CN102295465B - Hot-press preparation method of short carbon fiber/silicon carbide composite material - Google Patents
Hot-press preparation method of short carbon fiber/silicon carbide composite material Download PDFInfo
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Abstract
The invention discloses a hot-press preparation method of a short carbon fiber/silicon carbide composite material, comprising the following steps: putting a preoxidized fiber in heated alkali liquor, carrying out splitting processing, then washing with distilled water; mixing the preoxidized fiber processed by splitting with silicon carbide powder, sintering aid, binder, interfacial wetting agent, antifoaming agent and water, and uniformly pounding to obtain a slurry; putting the slurry in a graphite die, compacting and drying, finally putting the graphite die with the body in a hotpressing furnace, and sintering at high temperature to obtain the short carbon fiber/silicon carbide composite material. The method adopts the preoxidized fiber with good toughness as the raw material instead of the short carbon fiber with brittleness, so that the problem that the preoxidized fiber is easy to break in the splitting process is avoided; and the preoxidized fiber can in situ conversed into a carbon fiber in the sintering process, so that the resource of the carbon fiber is widened, and the cost is reduced; and simultaneously, Al-Si eutectic powder and B-Al alloy powder are used in the sintering aid instead of a mixture of aluminium powder and boron powder, so that the problem that aluminium reacts with carbon to generate easy hydrolytic compound A14C3 can be avoided.
Description
Technical field
The present invention relates to a kind of preparation method of chopped carbon fiber/composite material of silicon carbide, be specifically related to the hot pressing method for preparing of chopped carbon fiber/composite material of silicon carbide.
Background technology
Chopped carbon fiber/silicon carbide (C
Sf/ SiC) having the structure and function characteristic concurrently, over-all properties is superior, has application prospect in fields such as braking, sliding friction, bone implantation, elevated-temperature seal, speculums.Tang Hanling etc. has proposed a kind of employing chopped carbon fiber as strengthening toughened fiber, with silicon, aluminium, boron is done sintering aid, the method of hot pressing chopped carbon fiber/silicon carbide (Hanling Tang, XierongZeng, XinboXiong, LongLi, JizhaoZou.Mechanical and tribological properties of short-fiber-reinforced SiC composites, Tribology International, 2009,42:823-827), it is high that the method can obtain material density, reach more than 99%, and the carbon fiber large volume fraction is large, and Uniform Dispersion.But the carbon fiber that the method adopts is expensive, and owing in the sintering aid pure aluminum being arranged, if therefore directly take out immediately behind the ball milling, vigorous reaction can occur in ball milling hybrid technique step from ball grinder, causes mixture to burn even explodes; If take out Deng after the ball grinder cooling, easy and carbon reaction generates Al owing to aluminium in the mechanical milling process
4C
3Phase, this steeping in water for reconstitution of meeting is given birth to vigorous reaction, can destroy carbon fiber, therefore when ball milling hybrid technique step, must add the gas protection and want careful operation.
Summary of the invention
The object of the present invention is to provide the hot pressing method for preparing of chopped carbon fiber/composite material of silicon carbide that a kind of cost is low, the fiber protectiveness is good, technological process is easy to control, safe.
For achieving the above object, the technical solution used in the present invention is:
1) at first the pre-oxygen silk of 2～20mm or pre-oxygen silk and 2～20mm carbon fiber are placed NaOH, KOH or the Ca (OH) of 1～10mol/L with the mixture of any ratio
2The aqueous solution in, be that 40 ℃～100 ℃ lower heating 1～24h open fine the processing in temperature, then and oven dry, for subsequent use clean with the distilled water ultrasonic cleaning;
2) silicon carbide powder, sintering aid, binding agent, interface wetting agent, defoamer and water are mixed, and stir into uniform slip;
3) with step 1) the silk union adding step 2 of the pre-oxygen silk that obtains or pre-oxygen silk and carbon fiber) in the slip that obtains, smash evenly, obtain containing the slip of pre-oxygen silk or silk union;
4) the more resulting slip that contains pre-oxygen silk or silk union being placed graphite jig, is to make base substrate under 5～10MPa at pressure, and the graphite jig that then will contain base substrate places the vacuum drying oven that vacuumizes, 100～120 ℃ of dryings;
5) dried base substrate is placed hot pressing furnace together with graphite jig, be warming up to 900 ℃～1200 ℃ from room temperature with stove, be to process 2～4h under the 20MPa at pressure, and then rise to 1800 ℃～2400 ℃, be 20MPa～40MPa at pressure, insulation 30min～60min sintering cools to room temperature with the furnace and obtains chopped carbon fiber/composite material of silicon carbide.
