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CN103204693A - Preparation method for short carbon fiber/silicon carbide composites - Google Patents

Preparation method for short carbon fiber/silicon carbide composites Download PDF

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CN103204693A
CN103204693A CN2013100771122A CN201310077112A CN103204693A CN 103204693 A CN103204693 A CN 103204693A CN 2013100771122 A CN2013100771122 A CN 2013100771122A CN 201310077112 A CN201310077112 A CN 201310077112A CN 103204693 A CN103204693 A CN 103204693A
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carbon fiber
silicon carbide
chopped carbon
sintering
composite material
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程兴旺
何旭道
王琪
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Beijing Institute of Technology BIT
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Beijing Institute of Technology BIT
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Abstract

本发明公开了一种利用放电等离子烧结（SPS）制备短切碳纤维/碳化硅复合材料的制备方法。该方法的具体步骤是：步骤1、短切碳纤维去胶粗化预处理：将短切碳纤维放于热处理炉中，在400°C条件下保温30分钟，再使用成分为硝酸、重铬酸钾、双氧水和过硫酸铵的粗化液浸泡进行粗化后用去离子水洗净烘干备用；步骤2、球磨混料：将短切碳纤维、碳化硅粉末及烧结助剂放入球磨罐进行球磨；步骤3、干燥过筛：利用旋转蒸发干燥并对混合粉末进行研磨过筛；步骤4、放电等离子（SPS）烧结：将制成粉末放入石墨模具中，利用放电等离子设备进行烧结。本发明制备的短切碳纤维/碳化硅复合材料性能良好，短切碳纤维体积含量可控。该复合材料具有高比模量、高比强度、良好韧性，有望在轻质装甲防护领域得到运用。The invention discloses a method for preparing a chopped carbon fiber/silicon carbide composite material by using spark plasma sintering (SPS). The specific steps of the method are: step 1, chopped carbon fiber degumming and coarsening pretreatment: put the chopped carbon fiber in a heat treatment furnace, keep it warm for 30 minutes at 400°C, and then use the ingredients of nitric acid and potassium dichromate , hydrogen peroxide and ammonium persulfate roughening liquid soaked for coarsening, washed with deionized water and dried for later use; step 2, ball milling mixing: put chopped carbon fiber, silicon carbide powder and sintering aid into a ball mill tank for ball milling ; Step 3, drying and sieving: use rotary evaporation to dry and grind and sieve the mixed powder; Step 4, spark plasma (SPS) sintering: put the prepared powder into a graphite mold, and use spark plasma equipment for sintering. The performance of the chopped carbon fiber/silicon carbide composite material prepared by the invention is good, and the volume content of the chopped carbon fiber is controllable. The composite material has high specific modulus, high specific strength, and good toughness, and is expected to be used in the field of lightweight armor protection.

Description

A kind of preparation method of chopped carbon fiber/composite material of silicon carbide
Technical field
The present invention relates to a kind of preparation method of chopped carbon fiber/composite material of silicon carbide, belong to the fibre reinforced composites preparation field, be specifically related to a kind of plasma discharging (SPS) sintering preparation method of chopped carbon fiber/composite material of silicon carbide.
Background technology
Carbon fiber/composite material of silicon carbide is composited by having low density, high rigidity, high strength, high temperature resistant, corrosion resistant silicon carbide ceramics and having high ratio modulus, excellent toughness and high-tensile carbon fiber, has advantages such as density is low, high specific strength, high ratio modulus.Its mechanical property can be carried out adjustment in the certain limit by the content of carbon fiber in silicon carbide substrate.It has good prospects for application in fields such as military project, space flight and aviation.
Present stage is very extensive about the research that long carbon fiber strengthens composite material of silicon carbide, but macrofiber reinforced composite complicated process of preparation, and technical difficulty is big and cost is high, makes that matrix material is difficult to find broad application.And less as the matrix material research that strengthens body about chopped carbon fiber in the open source literature report, if replace macrofiber with chopped carbon fiber, its advantage is that preparation technology is simple, and low cost of manufacture, Application Areas also enlarge day by day.
