

Further, even after being left in the air for 24 hours, the sputtering discharge was stable from the beginning, and the film magnetic characteristics were also stable from the beginning.

 The effect of the present invention was confirmed also for GdTbFeCo.

In addition to the composition systems shown in these Examples 2-1, 2-2, 2-3, TbDyFeCo, DyGdFeCo, GdFeCo, GdTbFe, TbDyFe, TbCo, Dy
The effect of the present invention is present in all composition systems containing at least one heavy rare earth metal of Gd, Tb, Dy such as GdCo, and at least one transition metal of Fe, Co. It was confirmed.

Next, as another example, another manufacturing method of the target of the present invention will be described. This manufacturing method is called an impregnation method or an infiltration method. The outline of this manufacturing method will be described.

TM powder is spread in a mold, and a RE-TM alloy ingot (called mother alloy) is placed on it. This mother alloy composition is a low melting point alloy having a melting point of 1200 ° C. or less in the vicinity of the rare earth metal eutectic composition in the phase diagram. This powder and the mother alloy are heated to melt the mother alloy, and the melted mother alloy is soaked in the pores of the powder. When the melted master alloy solidifies, it separates into RE and RE ₁ TM ₂ phases, so the resulting metallic structure of the target becomes the TM phase, the RE single phase, and the RE-TM alloy phase. is there.

[Example 3-1] First, as a raw material, (Nd _0.2 Dy _0.8 ) _72.2 (Fe _0.8 Co _0.2 ).
_{A 27.8} at% ingot is formed (hereinafter, this ingot is referred to as an R + R ₁ T ₂ master alloy). The melting point of this master alloy is as low as 830 ℃, and the shape is 4 ″ φ × 2t. Then, Fe ₈₀ Co ₂₀ at% 200
A powder having a particle size of μm was prepared. The melting point of this powder is as high as 1500 ° C, and the porosity of this powder is 62.4%.

This powder is put into a 4 ″ φ inner diameter crucible, and R
+ R ₁ T ₂ Master alloy is added. The schematic diagram showing this state is
14 is a figure. 141 is a crucible, 142 is a high frequency induction heating coil, 143 is an R + R ₁ T ₂ mother alloy, and 144 is a Fe ₈₀ Co ₂₀ at% powder. A vacuum is drawn from this state, and then the temperature is raised to 1050 ° C. At this time, the R + R ₁ T ₂ mother alloy is melted, and the Fe—Co powder remains in a powder state without being melted. That is, the molten metal in which the R + R ₁ T ₂ ingot is melted penetrates into the pores of the Fe—Co powder and fills the pores. After cooling, the molded body in the crucible was taken out, and the outer periphery was processed and polished to prepare a sputtering target of 4 ″ φ × 3t.
The target composition is Nd _5.5 Dy _22.0 Nd _58.0 Co _14.5 at%. Figure 15 shows a schematic diagram of the surface texture of this target.
Shown in the figure. The phase of 151 is Fe-Co particles, the phase of 152 is a rare-earth-only phase of Nd-Dy, and the phase of 153 is a rare-earth transition metal alloy phase of (NdDy) ₁ (FeCo) ₂ . That is, there are three phases of the rare earth single phase, the rare earth transition metal phase, and the transition metal single phase.

This NdDyFeCo target was attached to a sputtering apparatus similar to that shown in FIG. 2, a film was formed, and its magnetic characteristics and composition distribution were examined. Film forming conditions are Ar pressure 2.5 mTorr, initial vacuum degree 3 ×
The applied power was 10 ^-7 Torr, and DC power was applied at 1.0 A 340V. FIG. 16 is a composition distribution and magnetic characteristic distribution diagram in a substrate holder using the target of the present invention. As shown in this figure, the composition is uniform with RE of 28.0 to 28.5 at%, and the magnetic characteristics are Hc.
Is uniform from 9.7 to 10.5 KOe and shows magnetic characteristics matching the film composition. A uniform film is formed almost in the substrate holder. Naturally, this target is not a sintering method, the mother alloy is not a powder but a bulk, and since it is an infiltration target by complete melting, the amount of oxygen is small and it is 350 ppm. Moreover, since it was not a method of pouring into the mold described above, the occurrence of cavities was extremely small, and the packing density was 99.5%, which was extremely high.

This target also has a very stable discharge from the beginning of sputtering, and DC sputtering is possible with an Ar pressure of 2.5 mTorr. And, even after being left in the atmosphere for 24 hours, stable film characteristics are exhibited immediately after sputtering.

[Example 3-2] Next, the effect of the method of the present invention was confirmed for PrTbArFeCo. The manufacturing method is the same as in Example 3-1, first as matrix alloy _{(Pr 0.2 Tb 0.8) 80 (} Fe 0.8 Co 0.2) make ₂₀ at% of the ingot. The melting point of this master alloy is about 810 ° C, and the shape is 4 ″ φ × 2.5t bulk. And then Fe ₈₀ Co ₂₀ at%
Powder of 200 μm particle size is prepared, and this powder is laid on a mold made of alumina with a 4 ″ φ inner diameter. Then, the mother alloy is placed on it and heated in a furnace at 1050 ° C. under vacuum. After melting, the mixture was cooled, and the formed body was taken out of the mold, processed for outer circumference, and polished to prepare a sputtering target of 4 ″ φ × 3t. After all the target composition is RE, RE-T
It has three phases, M and TM, and the overall composition is Pr _5.5 Tb _22.0 Fe.
_{It was 58.0} Co _14.5 at%. Then, as a result of evaluating the composition distribution and the magnetic property distribution in the substrate holder with the same film forming apparatus and film forming method as in Example 3-1, RE was 28.0 to 28.5 at% and Hc was
It was uniform at 18.0 to 19.0 KOe. Also, the oxygen content was as low as 380 ppm, and the sputtering was stable from the beginning even after being left in the air for 24 hours, and the film magnetic characteristics were also stable from the beginning.

For the PrTbFeCo composition, the manufacturing method of the present invention is possible, and the same effect was confirmed.

[Example 3-3] Next, the effect of the method of the present invention was confirmed for SmGdFeCo. The manufacturing method is the same as in Examples 3-1 and 3-2. First, as a master alloy, (Sm _0.2 Gd _0.8 ) _72.2 (Fe _0.8 Co _0.2 ) _27.8 at
Make% ingot. The melting point of this master alloy is about 808 ° C. Then, prepare a powder of Fe ₈₀ Co ₂₀ at% with a particle size of 200 μm, and spread this powder on a mold made of mullite with a 4 ″ φ inner diameter. The atmosphere was heated. After the mother alloy was melted, it was cooled and the formed body was taken out in the mold, the outer circumference was opened, and it was polished to 4 ″ φ ×
A 3t sputtering target was created. After all, the target composition was three phases of RE, RE-TM, and TM, and the overall composition was Sm _5.5 Gd _22.0 Fe _58.0 Co _14.5 at%. Then, the composition distribution and the magnetic property distribution in the substrate holder were evaluated by the same film forming apparatus and film forming method as those in Examples 3-1, 3-2, and as a result, RE was 28.0 to 28.5 at% and Hc was 5 to 5.5 KOe. Was uniform. Also, the amount of oxygen was as small as 390 ppm, the sputtering was stable from the beginning even after standing for 24 hours in the air, and the film magnetic characteristics were also stable from the beginning.

For the SmGdFeCo composition, the production method of the present invention is possible, and the same effect was confirmed.

Example 3-4 Next, the effect of the method of the present invention was confirmed for NdSmDyTbFeCo. The manufacturing method is the same as in Examples 3-1, 3-2, and 3-3. First, as a master alloy (Nd _0.1 Sm _0.1 Dy _0.4 Tb _0.4 )
_72.2 (Fe _0.8 Co _0.2 ) Make _27.8 at% ingot. The melting point of this ingot is about 830 ° C, and the shape is a bulk of 4 ″ φ × 2.5t. Then, prepare a powder of Fe ₈₀ Co ₂₀ at% with a particle size of 200 μm, and use this powder for 4 ″ φ. Lay it on a mold made of Isolite with an inner diameter. Then put the mother alloy on it and under vacuum 1030
The atmosphere was heated to ° C. After the mother alloy has melted, it is cooled and the resulting molded product is taken out from the mold and processed to the outer periphery and polished to 4 "φ
A × 3t sputtering target was prepared. The target composition is RE, RE-TM, T,
The total composition is Nd _2.75 Sm _2.75 Dy _11.0.
It was Tb _11.0 Fe _58.0 Co _14.5 at%. And Example 3-1
As a result of evaluating the composition distribution and magnetic property distribution in the substrate holder with the same film forming apparatus and film forming method as 3-2 and 3-3, RE was 2
The homogeneity was 8.0 to 28.5 at%, and the Hc was also uniform from 17 to 17.5 KOe. Also, the amount of oxygen was as small as 375 ppm, and sputtering was stable from the beginning even after being left in the air for 24 hours.

For the NdSmDyTbFeCo composition, the manufacturing method of the present invention is possible, and the same effect was confirmed.

In addition to the composition systems shown in these Examples 3-1, 3-2, 3-3, 3-4, NdGdFeCo, NdTbFeCo, NdPrDyFeCo, NdPrDyTbFeCo, PrDy
FeCo, NdSmGdFeCo, CeNdDyFeCo, CeNdPrDyFeCo, etc. Sm, Nd,
At least one light rare earth metal of Pr or Ce, and G
The production method of the present invention is possible for all composition systems containing at least one heavy rare earth metal of d, Td, Dy and at least one transition metal of Fe, Co, and the same It was confirmed that the effect of exists.