Described carbon fiber is the mixture of one or more arbitrary proportions in PAN-based carbon fiber, viscose-based carbon fiber, asphalt base carbon fiber or the graphite fibre.
The granularity of described silicon carbide powder is less than 2 μ m.
Described sintering aid is the mixture of silica flour, al-si eutectic powder and boron Al alloy powder, and wherein the mass percent of silica flour is 55%～70%, and the al-si eutectic powder is 20～30%, and the boron Al alloy powder is 10～25%.
Described binding agent is one or more of commercial phenolic resin or modified phenolic resins, Resins, epoxy and versamid 900.
Described interface wetting agent is one or more in ethanol, acetone and the glycerol.
Described defoamer is one or more in commercially available basic phenol polyethenoxy ether 9 in the ninth of the ten Heavenly Stems (suffering), the ninth of the ten Heavenly Stems (suffering) basic phenol polyethenoxy ether 15, op-10, tween 20, tween-80, this dish-60, the Span-80.
Described silicon carbide powder, sintering aid, binding agent, interface wetting agent, defoamer and water finish mix slurry, by 100 parts of mass fractions, wherein silicon carbide powder 27-37 part, 3～12 parts of sintering aids, 5～10 parts of binding agents, 5～10 parts of interface wetting agents, 1～5 part of defoamer, surplus is water.
Described step 3) volume fraction that contains the silk union of pre-oxygen silk in the slip of pre-oxygen silk or silk union or pre-oxygen silk and carbon fiber is 15%～50%.
The present invention adopts pre-oxygen silk to substitute carbon fiber, with the mixture replacing boron powder of commercially available silica flour, al-si eutectic powder and boron Al alloy powder and the mixture of aluminium powder, and the method for employing aqueous slurries/hot pressing chopped carbon fiber/silicon carbide.The present invention has the advantages that cost is low, the fiber protectiveness is good, technological process is more easy to control and safe.
Description of drawings
Fig. 1 is at the flying-spot microscope picture that is incubated sintering 60min gained chopped carbon fiber/silicon carbide under 130min, the 1800 ℃ of 30MPa pressure under 1000 ℃ of lower 20MPa pressure.
Embodiment
Below in conjunction with drawings and Examples the present invention is described in further detail.
Embodiment 1:
1) at first the pre-oxygen silk of 2～20mm being placed the aqueous solution of the NaOH of 5mol/L, is that 40 ℃ of lower heating 24h open fine the processing in temperature, then and oven dry, for subsequent use clean with the distilled water ultrasonic cleaning;
2) by 100 parts of mass fractions, 27 parts of granularities silicon carbide powder, 12 component sintering additives, 6 parts of binding agent commercial phenolic resin, 8 parts of interface wetting agent ethanol, 2 parts of commercially available polyoxyethylene octylphenol ether 9 and water of defoamer less than 2 μ m are mixed, and stir into uniform slip;
Described sintering aid is the mixture of silica flour, al-si eutectic powder and boron Al alloy powder, and wherein the mass percent of silica flour is 55%, and the al-si eutectic powder is 20%, and the boron Al alloy powder is 25%;
3) with step 1) the pre-oxygen silk that obtains adds step 2) in the slip that obtains, smash evenly, obtain containing the slip of pre-oxygen silk;
Wherein the volume fraction of pre-oxygen silk is 50%;
4) the more resulting slip that contains pre-oxygen silk being placed graphite jig, is to make base substrate under the 6MPa at pressure, and the graphite jig that then will contain base substrate places the vacuum drying oven that vacuumizes, 100 ℃ of dryings;
5) dried base substrate is placed hot pressing furnace together with graphite jig, being warming up to 1000 ℃ from room temperature with stove, is to process 3h under the 20MPa at pressure, and then rise to 1800 ℃, be 30MPa at pressure, insulation 60min sintering cools to room temperature with the furnace and obtains chopped carbon fiber/composite material of silicon carbide.Referring to Fig. 1, as seen from Figure 1, silicon carbide substrate is very fine and close, and fiber is evenly distributed in silicon carbide substrate.
