CN104130013B - The preparation method of the crystal whisker toughened mullite compound coating of a kind of carbon/carbon compound material SiC - Google Patents
The preparation method of the crystal whisker toughened mullite compound coating of a kind of carbon/carbon compound material SiC Download PDFInfo
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- CN104130013B CN104130013B CN201410328206.7A CN201410328206A CN104130013B CN 104130013 B CN104130013 B CN 104130013B CN 201410328206 A CN201410328206 A CN 201410328206A CN 104130013 B CN104130013 B CN 104130013B
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Abstract
The invention provides the preparation method of the crystal whisker toughened mullite compound coating of a kind of carbon/carbon compound material SiC: be scattered in butanols by mullite powder and SiC whisker, heat while stirring after ultrasonic vibration to obtain suspending liquid A 2; In suspending liquid A 2, add iodate carbon, heat while stirring to obtain suspension B; Suspension B being poured into one with Graphite Electrodes is anode, conducting base be negative electrode water heating kettle in carry out electromagnetic induction heating two pulse electrophoretic deposition, by the samples dried of taking out, carbon/carbon compound material SiC crystal whisker toughened mullite compound external coating (EC) prepared by the present invention surface flawless, external coating (EC) and substrate combinating strength large; Structure-controllable can be obtained at low temperatures and carbon/carbon compound material SiC of good performance crystal whisker toughened mullite compound external coating (EC); Preparation technology is simple, and easy to operate, raw material is easy to get, and preparation cost is lower, has vast potential for future development.
Description
Technical field
The present invention relates to a kind of method preparing carbon/carbon compound material compound external coating (EC), be specifically related to the preparation method of a kind of electromagnetic induction heating-two pulse electrophoretic deposition carbon/carbon compound material SiC crystal whisker toughened mullite compound external coating (EC).
Background technology
C/C matrix material is otherwise known as carbon fiber carbon based composites, because it is made up of single carbon, not only has the ablation resistance of charcoal and graphite material excellence, the advantages such as low density, thermal expansivity are low, and also has excellent mechanical property under high temperature.Especially the performance that goes up not down of the increase of its intensity temperature, becomes one of the most rising hi tech and new material, is widely used as ablator and the thermal structure material of aerospace technical field.But C/C matrix material is rapid oxidation under the oxidizing atmosphere of temperature more than 500 DEG C, which greatly limits its application, therefore the oxidation protection problem of C/C matrix material becomes one of study hotspot in recent years.Carry out high-temperature oxidation resistant protection to it to have great importance to the application of its high temperature simultaneously.
Oxidation resistant coating is considered to the effective ways solving carbon/carbon compound material oxidant protection under high temperature problem.The physics of SiC coating and C/C matrix material, chemical compatibility are good and generally use as transition layer, but single SiC coating can not provide effective protection to C/C matrix, and thus anti-oxidant external coating (EC) becomes current study hotspot.
Up to the present, the compound coating of preparation has a variety of, the crystal whisker toughened MoSi of such as SiC
2-SiC-Si coating [FuQian-Gang, LiHe-Jun, LiKe-Zhi, ShiXiao-Hong, HuZhi-Biao, HuangMin, SiCwhisker-toughenedMoSi
2-SiC-Sicoatingtoprotectcarbon/carboncompositesagainstoxid ation, Carbon.2006,44,1866.], MoSi
2/ SiC coating [HuangJF, WangB, LiHJ, etal.AMoSi
2/ SiCoxidationprotectivecoatingforcarbon/carboncomposites. CorrosionScience, 2011,2 (53): 834-839.], SiC-MoSi
2-(Ti
0.8mo
0.2) Si
2compound coating [JiaoGS, LiHJ, LiKZ, etal.SiC-MoSi
2-(Ti
0.8mo
0.2) Si
2multi-compositioncoatingforcarbon/carboncomposites.Surf. Coat.Technol, 2006,201 (6): 3452-3456.] etc.The compound coating of preparation can play effective protective effect to C/C matrix material.But also need continuous effort in order to make oxidation resistant coating towards future developments such as long lifetime, high temperature resistant, antiscours.(thermal expansivity is 5.0 × 10 to mullite
-6/ DEG C) stupalith refractoriness is high, good thermal shock, chemical resistance of concrete, creep resistance, refractoriness under load are high, volume stability good, is desirable high grade refractory, is widely used in each field.SiC whisker has and the feature such as mullite thermal expansivity is close, high temperature resistant, intensity is high, Young's modulus is high, chemical stability is good, become the effective way improving mullite ceramic toughness and reliability, and up to the present, with its research as oxidation resistant coating also rarely found report.
