CN106587937A - High-strength carbon fiber based composite ceramic material and preparation method thereof - Google Patents

High-strength carbon fiber based composite ceramic material and preparation method thereof Download PDF

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CN106587937A
CN106587937A CN201611112533.4A CN201611112533A CN106587937A CN 106587937 A CN106587937 A CN 106587937A CN 201611112533 A CN201611112533 A CN 201611112533A CN 106587937 A CN106587937 A CN 106587937A
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parts
carbon fiber
ceramic material
based composite
composite ceramic
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马志明
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Suzhou Luotelan New Material Technology Co Ltd
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Suzhou Luotelan New Material Technology Co Ltd
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Abstract

The invention discloses a high-strength carbon fiber based composite ceramic material and a preparation method thereof. The high-strength carbon fiber based composite ceramic material is prepared from the following raw materials in parts by weight: 30-40 parts of ceramic powder, 5-8 parts of hydroxyapatite, 5-8 parts of celsian, 5-6 parts of lepidolite, 12-15 parts of cellulose acetate fiber, 2-5 parts of polyurethane, 2-3 parts of tert-butyl hydroperoxide, 3-6 parts of trimethoxy silane, 1-4 parts of methylsilanetriyl triacetate, 4-7 parts of sodium lignin sulfonate, 2-5 parts of hydroxy propyl acrylate, 1-4 parts of polyethylene glycol, 4-8 parts of sodium laurylsulfonate, 1-2 parts of aluminum nitride, 1-4 parts of ammonium chloride, 2-5 parts of ferric oxide, 2-6 parts of cuprous oxide, 2-5 parts of sodium silicate, 1-2 parts of sodium tripolyphosphate, 1-4 parts of an antioxidant, 2-5 parts of a stabilizer and 1-2 parts of a coupling agent. The prepared high-strength carbon fiber based composite ceramic material is stable in property, high in strength, not liable to deform, good in high temperature resistance and good in heat conduction property. Meanwhile the invention further discloses a corresponding preparation method.

Description

A kind of high-strength carbon fiber based composite ceramic material and preparation method thereof
Technical field
The present invention relates to Material Field, is related specifically to a kind of high-strength carbon fiber based composite ceramic material and its preparation side Method.
Background technology
Ceramic material is through shaping and a class inorganic non-metallic material made by high temperature sintering with naturally occurring or synthetic compound Material.It has the advantages that high-melting-point, high rigidity, high-wearing feature, resistance to oxidation.Can be used as structural material, cutter material, due to ceramics Also there are some special performances, but also as functional material.Ceramic material has its unique superiority in performance, heat and Mechanical properties, there is high temperature resistant, heat-insulated, high rigidity, abrasion performance etc.；There are insulating properties, piezoelectricity, quasiconductor in terms of electrical property Property, magnetic etc.；There is the function such as catalysis, corrosion-resistant, absorption in terms of chemistry；In terms of biology, with certain bio-compatible performance, Can be used as biological structure material etc..But meanwhile, ceramic material also has the shortcomings that it.So the present invention strengthens pottery using carbon fiber Some performances of ceramic material, such as intensity, hardness, heat conduction, high temperature resistant, are property of the ceramic material with some property being composited Can, widen its scope of application.
The content of the invention
To solve above-mentioned technical problem, the present invention provides a kind of high-strength carbon fiber based composite ceramic material and its preparation side Method, by being combined using specified raw material, coordinates corresponding production technology, the high-strength carbon fiber base composite ceramic material for obtaining Material, its stable performance, intensity is big, be unlikely to deform, high temperature resistant and good heat conductivity, the requirement of industry is disclosure satisfy that, with preferable Application prospect.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of high-strength carbon fiber based composite ceramic material, is prepared by the raw materials in：Ceramics 30-40 parts, hydroxyl Apatite 5-8 parts, baryta fledspar 5-8 parts, lepidolite 5-6 parts, acetate fiber 12-15 parts, polyurethane 2-5 parts, tert-butyl hydroperoxide Hydrogen 2-3 parts, trimethoxy silane 3-6 parts, methyl triacetoxysilane 1-4 parts, sodium lignin sulfonate 4-7 parts, acrylic acid hydroxyl Propyl ester 2-5 parts, Polyethylene Glycol 1-4 parts, lauryl amine base sodium sulfonate 4-8 parts, aluminium nitride 1-2 parts, ammonium chloride 1-4 parts, ferrum oxide 2-5 Part, Red copper oxide 2-6 parts, sodium silicate 2-5 parts, sodium tripolyphosphate 1-2 parts, antioxidant 1-4 parts, stabilizer 2-5 parts, coupling Agent 1-2 parts.
