KR20170005305A - Process for the preparation of trisalkylaminosilane - Google Patents

Abstract

The present invention relates to a method of preparing tris(alkylamino)silane comprising the steps in which: (a) an amine represented by chemical formula of R^1R^2NH is made to react with a halosilane represented by chemical formula of SiH_nX_4-n; and (b) tris(alkylamino)silane, a product of the step (a), is made to react with a metal hydride and converted into tris(alkylamino)silane. In the chemical formulas, R^1 and R^2 each independently represent a linear, branched or cyclic alkyl group having 1 to 6 carbon atoms; n is 0 or 1; X is a fluoro-, chloro-, bromo-, or iodo-group; and the step (a) necessarily includes a compound in which n equals zero. According to the present invention, by using a metal hydride to reduce a tris(alkylamino)silane intermediate, which is a reaction product of amine and halosilane, and thus convert the same into tris(alkylamino)silane, tris(alkylamino)silane can be obtained in a high yield and alkylamine hydrochloride produced as a byproduct can be easily removed, and accordingly, the impurity content in the final product can be reduced to a few ppb or less.

Description

PROCESS FOR THE PREPARATION OF TRISALKYLAMINOSILANE < RTI ID = 0.0 >

The present invention relates to a process for preparing tris (alkylamino) silanes. (Alkylamino) silane intermediate, which comprises reacting an amine with at least one halosilane to obtain a tris (alkylamino) halosilane intermediate, and reacting the intermediate with a reducing agent to obtain a tris And a method for producing the same.

Aminosilane is a compound useful as a film-forming material for electronic materials. The aminosilane precursors may be formed by a chemical vapor deposition (CVD) or an atomic layer deposition (ALD) in a semiconductor manufacturing process, such as a silicon-containing film such as a silicon nitride film, a silicon carbonitride film, or a silicon oxynitride ) Thin films. ≪ / RTI >

Japanese Patent Laid-Open Publication No. H06-132284 discloses a process for producing ammonia and an aminosilane derivative represented by the general formula (R ¹ R ² N) _n SiH _{4 -n wherein} R ¹ and R ² are -H, -CH ₃ , -C ₂ H ₅ , -C ₃ H ₇ or C ₄ H ₉ ) is formed by plasma chemical vapor deposition or thermochemical deposition in the presence of nitrogen.

U.S. Pat. No. 5,234,869 reports that a silicon nitride film is formed by chemical vapor deposition of Si (N (CH ₃ ) ₂ ) ₄ (TDMASi) and ammonia at a chamber temperature of 700 ° C. and a pressure of 0.5 torr. Under the addition of the combined gas of ammonia or nitrogen _{SiH (N (CH 3) 2} ) 3 (tDMASi), SiH 2 (N (CH 3) 2) 2 (BDMASi) , and _{SiH 3 (N (CH 3)} 2) ( MDMASi) have been proposed as alternative reactants.

In US Patent No. 5,874,368, bis (t-butylamino) silane was used as a precursor for depositing a silicon nitride thin film by low-pressure chemical vapor deposition (CVD) at 500 to 800 ° C. Also in U.S. Patent Nos. 5,874,368 and 6,153,261, a silicon nitride film was formed using bis (t-butylamino) silane. U.S. Patent No. 6,391,803 discloses a _{Si (N (CH 3) 2} ) 4, SiH (N (CH 3) 2) 3, SiH 2 (N (CH 3) 2) 2, SiH 3 (N (CH 3) 2) , A thin film was formed by atomic layer deposition using tris (dimethylamino) silane as the first reactant.

Recently, as commercial use and use of tris (alkylamino) silane has increased, a process for producing aminosilane with high yield and efficiency by various synthesis methods has been of interest. A typical method for producing an aminosilane derivative is to react the halosilane with a secondary amine, separate the formed ammonium chloride and aminosilane, and then distillate and purify to obtain high purity aminosilane.

A typical preparation method of tris (alkylamino) silane is to obtain tris (alkylamino) silane through a process such as filtration and distillation purification after reacting chlorosilane and amine which are commercially available at a low temperature.

Reaction of chlorosilane with amine gives tris (alkylamino) silane and alkylamine hydrochloride which is a white solid and a sublimation byproduct. When a distillation purification process is performed to obtain pure tris (alkylamino) silane, the resulting tris (alkylamino) silane is obtained in the state that a halogen-containing impurity such as an alkylamine hydrochloride is contained in a concentration of several ppm to several hundred ppm.