Embodiment 2:
1) at first the pre-oxygen silk of 2～20mm being placed the aqueous solution of the KOH of 8mol/L, is that 60 ℃ of lower heating 15h open fine the processing in temperature, then and oven dry, for subsequent use clean with the distilled water ultrasonic cleaning;
2) by 100 parts of mass fractions, 37 parts of granularities are mixed less than the silicon carbide powder of 2 μ m, 3 component sintering additives, 10 parts of binder modification resol, 5 parts of interface wetting agent acetone, 5 parts of defoamer polyoxyethylene octylphenol ethers 15 and water, and stir into uniform slip;
Described sintering aid is the mixture of silica flour, al-si eutectic powder and boron Al alloy powder, and wherein the mass percent of silica flour is 70%, and the al-si eutectic powder is 20%, and the boron Al alloy powder is 10%;
3) with step 1) the pre-oxygen silk that obtains adds step 2) in the slip that obtains, smash evenly, obtain containing the slip of pre-oxygen silk;
Wherein the volume fraction of pre-oxygen silk is 10%;
4) the more resulting slip that contains pre-oxygen silk being placed graphite jig, is to make base substrate under the 10MPa at pressure, and the graphite jig that then will contain base substrate places the vacuum drying oven that vacuumizes, 120 ℃ of dryings;
5) dried base substrate is placed hot pressing furnace together with graphite jig, being warming up to 1200 ℃ from room temperature with stove, is to process 2h under the 20MPa at pressure, and then rise to 2000 ℃, be 20MPa at pressure, insulation 30min sintering cools to room temperature with the furnace and obtains chopped carbon fiber/composite material of silicon carbide.
Embodiment 3:
1) at first the pre-oxygen silk of 2～20mm and the PAN-based carbon fiber of 2～20mm are placed the Ca (OH) of 1mol/L with the mixture of any ratio
2The aqueous solution in, be that 100 ℃ of lower heating 1h open fine the processing in temperature, then and oven dry, for subsequent use clean with the distilled water ultrasonic cleaning;
2) by 100 parts of mass fractions, 30 parts of granularities are mixed less than the silicon carbide powder of 2 μ m, 10 component sintering additives, 8 parts of epoxy resin of binder, 10 parts of interface wetting agent glycerol, 1 part of defoamer op-10 and water, and stir into uniform slip;
Described sintering aid is the mixture of silica flour, al-si eutectic powder and boron Al alloy powder, and wherein the mass percent of silica flour is 60%, and the al-si eutectic powder is 30%, and the boron Al alloy powder is 10%;
3) with step 1) the pre-oxygen silk that obtains and the silk union of PAN-based carbon fiber add step 2) in the slip that obtains, smash evenly, obtain containing the slip of silk union;
Wherein the volume fraction of the silk union of pre-oxygen silk and PAN-based carbon fiber is 40%;
4) the more resulting slip that contains silk union being placed graphite jig, is to make base substrate under the 8MPa at pressure, and the graphite jig that then will contain base substrate places the vacuum drying oven that vacuumizes, 110 ℃ of dryings;
5) dried base substrate is placed hot pressing furnace together with graphite jig, being warming up to 900 ℃ from room temperature with stove, is to process 4h under the 20MPa at pressure, and then rise to 2400 ℃, be 40MPa at pressure, insulation 50min sintering cools to room temperature with the furnace and obtains chopped carbon fiber/composite material of silicon carbide.