Preferably, the antioxidant is 2,2'- methylene bis (4- methyl -6- tert-butyl phenols), 4- hydroxy-dodecanoic acids One or more in anilid, the t-octyl diphenylamines of 4,4'- bis-, 4- hydroxyoctadecanoic acid anilids.
Preferably, the stabilizer is any one in 2- ethyl acetic acid lead, calcium ricinoleate, zinc stearate, Osmanthus tragranscv.Aurantiacu acid barium Kind.
Preferably, the coupling agent is selected from three iso stearate isopropyl titanates, isopropyl three（Dioctyl pyrophosphoryl base) titanium Acid esters, two (dioctyl pyrophosphoryl bases) close any in fluoroacetic acid ester titanium, isopropyl three (positive ethylamino-ethylamino) titanate esters One or more.
The preparation method of described high-strength carbon fiber based composite ceramic material, comprises the following steps：
（1）Each raw material is weighed according to weight portion；
（2）Ceramics, hydroxyapatite, baryta fledspar, lepidolite are added and is ground in raymond mill, pulverizing acc power is 22KW, mixture granularity is 200-300 mesh;
（3）By acetate fiber, polyurethane, tert-butyl hydroperoxide, trimethoxy silane, methyl triacetoxysilane, nitridation Aluminum, ammonium chloride, ferrum oxide, Red copper oxide, antioxidant, step（2）Mixture of powders add together hot test electric furnace burn Knot, by the high temperature sintering thing water quenching for obtaining, cooling obtains ceramic block, and high temperature sintering temperature is 450-500 DEG C, the high temperature sintering time For 10-25 minutes；
（4）By step（3）Ceramic block, sodium lignin sulfonate, Hydroxypropyl acrylate, Polyethylene Glycol, lauryl amine base sodium sulfonate one Rise and add ball mill, pellet ratio is 1：8, Ball-milling Time is 4 hours；
（5）By step（4）Ball milling powder mince sorting of sieving, collection is sieved mixture；
（6）By step（5）The mixture that sieves, sodium silicate, sodium tripolyphosphate, stabilizer, coupling agent injection high pressure homogenizer in Stir, 1000-1500 rev/min of rotating speed, pressure is 0.5-1MPa, mix 15-30 minutes；
（7）By step（6）Stirring mixture injection mould in it is compressing, gained idiosome is solid in 4-10 DEG C of nitrogen couveuse Calmly, degumming 30 minutes；
（8）By step（7）Idiosome be put in vacuum high-temperature calcining furnace and be sintered molding, calcining heat is 780-860 DEG C, very Pneumatics is by force 0.2-0.5Pa, and the vacuum-sintering time is 60-90 minutes；
（9）By step（8）Calcining model be slowly dropped to after room temperature, mould from, dewax, be put in 60 DEG C of nitrogen couveuses and conserve 2- 4 hours, get product.
Preferably, the condition of the water quenching is：Enter coolant-temperature gage for 10-15 DEG C, the water quenching time is 45 seconds.
Preferably, the mesh size is 200 mesh.
Compared with prior art, its advantage is the present invention：
（1）The present invention high-strength carbon fiber based composite ceramic material, with ceramics, hydroxyapatite, baryta fledspar, lepidolite, Acetate fiber, polyurethane, tert-butyl hydroperoxide, trimethoxy silane, methyl triacetoxysilane, aluminium nitride, ammonium chloride, Ferrum oxide, Red copper oxide are main component, by adding sodium lignin sulfonate, Hydroxypropyl acrylate, Polyethylene Glycol, lauryl amine base Sodium sulfonate, sodium silicate, sodium tripolyphosphate, antioxidant, stabilizer, coupling agent, are aided with mechanical activation comminution, high temperature sintering, at water quenching The technique such as reason, ball milling sorting, the homogeneous, mold that pressurizes is fixed, vacuum calcining, mould from dewax, maintenance molding so that be prepared from High-strength carbon fiber based composite ceramic material, its stable performance, intensity is big, be unlikely to deform, high temperature resistant and good heat conductivity, can The requirement of industry is met, with preferable application prospect.
