JPH03275560A - Light transmissive sintered body of yttrium, aluminum and garnet and production thereof - Google Patents
Light transmissive sintered body of yttrium, aluminum and garnet and production thereofInfo
- Publication number
- JPH03275560A JPH03275560A JP7380690A JP7380690A JPH03275560A JP H03275560 A JPH03275560 A JP H03275560A JP 7380690 A JP7380690 A JP 7380690A JP 7380690 A JP7380690 A JP 7380690A JP H03275560 A JPH03275560 A JP H03275560A
- Authority
- JP
- Japan
- Prior art keywords
- sintered body
- aluminum
- yttrium
- garnet
- molding
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000002223 garnet Substances 0.000 title claims abstract 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract 5
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract 5
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 229910052727 yttrium Inorganic materials 0.000 title abstract description 4
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 title abstract description 4
- 238000005245 sintering Methods 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 17
- 238000000465 moulding Methods 0.000 claims abstract description 11
- 238000002834 transmittance Methods 0.000 claims description 15
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 claims description 8
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 claims description 8
- 230000005484 gravity Effects 0.000 claims description 3
- 230000003068 static effect Effects 0.000 claims description 2
- PSNPEOOEWZZFPJ-UHFFFAOYSA-N alumane;yttrium Chemical compound [AlH3].[Y] PSNPEOOEWZZFPJ-UHFFFAOYSA-N 0.000 claims 1
- 239000007787 solid Substances 0.000 claims 1
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 27
- 239000007789 gas Substances 0.000 description 13
- 238000000034 method Methods 0.000 description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 7
- 239000011148 porous material Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- 230000007423 decrease Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 4
- 238000000280 densification Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 229910001882 dioxygen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000001272 pressureless sintering Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 239000012780 transparent material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
Description
【発明の詳細な説明】
〈産業上の利用分野〉
この発明は透光性にすぐれた多結晶イットリウム・アル
ミニウム・ガーネット（以下、ＹＡＧという）焼結体お
よびその製造方法に係り、特に波長２〜４μｍの中赤外
領域での赤外光透過窓として好適な高密度のＹＡＧ焼結
体およびその製造方法に関するものである。[Detailed Description of the Invention] <Industrial Application Field> The present invention relates to a polycrystalline yttrium aluminum garnet (hereinafter referred to as YAG) sintered body with excellent translucency and a method for manufacturing the same, particularly for wavelengths 2 to 2. The present invention relates to a high-density YAG sintered body suitable as a 4 μm infrared light transmitting window in the mid-infrared region, and a method for manufacturing the same.
〈従来の技術〉
Ｙ Ａ Ｇ （ＹｓＡｊ ｓＯ□）は結晶型が立方晶で
あるため、粒界散乱が起こりにくく、従来各種の製法に
よって透光性焼結体を得る試みがなされている。<Prior Art> Since YAG (YsAj sO□) has a cubic crystal type, grain boundary scattering is less likely to occur, and attempts have been made to obtain translucent sintered bodies using various manufacturing methods.
例えば特開昭６３−２６０８５６号公報に示されるよう
に、Ｚｒ化合物（ＺｒＯ＊ ）を添加して不活性雰囲気
中あるいは水素中において焼結する方法が知られている
。この所謂、常圧焼結法（無加圧焼結法）では、焼結助
剤を添加することが必要であり、上記のＺｒ０ｍのほか
に酸化マグネシウム（Ｍｇ０）あるいは酸化ケイ素（Ｓ
ｉｎｓ）も有効であることが知られている。For example, as shown in JP-A No. 63-260856, a method is known in which a Zr compound (ZrO*) is added and sintered in an inert atmosphere or in hydrogen. In this so-called pressureless sintering method (pressureless sintering method), it is necessary to add a sintering aid, and in addition to the above Zr0m, magnesium oxide (Mg0) or silicon oxide (S
ins) is also known to be effective.
（発明が解決しようとする課題〉
上記した従来の透光性ＹＡＧ焼結体の製造方法において
は、何れも粉末成形体の無加圧焼結によるものであり、
粒成長のコントロールが難しいために、空孔が残留しや
すく、例えば体積比でｌＯ〜１１００ｐｐの空孔が残留
することにより、光が散乱され、直線透過率が低下し、
吸収係数に換算して０、５ｃｍ−’程度が限界であった
。(Problems to be Solved by the Invention) The above-described conventional methods for producing a translucent YAG sintered body are all based on pressureless sintering of a powder compact,
Since it is difficult to control grain growth, pores tend to remain. For example, if pores with a volume ratio of 10 to 1100 pp remain, light is scattered and the in-line transmittance decreases.
