TWI392760B - Methods for producing silicon nitride films by vapor-phase growth - Google Patents

Description

Method for producing a tantalum nitride film by vapor phase growth

The present invention relates to a method of producing a tantalum nitride film, and more particularly to a method of producing a tantalum nitride film by vapor phase growth such as chemical vapor deposition (CVD).

Tantalum nitride film has excellent barrier properties and excellent oxidation resistance, and is therefore used in microelectronic device fabrication (such as as an etch stop layer, barrier layer or gate insulating layer) and an oxide/nitride stack. in.

Plasma-assisted CVD (PECVD) and low-pressure CVD (LPCVD) are the main methods currently used to form tantalum nitride films.

PECVD is usually carried out by introducing a helium source (usually decane) and a nitrogen source (usually ammonia, but more recently nitrogen) between a pair of parallel plate electrodes, and at low temperatures (about 350 ° C) and low pressure (0.001 torr). At 5 torr, high frequency energy is applied between the electrodes to induce plasma generation from the helium source and the nitrogen source. The active cerium species and the reactive nitrogen species in the formed plasma react with each other to produce a tantalum nitride film. The tantalum nitride film formed in this manner by PECVD generally does not have a stoichiometric composition and is rich in hydrogen, thus having low film density, poor step coverage, fast etch rate, and poor thermal stability.

LPCVD uses low pressure (0.1 to 2 torr) and high temperature (800 ° C to 900 ° C) to produce a tantalum nitride film that is superior in quality to the tantalum nitride film produced by PECVD. Currently, tantalum nitride is usually made from dichloroguanidine by LPCVD. The reaction of an alkane with gaseous ammonia is produced. However, the reaction of methylene chloride with gaseous ammonia during the LPCVD process produces by-products, ammonium chloride, which accumulates in the reactor exhaust and blocks it and is also deposited on the wafer. Furthermore, the existing LPCVD technology has the disadvantage that the growth rate of the tantalum nitride film is slow and has a high thermal budget. In order to reduce the thermal budget required to produce a tantalum nitride film, a method of producing a tantalum nitride film by reacting ammonia gas with hexachlorodioxane (as a tantalum nitride precursor) has recently been developed. However, this method is significantly exacerbated by the presence of a large amount of chlorine in hexachlorodioxane. This method also produces ruthenium containing particles which will substantially reduce the life of the vent line. Finally, although the method can provide a high quality tantalum nitride film (good step coverage ratio and low chlorine content) at an excellent growth rate at a reaction temperature such as 600 ° C, when a reaction temperature lower than 550 ° C is used These properties will be significantly degraded.

It has been proposed to use volatile carbon-containing decane, azide and alkane as a cerium nitride precursor to solve the above problems (see Non-Patent References 1 and 2). However, these tantalum nitride precursors used alone or in combination with ammonia gas may incorporate niobium carbide and/or a large amount of carbon into the tantalum nitride film product.

(Non-patent Reference 1) Grow et al., Mater. Lett. 23, 187, 1995

(Non-patent Reference 2) Levy et al., J. Mater. Res., 11, 1483, 1996

Therefore, the problem to be solved by the present invention is to provide a vapor phase growth method for producing a tantalum nitride film, wherein the vapor phase growth method can produce a tantalum nitride film having improved film properties, even at relatively low temperatures. The reaction is carried out, and the vapor phase growth process is not accompanied by the production of ammonium chloride, and no significant carbonaceous contaminants are incorporated into the film product.

According to a first aspect of the present invention, there is provided a method for producing a tantalum nitride film by vapor phase growth, the method characterized by: a hydrazine gas selected from the group consisting of a trimethyl hydrazine alkyl gas and a methyl hydrazine alkylamine At least one precursor gas of the group of gases is supplied into the reactor containing at least one substrate, and a tantalum nitride film is formed on the at least one substrate by the reaction of the two gases.

According to a second aspect of the present invention, there is provided a method for producing a tantalum nitride film by vapor phase growth, the method comprising: feeding a methyl hydrazine hydrazine gas into a reactor containing at least one substrate And forming a tantalum nitride film on the at least one substrate by decomposition of the methotrexate hydrazine gas.

Specific examples of the invention

The present invention is more specifically described below.