The present invention adopts chopped carbon fiber as strengthening toughened fiber, as sintering aid, uses the method for plasma discharging to prepare chopped carbon fiber/composite material of silicon carbide with aluminum oxide, yttrium oxide.The material that this method is made has high specific strength, high ratio modulus, good obdurability, and along with the fibre content variation all can be controlled.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing chopped carbon fiber/composite material of silicon carbide, the chopped carbon fiber that this method obtains/composite material of silicon carbide density height has good bending strength and fracture toughness property.
For achieving the above object, technical scheme of the present invention is: a kind of plasma discharging (SPS) sintering method for preparing chopped carbon fiber/composite material of silicon carbide is characterized in that it comprises the steps:
1) 0.5mm～3mm chopped carbon fiber is put in wherein after at first heat treatment furnace being warming up to 400 ° of C, insulation 30min takes out air cooling to room temperature.
2) use composition to carry out cleaning and dry for standby with deionized water after the alligatoring as the coarsening solution immersion 24h of nitric acid, potassium bichromate, hydrogen peroxide and ammonium persulphate.
3) press the shared mass percent of raw material: chopped carbon fiber (5%～30wt%), carborundum powder (60%～80wt%), sintering aid (10wt%) takes by weighing raw material and adds in the nylon spheroidal graphite jar, add the silicon carbide mill ball by certain ratio of grinding media to material, add dehydrated alcohol as dispersion medium, the cumulative volume of ball, material and ethanol accounts for 2/3 of ball grinder volume.
4) ball grinder sealing is placed carry out ball milling on the high energy ball mill, ball milling speed is 300r/min, time 2-4h.
5) ball milling gained uniform sizing material is rotated is put in the vacuum-drying railway carriage or compartment the dry 24h of ° C in 100 ° of C～120 after the evaporation, take out afterwards and grind, cross 100 mesh sieves, the powder that obtains mixing.
6) powder after will mixing is put into graphite jig, places and carries out sintering in the discharge plasma sintering stove.100 ° of C/min of heat-up rate, 1600 ° of C～1800 ° C of sintering temperature, soaking time 5min～15min, sintering pressure 50MPa, furnace cooling obtains chopped carbon fiber/silicon carbide (Csf/SiC) matrix material.
The described chopped carbon fiber of step 1) is the mixture of one or more arbitrary proportions in the fine carbon fiber of polypropylene, viscose-based carbon fiber, asphalt base carbon fiber or the graphite fibre, and length is 0.5mm～3mm, and Fibre diameter is 7 μ m.
Step 2) the described coarsening solution mixed solution that is nitric acid, potassium bichromate, hydrogen peroxide and ammonium persulphate.
The described silicon carbide micro-powder of step 3), median size are 0.2～0.7 μ m.
The described sintering aid of step 3) is aluminum oxide and yttrium oxide, and the mol ratio of aluminum oxide and yttrium oxide is 5:3.
The present invention has following beneficial effect:
1) carbon fiber/composite material of silicon carbide is a kind of novel composite material, but long carbon fiber strengthens composite material of silicon carbide because complicated process of preparation, cost is high and limit its extensive utilization, the present invention adopts the method for discharge plasma sintering to prepare chopped carbon fiber enhancing composite material of silicon carbide, under the prerequisite that guarantees its high-compactness, high rigidity, improved its obdurability greatly.
2) to have preparation technology simple, workable in the present invention, and preparation cost is low, and the fiber protectiveness is good, the characteristics that technological process is easy to control and safe.
Description of drawings
Figure is chopped carbon fiber behind the SPS sintering/composite material of silicon carbide SEM photo.
Embodiment
Below in conjunction with five specific embodiments, the present invention is further understood in exemplary illustration and help.But the embodiment detail only is for the present invention is described, does not represent the whole technical schemes of the present invention under conceiving, and therefore can not be interpreted as the restriction to technical solution of the present invention.Some do not depart from the unsubstantiality of the present invention's design changes, and for example simple the change or replacement of technical characterictic to have same or similar technique effect all belongs to rights protection scope of the present invention.
