CN106810285A - A kind of preparation method of the carbon fiber-reinforced aluminium oxide ceramics of in-situ preparation - Google Patents

A kind of preparation method of the carbon fiber-reinforced aluminium oxide ceramics of in-situ preparation Download PDF

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CN106810285A
CN106810285A CN201710026768.XA CN201710026768A CN106810285A CN 106810285 A CN106810285 A CN 106810285A CN 201710026768 A CN201710026768 A CN 201710026768A CN 106810285 A CN106810285 A CN 106810285A
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sintering
temperature
carbon fiber
preparation
aluminium oxide
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陈华辉
范磊
马峰
曹晶晶
高占峰
赵赋
赵红超
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China University of Mining and Technology CUMT
China University of Mining and Technology Beijing CUMTB
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China University of Mining and Technology Beijing CUMTB
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    • C04B35/803
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64Burning or sintering processes
    • C04B35/645Pressure sintering
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52Constituents or additives characterised by their shapes
    • C04B2235/5208Fibers
    • C04B2235/5216Inorganic
    • C04B2235/524Non-oxidic, e.g. borides, carbides, silicides or nitrides
    • C04B2235/5248Carbon, e.g. graphite

Abstract

The invention provides a kind of preparation method of the carbon fiber-reinforced aluminium oxide ceramics of in-situ preparation, including:Pre-oxidized polyacrylonitrile fiber is mixed with sintering aid powder, so that the adsorption of the pre-oxidized polyacrylonitrile fiber has the sintering aid powder;The pre-oxidized polyacrylonitrile fiber, high-purity alpha-alumina and abrading-ball that adsorption has the sintering aid powder are placed in ball grinder, and carry out ball milling to obtain target mixture;The target mixture is placed in carries out pre-molding in specified mould;The described specified mould that will be equipped with the target mixture is placed in hot pressed sintering is carried out in vacuum sintering funace, to obtain the carbon fiber-reinforced alumina ceramic-base composites of in-situ preparation.

Description

A kind of preparation method of the carbon fiber-reinforced aluminium oxide ceramics of in-situ preparation
Technical field
The present invention relates to technical field of composite materials, in particular to a kind of carbon fiber-reinforced aluminum oxide of in-situ preparation The preparation method of ceramics.
Background technology
Alumina ceramic material is the purposes most maximum ceramic new material of wide, volume of production and marketing, its tool in current oxide ceramics There is high mechanical strength, insulaion resistance is big, and hardness is high, wear-resistant, corrosion-resistant, and high temperature resistant and antioxygenic property are good, and density is small etc. The advantage that metal material hardly matches.But the fracture toughness of aluminium oxide ceramics is very low, generally only 3~4MPam1/2.This Greatly limit performance and the broader applications of aluminium oxide ceramics premium properties, therefore aluminum oxide toughness reinforcing is into ceramic research field Key issue.
In order to improve the toughness of aluminium oxide ceramics, people employ particulate reinforcement, whisker, fiber reinforced, transformation toughening, from The methods such as toughness reinforcing.In above-mentioned method for toughening, particulate reinforcement low cost, but toughening effect is limited, and nanometer toughness reinforcing is then relatively costly, outward Plus crystal whisker toughened be also gradually abandoned because whisker is harmful to the person.It is preferable that self toughening can obtain toughness to a certain extent Aluminium oxide ceramics, because the brilliant generation of rod increases the porosity of matrix, and then has influence on the anti-wear performance of material.ZrO2Phase transformation Toughening mechanisms are more sensitive to temperature, under medium and high temperature, t-ZrO2Stability with temperature raise increase, transformation toughening lose Effect, causes intensity and toughness drastically to decline, and this defect limits application of such material under high temperature environment.It is fiber reinforced Method toughening effect substantially, is more and more valued by people.