U.S. Patent Publication No. 2012-0165564 discloses a method of reducing the concentration of byproducts such as alkyl lithium, Grignard reagent or an amine such as dimethylamine, triethylamine or trihexylamine to several ppb to several ppm, (Alkylamino) silane.

On the other hand, although the reaction of amine with trichlorosilane appears to be a one-step reaction in the US patent application publication no. 2012-0165564 and Japanese patent application publication No. S56-068686, in practice, in order to remove halogen impurities such as alkyl amine hydrochloride (Alkylamino) silane by a two-step process comprising adding a metal hydride, a Grignard reagent and / or a new amine to obtain tris (alkylamino) silane.

In the semiconductor manufacturing process, chemical vapor deposition is performed at a temperature of 700 ° C or higher to obtain the best film characteristics by depositing a silicon nitride thin film having a proper growth rate and uniformity from a mixture of ammonia (NH ₃ ) and tris (alkylamino) silane. However, when sublimating ammonium chloride (NH ₄ Cl) or other halogen-containing by-products are present at the time of distillation purification, problems such as particle formation or turbid film formation may occur in the film production process. Furthermore, they may cause particle formation and deposition in the back of the tubes, piping lines and pump systems, which may cause damage to the wafer and the pump.

Accordingly, there is a need to develop a method for producing tris (alkylamino) silane which has a low content of halogen atom-containing impurities at a low cost and at a high yield to an extent suitable for use in a semiconductor manufacturing process.

U.S. Published Patent Application No. 2012-0165564 U.S. Published Patent Application No. 2012-0165564 Japanese Laid-Open Patent S56-068686

It is an object of the present invention to provide a method for producing tris (alkylamino) silane in high yield using commercially available and inexpensive raw materials.

Another object of the present invention is to provide a method for producing a high-purity tris (alkylamino) silane in which the content of a halogen-containing impurity, particularly a salt of alkylamine hydrochloride, is reduced to several ppb or less.

The technical problem of the present invention described above

(a) reacting an amine represented by the following formula (1) with a halosilane represented by the formula (2); And

(alkylamino) silane in the product of step (a) with a metal hydride to convert the tris (alkylamino) halosilane to a tris (alkylamino)

(Alkylamino) silane represented by the following formula (3).

[Chemical Formula 1]

(2)

SiH _n X _{4 -n}

(3)

Wherein R ¹ and R ² are each independently a linear, branched or cyclic alkyl group having 1 to 6 carbon atoms, n is 0 or 1, X is fluoro, chloro, bromo, or iodo, (a) in which n = 0.

According to the present invention, there is provided a method for producing a high-purity tris (alkylamino) silane having a content of halogen-containing impurities reduced to several ppb or less while using a commercially available and inexpensive raw material in a high yield.

In the present invention, the tris (alkylamino) halosilane intermediate produced by the reaction of an amine with halosilane is reacted with a metal hydride to obtain trisalkylaminosilane in a high yield, and the alkylamine hydrogens Chloride can be easily removed, thereby achieving the effect of reducing the impurity content in the final product to several ppb or less.

1 is a gas chromatographic (GC) analysis result of a mixture of tris (dimethylamino) chlorosilane and tris (dimethylamino) silane, which is an intermediate of Example 3 of the present invention.
2 shows the results of mass spectrometry (GC-MS) of a mixture of tris (dimethylamino) chlorosilane and tris (dimethylamino) silane, which are intermediates of Example 3 of the present invention. (A: tris (dimethylamino) b: tris (dimethylamino) silane)
3 is a hydrogen nuclear magnetic resonance (H-NMR) spectrum of the tris (dimethylamino) silane prepared in Example 3 of the present invention.
4 is a carbon nuclear magnetic resonance (C-NMR) spectrum of the tris (dimethylamino) silane prepared in Example 3 of the present invention.
5 is a silicon nuclear magnetic resonance (Si-NMR) spectrum of the tris (dimethylamino) silane prepared in Example 3 of the present invention.
6 is a GC analysis result of the pure tris (dimethylamino) silane obtained in Example 3 of the present invention.
7 is a mass analysis (GC-MS) result of the pure tris (dimethylamino) silane obtained in Example 3 of the present invention.
8 is a TG-DSC analysis result of the pure tris (dimethylamino) silane obtained in Example 3 of the present invention.