Embodiment 1
1, the 0.5mm chopped carbon fiber is put in wherein after at first heat treatment furnace being warming up to 400 ° of C, insulation 30min takes out air cooling to room temperature, and the coarsening solution that re-uses composition and be nitric acid, potassium bichromate, hydrogen peroxide and ammonium persulphate soaks 24h to carry out cleaning dry for standby with deionized water after the alligatoring;
2, by 100 parts of mass fractions, take by weighing 10 parts of chopped carbon fibers respectively, 80 parts of silicon carbide micro-powders, sintering aid adds in the nylon spheroidal graphite jar for 10 parts, press the 2:1 ratio of grinding media to material and add the silicon carbide mill ball, add dehydrated alcohol as dispersion medium, the cumulative volume of ball, material and ethanol accounts for 2/3 of ball grinder volume;
3, ball grinder sealing is placed carry out ball milling on the high energy ball mill, ball milling speed is 300r/min, time 2h;
4, ball milling gained uniform sizing material is rotated is put in the vacuum-drying railway carriage or compartment the dry 24h of ° C in 100 ° of C～120 after the evaporation, take out afterwards and grind, cross 100 mesh sieves, the powder that obtains mixing;
5, the powder after will mixing is put into graphite jig, places and carries out sintering in the discharge plasma sintering stove.100 ° of C/min of heat-up rate, 1600 ° of C of sintering temperature, soaking time 15min, sintering pressure 50MPa, furnace cooling obtains chopped carbon fiber/silicon carbide (Csf/SiC) matrix material.
Embodiment 2
1, the 1mm chopped carbon fiber is put in wherein after at first heat treatment furnace being warming up to 400 ° of C, insulation 30min takes out air cooling to room temperature, and the coarsening solution that re-uses composition and be nitric acid, potassium bichromate, hydrogen peroxide and ammonium persulphate soaks 24h to carry out cleaning dry for standby with deionized water after the alligatoring;
2, by 100 parts of mass fractions, take by weighing 20 parts of chopped carbon fibers respectively, 70 parts of silicon carbide micro-powders, sintering aid adds in the nylon spheroidal graphite jar for 10 parts, press the 3:1 ratio of grinding media to material and add the silicon carbide mill ball, add dehydrated alcohol as dispersion medium, the cumulative volume of ball, material and ethanol accounts for 2/3 of ball grinder volume;
3, ball grinder sealing is placed carry out ball milling on the high energy ball mill, ball milling speed is 300r/min, time 2h;
4, ball milling gained uniform sizing material is rotated is put in the vacuum-drying railway carriage or compartment the dry 24h of ° C in 100 ° of C～120 after the evaporation, take out afterwards and grind, cross 100 mesh sieves, the powder that obtains mixing;
5, the powder after will mixing is put into graphite jig, places and carries out sintering in the discharge plasma sintering stove.100 ° of C/min of heat-up rate, 1700 ° of C of sintering temperature, soaking time 10min, sintering pressure 50MPa, furnace cooling obtains chopped carbon fiber/silicon carbide (Csf/SiC) matrix material.
Embodiment 3
1, the 2mm chopped carbon fiber is put in wherein after at first heat treatment furnace being warming up to 400 ° of C, insulation 30min takes out air cooling to room temperature, and the coarsening solution that re-uses composition and be nitric acid, potassium bichromate, hydrogen peroxide and ammonium persulphate soaks 24h to carry out cleaning dry for standby with deionized water after the alligatoring;
2, by 100 parts of mass fractions, take by weighing 30 parts of chopped carbon fibers respectively, 60 parts of silicon carbide micro-powders, sintering aid adds in the nylon spheroidal graphite jar for 10 parts, press the 4:1 ratio of grinding media to material and add the silicon carbide mill ball, add dehydrated alcohol as dispersion medium, the cumulative volume of ball, material and ethanol accounts for 2/3 of ball grinder volume;
3, ball grinder sealing is placed carry out ball milling on the high energy ball mill, ball milling speed is 300r/min, time 4h;
4, ball milling gained uniform sizing material is rotated is put in the vacuum-drying railway carriage or compartment the dry 24h of ° C in 100 ° of C～120 after the evaporation, take out afterwards and grind, cross 100 mesh sieves, the powder that obtains mixing;
5, the powder after will mixing is put into graphite jig, places and carries out sintering in the discharge plasma sintering stove.100 ° of C/min of heat-up rate, 1800 ° of C of sintering temperature, soaking time 5min, sintering pressure 50MPa, furnace cooling obtains chopped carbon fiber/silicon carbide (Csf/SiC) matrix material.
