CN103482994A - 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 the ceramic matric composite technical field, be specifically related to the preparation method that a kind of carbon fiber strengthens quartz ceramic-base composite material.
Background technology
The deadly defect of stupalith is fragility, under external force, at material surface or the most advanced and sophisticated stress concentration that produces of internal tiny crack, crack propagation forms surface can be with consumed energy, thereby the propagation rate of crackle is extremely rapid, often in moment, just make stupalith suffer catastrophic destruction.According to the matrix material theory, when crack propagation runs into fiber, the disengaging by fiber and basal body interface absorbs energy, relaxes stress concentration; Part fiber fracture and while extracting, also will absorb larger energy from matrix under the tension stress effect.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 the fibrous reinforcement stupalith, to improving the fragility of stupalith, under this background, develop carbon fiber and strengthened 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 under nitrogen atmosphere, it is little that this material has a thermal conductivity, heatproof is high, the characteristics of mechanical property excellence, be widely used in aviation, the ablation resistant material of aerospacecraft, as end cap, mount pad etc., fully verified the excellent properties of such material.
Continuous expansion along with this materials'use environment, its performance, workability and globality have all been proposed to new requirement, the purpose of this invention is to provide a kind of new carbon fiber and strengthen quartz ceramic-base composite material preparation technology, reduce production costs and improve globality and the workability of material, the abnormally-structured workpiece that its production profile easily and size are not limit.
Summary of the invention
The purpose of this invention is to provide the preparation method that a kind of carbon fiber strengthens 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 the workpiece profile is not limit.
Carbon fiber of the present invention strengthens the preparation method of quartz ceramic-base composite material, comprises the following steps:
(1) fiber preform pre-treatment;
(2) liquid impregnation moulding: will be placed in the slip that quartzy powder and silicon sol mix through pretreated fiber preform, under vacuum, auxiliary vibratory process dip treating, be dried to constant weight after having flooded, thermal treatment, then furnace cooling, obtain 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 processing in step (3) is carried out to mechanical workout, clean, be dried to constant weight, make finished product.
Fiber preform pre-treatment described in step (1) is carbon fabric perform is to soak 12～24h in 40～60 ℃, the massfraction nitric acid that is 20～35% in temperature, then with deionized water rinsing to neutral, be dried to constant weight standby; Or pre-oxygen silky fibre precast body is fixed in heat treatment tooling, then being warming up to 1000～1200 ℃ under vacuum or inert atmosphere and making, vacuum tightness is-0.07～-0.1MPa, inert atmosphere is in nitrogen or helium.Using the purpose of heat treatment tooling is to prevent that pre-oxygen silky fibre precast body 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%.
Auxiliary vibratory process described in step (2) is vibration 5～10min, suspends 5～20min, repetitive vibrations and time-out process 5～300 times; Described vacuum condition be vacuum tightness be-0.07～-0.1Mpa; Described drying temperature is 100～150 ℃.
Thermal treatment described in step (2) is to be warming up to 500～900 ℃ with 10～20 ℃/min speed, and soaking time is 2～4h; Described thermal treatment is carried out under vacuum or inert atmosphere, and vacuum tightness is-0.07～-0.1MPa, 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 μ m; 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; In silicone resin, can add conventional solidifying agent to improve dipping effect.
Vacuum-impregnated vacuum tightness described in step (3) is-0.07～-0.1MPa, dipping time is 0.5～3h; Described drying temperature is 100～150 ℃.
Thermal treatment described in step (3) is to be warming up to 800～1000 ℃ with 5～20 ℃/min speed, and soaking time is 2～4h; Described thermal treatment is carried out under vacuum or inert atmosphere, and vacuum tightness is-0.07～-0.1MPa, inert atmosphere is nitrogen or helium.
Drying temperature described in step (4) is 100～150 ℃.