The present invention relates to a process for the preparation of trisalkylaminosilanes and a process for the effective removal of salts of alkylamine hydrochlorides. According to the process for producing tris (alkylamino) silane according to the present invention, tetrahalosilane, which is commercially available and cheap in price, can be used singly or in combination with trihalosilane as a reactant, whereby the content of halogen impurities is several ppb Lt; / RTI > can be prepared.

Therefore,

(a) reacting an amine represented by the following formula (1) with a halosilane represented by the formula (2); And

(b) adding a metal hydride to the filtrate of the reaction mixture of step (a) and stirring to obtain a tris (alkylamino) silane represented by the following formula (3)

Tris (alkylamino) silane.

[Chemical Formula 1]

(2)

SiH _n X _4-n

(3)

In the above Chemical Formulas 1 to 3, R ¹ and R ² are each independently a straight, branched or cyclic alkyl group having 1 to 6 carbon atoms, preferably independently methyl, ethyl, n-propyl, isopropyl, n Wherein n is 0 or 1 and X is selected from the group consisting of methyl, ethyl, propyl, isopropyl, butyl, isobutyl, tert- butyl, pentyl, methylcyclopentyl, hexyl and cyclohexyl, Iodo, and in step (a) n = 0.

In the step (a), it is preferable in terms of yield to react the amine of the formula (1) and the halosilane of the formula (2) in a stoichiometric ratio, that is, a molar ratio of 6.0 to 6.4: 1, Tris (alkylamino) halosilane, which is the main product of a), is obtained in the highest yield.

When the trihalosilane and the tetrahalosilane are used in combination as the halosilane in the step (a), the molar ratio of the amine to the halosilane is the same as described above. In this case, the molar ratio of the trihalosilane and the tetrahalosilane The sum of mole% should not exceed 100%.

Tetrahalosilanes, such as tetrachlorosilane, are a raw material widely used in the field of electronic materials and are relatively inexpensive compared to trihalosilanes such as trichlorosilane. Since trichlorosilane has a boiling point of 32 to 34 캜, it is inconvenient to react at a low temperature. However, tetrachlorosilane has an advantage of being able to produce aminosilane under mild reaction conditions at a boiling point of about 58 캜. Thus, in the present invention, it is possible to lower the manufacturing cost of tris (alkylamino) silane by using tetrahalosilane alone or in combination with trihalosilane.

Tris (alkylamino) halosilane is produced when tetrahalosilane alone is used as the reactant in the step (a). In this case, when the reaction mixture is filtered and a metal hydride is added to the filtrate, a trace amount of alkylamine hydrohalide is converted into a salt such as an amine and a metal halide. Therefore, the salt is removed by filtration, and the filtrate is purified by distillation High-purity tris (alkylamino) silane can be obtained.

When trichlorosilane and tetrachlorosilane are used in combination as the halosilane according to one embodiment of the present invention, the reaction formulas of the above-mentioned steps (a) and (b) can be represented by the following Reaction Schemes 1 and 2.

[Reaction Scheme 1]

[Reaction Scheme 2]

In the above Reaction Schemes 1 and 2, R ¹ and R ² are as defined in Chemical Formulas 1 to 3.

In one embodiment of the present invention, in step (a), trichlorosilane and tetrachlorosilane were mixed as halosilane in a molar ratio of 50:50 and reacted with dimethylamine, and analyzed by gas chromatography. As a result, 46% It was confirmed that tris (dimethylamino) silane and 54% tris (dimethylamino) chlorosilane were produced.

When the amine reacts with trichlorosilane as shown in Reaction Scheme 3 below, the amine attacks Si and the chlorine atom of the Si-Cl bond is released as in Path A. As a result, tris Dimethylamino) silane is produced. However, tris (dimethylamino) chlorosilane is produced in a proportion of 1 to 8% as the hydrogen atoms of the Si-H bond are released as in the case of the path B.

[Reaction Scheme 3]

Thus, in the present invention, the tris (alkylamino) silane in the reaction product of step (a) is reduced to tris (alkylamino) silane by reacting with the metal hydride in step (b) .

In the present invention, it is effective that the reaction temperature of step (a) is carried out at a temperature in the range of -30 to 80 ° C, preferably -20 to 60 ° C. If it is necessary to control the heat generated during the reaction, circulating refrigerant may be introduced into the jacket reactor or a cooling temperature control device may be installed.