Embodiment 4:
1) at first the pre-oxygen silk of 2～20mm and the viscose-based carbon fiber of 2～20mm are placed the aqueous solution of the NaOH of 3mol/L with the mixture of any ratio, heating 20h open fine the processing under temperature is 50 ℃, then use the distilled water ultrasonic cleaning totally and oven dry, for subsequent use;
2) by 100 parts of mass fractions, 32 parts of granularities are mixed less than the mixture of the silicon carbide powder of 2 μ m, 8 component sintering additives, 5 parts of binding agent versamid 900s, 7 parts of interface wetting agent ethanol and acetone, 4 parts of defoamer tween 20s and water, and stir into uniform slip;
Described sintering aid is the mixture of silica flour, al-si eutectic powder and boron Al alloy powder, and wherein the mass percent of silica flour is 65%, and the al-si eutectic powder is 25%, and the boron Al alloy powder is 10%;
3) with step 1) the pre-oxygen silk that obtains and the silk union of carbon fiber add step 2) in the slip that obtains, smash evenly, obtain containing the slip of silk union;
Wherein the volume fraction of the silk union of pre-oxygen silk and carbon fiber is 15%;
4) the more resulting slip that contains silk union being placed graphite jig, is to make base substrate under the 5MPa at pressure, and the graphite jig that then will contain base substrate places the vacuum drying oven that vacuumizes, 103 ℃ of dryings;
5) dried base substrate is placed hot pressing furnace together with graphite jig, be warming up to 1100 ℃ from room temperature with stove, be to process 2.5h under the 20MPa at pressure, and then rise to 1900 ℃, be 25MPa at pressure, insulation 45min sintering cools to room temperature with the furnace and obtains chopped carbon fiber/composite material of silicon carbide.
Embodiment 5:
1) at first the pre-oxygen silk of 2～20mm and the asphalt base carbon fiber of 2～20mm are placed the aqueous solution of the KOH of 7mol/L with the mixture of any ratio, heating 10h open fine the processing under temperature is 80 ℃, then use the distilled water ultrasonic cleaning totally and oven dry, for subsequent use;
2) by 100 parts of mass fractions, 34 parts of granularities are mixed less than the mixture of the silicon carbide powder of 2 μ m, 6 component sintering additives, 9 parts of binding agent commercial phenolic resin and the mixture of Resins, epoxy, 6 parts of interface wetting agent ethanol, acetone and glycerol, 3 parts of defoamer these dishes-60 and water, and stir into uniform slip;
Described sintering aid is the mixture of silica flour, al-si eutectic powder and boron Al alloy powder, and wherein the mass percent of silica flour is 57%, and the al-si eutectic powder is 23%, and the boron Al alloy powder is 20%;
3) with step 1) the pre-oxygen silk that obtains and the silk union of carbon fiber add step 2) in the slip that obtains, smash evenly, obtain containing the slip of silk union;
Wherein the volume fraction of the silk union of pre-oxygen silk and carbon fiber is 30%;
4) the more resulting slip that contains silk union being placed graphite jig, is to make base substrate under the 9MPa at pressure, and the graphite jig that then will contain base substrate places the vacuum drying oven that vacuumizes, 108 ℃ of dryings;
5) dried base substrate is placed hot pressing furnace together with graphite jig, be warming up to 950 ℃ from room temperature with stove, be to process 3.5h under the 20MPa at pressure, and then rise to 2100 ℃, be 32MPa at pressure, insulation 35min sintering cools to room temperature with the furnace and obtains chopped carbon fiber/composite material of silicon carbide.
Embodiment 6:
1) at first the pre-oxygen silk of 2～20mm and the graphite fibre of 2～20mm are placed the Ca (OH) of 10mol/L with the mixture of any ratio
2The aqueous solution in, be that 70 ℃ of lower heating 18h open fine the processing in temperature, then and oven dry, for subsequent use clean with the distilled water ultrasonic cleaning;
2) by 100 parts of mass fractions, 35 parts of granularities are mixed with mixture and the water of tween-80, and stirred into uniform slip less than the silicon carbide powder of 2 μ m, 5 component sintering additives, the mixture of 7 parts of binder modification resol, Resins, epoxy and versamid 900s, 9 parts of interface wetting agent ethanol, 3 parts of commercially available polyoxyethylene octylphenol ethers 15 of defoamer;
Described sintering aid is the mixture of silica flour, al-si eutectic powder and boron Al alloy powder, and wherein the mass percent of silica flour is 59%, and the al-si eutectic powder is 26%, and the boron Al alloy powder is 15%;
3) with step 1) the pre-oxygen silk that obtains and the silk union of carbon fiber add step 2) in the slip that obtains, smash evenly, obtain containing the slip of silk union;
Wherein the volume fraction of the silk union of pre-oxygen silk and carbon fiber is 35%;
4) the more resulting slip that contains silk union being placed graphite jig, is to make base substrate under the 7MPa at pressure, and the graphite jig that then will contain base substrate places the vacuum drying oven that vacuumizes, 115 ℃ of dryings;
5) dried base substrate is placed hot pressing furnace together with graphite jig, being warming up to 1050 ℃ from room temperature with stove, is to process 3h under the 20MPa at pressure, and then rise to 2300 ℃, be 36MPa at pressure, insulation 55min sintering cools to room temperature with the furnace and obtains chopped carbon fiber/composite material of silicon carbide.