The present invention relating to a method for producing a tantalum nitride film on a substrate by a vapor phase growth process such as CVD uses trimethylsulfonylamine ((H ₃ Si) ₃ N ) and/or a mercaptoalkylamine as a nitride.矽Precursor. These precursors produce a tantalum nitride film by gas phase reaction with hydrazine. Among these precursors, the mercapto hydrazine can form a tantalum nitride film by thermal decomposition of itself.

The formazan hydrazine used in the present invention comprises a dimethyl hydrazine H ₃ Si(R ^a )NN(R ^b )R ^c (I) as defined by the formula (I).

Wherein R ^a , R ^b and R ^c are each independently selected from the group consisting of a methyl group, a hydrogen atom, a methyl group, an ethyl group and a phenyl group.

The hydrazine reacted with the previously disclosed precursor contains the hydrazine H(R ¹ )NN(R ² )R ³ (II) defined by the formula (II)

Wherein R ¹ , R ² and R ³ are each independently selected from a hydrogen atom, a methyl group, an ethyl group and a phenyl group.

First, a method of producing a tantalum nitride film by a reaction of a hydrazine with a precursor (CVD process) will be described. In this case, a preform gas, a hydrazine gas, and optionally an inert diluent gas are supplied into a reactor containing at least one substrate (specifically, a semiconductor substrate such as a ruthenium substrate), and by a preform gas A tantalum nitride film is formed on the substrate by a reaction with a hydrazine gas.

During the reaction of the preform gas with the hydrazine gas, the pressure inside the reaction chamber can be maintained at a pressure of 0.1 to rr to 1,000 torr, and it is preferred to maintain the pressure in the reaction chamber at a pressure of 0.1 to rr to 10 torr.

The reaction of the preform gas with the hydrazine gas can usually be no more than 1,000 The temperature is °C (CVD reaction temperature). However, almost no tantalum nitride is produced at temperatures below 300 °C. Therefore, the reaction of the preform gas with the hydrazine gas can be carried out at 300 ° C to 1,000 ° C. Even at a low temperature of 400 ° C to 700 ° C, the preform and the hydrazine are still capable of producing a tantalum nitride at a sufficiently high growth rate (film formation rate). Further, when the CVD reaction temperature is from 300 ° C to 500 ° C, even if the aspect ratio of the opening is 10, it is still possible to obtain a step coverage ratio such as at least about 0.8. The step coverage ratio can be defined as the value obtained by dividing the minimum film thickness of the trapezoidal body by the film thickness of the flat or planar region. The CVD reaction temperature is usually the temperature of the substrate on which the tantalum nitride is formed.

The hydrazine gas and the preformed gas can typically be fed into the reaction chamber at a hydrazine/preform flow rate ratio of no more than 100. Although tantalum nitride can be produced when the hydrazine/preform flow rate ratio exceeds 100, a hydrazine/preform flow rate ratio of more than 100 is generally uneconomical. Preferred hydrazine/preform flow ratio values are from 1 to 80.

The inert diluent gas input into the reaction chamber in a manner selected as needed may be an inert gas such as nitrogen or a rare gas such as argon.

Since neither the preform nor the hydrazine used in the present invention contains chlorine, the reaction does not produce the previously troubled ammonium chloride by-product. Furthermore, although the formazan hydrazine and/or hydrazine used in the present invention contains a carbonaceous species, even in the case of using the carbonaceous material, only a relatively low carbon concentration is found in the tantalum nitride product. .

A method of producing a tantalum nitride bismuth film alone and a thermal decomposition thereof to produce a tantalum nitride film will now be described. In this case, the methotrexate hydrazine gas and Any inert diluent gas selected as needed is fed into the reaction chamber and a tantalum nitride film is produced by thermal decomposition of the methyl hydrazine amide. As in the previously disclosed CVD process, the pressure in the reaction chamber can be maintained at 0.1 torr to 1,000 torr, and the pressure in the reaction chamber is preferably maintained at 0.1 torr to 10 torr.

As in the CVD process previously disclosed, the decomposition of the germyl hydrazine gas can generally be carried out at 300 ° C to 1,000 ° C. Even at a low temperature of 400 ° C to 700 ° C, the carzolidine hydrazine is decomposed to a sufficiently high growth rate (film formation rate) to produce tantalum nitride. Further, when the decomposition temperature is from 300 ° C to 500 ° C, a high step coverage ratio can still be obtained.