In order to effectively separate the (trisalkylamino) halosilane produced in the step (a) reaction and the alkylamine hydrohalide salt produced as a by-product, it is preferable to use at least one filter. A suitable filtration medium is a 0.5 to 5 micron mesh filter, wherein the reduced pressure is suitably performed at 500 to 750 Torr. In order to effectively remove ammonium chloride, filtration is preferably carried out at a temperature in the range of 0 to 30 ° C.

The step (b) is a reduction reaction in which the halogen of tris (alkylamino) halosilane, which is the product of step (a), is replaced with hydrogen. Thus the metal hydride used in step (b) is a metal hydride which is known as a reducing agent in the art, for example, LiH, NaH, KH, NaBH _4, KBH _4, LiAlH ₄ and NaAlH ₄ from the group consisting of: 1 More than one species can be selected.

In step (b), the reaction mixture of step (a) is heated to a molar ratio of tris (alkylamino) halosilane, tris (alkylamino) silane or a mixture thereof and metal hydride, 0.25 - 1.0 by adding a metal hydride. However, when reacting with an amine using a combination of trihalosilane and tetrachlorosilane as the halosilane in the step (a), the amount of the metal hydride added in the step (b) Lt; RTI ID = 0.0 > 1.0 < / RTI >

If the reaction of substituting the halogen with hydrogen in the reaction of step (b) is slow, refluxing when the metal hydride (e.g., LAlH ₄ ) remains in the reactant, or refluxing about 1/10 of the metal hydride (e.g., LAlH ₄ ) may be added and the reaction mixture may be refluxed to proceed to the product. However, it is effective to keep the reaction temperature in the step (b) not to exceed the range of 0 ° C to 80 ° C, and the most suitable reaction temperature is 30 ° C to 40 ° C. When the reaction is carried out under such conditions for 4 to 24 hours, the reduction reaction is completed.

In the above steps (a) and (b), the solvent may be selected from the group consisting of linear, branched and cyclic saturated hydrocarbon solvents, aromatic hydrocarbon solvents, ketone solvents, ether solvents, ester solvents, Preferably selected from the group consisting of n-pentane, i-pentane, n-hexane, i-hexane, benzene, toluene, xylene, trimethylbenzene, ethylbenzene, methylethylbenzene, tetrahydrofuran, dimethylether, diethyl Ether, dimethoxy methane, diisopropyl ether, diglyme, and acetonitrile.

In order to prevent the introduction of impurities into the final product, to prevent the raw material from being decomposed by the water to generate siloxane, and to prevent hydrolysis from each amine, the purity is high, the moisture content is as low as possible, It may be preferable to use an electronic grade solvent which does not cause a metal impurity problem when purifying the organic solvent.

When producing high purity tris (alkylamino) silane that can be used as a semiconductor device material, it is preferable to use a tetrahalosilane having a purity of 99.99% or more as a reactant, and an alkylamine compound having a purity of 99.98% Or more, but the scope of the present invention is not limited thereto.

When introducing a reagent into a reactor used for producing tris (alkylamino) silane according to the present invention, it may be preferable to use an inert gas as a carrier gas so as not to be exposed to air or water. As such an inert gas, Any inert gas well known in the art, for example, nitrogen, argon, helium, and combinations thereof, may be used.

In the present invention, the final product can be obtained in a yield of 80% or more in the present invention, and tris (alkylamino) silane having a purity of 99.99% or more can be obtained through two distillation purification steps.

Example

Hereinafter, the present invention will be described in more detail with reference to the following examples. However, the examples are merely examples of the present invention and the scope of the present invention should not be construed as being limited to these examples.

< Example  1> From tetrachlorosilane Of tris (dimethylamino) silane  Produce

(1) Preparation of intermediate

A mechanical stirrer, a digital thermometer and a condenser were installed in a 5-necked 20 L round-bottomed flask which was dried under a nitrogen stream, 6,000 mL of isopropyl ether was added, cooled to -20 ° C, and stirred for 30 minutes. Dimethylamine (2,000 g, 44.3424 mol) was added while keeping the temperature at -20 ° C, and then a solution of tetrachlorosilane (1,215 g, 7.152 mol) dissolved in 1,000 mL of isopropyl ether was slowly added to the above reaction solution. After the introduction of tetrachlorosilane was completed, the temperature of the reaction product was raised to room temperature. The reaction was stirred at room temperature for 2 hours and then at 40 ° C for 3 hours. The reaction mixture was sampled and analyzed by gas chromatography to confirm reaction conversion ratio and end point.