Embodiment 7:
1) at first the pre-oxygen silk of 2～20mm and PAN-based carbon fiber, viscose-based carbon fiber and the asphalt base carbon fiber of 2～20mm are placed the aqueous solution of the NaOH of 6mol/L with the mixture of any ratio, heating 10h open fine the processing under temperature is 90 ℃, then use the distilled water ultrasonic cleaning totally and oven dry, for subsequent use;
2) by 100 parts of mass fractions, 29 parts of granularities are mixed less than the silicon carbide powder of 2 μ m, 11 component sintering additives, 8 parts of binding agent commercial phenolic resin, 7 parts of interface wetting agent glycerol, 2 parts of defoamer Span-80s and water, and stir into uniform slip;
Described sintering aid is the mixture of silica flour, al-si eutectic powder and boron Al alloy powder, and wherein the mass percent of silica flour is 59%, and the al-si eutectic powder is 26%, and the boron Al alloy powder is 15%;
3) with step 1) the pre-oxygen silk that obtains and the silk union of carbon fiber add step 2) in the slip that obtains, smash evenly, obtain containing the slip of silk union;
Wherein the volume fraction of the silk union of pre-oxygen silk and carbon fiber is 25%;
4) the more resulting slip that contains silk union being placed graphite jig, is to make base substrate under the 8MPa at pressure, and the graphite jig that then will contain base substrate places the vacuum drying oven that vacuumizes, 118 ℃ of dryings;
5) dried base substrate is placed hot pressing furnace together with graphite jig, being warming up to 1150 ℃ from room temperature with stove, is to process 2h under the 20MPa at pressure, and then rise to 2200 ℃, be 28MPa at pressure, insulation 40min sintering cools to room temperature with the furnace and obtains chopped carbon fiber/composite material of silicon carbide.
Claims (8)
1. the hot pressing method for preparing of a chopped carbon fiber/composite material of silicon carbide is characterized in that comprising the steps:
1) at first the pre-oxygen silk of 2～20mm or pre-oxygen silk and 2～20mm carbon fiber are placed the aqueous solution of NaOH or the KOH of 1～10mol/L with the mixture of any ratio, heating 1～24h open fine the processing under temperature is 40 ℃～100 ℃, then use the distilled water ultrasonic cleaning totally and oven dry, for subsequent use;
2) silicon carbide powder, sintering aid, binding agent, interface wetting agent, defoamer and water are mixed, and stir into uniform slip;
Described sintering aid is the mixture of silica flour, al-si eutectic powder and boron Al alloy powder, and wherein the mass percent of silica flour is 55%～70%, and the al-si eutectic powder is 20～30%, and the boron Al alloy powder is 10～25%;
The silk union adding step 2 of the pre-oxygen silk that 3) step 1) is obtained or pre-oxygen silk and carbon fiber) in the slip that obtains, smashes evenly, obtain containing the slip of pre-oxygen silk or silk union;
4) the more resulting slip that contains pre-oxygen silk or silk union being placed graphite jig, is to make base substrate under 5～10MPa at pressure, and the graphite jig that then will contain base substrate places the vacuum drying oven that vacuumizes, 100～120 ℃ of dryings;
5) dried base substrate is placed hot pressing furnace together with graphite jig, be warming up to 900 ℃～1200 ℃ from room temperature with stove, be to process 2～4h under the 20MPa at pressure, and then rise to 1800 ℃～2400 ℃, be 20MPa～40MPa at pressure, insulation 30min～60min sintering cools to room temperature with the furnace and obtains chopped carbon fiber/composite material of silicon carbide.