For the CVD process and the thermal decomposition process, the methotrexate hydrazine gas may be prepared in advance or stored in a sealed container until use, or may be synthesized on the spot, and the gaseous reaction mixture containing the synthetic methionine hydrazine gas may be Enter the reaction chamber. The methotrexate gas and the hydrazine gas are fed into the synthesis chamber for on-site synthesis of the methyl hydrazine hydrazine gas. At this time, an inert diluent gas (such as an inert diluent gas previously introduced into the reaction chamber) and a preliminary reaction gas may be introduced into the synthesis chamber. Regarding the conditions for the input of the methotrexate gas and the hydrazine gas in the synthesis chamber, the pressure in the synthesis chamber should be maintained at 0.1 to 1,000 torr, and the flow rate ratio of the hydrazine gas/formamidine gas should be 10 to 1,000. The two gases can be reacted at a temperature of from room temperature to 500 °C. The formylalkylamine is produced by this reaction. Secondly, the methotrexate-containing hydrazine-containing gaseous reaction mixture produced in the synthesis chamber can be pressure-regulated by a pressure regulator and input into the previously exposed reaction chamber. The formalkaneamine used herein comprises a methylideneamine (H ₃ Si) _m N(H) _3-m (III) as defined by the formula (III).

Wherein m is an integer from 1 to 3. The hydrazine input into the synthesis chamber contains the hydrazine H(R ^x )NN(R ^y )R ^z (IV) defined by the formula (IV)

Wherein R ^x , R ^y and R ^z are each independently selected from a hydrogen atom, a methyl group, an ethyl group and a phenyl group.

For example, the formylalkylamine (I) can be produced by the reaction of a mercaptoalkylamine (III) with a hydrazine (IV).

1 is a block diagram of an embodiment of a CVD-based device for producing a tantalum nitride film, wherein the CVD-based device facilitates performing the method of the present invention for producing a tantalum nitride film. Example 1 exemplifies the use of a preformed gas source containing the prepared preform gas.

The production apparatus 10 shown in Fig. 1 is provided with a reaction chamber 11, a preform gas source 12, a hydrazine gas source 13, and an inert diluent gas source 14, wherein the gas can be supplied in a manner compliant with the environment.

The susceptor 111 is disposed in the reaction chamber 11, and the semiconductor substrate 112 such as a ruthenium substrate is mounted on the susceptor 111 (since the device illustrated in FIG. 1 is a single wafer device, only a single semiconductor substrate is mounted on the pedestal 111. on). A heater 113 is disposed in the susceptor 111 to heat the semiconductor substrate 112 to a set CVD reaction temperature. In the case of a batch device, a plurality of semiconductor substrates can be housed in the reaction chamber within 250 semiconductor substrates. The heater used in the batch device can have a different structure than the heater used in the single wafer device.

The preformed gas source 12 contains a sealed container containing a liquefied preform. The preformed body gas system is input from the preform gas source 12 via the preform gas supply line L1 and enters the reaction chamber 11. A shut-off valve V1 of the preformed gas source 12 and a flow rate controller such as a mass flow controller MFC1 are disposed in the line L1, wherein the mass flow controller MFC1 is located downstream of the shut-off valve V1. The preformed body gas system is controlled to a set flow rate by the mass flow controller MFC1 and is input into the reaction chamber 11.

The hydrazine gas source 13 contains a sealed container containing a liquefied hydrazine. The hydrazine gas system is input from the hydrazine gas source 13 via the hydrazine gas feed line L2 and enters the reaction chamber 11. A shut-off valve V2 and a flow rate controller such as a mass flow controller MFC2 are disposed in the line L2, wherein the mass flow controller MFC2 is located downstream of the shut-off valve V2. The hydrazine gas system is controlled to a set flow rate by the mass flow controller MFC2 and is input into the reaction chamber 11.

The inert diluent gas source 14 contains a sealed container containing an inert diluent gas. If necessary or desired, the inert diluent gas system is passed through an inert diluent gas feed line L3 and fed from an inert diluent gas source 14 and into the reaction chamber 11. As shown in Fig. 1, the inert diluent gas feed line L3 can be joined to the preform gas feed line L1, so that the inert diluent gas can be introduced into the reaction chamber 11 together with the preform gas. A shut-off valve V3 and a flow rate controller such as a mass flow controller MFC3 are disposed in the line L3, wherein the mass flow controller MFC3 is located at the outlet end of the shut-off valve V3. The inert gas system is controlled to a set flow rate by the mass flow controller MFC3 and is input into the reaction chamber 11.