Due to itself excellent mechanical property, they can crack deflection, crackle bridge joint and spike protein gene to carbon fiber Etc. playing significant toughening effect.Room temperature and high-temperature bending strength and fracture by carbon fiber-reinforced ceramic composite is tough Property, thermal shock resistance, anti-wear performance and croop property are obtained for different degrees of raising and improvement.But it is up to the present, big absolutely Partial carbon fiber-reinforced ceramics are all utilized in directly adding high-strength carbon fiber in ceramic matrix and carry out toughened ceramic material.This The method for planting directly addition carbon fiber has the following disadvantages:
1) carbon fiber impact resistance is poor, is afraid of " discounting " and " zig zag ", the carbon in the compound preparation process of composite Fiber is easily damaged fracture, and then influences the performance of composite;
Although 2) carbon fiber excellent performance, price is too high;
3) interface cohesion between additional carbon fiber and matrices of composite material is poor.
The content of the invention
The present invention is based at least one above-mentioned technical problem, it is proposed that a kind of carbon fiber-reinforced oxygen of new in-situ preparation Change the preparation scheme of aluminium ceramics, the alumina ceramic-base composites that carbon fiber is well combined with ceramic matrix can be prepared, Realize parameter controllable, and process is simple, preoxidized polyacrylonitrile pioneer fiber is in sintering in prepared ceramic matric composite During successful conversion be carbon fiber, solve the Carbon Fiber Damage for being directly added into carbon fiber and causing, reduce composite Production cost, for alumina ceramic-base composites prepare provide a kind of new way.
In consideration of it, the present invention proposes a kind of preparation method of the carbon fiber-reinforced aluminium oxide ceramics of in-situ preparation, including:Will Pre-oxidized polyacrylonitrile fiber is mixed with sintering aid powder, so that the adsorption of the pre-oxidized polyacrylonitrile fiber There is the sintering aid powder;Adsorption there is into the pre-oxidized polyacrylonitrile fiber of the sintering aid powder, high-purity Degree aluminum oxide and abrading-ball are placed in ball grinder, and carry out ball milling to obtain target mixture;The target mixture is placed in Pre-molding is carried out in specified mould;The described specified mould that will be equipped with the target mixture is placed in vacuum sintering funace Hot pressed sintering is carried out, to obtain the carbon fiber-reinforced alumina ceramic-base composites of in-situ preparation.
In the technical scheme, mixed with sintering aid powder by by pre-oxidized polyacrylonitrile fiber, so that poly- The adsorption of acrylonitrile pre-oxidized fibers has sintering aid powder, and adsorption is had the polyacrylonitrile of sintering aid powder Pre-oxidized fibers, high-purity alpha-alumina and abrading-ball are carried out being mixed to get target mixture, and target mixture is sintered, The sintering characteristic of hot physical property, phase structure and the aluminum oxide of pre-oxidized polyacrylonitrile fiber is combined, polyacrylonitrile can be made pre- Oxidized fibre generation cyclisation, cross-linking reaction, are allowed to be eventually converted into carbonation rate carbon fiber higher, obtain carbon fiber in situ and height The good composite of Purity Alumina interface cohesion, while the preparation of carbon fiber is closed into two with the preparation technology of composite being One, the problem of finished product carbon fiber easy damaged fracture in batch mixing preparation process is not only overcome, and simplify the life of composite Flow is produced, the production cost of composite is reduced, the energy has been saved.
In the above-mentioned technical solutions, it is preferable that the described specified mould that will be equipped with the target mixture is placed in Vacuum Heat The step of carrying out hot pressed sintering in pressure sintering furnace, specifically includes:The vacuum sintering furnace is controlled using multiple difference sintering stages Hot pressed sintering is carried out to the target mixture.
In the technical scheme, hot pressed sintering is carried out to target mixture by multiple difference sintering stages, it is ensured that target Each constituent element in mixture can be combined preferably.
In any of the above-described technical scheme, it is preferable that the control vacuum sintering furnace is using multiple difference sintering stages The step of being sintered to the target mixture, specifically includes:In sintering process, the vacuum sintering funace is controlled Sintering temperature rises to the first temperature from room temperature, and heating rate is first rate, and first temperature is reached in the sintering temperature When, the first duration is persistently incubated, when the sintering temperature rises to second temperature from first temperature, heating rate is second Speed, when the sintering temperature reaches the second temperature, is persistently incubated the second duration, in the sintering temperature from described the Two temperature rise to target temperature, and heating rate is third speed, when the target temperature is reached, persistently after the 3rd duration of insulation, It is cooled to room temperature.
