CN105967712A - Method for preparing carbon fiber reinforced silicon carbide (Csf/C-SiC) composite material - Google Patents

Method for preparing carbon fiber reinforced silicon carbide (Csf/C-SiC) composite material Download PDF

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CN105967712A
CN105967712A CN201610277281.4A CN201610277281A CN105967712A CN 105967712 A CN105967712 A CN 105967712A CN 201610277281 A CN201610277281 A CN 201610277281A CN 105967712 A CN105967712 A CN 105967712A
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carbon fiber
sic
silicon carbide
csf
powder
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李爱军
吴彪
彭雨晴
白瑞成
贾林涛
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University of Shanghai for Science and Technology
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Abstract

The invention discloses a method for preparing a carbon fiber reinforced silicon carbide (Csf/C-SiC) composite material, wherein the method comprises the steps: (1) putting a 3-30 mm short-cut carbon fiber in a dimethylsulfoxide solution, soaking for 2 h, and degumming; (2) strongly dispersing the short-cut carbon fiber to obtain a dispersed short-cut carbon fiber; (3) placing a weighed silicon carbide (SiC) powder in an organic solvent solution, adding polycarbosilane, a silicon powder, an aluminum powder and a boron powder under stirring, and mixing to obtain a suspension; (4) heating the suspension to 80 DEG C-120 DEG C, evaporating, to obtain a block mixture, grinding the mixture, and allowing to pass through a sieve with 200 mesh or less, to obtain a mixed powder; (5) pounding and mixing the dispersed short-cut carbon fiber and the mixed powder, to obtain a slurry; and (6) placing the slurry in a mold, finalizing the design, carrying out hot pressed sintering, and thus obtaining the carbon fiber reinforced silicon carbide (Csf/C-SiC) composite material. The method can improve the densification degree of high temperature performance materials in high temperature service environments.