The outlet of the reaction chamber 11 is connected to the exhaust gas treatment device by a line L4. Set 15. The exhaust gas treatment device 15 removes, for example, by-products and unreacted materials, and the gas system purified by the exhaust gas treatment device 15 is discharged from the system. A pressure sensor PG, a pressure regulator such as a butterfly valve BV1, and a vacuum pump PM are disposed in the line L4. Various gases are introduced into the reaction chamber 11 by respective mass flow controllers, and the pressure in the reaction chamber 11 is monitored by the pressure sensor PG, and is established by the operation of the pump PM and the opening control of the butterfly valve BV1. The set pressure value.

When a tantalum nitride film is produced by thermal decomposition of a mercaptoalkylamine gas, the use of the hydrazine feed system (the hydrazine gas source 13, the feed line L2, the shut-off valve V2, and the mass flow controller MFC2) becomes Not necessary, no need to set.

Figure 2 contains a block diagram of an apparatus for producing a tantalum nitride film containing a field device for producing a dimethyl hydrazine. The components in the second drawing that are the same as in the first embodiment are denoted by the same reference numerals, and the detailed description thereof will be omitted.

The production facility 20 shown in Fig. 2 includes a synthesis chamber 21 for synthesizing a methylenediamine in situ, in addition to the same reaction chamber 11 as shown in Fig. 1. A heater 211 is disposed around the synthesis chamber 21 for heating the inside of the synthesis chamber 21 to a set reaction temperature.

The production apparatus 20 shown in Fig. 2 is not provided with the preform gas source 12 shown in Fig. 1, but contains a source of the mercaptoalkylamine 22 which is reacted with a hydrazine to produce a dimethyl hydrazine. The form of the mercaptoalkylamine 22 comprises a sealed container containing the methylformamide in liquid form. The formamidine amine gas is fed from the formamidine source 22 via feed line L21 and enters synthesis chamber 21. The A shut-off valve V21 and a flow rate controller such as a mass flow controller MFC21 are disposed in the line L21, wherein the mass flow controller MFC21 is located downstream of the shut-off valve V21. The formamidine gas system is controlled to a set flow rate by the mass flow controller MFC21, and is input into the synthesis chamber 21.

The hydrazine gas source 13 is provided with a feed line L22 connected to the synthesis chamber 21, except for the feed line L2 connected to the reaction chamber 11. A shut-off valve V22 and a flow rate controller such as a mass flow controller MFC 22 are disposed in the line L22, wherein the mass flow controller MFC 22 is located at the outlet end of the shut-off valve V22. The hydrazine gas system is controlled to a set flow rate by the mass flow controller MFC22, and is input into the synthesis chamber 21.

The inert diluent gas source 14 is provided with a feed line L23 connected to the synthesis chamber 21, except for the feed line L3 connected to the reaction chamber 11. A shut-off valve V23 and a flow rate controller such as a mass flow controller MFC23 are disposed in the feed line L23, wherein the mass flow controller MFC23 is located at the outlet end of the shut-off valve V23. If necessary or desired, the inert diluent gas system is controlled to a set flow rate by the mass flow controller MFC 23 and is input into the synthesis chamber 21. The line L3 in the apparatus of Fig. 2 is directly connected to the reaction chamber 11.

The outlet of the synthesis chamber 21 is connected to the reaction chamber 11 by a line L24. A regulator such as a butterfly valve BV2 is provided in the line L24. After the pressure in the synthesis chamber 21 has been adjusted to a pressure suitable for input into the reaction chamber 11 by the butterfly valve BV2, the gaseous reaction mixture containing the methyl hydrazine hydrazine gas supplied from the synthesis chamber 21 is introduced into the reaction chamber 11.