The limit was about 0.5 cm-' in terms of absorption coefficient.
また、緻密化を促進するために焼結助剤を添加する方法
は、焼結助剤が第２相として出現しやすいために組織的
不均一性により光が散乱されたり、焼結助剤自身の不純
物吸収により透光性が低下しやすいため、透光性のレベ
ルが低く、直線透過率が更に低下し、吸収係数が大きく
なる欠点があった。In addition, the method of adding a sintering aid to promote densification is such that the sintering aid tends to appear as a second phase, which may cause light to be scattered due to structural non-uniformity, or the sintering aid itself may Since the light transmittance tends to decrease due to the absorption of impurities, the light transmittance level is low, the linear transmittance further decreases, and the absorption coefficient increases.
このように、従来の方法で製造された透光性ＹＡＧ焼結
体では直線透過率が試料厚さ３１１１１１１で７０％程
度（吸収係数にして０．５ｃｍ−’程度）が最大であり
、試料厚さ３ｍｍ以上で使用される赤外透過窓の材料に
用いるためには更に直線透過率の向上（即ち、吸収係数
にして０．２〜０．１ ｃｍ−’以下）が必要であった
。In this way, for the translucent YAG sintered body manufactured by the conventional method, the in-line transmittance is maximum at about 70% (absorption coefficient is about 0.5 cm-') at a sample thickness of 3111111, and In order to use it as a material for an infrared transmission window used at a diameter of 3 mm or more, it was necessary to further improve the in-line transmittance (ie, the absorption coefficient is 0.2 to 0.1 cm-' or less).
この発明は、かかる従来の事情に鑑み、高純度かつ高密
度で透光性のレベルが高く、特に厚さ３ｍｍ以上の赤外
透過窓材として好適な直線透過率（吸収係数）を有する
透光性ＹＡＧ焼結体、およびその製造方法を提供するこ
とを目的とする。In view of the above-mentioned conventional circumstances, the present invention provides a light-transmitting material having high purity, high density, and a high level of light-transmitting properties, and having a straight-line transmittance (absorption coefficient) particularly suitable as an infrared-transmitting window material with a thickness of 3 mm or more. The object of the present invention is to provide a YAG sintered body and a method for manufacturing the same.
〈課題を解決するための手段〉
この発明は上記従来法の課題を解決するべく検討の結果
、−旦焼結した高密度ＹＡＧ焼結体を、さらに高温高圧
で熱間静水圧（ＨＩＰ）処理することにより、さらに高
密度化を促進し、厚内材料でも透光性にすぐれたＹＡＧ
焼結体を製造する方法を見出したのである。<Means for Solving the Problems> As a result of studies to solve the above-mentioned problems of the conventional method, the present invention is based on the following: - A high-density YAG sintered body that has been sintered is further subjected to hot isostatic pressure (HIP) treatment at high temperature and high pressure. By doing so, it is possible to further increase the density of YAG, which has excellent translucency even in thick materials.
They discovered a method for manufacturing sintered bodies.
即ち、この発明は純度９９．６％以上、比表面積３ｍ＋
”／ｇ（ＢＥＴ値）以上の高純度で、かつ微細なＹＡＧ
粉末を圧力１．０ｔｏｎ／ｃｍ”以上で静圧成形し、成
形比重を２．５以上の成形体としたのち、真空または水
素またはヘリウムの雰囲気中で１５００〜１８００℃の
範囲で２〜２４時間焼結して理論密度の９５％以上に高
密度化し、次いでこの焼結体をさらに１５００〜１８０
０℃、圧力５００〜２０００ｋｇ／ｃｍ”の高圧の・窒
素ガス、アルゴンガスまたは酸素ガスを混合した窒素ガ
スまたはアルゴンガスの雰囲気下でＨＩＰ処理すること
によりさらに高密度で透光性にすぐれた透光性ＹＡＧ焼
結体を提供するものである。That is, this invention has a purity of 99.6% or more and a specific surface area of 3 m+.
