CN103482994B - Preparation method of carbon fiber-reinforced quartz ceramic-based composite material - Google Patents
Preparation method of carbon fiber-reinforced quartz ceramic-based composite material Download PDFInfo
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Abstract
The invention belongs to the technical field of ceramic-based composite materials and specifically relates to a preparation method of a carbon fiber-reinforced quartz ceramic-based composite material. The preparation method comprises the following steps: pretreatment of a fiber preform, liquid-phase dip forming, silicone resin dipping and machining. By adopting the preparation method provided by the invention, a plurality of carbon fiber-reinforced quartz ceramic-based composite material workpieces with identical material performances can be formed once, carbon fiber-reinforced quartz ceramic-based composite material workpieces with same material systems but different reinforcement/ceramic matrix proportions can also be formed once, the forming is not limited by the shape of the preform, and the forming efficiency is high. Carbon fiber is introduced in the form of the fiber preform, the content of the carbon fiber is high, and the dispersion is uniform. The prepared composite material has the advantages of good machinability, easiness in control of the shape and internal quality and high product qualification rate. The equipment investment cost is low, the cost is low, the production efficiency is high, and a special-shaped structural member with relatively small machining allowance can be directly prepared.
Description
Technical field
The invention belongs to technology field of ceramic matrix composite material, be specifically related to a kind of preparation method of fibre reinforced quartz ceramic-base composite material.
Background technology
The deadly defect of stupalith is fragility, under external force, produce stress concentration at material surface or internal tiny crack tip, crack propagation forms surface energy with consumed energy, thus the propagation rate of crackle is extremely rapid, often just makes stupalith suffer catastrophic destruction in moment.Theoretical according to matrix material, when crack propagation runs into fiber, absorb energy by the disengaging of fiber and basal body interface, relax stress concentration; When few fibers fracture occurs under tension stress effect and extracts from matrix, also larger energy will be absorbed.Therefore, FRCMC is a kind of approach of effective solution stupalith fragility.
From the seventies in last century, domestic a lot of scientific research institutions start to explore fibrous reinforcement stupalith, to improving the fragility of stupalith, in this context, have developed fibre reinforced quartz ceramic-base composite material, fiber adopts chopped strand to be scattered in powder, the mode of one-way fiber arrangement and fiber perpendicular array, then with quartzy powder hot pressed sintering in a nitrogen atmosphere, it is little that this material has thermal conductivity, heatproof is high, the feature of excellent in mechanical performance, be widely used in aviation, the ablation resistant material of aerospacecraft, as end cap, mount pad etc., fully demonstrate the excellent properties of such material.
Along with the continuous expansion of this materials'use environment, new requirement is all proposed to its performance, workability and globality, the object of this invention is to provide a kind of new fibre reinforced quartz ceramic-base composite material preparation technology, reduce production cost and improve globality and the workability of material, making the abnormally-structured workpiece that its production profile easily and size are not limit.
Summary of the invention
The object of this invention is to provide a kind of preparation method of fibre reinforced quartz ceramic-base composite material, cycle is short, cost is low, be suitable for industrialized mass production, and the material workability of preparation is good, physical strength is high, thermal conductivity is low and workpiece configurations is not limit.
The preparation method of fibre reinforced quartz ceramic-base composite material of the present invention, comprises the following steps:
(1) fiber preform pre-treatment;
(2) liquid impregnation is shaping: by the slip being placed in quartzy powder and silicon sol through pretreated fiber preform and mixing, ancillary vibration technique dip treating, is dried to constant weight after having flooded under vacuo, thermal treatment, then furnace cooling, obtains base substrate;
(3) silicone-impregnated: with the base substrate obtained in silicone resin vacuum impregnation step (2), carry out ambient cure after having flooded, be dried to constant weight, thermal treatment, then furnace cooling;
(4) mechanical workout: the base substrate after process in step (3) is carried out mechanical workout, cleaning, is dried to constant weight, obtained finished product.