With respect to the preform gas treatment portion of the apparatus for producing a tantalum nitride film shown in Fig. 1, the vapor phase material is withdrawn from the preform gas source 12 containing the liquid form preform gas, and by opening the valve V1 It is adjusted by the mass flow controller MFC1 and is input into the reaction chamber 11 via the line L1. However, the preformed gas may also be introduced into the reaction chamber 11 via the line L1 using a bubbler or an evaporator. Figure 3 shows a preformed gas feed system using a bubbler. The feed system acts to replace the preform gas source 12 and valve V1 in the production facility shown in Figure 1 and to provide a preformed gas source 32 containing the preform gas 31 in liquid form. Line L31 is inserted into the preform gas source 32 to bubble the inert gas into the preform gas 31 contained in the preform gas source 32 from the same inert gas source 33 as previously disclosed. The closing valve V31 is disposed in the line L31. The line L1 of the production plant shown in Fig. 1 is inserted into the preform gas source 32 located above the level of the preform gas 31. The shutoff valve V32 is disposed in the line L1. When the inert gas is bubbled into the preform, the preform is mixed into the inert gas and applied to the reaction chamber 11 shown in Fig. 1 via the line L1 by the flow rate control by the mass flow controller MFC1.

Figure 4 shows a preformed gas feed system using an evaporator. The feed system acts to replace the preform gas source 12 and the mass flow controller MFC1 in the production plant shown in Fig. 1 and to provide a preform gas source 42 containing the preform gas 22 in liquid form. A line L41 is provided in the preform gas source 42 to pressurize the liquid precursor gas 31 as an inert gas, and the inert gas is supplied from the same inert gas source 43 as previously disclosed. The shutoff valve V41 is disposed in the line L41. In addition, will be the first The line L1 of the production plant shown in the drawing is inserted into the preform gas 41 in the preform gas source 42. A shut-off valve V42, a liquid mass flow controller MFC41 at the outlet end of the shut-off valve V42, and an evaporator 44 located downstream of the liquid mass flow controller LMFC41 are disposed in the line L1. The liquid preform gas 41 pressurized for the inert gas from the inert gas source 43 flows through the line L1, is controlled by the liquid mass flow controller LMFC41, and is supplied to the evaporator 44. The liquid precursor is evaporated in the evaporator 44 and is fed into the reaction chamber 11 shown in Fig. 1. The inert gas may also be supplied to the evaporator 44 via the inert gas source 45 via line L42 to enhance evaporation of the liquid precursor within the evaporator 44. The line L42 is provided with, for example, a mass flow controller MFC42 for controlling the flow rate of the inert gas from the inert gas source 45, and a shut-off valve V43, which is located downstream of the mass flow controller MFC42. .

Example

The invention will be explained in more detail by the following working examples, but the invention is not limited to these working examples.

Example 1

This embodiment uses a production apparatus having the structure shown in Embodiment 1. When a TSA gas having a feed flow rate of 0.5 sccm or 4 sccm and a 1,1-bismethyl hydrazine (UDMH) gas having a feed flow rate of 40 sccm are input into a reaction chamber containing a ruthenium substrate, different CVD reactions are performed. A tantalum nitride film is formed on the tantalum substrate at a temperature (T). The pressure in the reaction chamber is maintained at 1 torr. Measure the rate of deposition (growth) of tantalum nitride during the process and The value obtained is plotted in Figure 5 for 1,000 times the reciprocal of the reaction temperature (in K). Line a in Figure 5 is the result of the feed 0.5 sccm TSA gas (UDMH/TSA feed flow ratio = 80), while line b is the feed 4 sccm TSA gas (UDMH/TSA feed flow ratio = 10) The result graph.

From the results of Fig. 5, it is known that the growth rate of the tantalum nitride film is higher at a lower UDMH/TSA feed flow rate ratio and increases as the reaction temperature increases. However, even when performed at temperatures as low as 480 ° C, the growth rate of the tantalum nitride film is still high enough.

The composition of the obtained tantalum nitride film was found to be Si _0.8-0.9 N by Auger elemental analysis and ellipsometry. The carbon nitride content of the tantalum nitride film prepared at a feed rate ratio of UDMH/TSA of 80 was only 3% by weight. The etch rate of each tantalum nitride film by 0.25% aqueous hydrogen fluoride is 30-50 angstroms/minute in all cases, which is substantially lower than the etch rate of the PECVD tantalum nitride film.