（2）The high-strength carbon fiber based composite ceramic material raw material of the present invention is cheap, process is simple, is suitable to large-scale industry Change and use, it is practical.
Specific embodiment
The technical scheme invented is described in detail with reference to specific embodiment.
Embodiment 1
（1）30 parts of ceramics, 5 parts of hydroxyapatite, 5 parts of baryta fledspar, 5 parts of lepidolite, acetate fiber 12 are weighed according to weight portion Part, 2 parts of polyurethane, 2 parts of tert-butyl hydroperoxide, 3 parts of trimethoxy silane, 1 part of methyl triacetoxysilane, sulfomethylated lignin 4 parts of sour sodium, 2 parts of Hydroxypropyl acrylate, 1 part of Polyethylene Glycol, 4 parts of lauryl amine base sodium sulfonate, 1 part of aluminium nitride, 1 part of ammonium chloride, oxygen Change 2 parts of ferrum, 2 parts of Red copper oxide, 2 parts of sodium silicate, 1 part of sodium tripolyphosphate, 2,2'- methylene bis (4- methyl -6- tert-butyl phenols) 1 part, 2 parts of 2- ethyl acetic acids lead, 1 part of three iso stearate isopropyl titanate；
（2）Ceramics, hydroxyapatite, baryta fledspar, lepidolite are added and is ground in raymond mill, pulverizing acc power is 22KW, mixture granularity is 200 mesh;
（3）By acetate fiber, polyurethane, tert-butyl hydroperoxide, trimethoxy silane, methyl triacetoxysilane, nitridation Aluminum, ammonium chloride, ferrum oxide, Red copper oxide, 2,2'- methylene bis (4- methyl -6- tert-butyl phenols), step（2）Powder mixing Thing adds together hot test electric furnace to sinter, and by the high temperature sintering thing water quenching for obtaining, cooling obtains ceramic block, high temperature sintering temperature For 450 DEG C, the high temperature sintering time is 10 minutes, and the coolant-temperature gage that enters of water quenching is 10 DEG C, and the water quenching time is 45 seconds；
（4）By step（3）Ceramic block, sodium lignin sulfonate, Hydroxypropyl acrylate, Polyethylene Glycol, lauryl amine base sodium sulfonate one Rise and add ball mill, pellet ratio is 1：8, Ball-milling Time is 4 hours；
（5）By step（4）Ball milling powder mince sorting of sieving, collection is sieved mixture, and mesh size is 200 mesh；
（6）By step（5）The mixture that sieves, sodium silicate, sodium tripolyphosphate, 2- ethyl acetic acid lead, three iso stearate metatitanic acids it is different Stir in propyl ester injection high pressure homogenizer, 1000 revs/min of rotating speed, pressure is 0.5MPa, is mixed 15 minutes；
（7）By step（6）Stirring mixture injection mould in it is compressing, gained idiosome is fixed in 4 DEG C of nitrogen couveuses, Degumming 30 minutes；
（8）By step（7）Idiosome be put in vacuum high-temperature calcining furnace and be sintered molding, calcining heat is 780 DEG C, vacuum pressure It is by force 0.2Pa, the vacuum-sintering time is 60 minutes；
（9）By step（8）Calcining model be slowly dropped to after room temperature, mould from, dewax, be put in 60 DEG C of nitrogen couveuses and conserve 2 Hour, get product.
The performance test results of obtained high-strength carbon fiber based composite ceramic material are as shown in table 1.