Carbon fiber of the present invention strengthens the preparation method of quartz ceramic-base composite material, and 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, in temperature, be to soak 12～24h in 40～60 ℃, the massfraction nitric acid that is 20～35%, then with deionized water rinsing to neutral, 100～120 ℃ to be dried to constant weight standby;
Or pre-oxygen silky fibre precast body pre-treatment: according to the profile of required preparation, select the pre-oxygen silky fibre precast body of suitable configuration and size, then precast body is fixed in heat treatment tooling, then slowly be warming up to 1000～1200 ℃ under vacuum or inert atmosphere, furnace cooling, obtain carbon fabric perform;
(2) liquid impregnation moulding:
Quartzy powder mixes in the ball mill of 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, under vacuum, auxiliary vibratory process dip treating, carry out drying and thermal treatment successively after having flooded, and then furnace cooling, obtain base substrate;
(3) silicone-impregnated:
Base substrate with obtaining in silicone resin vacuum impregnation step (2), be cured after having flooded, and then carries out successively drying and thermal treatment, then furnace cooling;
(4) mechanical workout and cleaning:
Base substrate after processing in step (3) is processed according to required profile and size, can be adopted the operations such as grinding, cutting, auger shell pit, then the goods after mechanical workout are cleaned, taken out drying, made finished product.
It is to take SiO 2-ceramic as matrix that the carbon fiber that the present invention makes strengthens quartz ceramic-base composite material, take carbon fiber as reinforcement, wherein silicon-dioxide is introduced by quartzy powder, silicon sol, silicone resin and inorganic polysiloxane, fiber adopts the business to sell carbon fiber, also can be transformed and be obtained by the thermal treatment under vacuum or inert atmosphere of pre-oxygen silky fibre precast body.
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, the precast body profile can be dull and stereotyped, can be also the random appearance structure.
The present invention can process the abnormal members such as screw that diameter is less than M6, swivel nut.
The present invention compared with prior art, has following beneficial effect:
The present invention can realize that the carbon fiber that physical strength is high, thermal conductivity is low and workability is good strengthens the quartz ceramic-base composite material preparation, and the abnormally-structured workpiece that production profile easily and size are not limit, have good practical value, and its advantage main manifestations is:
1, with hot pressing formation process, compare, but the present invention's once shaped goes out many identical carbon fibers of material property strengthens the quartz ceramic-base composite material workpiece, also but to go out material system identical in once shaped, but the carbon fiber that reinforcement is different from the ceramic matrix ratio strengthens the quartz ceramic-base composite material workpiece, moulding is not subject to the precast body shape limitation, and 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, and profile and inner quality are easy to control, and conforming product rate is high.
3, facility investment expense is low, and cost is low, and production efficiency is high, can directly prepare the special-shaped structure piece that process redundancy is less.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
Adopt pre-oxygen silky fibre precast body to prepare high temperature resistant nonmetal swivel nut, fabric adopts needling structure, fiber volume fraction 30%.
(1) pre-treatment of fiber preform
Pre-oxygen silky fibre precast body is placed on and burns till in frock fixingly, with the intensification temperature of 0.5 ℃/min, is warming up to 1200 ℃, insulation 2h, then furnace cooling.
(2) sluny impregnation
Quartzy Pulp preparation: 4000g fused quartz powder mixes with the 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, be evacuated to-0.07MPa, then suck quartzy slip, auxiliary vibratory process dip treating under vacuum, vibration 5min, suspend 5min, repetitive vibrations and time-out process 30 times; Flooded latter 100 ℃ and be dried to constant weight, thermal treatment under nitrogen atmosphere, be warming up to 500 ℃ with 20 ℃/min, insulation 2h, and then furnace cooling, obtain base substrate.
(3) inorganic polysiloxane dipping
Inorganic polysiloxane ND-SIR be take mass ratio and is fully mixed altogether 4000g as 1:3 with ethanol, vacuum impregnation base substrate then, and vacuum tightness is-0.07MPa that dipping time is 0.5h; After having flooded, be cured, 100 ℃ are dried to constant weight, thermal treatment, and heat-treat condition is under nitrogen atmosphere, with the heat-up rate of 10 ℃/min, is warming up to 900 ℃, and insulation 2h, then furnace cooling.
