Method for forming dielectric layer and method for manufacturing semiconductor device
A technology of a dielectric layer and an insulating layer, applied in the field of semiconductor devices, can solve the problems of difficulty in manufacturing semiconductor devices, reducing process margins, etc.
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example 1
[0077] Example 1: Preparation of 1-((bicycloheptenyl)diethoxysilyl)-2-(methyldiethoxysilyl)methane
[0078] Step 1. Preparation of 1-(trichlorosilyl)-2-(methyldichlorosilyl)methane
[0079] Acetonitrile (1500 mL) and (chloromethyl)dichloromethylsilane (500 g, 3.06 mol, 1.0 equiv) were added to a flame-dried 5000 mL Schlenk flask and heated to 70°C. Triethylamine (340.37 g, 3.36 mol, 1.1 eq) was added to the reaction solution, and then trichlorosilane (455.61 g, 3.36 mol, 1.1 eq) was slowly added to the flask while maintaining the temperature at 70°C. The reaction solution was stirred at 70°C for 5 hours, filtered, and then treated four times with n-pentane (1500 mL). The resulting solution was depressurized to remove solvent and purified (at 28 °C and 1.01 Torr) to obtain colorless MeCl 2 Si-CH 2 -SiCl 3 Liquid (160.54 g, yield: 20%).
[0080] 1 H-NMR (C 6 D. 6 )δ0.38(3H), 0.69(2H).
[0081] Step 2. Preparation of 1-(bis(dimethylamino)chlorosilyl)-2-(bis(dimethylamino...
example 2
[0094] Example 2: Preparation of 1-((bicycloheptenyl)diethoxysilyl)-2-(methyldiethoxysilyl)ethane
[0095] Step 1. Preparation of 1-(trichlorosilyl)-2-(methyldichlorosilyl)ethane
[0096] Trichlorovinylsilane (200g, 1.24mol, 1.0 equivalent) and chloroplatinic acid (H 2 Cl 6 Pt 6H 2 O) Added to a flame-dried 3000 mL Schlenk flask, and then heated the reaction solution to 60°C. Dichloromethylsilane (156.7 g, 1.36 mol, 1.1 equiv) was slowly added to the reaction solution. The mixed solution was refluxed for 8 hours to obtain MeCl 2 Si-CH 2 CH 2 -SiCl 3 (384.81 g, yield: 98%).
[0097] 1 H-NMR (C 6 D. 6 )δ0.21(3H), 0.86(2H), 1.06(2H).
[0098] Step 2. Preparation of 1-(bis(dimethylamino)chlorosilyl)-2-(bis(dimethylamino)methylsilyl)ethane
[0099] 1-(trichlorosilyl)-2-(methyldichlorosilyl)ethane (384.81g, 1.39mol, 1.0 equivalent) prepared in step 1 and n-pentane (3000mL) were added to the flame-dried 5000 mL Schlenk flask, and dimethylamine (501.87 g, 11.13 mol, 8.0 ...
example 3
[0111] Example 3: Preparation of 1-(phenylethoxymethylsilyl)-2-(methyldiethoxysilyl)ethane
[0112] Step 1. Preparation of Diethylaminomethylphenylchlorosilane
[0113] Pentane (1500 mL) and dichloromethylphenylsilane (150 g, 0.79 mol, 1.0 equiv) were added to a flame-dried 5000 mL Schlenk flask, and diethylamine (114.8 g, 1.57 mol, 2.0 equivalents), while maintaining the temperature at 0°C. The reaction solution was warmed to room temperature (20° C.) and stirred for 12 hours. The reaction solution was filtered, the solvent was removed under reduced pressure, and then diethylaminomethylphenylchlorosilane (159.12 g, yield: 89%) was obtained.
[0114] 1 H-NMR (C 6 D. 6 )δ0.5(3H), 0.89(6H), 2.75(4H), 7.16(3H), 7.78(2H).
[0115] Step 2. Preparation of Diethylaminomethylsilane
[0116] LiAlH 4 (7.42 g, 0.2 mol, 0.28 equiv) was added to a flame-dried 3000 mL Schlenk flask, and THF (1500 mL) was added to the flask while maintaining the temperature at -10 °C. The ethylamino...
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