Embodiment 2
（1）33 parts of ceramics, 6 parts of hydroxyapatite, 6 parts of baryta fledspar, 5 parts of lepidolite, acetate fiber 13 are weighed according to weight portion Part, 3 parts of polyurethane, 2 parts of tert-butyl hydroperoxide, 4 parts of trimethoxy silane, 2 parts of methyl triacetoxysilane, sulfomethylated lignin 5 parts of sour sodium, 3 parts of Hydroxypropyl acrylate, 2 parts of Polyethylene Glycol, 5 parts of lauryl amine base sodium sulfonate, 1 part of aluminium nitride, 2 parts of ammonium chloride, oxygen Change 3 parts of ferrum, 3 parts of Red copper oxide, 3 parts of sodium silicate, 1 part of sodium tripolyphosphate, 2 parts of 4- hydroxy-dodecanoic acids anilid, ricinoleic acid 3 parts of calcium, isopropyl three（Dioctyl pyrophosphoryl base) 1 part of titanate esters；
（2）Ceramics, hydroxyapatite, baryta fledspar, lepidolite are added and is ground in raymond mill, pulverizing acc power is 22KW, mixture granularity is 250 mesh;
（3）By acetate fiber, polyurethane, tert-butyl hydroperoxide, trimethoxy silane, methyl triacetoxysilane, nitridation Aluminum, ammonium chloride, ferrum oxide, Red copper oxide, 4- hydroxy-dodecanoic acid anilids, step（2）Mixture of powders add together Hot test electric furnace is sintered, and by the high temperature sintering thing water quenching for obtaining, cooling obtains ceramic block, and high temperature sintering temperature is 470 DEG C, high Warm sintering time is 15 minutes, and the coolant-temperature gage that enters of water quenching is 12 DEG C, and the water quenching time is 45 seconds；
（4）By step（3）Ceramic block, sodium lignin sulfonate, Hydroxypropyl acrylate, Polyethylene Glycol, lauryl amine base sodium sulfonate one Rise and add ball mill, pellet ratio is 1：8, Ball-milling Time is 4 hours；
（5）By step（4）Ball milling powder mince sorting of sieving, collection is sieved mixture, and mesh size is 200 mesh；
（6）By step（5）The mixture that sieves, sodium silicate, sodium tripolyphosphate, calcium ricinoleate, isopropyl three（Dioctyl pyrophosphoryl Base) titanate esters injection high pressure homogenizer in stir, 1200 revs/min of rotating speed, pressure is 0.7MPa, mix 20 points Clock；
（7）By step（6）Stirring mixture injection mould in it is compressing, gained idiosome is fixed in 6 DEG C of nitrogen couveuses, Degumming 30 minutes；
（8）By step（7）Idiosome be put in vacuum high-temperature calcining furnace and be sintered molding, calcining heat is 800 DEG C, vacuum pressure It is by force 0.3Pa, the vacuum-sintering time is 70 minutes；
（9）By step（8）Calcining model be slowly dropped to after room temperature, mould from, dewax, be put in 60 DEG C of nitrogen couveuses conserve 2.5 hours, get product.
The performance test results of obtained high-strength carbon fiber based composite ceramic material are as shown in table 1.
Embodiment 3
（1）37 parts of ceramics, 7 parts of hydroxyapatite, 7 parts of baryta fledspar, 6 parts of lepidolite, acetate fiber 14 are weighed according to weight portion Part, 4 parts of polyurethane, 3 parts of tert-butyl hydroperoxide, 5 parts of trimethoxy silane, 3 parts of methyl triacetoxysilane, sulfomethylated lignin 6 parts of sour sodium, 4 parts of Hydroxypropyl acrylate, 3 parts of Polyethylene Glycol, 7 parts of lauryl amine base sodium sulfonate, 2 parts of aluminium nitride, 3 parts of ammonium chloride, oxygen Change 4 parts of ferrum, 5 parts of Red copper oxide, 4 parts of sodium silicate, 2 parts of sodium tripolyphosphate, 3 parts of 4,4'-, bis- t-octyl diphenylamines, zinc stearate 4 Part, two (dioctyl pyrophosphoryl bases) close 2 parts of fluoroacetic acid ester titanium；
（2）Ceramics, hydroxyapatite, baryta fledspar, lepidolite are added and is ground in raymond mill, pulverizing acc power is 22KW, mixture granularity is 250 mesh;
（3）By acetate fiber, polyurethane, tert-butyl hydroperoxide, trimethoxy silane, methyl triacetoxysilane, nitridation Aluminum, ammonium chloride, ferrum oxide, Red copper oxide, the t-octyl diphenylamines of 4,4'- bis-, step（2）Mixture of powders add high temperature together Testing furnace is sintered, and by the high temperature sintering thing water quenching for obtaining, cooling obtains ceramic block, and high temperature sintering temperature is 490 DEG C, and high temperature burns The knot time is 20 minutes, and the coolant-temperature gage that enters of water quenching is 14 DEG C, and the water quenching time is 45 seconds；
（4）By step（3）Ceramic block, sodium lignin sulfonate, Hydroxypropyl acrylate, Polyethylene Glycol, lauryl amine base sodium sulfonate one Rise and add ball mill, pellet ratio is 1：8, Ball-milling Time is 4 hours；
（5）By step（4）Ball milling powder mince sorting of sieving, collection is sieved mixture, and mesh size is 200 mesh；
（6）By step（5）The mixture that sieves, sodium silicate, sodium tripolyphosphate, zinc stearate, two (dioctyl pyrophosphoryl bases) close Stir in fluoroacetic acid ester titanium injection high pressure homogenizer, 1400 revs/min of rotating speed, pressure is 0.9MPa, mixes 25 points Clock；
（7）By step（6）Stirring mixture injection mould in it is compressing, gained idiosome is fixed in 8 DEG C of nitrogen couveuses, Degumming 30 minutes；
（8）By step（7）Idiosome be put in vacuum high-temperature calcining furnace and be sintered molding, calcining heat is 820 DEG C, vacuum pressure It is by force 0.4Pa, the vacuum-sintering time is 80 minutes；
（9）By step（8）Calcining model be slowly dropped to after room temperature, mould from, dewax, be put in 60 DEG C of nitrogen couveuses and conserve 3 Hour, get product.