In any of the above-described technical scheme, it is preferable that first temperature is 440 DEG C, the second temperature is 1070 DEG C, the first rate be 8~10 DEG C/min, second speed be 8~10 DEG C/min, the third speed be 5~8 DEG C/ Min, a length of 5~15min when described first, a length of 5~15min, a length of 60~120min when the described 3rd when described second.Institute Target temperature is stated for 1600-1700 DEG C.
In any of the above-described technical scheme, it is preferable that also include:In sintering process, the vacuum sintering furnace is controlled The target mixture is pressurizeed using uniform step pressuring method.
In the technical scheme, uniform pressuring method can increase the consistency of composite, reduce composite and exist Defect in preparation process.
In any of the above-described technical scheme, it is preferable that the duration for carrying out ball milling is 1~10min.
In any of the above-described technical scheme, it is preferable that the ratio of the pre-oxidized polyacrylonitrile fiber be 5~30%, The ratio of the sintering aid powder is 1~30%, and the ratio of the high-purity alpha-alumina is 65~89%.
By above technical scheme, can be multiple to the alumina ceramic-base for preparing carbon fiber with ceramic matrix is well combined Condensation material, it is controllable to realize parameter, and process is simple, preoxidized polyacrylonitrile pioneer fiber in prepared ceramic matric composite Successful conversion is carbon fiber, aluminium oxide ceramics toughness is improved largely, and solves the carbon for being directly added into carbon fiber and causing Fibre damage, reduces the production cost of composite, and a kind of new way is provided for prepared by alumina ceramic-base composites.
Brief description of the drawings
Fig. 1 shows the preparation method of the carbon fiber-reinforced aluminium oxide ceramics of in-situ preparation according to an embodiment of the invention;
Fig. 2 shows the scanning of the carbon fiber-reinforced aluminium oxide ceramics of in-situ preparation according to first embodiment of the invention Electron microscope;
Fig. 3 shows the scanning of the carbon fiber-reinforced aluminium oxide ceramics of in-situ preparation of second embodiment of the invention Electron microscope;
Fig. 4 shows the scanning of the carbon fiber-reinforced aluminium oxide ceramics of in-situ preparation of the 3rd embodiment of the invention Electron microscope;
Fig. 5 show the fracture toughness of the carbon fiber-reinforced aluminium oxide ceramics of in-situ preparation according to an embodiment of the invention with The situation of change figure line of fiber content;
Fig. 6 shows the carbon fiber that pioneer's fiber is formed after sintering in composite according to embodiments of the present invention (002) face diffraction image.
Fig. 7 is the atomic lens of the carbon fiber formed after sintering, and shows that pioneer's fiber forms carbon fiber, carbon in the carbonized Layer crystal interplanar distance is 0.3455nm.
Specific embodiment
It is below in conjunction with the accompanying drawings and specific real in order to be more clearly understood that the above objects, features and advantages of the present invention Mode is applied to be further described in detail the present invention.It should be noted that in the case where not conflicting, the implementation of the application Feature in example and embodiment can be mutually combined.
Many details are elaborated in the following description in order to fully understand the present invention, but, the present invention may be used also Implemented with being different from other modes described here using other, therefore, protection scope of the present invention is not by described below Specific embodiment limitation.
Fig. 1 shows the preparation method of the carbon fiber-reinforced aluminium oxide ceramics of in-situ preparation according to an embodiment of the invention.
As shown in figure 1, the preparation method of the carbon fiber-reinforced aluminium oxide ceramics of in-situ preparation according to an embodiment of the invention, Including:
Step 102, pre-oxidized polyacrylonitrile fiber is mixed with sintering aid powder, so that the polyacrylonitrile is pre- The adsorption of oxidized fibre has the sintering aid powder SiO2-MgO-CaO;
Step 104, the pre-oxidized polyacrylonitrile fiber, the high purity oxygen that adsorption is had the sintering aid powder Change aluminium and abrading-ball is placed in ball grinder, and carry out ball milling to obtain target mixture;
Step 106, the target mixture is placed in carries out pre-molding in specified mould;
Step 108, the described specified mould that will be equipped with the target mixture is placed in heat is carried out in vacuum sintering funace Pressure sintering, to obtain the carbon fiber-reinforced alumina ceramic-base composites of in-situ preparation.
