CN108410170A - A kind of ceramic fibre enhancing polyimides electrical insulating property composite material - Google Patents

A kind of ceramic fibre enhancing polyimides electrical insulating property composite material Download PDF

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CN108410170A
CN108410170A CN201810363272.6A CN201810363272A CN108410170A CN 108410170 A CN108410170 A CN 108410170A CN 201810363272 A CN201810363272 A CN 201810363272A CN 108410170 A CN108410170 A CN 108410170A
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ceramic fibre
composite material
polyimides
sericite
insulating property
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郭平
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/02Fibres or whiskers
    • C08K7/04Fibres or whiskers inorganic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • C08K9/06Ingredients treated with organic substances with silicon-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives

Abstract

The invention discloses a kind of ceramic fibres to enhance polyimides electrical insulating property composite material, is related to technology field of ceramic matrix composite material, includes the following steps and be made:(1) nanometer sericite is modified using polyacrylamide, obtains polyacrylamide modified Nano sericite;(2) polyacrylamide modified Nano sericite is distributed in absolute ethyl alcohol, then polyimide powder is distributed in absolute ethyl alcohol, be configured to mixed dispersion liquid;(3) mixed dispersion liquid under ultrasonic field is subjected to high-speed stirred, be then ground again, high temperature drying obtains mixed material;(4) mixed material is mixed with ceramic fibre, is obtained by compression molding;A kind of ceramic fibre provided by the invention enhances polyimides electrical insulating property composite material, can not only significantly improve high temperature resistance, the acid-proof alkaline of material, while also improving its elongation.

Description

A kind of ceramic fibre enhancing polyimides electrical insulating property composite material
Technical field
The invention belongs to technology field of ceramic matrix composite material, and in particular to a kind of ceramic fibre enhancing polyimides electricity is exhausted Edge composite material.
Background technology
Fiber-reinforced polymer material(Fiber-reinforced poly-mers, FRPs)With its excellent comprehensive performance It is had been more and more widely used in modern industry.By development for many years, FRPs takes on basis with Applied research fields Obtained important development, various high-performance FRPs products have been applied to that Aeronautics and Astronautics, machinery, electrician, electronics etc. be military and the people With in high-tech sector.With Modern High-Tech field to the continuous improvement of material performance requirement and global conventional energy resource increasingly Exhausted and environmental protection consciousness raising, an important research direction of FRPs be how by developing low-cost, high-performance with And environmental-friendly new material.As the important component of FRPs, above-mentioned target is realized in developing into for fibrous material Important channel.Traditional fibre reinforced materials, such as asbestos fibre, glass fibre(Glass fiber, GF), carbon fiber (Carbon fiber, CF), organic polymer fiber(Aramid fiber, ultra-high molecular weight polyethylene, polybenzimidazoles, polybenzoxazole Deng)Etc. there is cost, performance or Environmental compatibility, therefore high-performance, low cost, environmental-friendly fiber type in recent years Development had received widespread attention with exploitation.
Polyimides is best one of the high-molecular organic material of comprehensive performance, and temperature is used for a long time up to 400 DEG C in high temperature resistant Range -200~300 DEG C, no sharp melting point are spent, although polyimide material has certain electrical insulation capability, its resistance to height Warm nature can be general, and acid-proof alkaline is poor, and elongation is low.
Ceramic fibre is a kind of fibrous light refractory material, has that light-weight, high temperature resistant, thermal stability be good, thermal conductivity The advantages that low, specific heat is small and mechanical resistant shakes, thus the industries such as machinery, metallurgy, chemical industry, oil, ceramics, glass, electronics all It is widely used.
The mechanicalness of polyimides can be improved to a certain extent using common ceramic alumina fiber enhancing polyimides Energy and high temperature resistance, but still good can not solve the problems, such as that acid-proof alkaline is poor, elongation is low, simultaneously for its electricity Insulation performance also not how many improvement effect.
Invention content
The purpose of the present invention is for existing problem, it is multiple to provide a kind of ceramic fibre enhancing polyimides electrical insulating property Condensation material.