The performance test results of obtained high-strength carbon fiber based composite ceramic material are as shown in table 1.
Embodiment 4
（1）40 parts of ceramics, 8 parts of hydroxyapatite, 8 parts of baryta fledspar, 6 parts of lepidolite, acetate fiber 15 are weighed according to weight portion Part, 5 parts of polyurethane, 3 parts of tert-butyl hydroperoxide, 6 parts of trimethoxy silane, 4 parts of methyl triacetoxysilane, sulfomethylated lignin 7 parts of sour sodium, 5 parts of Hydroxypropyl acrylate, 4 parts of Polyethylene Glycol, 8 parts of lauryl amine base sodium sulfonate, 2 parts of aluminium nitride, 4 parts of ammonium chloride, oxygen Change 5 parts of ferrum, 6 parts of Red copper oxide, 5 parts of sodium silicate, 2 parts of sodium tripolyphosphate, 4 parts of 4- hydroxyoctadecanoic acids anilid, Osmanthus tragranscv.Aurantiacu acid 5 parts of barium, isopropyl three (positive ethylamino-ethylamino) 2 parts of titanate esters；
（2）Ceramics, hydroxyapatite, baryta fledspar, lepidolite are added and is ground in raymond mill, pulverizing acc power is 22KW, mixture granularity is 300 mesh;
（3）By acetate fiber, polyurethane, tert-butyl hydroperoxide, trimethoxy silane, methyl triacetoxysilane, nitridation Aluminum, ammonium chloride, ferrum oxide, Red copper oxide, 4- hydroxyoctadecanoic acid anilids, step（2）Mixture of powders add together Hot test electric furnace is sintered, and by the high temperature sintering thing water quenching for obtaining, cooling obtains ceramic block, and high temperature sintering temperature is 500 DEG C, high Warm sintering time is 25 minutes, and the coolant-temperature gage that enters of water quenching is 15 DEG C, and the water quenching time is 45 seconds；
（4）By step（3）Ceramic block, sodium lignin sulfonate, Hydroxypropyl acrylate, Polyethylene Glycol, lauryl amine base sodium sulfonate one Rise and add ball mill, pellet ratio is 1：8, Ball-milling Time is 4 hours；
（5）By step（4）Ball milling powder mince sorting of sieving, collection is sieved mixture, and mesh size is 200 mesh；
（6）By step（5）The mixture that sieves, sodium silicate, sodium tripolyphosphate, Osmanthus tragranscv.Aurantiacu acid barium, (positive ethylamino-the second of isopropyl three Amino) titanate esters injection high pressure homogenizer in stir, 1500 revs/min of rotating speed, pressure is 1MPa, mix 30 points Clock；
（7）By step（6）Stirring mixture injection mould in it is compressing, gained idiosome is solid in 10 DEG C of nitrogen couveuses Calmly, degumming 30 minutes；
（8）By step（7）Idiosome be put in vacuum high-temperature calcining furnace and be sintered molding, calcining heat is 860 DEG C, vacuum pressure It is by force 0.5Pa, the vacuum-sintering time is 90 minutes；
（9）By step（8）Calcining model be slowly dropped to after room temperature, mould from, dewax, be put in 60 DEG C of nitrogen couveuses and conserve 4 Hour, get product.
The performance test results of obtained high-strength carbon fiber based composite ceramic material are as shown in table 1.