2. the hot pressing method for preparing of chopped carbon fiber/composite material of silicon carbide according to claim 1, it is characterized in that: described carbon fiber is the mixture of one or more arbitrary proportions in PAN-based carbon fiber, viscose-based carbon fiber, asphalt base carbon fiber or the graphite fibre.
3. the hot pressing method for preparing of chopped carbon fiber/composite material of silicon carbide according to claim 1, it is characterized in that: the granularity of described silicon carbide powder is less than 2 μ m.
4. the hot pressing method for preparing of chopped carbon fiber/composite material of silicon carbide according to claim 1, it is characterized in that: described binding agent is one or more of commercial phenolic resin or modified phenolic resins, Resins, epoxy and versamid 900.
5. the hot pressing method for preparing of chopped carbon fiber/composite material of silicon carbide according to claim 1, it is characterized in that: described interface wetting agent is one or more in ethanol, acetone and the glycerol.
6. the hot pressing method for preparing of chopped carbon fiber/composite material of silicon carbide according to claim 1 is characterized in that: described defoamer is one or more in commercially available nonyl or polyoxyethylene octylphenol ether 9, nonyl or polyoxyethylene octylphenol ether 15, op-10, tween 20, tween-80, this dish-60, the Span-80.
7. the hot pressing method for preparing of chopped carbon fiber/composite material of silicon carbide according to claim 1, it is characterized in that: described silicon carbide powder, sintering aid, binding agent, interface wetting agent, defoamer and water finish mix slurry, by 100 parts of mass fractions, wherein silicon carbide powder 27-37 part, 3～12 parts of sintering aids, 5～10 parts of binding agents, 5～10 parts of interface wetting agents, 1～5 part of defoamer, surplus is water.
8. the hot pressing method for preparing of chopped carbon fiber/composite material of silicon carbide according to claim 1 is characterized in that: the volume fraction that described step 3) contains the silk union of pre-oxygen silk in the slip of pre-oxygen silk or silk union or pre-oxygen silk and carbon fiber is 15%～50%.
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| CN104721884B (en) * | 2015-02-11 | 2017-09-22 | 深圳大学 | Bioactivity chopped carbon fiber/carborundum artificial bone and preparation method thereof |
| CN104876621B (en) * | 2015-05-07 | 2017-08-29 | 陕西科技大学 | One kind has porous composite ceramicses of biomimetic features C/SiC and preparation method thereof |
| CN106747267B (en) * | 2016-12-02 | 2019-01-08 | 航天特种材料及工艺技术研究所 | A kind of Carbon Fiber Rigid thermal insulation tile and preparation method thereof |
| CN106830963B (en) * | 2017-03-29 | 2019-12-03 | 陕西天策新材料科技有限公司 | A kind of chopped carbon fiber/composite material of silicon carbide and preparation method thereof |
| CN108249945B (en) * | 2018-01-24 | 2018-12-11 | 北京航空航天大学 | The processing method of PAN-based stabilized fiber fibre reinforced composites bearing |
| CN109987955A (en) * | 2019-04-12 | 2019-07-09 | 王小玲 | A kind of C effectively improving interfacial combined functionf/ SiC ceramic matrix composite material and preparation method |
| CN114801353B (en) * | 2022-03-31 | 2024-04-09 | 西安航空制动科技有限公司 | Pre-oxidized fiber/carbon fiber structure preform and preparation method thereof |
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Inventor after: Huang Jianfeng Inventor after: Xiong Xinbai Inventor after: Zeng Xierong Inventor after: Zeng Liyun Inventor after: Wang Yong Inventor after: Xie Shenghui Inventor after: Zou Jizhao Inventor before: Xiong Xinbai Inventor before: Huang Jianfeng Inventor before: Zeng Xierong Inventor before: Zeng Liyun Inventor before: Wang Yong Inventor before: Xie Shenghui Inventor before: Zou Jiguang |
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Free format text: CORRECT: INVENTOR; FROM: XIONG XINBAI HUANG JIANFENG CENG XIERONG CENG LIYUN WANG YONG XIE SHENGHUIZOU JIGUANG TO: HUANG JIANFENG XIONG XINBAI CENG XIERONG CENG LIYUN WANG YONG XIE SHENGHUI ZOU JIZHAO |
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