Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Low-molecular carbon-free polysilazane and liquid-phase synthesis method thereof

A carbon polysilazane, liquid phase synthesis technology, applied in silicon compounds, chemical instruments and methods, nitrogen and non-metallic compounds, etc., can solve problems such as adverse effects on electrical properties of materials, and achieve low price and good controllability. , the effect of high purity

Inactive Publication Date: 2011-09-07
NAT UNIV OF DEFENSE TECH
View PDF1 Cites 20 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, as the precursor of silicon nitride ceramics, the structure of polysilazane often contains a certain number of alkyl groups, which will have an adverse effect on the electrical properties of the material.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Low-molecular carbon-free polysilazane and liquid-phase synthesis method thereof
  • Low-molecular carbon-free polysilazane and liquid-phase synthesis method thereof
  • Low-molecular carbon-free polysilazane and liquid-phase synthesis method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Check the airtightness of the synthesis device, fully dry the whole device, evacuate, fill the container 5 with nitrogen through the inert gas branch pipe 6, and repeat the process three times to replace the air in the container 5;

[0030] (2) Add tetrahydrofuran and trichlorosilane to container 5 through silicon source raw material inlet pipe 1, wherein tetrahydrofuran is excessive; start agitator 2 to stir, so that trichlorosilane is completely dissolved in tetrahydrofuran;

[0031] (3) Start the condenser 4, pass excess ammonia gas into the container 5 through the nitrogen source raw material inlet pipe 3, heat the container 5 to 60°C through the temperature-controlled water bath 7, and let it stand for 3 hours. After the reaction is completed, protect it in an inert atmosphere Filtration to obtain a clear solution;

[0032] (4) Distill under reduced pressure at room temperature to remove the solvent tetrahydrofuran to obtain a transparent liquid, which is the c...

Embodiment 2

[0035] (1) Same as step (1) of Example 1;

[0036] (2) Add pyridine and dihydrodichlorosilane to container 5, where pyridine is excessive; start stirrer 2 for stirring;

[0037] (3) Start the condenser 4, pass excess ammonia gas into the container, let it stand at room temperature for 6 hours, and the reaction ends; filter under the protection of an inert atmosphere to obtain a clear solution;

[0038] (4) Distill under reduced pressure at normal temperature or under heating conditions to remove the solvent pyridine to obtain a transparent liquid, namely the carbon-free polysilazane of the present invention. The yield is about 70%.

[0039] The dielectric constant of the pyrolysis product of the carbon-free polysilazane synthesized in this example (ie silicon nitride ceramic) is 3.3.

Embodiment 3

[0041] (1) Same as step (1) of Example 1;

[0042] (2) Add triethylene glycol dimethyl ether and monochlorosilane to the container 5, wherein the solvent triethylene glycol dimethyl ether is excessive; start the agitator 2 for stirring;

[0043] (3) Start the condenser 4, pass excess hydrazine into the container 5, heat to 100°C, let it stand for 1 hour, and the reaction ends; filter under the protection of an inert atmosphere to obtain a clear solution;

[0044] (4) Distill under reduced pressure at normal temperature or under heating conditions to remove the solvent pyridine to obtain a transparent liquid, namely the carbon-free polysilazane of the present invention. The yield is about 75%.

[0045] The dielectric constant of the pyrolysis product of the carbon-free polysilazane synthesized in this example (ie silicon nitride ceramic) is 3.6.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a low-molecular carbon-free polysilazane and a liquid-phase synthesis method thereof, and is characterized in that the low-molecular carbon-free polysilazane is liquid state, structurally contains Si-N, Si-H and N-H bonds and does not contains carbon or other foreign elements. The liquid-phase synthesis method comprises the following steps: (1) feeding organic solvents and halogenated silicane in a container which is provided with a raw material feed pipe, a gas pipe, a stirrer and a condenser; (2) introducing an excessive amount of hydronitrogen compounds into the container, standing for 0.5 to 7 hours, filtering in an inert atmosphere to obtain a clear solution; and (3) distilling under reduced pressure at room temperature or under heating to remove the organic solvents, to obtain a transparent solution. The silicon nitride ceramics produced by cracking the low-molecular carbon-free polysilazane are excellent in dielectric properties. The starting compounds for synthesis are easily available and low in price. The synthesis device has a simple structure, is convenient to operate and has good controllability. The synthetic product has a high purity and a high yield.

Description

technical field [0001] The invention relates to a polysilazane and its synthesis method and device, in particular to a low-molecular carbon-free polysilazane and its liquid phase synthesis method and device. Background technique [0002] Silicon nitride (Si 3 N 4 ) is a covalent bond compound, which belongs to the hexagonal crystal system and has two structures: α-crystal form and β-crystal form. The chemical composition and density of the two crystal forms are the same, both are hexagonal. The difference is that the c-axis length of the α-form unit cell is about twice that of the β-form. Silicon nitride is an important non-oxide advanced ceramic material with good comprehensive properties, such as high strength, high hardness, high temperature resistance, thermal shock resistance, self-lubrication, etc. Therefore, silicon nitride is used in high temperature structural materials, High-performance bearing materials and other fields have extremely broad application prospec...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C01B21/082C01B33/00
Inventor 张长瑞李斌曹峰王思青齐共金李俊生刘荣军
Owner NAT UNIV OF DEFENSE TECH
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com