Comparative example 1
（1）30 parts of ceramics, 5 parts of hydroxyapatite, 5 parts of baryta fledspar, 5 parts of lepidolite, acetate fiber 12 are weighed according to weight portion Part, 2 parts of polyurethane, 2 parts of tert-butyl hydroperoxide, 3 parts of trimethoxy silane, 1 part of methyl triacetoxysilane, acrylic acid hydroxyl 2 parts of propyl ester, 1 part of Polyethylene Glycol, 4 parts of lauryl amine base sodium sulfonate, 1 part of aluminium nitride, 2 parts of Red copper oxide, 2 parts of sodium silicate, trimerization phosphorus 1 part of sour sodium, 1 part of 2,2'- methylene bis (4- methyl -6- tert-butyl phenols), 2 parts of 2- ethyl acetic acids lead, three iso stearate metatitanic acids are different 1 part of propyl ester；
（2）Ceramics, hydroxyapatite, baryta fledspar, lepidolite are added and is ground in raymond mill, pulverizing acc power is 22KW, mixture granularity is 200 mesh;
（3）By acetate fiber, polyurethane, tert-butyl hydroperoxide, trimethoxy silane, methyl triacetoxysilane, nitridation Aluminum, Red copper oxide, 2,2'- methylene bis (4- methyl -6- tert-butyl phenols), step（2）Mixture of powders add high temperature together Testing furnace is sintered, and by the high temperature sintering thing water quenching for obtaining, cooling obtains ceramic block, and high temperature sintering temperature is 450 DEG C, and high temperature burns The knot time is 10 minutes, and the coolant-temperature gage that enters of water quenching is 10 DEG C, and the water quenching time is 45 seconds；
（4）By step（3）Ceramic block, Hydroxypropyl acrylate, Polyethylene Glycol, lauryl amine base sodium sulfonate add ball mill together, Pellet ratio is 1：8, Ball-milling Time is 4 hours；
（5）By step（4）Ball milling powder mince sorting of sieving, collection is sieved mixture, and mesh size is 200 mesh；
（6）By step（5）The mixture that sieves, sodium silicate, sodium tripolyphosphate, 2- ethyl acetic acid lead, three iso stearate metatitanic acids it is different Stir in propyl ester injection high pressure homogenizer, 1000 revs/min of rotating speed, pressure is 0.5MPa, is mixed 15 minutes；
（7）By step（6）Stirring mixture injection mould in it is compressing, gained idiosome is fixed in 4 DEG C of nitrogen couveuses, Degumming 30 minutes；
（8）By step（7）Idiosome be put in vacuum high-temperature calcining furnace and be sintered molding, calcining heat is 780 DEG C, vacuum pressure It is by force 0.2Pa, the vacuum-sintering time is 60 minutes；
（9）By step（8）Calcining model be slowly dropped to after room temperature, mould from, dewax, be put in 60 DEG C of nitrogen couveuses and conserve 2 Hour, get product.
The performance test results of obtained high-strength carbon fiber based composite ceramic material are as shown in table 1.
Comparative example 2
（1）40 parts of ceramics, 8 parts of hydroxyapatite, 8 parts of baryta fledspar, 6 parts of lepidolite, acetate fiber 15 are weighed according to weight portion Part, 5 parts of polyurethane, 3 parts of tert-butyl hydroperoxide, 6 parts of trimethoxy silane, 4 parts of methyl triacetoxysilane, sulfomethylated lignin 7 parts of sour sodium, 5 parts of Hydroxypropyl acrylate, 4 parts of Polyethylene Glycol, 4 parts of ammonium chloride, 5 parts of ferrum oxide, 6 parts of Red copper oxide, tripolyphosphate 2 parts of sodium, 4 parts of 4- hydroxyoctadecanoic acids anilid, Osmanthus tragranscv.Aurantiacu 5 parts of barium of acid, isopropyl three (positive ethylamino-ethylamino) titanate esters 2 parts；
（2）Ceramics, hydroxyapatite, baryta fledspar, lepidolite are added and is ground in raymond mill, pulverizing acc power is 22KW, mixture granularity is 300 mesh;
（3）By acetate fiber, polyurethane, tert-butyl hydroperoxide, trimethoxy silane, methyl triacetoxysilane, chlorination Ammonium, ferrum oxide, Red copper oxide, 4- hydroxyoctadecanoic acid anilids, step（2）Mixture of powders add hot test together Electric furnace is sintered, and by the high temperature sintering thing water quenching for obtaining, cooling obtains ceramic block, and high temperature sintering temperature is 500 DEG C, during high temperature sintering Between be 25 minutes, water quenching enters coolant-temperature gage for 15 DEG C, and the water quenching time is 45 seconds；