Up to the present the preparation method of external coating (EC) is varied, mainly contains following several: supercritical fluid technology, chemical vapour deposition, entrapping method, formed in situ, sol-gel method, molten slurry coating reaction, detonation flame spraying and ultrasonic spray method etc.Adopt supercritical fluid technology to prepare C/C composite coating due to the process implementing of preparation to need to carry out at high temperature under high pressure, higher to the requirement of equipment, and the external coating (EC) formed will be heat-treated under an inert atmosphere, long [the BemeburgPL of preparation cycle, KrukonisVJ.Processingofcarbon/carboncompositesusingsuper criticalfluidtechnology [P] .UnitedStatesPatentUS5035921, 1991], the coating adopting formed in situ legal system standby needs pyroprocessing at 1500 DEG C, and can not once prepare [HuangJian-Feng, LiHe-Jun, ZengXie-Rong, LiKe-Zhi.Surf.coat.Technol.2006, 200, 5379.], easily ftracture and coat-thickness deficiency [HuangJian-Feng in the external coating (EC) surface adopting sol-gel method to prepare, ZengXie-Rong, LiHe-Jun, XiongXin-Bo, SunGuo-ling.Surf.coat.Technol.2005, 190, 255.], although and adopt detonation flame spraying and ultrasonic spray method to prepare alloy part coating, but, this technique also has a lot of incomplete place, the high-temp antioxidizing performance of prepared coating is still needed and will further be improved [TerentievaVS, BogachkovaOP, GoriatchevaEV.Methodforprotectingproductsmadeofarefracto rymaterialagainstoxidation, andresultingproducts [p] .US5677060, 1997.].And the method adopting electromagnetic induction heating-two pulse electrophoretic deposition method to prepare SiC crystal whisker toughened mullite compound external coating (EC) have not been reported.
Summary of the invention
The object of the present invention is to provide the preparation method of the crystal whisker toughened mullite compound coating of a kind of carbon/carbon compound material SiC, adopt this method can prepare thickness evenly, without the carbon/carbon compound material SiC crystal whisker toughened mullite compound external coating (EC) of through-wall crack and micropore, and its processing unit is simple, reaction time is short, and cost is low.
For achieving the above object, present invention employs following technical scheme:
1) first the mixed powder that mullite powder and SiC whisker form is scattered in 50 ~ 80mL butanols and is mixed with the suspending liquid A 1 that mixed powder concentration is 30 ~ 45g/L, in mixed powder, the massfraction of SiC whisker is 20 ~ 40%, the massfraction of mullite powder is 60 ~ 80%, by suspending liquid A 1 ultrasonic vibration 5 ~ 10min, then limit heating edge stirs 1 ~ 2h on magnetic stirring apparatus, obtain suspending liquid A 2, heating and temperature control is at 60 ~ 80 DEG C;
2) in suspending liquid A 2, add iodate carbon and obtain mixture, in mixture, the concentration of iodate carbon is 0.5 ~ 1.0g/L, mixture is stirred 1 ~ 2h on magnetic stirring apparatus, heats in stirring simultaneously, and heating and temperature control, at 60 ~ 80 DEG C, obtains suspension B;
3) pouring suspension B into one with Graphite Electrodes is anode, conducting base is in the water heating kettle of negative electrode, C/C composite sample with SiC coating is clipped on negative electrode, then electromagnetic induction heater is put into after being sealed by water heating kettle, then negative and positive the two poles of the earth of water heating kettle be connected with the pulse power and carry out electromagnetic induction heating two pulse electrophoretic deposition, in deposition process, the heating current of electromagnetic induction heater controls at 200 ~ 300A, the insulation power current of electromagnetic induction heater controls 200 ~ 300A (making hydrothermal temperature control at 180 ~ 250 DEG C), pulse power voltage is 220V, pulse power periodic Control is at 1000 ~ 3000ms, pulse power peak value comparison method is at 40 ~ 60A, pulse power direct impulse working time control is at 400 ~ 800ms, pulse power reverse impulse working time control is at 100 ~ 300ms, the positive and negative pulse width control of the pulse power is at 100 ~ 300 μ s, pulse power group working time control is at 8 ~ 12min, pulse power net cycle time controls at 10 ~ 25min, room temperature is naturally cooled to after deposition terminates,
4) through step 3) after, open water heating kettle and take out sample, then by the sample that takes out in electric drying oven with forced convection at 40 ~ 80 DEG C dry 2 ~ 6h.