The present invention is achieved by the following technical solutions:
A kind of ceramic fibre enhancing polyimides electrical insulating property composite material, includes the following steps and is made:
(1) nanometer sericite is modified using polyacrylamide, obtains polyacrylamide modified Nano sericite;
(2) polyacrylamide modified Nano sericite is distributed in absolute ethyl alcohol, then polyimide powder is distributed to anhydrous In ethyl alcohol, the silane coupling agent of polyimides quality 0.12% is then added again, is heated to 80 DEG C, is stirred with 1800r/min rotating speeds 2 hours, obtain mixed dispersion liquid;
(3) polyimides and mixed dispersion liquid are pressed into 150-200g:300mL ratios carry out high-speed stirred under ultrasonic field, then It is ground again, high temperature drying is then carried out under atmosphere of inert gases, obtains mixed material;
(4) mixed material and ceramic fibre are pressed 12:1-2 mass ratioes mix, and it is poly- to obtain ceramic fibre enhancing by compression molding Acid imide electrical insulating property composite material.
Further, the step(1)Middle polyacrylamide modified Nano sericite preparation method is:
(1)The silane coupling agent that quality is nanometer sericite 4.0% is diluted with absolute ethyl alcohol, it is 10% to be configured to mass fraction Silane coupler solution;
(2)Nanometer sericite and silane coupler solution are pressed into 100g:The ratio of 250mL mixes, and is heated to 78-85 DEG C, with 1800r/min rotating speeds stir 2 hours, then add the hydrogen peroxide solution that the isometric mass fraction of silane coupler solution is 15%, Continue stirring 4 hours, then add a nanometer polyacrylamide of quality of sericite 3-5%, nanometer sericite matter is added after stirring evenly Amount 0.02% catalyst, after keeping the temperature 15 hours at 80 DEG C, then be filtered, drying to constant weight to get.
Further, the silane coupling agent is KH560.
Further, the catalyst is cumyl peroxide.
Further, the ceramic fibre preparation method is:
(1) borax, cerous nitrate and maleic acid are added separately in suitable quantity of water, it is molten is configured to the borax that mass fraction is 5.5% Liquid, 1.5% cerous nitrate solution and 10% maleic acid solution press 2 successively:1:3 mass ratioes uniformly mix, and obtain mixed solution, The zirconium nitrate of its quality 10% and 2.5% sodium metasilicate are added into mixed solution, is stirred evenly, and are placed 10-15 hours, are obtained preparation Liquid;
(2) it carries out preparation liquid prepared by step (1) to be centrifuged into fibre, being centrifuged into fine process conditions is:It is a diameter of to get rid of wire hole 0.35mm, it is 6500r/min to get rid of a revolution, and it is 50 DEG C to get rid of a temperature within the barrel, relative humidity 55%;Obtain gelatinous fibre;
(3) the gelatinous fibre calcining prepared step (2) carries out ceramic, and ceramming process condition is:It is kept the temperature at 150 DEG C Then 30min is warming up to 720 DEG C with 5 DEG C/min rates again, keep the temperature 1.5h, be further continued for rising to 1350 DEG C with 5 DEG C/min rates, 2h is kept the temperature, then 1250 DEG C are reduced to 1 DEG C/min rates, continues to keep the temperature 8h, then cooled to room temperature, obtains ceramic fibre.
Further, the step(2)Middle polyacrylamide modified Nano sericite is with absolute ethyl alcohol mixed proportion 20g:350mL, the polyimide powder are 5-6 with polyacrylamide modified Nano quality of sericite ratio:1.
Further, the step(2)Described in ultrasonic field frequencies range be 50kHz, power 1200W, high-speed stirred speed For 3000r/min, grinding rate 2500r/min.
Further, the inert gas is nitrogen, and high temperature drying temperature is 200 DEG C.
Further, the die press technology for forming is:Mixed material is added to ceramic fibre in blender and is stirred 45min is to uniform, and then ground 2500 mesh sieve, is added metal die, is warming up to 440 DEG C, with 520MPa pressure precompressed 3 times, Each 8min, then 510 DEG C are warming up to, pressure increases to 550MPa, heat-insulation pressure keeping 1.5h, then cooled to room temperature, release Die sinking obtains ceramic fibre enhancing polyimides electrical insulating property composite material.