Embodiment 4
1, the 0.5mm chopped carbon fiber is put in wherein after at first heat treatment furnace being warming up to 400 ° of C, insulation 30min takes out air cooling to room temperature, and the coarsening solution that re-uses composition and be nitric acid, potassium bichromate, hydrogen peroxide and ammonium persulphate soaks 24h to carry out cleaning dry for standby with deionized water after the alligatoring;
2, by 100 parts of mass fractions, take by weighing 20 parts of chopped carbon fibers respectively, 70 parts of silicon carbide micro-powders, sintering aid adds in the nylon spheroidal graphite jar for 10 parts, press the 2:1 ratio of grinding media to material and add the silicon carbide mill ball, add dehydrated alcohol as dispersion medium, the cumulative volume of ball, material and ethanol accounts for 2/3 of ball grinder volume;
3, ball grinder sealing is placed carry out ball milling on the high energy ball mill, ball milling speed is 300r/min, time 2h;
4, ball milling gained uniform sizing material is rotated is put in the vacuum-drying railway carriage or compartment the dry 24h of ° C in 100 ° of C～120 after the evaporation, take out afterwards and grind, cross 100 mesh sieves, the powder that obtains mixing;
5, the powder after will mixing is put into graphite jig, places and carries out sintering in the discharge plasma sintering stove.100 ° of C/min of heat-up rate, 1800 ° of C of sintering temperature, soaking time 10min, sintering pressure 50MPa, furnace cooling obtains chopped carbon fiber/silicon carbide (Csf/SiC) matrix material.

Claims (5)

1.一种短切碳纤维/碳化硅复合材料的制备方法，其特征在于包括如下步骤：1. a preparation method of chopped carbon fiber/silicon carbide composite material, is characterized in that comprising the steps: 1）首先将热处理炉升温至400°C后将0.5mm～3mm短切碳纤维放于其中，保温30min取出空冷至室温。1) First heat the heat treatment furnace to 400°C, then put 0.5mm~3mm chopped carbon fibers in it, keep it warm for 30min, take it out and cool it to room temperature. 2）使用成分为硝酸、重铬酸钾、双氧水和过硫酸铵的粗化液浸泡24h进行粗化后用去离子水洗净并烘干备用。2) Soak in a roughening solution consisting of nitric acid, potassium dichromate, hydrogen peroxide and ammonium persulfate for 24 hours for roughening, then wash with deionized water and dry for later use. 3）按原料所占的质量百分数：短切碳纤维（5%～30wt%），碳化硅粉（60%～85wt%），烧结助剂（10wt%）称取加入尼龙球墨罐中，按一定球料比加入碳化硅研磨球，加入无水乙醇作为分散介质，球、料和乙醇的总体积占球磨罐体积的2/3。3) According to the mass percentage of raw materials: chopped carbon fiber (5% ~ 30wt%), silicon carbide powder (60% ~ 85wt%), sintering aid (10wt%) weighed into the nylon ball ink tank, press a certain ball Material ratio Add silicon carbide grinding balls, add absolute ethanol as a dispersion medium, the total volume of balls, materials and ethanol accounts for 2/3 of the volume of the ball mill tank. 4）将球磨罐密封置于高能球磨机上进行球磨，球磨速度为300r/min，时间2-4h。4) Seal the ball mill jar and place it on a high-energy ball mill for ball milling at a speed of 300r/min for 2-4 hours. 5）将球磨所得均匀浆料进行旋转蒸发后放于真空干燥厢中于100°C～120°C干燥24h，之后取出进行研磨，过100目筛，得到混合均匀的粉末。5) The uniform slurry obtained by the ball mill is subjected to rotary evaporation, and then placed in a vacuum drying chamber to dry at 100°C to 120°C for 24 hours, then taken out for grinding, and passed through a 100-mesh sieve to obtain a uniformly mixed powder. 6）将混合均匀后的粉末放入石墨模具中，置于放电等离子烧结炉内进行烧结。升温速度100°C/min，烧结温度1600°C～1800°C，保温时间5min～15min，烧结压力50MPa，随炉冷却，得到短切碳纤维/碳化硅（Csf/SiC）复合材料。6) Put the uniformly mixed powder into a graphite mold and place it in a spark plasma sintering furnace for sintering. The heating rate is 100°C/min, the sintering temperature is 1600°C-1800°C, the holding time is 5min-15min, the sintering pressure is 50MPa, and the furnace is cooled to obtain chopped carbon fiber/silicon carbide (Csf/SiC) composite material. 