The resulting white solid was then filtered and washed with isopropyl ether three times with 200 mL each. The white solid was removed from the filter, and a filtrate was obtained.

(2) Production of tris (dimethylamino) silane

LiAlH ₄ (135.86 g, 3.577 mol) was slowly added while maintaining the filtrate at room temperature. After the addition, the temperature was raised to 50 DEG C and refluxed for 6 hours. After refluxing, the reaction was cooled to room temperature, filtered and washed with isopropyl ether three times with 200 mL each to give a clear filtrate. Samples were taken from the obtained filtrate and analyzed by gas chromatography to confirm the reaction conversion ratio and the end point.

The filtrate was transferred little by little to a 2 L flask of a fractionation distillation apparatus equipped with distillation head, column, condenser and diaphram pump, and concentrated and repeatedly worked to remove the solvent. After removing the solvent, the residue was vacuum distilled to obtain 946 g (yield: 82%) of tris (dimethylamino) silane at 74 DEG C to 75 DEG C at 100 Torr (760 Torr to 142 DEG C (Document Value)). The residual chlorine content of the obtained tris (dimethylamino) silane was measured by ion chromatography to obtain 7.1 ppb.

< Example  2> From tetrachlorosilane Of tris (dimethylamino) silane  Produce

60% NaH (21.5 g, 0.5366 mol) and LiAlH ₄ (135.86 g, 3.577 mol) were slowly added while maintaining the filtrate at room temperature after an intermediate was prepared in the same manner as in (1) After the addition was completed, the temperature was raised to 50 DEG C and refluxed for 7 hours. After refluxing, the reaction was cooled to room temperature, filtered and washed with isopropyl ether three times with 200 mL each to give a clear filtrate. Samples were taken from the obtained filtrate and analyzed by gas chromatography to confirm the reaction conversion ratio and the end point.

The filtrate was transferred little by little to a 2 L flask of a fractionation distillation apparatus equipped with distillation head, column, condenser and diaphram pump, and concentrated and repeatedly worked to remove the solvent. After removal of the solvent, the residue was vacuum distilled to give 992 g (yield: 86%) of tris (dimethylamino) silane at 74 ° C to 75 ° C and 100 torr (760 torr to 142 ° C (literature value)). The residual chlorine content of the obtained tris (dimethylamino) silane was measured by ion chromatography to obtain a result of 6.9 ppb.

< Example  3 > 50:50 Tetrachlorosilane and From trichlorosilane Of tris (dimethylamino) silane  Produce

(1) Preparation of intermediate

A mechanical stirrer, a digital thermometer and a condenser were installed in a 5-necked 20 L round-bottomed flask which was dried under a nitrogen stream, 6,000 mL of isopropyl ether was added, cooled to -20 ° C, and stirred for 30 minutes. Dimethylamine (2,000 g, 44.3424 mol) was added while maintaining the temperature at -20 ° C, and then tetrachlorosilane (607.5 g, 3.576 mol) and trichlorosilane (484.33 g, 3.576 mol) were dissolved in 1,000 mL of isopropyl ether The mixed solution was gradually added to the above reaction solution. After the addition of chlorosilane was completed, the temperature of the reaction was raised to room temperature. The reaction was stirred at room temperature for 2 hours and then at 2O &lt; 0 &gt; C for 2 hours. The reaction mixture was sampled and analyzed by gas chromatography to confirm reaction conversion ratio and end point.

The resulting white solid was then filtered and washed with isopropyl ether three times with 200 mL each. The white solid was removed from the filter, and a filtrate was obtained. The GC analysis of the filtrate yielded the results of the GC shown in FIG. 1 and the GC-MS shown in FIG. 2.

FIG. 2 (a) is a mass spectrometry (GC-MS) result of an intermediate tris (dimethylamino) chlorosilane and FIG. 2 (b) is a mass spectrometry (GC-MS) result of tris (dimethylamino) silane.

Therefore, it was confirmed that the filtrate contained the intermediate tris (dimethylamino) chlorosilane and tris (dimethylamino) silane.

(2) Production of tris (dimethylamino) silane

60% NaH (21.5 g, 0.5366 mol) and LiAlH ₄ (135.86 g, 1.788 mol) were slowly added while maintaining the filtrate at room temperature. After the addition, the temperature was raised to 50 DEG C and refluxed for 6 hours. After refluxing, the reaction was cooled to room temperature, filtered and washed with isopropyl ether three times with 200 mL each to give a clear filtrate. Samples were taken from the obtained filtrate and analyzed by gas chromatography to confirm the reaction conversion ratio and the end point.