(4) mechanical workout and cleaning
According to the requirement of high temperature resistant nonmetal swivel nut physical dimension, to base substrate punched, threading, then carry out Excircle machining, then the finished product after mechanical workout is cleaned in acetone, take out dryly, obtain finished product.
The 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 the 2.5D braiding structure.
(1) pre-treatment of fiber preform
It is in 40 ℃, the massfraction nitric acid that is 20% that carbon fabric perform is positioned over to temperature, soaks 20h, then takes out, and in deionized water, cleans until become neutral; Then 120 ℃ are dried to constant weight.
(2) sluny impregnation
Quartzy Pulp preparation: 4000g fused quartz powder mixes with the 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.
To be placed in vacuum tank through pretreated carbon fabric perform, be evacuated to-0.1MPa, then suck quartzy slip, auxiliary vibratory process moulding under vacuum; Vibration 10min, suspend 20min, repetitive vibrations and time-out process 100 times; Flooded latter 150 ℃ and be dried to constant weight, thermal treatment under helium atmosphere, be warming up to 900 ℃ with 10 ℃/min, insulation 4h, and then furnace cooling, obtain base substrate.
(3) silicone resin dipping
Silicone resin SAR-9 be take mass ratio and is fully mixed altogether 4000g as 100:0.5 with solidifying agent KH550, vacuum impregnation base substrate then, and vacuum tightness is-0.1MPa that dipping time is 3h; After having flooded, be cured, 120 ℃ are dried to constant weight, thermal treatment, and heat-treat condition is under helium atmosphere, with the heat-up rate of 5 ℃/min, is warming up to 950 ℃, and insulation 4h, then furnace cooling.
(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, taken out drying, obtained finished product.
The finished product index: density is 1.55g/cm
3, the hoop flexural strength is greater than 100MPa.
Embodiment 3
Carbon fabric perform volume fraction 50%, fabric adopts the thin puncture structure of compiling.
(1) pre-treatment of fiber preform
It is in 60 ℃, the massfraction nitric acid that is 30% that carbon fabric perform is positioned over to temperature, soaks 12h, then takes out, and in deionized water, cleans until become neutral; Then 100 ℃ are dried to constant weight.
(2) sluny impregnation
Quartzy Pulp preparation: 4000g fused quartz powder mixes with the 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.
To be placed in vacuum tank through pretreated carbon fabric perform, be evacuated to-0.08MPa, then suck quartzy slip, auxiliary vibratory process moulding under vacuum; Vibration 8min, suspend 10min, repetitive vibrations and time-out process 300 times; Flooded latter 120 ℃ and be dried to constant weight, thermal treatment under nitrogen atmosphere, be warming up to 550 ℃ with 15 ℃/min, insulation 3h, and then furnace cooling, obtain base substrate.
(3) silicone resin dipping
Get 806 silicone resin 4000g vacuum impregnation base substrates, vacuum tightness is-0.08MPa that dipping time is 2h; After having flooded, be cured, 150 ℃ are dried to constant weight, thermal treatment, and heat-treat condition is under nitrogen atmosphere, with the heat-up rate of 20 ℃/min, is warming up to 1000 ℃, and insulation 3h, then furnace cooling.
(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, taken out drying, obtained finished product.
The 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
It is in 50 ℃, the massfraction nitric acid that is 35% that carbon fabric perform is positioned over to temperature, soaks 24h, then takes out, and in deionized water, cleans until become neutral; Then 110 ℃ are dried to constant weight.
(2) sluny impregnation
Quartzy Pulp preparation: 4000g fused quartz powder mixes with the 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.
To be placed in vacuum tank through pretreated carbon fabric perform, be evacuated to-0.09MPa, then suck quartzy slip, auxiliary vibratory process moulding under vacuum; Vibration 6min, suspend 15min, repetitive vibrations and time-out process 5 times; Flood latter 140 ℃ and be dried to constant weight, thermal treatment under vacuum, vacuum tightness is-0.07MPa, with 20 ℃/min, is warming up to 800 ℃, insulation 2h, then furnace cooling, obtain base substrate.