Description

The preparation method of carbon fibre reinforced silicon carbide (Csf/C-SiC) composite
Technical field
The present invention relates to a kind of hot-pressing sintering technique and prepare the preparation method of carbon fibre reinforced silicon carbide (Csf/C-SiC) composite, particularly relate to that a kind of remaining silicon is few, high temperature friction carbon fibre reinforced silicon carbide of good performance (Csf/C-SiC) composite.
Background technology
Hot pressed sintering (Hot pressed sintering) is currently manufactured SiC and the most widely used flash sintering method of composite material engineering device thereof.But, silicon carbide ceramics has the highest imperfection sensitivity, and toughness deficiency is considered the critical defect of ceramic-like materials, and therefore its range of application is extremely limited.
At present, introducing fiber as reinforcement is to improve thyrite toughness and the effective ways of intensity.But, owing to the composite material preparation process of continuous lod is complicated, technical difficulty is big, and relatively costly.Therefore, occur in that the composite using chopped fiber as toughness reinforcing body, do agglutinant can effectively reduce sintering temperature with silicon, aluminum, boron, improve material density.But, technically there is more difficulty in chopped strand and being evenly mixed in of powder body, in Csf/C-SiC composite prepared by the hot-pressing sintering method with silicon as sintering aid, remaining silicon is higher, and this material density declines, and mechanical property the most in high temperature environments can be remarkably decreased.
Summary of the invention
The deficiency existed for prior art, the purpose of the present invention is to propose to the material preparation method of a kind of carbon fibre reinforced silicon carbide (Csf/C-SiC) composite, material prepared by the method can improve material at high temperature performance under high-temperature service environment significantly, the crystallite that Polycarbosilane cracking produces in sintering process can effectively fill matrix micropore, improves the consistency of material.
For reaching above-mentioned purpose, the present invention adopts the following technical scheme that.
A kind of preparation method preparing carbon fibre reinforced silicon carbide (Csf/C-SiC) composite with Polycarbosilane for presoma, it is characterised in that concretely comprising the following steps of the method:
(1). 3-30mm chopped carbon fiber is placed in dimethyl sulfoxide solution, soaks 2h, carry out removing glue；
(2). the chopped carbon fiber after removing glue is carried out high force dispersion, the chopped carbon fiber after being disperseed；
(3) weigh a certain amount of carborundum (SiC) powder to be placed in organic solvent solution, in this solution, add Polycarbosilane, silica flour, aluminium powder, boron powder under stirring successively, after mix homogeneously, obtain suspension；
(4). the suspension obtained in above-mentioned steps (3) is heated to 80 DEG C～120 DEG C, is evaporated, until solvent volatilizees completely, obtain block mixture, block mixture is ground, cross the sieve of below 200 mesh, obtain mixed-powder；
(5). the mixed-powder obtained in chopped carbon fiber after the dispersion that will obtain in above-mentioned steps (1) and above-mentioned steps (4) is smashed to pieces, is mixed, and obtains the mud of mix homogeneously；
(6). the mud being uniformly mixed in above-mentioned steps (5) is placed in graphite jig and carries out sizing of colding pressing, it is placed in again in vacuum hotpressing stove, in argon gas atmosphere, it is heated to 300 DEG C, again with the programming rate of 1～5 DEG C/min, pressure is that 12.4MPa. is heated to 300 DEG C～1000 DEG C, and pressure be 26.5MPa, temperature be that at 1000 DEG C～1900 DEG C, constant temperature 2～4h carries out hot pressed sintering, after sintering, it is naturally cooling to room temperature, prepares carbon fibre reinforced silicon carbide (Csf/C-SiC) composite.
Carbon fiber described in step (1) is one or more in polypropylene cyano group carbon fiber, asphalt base carbon fiber.
The volume fraction of the carbon fiber described in step (2) is 40vol%-60vol%, and after high force dispersion, staple length is 1mm-5mm.
SiC mass described in step (3) accounts for 40-50 part of carbon fibre reinforced silicon carbide composite material quality, Polycarbosilane accounts for 0-20 part of carbon fibre reinforced silicon carbide composite material quality, sintering aid accounts for 5-15 part of carbon fibre reinforced silicon carbide composite material quality, and (wherein silica flour accounts for the 65%-75% of carbon fibre reinforced silicon carbide composite material quality, aluminium powder accounts for the 20%-30% of carbon fibre reinforced silicon carbide composite material quality, and boron powder accounts for the 1%-5% of carbon fibre reinforced silicon carbide composite material quality).
Organic solvent described in step (3) is the one in normal hexane, dimethylbenzene.
The invention has the beneficial effects as follows,
Carbon fibre reinforced silicon carbide (Csf/C-SiC) composite prepared by the present invention improves material mechanical property under high-temperature service environment；The method in sintering Csf/C-SiC composite material, the free carbon that Polycarbosilane is cracked to form and remaining pasc reaction, be avoided that the remaining silicon erosion to fiber, improve material at high temperature performance；The method has liquid-phase sintering effect in Polycarbosilane presoma sintering process, and the produced crystallite of Polycarbosilane cracking can effectively be filled matrix micropore, be improved the densification degree of material.
Accompanying drawing explanation
Fig. 1 is the SEM Electronic Speculum figure of carbon fibre reinforced silicon carbide (Csf/C-SiC) composite prepared by the present invention.
Detailed description of the invention
Now the specific embodiment of the present invention is summarized in rear.
Embodiment
One prepares the preparation method of carbon fibre reinforced silicon carbide (Csf/C-SiC) composite with Polycarbosilane for presoma, and it concretely comprises the following steps:
(1). the 3-30mm chopped polyacrylonitrile-based carbon fibre of 9g is placed in dimethyl sulfoxide solution (3vol%) and soaks 2h, carry out removing glue；
(2). the chopped carbon fiber after removing glue is carried out high force dispersion, the chopped carbon fiber after being disperseed；
(3). the carborundum SiC powder weighing 16g is placed in ethanol solution, and under stirring, in this solution, add 1.6g～the Polycarbosilane of 4 g, the silica flour of 1.6g, the aluminium powder of 0.8g, the boron powder of 0.096g successively, obtain alcohol suspension after mix homogeneously；
(4). the alcohol suspension being uniformly mixed in above-mentioned steps (3) is heated to 150 DEG C of evaporations, until solvent volatilizees completely, obtains block mixture, this block mixture is ground, the sieve to 200 mesh, obtain mixed-powder；
(5). the mixed-powder obtained in chopped carbon fiber after the dispersion that will obtain in above-mentioned steps (1) and above-mentioned steps (4) is smashed to pieces, is mixed, and obtains the mud of mix homogeneously；
(6) mud being uniformly mixed in above-mentioned steps (5) is placed in graphite jig carries out sizing of colding pressing, it is placed in again in vacuum drying oven, under an argon atmosphere, it is heated to 300 DEG C, again with the programming rate of 2 DEG C/min, pressure is that 12.4MPa. is heated to 300 DEG C～1000 DEG C, and it is 26.5MPa at pressure, constant temperature 2 hours at 1000 DEG C, again with the programming rate of 5 DEG C/min, it is heated to constant temperature at 1800 DEG C and carries out hot pressed sintering in 2 hours, after sintering, it is naturally cooling to room temperature, prepare carbon fibre reinforced silicon carbide (Csf/C-SiC) composite, as shown in Figure 1.