Fiber preform pre-treatment described in step (1) be carbon fabric perform temperature be 40 ~ 60 DEG C, massfraction is soak 12 ~ 24h in the nitric acid of 20 ~ 35%, then with deionized water rinsing to neutral, be dried to constant weight for subsequent use; Or oxidization fiber fiber preform is fixed in heat treatment tooling, be then warming up to 1000 ~ 1200 DEG C in a vacuum or inert atmosphere and obtain, vacuum tightness is-0.07 ~-0.1MPa, and inert atmosphere is in nitrogen or helium.The object using heat treatment tooling prevents oxidization fiber fiber preform from deforming in heat treatment process.
In the slip that quartzy powder described in step (2) and silicon sol mix, the mass percent of quartzy powder is 40 ~ 65%.
Ancillary vibration technique described in step (2) is vibration 5 ~ 10min, suspends 5 ~ 20min, repetitive vibrations and suspend process 5 ~ 300 times; Described vacuum condition is vacuum tightness is-0.07 ~-0.1Mpa; Described drying temperature is 100 ~ 150 DEG C.
Thermal treatment described in step (2) is warming up to 500 ~ 900 DEG C with 10 ~ 20 DEG C/min speed, and soaking time is 2 ~ 4h; Described thermal treatment is carried out in a vacuum or inert atmosphere, and vacuum tightness is-0.07 ~-0.1MPa, and inert atmosphere is nitrogen or helium.
Quartzy powder described in step (2) is silicon-dioxide (SiO
2) content is greater than 99.90wt%, particle diameter is 1 ~ 15 μm; Silicon sol is colourless transparent liquid, wherein silicon-dioxide (SiO
2) content is 20 ~ 35wt%, particle diameter is 10 ~ 20nm.
Silicone resin described in step (3) is silicone resin or inorganic polysiloxane, and silicone resin is silicon-dioxide (SiO
2) content is greater than 50wt%, viscosity is less than 500mPas; Inorganic polysiloxane is silicon-dioxide (SiO
2) content is greater than 50wt%, viscosity is less than 500mPas; Conventional solidified dose can be added improve dipping effect in silicone resin.
Vacuum-impregnated vacuum tightness described in step (3) is-0.07 ~-0.1MPa, and dipping time is 0.5 ~ 3h; Described drying temperature is 100 ~ 150 DEG C.
Thermal treatment described in step (3) is warming up to 800 ~ 1000 DEG C with 5 ~ 20 DEG C/min speed, and soaking time is 2 ~ 4h; Described thermal treatment is carried out in a vacuum or inert atmosphere, and vacuum tightness is-0.07 ~-0.1MPa, and inert atmosphere is nitrogen or helium.
Drying temperature described in step (4) is 100 ~ 150 DEG C.
The preparation method of fibre reinforced quartz ceramic-base composite material of the present invention, concrete steps are as follows:
(1) fiber preform pre-treatment:
Carbon fabric perform pre-treatment: according to the profile of required preparation, select the carbon fabric perform of suitable configuration and size, temperature be 40 ~ 60 DEG C, massfraction is soak 12 ~ 24h in the nitric acid of 20 ~ 35%, then with deionized water rinsing to neutral, 100 ~ 120 DEG C to be dried to constant weight for subsequent use;
Or the pre-treatment of oxidization fiber fiber preform: according to the profile of required preparation, select the oxidization fiber fiber preform of suitable configuration and size, then precast body is fixed in heat treatment tooling, then 1000 ~ 1200 DEG C are slowly warming up in a vacuum or inert atmosphere, furnace cooling, obtains carbon fabric perform;
(2) liquid impregnation is shaping:
Quartz powder mixes in the ball mill that mill ball is housed with silicon sol, and material ball ratio is 1:1 ~ 3, and Ball-milling Time is 24 ~ 72h, prepares quartzy slip.To be placed in quartzy slip through pretreated carbon fabric perform, ancillary vibration technique dip treating, carries out drying and thermal treatment after having flooded successively under vacuo, then furnace cooling, obtains base substrate;
(3) silicone-impregnated:
With the base substrate obtained in silicone resin vacuum impregnation step (2), be cured after having flooded, then carry out drying and thermal treatment successively, then furnace cooling;
(4) mechanical workout and cleaning:
Base substrate after process in step (3) is processed according to required profile and size, the operations such as grinding, cutting, auger shell pit can be adopted, then the goods after mechanical workout are cleaned, take out dry, obtained finished product.