(3) silicone resin dipping
Silicone resin SAR-5 be take mass ratio and is fully mixed altogether 4000g as 100:0.5 with solidifying agent HP2000, vacuum impregnation base substrate then, and vacuum tightness is-0.07MPa that dipping time is 1h; After having flooded, be cured, 130 ℃ are dried to constant weight, thermal treatment under vacuum, and vacuum tightness is-0.08MPa, with the heat-up rate of 15 ℃/min, is warming up to 800 ℃, and insulation 2h, then furnace cooling.
(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, taken out drying, obtained finished product.
The finished product index: density is 1.63g/cm
3, flexural strength is greater than 110MPa.
Claims (10)
1. a carbon fiber strengthens the preparation method of quartz ceramic-base composite material, it is characterized in that comprising the following steps:
(1) fiber preform pre-treatment;
(2) liquid impregnation moulding: will be placed in the slip that quartzy powder and silicon sol mix through pretreated fiber preform, under vacuum, auxiliary vibratory process dip treating, be dried to constant weight after having flooded, thermal treatment, then furnace cooling, obtain 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 processing in step (3) is carried out to mechanical workout, clean, be dried to constant weight, make finished product.
2. carbon fiber according to claim 1 strengthens the preparation method of quartz ceramic-base composite material, it is characterized in that the fiber preform pre-treatment described in step (1) be carbon fabric perform is to soak 12～24h in 40～60 ℃, the massfraction nitric acid that is 20～35% in temperature, then extremely neutral with deionized water rinsing, be dried to constant weight standby; Or pre-oxygen silky fibre precast body is fixed in heat treatment tooling, then be warming up to 1000～1200 ℃ under vacuum or inert atmosphere and make.
3. carbon fiber according to claim 1 strengthens the preparation method of quartz ceramic-base composite material, it is characterized in that the mass percent of quartzy powder in slip that the quartzy powder described in step (2) and silicon sol mix is 40～65%.
4. carbon fiber according to claim 1 strengthens the preparation method of quartz ceramic-base composite material, it is characterized in that the auxiliary vibratory process described in step (2) is vibration 5～10min, suspends 5～20min, repetitive vibrations and time-out process 5～300 times; Described vacuum condition be vacuum tightness be-0.07～-0.1MPa.
5. carbon fiber according to claim 1 strengthens the preparation method of quartz ceramic-base composite material, it is characterized in that the thermal treatment described in step (2) is to be warming up to 500～900 ℃ with 10～20 ℃/min speed, and soaking time is 2～4h; Described thermal treatment is carried out under vacuum or inert atmosphere.
6. carbon fiber according to claim 1 strengthens the preparation method of quartz ceramic-base composite material, it is characterized in that the silicone resin described in step (3) is silicone resin or inorganic polysiloxane.
7. carbon fiber according to claim 1 strengthens the preparation method of quartz ceramic-base composite material, it is characterized in that the vacuum-impregnated vacuum tightness described in step (3) be-0.07～-0.1MPa, dipping time is 0.5～3h.
8. carbon fiber according to claim 1 strengthens the preparation method of quartz ceramic-base composite material, it is characterized in that the thermal treatment described in step (3) is to be warming up to 800～1000 ℃ with 5～20 ℃/min speed, and soaking time is 2～4h; Described thermal treatment is carried out under vacuum or inert atmosphere.
9. strengthen the preparation method of quartz ceramic-base composite material according to the described carbon fiber of claim 5 or 6, it is characterized in that described vacuum condition be vacuum tightness be-0.07～-0.1MPa.
10. strengthen the preparation method of quartz ceramic-base composite material according to the described carbon fiber of claim 5 or 6, it 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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| CN105732068A (en) * | 2016-01-29 | 2016-07-06 | 山东工业陶瓷研究设计院有限公司 | Preparation method of detection window for smelting furnace |
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| CN110406134A (en) * | 2019-08-01 | 2019-11-05 | 帝国理工创新有限公司 | A kind of method of forming carbon fiber reinforced thermolplastic 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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