The present invention has the following advantages compared with prior art:A kind of ceramic fibre enhancing polyimides electricity provided by the invention Insulating properties composite material, can not only significantly improve high temperature resistance, the acid-proof alkaline of material, while also improve its elongation Rate.For ceramic fibre prepared by the present invention compared to traditional ceramic alumina fiber, comprehensive performance is more superior, especially has Good heat resistance can be used for a long time in the range of -280-1560 DEG C, be not in being greatly lowered for mechanical property Phenomenon has excellent mechanical property and electrical insulation capability, and surface resistivity is with volume resistivity respectively more than 1012Ω with 1015Ω m, for the ceramic fibre prepared through the invention in composite system, ceramic fibre can also play significant increasing Strong body effect, polyimides plays the role of link enhancement body and transmits load, and polyacrylamide modified Nano sericite position Link role is played between ceramic fibre and polyimides, ceramic fibre reinforcement plays the bridge of useful effect in fact, when When composite material is acted on by external load, polyimide-based cognition transfers load to ceramic fibre reinforcement, so that The all day that can play comprehensive mechanical property is formed between ceramic fibre reinforcement and polyimide matrix, to significantly The comprehensive mechanical property for improving composite material, the extensibility of especially composite material is significantly improved;Studies have shown that A plurality of types of organo-functional groups of ceramic fibre Surface Creation prepared by the present invention so that the ceramic fibre and polyimides of preparation Between wellability be significantly improved, the interlaminar fracture toughness of composite material improves 20% or more;The present invention is prepared compound Material enables to form stable network structure between polyimides and polyacrylamide modified Nano sericite, to substantially Degree inhibits polyimide surface active group to be in contact the possibility reacted with external world's group, and then is greatly improved The stability of composite material especially uses under acid or alkali environment for a long time, can effectively resist the erosion of soda acid, avoid general The defect of logical polyimides not acid and alkali-resistance;With the increase of polyacrylamide modified Nano sericite dosage, the drawing of composite material It stretches intensity and bending strength constantly increases, in addition, the flame retardant property of composite material reaches V-0 grades of UL94, and limit oxygen index It is increased slightly as ceramic fibre dosage increases, mixed material presses 12 with ceramic fibre:When 1 mass ratio, reach maximum value;It is multiple Condensation material has excellent high temperature dimensional stability, this is highly beneficial for its application in high-temperature insulation field.
Since polyimides is the non-conductor of heat, causes frictional heat to be gathered in friction surface, make friction surface temperature liter Height, specimen surface layer softens, and is plastically deformed in friction process, causes wear rate to significantly improve, the present invention passes through to receiving Rice sericite be modified, by modified nanometer sericite have higher strength and stiffness, good thermal conductivity and from Greasy property contributes to the conduction of CONTACT WITH FRICTION area heat or distributes, and so that friction zone temperature increasing degree is reduced, while also helping It is shifted to mating plate surface in polyimides, generates thin and continuous uniform transfer membrane, mitigate plow, tearing and other non-stickiness Abrasion makes composite-material abrasive improve.
Specific implementation mode
Embodiment 1
A kind of ceramic fibre enhancing polyimides electrical insulating property composite material, includes the following steps and is made:
(1) nanometer sericite is modified using polyacrylamide, obtains polyacrylamide modified Nano sericite;
(2) polyacrylamide modified Nano sericite is distributed in absolute ethyl alcohol, then polyimide powder is distributed to anhydrous In ethyl alcohol, the silane coupling agent of polyimides quality 0.12% is then added again, is heated to 80 DEG C, is stirred with 1800r/min rotating speeds 2 hours, obtain mixed dispersion liquid;
(3) polyimides and mixed dispersion liquid are pressed into 150g:300mL ratios carry out high-speed stirred under ultrasonic field, then again into Row grinding, high temperature drying is then carried out under atmosphere of inert gases, obtains mixed material;
(4) mixed material and ceramic fibre are pressed 12:1 mass ratio mixes, and obtaining ceramic fibre by compression molding enhances polyamides Imines electrical insulating property composite material.