2.根据权利要求1所述的一种短切短切碳纤维/碳化硅复合材料的制备方法，其特征在于：步骤1）所述的短切碳纤维为聚丙烯晴碳纤维、粘胶基碳纤维、沥青基碳纤维或石墨纤维中的一种或几种任意比例的混合物，长度为0.5mm～2mm，纤维直径为7μm。2. A method for preparing chopped carbon fiber/silicon carbide composite material according to claim 1, characterized in that: the chopped carbon fiber in step 1) is polyacrylonitrile carbon fiber, viscose-based carbon fiber, pitch One or several mixtures in any proportion of carbon fiber or graphite fiber, the length is 0.5mm-2mm, and the fiber diameter is 7μm. 3.根据权利要求1所述的一种短切短切碳纤维/碳化硅复合材料的制备方法，其特征在于：步骤2）所述的粗化液为硝酸、重铬酸钾、双氧水和过硫酸铵的混合液。3. A method for preparing chopped carbon fiber/silicon carbide composite material according to claim 1, characterized in that: the roughening solution in step 2) is nitric acid, potassium dichromate, hydrogen peroxide and persulfuric acid ammonium mixture. 4.根据权利要求1所述的一种短切短切碳纤维/碳化硅复合材料的制备方法，其特征在于：步骤3）所述的碳化硅微粉，平均粒径为0.5～0.7μm。4. The method for preparing chopped carbon fiber/silicon carbide composite material according to claim 1, characterized in that the silicon carbide micropowder in step 3) has an average particle size of 0.5-0.7 μm. 5.根据权利要求1所述的一种短切短切碳纤维/碳化硅复合材料的制备方法，其特征在于：步骤3）所述的烧结助剂为氧化铝和氧化钇，氧化铝与氧化钇的摩尔比为5:3。5. A method for preparing chopped carbon fiber/silicon carbide composite material according to claim 1, characterized in that: the sintering aid in step 3) is alumina and yttrium oxide, and alumina and yttrium oxide The molar ratio is 5:3.
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CN105350294B (en) * 2015-10-29 2018-04-03 燕山大学 A kind of chopped carbon fiber of applying silicon carbide layer and preparation method thereof
CN105350294A (en) * 2015-10-29 2016-02-24 燕山大学 Silicon carbide layer coated short carbon fiber and preparation method thereof
CN105967712A (en) * 2016-05-01 2016-09-28 上海大学 Method for preparing carbon fiber reinforced silicon carbide (Csf/C-SiC) composite material
CN106810285A (en) * 2017-01-14 2017-06-09 中国矿业大学(北京) A kind of preparation method of the carbon fiber-reinforced aluminium oxide ceramics of in-situ preparation
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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
CN108118524A (en) * 2017-12-08 2018-06-05 北京科技大学 A kind of preparation of coaxial configuration absorbing material and performance regulation and control method
CN110372407A (en) * 2019-07-20 2019-10-25 肖建堤 A kind of preparation method of rail traffic brake disc Cf-SiC composite material
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CN112760643A (en) * 2020-11-11 2021-05-07 健康力（北京）医疗科技有限公司 Composite heat-insulating coating for CT bulb tube liquid metal bearing and preparation method thereof
CN112760643B (en) * 2020-11-11 2022-07-05 健康力（北京）医疗科技有限公司 Composite heat insulation coating for CT bulb tube liquid metal bearing and preparation method thereof
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CN116143549A (en) * 2023-02-14 2023-05-23 福建立亚新材有限公司 Repair method for local damage and microcrack of small and medium-sized SiCf/SiC composite material
CN116143549B (en) * 2023-02-14 2024-05-10 福建立亚新材有限公司 Repair method for local damage and microcrack of small and medium-sized SiCf/SiC composite material
CN116924810A (en) * 2023-07-21 2023-10-24 中原工学院 Method for preparing fiber-toughened silicon carbide ceramic valve element by liquid phase sintering and compression molding
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Application publication date: 20130717