Claims (4)

1. the preparation method of carbon fibre reinforced silicon carbide (Csf/C-SiC) composite, it is characterised in that concretely comprising the following steps of the method:
(1). 3-30mm chopped carbon fiber is placed in dimethyl sulfoxide solution, soaks 2h, carry out removing glue；
Chopped carbon fiber after removing glue is carried out high force dispersion, the chopped carbon fiber after being disperseed；
Weigh a certain amount of carborundum (SiC) powder to be placed in organic solvent solution, in this solution, add Polycarbosilane, silica flour, aluminium powder, boron powder under stirring successively, after mix homogeneously, obtain suspension；
The suspension obtained in above-mentioned steps (3) is heated to 80 DEG C～120 DEG C, is evaporated, until solvent volatilizees completely, obtain block mixture, block mixture is ground, cross the sieve of below 200 mesh, obtain mixed-powder；
The mixed-powder obtained in chopped carbon fiber after the dispersion that will obtain in above-mentioned steps (1) and above-mentioned steps (4) is smashed to pieces, is mixed, and obtains the mud of mix homogeneously；
The mud being uniformly mixed in above-mentioned steps (5) is placed in graphite jig and carries out sizing of colding pressing, it is placed in again in vacuum hotpressing stove, in argon gas atmosphere, it is heated to 300 DEG C, again with the programming rate of 1～5 DEG C/min, pressure is that 12.4MPa. is heated to 300 DEG C～1000 DEG C, and pressure be 26.5MPa, temperature be that at 1000 DEG C～1900 DEG C, constant temperature 2～4h carries out hot pressed sintering, after sintering, it is naturally cooling to room temperature, prepares carbon fibre reinforced silicon carbide (Csf/C-SiC) composite.
The preparation method of carbon fibre reinforced silicon carbide the most according to claim 1 (Csf/C-SiC) composite, it is characterized in that, the carbon fiber described in above-mentioned steps (1) is one or more in polypropylene cyano group carbon fiber, asphalt base carbon fiber.
The preparation method of carbon fibre reinforced silicon carbide the most according to claim 1 (Csf/C-SiC) composite, it is characterized in that, the volume fraction of the carbon fiber described in above-mentioned steps (2) is 40vol%-60vol%, and after high force dispersion, staple length is 1mm-5mm.
The preparation method of carbon fibre reinforced silicon carbide the most according to claim 1 (Csf/C-SiC) composite, it is characterised in that the organic solvent described in above-mentioned steps (3) is the one in normal hexane, dimethylbenzene.
CN201610277281.4A 2016-05-01 2016-05-01 Method for preparing carbon fiber reinforced silicon carbide (Csf/C-SiC) composite material Pending CN105967712A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106582521A (en) * 2016-12-17 2017-04-26 牟燕蓉 Preparation method of silicon carbide-asphalt adsorption particles
CN108101542A (en) * 2017-12-07 2018-06-01 南京航空航天大学 A kind of SiC foam and preparation method thereof
CN109437955A (en) * 2018-12-13 2019-03-08 上海康碳复合材料科技有限公司 A kind of brake material fast preparation method modified based on Polycarbosilane
RU2718682C2 (en) * 2018-09-12 2020-04-13 Федеральное государственное бюджетное учреждение науки Институт металлургии и материаловедения им. А.А. Байкова Российской академии наук (ИМЕТ РАН) Method of making ceramics based on silicon carbide, reinforced with silicon carbide fibres
CN112191725A (en) * 2020-09-29 2021-01-08 马鞍山市凯通新能源科技有限公司 Pressing process of new energy automobile battery box
CN112552063A (en) * 2020-12-25 2021-03-26 长沙三泰新材料有限公司 Preparation method of carbon fiber reinforced silicon carbide composite material

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106582521A (en) * 2016-12-17 2017-04-26 牟燕蓉 Preparation method of silicon carbide-asphalt adsorption particles
CN106582521B (en) * 2016-12-17 2019-02-05 河北亚鼎新材料科技有限公司 Silicon carbide-asphalt carbon absorption grain preparation method
CN108101542A (en) * 2017-12-07 2018-06-01 南京航空航天大学 A kind of SiC foam and preparation method thereof
RU2718682C2 (en) * 2018-09-12 2020-04-13 Федеральное государственное бюджетное учреждение науки Институт металлургии и материаловедения им. А.А. Байкова Российской академии наук (ИМЕТ РАН) Method of making ceramics based on silicon carbide, reinforced with silicon carbide fibres
CN109437955A (en) * 2018-12-13 2019-03-08 上海康碳复合材料科技有限公司 A kind of brake material fast preparation method modified based on Polycarbosilane
CN109437955B (en) * 2018-12-13 2021-06-29 上海康碳复合材料科技有限公司 Quick preparation method of brake material based on polycarbosilane modification
CN112191725A (en) * 2020-09-29 2021-01-08 马鞍山市凯通新能源科技有限公司 Pressing process of new energy automobile battery box
CN112552063A (en) * 2020-12-25 2021-03-26 长沙三泰新材料有限公司 Preparation method of carbon fiber reinforced silicon carbide composite material

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Application publication date: 20160928