TRIPHENYLGERMYLSILANE AND TRICHLOROSILYL-TRICHLOROGERMANE FOR THE PRODUCTION OF GERMANIUM-SILICON LAYERS, AND METHOD FOR THE PRODUCTION THEREOF FROM TRICHLOROSILYL-TRIPHENYLGERMANE

Abstract

Triphenylgermylsilane (Ph.sub.3GeSiH.sub.3) is useful for the production of germanium-silicon layers (GeSi) or as transfer agent of silane groups (SiH.sub.3). Further, a method describes the production of triphenylgermylsilane (Ph.sub.3GeSiH.sub.3) by reducing trichlorosilyltriphenylgermane (Ph.sub.3GeSiCl.sub.3) with a hydride in solution, and another method describes the production of trichlorosilyltrichlorogermane (C.sub.3GeSiCl.sub.3) by reacting trichlorosilyltriphenylgermane (Ph.sub.3GeSiCl.sub.3) with hydrogen chloride (HCl) in the presence of AlCl.sub.3 in solution. In addition, trichlorosilyltrichlorogermane is also used for the production of germanium-silicon layers (GeSi).

Claims

1. A triphenylgermylsilane with a formula of Ph.sub.3GeSiH.sub.3.

2. A process for preparing triphenylgermylsilane, the process comprising: dissolving trichlorosilyltriphenylgermane of formula Ph.sub.3GeSiCl.sub.3 in a solvent, and reducing the trichlorosilyltriphenylgermane with addition of a hydride to obtain a product solution.

3. The process according to claim 2, wherein the solvent is diethyl ether.

4. The process according to claim 2, wherein the hydride is lithium aluminium hydride.

5. The process according to claim 2, wherein the hydride is used in a molar ratio to the trichlorosilyltriphenylgermane in the range from 2:1 to 1:2.

6. The process according to claim 2, wherein a the mixture of feedstocks reacts at a temperature of 5 C. to 30 C. over a period of 1 to 24 hours.

7. The process according to claim 2, further comprising: separating a proportion of solids from the product solution, removing the solvent, and obtaining triphenylgermysilane as a crystalline product.

8. The process according to claim 2, wherein a trichlorosilyltriphenylgermane feedstock is obtained from a reaction of Ph.sub.3GeCl with Si.sub.2Cl.sub.6.

9. A method for production of GeSi layers, the method comprising: reacting the compound according to claim 1 to form the GeSi layers.

10. A process for preparing trichlorosilyltrichlorogermane, comprising: dissolving trichlorosilyltriphenylgermane and AlCl.sub.3 (aluminium trichloride) in a solvent to obtain a reaction solution, and condensing hydrogen chloride onto this reaction solution in a stoichiometric amount.

11. The process according to claim 10, wherein hydrogen chloride is used in an amount of 1 to 5 mol hydrogen chloride per mole of the trichlorosilyltriphenylgermane, and/or aluminium trichloride is used in an amount of 0.1 to 3 mol of aluminium trichloride per mole of the trichlorosilyltriphenylgermane.

12. A method for production of GeSi layers, the method comprising: reacting the trichlorosilyltrichlorogermane prepared according to claim 10 to form the GeSi layers.

13.: The process according to claim 5, wherein the molar ratio is 1:1.

14. The process according to claim 7, wherein the solvent is removed under reduced pressure in a range from to 500 hPa.

15. A method, comprising: reacting the triphenylgermylsilane according to claim 1 to transfer SiH.sub.3 groups from a first compound to a second compound.

16. The method according to claim 15, wherein the first compound is a tin compound.

17. The process according to claim 11, wherein hydrogen chloride is used in an amount of 3 mol of hydrogen chloride per mole of trichlorosilyltriphenylgermane, and/or aluminium trichloride is used in an amount of 1 to 2 mol of aluminium trichloride per mole of trichlorosilyltriphenylgermane.

Description

EXAMPLE A: PREPARATION OF SILYLTRIPHENYLGERMANE (2)

[0032] First of all, a synthesis was effected according to Equation 1 from Ph.sub.3GeCl and Si.sub.3Cl.sub.6 with addition of a catalytic amount of 0.1 eq. of [nBu.sub.4N]Cl.