In the technical scheme, mixed with sintering aid powder by by pre-oxidized polyacrylonitrile fiber, so that poly- The adsorption of acrylonitrile pre-oxidized fibers has sintering aid powder, and adsorption is had the polyacrylonitrile of sintering aid powder Pre-oxidized fibers, high-purity alpha-alumina and abrading-ball are carried out being mixed to get target mixture, and target mixture is sintered, The sintering characteristic of hot physical property, phase structure and the aluminum oxide of pre-oxidized polyacrylonitrile fiber is combined, polyacrylonitrile can be made pre- Oxidized fibre generation cyclisation, cross-linking reaction, are allowed to be eventually converted into carbonation rate carbon fiber higher, obtain carbon fiber in situ and height The good composite of Purity Alumina interface cohesion, while the preparation of carbon fiber is closed into two with the preparation technology of composite being One, the problem of finished product carbon fiber easy damaged fracture in batch mixing preparation process is not only overcome, and simplify the life of composite Flow is produced, the production cost of composite is reduced, the energy has been saved.
In the above-mentioned technical solutions, it is preferable that the described specified mould that will be equipped with the target mixture is placed in Vacuum Heat The step of being sintered in pressure sintering furnace, specifically includes:Control the vacuum sintering furnace using multiple difference sintering stages to institute Stating target mixture carries out hot pressed sintering.
In the technical scheme, target mixture is sintered by multiple difference sintering stages, it is ensured that target mixes Each constituent element in thing can be combined preferably.
In any of the above-described technical scheme, it is preferable that the control vacuum sintering furnace is using multiple difference sintering stages The step of being sintered to the target mixture, specifically includes:In sintering process, the vacuum sintering funace is controlled Sintering temperature rises to the first temperature from room temperature, and heating rate is first rate, and first temperature is reached in the sintering temperature When, the first duration is persistently incubated, when the sintering temperature rises to second temperature from first temperature, heating rate is second Speed, when the sintering temperature reaches the second temperature, is persistently incubated the second duration, in the sintering temperature from described the Two temperature rise to target temperature, and heating rate is third speed, when the target temperature is reached, persistently after the 3rd duration of insulation, It is cooled to room temperature.
In any of the above-described technical scheme, it is preferable that first temperature is 440 DEG C, the second temperature is 1070 DEG C, the first rate be 8~10 DEG C/min, second speed be 8~10 DEG C/min, the third speed be 5~8 DEG C/ Min, a length of 5~15min when described first, a length of 5~15min, a length of 60~120min when the described 3rd when described second.Institute Target temperature is stated for 1600-1700 DEG C.
In any of the above-described technical scheme, it is preferable that also include:In sintering process, the vacuum sintering furnace is controlled The target mixture is pressurizeed using uniform step pressuring method.
In the technical scheme, uniform pressuring method can increase the consistency of composite, reduce composite and exist Defect in preparation process.
In any of the above-described technical scheme, it is preferable that the duration for carrying out ball milling is 1~10min.
In any of the above-described technical scheme, it is preferable that the ratio of the pre-oxidized polyacrylonitrile fiber be 5~30%, The ratio of the sintering aid powder is 1~30%, and the ratio of the high-purity alpha-alumina is 65~89%.
Technical scheme is further described below in conjunction with Fig. 2 to Fig. 7.
