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Novel trisilyl amine derivative, method for preparing the same and silicon-containing thin film using the same

一种三甲硅烷基胺、衍生物的技术，应用在化学仪器和方法、半导体/固态器件制造、周期表第4/14族元素的化合物等方向，达到优良内聚性、高反应性、高纯度物理和电学特性的效果

Active Publication Date: 2018-11-13
DNF
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] However, in accordance with device miniaturization resulting from ultrahigh integration of devices, increase in aspect ratio, and diversification of device materials, techniques for forming ultrafine thin films with uniform and thin thickness and excellent electrical characteristics at desired low temperatures are required, And therefore, when using existing silicon precursors, a high temperature process of 600 or more, deterioration of step coverage, etching characteristics, and physical and electrical properties of thin films become problems, and therefore, development of excellent new silicon precursors is required

Method used

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  • Novel trisilyl amine derivative, method for preparing the same and silicon-containing thin film using the same
  • Novel trisilyl amine derivative, method for preparing the same and silicon-containing thin film using the same
  • Novel trisilyl amine derivative, method for preparing the same and silicon-containing thin film using the same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] [Example 1] Synthesis of Tetramethyldisilazane

[0076] 80g (0.84mol) chlorodimethylsilane (CH 3 ) 2 SiHCl and 400 ml of n-hexane were placed in a 1000 ml flame-dried Schlenk flask and stirred under anhydrous and inert atmosphere and cooled to a temperature of -30°C. Add 72g (4.23mol) of ammonia (NH 3 ) while maintaining the temperature at -30°C. After the addition was complete, the temperature of the reaction solution was slowly raised to room temperature, and the reaction solution was stirred at room temperature for 6 hours. After filtering the reaction solution, the white ammonium salt (NH 4 Cl) solid to obtain a filtrate, and the solvent in the filtrate was removed under reduced pressure to obtain 50.73 g (0.38 mol) of tetramethyldisilazane (((CH 3 ) 2 SiH) 2 NH), the yield was 90%.

[0077] 1 HNMR (C 6 D. 6 Middle): δ0.09(d, 12H, HN(HSi(CH 3 ) 2 )) 2 , 4.66(m, 2H, HN(HSi(CH 3 ) 2 )) 2 );

[0078] Boiling point 99°C

Embodiment 2

[0079] [Example 2] Synthesis of two-tetramethylsilyl dichlorosilylamine

[0080] With 40g (0.30mol) tetramethyldisilazane (((CH 3 ) 2 SiH) 2 NH) and 100ml of organic solvent (n-hexane) were put into a 2000ml flame-dried flask and stirred under anhydrous and inert atmosphere, and slowly added 92.85g (0.30mol) of 2.29M n-butyllithium (n-C 4 h 9 Li) Hexane (C 6 h 14 ) solution while maintaining the temperature at -15°C. After the addition was complete, the temperature of the reaction solution was slowly raised to room temperature, and the reaction solution was stirred for 6 hours, and 150 ml of tetrahydrofuran (O(C 2 h 2 ) 2 ). Slowly add 4.47g (0.33mol) trichlorosilane (SiHCl 3 ) while maintaining the temperature at -20°C. After the addition was complete, the temperature of the reaction solution was slowly raised to 25°C, and the reaction solution was stirred for 8 hours while maintaining the temperature at 25°C. After the reaction was completed, the reaction mixture...

Embodiment 3

[0082] [Example 3] Synthesis of two-dimethylsilylsilylamine

[0083] With 55.7g (0.24mol) two-tetramethylsilyl dichlorosilylamine (((CH 3 ) 2 HSi) 2 NSiHCl 2 ) and 200 ml of organic solvent (THF) were placed in a 2000 ml flame-dried flask and stirred under anhydrous and inert atmosphere, and cooled to a temperature of -15°C. 4.77 g (0.60 mol) of lithium hydride (LiH) was slowly added thereto while maintaining the temperature at -15°C. After the addition was complete, the temperature of the reaction solution was slowly raised to 65° C. and the reaction solution was stirred for 12 hours. After filtering the reaction solution, a white solid obtained by filtering was removed to obtain a filtrate. The solvent in the filtrate was removed under reduced pressure by distillation under reduced pressure to obtain 25.50 g (0.16 mol) of bis-dimethylsilylsilylamine (((CH 3 ) 2 HSi) 2 NSiH 3 ), the yield is 65%.

[0084] 1 H-NMR (C 6 D.6 Middle): δ0.16(d, 12H, (((CH 3 ) 2 HSi) ...

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Abstract

Provided is a novel trisilyl amine derivative, wherein the trisilyl amine derivative, which is a compound having thermal stability, high volatility, and high reactivity and being present in a liquid state at room temperature and under pressure where handling is possible, may form a high purity siliconcontaining thin film having excellent physical and electrical properties by various deposition methods.

Description

[0001] This application is a divisional application of a Chinese invention patent application titled "New Trisilylamine Derivatives, Preparation Method and Silicon-Containing Thin Film Using It", filed on January 8, 2015, and with application number 201580009063.6. Application 201580009063.6 is a national application for entering the Chinese national phase of the international application PCT / KR2015 / 000168 filed under the Patent Cooperation Treaty. technical field [0002] The present invention relates to novel trisilylamine derivatives, methods for their preparation and silicon-containing thin films using them, and more particularly to thermally stable and highly volatile liquids at room temperature and pressure (which can undergo Novel trisilylamine derivatives, methods for preparing them, and silicon-containing films using them. Background technique [0003] Through a variety of deposition methods in the semiconductor field, silicon-containing thin films are made into var...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/10C07F7/12
CPCC07F7/10C23C16/402C23C16/45536C23C16/45553H01L21/02164H01L21/0217H01L21/02219H01L21/02274H01L21/0228C07F7/081C07F7/0825
Inventor 张世珍李相道金宗炫金成基金度延杨炳日昔壮衒李相益金铭云
Owner DNF
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