In this embodiment, the gaseous reaction mixture in the reaction chamber is also analyzed by Fourier transform infrared spectroscopy (FTIR). At two UDMH/TSA feed flow ratios, it has been confirmed that: (a) the two main peaks of TSA (the peak at about 947 cm ^-1 is SiN bonding, and the peak at about 2172 cm ^-1 is SiH) The intensity ratio of the bond (I(947)/I(2172)) changes (see Figure 6), and (b) the peak of the SiH bond migrates from 2172 cm ^-1 to 2163 cm ^-1 . This result confirmed that the bis-decylalkylmethylamine (SiH ₃ ) ₂ NN(CH ₃ ) ₂ was produced by the reaction of TSA with UDMH at 450 ° C or higher. The relationship and synthesis related to the production of the tantalum nitride film in the present embodiment are as follows: (I) the methylidene hydrazine can act as a precursor; (II) the methylidene hydrazine can be obtained by the formylamine and the hydrazine. And (III) forming a tantalum nitride using a gaseous reaction mixture containing a methyl hydrazine alkylamine produced by the reaction of a mercaptoalkylamine with a hydrazine.

Example 2

Using a production apparatus having the structure shown in FIG. 1, a tantalum nitride film is formed in a reaction chamber containing a tantalum substrate at a different reaction temperature, wherein a trench having an aspect ratio (depth/diameter) of 10 is formed on the tantalum substrate. (Diameter: 0.6 microns). UDMH was fed at a flow rate of 40 sccm; TSA gas was fed at a flow rate of 4 sccm; and the pressure in the reaction chamber was 1 torr. The step coverage ratio of the tantalum nitride film obtained at different temperatures was measured by a scanning electron microscopy (SEM), and the results are shown in Fig. 7.

The results of Fig. 7 show not only that the step coverage ratio of the tantalum nitride film product can be improved by establishing a reaction temperature of 500 ° C, but also that the step coverage ratio can be further improved by setting the reaction temperature to a lower value.

The present invention has been described above by way of various specific examples and working examples, but the invention is not limited thereto. Different specific examples of the foregoing can be used in combination.

The beneficial effects of the invention

As stated previously, the process of the present invention does not concomitantly produce ammonium chloride, and no significant carbonaceous contaminants are incorporated into the film product, and even at relatively low levels. A tantalum nitride film having better film properties can also be produced at a temperature.

10,20‧‧‧Nitrided Niobium Thin Film Production Equipment

11‧‧‧Reaction room

12‧‧‧Precursor gas source

13‧‧‧Hydrazine gas source

14‧‧‧Inert diluent source

15‧‧‧Exhaust gas treatment device

21‧‧‧Methylalkyl hydrazine synthesis room

22‧‧‧Mercaptoalkylamine gas source

111‧‧‧Base

112‧‧‧Semiconductor substrate

113,211‧‧‧heater

L1-L4, L21-L24‧‧‧ gas feed line

V1-V3, V21-V23‧‧‧Close valve

PG‧‧‧ pressure device

MFC1-MFC3, MFC21-MFC23‧‧‧ Mass flow controller

BV1, BV2‧‧‧ butterfly valve

PM‧‧‧vacuum pump

Schema part

Figure 1 contains a block diagram of an embodiment of an apparatus for producing a tantalum nitride film.

Figure 2 contains a block diagram of another embodiment of an apparatus for producing a tantalum nitride film.

Figure 3 contains a block diagram of the precursor gas feed system prior to use of the bubbler.

Figure 4 contains a block diagram of the precursor gas feed system prior to use of the evaporator.

Figure 5 contains a graph of the relationship between the CVD reaction temperature and the growth rate of the tantalum nitride film.

Figure 6 contains a plot of the relationship between the two main peak intensity ratios of the TSA and the reaction temperature.

Figure 7 contains a graph of the relationship between the CVD reaction temperature and the step coverage ratio of the tantalum nitride film.