Then, it was confirmed that a method is also possible in which the transition metal powder is made into Fe powder and the Co content of the master alloy is adjusted to make the Co composition of the target desired.

Next, if the target composition does not include light rare earth metals,
That is, an example in which a heavy rare earth metal and a transition metal are contained will be described.

Example 3-5 First, an ingot of Tb ₇₂ (Fe _0.9 Co _0.1 ) ₂₈ at% is made as a raw material (hereinafter, this ingot is referred to as an R + R ₁ T ₂ mother alloy). The melting point of this master alloy is as low as 847 ° C, and the shape is also 4 ″ φ × 2.5t. Then, prepare powder of Fe ₉₀ Co ₁₀ at% with a particle size of 200 μm. This melting point is as high as 1500 ° C. The porosity of this powder is 43.4 mother alloy.

Spread this powder on a mold made of alumina with a 4 "φ inner diameter,
The mother alloy was placed on it and heated in an Ar gas atmosphere. After the mother alloy was melted, it was cooled, and the formed body was taken out from the die and processed on the outer periphery and polished to form a 4 ″ φ × 3t sputtering target. Again, the target composition was RE, RE-
It has three phases, TM and TM, and the overall composition is Tb ₂₂ Fe _70.2 Co.
_{It is 7.8} at%. Then, as a result of evaluating the composition distribution and the magnetic property distribution in the substrate holder by the film forming apparatus and the film forming method similar to those in Examples 3-1, 3-2, RE was 22.0 to 22.5 at% and the The properties were also uniform at Hc of 14.7 to 15.5 KOe. The more uniform the film is, the better the film can be placed in the substrate holder. Also, the amount of oxygen was as low as 350 ppm, the sputtering was stable from the beginning even after being left in the air for 24 hours, and the magnetic properties of the film were also stable from the beginning.

[Example 3-6] Next, the effect of the method of the present invention was confirmed for DyFeCo.
The manufacturing method is the same as in Examples 3-1 and 3-2. First, an ingot of Dy _71.5 (Fe _0.9 Co _0.1 ) _28.5 at% is made as a raw material.
The melting point of this ingot is about 890 ° C. And then Fe ₉₀ Co ₁₀ a
A powder having a particle diameter of 200 μm of t% was prepared. This melting point is 1500 ° C
The porosity of this powder is 43.2%.

Spread this powder on a mold made of mullite with a 4 "φ inner diameter,
Place the ingot on it, raise the temperature to 1050 ° C in vacuum, melt the ingot, and then cool it. Take out the formed body in the mold, process the outer periphery, and polish it. 4 ″ φ × 3t sputtering target After all, the target composition is RE, R
It has three phases, E-TM and TM, and the overall composition is Dy ₂₂ Fe _70.2 C.
It was _7.8 at%. Then, the composition distribution and the magnetic property distribution in the substrate holder were evaluated by the same film forming apparatus and film forming method as those in Examples 3-1, 3-2 and the like. As a result, RE was 21.5 to 22.0 at% and the magnetic distribution was uniform. The characteristics are uniform with Hc of 13.5-13.0 KOe. Almost almost uniform film can be formed in the substrate holder. The oxygen content of this target is also 350p
Sputtering was stable from the beginning even after being left in the atmosphere for 24 hours, and the magnetic properties of the film were also stable from the beginning.

[Example 3-7] Next, the effect of the method of the present invention was confirmed for TbGdFeCo. The manufacturing method is the same as in Examples 3-1 and 3-2. First, as a master alloy, (Tb _0.5 Gd _0.5 ) _71.5 (Fe _0.9 Co _0.1 ) _28.5
Make at% ingot. The melting point of this master alloy is about 838 ° C. Then, a powder of Fe ₉₀ Co ₁₀ at% and a particle size of 200 μm was prepared. This melting point is as high as 1500 ° C, and the porosity of this powder is 43.7%.

This powder is laid on a mold made of isolite with a 4 ″ φ inner diameter, and the master alloy is put on it. After that, it is heated in the atmosphere to 1050 ° C. in a vacuum, and the master alloy is melted and cooled. Remove the body, process the outer circumference, and polish it to 4 "φ
A × 3t sputtering target was prepared. After all, the target composition was three phases of RE, RE-TM, and TM, and the overall composition was Gd ₁₁ Fe _70.2 Co _7.8 at%. And, as a result of evaluating the composition distribution and the magnetic characteristic distribution in the substrate holder by the film forming apparatus and the film forming method similar to those in Examples 3-1 and 3-2,
RE is uniform at 22.0-22.3at% and magnetic properties are Hc of 15.5
Uniform at ~ 16.0 KOe. Almost almost uniform film can be formed in the substrate holder. Also, the amount of oxygen was as low as 300 ppm, the sputtering was stable from the beginning even after standing in the air for 24 hours, and the film magnetic characteristics were also stable from the beginning.

In addition to the composition systems shown in these Examples 3-5, 3-6, 3-7, Tb
Fe, TbCo, GdFeCo, GdDyFeCo, GdDyTbFeCo, DyTbFeCo, GdTbF
The present invention for all composition systems containing at least one heavy rare earth metal of Gd, Tb, Dy such as e, DyCo, TbGdCo, TbDyCo and at least one transition metal of Fe, Co It was confirmed that a manufacturing method is possible and that the same effect is present.

Then, it was confirmed that a method in which the transition metal powder is changed to Fe powder and the Co content of the master alloy is adjusted to make the target Co composition desirable is also possible.

Next, as another example, another manufacturing method of the target of the present invention will be described. This manufacturing method is basically the same as the impregnation method described above, but instead of using TM powder,
TM is used. Foamed TM is, for example, "industrial materials, 1
The skeleton is a spongy metal porous body with high porosity, as seen in the October 987 issue.

Place a foamed TM sheet in the mold and place the RE-TM mother alloy ingot on it. This master alloy composition is a low melting point alloy having a melting point of 1200 ° C. or less in the vicinity of the eutectic composition on the rare earth metal side in the phase diagram. This sheet and the mother alloy are heated to melt the mother alloy, and the molten mother alloy is soaked in the pores of the sheet. When the melted master alloy solidifies, it separates into RE and RE ₁ TM ₂ phases, so the resulting metallic structure of the target becomes the TM phase, RE phase, and RE-TM alloy phase. . In this foamed TM, since TM is not a powder, continuous TM becomes the skeleton. Therefore, the resulting target has an increased strength and toughness in the TM skeleton, making it a very strong target.

Example 4-1 First, as a raw material, a master alloy ingot having a composition of Tb ₇₂ Fe _26.2 Co _1.8 at% is prepared. In addition, foamed F with a composition of Fe _93.6 Co _6.4 at%
Prepare an eCo sheet. This foamed sheet has a porosity of 91.
Since it cannot be used as it is, the foamed sheet was pressed so that the porosity was 43.5%.

This foamed FeCo sheet is laid on a mold made of alumina with a 4 ″ φ inner diameter, and the mother alloy is placed on top of it and placed under vacuum for 10
The atmosphere was heated to 00 ° C. The melting point of the master alloy is as low as about 850 ° C, and the melted master alloy ingot permeates into the expanded FeCo sheet. After cooling, the molded body was taken out from the mold, processed to the outer periphery and polished to prepare a sputtering target of 4 ″ φ × 3t. A schematic diagram of the metal structure of this target is shown in FIG. Metal (Fe _93.6 Co _6.4 ) single phase 171, rare earth metal (Tb) single phase 172, transition metal and rare earth metal alloy phase (TbFeCo) 173 are mixed.The total composition of the target is Tb ₂₂ Fe ₇₃ Co. It was ₅ at%.

This target of the present invention was mounted on the same sputtering apparatus as that shown in FIG. 2, and a film was formed to examine its magnetic characteristics and composition distribution. Film formation conditions are Ar pressure 2.5 mTorr, initial vacuum degree 3 × 10
^-7 Torr, input power was 1.0A340V using DC power supply. FIG. 18 is a composition distribution and magnetic characteristic distribution diagram in a substrate holder using the target of the present invention. As shown in this figure, the composition is uniform with RE of 22.0 to 22.5 at% and Hc of 14.7 at.
Uniform at ~ 15.5KOe. A uniform film is formed almost in the substrate holder. Naturally, this target was not a sintering method, neither the mother alloy nor the TM sheet was a powder, and because it was an infiltration target by total melting, the amount of oxygen was small and was 500 ppm. Also, the packing density was 99.8%, which is a complete packing.

This target also has a very stable discharge from the beginning of sputtering, and DC sputtering is possible with an Ar pressure of 2.5 mTorr. And, even after being left in the air for 24 hours, it exhibits stable film characteristics immediately after sputtering.

Example 4-2 Next, as a raw material, a master alloy ingot having a composition of Dy ₇₂ Fe _26.2 Co _1.8 at% is prepared. In addition, a foamed F with a composition of Fe _93.6 Co _6.4 at%
Prepare an eCo sheet. This foamed FeCo sheet was pressed and adjusted to have a porosity of 43.1%.
The FeCo sheet was laid on a mold made of zirconia with a 4 ″ φ inner diameter, and the mother alloy was placed on it and heated in a vacuum atmosphere at 1050 ° C. After the mother alloy was melted, it was cooled and molded into the mold. Take out the body, process the outer circumference, and polish it to 4 "φ
A 3t sputtering target was created. After all, the target composition was three phases of RE, RE-TM, and TM, and the overall composition was Dy ₂₂ Fe ₇₃ Co ₅ at%. And Example 4-
As a result of evaluating the composition distribution and magnetic property distribution in the substrate holder with the same film forming apparatus and film forming method as in 1, the RE was 21.5 to 22.0.
The magnetic properties are uniform at at%, and the magnetic properties are also uniform at Hc of 13.5-13.0 KOe. The more uniform the film is, the better the film can be placed in the substrate holder. Also, the oxygen content of this target was as small as 430 ppm, and the sputtering was stable from the beginning even after standing in the air for 24 hours, and the film magnetic characteristics were also stable from the beginning.

