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Hyperbranched polyborosiloxane ceramic precursor and preparation method thereof, and preparation method of Si-B-O-C ceramic

A technology of ceramic precursor and hyperbranched polymerization, applied in the field of ceramic materials, can solve the problems of weight loss and reduced mechanical properties, and achieve the effects of crystal enhancement, excellent high temperature oxidation resistance and broad application prospects.

Pending Publication Date: 2022-08-02
NORTHWESTERN POLYTECHNICAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Silicon oxygen carbon (Si-O-C) ceramics have attracted extensive attention due to their good chemical, mechanical and thermal properties, but at temperatures higher than 1300 °C, they will rapidly degrade and rapidly lose weight, resulting in a significant decrease in mechanical properties.

Method used

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  • Hyperbranched polyborosiloxane ceramic precursor and preparation method thereof, and preparation method of Si-B-O-C ceramic
  • Hyperbranched polyborosiloxane ceramic precursor and preparation method thereof, and preparation method of Si-B-O-C ceramic
  • Hyperbranched polyborosiloxane ceramic precursor and preparation method thereof, and preparation method of Si-B-O-C ceramic

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preparation example Construction

[0029] The invention provides a preparation method of a hyperbranched polyborosiloxane ceramic precursor, comprising the following steps:

[0030] Under a protective atmosphere, 1,4-dioxane and boronic acid derivatives are mixed to obtain a solution of boronic acid derivatives;

[0031] Mixing the boronic acid derivative solution with acrylic acid-substituted trialkoxysilane, dialkoxysilane, phenyl-substituted dialkoxysilane and substituted monoalkoxysilane, and carrying out a polymerization reaction to obtain Hyperbranched polyborosiloxane ceramic precursor.

[0032] In the present invention, under protective atmosphere, 1,4-dioxane and boronic acid derivatives are mixed to obtain a solution of boronic acid derivatives. In the present invention, the boronic acid derivative preferably includes boric acid, aryl boronic acid or alkyl boronic acid; the aryl boronic acid is preferably phenyl boronic acid; the alkyl boronic acid is preferably methyl boronic acid or ethyl boronic a...

Embodiment 1

[0058] (1) Synthesis of UV-curable hyperbranched polyborosiloxane ceramic precursor (UV-curable hyperbranched polyborosiloxane, UV-HB-PBS)

[0059] The entire process uses Schlenk technology. The Schlenk bottle was subjected to three cycles of water and oxygen removal using the double-row tube technology. Under an argon atmosphere, 200 mL of ultra-dry 1,4-dioxane and 22.15 g of methylboronic acid were added to the Schlenk bottle, and stirred at room temperature. , to obtain methylboronic acid solution; use a syringe to sequentially add 0.075mol 3-(methacryloyloxy)propyltrimethoxysilane, 0.325mol methylvinyldimethoxysilane, 0.1mol diphenyldimethoxysilane Silane and 0.05mol of methoxytrimethylsilane were added to the methylboronic acid solution, a reflux device was installed, and after 15 minutes of reaction at room temperature, the reaction was heated to 80 °C for 8 hours, and cooled to room temperature naturally; the liquid phase product was decompressed at 55 °C The solvent ...

Embodiment 2

[0072] Synthesis of UV-curable hyperbranched polyborosiloxane ceramic precursor (UV-curable hyperbranched polyborosiloxane, UV-HB-PBS)

[0073] The entire process uses Schlenk technology. The Schlenk bottle was subjected to three cycles of water and oxygen removal using the double-row tube technique. Under an argon atmosphere, 200 mL of ultra-dry 1,4-dioxane and 17.95 g of methylboronic acid were added to the Schlenk bottle and stirred at room temperature. , to obtain methylboronic acid solution; use a syringe to sequentially add 0.15mol 3-(methacryloyloxy)propyltrimethoxysilane, 0.35mol methylvinyldimethoxysilane, 0.10mol diphenyldimethoxysilane Silane and 0.10 mol of methoxytrimethylsilane were added to the methylboronic acid solution, and a reflux device was installed. After 15 minutes of reaction at room temperature, the reaction was heated to 80 °C for 8 hours, and cooled to room temperature naturally; the liquid phase product was decompressed at 55 °C The solvent and un...

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Abstract

The invention provides a hyperbranched polyborosiloxane ceramic precursor for photocuring 3D printing, a preparation method of the hyperbranched polyborosiloxane ceramic precursor and a preparation method of Si-B-O-C ceramic, and relates to the technical field of ceramic materials. The preparation method of the hyperbranched polyborosiloxane ceramic precursor provided by the invention comprises the following steps: mixing 1, 4-dioxane and a boric acid derivative in a protective atmosphere to obtain a boric acid derivative solution; and mixing the boric acid derivative solution with trialkoxysilane containing acrylic acid substitution, dialkoxysilane, phenyl substituted dialkoxysilane and monoalkoxysilane containing a substituent group, and carrying out a polymerization reaction to obtain the hyperbranched polyborosiloxane ceramic precursor. The decomposition temperature of the ceramic prepared from the hyperbranched polyborosiloxane ceramic precursor is at least increased to 1400 DEG C, and the ceramic has excellent high-temperature oxidation resistance.

Description

technical field [0001] The invention relates to the technical field of ceramic materials, in particular to a hyperbranched polyborosiloxane ceramic precursor for photocuring 3D printing, a preparation method thereof, and a preparation method of Si-B-O-C ceramics. Background technique [0002] As special ceramics play an increasingly important role in various high-end fields, the demand for high-performance micro-nano ceramics is growing. The functionalization of ceramic devices depends on the micro-macro and multi-level orderly regulation of physical structure and the reorganization of multi-component molecular structure in chemical materials. However, due to the limitations of traditional ceramic preparation technology and the "hard and brittle" characteristics of ceramic materials, industrial The ceramic products used often only have a simple three-dimensional shape, and it is impossible to obtain high-performance ceramic devices with complex micro-nano structures by tradi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/22C08G77/06C04B35/563C04B35/571C04B35/622
CPCC08G77/22C08G77/06C04B35/5603C04B35/571C04B35/563C04B35/622C04B2235/9684
Inventor 孔杰周睿张禧澄于震孙语瑶宋燕
Owner NORTHWESTERN POLYTECHNICAL UNIV
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