”/g (BET value) or higher purity and fine YAG
The powder is statically molded at a pressure of 1.0 ton/cm" or more to form a compact with a specific gravity of 2.5 or more, and then molded in a vacuum or hydrogen or helium atmosphere at a temperature of 1500 to 1800°C for 2 to 24 hours. The density is increased to 95% or more of the theoretical density by sintering, and then this sintered body is further heated to a density of 1500 to 180%.
By performing HIP treatment in an atmosphere of nitrogen gas, argon gas, or oxygen gas mixed at high pressure of 500 to 2000 kg/cm'' at 0°C, a transparent material with higher density and excellent translucency can be obtained. A photosensitive YAG sintered body is provided.
〈作用〉
この発明において、ＨＩＰ処理は焼結により９５％以上
に高密度化したＹＡＧ焼結体の表面を１５００〜１８０
０℃の高温下、５００〜２０００ｋｇ／ｃｍ”の高圧で
等方向に圧縮する方向に加圧するため、塑性変形および
拡散機構による空孔の除去が促進され、さらに高密度化
が達成される。これが透光性の向上に有効に寄与するの
である。ＨＩＰ処理前の密度が９５％未満の場合には残
留空孔の多くが所謂開気孔状態となって高圧ガスが焼結
体内部に侵入してしまうため、ＨＩＰ処理による高密度
化が十分に進行しない。<Function> In this invention, the HIP treatment reduces the surface of the YAG sintered body, which has been densified to 95% or more by sintering, to a
Because the pressure is applied in the same direction at a high pressure of 500 to 2000 kg/cm'' at a high temperature of 0°C, removal of pores by plastic deformation and diffusion mechanism is promoted, and higher density is achieved. This effectively contributes to improving translucency.If the density before HIP treatment is less than 95%, most of the remaining pores become so-called open pores, allowing high pressure gas to enter the inside of the sintered body. As a result, densification through HIP processing does not proceed sufficiently.
ＨＩＰ処理における高圧ガスはＹＡＧ焼結体に対して等
方向に働くため、従来のホットプレス法による上下方向
のみの加圧よりも均一に高密度化が進行し、透光性の均
一な焼結体が得られる。Because the high-pressure gas in the HIP process acts on the YAG sintered body in the same direction, the density progresses more uniformly than when pressurizing only in the vertical direction using the conventional hot press method, resulting in uniform sintering with translucency. You get a body.
また焼結時に発生した組成的不均一相も均一化する効果
がある。It also has the effect of homogenizing the compositionally heterogeneous phases generated during sintering.
高圧ガスの圧力は５００〜２０００ｋｇ／ｃｍ”と高圧
であるため、従来のホットプレス法（１０００ｋｇ／ａ
ｍ”が限度）よりも空孔の除去効果が大きく、すぐれた
透光性の焼結体が得られる。Because the pressure of high-pressure gas is as high as 500 to 2000 kg/cm, the conventional hot press method (1000 kg/a
The effect of removing pores is greater than that of the sintered body (limited to m''), and a sintered body with excellent translucency can be obtained.
高圧ガスの種類はアルゴンガスまたは窒素ガスまたは酸
素ガスを混合したアルゴンガスまたは窒素ガスが望まし
く、若干の酸素ガスの混合ガスを使用した場合、ＨＩＰ
処理時のＹＡＧ焼結体からの脱酸素による透光性の低下
を防止できる効果を有する。The type of high-pressure gas is preferably argon gas, nitrogen gas, or argon gas mixed with oxygen gas, or nitrogen gas, and if a mixed gas with some oxygen gas is used, HIP
This has the effect of preventing a decrease in translucency due to deoxidation from the YAG sintered body during processing.
高圧ガス投入前の焼結は、ＹＡＧ成形体の焼結による高
密度化過程に於て残留空孔の内部に窒素、アルゴン等の
分子径の大きなガスが取込まれることは以後の高密度化
を阻害するので、この焼結は真空雰囲気または分子径の
小さな水素やヘリウム雰囲気が望ましい。During sintering before high-pressure gas is introduced, gases with large molecular diameters such as nitrogen and argon may be taken into the residual pores during the densification process by sintering the YAG compact, which will occur during subsequent densification. Therefore, this sintering is preferably performed in a vacuum atmosphere or in a hydrogen or helium atmosphere with a small molecular diameter.