[Example 4-3] Next, the effect of the method of the present invention was confirmed for TbGdFeCo. The manufacturing method is the same as in Examples 4-1 and 4-2. First, as a raw material, a master alloy ingot containing Tb ₃₆ Gd ₃₆ Fe _26.2 Co _1.8 at% is prepared. Further, a foamed FeCo sheet having a composition of Fe _93.6 Co _6.4 at% was prepared, and pressed to adjust the porosity to 43.5%. Then, this foamed FeCo sheet is laid on a mold made of mullite with a 4 ″ φ inner diameter, and a mother alloy is placed on it.
The atmosphere was heated to 1020 ° C. under vacuum. After the mother alloy was melted, it was cooled and the molded body was taken out from the mold, processed on the outer circumference, and polished to prepare a 4 ″ φ × 3t sputtering target. The target composition was also RE, RE-TM, or TM.
The composition of the whole is Tb ₁₁ Gd ₁₁ Fe ₇₃ Co ₅ at%. Then, the composition distribution and the magnetic characteristic distribution in the substrate holder were evaluated by the same film forming apparatus and film forming method as those in Examples 4-1, 4-2, and as a result, RE was 21.5 to 22.0 at% and the magnetic characteristics were uniform. Hc is uniform at 14 to 15.0 KOe. Almost almost uniform film can be formed in the substrate holder. The oxygen content of this target was as low as 480 ppm, and the sputtering was stable from the beginning even after standing in the air for 24 hours, and the film magnetic characteristics were also stable from the beginning.

In addition to the composition systems shown in these Examples 4-1, 4-2 and 4-3, Tb
Fe, TbCo, GdFeCo, GdDyTbFeCo, DyTbFeCo, GdTbFe, DyCo, TbG
The present invention uses a foam metal for all composition systems containing at least one heavy rare earth metal of Gd, Tb, Dy such as dCo, TbDyCo and at least one transition metal of Fe, Co It was confirmed that a manufacturing method is possible and that the same effect exists.

It was also confirmed that a method in which the foaming transition metal is Fe and the Co content of the master alloy is adjusted to make the Co composition of the target desired is possible.

Next, an example of the production method of the present invention using a foam metal when the target composition contains a light rare earth metal, that is, when it contains a light rare earth metal, a heavy rare earth metal, and a transition metal will be described.

Example 4-4 The effect of the method of the present invention was confirmed for NdDyFeCo. The manufacturing method is the same as in Examples 4-1 and 4-2. First, a master alloy ingot of (Nd _0.2 Dy _0.8 ) _72.2 (Fe _0.8 Co _0.2 ) _27.8 at% is prepared as a raw material. In addition, a foamed composition composed of Fe ₈₀ Co ₂₀ at%
An FeCo sheet was prepared and pressed to adjust the porosity to 62.6%. Then, this foamed FeCo sheet was laid on a mold made of isolite having a 4 ″ φ inner diameter, and a mother alloy was placed on it, and heated in an atmosphere at 1030 ° C. under vacuum. After the mother alloy melted, it was cooled in the mold. The formed body was taken out, processed by an outer mold, and polished to prepare a 4 ″ φ × 3t sputtering target. After all, the target composition is three phases of RE, RE-TM, TM, and the overall composition is Nd _5.5 Dy _22.0 Fe _58.0 Co.
It was _14.5 at%. Then, the composition distribution and the magnetic property distribution in the substrate holder were evaluated by the same film forming apparatus and film forming method as in Examples 4-1, 4-2 and the like, and as a result, RE was 28.0 to 28.5 at% and the magnetic distribution was uniform. The characteristics are even at Hc of 9.7 to 10.5 KOe.
Almost almost uniform film can be formed in the substrate holder. The oxygen content of this target was also low at 475 ppm, and sputtering was stable from the beginning even after being left in the air for 24 hours, and the magnetic properties of the film were also stable from the beginning.

[Example 4-5] Next, the effect of the method of the present invention was confirmed for PrTbDyFeCo. The manufacturing method is the same as in Examples 4-1 and 4-2. First, as a master alloy, (Pr _0.2 Tb _0.4 Dy _0.4 ) ₈₀ (Fe _0.8 Co _0.2 ).
Make a ₂₀ at% ingot. The melting point of this master alloy is about 820 ° C. A foamed FeCo sheet having a composition of Fe ₈₀ Co ₂₀ at% was prepared, and pressed to adjust the porosity to 62.8%. Then, this foamed FeCo sheet is laid on a mold made of alumina with a 4 ″ φ inner diameter, the mother alloy is placed on it, and it is placed under vacuum.
The atmosphere was heated to 1030 ° C. After the mother alloy was melted, it was cooled and the molded body was taken out from the mold, processed by an outer mold and polished to prepare a 4 ″ φ × 3t sputtering target. Again, the target composition was RE, RE-TM, TM. It had three phases, and the overall composition was Pr _5.5 Tb ₁₁ Dy ₁₁ Fe ₅₈ Co _14.5 at%. Then, the substrate was formed by the same film forming apparatus and film forming method as in Examples 4-1 and 4-2. As a result of evaluating the composition distribution and magnetic property distribution in the holder, RE was 28.0 to 27.8 at% and was uniform.
The magnetic properties were also uniform at Hc of 15.5 to 15.8 KOe. Almost almost uniform film can be formed in the substrate holder. The oxygen content of this target was as low as 420 ppm, and the sputtering was stable from the beginning even after being left in the air for 24 hours, and the magnetic properties of the film were also stable from the beginning.

[Example 4-6] Next, the effect of the method of the present invention was confirmed for PrSmDyGdFeCo. The manufacturing method is the same as in Examples 4-1 and 4-2,
First, as a master alloy (Pr _0.1 Sm _0.1 Dy _0.4 Gd _0.4 ) _72.2 (Fe
_0.8 Co _0.2 ) Make a _20.8 at% ingot. The melting point of this ingot is 88
It is about 0 ° C. In addition, a foamed F composed of Fe ₈₀ Co ₂₀ at%
An eCo sheet was prepared and pressed to adjust the porosity to 63.1%. Then, this foamed FeCo sheet was laid on a mold made of alumina having a 4 ″ φ inner diameter, and the mother alloy was placed on it and heated under atmosphere at 1040 ° C. under vacuum. The formed body was taken out, processed with an outer mold, and polished to prepare a 4 ″ φ × 3t sputtering target. After all, the target composition is three phases of RE, RE-TM, TM, and the overall composition is Pr _2.75 Sm _2.75 Dy ₁₁ Gd ₁₁
It was Co _14.5 at%. Then, as a result of evaluating the composition distribution and the magnetic property distribution in the substrate holder by the film forming apparatus and the film forming method similar to those in Examples 4-1, 4-2 and the like, RE was 28.0 to 28.1 at% and the magnetic distribution was uniform. The properties were even at Hc of 7.2 to 7.5 KOe. Almost almost uniform film can be formed in the substrate holder. The oxygen content of this target is also 490p
Sputtering was stable from the beginning even after being left in the atmosphere for 24 hours, and the magnetic properties of the film were also stable from the beginning.

In addition to the composition systems shown in these Examples 4-4, 4-5, and 4-6, Nd
GdFeCo, NdTbFeCo, NdPrDyFeCo, NdPrDyTbFeCo, PrDyFeCo, N
S such as dSmGdFeCo, PrTbFeCo, CeNdDyFeCo, CeNdPrDyFeCo
At least one light rare earth metal among m, Nd, Pr and Ce, at least one heavy rare earth metal among Gd, Dy and Tb, and at least one transition metal among Fe and Co The production method of the present invention is possible for all composition systems including
It was also confirmed that a similar effect exists.

It was also confirmed that a method in which the foaming transition metal is Fe and the Co content of the master alloy is adjusted to make the target Co composition desirable is also possible.

In the impregnation method or the infiltration method, which is one of the methods of the present invention, the porosity of the powder or foam sheet becomes important. This is because the molten ingot penetrates into the pores of the powder or foam sheet to form the target, and the target composition is determined by the porosity. That is, the target having a desired composition must be provided by controlling the porosity.

Since the composition of the medium is required to have a rare earth metal content of about 15 at% to 35 at%, the composition of the target must be adjusted accordingly. In order to satisfy this, the target composition is to be adjusted by variously changing the porosity of the powder or foam metal.

A specific brief description will be given. Prepare a powder with a porosity of about 30% and place the ingot on it. It is shown in FIG. 19 (a). The state where the ingot is melted and impregnated in the powder is
It is FIG. 19 (b). It can be seen that the molten ingot enters only the pores in the powder. Next, a powder having a porosity of 80% was prepared, and an ingot was placed on the powder, as shown in FIG. 20 (a). Similarly, the state where the ingot is melted and impregnated in the powder is
Fig. 20 (b). By doing so, the porosity of the powder can be controlled and the composition can be determined.

[Example 5-1] With respect to NdDyFeCo, powders having various porosities and foamed TM sheets were prepared, and a sputtering target was prepared by the impregnation method which is the manufacturing method of the present invention.