The fibre reinforced quartz ceramic-base composite material that the present invention obtains take SiO 2-ceramic as matrix, take carbon fiber as reinforcement, wherein silicon-dioxide is introduced by quartzy powder, silicon sol, silicone resin and inorganic polysiloxane, fiber adopts commercially carbon fiber, also can by oxidization fiber fiber preform in a vacuum or inert atmosphere thermal treatment transform obtain.
The fiber volume fraction of fiber preform is 30% ~ 55%, braiding structure can select needling structure, 2.5D braiding structure, three-dimensional braided structure (comprise three-dimensional four-way, three-dimensional five to or three-dimensional six to), carefully compile puncture, precast body profile can be dull and stereotyped, also can be random appearance structure.
The present invention can process the abnormal member such as screw, swivel nut that diameter is less than M6.
The present invention compared with prior art, has following beneficial effect:
The present invention can realize the preparation of physical strength is high, thermal conductivity is low and workability is good fibre reinforced quartz ceramic-base composite material, can the abnormally-structured workpiece do not limit of production profile easily and size, and have good practical value, its advantage main manifestations is:
1, compared with hot pressing formation process, the present invention once shaped can go out more than one piece material property identical fibre reinforced quartz ceramic-base composite material workpiece, also can once shaped to go out material system identical, but the fibre reinforced quartz ceramic-base composite material workpiece that reinforcement is different from ceramic matrix ratio, shapingly do not limit by precast body profile, shaping efficiency is high.
2, carbon fiber is introduced with the form of fiber preform, and carbon fiber content is high, is uniformly dispersed, and prepared matrix material processability is good, profile and inner quality easy to control, conforming product rate is high.
3, facility investment expense is low, and cost is low, and production efficiency is high, directly can prepare the less special-shaped structure piece of process redundancy.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
Adopt oxidization fiber fiber preform to prepare high temperature resistant nonmetal swivel nut, fabric adopts needling structure, fiber volume fraction 30%.
(1) pre-treatment of fiber preform
Oxidization fiber fiber preform is placed on and burns till frock internal fixtion, is warming up to 1200 DEG C with the warming temperature of 0.5 DEG C/min, insulation 2h, then furnace cooling.
(2) sluny impregnation
Quartz Pulp preparation: 4000g fused quartz powder mixes with 2500ml silicon sol, and selected high-purity silicasol is colourless transparent liquid, wherein SiO
2solid content is 30wt%, and particle diameter is 10nm, pH=2.
To be placed in vacuum tank through pretreated carbon fabric perform, and be evacuated to-0.07MPa, and then suck quartzy slip, under vacuo ancillary vibration technique dip treating, vibration 5min, suspends 5min, repetitive vibrations and suspend process 30 times; Flooded latter 100 DEG C and be dried to constant weight, thermal treatment in a nitrogen atmosphere, be warming up to 500 DEG C with 20 DEG C/min, insulation 2h, then furnace cooling, obtain base substrate.
(3) inorganic polysiloxane dipping
Inorganic polysiloxane ND-SIR and ethanol are that 1:3 fully mixes 4000g, then vacuum impregnation base substrate altogether with mass ratio, and vacuum tightness is-0.07MPa, and dipping time is 0.5h; Be cured after having flooded, 100 DEG C are dried to constant weight, thermal treatment, and heat-treat condition is in a nitrogen atmosphere, is warming up to 900 DEG C, and is incubated 2h, then furnace cooling with the heat-up rate of 10 DEG C/min.