そして焼結条件としては１５００〜１８００℃で２〜２
４時間が好ましく、第１段階の焼結で理論密度の９５％
以上に高密度化される。The sintering conditions are 1500~1800℃ and 2~2
Preferably 4 hours, 95% of theoretical density in first stage sintering
The density is further increased.
またＭｇＯまたはＳｉｎｇまたはＺｒＯ□なとの焼結助
剤を添加した場合には、４〜ｌＯ時間程度の短時間保持
でも９５％以上の高密度焼結を容易に達成することがで
きる。Furthermore, when a sintering aid such as MgO, Sing, or ZrO□ is added, high-density sintering of 95% or more can be easily achieved even with a short holding time of about 4 to 10 hours.
この発明において使用するＹＡＧ粉末は純度９９．６％
以上で比表面積３ｍ”／ｇ（ＢＥＴ値）以上であること
が望ましい。The YAG powder used in this invention has a purity of 99.6%.
It is desirable that the specific surface area is 3 m''/g (BET value) or more.
これは−次粒子の粒径がおよそ０．４μｍ以下であるこ
とを示しており、上記の焼結条件で緻密な焼結体を得る
ためには必要な条件である。また純度を９９．６％以上
とするのは、不純物が多く含有しているとたとえ十分な
高密度化焼結体が得られたとしても不純物吸収により透
光性の低下をもたらすためである。This indicates that the particle size of the secondary particles is approximately 0.4 μm or less, which is a necessary condition for obtaining a dense sintered body under the above sintering conditions. The reason why the purity is set to 99.6% or more is that if a large amount of impurities is contained, even if a sufficiently high-density sintered body is obtained, the absorption of impurities will result in a decrease in translucency.
特に、鉄などの遷移金属元素を含むことは好ましくない
。In particular, it is not preferable to include transition metal elements such as iron.
このように、高純度でかつ微細なＹＡＧ粉末としては、
イツトリウムとアルミニウムの塩化物を溶かした水の中
に硫酸イオンを添加し、さらに尿素を入れて加熱し、Ｙ
ＡＧ粉末を沈殿させ、これを乾燥して得られるもの等が
好適である。In this way, as a highly pure and fine YAG powder,
Sulfate ions are added to water in which yttrium and aluminum chloride are dissolved, and urea is added and heated.
Preferably, it is obtained by precipitating AG powder and drying it.
上記したこの発明の製造方法によると、波長３〜４μｍ
の赤外光による厚さ３■の直線透過率が７５％以上の透
光性ＹＡＧ焼結体を得ることがきる。According to the manufacturing method of the present invention described above, the wavelength is 3 to 4 μm.
It is possible to obtain a translucent YAG sintered body having a linear transmittance of 75% or more with a thickness of 3 cm by infrared light.
〈実施例〉 以下、この発明を実施例により詳細に説明する。<Example> Hereinafter, this invention will be explained in detail with reference to Examples.
実施例１
純度９９．６％、比表面積３．３ｍ”／ｇ（Ｂ Ｅ Ｔ
値）の高純度ＹＡＧ粉末を乾燥後、直径３０ｍｍのゴム
モールドを用いて２．０ｔｏｎ／ｃ１で静圧成形を行な
い、比重２．６の成形体を得た。Example 1 Purity 99.6%, specific surface area 3.3 m”/g (B E T
After drying the high-purity YAG powder (value), static pressure molding was performed at 2.0 ton/c1 using a rubber mold with a diameter of 30 mm to obtain a molded body with a specific gravity of 2.6.
この成形体を真空中で１７００℃で２４時間焼結し、理
論密度比９８％以上の焼結体を得た。さらにこの焼結体
をＨＩＰ装置に入れ、１０％０□−Ｍの混合ガスを用い
て１７５０℃、２０００ｋｇ／ｃｍ”で１時間保持した
。This molded body was sintered in vacuum at 1700° C. for 24 hours to obtain a sintered body having a theoretical density ratio of 98% or more. Further, this sintered body was placed in a HIP device and maintained at 1750° C. and 2000 kg/cm” for 1 hour using a 10% 0□-M mixed gas.
かくして得られたＹＡＧ焼結体を厚さ３ｍｍに鏡面研磨
加工し、赤外分光光度計で透過率を測定したところ、波
長３〜４μｍの赤外領域で平均８０％の良好な透光性を
示した。The thus obtained YAG sintered body was mirror-polished to a thickness of 3 mm, and its transmittance was measured with an infrared spectrophotometer, and it was found that it had good transmittance of 80% on average in the infrared region with a wavelength of 3 to 4 μm. Indicated.