As mother alloy (Nd _0.2 Dy _0.8 ) _72.2 (Fe _0.8 Co _0.2 ) _27.8
Make at% ingot. And next, Fe ₈₀ Co ₂₀ at% 200μm
A powder having a particle size was prepared. Porosity of powder is 30%, 40%, 50
%, 62%, 70%, 80% were prepared. The porosity can be controlled by preparing spherical particles and irregular particles. Similarly, prepare a metal foam sheet of Fe ₈₀ Co ₂₀ at% and press it to obtain porosities of 30%, 40%, 50%, 62%, 70%.
%, 80% were prepared. By the same manufacturing method as in Examples 3-1 and 4-4 above, sputtering targets using FeCo powders or foamed FeCo sheets having different porosities were prepared. The following table shows the porosity of the powder used and the resulting target composition, and the porosity of the foam sheet and the achieved target composition.

Targets with different porosity of FeCo or FeCo
Using a target with a different porosity of the foamed sheet, a film was formed by the same sputtering device as in FIG. 2 and the composition distribution in the substrate holder was observed. FIG. 21 is a composition distribution diagram of a target using various porosity powders, and FIG. 22 is a composition distribution diagram of a target using various porosity foam sheets.

211 is a composition distribution formed by a target having a porosity of 30% powder, 212 is a composition distribution formed by a target having a porosity of 40% powder, and 213 is a composition distribution formed by a target having a porosity of 50% powder. , 214 is a composition distribution formed by a target having a porosity of 62% powder, 215 is a composition distribution formed by a target having a porosity of 70% powder, and 216 is a composition formed by a target having a porosity of 80% powder Distribution. Further, 221 is a composition distribution formed by a target of a foam sheet having a porosity of 30%, 222 is a composition distribution formed by a target of a foam sheet having a porosity of 40%, and 223 is a target of a foam sheet having a porosity of 50%. Compositional distribution of the deposited film, 224 is porosity 6
The composition distribution formed with the target of 2% foam sheet, 225 is the composition distribution formed with the target of foam sheet 70% porosity, and 226 is the composition distribution formed with the target of foam sheet 80% porosity. . In any of these targets, the composition distribution formed by the target according to the manufacturing method of the present invention is extremely small and shows good uniformity, and the film composition can be variously changed by controlling the porosity. is there.

Other composition systems, PrTbFeCo, SmGdFeCo, SmDyTbFeCo, NdTbFeC
o, NdGdFeCo, NdPrDyFeCo, NdPrDyTbFeCo, PrDyFeCo, NdSmGd
TbFeCo, CeNdDyFeCo, CeNdPrDyFeCo and other Sm, Nd, Pr, Ce at least one light rare earth metal and Gd, Dy, Tb at least one heavy rare earth metal, and Fe, Co It was confirmed that the method of the present invention is effective for all composition systems containing at least one transition metal of

[Example 5-2] Next, regarding TbFeCo, powders having various porosities and foaming TM
A sheet was prepared and a sputtering target was prepared by the impregnation method which is the manufacturing method of the present invention.

As a master alloy, an ingot of Tb ₇₂ (Fe _0.9 Co _0.1 ) ₂₈ at% is made. Then, a powder of Fe ₉₀ Co ₁₀ at% and a particle size of 200 μm was prepared. Porosity of powder is 30%, 43%, 50%, 60%, 70%, 8
0% was used, and the porosity was controlled by preparing spherical particles to irregular shapes. Also, Fe ₉₀
A foamed metal sheet of Co ₁₀ at% was prepared and pressed to have porosities of 30%, 43%, 50%, 60%, 70% and 80%.
Using the same manufacturing method as in Examples 3-5 and 4-1, a sputtering target was prepared using FeCo powder or foamed FeCo sheet having different porosities. The following table shows the porosity of the powder used and the resulting target composition, and the porosity of the foam sheet and the achieved target composition.

Targets with different porosity of FeCo or FeCo
Using a target with a different porosity of the foamed sheet, a film was formed by the same sputtering device as in FIG. 2 and the composition distribution in the substrate holder was observed. FIG. 23 is a composition distribution diagram of a target using various porosity powders, and FIG. 24 is a composition distribution diagram of a target using various porosity foam sheets.

231 is a composition distribution formed by a target having a porosity of 30% powder, 232 is a composition distribution formed by a target having a porosity of 43% powder, and 233 is a composition distribution formed by a target having a porosity of 50% powder. , 234 is a composition distribution formed by a target having a porosity of 60% powder, 235 is a composition distribution formed by a target having a porosity of 70% powder, and 236 is a composition formed by a target having a porosity of 80% powder Distribution. Further, 241 is a composition distribution formed by a target having a porosity of 30% foamed sheet, 242 is a composition distribution formed by a target having a porosity of 43% foamed sheet, and 243 is a target having a porosity of 50% foamed sheet. The composition distribution of the deposited film, 244 is the porosity 6
The composition distribution formed with the target of 0% foam sheet, and 245 is the composition distribution formed with the target of foam sheet of 70% porosity. 246 is a composition distribution formed by forming a film on a foamed sheet target having a porosity of 80%. In any of these targets, the composition distribution formed by the target according to the manufacturing method of the present invention is extremely small and shows good uniformity, and the film composition can be variously changed by controlling the porosity. Is.

Other composition systems, DyFeCo, TbGdFeCo, TbFe, CdFeCo, GdDyFeC
o, GdDyTbFeCo, DyTbFeCo, GdTbFe, TbDyCo and other Gd, Tb, Dy heavy rare earth metals of at least one or more, and all composition systems containing at least one or more transition metals of Fe, Co It was confirmed that the invention method was available.

Next, in the preparation of the method target of the present invention using a transition metal powder, the target was prepared by preparing powders having different particle diameters.

[Example 6-1] The basic production method is the same as that of Example 3-1, and a (Nd _0.2 Dy _0.8 ) _72.2 (Fe _0.8 Co _0.2 ) _27.8 at% mother alloy ingot was prepared as a raw material (4 ″ Φ × 4t), then various powders with different particle size of Fe ₈₀ Co ₂₀ at% are prepared. Using these, the mother alloy is placed on the powder and heated at 1000 ° C. in a vacuum atmosphere, and the sputtering target is used. Was created. The result is 4 ″ φ
Create a target of × 6t.

The average particle size of the powder used was 5μm, 8μm, 10μm, 24μm, 3
8 μm, 53 μm, 120 μm, 230 μm, 570 μm, 730 μm, 1 mm, 1.5 mm, 2
mm, 3 mm, 3.2 mm, 4 mm.

The table below shows the finished state of the target for the powder used.

From the results shown in the above table, it is understood that when powders having an average particle size of 5 μm and 8 μm are used, the target cannot be manufactured without the master alloy infiltrating. This is because the particle size of the powder is too small, and the pores themselves are too small, and there is a relationship with the viscosity of the melted master alloy solution, so that the particles do not penetrate. A powder having an average particle size of 10 μm or more can be a 100% impregnated target.

A target using a powder having an average particle diameter of 10 μm or more in the above table was mounted on the sputtering apparatus shown in FIG. 2 to attempt film formation. All targets had stable discharge from the beginning of sputtering, and there was no problem. Each target was sputtered for a long time and the relationship with the magnetic properties of the film was observed. FIGS. 25 and 26 are diagrams showing the dependence of the magnetic properties of the film on the sputtering time.
251 is a target using 10 μm particle size powder, 252 is a target using 24 μm particle size powder, 253 is a target using 38 μm particle size powder, 254 is a target using 53 μm particle size powder, 2
55 is a target using 120 μm particle size powder, 256 is 230 μm
The target using the particle size powder and 257 are the targets using the 570 μm particle size powder.

It was confirmed that the target using the powder having a particle size of 10 μm to 570 μm has a constant magnetic film property over the entire sputtering time and is sufficiently usable. The magnetic properties of the film are different for each target because the porosity of the powder is different and therefore the target composition is different, which is not directly related to the purpose of this embodiment. 26
1 is a target using 730 μm particle size powder, 262 is a target using 1.0 mm particle size powder, 263 is a target using 1.5 mm particle size powder, 264 is a target using 2.5 mm particle size powder, 265 is
A target using 3.0 mm particle size powder, 266 is a target using 3.2 mm particle size powder, and 267 is a target using 4.0 mm particle size powder. It was confirmed that the target using 730 μm to 2.5 mm particle size powder has a constant magnetic film property over the entire sputtering time and is sufficiently usable. In the target using 3.0 mm particle size powder, the magnetic properties of the film fluctuate slightly depending on the sputtering time. This is because the size of the particles has increased and the ratio of RE, RE-TM, TM on the target surface changes depending on the sputtering time.

However, if the particle size is around 3.0 mm, even during fluctuation,
It is possible to use it without being too large. However, it was found that the target using 3.2 mm grain size powder and the target using 4.0 mm grain size powder could not be used because the fluctuation of the magnetic properties of the film was too large. Therefore, in order to manufacture the target of the present invention, it is necessary that the TM powder has an average particle size of 10 μm or more and 3.0 mm or less.

Other composition systems, PrTbFeCo, SmGdFeCo, SmDyTbFeCo, NdTbFeC
o, NdGdFeCo, NdPrDyFeCo, NdPrDyTbFeCo, PrDyFeCo, NdSmGd
TbFeCo, CeNdDyFeCo, CeNdPrDyFeCo and other Sm, Ns, Pr, Ce at least one light rare earth metal, and Gd, Dy, Tb at least one heavy rare earth metal, and Fe, Co It was confirmed that it is necessary to use the particle size in the same range for all the composition systems containing at least one or more kinds of transition metals.

[Example 6-2] Next, as TbFeCo, those having different TM powder particle sizes were prepared, and the same production method as in Example 3-5 was tried.