(4) mechanical workout and cleaning
According to the requirement of high temperature resistant nonmetal swivel nut physical dimension, base substrate to be punched, threading, then carry out Excircle machining, then the finished product after mechanical workout is cleaned in acetone, take out dry, obtain finished product.
Finished product index: density is 1.45g/cm
3, flexural strength is greater than 80MPa.
Embodiment 2
Carbon fabric perform volume fraction 42%, fabric adopts 2.5D braiding structure.
(1) pre-treatment of fiber preform
Carbon fabric perform is positioned over temperature is 40 DEG C, massfraction is in the nitric acid of 20%, soaks 20h, then take out, cleaning is until become neutral in deionized water; Then 120 DEG C are dried to constant weight.
(2) sluny impregnation
Quartz Pulp preparation: 4000g fused quartz powder mixes with 2000ml silicon sol, and selected high-purity silicasol is colourless transparent liquid, wherein SiO
2solid content is 23.8wt%, and particle diameter is 20nm, pH=3.
Vacuum tank will be placed in through pretreated carbon fabric perform, be evacuated to-0.1MPa, then suck quartzy slip, under vacuo ancillary vibration technological forming; Vibration 10min, suspends 20min, repetitive vibrations and suspend process 100 times; Flooded latter 150 DEG C and be dried to constant weight, thermal treatment under helium atmosphere, be warming up to 900 DEG C with 10 DEG C/min, insulation 4h, then furnace cooling, obtain base substrate.
(3) silicone resin dipping
Silicone resin SAR-9 and solidifying agent KH550 are that 100:0.5 fully mixes 4000g, then vacuum impregnation base substrate altogether with mass ratio, and vacuum tightness is-0.1MPa, and dipping time is 3h; Be cured after having flooded, 120 DEG C are dried to constant weight, thermal treatment, and heat-treat condition is under helium atmosphere, is warming up to 950 DEG C, and is incubated 4h, then furnace cooling with the heat-up rate of 5 DEG C/min.
(4) mechanical workout and cleaning
Base substrate is processed according to required profile and size, then the finished product after mechanical workout is cleaned in acetone, take out dry, obtain finished product.
Finished product index: density is 1.55g/cm
3, hoop flexural strength is greater than 100MPa.
Embodiment 3
Carbon fabric perform volume fraction 50%, fabric adopts and carefully compiles puncturing structure.
(1) pre-treatment of fiber preform
Carbon fabric perform is positioned over temperature is 60 DEG C, massfraction is in the nitric acid of 30%, soaks 12h, then take out, cleaning is until become neutral in deionized water; Then 100 DEG C are dried to constant weight.
(2) sluny impregnation
Quartz Pulp preparation: 4000g fused quartz powder mixes with 3000ml silicon sol, and selected high-purity silicasol is colourless transparent liquid, wherein SiO
2solid content is 30wt%, and particle diameter is 15nm, pH=2.5.
Vacuum tank will be placed in through pretreated carbon fabric perform, be evacuated to-0.08MPa, then suck quartzy slip, under vacuo ancillary vibration technological forming; Vibration 8min, suspends 10min, repetitive vibrations and suspend process 300 times; Flooded latter 120 DEG C and be dried to constant weight, thermal treatment in a nitrogen atmosphere, be warming up to 550 DEG C with 15 DEG C/min, insulation 3h, then furnace cooling, obtain base substrate.
(3) silicone resin dipping
Get 806 silicone resin 4000g vacuum impregnation base substrates, vacuum tightness is-0.08MPa, and dipping time is 2h; Be cured after having flooded, 150 DEG C are dried to constant weight, thermal treatment, and heat-treat condition is in a nitrogen atmosphere, is warming up to 1000 DEG C, and is incubated 3h, then furnace cooling with the heat-up rate of 20 DEG C/min.
(4) mechanical workout and cleaning
Base substrate is processed according to required profile and size, then the finished product after mechanical workout is cleaned in acetone, take out dry, obtain finished product.
Finished product index: density is 1.60g/cm
3, flexural strength is greater than 150MPa.
