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Boride ceramic in-situ filling cyanate ester resin base composite material and preparation method thereof

A resin composite material, filling cyanate ester technology, applied in the field of composite materials, can solve the problems that have not yet been reported, and achieve the effects of excellent performance, uniform structure characteristics and high melting point

Active Publication Date: 2016-10-26
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to previous studies, the inorganic fillers used to fill modified cyanate resins are mainly concentrated in carbon nanotubes, graphene, SiO 2 、TiO 2 And BN, etc., the material preparation mainly adopts the method of physical mechanical blending, but there are few reports on the use of boride ceramics, especially metal boride ceramics, to fill modified cyanate esters, especially through in-situ polymerization. The study of high thermal conductivity metal boride ceramics filled modified cyanate ester resin composites has not been reported so far

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 100g of bisphenol A, 105g of cyanogen bromide and 400ml of acetone solution in a 1000ml three-necked flask, place the three-necked flask in an ice water or ice-salt water bath, and add 6g of zirconium diboride (ZrB 2 ), the temperature should be controlled at 0 °C or below throughout the synthesis process. Add 90 g of triethylamine dropwise from a separatory funnel under stirring at 1200 r / min at a rate of 0.5 drops / s. The dropwise addition is completed in about 3.5 hours, and the stirring is continued for 1 hour to obtain a suspension. Then wash the suspension with distilled water to neutrality, soak the separated amine hydrobromide salt with acetone to filter out the residual cyanate resin and pour it back into the original suspension. The suspension system after separating the ammonium hydrobromide salt is rotary evaporated, and the acetone solvent is removed to obtain zirconium diboride powder filled with cyanate resin in situ, and then add 0.014gZn / nonylphenol ...

Embodiment 2

[0028]Add 50g of bisphenol A, 52.5g of cyanogen bromide and 200ml of acetone solution in a 500ml three-necked flask, place the three-necked flask in an ice water or ice-salt bath, and add 3g of titanium diboride ( TiB 2 ), the temperature should be controlled at 0 °C or below throughout the synthesis process. Add 45 g of triethylamine dropwise from a separatory funnel under stirring at 1000 r / min at a rate of 0.3 drops / s. After about 3.0 hours, the dropwise addition is completed, and the stirring is continued for 1 hour to obtain a suspension. Then wash the suspension with distilled water to neutrality, soak the separated amine hydrobromide salt with acetone to filter out the residual cyanate resin and pour it back into the original suspension. The suspension system after separating the ammonium hydrobromide salt is rotary evaporated, and the acetone solvent is removed to obtain titanium diboride powder filled with cyanate resin in situ, and then add 0.01g of Zn / nonylphenol c...

Embodiment 3

[0030] Add 25g of bisphenol A, 26.25g of cyanogen bromide and 100ml of acetone solution into a 250ml three-necked flask, place the three-necked flask in an ice water or ice-salt water bath, and add 3.05g of zirconium diboride under mechanical stirring at 800r / min (ZrB 2 ), the temperature should be controlled at 0 °C or below throughout the synthesis process. Add 22.5 g of triethylamine dropwise from a separatory funnel under stirring at 900 r / min at a rate of 0.1 drop / s. The dropwise addition is completed in about 3.0 hours, and the stirring is continued for 1 hour to obtain a suspension. Then wash the suspension with distilled water to neutrality, soak the separated amine hydrobromide salt with acetone to filter out the residual cyanate resin and pour it back into the original suspension. The suspension system after separating the ammonium hydrobromide salt is rotary evaporated, and the acetone solvent is removed to obtain zirconium diboride powder filled with cyanate resin...

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Abstract

The invention belongs to the technical field of an advanced composite material science, and particularly relates to a boride ceramic in-situ filling cyanate ester resin base composite material and a preparation method thereof. By an in-situ polymerization method, firstly, bisphenol A is dissolved in a benzene or alkane type organic solvent; a certain amount of cyanogen halide is added; mechanical stirring is performed in an environment being -10 to 0 DEG C to obtain a mixed solution; under the strong stirring, metal boride ceramic powder is added into the mixed solution; the stirring is continuously performed; at -10 to 0 DEG C, triethylamine is dropwise added into the system; the system takes polymerization; after the organic solvent is removed through distillation, metal boride powder in-situ filling cyanate ester resin is obtaine; then, a catalyst is added for stirring; after vacuum degassing treatment, curing formation is performed at a high temperature. The prepared metal boride in-situ filling cyanate ester resin base composite material has the structure performance characteristics of uniform material tissue, heat resistance and excellent heat conduction performance, and can be used as a base board material, an encapsulating material and the like of a printed circuit board in electronic equipment for space navigation industry and aerospace industry.

Description

technical field [0001] The invention belongs to the technical field of composite materials, and in particular relates to a boride ceramic in-situ filled cyanate resin-based composite material and a preparation method thereof. Background technique [0002] With the development of high power, high integration and miniaturization of modern microelectronic components, the timely heat dissipation and stability of substrate materials and packaging materials in industrial application electronic equipment are very important. Cyanate Ester (CE) resin is an important high-performance thermosetting resin, due to its comprehensive properties such as good heat resistance, low dielectric constant and dielectric loss, and good weather resistance, it is used in high Advanced technology fields such as high-performance printed circuit boards, aerospace structural components, stealth materials, radar radomes and artificial satellites have broad application prospects. After the cyanate ester m...

Claims

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Application Information

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IPC IPC(8): C08L79/04C08K3/38C08G73/06
CPCC08G73/0644C08G73/065C08K3/38C08K2201/003C08L79/04
Inventor 于志强何延楠
Owner FUDAN UNIV
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