Further, the step(1)Middle polyacrylamide modified Nano sericite preparation method is:
(1)The silane coupling agent that quality is nanometer sericite 4.0% is diluted with absolute ethyl alcohol, it is 10% to be configured to mass fraction Silane coupler solution;
(2)Nanometer sericite and silane coupler solution are pressed into 100g:The ratio of 250mL mixes, and 78 DEG C is heated to, with 1800r/ Min rotating speeds stir 2 hours, then add the hydrogen peroxide solution that the isometric mass fraction of silane coupler solution is 15%, continue to stir It mixes 4 hours, then adds the polyacrylamide of nanometer quality of sericite 3%, nanometer quality of sericite 0.02% is added after stirring evenly Catalyst, after keeping the temperature 15 hours at 80 DEG C, then be filtered, drying to constant weight to get.
Further, the silane coupling agent is KH560.
Further, the catalyst is cumyl peroxide.
Further, the ceramic fibre preparation method is:
(1) borax, cerous nitrate and maleic acid are added separately in suitable quantity of water, it is molten is configured to the borax that mass fraction is 5.5% Liquid, 1.5% cerous nitrate solution and 10% maleic acid solution press 2 successively:1:3 mass ratioes uniformly mix, and obtain mixed solution, The zirconium nitrate of its quality 10% and 2.5% sodium metasilicate are added into mixed solution, is stirred evenly, and are placed 10 hours, are obtained preparation liquid;
(2) it carries out preparation liquid prepared by step (1) to be centrifuged into fibre, being centrifuged into fine process conditions is:It is a diameter of to get rid of wire hole 0.35mm, it is 6500r/min to get rid of a revolution, and it is 50 DEG C to get rid of a temperature within the barrel, relative humidity 55%;Obtain gelatinous fibre;
(3) the gelatinous fibre calcining prepared step (2) carries out ceramic, and ceramming process condition is:It is kept the temperature at 150 DEG C Then 30min is warming up to 720 DEG C with 5 DEG C/min rates again, keep the temperature 1.5h, be further continued for rising to 1350 DEG C with 5 DEG C/min rates, 2h is kept the temperature, then 1250 DEG C are reduced to 1 DEG C/min rates, continues to keep the temperature 8h, then cooled to room temperature, obtains ceramic fibre.
Further, the step(2)Middle polyacrylamide modified Nano sericite is with absolute ethyl alcohol mixed proportion 20g:350mL, the polyimide powder are 5 with polyacrylamide modified Nano quality of sericite ratio:1.
Further, the step(2)Described in ultrasonic field frequencies range be 50kHz, power 1200W, high-speed stirred speed For 3000r/min, grinding rate 2500r/min.
Further, the inert gas is nitrogen, and high temperature drying temperature is 200 DEG C.
Further, the die press technology for forming is:Mixed material is added to ceramic fibre in blender and is stirred 45min is to uniform, and then ground 2500 mesh sieve, is added metal die, is warming up to 440 DEG C, with 520MPa pressure precompressed 3 times, Each 8min, then 510 DEG C are warming up to, pressure increases to 550MPa, heat-insulation pressure keeping 1.5h, then cooled to room temperature, release Die sinking obtains ceramic fibre enhancing polyimides electrical insulating property composite material.
Embodiment 2
A kind of ceramic fibre enhancing polyimides electrical insulating property composite material, includes the following steps and is made:
(1) nanometer sericite is modified using polyacrylamide, obtains polyacrylamide modified Nano sericite;
(2) polyacrylamide modified Nano sericite is distributed in absolute ethyl alcohol, then polyimide powder is distributed to anhydrous In ethyl alcohol, the silane coupling agent of polyimides quality 0.12% is then added again, is heated to 80 DEG C, is stirred with 1800r/min rotating speeds 2 hours, obtain mixed dispersion liquid;
(3) polyimides and mixed dispersion liquid are pressed into 200g:300mL ratios carry out high-speed stirred under ultrasonic field, then again into Row grinding, high temperature drying is then carried out under atmosphere of inert gases, obtains mixed material;
(4) mixed material and ceramic fibre are pressed 12:2 mass ratioes mix, and obtaining ceramic fibre by compression molding enhances polyamides Imines electrical insulating property composite material.