Embodiment 4
Carbon fabric perform volume fraction 55%, fabric adopts three-dimensional four-way structure.
(1) pre-treatment of fiber preform
Carbon fabric perform is positioned over temperature is 50 DEG C, massfraction is in the nitric acid of 35%, soaks 24h, then take out, cleaning is until become neutral in deionized water; Then 110 DEG C are dried to constant weight.
(2) sluny impregnation
Quartz Pulp preparation: 4000g fused quartz powder mixes with 3000ml silicon sol, and selected high-purity silicasol is colourless transparent liquid, wherein SiO
2solid content is 30wt%, and particle diameter is 20nm, pH=3.
Vacuum tank will be placed in through pretreated carbon fabric perform, be evacuated to-0.09MPa, then suck quartzy slip, under vacuo ancillary vibration technological forming; Vibration 6min, suspends 15min, repetitive vibrations and suspend process 5 times; Flooded latter 140 DEG C and be dried to constant weight, thermal treatment under vacuo, vacuum tightness is-0.07MPa, is warming up to 800 DEG C with 20 DEG C/min, and insulation 2h, then furnace cooling, obtain base substrate.
(3) silicone resin dipping
Silicone resin SAR-5 and solidifying agent HP2000 are that 100:0.5 fully mixes 4000g, then vacuum impregnation base substrate altogether with mass ratio, and vacuum tightness is-0.07MPa, and dipping time is 1h; Be cured after having flooded, 130 DEG C are dried to constant weight, thermal treatment under vacuo, and vacuum tightness is-0.08MPa, is warming up to 800 DEG C, and is incubated 2h, then furnace cooling with the heat-up rate of 15 DEG C/min.
(4) mechanical workout and cleaning
Base substrate is processed according to required profile and size, then the finished product after mechanical workout is cleaned in acetone, take out dry, obtain finished product.
Finished product index: density is 1.63g/cm
3, flexural strength is greater than 110MPa.
Claims (9)
1. a preparation method for fibre reinforced quartz ceramic-base composite material, is characterized in that comprising the following steps:
(1) fiber preform pre-treatment;
(2) liquid impregnation is shaping: by the slip being placed in quartzy powder and silicon sol through pretreated fiber preform and mixing, ancillary vibration technique dip treating, is dried to constant weight after having flooded under vacuo, thermal treatment, then furnace cooling, obtains base substrate;
(3) silicone-impregnated: with the base substrate obtained in silicone resin vacuum impregnation step (2), carry out ambient cure after having flooded, be dried to constant weight, thermal treatment, then furnace cooling;
(4) mechanical workout: the base substrate after process in step (3) is carried out mechanical workout, cleaning, is dried to constant weight, obtained finished product;
Fiber preform pre-treatment described in step (1) be carbon fabric perform temperature be 40 ~ 60 DEG C, massfraction is soak 12 ~ 24h in the nitric acid of 20 ~ 35%, then with deionized water rinsing to neutral, be dried to constant weight for subsequent use; Or oxidization fiber fiber preform is fixed in heat treatment tooling, be then warming up to 1000 ~ 1200 DEG C in a vacuum or inert atmosphere and obtain.
2. the preparation method of fibre reinforced quartz ceramic-base composite material according to claim 1, is characterized in that the mass percent of quartzy powder in the slip that the quartzy powder described in step (2) and silicon sol mix is 40 ~ 65%.
3. the preparation method of fibre reinforced quartz ceramic-base composite material according to claim 1, it is characterized in that the ancillary vibration technique described in step (2) is vibration 5 ~ 10min, suspend 5 ~ 20min, repetitive vibrations and suspend process 5 ~ 300 times; Described vacuum condition is vacuum tightness is-0.07 ~-0.1MPa.
4. the preparation method of fibre reinforced quartz ceramic-base composite material according to claim 1, it is characterized in that the thermal treatment described in step (2) is warming up to 500 ~ 900 DEG C with 10 ~ 20 DEG C/min speed, soaking time is 2 ~ 4h; Described thermal treatment is carried out in a vacuum or inert atmosphere.
