CN103204693A - Preparation method for short carbon fiber/silicon carbide composites - Google Patents
Preparation method for short carbon fiber/silicon carbide composites Download PDFInfo
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Abstract
The invention discloses a preparation method for short carbon fiber/silicon carbide composites by means of spark plasma sintering (SPS). The preparation method includes the steps: (1), pre-treating the short carbon fiber by placing the same in a heat-treatment furnace for heat preservation for 30 minutes under the temperature of 400 DEG C prior to soaking and coarsening the short carbon fibers in coarsening liquid composed of nitric acid, potassium dichromate, hydrogen peroxide and ammonium persulfate to be washed with deionized water and dried for standby; (2), placing the short carbon fiber, silicon carbide powder and sintering aids in a ball-milling pot to be ball-milled; (3), drying the materials in the step (2) through rotary evaporation prior to grinding the same to sieve the mixed powder; and (4), placing the mixed powder into a graphite mould and subjecting the mixed powder to the spark plasma sintering. The short carbon fiber/silicon carbide composites prepared by the method are good in performance, and volume content of the short carbon fibers can be controllable; and the short carbon fiber/silicon carbide composites have high specific modulus, high specific strength and excellent toughness, and can hopefully be applied to light weight armor field.
Description
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. the preparation method of a chopped carbon fiber/composite material of silicon carbide is characterized in that comprising 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%～85wt%), sintering aid (10wt%) takes by weighing 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.
2. a kind of weak point according to claim 1 preparation method of prescinding carbon fiber/composite material of silicon carbide, it is characterized in that: 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, length is 0.5mm～2mm, and Fibre diameter is 7 μ m.
3. a kind of weak point according to claim 1 preparation method of prescinding carbon fiber/composite material of silicon carbide is characterized in that: step 2) described coarsening solution is the mixed solution of nitric acid, potassium bichromate, hydrogen peroxide and ammonium persulphate.
4. a kind of weak point according to claim 1 preparation method of prescinding carbon fiber/composite material of silicon carbide, it is characterized in that: the described silicon carbide micro-powder of step 3), median size are 0.5～0.7 μ m.
5. a kind of weak point according to claim 1 preparation method of prescinding carbon fiber/composite material of silicon carbide, it is characterized in that: the described sintering aid of step 3) is aluminum oxide and yttrium oxide, the mol ratio of aluminum oxide and yttrium oxide is 5:3.
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| CN103922775A (en) * | 2014-04-01 | 2014-07-16 | 天地科技股份有限公司唐山分公司 | Hydrocyclone wear-resistant ceramic liner and preparation method thereof |
| CN104370562A (en) * | 2014-10-14 | 2015-02-25 | 荣成复合材料有限公司 | Carbon ceramic composite material and anti-explosion plate manufactured therefrom |
| CN104478459A (en) * | 2014-12-02 | 2015-04-01 | 荣成复合材料有限公司 | Carbon-ceramic composite material |
| CN104671790A (en) * | 2015-01-28 | 2015-06-03 | 安徽省和翰光电科技有限公司 | Silicon carbide ceramic for armor, and preparation method |
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Application publication date: 20130717 |