The filtrate was transferred little by little to a 2 L flask of a fractionation distillation apparatus equipped with distillation head, column, condenser and diaphram pump, and concentrated and repeatedly worked to remove the solvent. The solvent was removed and the residue was subjected to vacuum distillation to obtain 969 g (yield: 84%) of tris (dimethylamino) silane at 74 DEG C to 75 DEG C at 100 Torr (760 Torr to 142 DEG C (Document Value)). The residual chlorine content of the obtained tris (dimethylamino) silane was measured by ion chromatography to obtain a result of 6.6 ppb.

Hydrogen nuclear magnetic resonance (H-NMR), carbon nuclear magnetic resonance (C-NMR), silicon nuclear magnetic resonance (Si-NMR) and gas chromatography (GC) analyzes of the filtrate collected in the above- GC analysis, mass spectrometry (GC-MS), and TG-DSC analysis were performed on the finally obtained pure compound. As a result, it was confirmed that the collected filtrate and the final compound obtained were tris (dimethylamino) silane. FIG. 3 shows the nuclear magnetic resonance (H-NMR) spectrum of the hydrogen atom, FIG. 4 shows the carbon nuclear magnetic resonance (C-NMR) spectrum and FIG. 5 shows the spectrum of the silicon nuclear magnetic resonance The GC analysis results are shown in Fig. 6, the GC-MS analysis results are shown in Fig. 7, and the thermogravimetric (TG) analysis results are shown in Fig.

The present invention has been described above by way of examples. It will be understood by those skilled in the art that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. It is therefore to be understood that the above-described embodiments are only illustrative of the present invention and are not intended to limit the scope of the invention. The scope of the present invention is defined by the appended claims rather than the detailed description, and all changes or modifications derived from the meaning and scope of the claims and their equivalents should be construed as being included in the scope of the present invention.

Claims (9)

(a) reacting an amine represented by the following formula (1) with halosilane represented by the following formula (2); And
(alkylamino) silane, which comprises reacting tris (alkylamino) halosilane in the product of step (a) with a metal hydride to form tris (alkylamino) : &Lt;
[Chemical Formula 1]

(2)
SiH _n X _{4 -n}
(3)

R ¹ and R ² are each independently a straight, branched or cyclic alkyl group having 1 to 6 carbon atoms, X is fluoro, chloro, bromo or iodo, n is 0 or 1, It necessarily contains a compound in which n = 0 in step (a). The method according to claim 1,
Wherein R ¹ and R ² are each independently selected from the group consisting of methyl, ethyl, n-propyl, isopropyl, n-butyl, i-butyl, t-butyl, pentyl, methylcyclopentyl, hexyl and cyclohexyl (Alkylamino) silane. The method according to claim 1,
Wherein the secondary amine and halosilane are reacted in a molar ratio of 6.0 to 6.4: 1 in the step (a). The method according to claim 1,
Wherein the halosilane in step (a) is a tetrahalosilane alone or a combination of trihalosilane and tetrahalosilane. The method according to claim 1,
Wherein the metal hydride is added such that the molar ratio between halosilane and metal hydride in step (a) in step (b) is 1.0: 0.25-1.0. The method according to claim 1,
Wherein the metal hydride is reacted in step (b) to a molar ratio of tetrahalosilane used in step (a) of not more than 1.0 to the tris (alkylamino) silane. The method according to claim 1,
In the steps (a) and (b), one kind or two or more species selected from the group consisting of linear, branched and cyclic saturated hydrocarbon solvents, aromatic hydrocarbon solvents, ketone solvents, ether solvents, ester solvents and cyano solvents (Alkylamino) silane is used. 8. The method of claim 7,
The solvent is selected from the group consisting of n-pentane, i-pentane, n-hexane, i-hexane, benzene, toluene, xylene, trimethylbenzene, ethylbenzene, methylethylbenzene, tetrahydrofuran, dimethylether, diethylether, Diisopropyl ether, diglyme, and acetonitrile. &Lt; RTI ID = 0.0 &gt; 11. &lt; / RTI &gt; The method according to claim 1,
The metal hydride is _{LiH, NaH, KH, NaBH 4} , KBH 4, LiAlH the method for producing a tris (dialkylamino) silane to ₄ and NaAlH _4, which is at least one selected from the group consisting of.

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