As a raw material, a master alloy ingot of Tb ₇₂ (Fe _0.9 Co _0.1 ) ₂₈ at% was prepared (4 ″ φ × 4t), and then various powders of Fe ₉₀ Co ₁₀ at% having different particle sizes were prepared. Using, the mother alloy was placed on the powder and heated in a vacuum atmosphere at 1010 ° C. to prepare a sputtering target. The finished target was 4 ″.
φ × 6t.

The average particle size of the powder used is 5μm, 8μm, 10μm, 24μ
m, 38 μm, 53 μm, 120 μm, 230 μm, 570 μm, 730 μm, 1 mm, 1.5 m
It is m, 2mm, 3mm, 3.2mm, 4mm. The table below shows the finished state of the target for the powder used.

From the results shown in the above table, it is understood that when powders having an average particle size of 5 μm and 8 μm are used, the target cannot be manufactured without the master alloy infiltrating. This is because the particle size of the powder is too small, and the pores themselves are too small, and there is a relationship with the viscosity of the melted master alloy solution, so that the particles do not penetrate. A powder having an average particle size of 10 μm or more can be a 100% impregnated target.

A target using a powder having an average particle diameter of 10 μm or more in the above table was mounted on the sputtering apparatus shown in FIG. 2 to attempt film formation. All targets had stable discharge from the beginning of sputtering, and there was no problem. Each target was sputtered for a long time and the relationship with the magnetic properties of the film was observed. FIG. 27 and FIG. 28 are diagrams showing the dependence of the magnetic properties of the film on the sputtering time.
271 is a target using 10 μm particle size powder, 272 is a target using 24 μm particle size powder, 273 is a target using 38 μm particle size powder, 274 is a target using 53 μm particle size powder, 2
75 is a target using 120 μm particle size powder, 276 is 230 μm
A target using a particle size powder and 277 is a target using a 570 μm particle size powder.

It was confirmed that the target using the powder having a particle size of 10 μm to 570 μm has a constant magnetic film property over the entire sputtering time and is sufficiently usable. The magnetic properties of the film are different for each target because the porosity of the powder is different and therefore the target composition is different, which is not directly related to the purpose of this embodiment. 28
1 is a target using 730 μm particle size powder, 282 is a target using 1.0 mm particle size powder, 283 is a target using 1.5 mm particle size powder, 284 is a target using 2.5 mm particle size powder, and 285 is
A target using 3.0 mm particle size powder, 286 is a target using 3.2 mm particle size powder, and 287 is a target using 4.0 mm particle size powder. It was confirmed that the target using 730 μm to 2.5 mm particle size powder has a constant magnetic film property over the entire sputtering time and is sufficiently usable. In the target using 3.0 mm particle size powder, the magnetic properties of the film fluctuate slightly depending on the sputtering time. This is because the size of the particles has increased and the ratio of RE, RE-TM, TM on the target surface changes depending on the sputtering time.

However, if the particle size is around 3.0 mm, even during fluctuation,
It is possible to use it without being too large. However, it was found that the target for use with 3.2 mm grain size powder and the target for 4.0 mm grain size powder cannot be used because the fluctuation of the magnetic properties of the film is too large. Therefore, in order to manufacture the target of the present invention, it is necessary that the TM powder has an average particle size of 10 μm or more and 3.0 mm or less.

Other composition systems DyFeCo, TbGdFeCo, TbFe, GdFeCo, GdDyFeCo, G
Gd, Tb, Dy such as dDyTbFeCo, DyTbFeCo, TbCo, GdTbFe, TbDyCo
It has been confirmed that it is necessary to use the same range of particle sizes for all composition systems containing at least one heavy rare earth metal and at least one transition metal selected from Fe and Co.

Next, in the preparation of the target of the method of the present invention using a foamed transition metal sheet, the target was prepared by preparing foamed metal having various pore diameters.

The reason why the foamed transition metal sheet is used is that the pores are required in the metal in order to infiltrate the molten metal. This is because it is possible to predict that the foamed transition metal sheet has the same action and effect as the powder, paying attention to the fact that it is necessary to make the foamed structure in which the foamed structure is continuous or the bubbles are connected.

[Example 7-1] With respect to FeDyFeCo, various foamed transition metals having different pore sizes were prepared, and the same manufacturing method as in Example 4-4 was tried.

As a raw material (Nd _0.2 Dy _0.8 ) _72.2 (Fe _0.8 Co _0.2 ) _27.8 at
% Master alloy ingot (4 ″ φ × 4t), then Fe ₈₀ Co ₂₀
Various foam sheets having different at% pore diameters were prepared, and using these, a mother alloy was placed on the foam sheets and heated at 1000 ° C. in a vacuum atmosphere to prepare a sputtering target. The finished target is a 4 ″ φ × 6t target.

The average pore diameter of the used foam metal is 5μm, 8μm, 10μm, 2
4μm, 38μm, 53μm, 120μm, 230μm, 570μm, 730μm, 1mm,
They are 1.5mm, 2mm, 3mm, 3.2mm and 4mm.

The following table shows the finished state of the target for the foam metal used.

From the results in the above table, it is understood that when a foam metal having an average pore diameter of 5 μm or 8 μm is used, the target cannot be manufactured because the mother alloy does not penetrate. This is because the pore diameter of the foam metal is too small and is related to the viscosity of the melted mother alloy solution, so that it does not penetrate. Foamed metal having an average pore diameter of 10 μm or more can be made into a 100% impregnated target.

A target using a foam metal having an average pore diameter of 10 μm or more in the above table was attached to the sputtering apparatus shown in FIG. 2 to attempt film formation. All targets had stable discharge from the beginning of sputtering, and there was no problem. Each target was sputtered for a long time and the relationship with the magnetic properties of the film was observed. Fig. 29, Fig.
Fig. 30 shows the sputtering time dependence of the magnetic properties of the film. 291 is a target using a foam metal with a pore size of 10 μm, 2
92 is a target using a 24 μm pore diameter foam metal, 293 is 3
8μm pore size target using foam metal, 294 is 53μm
A target using a foam metal having a pore diameter, 295 is a target using a foam metal having a pore diameter of 120 μm, 296 is a target using a foam metal having a pore diameter of 230 μm, and 297 is a target using a foam metal having a pore diameter of 570 μm.

It was confirmed that the target using a foam metal having a pore diameter of 10 μm to 570 μm had a constant magnetic film property over the entire sputtering time and was sufficiently usable. The magnetic properties of the film are different for each target because the porosity of the powder is different and therefore the target composition is different, which is not directly related to the purpose of this embodiment. 301 is a target using 730 μm pore size foam metal,
302 is a target using 1.0 mm pore diameter foam metal, 303 is
Target with foam metal of 1.5mm pore size, 304 is 2.5mm
A target using a foam metal having a pore diameter, 305 is a target using a foam metal having a pore diameter of 3.0 mm, 306 is a target using a foam metal having a pore diameter of 3.2 mm, and 307 is a target using a foam metal having a pore diameter of 4.0 mm. It was confirmed that the target with 730 μm to 2.5 mm pore diameter foam metal has a constant magnetic film property over the entire sputtering time and is sufficiently usable. In the target using a foam metal with a 3.0 mm pore diameter, the magnetic properties of the film fluctuate slightly depending on the sputtering time.
This is because the size of the holes has increased and the ratio of RE, RE-TM, TM on the target surface fluctuates depending on the sputtering time.

However, as long as it has a porosity of about 3.0 mm, it can be used without being so large even during fluctuation. However, it was found that the targets using a foam metal with a pore diameter of 3.2 mm and the target using a foam metal with a pore diameter of 4.0 mm could not be used because the fluctuations of the magnetic properties of the film were too large. Therefore, in order to manufacture the target of the present invention, the YM foam metal has an average pore diameter of 10 μm or more and 3.0 mm.
It is necessary that:

Other composition systems PrTbFeCo, SmGdFeCo, SmDyTbFeCo, NdTbFeCo,
NdGdFeCo, NdPrDyFeCo, NdPrDyTbFeCo, PrDyFeCo, NdSmGdTb
FeCo, CeNdDyFeCo, CeNdPrDyFeCo and other Sm, Nd, Pr, Ce at least one light rare earth metal, Gd, Dy, Tb at least one or more heavy rare earth metal, and Fe, Co It was confirmed that it is necessary to use the same range of pore diameters for all composition systems containing at least one transition metal.

[Example 7-2] Next, with respect to TbFeCo, different foamed transition metals having different pore diameters were prepared, and the same production method as in Example 4-1 was tried.

As a raw material, prepare a master alloy ingot of Tb ₇₂ (Fe _0.9 Co _0.1 ) ₂₈ at% (4 ″ φ × 4t), then prepare various foamed metals of Fe ₉₀ Co ₁₀ at% with different pore diameters, Using these, a mother alloy was placed on the foam metal and heated in a vacuum atmosphere at 1010 ° C. to prepare a sputtering target. The finished target was 4 ″ φ × 6t.

The average pore diameter of the used foam metal is 5μm, 8μm, 10μm, 2
4μm, 38μm, 53μm, 120μm, 230μm, 570μm, 730μm, 1mm,
They are 1.5mm, 2mm, 3mm, 3.2mm and 4mm. The following table shows the finished state of the target for the foam metal used.

From the results in the above table, it is understood that when a foam metal having an average pore diameter of 5 μm or 8 μm is used, the target cannot be manufactured because the mother alloy does not penetrate. This is because the pore diameter of the foam metal is too small and is related to the viscosity of the melted mother alloy solution, so that it does not penetrate. Foamed metal having an average pore diameter of 10 μm or more can be made into a 100% impregnated target.