Embodiment one:
Initial feed 9.51g Al2O3 and 0.4156g polyacrylonitrile (PAN) pre-oxidized fibers are weighed to be fitted into ball grinder, With the aluminum oxide abrading-ball that purity is 99%, the blending agent (alcohol/glycerine is 3/1) of addition 50ml alcohol and glycerine is high Wet ball grinding can be carried out in ball mill 1 hour.It is 99% alumina ceramic crucible that mixture after high-energy ball milling is loaded into purity In, well mixed powder is dried to obtain in 75 DEG C of baking ovens.The powder of acquisition be fitted into ready graphite jig carry out it is pre- , then be fitted into graphite jig in vacuum sintering funace by pressing formation.Sintered 2 hours in 1700 DEG C under vacuum;Maximum sintering pressure Power is 40MPa, and pressuring method pressurizes for step;Respectively at 400 DEG C, 600 DEG C, 900 DEG C, 1400 DEG C of insulations in another sintering process 30 minutes.Obtain the alumina ceramic-base composites that pioneer's fiber volume fraction is 10%, its heterogeneous microstructure such as Fig. 2 institutes Show, as can be known from Fig. 2, prepared Fiber In Composite Material is uniformly distributed in matrix (i.e. high-purity alpha-alumina), can from Fig. 5 Know that alumina ceramic-base composites fracture toughness improves 70% or so with respect to the fracture toughness of pure alumina.
Embodiment two:
Weigh initial feed 8.5g Al2O3 and 0.6g PAN pre-oxidized fibers to be fitted into ball grinder, be 99% with purity The blending agent (alcohol/glycerine is 3/1) of aluminum oxide abrading-ball, addition 50ml alcohol and glycerine, is carried out in high energy ball mill Wet ball grinding 1 hour.Mixture after high-energy ball milling is fitted into purity in 99% alumina ceramic crucible, in 75 DEG C of baking ovens It is dried to obtain well mixed powder.The powder of acquisition carries out pre-compaction forming in being fitted into ready graphite jig, then by stone Black mould is fitted into vacuum sintering funace.Sintered 2 hours in 1700 DEG C under vacuum;Maximum sintering pressure is 40MPa, pressurization side Formula is pressurizeed for step;In another sintering process 30 minutes are incubated respectively at 400 DEG C, 600 DEG C, 900 DEG C, 1400 DEG C.Obtain pioneer Fiber volume fraction is 15% alumina ceramic-base composites, and its typical fractography pattern is as shown in figure 3, carbon fiber Be well combined with aluminium oxide ceramics matrix, section part have obvious fibre debonding and extract phenomenon, can be apparent from from Fig. 5 with The increase of fiber content, the fracture toughness of composite is significantly increased.
Embodiment three
Weigh initial feed 8.55g Al2O3 and 0.7556g PAN pre-oxidized fibers to be fitted into ball grinder, be with purity The blending agent (alcohol/glycerine is 2/1) of 99% aluminum oxide abrading-ball, addition 50ml alcohol and glycerine, high energy ball mill In carry out wet ball grinding 2 hours.Mixture after high-energy ball milling is fitted into purity in 99% alumina ceramic crucible, in 75 DEG C Well mixed powder is dried to obtain in baking oven.The powder of acquisition carries out pre-compaction forming in being fitted into ready graphite jig, so Graphite jig is fitted into vacuum sintering funace afterwards.Sintered 2 hours in 1700 DEG C under vacuum;Maximum sintering pressure is 40MPa, Pressuring method pressurizes for step;In another sintering process 30 minutes are incubated respectively at 400 DEG C, 600 DEG C, 900 DEG C, 1400 DEG C. To the alumina ceramic-base composites that pioneer's fiber volume fraction is 20%, its carbon fiber surface EDS maps is as shown in figure 4, from figure Understood in 4, with the gradually increase of carbon fiber content, the carbon fiber uniformity in the base is gradually reduced, can be by changing material The mixing procedure of material is solved.
Fig. 6 is carbon atom face (002) diffraction after prepared pioneer's fiber (i.e. pre-oxidized polyacrylonitrile fiber) conversion Image.
Fig. 7 is the atomic lens of the carbon fiber formed after sintering, and shows that pioneer's fiber forms carbon fiber, carbon in the carbonized Layer crystal interplanar distance is 0.3455nm.
Technical scheme is described in detail above in association with accompanying drawing, technical scheme proposes a kind of new The preparation scheme of the carbon fiber-reinforced aluminium oxide ceramics of in-situ preparation, can give and prepare what carbon fiber and ceramic matrix were well combined Alumina ceramic-base composites, it is controllable to realize parameter, and process is simple, polyacrylonitrile in prepared ceramic matric composite Pre-oxidation pioneer's fiber successful conversion is carbon fiber, solves the Carbon Fiber Damage fracture for being directly added into carbon fiber and causing, drop The low production cost of composite, makes aluminium oxide ceramics toughness be improved largely, and is alumina ceramic-base composites system It is standby to provide a kind of new way.