Further, the step(1)Middle polyacrylamide modified Nano sericite preparation method is:
(1)The silane coupling agent that quality is nanometer sericite 4.0% is diluted with absolute ethyl alcohol, it is 10% to be configured to mass fraction Silane coupler solution;
(2)Nanometer sericite and silane coupler solution are pressed into 100g:The ratio of 250mL mixes, and 85 DEG C is heated to, with 1800r/ Min rotating speeds stir 2 hours, then add the hydrogen peroxide solution that the isometric mass fraction of silane coupler solution is 15%, continue to stir It mixes 4 hours, then adds the polyacrylamide of nanometer quality of sericite 5%, nanometer quality of sericite 0.02% is added after stirring evenly Catalyst, after keeping the temperature 15 hours at 80 DEG C, then be filtered, drying to constant weight to get.
Further, the silane coupling agent is KH560.
Further, the catalyst is cumyl peroxide.
Further, the ceramic fibre preparation method is:
(1) borax, cerous nitrate and maleic acid are added separately in suitable quantity of water, it is molten is configured to the borax that mass fraction is 5.5% Liquid, 1.5% cerous nitrate solution and 10% maleic acid solution press 2 successively:1:3 mass ratioes uniformly mix, and obtain mixed solution, The zirconium nitrate of its quality 10% and 2.5% sodium metasilicate are added into mixed solution, is stirred evenly, and are placed 15 hours, are obtained preparation liquid;
(2) it carries out preparation liquid prepared by step (1) to be centrifuged into fibre, being centrifuged into fine process conditions is:It is a diameter of to get rid of wire hole 0.35mm, it is 6500r/min to get rid of a revolution, and it is 50 DEG C to get rid of a temperature within the barrel, relative humidity 55%;Obtain gelatinous fibre;
(3) the gelatinous fibre calcining prepared step (2) carries out ceramic, and ceramming process condition is:It is kept the temperature at 150 DEG C Then 30min is warming up to 720 DEG C with 5 DEG C/min rates again, keep the temperature 1.5h, be further continued for rising to 1350 DEG C with 5 DEG C/min rates, 2h is kept the temperature, then 1250 DEG C are reduced to 1 DEG C/min rates, continues to keep the temperature 8h, then cooled to room temperature, obtains ceramic fibre.
Further, the step(2)Middle polyacrylamide modified Nano sericite is with absolute ethyl alcohol mixed proportion 20g:350mL, the polyimide powder are 5-6 with polyacrylamide modified Nano quality of sericite ratio:1.
Further, the step(2)Described in ultrasonic field frequencies range be 50kHz, power 1200W, high-speed stirred speed For 3000r/min, grinding rate 2500r/min.
Further, the inert gas is nitrogen, and high temperature drying temperature is 200 DEG C.
Further, the die press technology for forming is:Mixed material is added to ceramic fibre in blender and is stirred 45min is to uniform, and then ground 2500 mesh sieve, is added metal die, is warming up to 440 DEG C, with 520MPa pressure precompressed 3 times, Each 8min, then 510 DEG C are warming up to, pressure increases to 550MPa, heat-insulation pressure keeping 1.5h, then cooled to room temperature, release Die sinking obtains ceramic fibre enhancing polyimides electrical insulating property composite material.