The length-to-diameter ratio of described SiC whisker is 50 ~ 100, and the median size of mullite powder controls at 50 ~ 100nm, purity >=99.7% of iodate carbon, purity >=99.8% of butanols.
The ultrasonic power of described ultrasonic vibration is 500 ~ 1000W.
The compactedness of described water heating kettle controls 50 ~ 80%.
Beneficial effect of the present invention is embodied in:
1) the present invention prepare carbon/carbon compound material SiC crystal whisker toughened mullite compound external coating (EC) surface flawless, external coating (EC) is combined closely with SiC undercoat;
2) the present invention can obtain structure-controllable and carbon/carbon compound material SiC of good performance crystal whisker toughened mullite compound external coating (EC) at low temperatures;
3) preparation technology of the present invention is simple, and easy to operate, raw material is easy to get, and preparation cost is lower, has vast potential for future development.
Accompanying drawing explanation
Fig. 1 be embodiment 5 prepare carbon/carbon compound material SiC crystal whisker toughened mullite compound external coating (EC) surperficial SEM photo;
Fig. 2 is the XRD figure spectrum of carbon/carbon compound material SiC crystal whisker toughened mullite compound external coating (EC) prepared by embodiment 5.
Embodiment
Below in conjunction with drawings and Examples, the present invention is elaborated.
Embodiment 1:
1) commercially available SiC whisker (length-to-diameter ratio is 50 ~ 100) is selected, (commercially available mullite powder is through dry ball milling about 45h for mullite powder, median size controls at about 100nm), iodate carbon (purity >=99.7%), and butanols (purity >=99.8%) is raw material;
2) first the mixed powder of mullite powder and SiC whisker composition is scattered in 50mL butanols, be mixed with the suspending liquid A 1 that mixed powder concentration is 30g/L, in mixed powder, the massfraction of SiC whisker is 20%, the massfraction of mullite powder is 80%, and by suspending liquid A 1 ultrasonic vibration 10min, ultrasonic power is 500W, then be placed on magnetic stirring apparatus and stir 1h, heat in stirring, heating and temperature control, at 60 DEG C, obtains suspending liquid A 2 simultaneously;
3) in suspending liquid A 2, add iodate carbon and obtain mixture, in mixture, the concentration of iodate carbon is 0.5g/L, is placed on by mixture on magnetic stirring apparatus and stirs 1h, heat in stirring simultaneously, and heating and temperature control, at 60 DEG C, obtains suspension B;
4) pouring suspension B into one with Graphite Electrodes is anode, conducting base is in the water heating kettle of negative electrode, compactedness is 50%, C/C composite sample with SiC coating is clipped in (sample floods into suspension B) on the negative electrode in this water heating kettle, then electromagnetic induction heater is put into after being sealed by this water heating kettle, then negative and positive the two poles of the earth of this water heating kettle are connected to SMD-P type intelligence multipulse electroplating power supply (great Shun electroplating device company limited of Handan City) corresponding the two poles of the earth and carry out electromagnetic induction heating two pulse electrophoretic deposition: the heating current of electromagnetic induction heater controls at 200A, insulation power current controls at 200A, hydrothermal temperature controls at 180 DEG C.Pulse power voltage is 220V, periodic Control is at 1000ms, peak value comparison method is at 40A, direct impulse working time control is at 400ms, reverse impulse working time control is at 100ms, and positive and negative pulse width control is at 100 μ s, and group working time control is at 9min, net cycle time controls at 20min, naturally cools to room temperature after deposition terminates;
5) through step 4) after, open above-mentioned water heating kettle, take out sample, then by take out sample in electric drying oven with forced convection at 40 DEG C dry 6h, obtain carbon/carbon compound material SiC crystal whisker toughened mullite compound external coating (EC).