5. the preparation method of fibre reinforced quartz ceramic-base composite material according to claim 1, is characterized in that the silicone resin described in step (3) is silicone resin or inorganic polysiloxane.
6. the preparation method of fibre reinforced quartz ceramic-base composite material according to claim 1, it is characterized in that the vacuum-impregnated vacuum tightness described in step (3) is-0.07 ~-0.1MPa, dipping time is 0.5 ~ 3h.
7. the preparation method of fibre reinforced quartz ceramic-base composite material according to claim 1, it is characterized in that the thermal treatment described in step (3) is warming up to 800 ~ 1000 DEG C with 5 ~ 20 DEG C/min speed, soaking time is 2 ~ 4h; Described thermal treatment is carried out in a vacuum or inert atmosphere.
8. the preparation method of the fibre reinforced quartz ceramic-base composite material according to claim 4 or 5, is characterized in that described vacuum condition be vacuum tightness is-0.07 ~-0.1MPa.
9. the preparation method of the fibre reinforced quartz ceramic-base composite material according to claim 4 or 5, is characterized in that described inert atmosphere is nitrogen or helium.
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| CN105088340A (en) * | 2015-09-06 | 2015-11-25 | 江苏协鑫硅材料科技发展有限公司 | Crucible and preparation method thereof |
| CN105646008A (en) * | 2016-01-29 | 2016-06-08 | 山东工业陶瓷研究设计院有限公司 | Method for preparing low-thermal-conductivity ceramic matrix composite fastener |
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| CN106892677A (en) * | 2017-02-20 | 2017-06-27 | 佛山市蓝瑞欧特信息服务有限公司 | A kind of carbon fiber ceramic material and preparation method thereof |
| CN107827474B (en) * | 2017-11-16 | 2020-05-08 | 湖北三江航天江北机械工程有限公司 | Rapid molding method for injection molding of high-solid-content low-viscosity slurry permeable ceramic matrix wave-transmitting composite material |
| CN108285354A (en) * | 2018-01-22 | 2018-07-17 | 航天特种材料及工艺技术研究所 | A kind of anti-wet fiber enhancing quartz-ceramics composite material and method |
| CN109524781B (en) * | 2018-11-21 | 2020-10-09 | 湖北三江航天江北机械工程有限公司 | Preparation method of Z-pin reinforced quartz composite ceramic wave-transparent radome |
| CN110194674B (en) * | 2019-06-06 | 2022-04-15 | 山东工业陶瓷研究设计院有限公司 | Preparation method of carbon fiber toughened quartz ceramic matrix composite material |
| CN110406134B (en) * | 2019-08-01 | 2021-08-13 | 帝国理工创新有限公司 | Method for forming carbon fiber reinforced thermoplastic composite material part |
| CN113857603A (en) * | 2021-09-29 | 2021-12-31 | 江苏科技大学 | Method for assisting in brazing ceramic matrix composite material and metal |
| CN114920572A (en) * | 2022-06-17 | 2022-08-19 | 中国联合重型燃气轮机技术有限公司 | Woven carbon fiber reinforced ceramic core, preparation method thereof and corresponding investment casting method |
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| CN101831178A (en) * | 2010-05-04 | 2010-09-15 | 中国人民解放军国防科学技术大学 | Quartz fiber reinforced composite material and preparation method thereof |
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| CN101903429B (en) * | 2007-06-19 | 2015-04-15 | 弗莱克斯伯陶器公司(加州公司) | Silicone resin composites for high temperature durable elastic composite applications and methods for fabricating same |
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| CN1160031A (en) * | 1997-03-14 | 1997-09-24 | 冶金工业部钢铁研究总院 | Fused quartz ceramic material |
| CN101831178A (en) * | 2010-05-04 | 2010-09-15 | 中国人民解放军国防科学技术大学 | Quartz fiber reinforced composite material and preparation method thereof |
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