（4）By step（3）Ceramic block, sodium lignin sulfonate, Hydroxypropyl acrylate, Polyethylene Glycol add ball mill together, expect Ball ratio is 1：8, Ball-milling Time is 4 hours；
（5）By step（4）Ball milling powder mince sorting of sieving, collection is sieved mixture, and mesh size is 200 mesh；
（6）By step（5）The mixture that sieves, sodium tripolyphosphate, Osmanthus tragranscv.Aurantiacu acid barium, isopropyl three (positive ethylamino-ethylamino) titanium Stir in acid esters injection high pressure homogenizer, 1500 revs/min of rotating speed, pressure is 1MPa, is mixed 30 minutes；
（7）By step（6）Stirring mixture injection mould in it is compressing, gained idiosome is solid in 10 DEG C of nitrogen couveuses Calmly, degumming 30 minutes；
（8）By step（7）Idiosome be put in vacuum high-temperature calcining furnace and be sintered molding, calcining heat is 860 DEG C, vacuum pressure It is by force 0.5Pa, the vacuum-sintering time is 90 minutes；
（9）By step（8）Calcining model be slowly dropped to after room temperature, mould from, dewax, be put in 60 DEG C of nitrogen couveuses and conserve 4 Hour, get product.
The performance test results of obtained high-strength carbon fiber based composite ceramic material are as shown in table 1.
The obtained high-strength carbon fiber based composite ceramic material of embodiment 1-4 and comparative example 1-2 is carried out thermal conductivity, resisted Compressive Strength, thermal coefficient of expansion, this several performance tests of impact flexibility.
Table 1
　 Thermal conductivity（W/m.K） Comprcssive strength（MPa） Thermal coefficient of expansion（10-6/K） Impact flexibility（KJ.M2）
Embodiment 1 138.88 678 8.46 3.87
Embodiment 2 138.17 672 0.49 4.28
Embodiment 3 140.61 670 0.47 4.18
Embodiment 4 141.12 675 0.51 3.98
Comparative example 1 89.02 334 1.21 1.22
Comparative example 2 97.48 424 1.33 1.43
The high-strength carbon fiber based composite ceramic material of the present invention, with ceramics, hydroxyapatite, baryta fledspar, lepidolite, acetic acid Fiber, polyurethane, tert-butyl hydroperoxide, trimethoxy silane, methyl triacetoxysilane, aluminium nitride, ammonium chloride, oxidation Ferrum, Red copper oxide are main component, by adding sodium lignin sulfonate, Hydroxypropyl acrylate, Polyethylene Glycol, lauryl amine base sulfonic acid Sodium, sodium silicate, sodium tripolyphosphate, antioxidant, stabilizer, coupling agent, are aided with mechanical activation comminution, high temperature sintering, Water Quenching, ball The techniques such as mill sorting, the homogeneous, mold that pressurizes are fixed, the dewaxing of vacuum calcining, mould from, maintenance molding so that what is be prepared from is high-strength Degree carbon fiber-based composite ceramic material, its stable performance, intensity is big, be unlikely to deform, high temperature resistant and good heat conductivity, disclosure satisfy that The requirement of industry, with preferable application prospect.The high-strength carbon fiber based composite ceramic material raw material of the present invention is cheap, technique Simply, heavy industrialization utilization is suitable to, it is practical.
Embodiments of the invention are the foregoing is only, the scope of the claims of the present invention is not thereby limited, it is every using this Equivalent structure or equivalent flow conversion that bright description is made, or directly or indirectly it is used in other related technology necks Domain, is included within the scope of the present invention.

Claims (7)

1. a kind of high-strength carbon fiber based composite ceramic material, it is characterised in that：It is prepared by the raw materials in：Ceramics 30-40 parts, hydroxyapatite 5-8 parts, baryta fledspar 5-8 parts, lepidolite 5-6 parts, acetate fiber 12-15 parts, polyurethane 2-5 parts, Tert-butyl hydroperoxide 2-3 part, trimethoxy silane 3-6 parts, methyl triacetoxysilane 1-4 parts, sodium lignin sulfonate 4-7 Part, Hydroxypropyl acrylate 2-5 parts, Polyethylene Glycol 1-4 parts, lauryl amine base sodium sulfonate 4-8 parts, aluminium nitride 1-2 parts, ammonium chloride 1-4 It is part, ferrum oxide 2-5 parts, Red copper oxide 2-6 parts, sodium silicate 2-5 parts, sodium tripolyphosphate 1-2 parts, antioxidant 1-4 parts, stable Agent 2-5 parts, coupling agent 1-2 parts.