The preferred embodiments of the present invention are the foregoing is only, is not intended to limit the invention, for the skill of this area For art personnel, the present invention can have various modifications and variations.It is all within the spirit and principles in the present invention, made any repair Change, equivalent, improvement etc., should be included within the scope of the present invention.

Claims (7)

1. the preparation method of the carbon fiber-reinforced aluminium oxide ceramics of a kind of in-situ preparation, it is characterised in that including:
Pre-oxidized polyacrylonitrile fiber is mixed with sintering aid powder, so that the table of the pre-oxidized polyacrylonitrile fiber Face is adsorbed with the sintering aid powder;
Adsorption is had the pre-oxidized polyacrylonitrile fiber, high-purity alpha-alumina and the abrading-ball of the sintering aid powder It is placed in ball grinder, and carries out ball milling to obtain target mixture;
The target mixture is placed in carries out pre-molding in specified mould;
The described specified mould that will be equipped with the target mixture is placed in vacuum sintering funace and is sintered, to obtain original position Generation reinforced alumina ceramic-base composites.
2. the preparation method of the carbon fiber-reinforced aluminium oxide ceramics of in-situ preparation according to claim 1, it is characterised in that will Described specified mould equipped with the target mixture is placed in the step of being sintered in vacuum sintering funace, specifically includes:
The vacuum sintering furnace is controlled to be sintered to the target mixture using multiple difference sintering stages.
3. the preparation method of the carbon fiber-reinforced aluminium oxide ceramics of in-situ preparation according to claim 2, it is characterised in that control The step of making the vacuum sintering furnace target mixture is sintered using multiple difference sintering stages, specifically include:
In sintering process, the sintering temperature of the vacuum sintering funace is controlled to rise to the first temperature, heating rate from room temperature Be first rate, the sintering temperature reach first temperature when, be persistently incubated the first duration, the sintering temperature from When first temperature rises to second temperature, heating rate is the second speed, when the sintering temperature reaches the second temperature When, the second duration is persistently incubated, target temperature is risen to from the second temperature in the sintering temperature, heating rate is the 3rd speed Rate, when the target temperature is reached, after being persistently incubated the 3rd duration, is cooled to room temperature.
4. the preparation method of the carbon fiber-reinforced aluminium oxide ceramics of in-situ preparation according to claim 3, it is characterised in that institute It is 440 DEG C to state the first temperature, and the second temperature is 1070 DEG C, and the first rate is 8~10 DEG C/min, second speed It is 8~10 DEG C/min, the third speed is 5~8 DEG C/min, a length of 5~15min when described first, a length of 5 when described second ~15min, a length of 60~120min when the described 3rd.The target temperature is 1600-1700 DEG C.
5. the preparation method of the carbon fiber-reinforced aluminium oxide ceramics of in-situ preparation according to claim 1, it is characterised in that also Including:
In sintering process, the vacuum sintering furnace is controlled to be carried out to the target mixture using uniform step pressuring method Pressurization.
6. the preparation method of the carbon fiber-reinforced aluminium oxide ceramics of in-situ preparation according to any one of claim 1 to 5, its It is characterised by, the duration for carrying out ball milling is 1~10min.
7. the preparation method of the carbon fiber-reinforced aluminium oxide ceramics of in-situ preparation according to any one of claim 1 to 5, its Be characterised by, the ratio of the pre-oxidized polyacrylonitrile fiber be 5~30%, the sintering aid powder ratio for 1~ 30%, the ratio of the high-purity alpha-alumina is 65~89%.
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CN111995414A (en) * 2020-07-31 2020-11-27 西安欧中材料科技有限公司 Polyacrylonitrile-based carbon fiber reinforced ceramic core and preparation method thereof
CN113416064A (en) * 2021-04-21 2021-09-21 郑州航空工业管理学院 Zirconia/alumina ceramic composite material and preparation method thereof
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