Embodiment 3
A kind of ceramic fibre enhancing polyimides electrical insulating property composite material, includes the following steps and is made:
(1) nanometer sericite is modified using polyacrylamide, obtains polyacrylamide modified Nano sericite;
(2) polyacrylamide modified Nano sericite is distributed in absolute ethyl alcohol, then polyimide powder is distributed to anhydrous In ethyl alcohol, the silane coupling agent of polyimides quality 0.12% is then added again, is heated to 80 DEG C, is stirred with 1800r/min rotating speeds 2 hours, obtain mixed dispersion liquid;
(3) polyimides and mixed dispersion liquid are pressed into 180g:300mL ratios carry out high-speed stirred under ultrasonic field, then again into Row grinding, high temperature drying is then carried out under atmosphere of inert gases, obtains mixed material;
(4) mixed material and ceramic fibre are pressed 12:1.5 mass ratioes mix, and it is poly- to obtain ceramic fibre enhancing by compression molding Acid imide electrical insulating property composite material.
Further, the step(1)Middle polyacrylamide modified Nano sericite preparation method is:
(1)The silane coupling agent that quality is nanometer sericite 4.0% is diluted with absolute ethyl alcohol, it is 10% to be configured to mass fraction Silane coupler solution;
(2)Nanometer sericite and silane coupler solution are pressed into 100g:The ratio of 250mL mixes, and 82 DEG C is heated to, with 1800r/ Min rotating speeds stir 2 hours, then add the hydrogen peroxide solution that the isometric mass fraction of silane coupler solution is 15%, continue to stir It mixes 4 hours, then adds the polyacrylamide of nanometer quality of sericite 4%, nanometer quality of sericite 0.02% is added after stirring evenly Catalyst, after keeping the temperature 15 hours at 80 DEG C, then be filtered, drying to constant weight to get.
Further, the silane coupling agent is KH560.
Further, the catalyst is cumyl peroxide.
Further, the ceramic fibre preparation method is:
(1) borax, cerous nitrate and maleic acid are added separately in suitable quantity of water, it is molten is configured to the borax that mass fraction is 5.5% Liquid, 1.5% cerous nitrate solution and 10% maleic acid solution press 2 successively:1:3 mass ratioes uniformly mix, and obtain mixed solution, The zirconium nitrate of its quality 10% and 2.5% sodium metasilicate are added into mixed solution, is stirred evenly, and are placed 12 hours, are obtained preparation liquid;
(2) it carries out preparation liquid prepared by step (1) to be centrifuged into fibre, being centrifuged into fine process conditions is:It is a diameter of to get rid of wire hole 0.35mm, it is 6500r/min to get rid of a revolution, and it is 50 DEG C to get rid of a temperature within the barrel, relative humidity 55%;Obtain gelatinous fibre;
(3) the gelatinous fibre calcining prepared step (2) carries out ceramic, and ceramming process condition is:It is kept the temperature at 150 DEG C Then 30min is warming up to 720 DEG C with 5 DEG C/min rates again, keep the temperature 1.5h, be further continued for rising to 1350 DEG C with 5 DEG C/min rates, 2h is kept the temperature, then 1250 DEG C are reduced to 1 DEG C/min rates, continues to keep the temperature 8h, then cooled to room temperature, obtains ceramic fibre.
Further, the step(2)Middle polyacrylamide modified Nano sericite is with absolute ethyl alcohol mixed proportion 20g:350mL, the polyimide powder are 5-6 with polyacrylamide modified Nano quality of sericite ratio:1.
Further, the step(2)Described in ultrasonic field frequencies range be 50kHz, power 1200W, high-speed stirred speed For 3000r/min, grinding rate 2500r/min.
Further, the inert gas is nitrogen, and high temperature drying temperature is 200 DEG C.
Further, the die press technology for forming is:Mixed material is added to ceramic fibre in blender and is stirred 45min is to uniform, and then ground 2500 mesh sieve, is added metal die, is warming up to 440 DEG C, with 520MPa pressure precompressed 3 times, Each 8min, then 510 DEG C are warming up to, pressure increases to 550MPa, heat-insulation pressure keeping 1.5h, then cooled to room temperature, release Die sinking obtains ceramic fibre enhancing polyimides electrical insulating property composite material.
Comparative example 1:It is differed only in embodiment 1 and polyacrylamide modified Nano sericite is replaced with into untreated receive Rice sericite.
Comparative example 2:It is differed only in embodiment 1 and does not add ceramic fibre prepared by the present invention.