A target using a foam metal having an average pore diameter of 10 μm or more in the above table was attached to the sputtering apparatus shown in FIG. 2 to attempt film formation. All targets had stable discharge from the beginning of sputtering, and there was no problem. Each target was sputtered for a long time and the relationship with the magnetic properties of the film was observed. Fig. 31, Fig.
Fig. 32 shows the dependence of the magnetic properties of the film on the sputtering time. 311 is a target using a foam metal with a pore size of 10 μm, 3
12 is a target using a 24 μm pore diameter foam metal, 313 is 3
8μm pore size target using foam metal, 314 is 53μm
315 is a target using a 120 μm pore diameter foam metal, 316 is a target using a 230 μm pore diameter foam metal, and 317 is a target using a 570 μm pore diameter foam metal.

It was confirmed that the target using a foam metal having a pore diameter of 10 μm to 570 μm had a constant magnetic film property over the entire sputtering time and was sufficiently usable. The magnetic properties of the film are different for each target because the porosity of the powder is different and therefore the target composition is different, which is not directly related to the purpose of this embodiment. 321 is a target using a 730 μm pore diameter foam metal,
322 is a target using a foam metal with a 1.0 mm pore size, 323 is
Target with 1.5 mm pore size foam metal, 324 is 2.5 mm
A target using a foam metal having a pore diameter, 325 is a target using a foam metal having a pore diameter of 3.0 mm, 326 is a target using a foam metal having a pore diameter of 3.2 mm, and 327 is a target using a foam metal having a pore diameter of 4.0 mm. It was confirmed that the target with 730 μm to 2.5 mm pore diameter foam metal has a constant magnetic film property over the entire sputtering time and is sufficiently usable. In the target using a foam metal with a 3.0 mm pore diameter, the magnetic properties of the film fluctuate slightly depending on the sputtering time.
This is because the size of the holes has increased and the ratio of RE, RE-TM, TM on the target surface fluctuates from the sputtering time.

However, if the porosity diameter is about 3.0 mm, it is possible to use it too much during the fluctuation. However, it was found that the targets using a foam metal with a pore diameter of 3.2 mm and the target using a foam metal with a pore diameter of 4.0 mm could not be used because the fluctuations of the magnetic properties of the film were too large. Therefore, in order to manufacture the target of the present invention, the TM foam metal needs to have an average pore diameter of 10 μm or more and 3.0 mm or less.

Other composition systems, DyFeCo, TbGdFeCo, TbFe, GdFeCo, GdDyFeC
Tb, Dy such as o, GdDyTbFeCo, DyTbFeCo, TbCo, GdTbFe, TdDyCo
It has been confirmed that it is necessary to use the same range of pore diameters for all composition systems containing at least one heavy rare earth metal among them and at least one transition metal among Fe and Co.

As described above, in the impregnation method or the infiltration method, which is one of the methods of the present invention, the porosity, particle size, and pore diameter of the powder or foam metal are important, and it is necessary to use those having a specific range. I found out that there is. On the other hand, the composition of the mother alloy is also important, and the mother alloy melting point for impregnation and the metal structure of the mother alloy, that is, the ratio of the rare earth single layer and the alloy phase of the rare earth ₁ transition metal ₂ are mixed, The alloy composition is determined. A specific example will be described below.

[Example 8-1] The present invention when preparing NdDyFeCo by the impregnation method is described in Example 3
-1,4-4, etc., and (Nd _0.2
Dy _0.8 ) _72.2 (Fe _0.8 Co _0.2 ) _27.8 at% composition is used. This composition is near the eutectic composition on the rare earth metal (RE) side in the phase diagram and has a low melting point (about 830 ° C.), which is convenient for preparation by the impregnation method. In the present example, it was investigated up to what range the composition of the master alloy could be used to prepare a target by the impregnation method.

Using the same Fe-Co powder (porosity 62.4%) as in Example 3-1, various master alloy compositions were prepared, and targets were prepared by the impregnation method. The following table shows the mother alloy composition used, the melting point of that composition, and the finished state of the impregnated target prepared by heating at that melting point.

From the results in the above table, it is understood that when the mother alloy having a melting point of more than 1200 ° C. is used, a part of the Fe—Co powder begins to melt and the impregnation method cannot be used. The target using the master alloy having a melting point of 1200 ° C or lower did not dissolve FeCo powder, and the target was finely formed by the impregnation method. In other words, the mother alloy composition has a melting point
It is necessary to use a temperature below 1200 ° C.

Other composition systems, PrTbFeCo, SmGdFeCo, SmDyTbFeCo, NdTbFeC
o, NdGdFeCo, NdPrDyFeCo, NdPrDyTbFeCo, PrDyFeCo, NdSmGd
Of Sm, Nd, Pr, Ce such as TbFeCo, CeNdDyFeCo, CeNdPrDyFeCo, at least one light rare earth metal, and at least one heavy rare earth metal of Gd, Dy, Tb, and Fe, Co It was confirmed that it is necessary to use a mother alloy having a melting point in the same range for all composition systems containing at least one or more transition metals.

[Example 8-2] With TbFeCo, various master alloy compositions were prepared, and a target was prepared by an impregnation method. The production method is the same as the method shown in Example 3-5. We prepared powders of Fe ₉₀ Co ₁₀ at% with porosity of 43% and prepared impregnation targets using various master alloy compositions. The following table shows the mother alloy composition used, the melting point of that composition, and the finished state of the impregnated target prepared by heating at that melting point.

From the results in the above table, the melting point is 1200 as well as NdDyFeCo.
It can be seen that when the mother alloy having a temperature higher than 0 ° C is used, a part of the Fe-Co powder begins to melt and the impregnation method cannot be used. 1200 ℃
The target using the master alloy having the following melting point did not dissolve the FeCo powder, and the target was finely formed by the impregnation method. That is, it is necessary to use a master alloy having a melting point of 1300 ° C. or less.

Other composition systems, DyFeCo, TbGdFeCo, TbFe, GdFeCo, GdDyFeC
o, GdDyTbFeCo, DyTbFeCo, TbCo, GdTbFe, TbDyCo and other Gd, Tb,
Fe, Co and at least one heavy rare earth metal of Dy
It was confirmed that it is necessary to use a master alloy having a melting point in the same range for all the composition systems containing at least one kind of transition metal among them.

The metal structures of the finished targets differ depending on the various master alloy compositions used in the NdDyFeCo and TbFeCo systems shown in Examples 8-1 and 8-2. In other words, the amount of RE ₁ -TM ₂ intermetallic compound phase is different. If the master alloy composition of RE ₄₀ side, for example, RE ₄₀ TM ₆₀ , is used, the intermetallic compound phase is increased. Conversely, if the master alloy composition of RE ₈₉ TM ₁₁ , for example, is used, the intermetallic compound phase is increased. Less. For these mother alloy compositions, an optimum mother alloy composition is selected depending on the sputtering apparatus or film forming method used.

When the amount of the intermetallic compound phase cannot be controlled only by the composition of the master alloy, the following method may be adopted.
That is, the intermetallic compound phase is controlled by heat-treating the finished target again at a temperature lower than the melting point.

[Example 9-1] Various heat treatments were performed using the NdDyFeCo-impregnated target prepared in Example 3-1, and the amount of the intermetallic compound phase of (NdDy) ₁ (FeCo) ₂ was examined. . The heat treatment conditions and the amount of the intermetallic compound phase are shown in the following table. The heat treatment was performed in vacuum without pressure.

As shown in the table above, the higher the temperature and the longer the time, the greater the amount of intermetallic compound. Since this is a phenomenon caused by solid phase diffusion, it is natural that there is a relationship between temperature and time.

The optimum value of the amount of these intermetallic compounds is determined by the sputtering device and the sputtering method. Specific examples will be described below.

In the case of the sputtering apparatus as shown in FIG. 2, if the substrate holder 22 is rotating and the substrate to be mounted rotates on its axis (that is, the substrate rotates on its axis), what is the amount of intermetallic compound? But it doesn't matter.
However, if it is a method in which the substrate does not rotate (that is, only revolution), the amount of intermetallic compound is preferably about 10 to 30 area%. Of these, the optimum amount is determined by the distance between the target substrates, the distance between the target center and the substrate holder center, and the sputtering conditions (Ar pressure, Power).

In the case of a sputtering device as shown in Fig. 33, 33
The target of 1 and the substrate of 332 face each other, and the substrate is also stationary without moving. In this case, the amount of intermetallic compound is 15-40 ar
ea% is good. Which of these is optimal depends on the distance between the target substrates and the sputtering conditions (Ar pressure, Power).

In the case of a sputtering device as shown in Fig. 34 in which the substrate passes over the target, the amount of intermetallic compound is 20-60 ar.
ea% is good (341 is target, 342 is substrate). The optimum amount among these is determined by the distance between the target substrates, the sputtering conditions (Ar pressure, Power), and the presence or absence of the deposition preventive plate.

Other composition systems PrTbFeCo, SmGdFeCo, SmDyTbFeCo, NdTbFeCo,
NdGdFeCo, NdPrDyFeCo, NdPrDyTbFeCo, PrDyFeCo, NdSmGdTb
FeCo, CeNdDyFeCo, CeNdPrDyFeCo and other Sm, Nd, Pr, Ce at least one light rare earth metal and Gd, Dy, Tb at least one heavy rare earth metal and at least Fe, Co Similar results as in this example were obtained for all composition systems containing one or more transition metals.

[Example 9-2] Using the TbFeCo-impregnated target prepared in Example 3-5, various heat treatments were carried out to see what the amount of the intermetallic compound phase of Tb ₁ (FeCo) ₂ would be. The heat treatment conditions and the amount of the intermetallic compound phase are shown in the following table. The heat treatment was performed in vacuum without pressure.

Similar to the case of Example 9-1, the higher the temperature of the heat treatment and the longer the time, the greater the amount of intermetallic compound.

