A kind of photocurable polysilazane and preparation method thereof, SICN ceramics and preparation method thereof

A technology of polysilazane and light curing, which is applied in the field of ceramic materials and can solve the problem of high cost

Active Publication Date: 2022-02-15
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, there are very few polysilazanes that can be used for 3D printing at present, and photocurable polysilazanes can only be obtained by introducing photocurable functional groups through isocyanate modification, which is costly

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 1. Preparation of photocurable polysilazane

[0040] (1) Dissolve 50g of methacrylate-3-(trimethyloxysilyl)propyl ester (TMSPM) and 0.25g of tetrabutylammonium fluoride (TBAF) in 50g of tetrahydrofuran solvent, add HCl solution (1 %molHCl and 2.4%mol water, adjust the pH value to 3 relative to TMSPM, and stir at 40°C for 0.5h to obtain the first mixed solution;

[0041] (2) Dissolve 80g of polysilazane HTA1500 SC in 80g of tetrahydrofuran and place it in a three-necked flask protected by argon for 0.5h to prepare the second mixed solution; Drop into the second mixed solution at the speed of / second and stir simultaneously, after the first stirring reaction for 1.5h, the third mixed solution is obtained;

[0042](3) Add 0.3 g of bis(tetrahydrofuran) calcium borohydride to the third mixed solution, carry out the second stirring reaction for 0.5 h, then place the reacted mixture in a centrifuge to separate the solid from the solution, and the separated solution The tetr...

Embodiment 2

[0046] 1. Preparation of photocurable polysilazane

[0047] (1) Dissolve 30g of 3-(trimethyloxysilyl)propyl methacrylate (TMSPM) and 0.1g of tetrabutylammonium fluoride (TBAF) in 40g of n-butyl ether solvent, add oxalic acid solution (1% mol oxalic acid and 2.4% mol water, relative to TMSPM) adjust the pH value to 4, stir at 50 ° C for 1 h to obtain the first mixed solution;

[0048] (2) 70g of polysilazane HTT1800 was dissolved in 80g of n-butyl ether and placed in a three-necked flask protected by argon for 0.5h with magnetic stirring to prepare the second mixed solution; The speed of drop / second is dripped in the second mixed solution and stirred simultaneously, after the first stirring reaction 2h, obtain the 3rd mixed solution;

[0049] (3) Add 0.25 g of bis(tetrahydrofuran) calcium borohydride to the third mixed solution, carry out the second stirring reaction for 0.5 h, then place the reacted mixture in a centrifugal device to separate the solid from the solution, and ...

Embodiment 3

[0053] 1. Preparation of photocurable polysilazane

[0054] (1) 35g methacrylic acid-3-(trimethyloxysilyl) propyl ester (TMSPM) and 0.15g tetrabutylammonium fluoride (TBAF) are dissolved in 60g toluene solvent, add glacial acetic acid solution ( 1% mol oxalic acid and 2.4% mol water, adjust the pH value to 4 relative to TMSPM), and stir at 50°C for 2h to obtain the first mixed solution;

[0055] (2) Dissolve 65g of perhydropolysilazane in 65g of toluene and place it in a three-necked flask protected by argon for 1h to prepare the second mixed solution; The second mixed solution was dropped into the second mixed solution at a speed of 2 seconds and stirred at the same time. After the first stirring reaction for 2 hours, the third mixed solution was obtained;

[0056] (3) Add 0.5 g of bis(tetrahydrofuran) calcium borohydride to the third mixed solution, carry out the second stirring reaction for 0.5 h, then place the reacted mixture in a centrifuge to separate the solid from th...

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Abstract

The invention belongs to the technical field of ceramic materials, and in particular relates to a photocurable polysilazane and a preparation method thereof, SiCN ceramics and a preparation method thereof. In the present invention, by using 3-(trimethyloxysilyl)propyl methacrylate as a modifying agent, tetrabutylammonium fluoride, potassium fluoride and / or cesium fluoride are used as catalysts to Silazane is modified to activate the Si-H and N-H bonds of the branch chain under the condition of ensuring the polysilazane main chain is continuous, and then react with the modifier to introduce a photocurable group to obtain a photocurable polysilazane. Curing polysilazane, the photocurable polysilazane of the present invention can be combined with 3D photocuring molding to prepare complex shape embryos, and SiCN ceramics can be prepared after sintering.

Description

technical field [0001] The invention belongs to the technical field of ceramic materials, and in particular relates to a photocurable polysilazane and a preparation method thereof, SiCN ceramics and a preparation method thereof. Background technique [0002] Polysilazane is a cyclic or linear polymer whose main chain is alternately arranged with silicon atoms and nitrogen atoms, and its molecular formula is [R 1 R 2 Si-NR 3 ] n, with excellent physical properties, high temperature pyrolysis can be derived into ceramic materials. Amorphous SiCN ceramics derived from polysilazane have excellent physical and mechanical properties, such as low thermal expansion coefficient, high hardness, excellent creep resistance and oxidation resistance, and its special microstructure makes it have excellent microwave absorption And dielectric properties, are widely used in sensors, invisible materials, etc. [0003] At present, the molding methods of ceramics mainly include dry pressing ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/58C04B35/622B33Y10/00B33Y70/00
CPCC04B35/58C04B35/622B33Y10/00B33Y70/00C04B2235/6026C04B2235/6562C04B2235/6567C04B2235/661
Inventor 伍尚华黎业华聂光临盛鹏飞
Owner GUANGDONG UNIV OF TECH
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