Comparative example 3:It is differed only in embodiment 1 and ceramic fibre prepared by the present invention is replaced with into basalt fibre.
Comparative example 4:It is differed only in embodiment 1 and ceramic fibre prepared by the present invention is replaced with into commercial alumina ceramics Fiber(Product code SYGX-121).
Experiment
The typical performance of ceramic fibre prepared by the present invention and other types fiber compares;
Table 1
As can be seen from Table 1, the ceramic fibre comprehensive performance that prepared by the present invention has aobvious compared to other types of fibre property The raising of work.
The composite material prepared with comparative example to embodiment using insulation characterisitic tester is detected:
Table 2
Show that embodiment composite material exhibits go out excellent electrical insulation capability by insulation performance test result in table 2, in addition, right Embodiment carries out resistance to y-x ray irradiation x performance test with composite material prepared by comparative example, through 1 × 108After rad dose deliveries, The volume resistivity of embodiment composite material and electrical strength conservation rate reach 97% or more, and the body of 1 composite material of comparative example Product resistivity and electrical strength conservation rate can only keep 92% or so, the volume resistivity of 2 composite material of comparative example with it is electrical strong Degree conservation rate can only keep 73% or so, and the volume resistivity of 3 composite material of comparative example can only be protected with electrical strength conservation rate 89% or so is held, volume resistivity and the electrical strength conservation rate of 4 composite material of comparative example can only keep 85% or so, thus may be used See, composite material prepared by the present invention also has good resistance to y-x ray irradiation x performance.
Abrasion test
Using the tribological property of MRH-3 rings-block friction wear testing machine test compound material, wherein test ring is CrWMn Steel loop is quenched, size is Φ 49mm × 12.7mm, and surface roughness Ra is 0.27 μm, hardness HRC62;Test block is Embodiment and comparative example composite material, the secondary contact form that rubs contact for line.Experimental condition:Load 450N, rotating speed 400r/ min(It is equivalent to sliding speed 1.03m/s)And 600r/min, room temperature, dry friction, test period 10min.Friction coefficient is by trying The machine of testing automatically records, using precision electronic balance(Precision is 0.1mg)Measure embodiment and comparative example worn composite quality Loss, and using the abrasion quality in unit sliding distance as wear rate, test result is 3 average value;
Table 3
Wear rate(10-7g/m)
Embodiment 1 1.356
Embodiment 2 1.328
Embodiment 3 1.335
Comparative example 1 5.893
Control group 14.385
Control group differs only in embodiment 1 and does not add polyacrylamide modified Nano sericite;
As can be seen from Table 3, although unmodified nanometer sericite can improve the wear-resisting property of composite material to a certain extent, But pass through the wear-resisting property that composite material can be greatly improved in the modified nanometer sericite of the present invention.

Claims (9)

1. a kind of ceramic fibre enhances polyimides electrical insulating property composite material, which is characterized in that include the following steps and be made:
(1) nanometer sericite is modified using polyacrylamide, obtains polyacrylamide modified Nano sericite;
(2) polyacrylamide modified Nano sericite is distributed in absolute ethyl alcohol, then polyimide powder is distributed to anhydrous In ethyl alcohol, the silane coupling agent of polyimides quality 0.12% is then added again, is heated to 80 DEG C, is stirred with 1800r/min rotating speeds 2 hours, obtain mixed dispersion liquid;
(3) polyimides and mixed dispersion liquid are pressed into 150-200g:300mL ratios carry out high-speed stirred under ultrasonic field, then It is ground again, high temperature drying is then carried out under atmosphere of inert gases, obtains mixed material;
(4) mixed material and ceramic fibre are pressed 12:1-2 mass ratioes mix, and it is poly- to obtain ceramic fibre enhancing by compression molding Acid imide electrical insulating property composite material.
