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Compound containing N amidino-silicon and application thereof

A technology of silicon compound and amidine group, which is applied in the field of microelectronic materials, can solve the problems of low volatility, danger, and easy volatility, and achieve the effects of simple and easy processing, reduced synthesis cost, and mild synthesis conditions

Active Publication Date: 2015-02-11
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Patents CN101648964A and CN102282291A disclose aminosilane precursors, and CN1518076A discloses hydrazinosilane precursors. These two types of precursors solve the problem of extremely volatile traditional materials to a certain extent and are convenient for storage. However, due to their own Contains more silicon-hydrogen bonds and is active in nature, so there are still some potential dangers and certain toxicity
Patent US2010 / 0285663A1 mainly introduces aminosilane precursors with hexachlorodisilane as the basic structure. The volatility is relatively low, which is not conducive to the further film-forming application of the precursor, and the synthesis of such substances is relatively complicated

Method used

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  • Compound containing N amidino-silicon and application thereof
  • Compound containing N amidino-silicon and application thereof
  • Compound containing N amidino-silicon and application thereof

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preparation example Construction

[0038] The preparation method of the N-amidino-containing silicon compound of the present invention is carried out according to the reaction of formula (I):

[0039]

[0040] where R 1 from C 1 ~C 10 Alkyl, C 2 ~C 10 Alkenyl, C 2 ~C 10 Alkynyl, C 3 ~C 10 Cycloalkyl, C 6 ~C 17 Aryl, —N(SiMe 3 ) 2 or—N(R 5 R 6 ), where R 2 , R 3 independent from C 1 ~C 10 Alkyl, C 2 ~C 10 Alkenyl, C 2 ~C 10 Alkynyl, C 3 ~C 10 Cycloalkyl, C 6 ~C 17 Aryl, where R 4 , R 5 , R 6 independently selected from hydrogen atom, halogen atom (F, Cl, Br, I), C 1 ~C 10 Alkyl, C 2 ~C 10 Alkenyl, C 2 ~C 10 Alkynyl, C 3 ~C 10 Cycloalkyl, C 6 ~C 17 Aryl, —Si(R 2 R 3 R 4 ), or—N(R 7 R 8 ), where R 5 , R 6 independently selected from hydrogen atom, C 1 ~C 10 Alkyl, C 2 ~C 10 Alkenyl, C 2 ~C 10 Alkynyl, C 3 ~C 10 Cycloalkyl, C 6 ~C 17 Aryl, where R 7 , R 8 independently selected from hydrogen atom, C 1 ~C 10 Alkyl, C 2 ~C 10 Alkenyl, C 2 ~C 10 Alkyny...

Embodiment 1

[0043] Embodiment one: a kind of preparation method that contains N-amidino silicon compound precursor body, comprises the following steps:

[0044] (1) will dissolved in n-hexane solvent, The mass ratio to n-hexane solvent is 1:10, and LiNiPr is added under the condition of stirring at -78°C 2 in ether solution, with LiNiPr 2 The molar ratio is 1:1, LiNiPr 2 The concentration of the diethyl ether solution was 1.0M, and the stirring speed was 800 rpm; after returning to room temperature, the stirring reaction was continued for 0.5 hours to obtain a reaction mixture;

[0045] (2) filter the reaction mixture obtained in step (1), collect the filter residue, obtain lithium salt solid, mix lithium salt solid with normal hexane, the mass ratio of lithium salt solid and normal hexane is 1:10, obtain the normal hexane of lithium salt alkane solution;

[0046] (3) According to lithium salt and SiH at 0°C 2Cl 2 The molar ratio is 2:1, the n-hexane solution of lithium salt is...

Embodiment 2

[0048] Embodiment two: a kind of preparation method that contains N-amidino silicon compound precursor body, comprises the following steps:

[0049] (1) will dissolved in toluene solvent, The mass ratio of toluene solvent is 1:15, and it is added to the n-hexane solution of tert-butyllithium under the condition of keeping stirring at -39°C, The molar ratio to tert-butyllithium is 1:1.1, the concentration of tert-butyllithium in n-hexane solution is 1.5M, and the stirring speed is 1500 rpm; after returning to room temperature, continue to stir and react for 1.5 hours to obtain a reaction mixture;

[0050] (2) filter the reaction mixture obtained in step (1), collect the filter residue, obtain lithium salt solid, mix lithium salt solid with toluene, the mass ratio of lithium salt solid and toluene is 1:20, obtain the toluene solution of lithium salt;

[0051] (3) According to lithium salt and SiF at -78°C 4 The molar ratio is 1:1, the toluene solution of lithium salt is ad...

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Abstract

The invention relates to a compound containing N amidino-silicon. The compound is prepared according to the following methods: (1) dissolving carbodiimide or derivatives thereof into a reaction solvent, adding an alkyl / amido lithium solution, aminopyridine or derivatives thereof and alkyl / amido lithium under the stirring condition of -78 DEG C to 0 DEG C according to the molar ratio of 1 to (1-1.2), restoring to room temperature, and then further stirring and reacting for 0.5-3 hours to obtain a reaction mixture; (2) filtering the reaction mixture obtained in the step (1) to obtain lithium salt solid, and dissolving the lithium salt solid into an organic solvent to obtain a lithium salt solution; (3) dropwise adding a silicon-containing reactant or a solution thereof to the lithium salt solution at -78 DEG C to 0 DEG C according to the molar ratio of lithium salt to silicon-containing reactant being (1-4) to (1-1.1), rising to a certain temperature and reacting for 3-10 hours; (4) filtering the reaction mixture obtained in the step (3), concentrating and crystallizing filtrate, or distilling at reduced pressure to obtain a silicon compound containing an amidine ligand. The compound disclosed by the invention can be applied to production of integrated circuits to prepare films of silicon nitride, carbon-containing silicon nitride and the like.

Description

technical field [0001] The invention relates to a silicon compound with a specific structure that contains N-amidino groups. At the same time, the compound can be used as a precursor of an integrated circuit thin film material, and belongs to the technical field of microelectronic materials. Background technique [0002] With the rapid and benign development of the integrated circuit industry, the requirements of its related industries also have the industry characteristics of high-tech content, high-quality requirements, and high entry barriers. This is for the entire integrated circuit related materials. , is facing new challenges and opportunities. [0003] In many process links of integrated circuits, silicon-containing thin films can be used as electronic components of electronic components such as capacitor films, gate films, barrier films, and gate insulating films, or as components of optical communication equipment such as optical waveguides, optical switches, and o...

Claims

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Application Information

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IPC IPC(8): C07F7/10C07F7/02C23C16/30
Inventor 丁玉强杜立永王大伟许从应
Owner JIANGNAN UNIV
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