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Light-sensitive Zr-B-Si-C ceramic precursor and in-situ preparation method thereof

A ceramic precursor, zr-b-si-c technology, applied in the field of ceramic materials, can solve the problems of large thermal stress, low polymerization rate, complex process, etc., to prevent premature gelation, solve solid phase agglomeration and viscosity Effect

Active Publication Date: 2019-07-19
XIAMEN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The invention solves the problems of high viscosity, low polymerization rate, large thermal stress, complex process and instability caused by the need to add ceramic powder and dispersant in traditional photocurable precursors, and provides a photosensitive photocurable photopolymer suitable for ultra-high temperature ceramic 3D printing. Sensitive Zr-B-Si-C ceramic precursor and its in-situ synthesis method

Method used

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  • Light-sensitive Zr-B-Si-C ceramic precursor and in-situ preparation method thereof
  • Light-sensitive Zr-B-Si-C ceramic precursor and in-situ preparation method thereof
  • Light-sensitive Zr-B-Si-C ceramic precursor and in-situ preparation method thereof

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preparation example Construction

[0026] The present invention provides a kind of preparation method of photosensitive Zr-B-Si-C ceramic precursor in the first aspect, described method comprises the following steps:

[0027] (1) Methyl vinyl dichlorosilane (C 3 h 6 Cl 2 Si) and borane dimethyl sulfide ((CH 3 ) 2 S·BH 3 ) to mix uniformly to obtain the first mixed solution, and then add metal sodium (Na) to the first mixed solution for dechlorination to obtain methylvinyl borosilane; in the present invention, the toluene solution is, for example, toluene standard solution;

[0028] (2) Chloromethyltrichlorosilane (CH 2 Cl 4 Si), Methylchloromethyldichlorosilane (C 2 h 5 Cl 3 Si) and dichlorozirconocene (C 10 h 10 Cl 2 Zr) mix uniformly to obtain a second mixed solution, then add metal magnesium (Mg) to the second mixed solution to carry out the first heat preservation reaction to obtain a reaction solution, then add a reducing agent to the reaction solution to carry out the second heat preservation...

Embodiment 1

[0056] This embodiment provides a preparation method for in-situ synthesis of a photosensitive Zr-B-Si-C ceramic precursor, the preparation method comprising the following steps:

[0057] S1. Melt 13.4g of trimethylolpropane into 100mL of toluene solvent, add 1g of concentrated sulfuric acid as an acidic catalyst; after heating to boiling, add 31.8g of 3-mercaptopropionic acid, fully react, wash with water until neutral, and then distill under reduced pressure to obtain Mercaptopropionate.

[0058] S2, in N 2 Under the protection of an inert gas, dissolve 21.2g of methylvinyldichlorosilane into 100mL of toluene solution, then add 3.8g of borane dimethyl sulfide to obtain the first mixed solution, and then add 6.9 g of metal Na was dechlorinated, and liquid methylvinyl borosilane was obtained after standing at room temperature, extraction, and filtration.

[0059] S3, in N 2 Under inert gas protection, 18.4g (chloromethyl) trichlorosilane (CH 2 Cl 4 Si), 16.4g (chloromethy...

Embodiment 2

[0064] Embodiment 2 is basically the same as Embodiment 1, the difference is:

[0065] In step S5, the amount of benzoin dimethyl ether photoinitiator is 1 mL, that is, the amount of benzoin dimethyl ether is 0.25 wt%.

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Abstract

The invention relates to a light-sensitive Zr-B-Si-C ceramic precursor and an in-situ preparation method thereof. The method comprises the following steps: uniformly mixing methylvinyldichlorosilane and a borane dimethyl sulfide complex, and then adding metal sodium for dechlorination to obtain methylvinyl borosilane; uniformly mixing chloromethyltrichlorosilane, methylchloromethyldichlorosilane and bis(cyclopentadienyl)zirconium dichloride, then adding metal magnesium to carry out a first heat preservation reaction, and then adding a reducing agent to carry out a second heat preservation reaction to obtain polyzirconocarbosilane; uniformly mixing methylvinyl borosilane and polyzirconocarbosilane to obtain vinyl Zr-B-Si-C alkane; and uniformly mixing the vinyl Zr-B-Si-C alkane with mercaptopropionate, and then adding a photoinitiator to initiate a polymerization reaction to prepare the ceramic precursor. The problems of high viscosity, high thermal stress, structural member mechanicalproperty attenuation and the like of a traditional photocuring system are solved, and a high-quality raw material is provided for photocuring 3D printing of an ultrahigh-temperature ceramic structuralmember.

Description

technical field [0001] The invention belongs to the technical field of ceramic materials, and in particular relates to a photosensitive Zr-B-Si-C ceramic precursor and an in-situ preparation method thereof. Background technique [0002] Based on the designability of the chemical composition of the organic polymer precursor, Zr-B-Si-C ceramic materials with specific properties can be customized according to actual application requirements. 2 A new approach to ultra-high temperature ceramic materials. At the same time, with the rapid development of 3D printing technology, this rapid net shape technology can effectively solve the problems of difficult processing of ceramic materials, long preparation cycle, and even the inability to process small and complex structural parts. Based on the particularity of ceramic printing, light curing is the preferred method for ultra-high temperature ceramic 3D printing. It is worth noting that for the precursors suitable for 3D printing of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F299/02C08G77/60C04B35/58C04B35/56
CPCC04B35/56C04B35/5805C04B2235/483C04B2235/486C08F299/02C08G77/60
Inventor 林佳张厚安杨益航黄桂美王金伙
Owner XIAMEN UNIV OF TECH
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