実施例２
純度９９．８％、比表面積４ｍ”／ｇ （Ｂ Ｅ Ｔ
値）の高純度ＹＡＧ粉末を、５ Ｘ １０−”ｔｏｒｒ
の真空中において１７５０℃で１０時間焼結し、理論密
度比９６％の白色の焼結体を得た。Example 2 Purity 99.8%, specific surface area 4 m”/g (B E T
high purity YAG powder of 5 x 10-”torr
The mixture was sintered in a vacuum at 1750° C. for 10 hours to obtain a white sintered body with a theoretical density ratio of 96%.
次に、この焼結体をＨＩＰ装置に入れ、Ａｒガスを用い
て１６５０℃の温度および２０００ｋｇ／Ｃｍ”の圧力
で２時間のＨＩＰ処理を行なった。Next, this sintered body was placed in a HIP apparatus, and HIP treatment was performed using Ar gas at a temperature of 1650° C. and a pressure of 2000 kg/cm'' for 2 hours.
得られたＹＡＧ焼結体は外観的に無色透明であった。こ
のＹＡＧ焼結体を厚さ３ｍｍに鏡面研磨加工し、分光光
度計で直線透過率を測定したところ、波長３〜５μｍの
赤外領域で平均８０％、および波長０．４〜３μｍの領
域で平均７４％のすぐれた透光性を示した。The obtained YAG sintered body was colorless and transparent in appearance. When this YAG sintered body was mirror-polished to a thickness of 3 mm and the linear transmittance was measured using a spectrophotometer, it was found to be 80% on average in the infrared region of wavelengths 3 to 5 μm, and in the wavelength region of 0.4 to 3 μm. It showed excellent translucency of 74% on average.
実施例３
純度９９．７％、比表面積６ｍ”／ｇ （Ｂ Ｅ Ｔ
値）の高純度ＹＡＧ粉末を、水素気流中で１７８０℃、
６時間焼結し、理論密度比９６％の白色の焼結体を得た
。Example 3 Purity 99.7%, specific surface area 6 m”/g (B E T
High-purity YAG powder of
After sintering for 6 hours, a white sintered body with a theoretical density ratio of 96% was obtained.
更に、この焼結体をＨＩＰ装置に入れ、Ｎ２ガスを用い
て１７００℃の温度および１５００ｋｇ／ｃｍ”の圧力
で３時間のＨＩＰ処理を行なった。Further, this sintered body was placed in a HIP apparatus and subjected to HIP treatment using N2 gas at a temperature of 1700° C. and a pressure of 1500 kg/cm'' for 3 hours.
得られたＹＡＧ焼結体は外観的に無色透明であった。The obtained YAG sintered body was colorless and transparent in appearance.
このＹＡＧ焼結体を厚さ３ｍｍに鏡面研磨加工し、分光
光度計で直線透過率を測定したところ、波長３〜５μｍ
の赤外領域で平均８１％、および波長０．４〜３μｍの
領域で平均７２％のすぐれた透光性を示した。When this YAG sintered body was mirror-polished to a thickness of 3 mm and the linear transmittance was measured with a spectrophotometer, it was found that the wavelength was 3 to 5 μm.
It exhibited excellent light transmittance of 81% on average in the infrared region and 72% on average in the wavelength range of 0.4 to 3 μm.
〈発明の効果〉
以上説明したように、この発明によればＹＡＧ成形体を
いったん高密度に焼結したのち、さらに高温高圧でＨＩ
Ｐ処理を施すことにより、高密度で透光性にすぐれたＹ
ＡＧ焼結体を得ることができるのである。<Effects of the Invention> As explained above, according to the present invention, after the YAG molded body is sintered to a high density, it is further HI'd at high temperature and high pressure.
By applying P treatment, Y has high density and excellent translucency.
This makes it possible to obtain an AG sintered body.
また、この発明により得られる透光性ＹＡＧ焼結体は、
透光性にすぐれているため、３ｍｍ以上の厚内で使用さ
れる赤外光透過窓材として有用であることが認められた
。Furthermore, the translucent YAG sintered body obtained by this invention is
Because of its excellent light transmittance, it was found to be useful as an infrared light transmitting window material used within a thickness of 3 mm or more.