10‧‧‧Nitrided Niobium Thin Film Production Equipment

11‧‧‧Reaction room

12‧‧‧Precursor gas source

13‧‧‧Hydrazine gas source

14‧‧‧Inert diluent source

15‧‧‧Exhaust gas treatment device

111‧‧‧Base

112‧‧‧Semiconductor substrate

113‧‧‧heater

L1-L4‧‧‧ gas feed line

V1-V3‧‧‧Close valve

PG‧‧‧ pressure device

MFC1-MFC3‧‧‧mass flow controller

BV1‧‧‧Butterfly Valve

PM‧‧‧vacuum pump

Claims (16)

A method for producing a tantalum nitride film by vapor phase growth, the method comprising: supplying a hydrazine gas and a methyl hydrazine hydrazine gas into a reaction chamber containing at least one substrate, and by the two gases Forming a tantalum nitride film on the at least one substrate, characterized in that the previously described formazanyl hydrazine is defined by the formula (I): H ₃ Si(R ^a )NN(R ^b )R ^c (I Wherein R ^a , R ^b and R ^c are each independently selected from the group consisting of a methyl group, a hydrogen atom, a methyl group, an ethyl group, and a phenyl group. The method for producing the first aspect of the patent application, characterized in that the formylalkylamine is fed into the reaction chamber by a reaction mixture containing a formazan hydrazine in a free synthesis chamber in the future. Wherein the reaction mixture containing the formylalkylamine is produced by the reaction of a formamidine gas and a second hydrazine gas in the synthesis chamber. The method for producing the first or second aspect of the patent application, characterized in that the hydrazine gas system fed into the pre-reaction chamber defines H(R ¹ )NN(R ² )R ³ (II) by the formula (II), wherein R ¹ , R ² and R ³ are each independently selected from a hydrogen atom, a methyl group, an ethyl group and a phenyl group. For example, the method for producing the second aspect of the patent application, wherein the methylalkane gas system disclosed above is defined by the formula (III) (H ₃ Si) _m N(H) _3-m (III) wherein m is from 1 An integer to 3. The method for producing the second aspect of the patent application is characterized in that the second hydrazine gas system disclosed above defines H(R ^x )NN(R ^y )R ^z (IV) wherein R ^{x is} represented by the formula (IV) R ^y and R ^z are each independently selected from a hydrogen atom, a methyl group, an ethyl group, and a phenyl group. The method for producing the first or second aspect of the patent application is characterized in that the reaction temperature between the precursor gas and the previously disclosed amine gas is set between 300 ° C and 700 ° C. The production method of claim 1 or 2, characterized in that a pressure of 0.1 to rr to 1,000 torr is established in the previously disclosed reaction chamber. The method of producing the first or second aspect of the patent application is characterized in that an inert diluent gas is also supplied to the previously exposed reaction chamber. A method for producing a tantalum nitride film by vapor phase growth, the method comprising: feeding a methyl hydrazine hydrazine gas into a reaction chamber containing at least one substrate, and decomposing by the methionine hydrazine gas And forming a tantalum nitride film on the at least one substrate. The method for producing the ninth aspect of the patent application, characterized in that the previously described methylalkane amide is defined by the formula (I): H ₃ Si(R ^a )NN(R ^b )R ^c (I) wherein R ^a , R ^b and R ^c are each independently selected from the group consisting of a methyl group, a hydrogen atom, a methyl group, an ethyl group, and a phenyl group. The method for producing a ninth or tenth aspect of the patent application, characterized in that the methyl hydrazine hydrazine is fed into the reaction chamber by a reaction mixture containing a dimethyl hydrazine amide from a synthesis chamber, thereby supplying a reaction In the chamber, wherein the reaction mixture containing the methylidene alkylamine is produced by the reaction of a formamidine gas and a second hydrazine gas in the synthesis chamber. The production method of claim 11, wherein the hydrazine gas system defined by the formula (IV) defines H(R ^x )NN(R ^y )R ^z (IV) wherein R ^x , R ^y It is independently selected from the R ^z system to be selected from a hydrogen atom, a methyl group, an ethyl group, and a phenyl group. For example, the method for producing the patent scope of claim 11 wherein the methylalkaneamine gas system is defined by the formula (III) (H ₃ Si) _m N(H) _3-m (III) wherein m is from 1 An integer to 3. The production method according to claim 9 or 10, characterized in that the decomposition of the previously disclosed methylenediamine gas is carried out at a temperature between 300 ° C and 700 ° C. The production method of claim 9 or 10, characterized in that a pressure of 0.1 torr to 1,000 torr is established in the previously disclosed reaction chamber. The method of producing the invention of claim 9 or 10, characterized in that the inert diluent gas is also supplied to the previously exposed reaction chamber.