2. a kind of ceramic fibre according to claim 1 enhances polyimides electrical insulating property composite material, which is characterized in that The step(1)Middle polyacrylamide modified Nano sericite preparation method is:
(1)The silane coupling agent that quality is nanometer sericite 4.0% is diluted with absolute ethyl alcohol, it is 10% to be configured to mass fraction Silane coupler solution;
(2)Nanometer sericite and silane coupler solution are pressed into 100g:The ratio of 250mL mixes, and is heated to 78-85 DEG C, with 1800r/min rotating speeds stir 2 hours, then add the hydrogen peroxide solution that the isometric mass fraction of silane coupler solution is 15%, Continue stirring 4 hours, then add a nanometer polyacrylamide of quality of sericite 3-5%, nanometer sericite matter is added after stirring evenly Amount 0.02% catalyst, after keeping the temperature 15 hours at 80 DEG C, then be filtered, drying to constant weight to get.
3. a kind of ceramic fibre according to claim 2 enhances polyimides electrical insulating property composite material, which is characterized in that The silane coupling agent is KH560.
4. a kind of ceramic fibre according to claim 2 enhances polyimides electrical insulating property composite material, which is characterized in that The catalyst is cumyl peroxide.
5. a kind of ceramic fibre according to claim 1 enhances polyimides electrical insulating property composite material, which is characterized in that The ceramic fibre preparation method is:
(1) borax, cerous nitrate and maleic acid are added separately in suitable quantity of water, it is molten is configured to the borax that mass fraction is 5.5% Liquid, 1.5% cerous nitrate solution and 10% maleic acid solution press 2 successively:1:3 mass ratioes uniformly mix, and obtain mixed solution, The zirconium nitrate of its quality 10% and 2.5% sodium metasilicate are added into mixed solution, is stirred evenly, and are placed 10-15 hours, are obtained preparation Liquid;
(2) it carries out preparation liquid prepared by step (1) to be centrifuged into fibre, being centrifuged into fine process conditions is:It is a diameter of to get rid of wire hole 0.35mm, it is 6500r/min to get rid of a revolution, and it is 50 DEG C to get rid of a temperature within the barrel, relative humidity 55%;Obtain gelatinous fibre;
(3) the gelatinous fibre calcining prepared step (2) carries out ceramic, and ceramming process condition is:It is kept the temperature at 150 DEG C Then 30min is warming up to 720 DEG C with 5 DEG C/min rates again, keep the temperature 1.5h, be further continued for rising to 1350 DEG C with 5 DEG C/min rates, 2h is kept the temperature, then 1250 DEG C are reduced to 1 DEG C/min rates, continues to keep the temperature 8h, then cooled to room temperature, obtains ceramic fibre.
6. a kind of ceramic fibre according to claim 1 enhances polyimides electrical insulating property composite material, which is characterized in that The step(2)Middle polyacrylamide modified Nano sericite is 20g with absolute ethyl alcohol mixed proportion:350mL, the polyamides are sub- Amine powder is 5-6 with polyacrylamide modified Nano quality of sericite ratio:1.
7. a kind of ceramic fibre according to claim 1 enhances polyimides electrical insulating property composite material, which is characterized in that The step(2)Described in ultrasonic field frequencies range be 50kHz, power 1200W, high-speed stirred speed is 3000r/min, grinding speed Degree is 2500r/min.
8. a kind of ceramic fibre according to claim 1 enhances polyimides electrical insulating property composite material, which is characterized in that The inert gas is nitrogen, and high temperature drying temperature is 200 DEG C.
9. a kind of ceramic fibre according to claim 1 enhances polyimides electrical insulating property composite material, which is characterized in that The die press technology for forming is:Mixed material and ceramic fibre are added in blender and stir 45min to uniform, is then ground 2500 mesh sieve is crossed, metal die is added, is warming up to 440 DEG C, with 520MPa pressure precompressed 3 times, each 8min, then is warming up to 510 DEG C, pressure increases to 550MPa, heat-insulation pressure keeping 1.5h, then cooled to room temperature, and release die sinking obtains ceramic fibre enhancing Polyimides electrical insulating property composite material.
CN201810363272.6A 2018-04-21 2018-04-21 A kind of ceramic fibre enhancing polyimides electrical insulating property composite material Pending CN108410170A (en)

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Application publication date: 20180817