Claims (4)
り、波長３〜４μｍの赤外光による ３ｍｍ厚さの直線透過率が７５％以上であることを特徴
とする透光性イットリウム・アルミニウム・ガーネット
焼結体。(1) A translucent yttrium-aluminum-garnet sintered body made of yttrium-aluminum-garnet, characterized in that the in-line transmittance of a 3 mm thick infrared light with a wavelength of 3 to 4 μm is 75% or more.
ガーネット粉末を成形後、焼結して高密度化したのち、
１５００〜１８００℃、５００ｋｇ／ｃｍ＾２以上にて
熱間静水圧処理することによりさらに高密度で透光性に
すぐれた焼結体とすることを特徴とする透光性イットリ
ウム・アルミニウム・ガーネット焼結体の製造方法。(2) High purity and fine yttrium aluminum
After molding the garnet powder and sintering it to make it more dense,
A translucent yttrium aluminum garnet sintered body characterized by a sintered body with higher density and excellent translucency by hot isostatic pressure treatment at 1500 to 1800°C and 500 kg/cm^2 or higher. Method for producing solids.
純度９９．６％以上で比表面積３ｍ＾２／ｇ以上である
ことを特徴とする請求項２記載の透光性イットリウム・
アルミニウム・ガーネット焼結体の製造方法。(3) The translucent yttrium-aluminum garnet powder according to claim 2, wherein the yttrium-aluminum-garnet powder has a purity of 99.6% or more and a specific surface area of 3 m^2/g or more.
Method for producing aluminum garnet sintered body.
成形は圧力１ｔｏｎ／ｃｍ＾２以上の静圧成形で行ない
、成形比重を２．５以上とすることを特徴とする請求項
２記載の透光性イットリウム・アルミニウム・ガーネッ
ト焼結体の製造方法。(4) The translucent yttrium-aluminum garnet powder according to claim 2, characterized in that the molding of the yttrium-aluminum-garnet powder is carried out by static pressure molding at a pressure of 1 ton/cm^2 or more, and the molding specific gravity is 2.5 or more. Method for producing aluminum garnet sintered body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7380690A JPH03275560A (en) | 1990-03-23 | 1990-03-23 | Light transmissive sintered body of yttrium, aluminum and garnet and production thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7380690A JPH03275560A (en) | 1990-03-23 | 1990-03-23 | Light transmissive sintered body of yttrium, aluminum and garnet and production thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03275560A true JPH03275560A (en) | 1991-12-06 |
Family
ID=13528781
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7380690A Pending JPH03275560A (en) | 1990-03-23 | 1990-03-23 | Light transmissive sintered body of yttrium, aluminum and garnet and production thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03275560A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7253129B2 (en) * | 2003-01-27 | 2007-08-07 | Konoshima Chemical Co., Ltd. | Rare earth garmet sintered compact |
| JP2009084060A (en) * | 2007-09-27 | 2009-04-23 | Covalent Materials Corp | Translucent oxidized yttrium aluminum garnet sintered compact and its producing method |
| KR20150112997A (en) | 2013-02-08 | 2015-10-07 | 신에쓰 가가꾸 고교 가부시끼가이샤 | Light transmitting metal oxide sintered body manufacturing method and light transmitting metal oxide sintered body |
-
1990
- 1990-03-23 JP JP7380690A patent/JPH03275560A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7253129B2 (en) * | 2003-01-27 | 2007-08-07 | Konoshima Chemical Co., Ltd. | Rare earth garmet sintered compact |
| JP2009084060A (en) * | 2007-09-27 | 2009-04-23 | Covalent Materials Corp | Translucent oxidized yttrium aluminum garnet sintered compact and its producing method |
| KR20150112997A (en) | 2013-02-08 | 2015-10-07 | 신에쓰 가가꾸 고교 가부시끼가이샤 | Light transmitting metal oxide sintered body manufacturing method and light transmitting metal oxide sintered body |
| US9604853B2 (en) | 2013-02-08 | 2017-03-28 | Shin-Etsu Chemical Co., Ltd. | Light transmitting metal oxide sintered body manufacturing method and light transmitting metal oxide sintered body |
| DE112013006623B4 (en) | 2013-02-08 | 2024-07-11 | Shin-Etsu Chemical Co., Ltd. | Manufacturing process for a translucent metal oxide sintered body |
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