The optimum value of the amount of these intermetallic compounds depends on the sputtering device and the sputtering method.

Other composition systems, DyFeCo, TbGdFeCo, TbFe, GdFeCo, GdDyFeC
o, GdDyTbFeCo, DyTbFeCo, TbCo, GdTbFe, TbDyCo and other Gd, Tb,
Fe, Co and at least one heavy rare earth metal of Dy
The same results as in this example were obtained for all the composition systems containing at least one or more of the above transition metals.

Among the methods of the present invention described so far, when powder or foam metal is used, and a master alloy ingot is placed on it, and the production is carried out by the impregnation method, the composition of the powder or foam metal should be controlled to control the composition. Porosity needs to be controlled. The method described below uses powder, but the composition can be controlled without controlling the porosity.

Briefly, the transition metal powder and the powder obtained by crushing the rare earth transition metal alloy ingot in the vicinity of the eutectic composition are appropriately mixed and thoroughly mixed until uniform. After that, this mixed powder is put in a mold, heated to about 1000 ° C., cooled, and then the molded body is processed to form a target.

Example 10-1 NdDyFeCo will be described. First, as raw material (Nd _0.2 Dy
_0.8 ) _72.2 (Fe _0.8 Co _0.2 ) _27.8 at% master alloy ingot is made. After roughly crushing this ingot with a jaw crusher, it is crushed with a ball mill etc. until the average particle size becomes 200 μm. Then, a powder of Fe ₈₀ Co ₂₀ at% having a particle diameter of 200 μm is prepared and sufficiently mixed with the above master alloy powder. This FeCo powder and NdDy
The total amount of FeCo master alloy powder was Nd _5.5 Dy _22.0 Fe _58.0 Co.
They are mixed in a quantity ratio of _14.0 at%. Then, this mixed powder is put into a crucible having a 4 ″ φ inner diameter, and after being evacuated, it is heated to 1050 ° C. in a non-pressurized state.At this time, the master alloy powder is melted and the FeCo powder is not melted. When the melted master alloy surrounds the surrounding FeCo powder and is cooled, the melt of the master alloy is separated into two phases, NdDy and (NdDy) ₁ (FeCo) ₂ , and a target with three phases mixed is completed.

Since the composition of the finished target is determined by the ratio of the amount of the mother alloy powder to be initially mixed with the FeCo powder, the porosity of the powder is not required to be controlled and is easy to control.

The target thus formed was mounted on the same sputtering apparatus as that shown in FIG. 2 to form a film, and its magnetic characteristics and composition distribution were evaluated. As a result, RE was 28 to 28.5 at% and Hc was 9.7.
Uniform at ~ 10.5 KOe. Also, the amount of oxygen was as small as 490 ppm, the sputtering was stable from the beginning even after standing for 24 hours in the air, and the film magnetic characteristics were also stable from the beginning.

This manufacturing method uses powder, but not the sintering method, because one master alloy powder is completely dissolved, the packing density is also 99.3%, and surface oxidation does not proceed to the inside even if left in the atmosphere. Absent.

Other composition systems, PrTbFeCo, SmGdFeCo, SmDyTbFeCo, NdTbFeC
o, NdGdFeCo, NdPrDyFeCo, NdPrDyTbFeCo, PrDyFeCo, NdSmGd
TbFeCo, CeNdDyFeCo, CeNdPrDyFeCo, etc. Sm, Nd, Pr, and Ce, for all composition systems containing at least one heavy rare earth metal and at least one transition metal of Fe and Co, It was also confirmed that the same manufacturing method is possible and that the same effect exists.

Example 10-2 Next, TbFeCo will be described. First, Tb ₇₂ Fe as a raw material
_26.2 Co Make a _1.8 at% mother alloy ingot. After roughly crushing this ingot with a jaw crusher, 200
Grind until the average particle size is μm. And Fe _93.6 Co _6.4 a
Prepare t% powder having a particle size of 200 μm and thoroughly mix it with the mother alloy powder. The amounts of the FeCo powder and the TbFeCo master alloy powder are mixed in a total amount ratio of Tb ₂₂ Fe ₇₃ Co ₅ at%. Then, this mixed powder was put into a 4 ″ φ inner diameter alumina mold and heated in an atmosphere at 1050 ° C. under vacuum. After that, the formed body was processed into a sputtering target. Tb ₁ (FeCo) ₂ , FeCo 3
It consists of phases.

Then, it was mounted on the same film forming apparatus as shown in Fig. 2, and the film formation was tried. As a result of evaluating the composition distribution and magnetic characteristic distribution in the substrate holder, RE was 21.5 to 22.0 at% and the magnetic characteristic was also uniform.
Hc was uniform at 14.5-15.2 KOe. The target oxygen content was 440 ppm and the packing density was 99.5%. The sputtering was stable from the beginning even after being left in the air for 24 hours, and the film magnetic characteristics were also stable from the beginning.

Other composition systems, DyFeCo, TbGdFeCo, TbFe, GdFeCo, GdDyFeC
o, GdDyTbFeCo, DyTbFeCo, TbCo, GdTbFe, TbDyCo and other Gd, Tb,
The same manufacturing method is possible and has the same effect for all composition systems containing at least one heavy rare earth metal of Dy and at least one transition metal of Fe and Co. It was also confirmed to do.

Even in the case of the method of the present invention (Examples 10-1 and 10-2), the total composition must have a melting point of 1200 ° C. or less, and needless to say, as in Examples 8-1 and 8-2. Is.

The transition metal powder or foamed transition metal used in the present invention (Example 1-1) to (Example 10-2) described above is based on FeCo alloy.
It was confirmed that RE-FeCo can be used as the mother alloy when RE-FeCo is used, and the same target of the present invention can be prepared. It has also been confirmed that they have the same effect. Further, the target of the present invention can be similarly prepared when FeCo alloy base or Co base powder or foamed metal is used and RE-Fe alloy is used as the mother alloy, and the same effect was confirmed. And, as a matter of course, the target of the present invention could be prepared by using a powder obtained by mixing Fe powder and Co powder.

In addition to the rare earth transition metal composition shown in this example,
Additives such as Ti, Cr, Al, Zr, Pt, Au, Ag, Cu, or Si, Ca, C
It has been confirmed that the production according to the method of the present invention is possible even when unavoidable impurities such as the above are mixed, and that the same effect is present.

〔The invention's effect〕

According to the invention of claim 1, since the rare earth metal powder and the transition metal powder are charged into the molten alloy of the rare earth metal and the transition metal, the surroundings of the rare earth metal powder and the transition metal powder are
Since the molten alloy of the rare earth metal and the transition metal surrounds it, there are no fine pores. Even if they exist, the pores are not connected to each other, so that the surface oxidation does not proceed to the inside. Therefore, there is an excellent effect that a sputtering target having excellent oxidation resistance can be manufactured. Further, it is possible to manufacture a sputtering target in which the rare earth metal single phase, the transition metal single phase and the rare earth metal-transition alloy phase are mixed. Sputtering on a substrate using this sputtering target has an excellent effect that a film having a uniform composition distribution can be formed.

According to the invention of claim 2, since the rare earth metal which is easily oxidized is used in the state of the lump of the rare earth metal-transition metal alloy, the surface area is smaller than that of the powder and is less likely to be oxidized. Therefore, there is an excellent effect that it is possible to manufacture a sputtering target containing less oxygen as compared with a sputtering target manufactured using a rare earth metal powder. Further, the composition can be easily controlled by setting the porosity of the transition metal powder, so that a sputtering target having a desired composition can be easily obtained. Further, the heat treatment brings about an excellent effect that the amount of the intermetallic compound phase can be controlled.

[Brief description of the drawings]