2. high-strength carbon fiber based composite ceramic material according to claim 1, it is characterised in that：The antioxidant is 2,2'- methylene bis (4- methyl -6- tert-butyl phenols), 4- hydroxy-dodecanoic acid anilids, the t-octyl diphenylamines of 4,4'- bis-, One or more in 4- hydroxyoctadecanoic acid anilids.
3. high-strength carbon fiber based composite ceramic material according to claim 1, it is characterised in that：The stabilizer is 2- Any one in ethyl acetic acid lead, calcium ricinoleate, zinc stearate, Osmanthus tragranscv.Aurantiacu acid barium.
4. high-strength carbon fiber based composite ceramic material according to claim 1, it is characterised in that：The coupling agent is selected from Three iso stearate isopropyl titanates, isopropyl three（Dioctyl pyrophosphoryl base) titanate esters, two (dioctyl pyrophosphoryl bases) close oxygen second Any one or a few in acid esters titanium, isopropyl three (positive ethylamino-ethylamino) titanate esters.
5., according to the preparation method of the arbitrary described high-strength carbon fiber based composite ceramic material of claim 1-4, its feature exists In comprising the following steps：
（1）Each raw material is weighed according to weight portion；
（2）Ceramics, hydroxyapatite, baryta fledspar, lepidolite are added and is ground in raymond mill, pulverizing acc power is 22KW, mixture granularity is 200-300 mesh;
（3）By acetate fiber, polyurethane, tert-butyl hydroperoxide, trimethoxy silane, methyl triacetoxysilane, nitridation Aluminum, ammonium chloride, ferrum oxide, Red copper oxide, antioxidant, step（2）Mixture of powders add together hot test electric furnace burn Knot, by the high temperature sintering thing water quenching for obtaining, cooling obtains ceramic block, and high temperature sintering temperature is 450-500 DEG C, the high temperature sintering time For 10-25 minutes；
（4）By step（3）Ceramic block, sodium lignin sulfonate, Hydroxypropyl acrylate, Polyethylene Glycol, lauryl amine base sodium sulfonate one Rise and add ball mill, pellet ratio is 1：8, Ball-milling Time is 4 hours；
（5）By step（4）Ball milling powder mince sorting of sieving, collection is sieved mixture；
（6）By step（5）The mixture that sieves, sodium silicate, sodium tripolyphosphate, stabilizer, coupling agent injection high pressure homogenizer in Stir, 1000-1500 rev/min of rotating speed, pressure is 0.5-1MPa, mix 15-30 minutes；
（7）By step（6）Stirring mixture injection mould in it is compressing, gained idiosome is solid in 4-10 DEG C of nitrogen couveuse Calmly, degumming 30 minutes；
（8）By step（7）Idiosome be put in vacuum high-temperature calcining furnace and be sintered molding, calcining heat is 780-860 DEG C, very Pneumatics is by force 0.2-0.5Pa, and the vacuum-sintering time is 60-90 minutes；
（9）By step（8）Calcining model be slowly dropped to after room temperature, mould from, dewax, be put in 60 DEG C of nitrogen couveuses and conserve 2- 4 hours, get product.
6. the preparation method of high-strength carbon fiber based composite ceramic material according to claim 5, it is characterised in that described Step（3）In, the condition of water quenching is：Enter coolant-temperature gage for 10-15 DEG C, the water quenching time is 45 seconds.
7. the preparation method of high-strength carbon fiber based composite ceramic material according to claim 5, it is characterised in that described Step（5）In, mesh size is 200 mesh.
CN201611112533.4A 2016-12-07 2016-12-07 High-strength carbon fiber based composite ceramic material and preparation method thereof Pending CN106587937A (en)

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CN108559315A (en) * 2018-02-28 2018-09-21 佛山市飞时达新材料科技有限公司 A kind of automobile-used molybdenum disulfide high temperature resistant wear-reduced coating and preparation method thereof

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Application publication date: 20170426