##STR00001##

[0033] To a clear, colourless solution of 500 mg, corresponding to 1.47 mmol, of Ph.sub.3GeCl and 40 mg or 0.14 mmol of [nBu.sub.4N]Cl in 5 ml of CH.sub.2Cl.sub.2 were added while stirring at room temperature 400 mg, corresponding to 1.49 mmol, of Si.sub.2Cl.sub.6. A clear colourless reaction solution was obtained which was stirred at room temperature over the course of 12 h. After gradual removal of the solvent, it was possible to isolate 1 from the reaction solution as crude product in the form of a colourless crystalline solid Ph.sub.3GeSiCl.sub.3 (1). The yield was 59%. The crude product still comprised up to about 30% of the reactant Ph.sub.3GeCl. By x-ray diffractometry, it was possible to determine the crystal structure of 1, shown in FIG. 1a.

[0034] The .sup.29Si NMR spectrum of 1 is shown in FIG. 1b.

[0035] All results of a .sup.1H, .sup.13C and .sup.29Si NMR spectroscopy analysis:

[0036] .sup.29Si NMR (99.4 MHz, CD.sub.2Cl.sub.2, 298 K):

[0037] =13.3.

[0038] .sup.1H NMR (500.2 MHz, CD.sub.2Cl.sub.2, 298 K):

[0039] =7.58 (m); 7.75 (dd.sup.3J(H, H)=8.0 Hz, .sup.2J(H, H)=1.4 Hz).

[0040] .sup.13C NMR (125.0 MHz, CD.sub.2Cl.sub.2, 298 K):

[0041] =128.9; 130.1; 132.2; 135.3.

[0042] Subsequently, the Ph.sub.3GeSiCl.sub.3 (I) obtained was reacted according to Equation 2 with LiAlH.sub.4 in diethyl ether.

##STR00002##

[0043] To a suspension of 9 mg LiAlH.sub.4, corresponding to 0.2 mmol, in Et.sub.2O was added, at room temperature, a clear, colourless solution of 1 in an amount of 100 mg or 0.2 mmol in Et.sub.2O. This reaction solution was stirred at room temperature for 12 h.

[0044] After removal of the residual LiAlH.sub.4 by filtration and gradual removal of the solvent, it was possible to isolate Ph.sub.3GeSiH.sub.3 (2) from the reaction solution as a colourless, crystalline solid in a yield of 76%.

[0045] By x-ray diffractometry, it was possible to determine the crystal structure of 2, shown in FIG. 2a.

[0046] The .sup.29Si NMR spectrum of 2 is shown in FIG. 2b, with the ordinate in relative units. All results of a .sup.1H, .sup.13C and .sup.29Si NMR spectroscopy analysis:

[0047] .sup.29Si NMR (99.4 MHz; c Et.sub.2O; 298 K):

[0048] =q 96.5 .sup.1J(.sup.1H, .sup.29Si)=197 Hz.

[0049] .sup.1H NMR (500.2 MHz; undeuterated Et.sub.2O; 298 K):

[0050] =s 4.3 (only 1 .sup.29Si satellite with coupling constant 98 Hz is apparent. The other is under the Et.sub.2O signal); m 8.1; m 8.2.

[0051] .sup.13C NMR (125.0 MHz; undeuterated Et.sub.2O; 298 K):

[0052] =128.9; 129.4; 135.5; 137.2.

EXAMPLE B: PREPARATION OF TRICHLOROSILYLTRICHLOROGERMANE (3)

[0053] The chlorination of Cl.sub.3SiGePh.sub.3 was effected according to Equation 3. This was done by condensing a stoichiometric amount, namely 3 mmol of HCl per mmol of Cl.sub.3SiGePh.sub.3 (2), onto a dichloromethane solution of 2 and AlCl.sub.3.

##STR00003##

[0054] To a clear and colourless solution of 180 mg or 0.41 mmol of 2 in 5 ml of CH.sub.2Cl.sub.2 were added while stirring at room temperature 100 mg or 0.75 mmol of AlCl.sub.3, whereupon the reaction solution turned an intense red. This red reaction solution was cooled with liquid nitrogen to 196.15 C. and then 44.846 g, corresponding to 30.75 ml or 1.23 mmol, of gaseous hydrogen chloride were condensed in.

[0055] After 10 minutes, the cooling was removed and the reaction mixture was warmed to room temperature.

[0056] A .sup.29Si NMR spectroscopy analysis of the reaction solution showed the NMR signal of 3 at a chemical shift of 6.3 ppm, shown in FIG. 3a.

[0057] All results of a .sup.29Si NMR spectroscopy analysis:

[0058] .sup.29Si NMR (99.4 MHz; CH.sub.2C.sub.12; 298 K):

[0059] =6.3.