FIG. 1 is a schematic diagram of the surface texture of a sputtering target according to the method of the present invention. FIG. 2 is a schematic diagram of a sputtering device. FIG. 3 is a composition distribution and magnetic characteristic distribution diagram in a substrate holder using the NdDyFeCo target of the present invention. FIG. 4 is a schematic diagram of the surface structure of a conventional cast alloy NdDyFeCo target. FIG. 5 is a composition distribution and magnetic characteristic distribution diagram in a substrate holder using a conventional cast alloy NdDyFeCo target. FIG. 6 is a composition distribution and magnetic characteristic distribution diagram in a substrate holder using a semi-melting method NdDyFeCo target. FIG. 7 is a diagram showing the relationship between the sputtering time and the magnetic film properties of the NdDyFeCo target of the present invention and the semi-molten NdDyFeCo target after being left in the air for 24 hours. FIG. 8 is a graph showing the sputtering time dependence of the magnetic properties of the film with respect to the exposure time of the semi-melted NdDyFeCo target to the atmosphere. FIG. 9 is a composition distribution and magnetic characteristic distribution diagram in a substrate holder using the TbFeCo target of the present invention. FIG. 10 is a composition distribution and magnetic characteristic distribution diagram in a substrate holder using a conventional cast alloy TbFeCo target. FIG. 11 is a composition distribution and magnetic characteristic distribution diagram in a substrate holder using a semi-molten TbFeCo target. FIG. 12 is a diagram showing the relationship between the sputtering time and the magnetic film properties of the TbFeCo target of the present invention and the semi-molten TbFeCo target after being left in the air for 24 hours. FIG. 13 is a graph showing the sputtering time dependence of the magnetic properties of the film with respect to the time period for which the semi-molten TbFeCo target was left in the atmosphere. FIG. 14 is a schematic diagram of the production method of the present invention by the impregnation method. FIG. 15 is a schematic diagram of the surface texture of the target of the present invention by the impregnation method. FIG. 16 is a composition distribution and magnetic characteristic distribution diagram in a substrate holder using the target of the present invention by the impregnation method. FIG. 17 is a schematic view of the metal structure of the target of the present invention using a foam metal sheet. FIG. 18 is a composition distribution and magnetic characteristic distribution diagram in a substrate holder using the target of the present invention using a foam metal sheet. FIG. 19 (a) is a schematic view before melting of a master alloy ingot using powder having a porosity of about 30%. FIG. 19 (b) is a schematic view of a portion where a mother alloy using a powder having a porosity of about 30% is melted and impregnated. FIG. 20 (a) is a schematic view before melting of a master alloy ingot using powder having a porosity of about 80%. FIG. 20 (b) is a schematic view of a portion where a mother alloy using a powder having a porosity of about 80% is melted and impregnated. FIG. 21 is a composition distribution diagram in the substrate holder of the NdDyFeCo target using various porosity powders. FIG. 22 is a composition distribution diagram in the substrate holder of the NdDyFeCo target using various porosity foam sheets. FIG. 23 is a compositional distribution diagram in a substrate holder of an NdFeCo target using various porosity powders. FIG. 24 is a composition distribution diagram in a substrate holder of a TbFeCo target using various porosity foam sheets. FIG. 25 is a diagram showing the relationship between the film magnetic characteristics and the sputtering time of the NdDyFeCo target using 10 μm to 570 μm particle size powder. FIG. 26 is a diagram showing the relationship between the film magnetic characteristics and the sputtering time of the NdDyFeCo target using powder of 730 μm to 4.0 mm in particle size. FIG. 27 is a diagram showing the relationship between the film magnetic characteristics and the sputtering time of the TbFeCo target using 10 μm to 570 μm particle size powder. FIG. 28 is a diagram showing the relationship between the film magnetic characteristics and the sputtering time of a TbFeCo target using a powder having a particle size of 730 μm to 4.0 mm. Fig. 29 shows NdD using foamed metal with a pore size of 10 to 570 μm.
FIG. 3 is a diagram showing the relationship between the magnetic film characteristics and the sputtering time of the yFeCo target. Fig. 30 shows NdDy using foam metal with a pore size of 730 μm to 4.0 mm.
FIG. 4 is a diagram showing the relationship between the magnetic properties of the film and the sputtering time of the FeCo target. Fig. 31 shows TbFeC using foamed metal with a pore size of 10 to 570 μm.
o Diagram showing the relationship between film magnetic properties and sputtering time for the target. Fig. 32 shows Tb using foamed metal with a pore size of 730 μm to 4.0 mm.
FIG. 4 is a diagram showing the relationship between the magnetic properties of the film and the sputtering time of the FeCo target. FIG. 33 is a schematic view of a sputtering device in which the substrate faces the target and is stationary. FIG. 34 is a schematic view of a sputtering apparatus in which the substrate passes over the target. FIG. 35 is a structural diagram of a magneto-optical recording medium. 1 …… (NdDy) ₃₃ (FeCo) ₆₇ at% composition phase 2 …… FeCo composition phase 3 …… FeDy composition phase 21 …… Sputtering target 22 …… Substrate holder 41 …… (Nd _0.12 Dy _0.88 ) ₂₅ (Fe _0.8 Co _0.2 ) ₇₅ at% composition phase 42 …… (Nd _0.3 Dy _0.7 ) _33.3 (Fe _0.8 Co _0.2 ) _66.7 at% composition phase 71 …… Invention target 72 …… Semi-melting method target 81 …… Atmosphere 10 minutes 82 …… 30 minutes in the atmosphere 83 …… 1 hour in the atmosphere 84 …… 5 hours in the atmosphere 85 …… 5 hours in the atmosphere 121 …… Target of the present invention 122 …… Target for the semi-melting method 131 …… 10 minutes in the atmosphere 132 …… 30 minutes in the atmosphere 133 …… 1 hour in the atmosphere 134 …… 3 hours in the atmosphere 141 …… Crucible 142 …… High frequency induction heating coil 143 …… R + R ₁ T ₂ mother alloy 144 …… Fe ₈₀ Co ₂₀ at% powder 151… … Fe-Co particles 152 …… Nd-Dy rare earth metal single phase 153 …… (NdDy) ₁ (FeCo) ₂ rare earth transition metal alloy phase 171 …… Fe _93.6 Co _6.4 a t% single phase 172 …… Rare earth metal (Tb) single phase 173 …… Transition metal and rare earth metal alloy phase (TbFeCo) 211 …… 30% porosity powder target 212 …… Porosity 40% powder Target 213 …… 50% porosity powder target 214 …… Porosity 62% powder target 215 …… Porosity 70% powder target 216 …… Porosity 80% powder target 221 …… Empty Porosity 30% Foamed sheet target 222 …… Porosity 40% Foamed sheet target 223 …… Porosity 50% Foamed sheet target 224 …… Porosity 62% Foamed sheet target 225 …… Porosity 70% Foamed sheet target 226 …… Porosity 80% Foamed sheet target 231 …… Porosity 30% Powder target 232 …… Porosity 43% Powder target 233 …… Porosity 50% Powder Target 234 …… 60% porosity powder target 235 …… Porosity 70% powder target 236 …… Porosity 80% powder target 241 …… 30% porosity foamed sheet target 242 …… Porosity 43% foamed sheet target 243 …… Porosity 50% foamed sheet target 244 …… Porosity 60% foamed sheet target 245 …… Target with 70% porosity foamed sheet 246 …… Target with 80% porosity foamed sheet 251 …… Target with 10 μm particle size powder 252 …… 24 μm Target with particle size powder 253 …… 38 μm Target with particle size powder 254 …… 53μm Target with particle size powder 255 …… 120μm Target with particle size powder 256 …… 230μm Target with particle size powder 257 …… 570μm particle size with powder Target 261 …… Target with 730 μm particle size powder 262 …… Target with 1.0 mm particle size powder 263 …… Target with 1.5 mm particle size powder 264 …… Target with 2.5 mm particle size powder 265… … Target with 3.0mm particle size 266 …… 3.2mm particle Target using powder 267 …… 4.0mm Target using powder with particle size 271 …… Target using 10μm particle size powder 272 …… Target using particle with particle size 24μm 273 …… Target using powder with particle size 38μm 274 …… Target with 53μm particle size powder 275 …… Target with 120μm particle size powder 276 …… 230μm particle size Target with powder 277 …… 570μm particle size Target with powder 281 …… 730μm particle size Target using powder 282 …… 1.0mm Target using powder with particle size 283 …… 1.5mm Target using powder with particle size 284 …… 2.5mm Target using powder with particle size 285 …… 3.0mm Particle using powder Targets used 286 …… Targets using 3.2mm particle size powders 287 …… Targets using 4.0mm particle size powders 291 …… Targets using 10 μm pore diameter foam metal 292 …… 24 μm pore diameter using foam metal Target 293 …… 38 μm pore size Target 294 …… 53 μm target with foamed metal foam 295 …… 120 μm target with foamed metal foam 296 …… 230 μm target with foamed metal foam 297 …… 570 μm target with foamed metal foam 301 ...... 730 μm pore diameter target using foam metal 302 …… 1.0 μm pore diameter target using foam metal 303 …… 1.5 mm pore diameter target using foam metal 304 …… 2.5 mm target using foam metal foam 305 …… Target with 3.0 mm pore diameter foam metal 306 …… 3.2 mm Target with pore diameter foam metal 307 …… 4.0 mm Target with pore diameter foam metal 311 …… 10 μm Hole diameter using foam metal Target 312 …… 24μm Target with foamed metal foam 313 …… 38μm Target with foamed metal foam 314 …… 53μm Target with foamed metal foam 315 …… 120μm Target with foamed metal foam 316 …… 230 μm Target with foamed metal foam 317 …… 570 μm Target with foamed metal foam 321 …… 730 μm Target with foamed metal foam 322 …… 1.0 mm empty Target made of foam metal 323 …… 1.5mm Target made of foam metal 324 …… 2.5mm Target made of foam metal 325 …… 3.0mm Target made of foam metal 326 …… 3.2 mm Target made of foam metal 327 …… 4.0 Target made of foam metal 331 …… Target 332 …… Substrate 341 …… Target 342 …… Substrate 351 …… Polycarbonate substrate 352 …… AlSiN dielectric film 353 …… NdDyFeCo magneto-optical recording film 354 …… AlSiN dielectric film

Claims (4)

(57) [Claims] 1. A process of heating and melting a rare earth metal and a transition metal to form a molten alloy, and adjusting the temperature of the molten alloy to a first temperature, and then adding the rare earth metal powder and the transition metal to the molten alloy. And a step of introducing a powder, wherein the first temperature is lower than a melting point of the rare earth metal powder and lower than a melting point of the transition metal powder. A method of manufacturing a sputtering target, comprising: 2. A container having a porosity of 30 having a first melting point.
-80% transition metal powder, and a second lower melting point than the first melting point on the transition metal powder.
Placing a rare earth-transition metal alloy ingot having a melting point of, and heating the transition metal powder and the rare earth-transition metal alloy ingot to a temperature between the first melting point and the second melting point, A method of manufacturing a sputtering target, comprising: a step of impregnating a transition metal powder with the rare earth-transition metal alloy to form a compact, and a step of heat-treating the compact. 3. The rare earth metal contains at least one kind of rare earth metal element selected from Sm, Nb, Pr, Ce, Tb and Dy, and the transition metal is at least one kind of transition metal selected from Fe and Co. The method for producing a sputtering target according to claim 1, further comprising a metal element. 4. The average particle size of the transition metal powder is from 10 μm to
The method of manufacturing a sputtering target according to claim 2, wherein the sputtering target is 3.0 mm.