Embodiment 2:
1) commercially available SiC whisker (length-to-diameter ratio is 50 ~ 100) is selected, (commercially available mullite powder is through dry ball milling about 45h for mullite powder, median size controls at about 100nm), iodate carbon (purity >=99.7%), and butanols (purity >=99.8%) is raw material;
2) first the mixed powder of mullite powder and SiC whisker composition is scattered in 50mL butanols, be mixed with the suspending liquid A 1 that mixed powder concentration is 30g/L, in mixed powder, the massfraction of SiC whisker is 30%, the massfraction of mullite powder is 70%, and by suspending liquid A 1 ultrasonic vibration 8min, ultrasonic power is 600W, then be placed on magnetic stirring apparatus and stir 1h, heat in stirring, heating and temperature control, at 60 DEG C, obtains suspending liquid A 2 simultaneously;
3) in suspending liquid A 2, add iodate carbon and obtain mixture, in mixture, the concentration of iodate carbon is 0.5g/L, is placed on by mixture on magnetic stirring apparatus and stirs 1h, heat in stirring simultaneously, and heating and temperature control, at 60 DEG C, obtains suspension B;
4) pouring suspension B into one with Graphite Electrodes is anode, conducting base is in the water heating kettle of negative electrode, compactedness is 50%, C/C composite sample with SiC coating is clipped in (sample floods into suspension B) on the negative electrode in this water heating kettle, then electromagnetic induction heater is put into after being sealed by this water heating kettle, then negative and positive the two poles of the earth of this water heating kettle are connected to SMD-P type intelligence corresponding the two poles of the earth of multipulse electroplating power supply and carry out electromagnetic induction heating two pulse electrophoretic deposition: the heating current of electromagnetic induction heater controls at 220A, insulation power current controls at 220A, hydrothermal temperature controls at 190 DEG C.Pulse power voltage is 220V, periodic Control is at 1500ms, peak value comparison method is at 45A, direct impulse working time control is at 400ms, reverse impulse working time control is at 100ms, and positive and negative pulse width control is at 100 μ s, and group working time control is at 11min, net cycle time controls at 25min, naturally cools to room temperature after deposition terminates;
5) through step 4) after, open above-mentioned water heating kettle, take out sample, then by take out sample in electric drying oven with forced convection at 50 DEG C dry 5h, obtain carbon/carbon compound material SiC crystal whisker toughened mullite compound external coating (EC).
Embodiment 3:
1) commercially available SiC whisker (length-to-diameter ratio is 50 ~ 100) is selected, (commercially available mullite powder is through dry ball milling about 45h for mullite powder, median size controls at about 100nm), iodate carbon (purity >=99.7%), and butanols (purity >=99.8%) is raw material;
2) first the mixed powder of mullite powder and SiC whisker composition is scattered in 60mL butanols, be mixed with the suspending liquid A 1 that mixed powder concentration is 45g/L, in mixed powder, the massfraction of SiC whisker is 35%, the massfraction of mullite powder is 65%, and by suspending liquid A 1 ultrasonic vibration 6min, ultrasonic power is 800W, then be placed on magnetic stirring apparatus and stir 2h, heat in stirring, heating and temperature control, at 60 DEG C, obtains suspending liquid A 2 simultaneously;
3) in suspending liquid A 2, add iodate carbon and obtain mixture, in mixture, the concentration of iodate carbon is 0.5g/L, is placed on by mixture on magnetic stirring apparatus and stirs 2h, heat in stirring simultaneously, and heating and temperature control, at 60 DEG C, obtains suspension B;
4) pouring suspension B into one with Graphite Electrodes is anode, conducting base is in the water heating kettle of negative electrode, compactedness is 60%, C/C composite sample with SiC coating is clipped in (sample floods into suspension B) on the negative electrode in this water heating kettle, then electromagnetic induction heater is put into after being sealed by this water heating kettle, then negative and positive the two poles of the earth of this water heating kettle are connected to SMD-P type intelligence corresponding the two poles of the earth of multipulse electroplating power supply and carry out electromagnetic induction heating two pulse electrophoretic deposition: the heating current of electromagnetic induction heater controls at 240A, insulation power current controls at 240A, hydrothermal temperature controls at 200 DEG C.Pulse power voltage is 220V, periodic Control is at 1500ms, peak value comparison method is at 50A, direct impulse working time control is at 400ms, reverse impulse working time control is at 200ms, and positive and negative pulse width control is at 200 μ s, and group working time control is at 10min, net cycle time controls at 12min, naturally cools to room temperature after deposition terminates;
5) through step 4) after, open above-mentioned water heating kettle, take out sample, then by take out sample in electric drying oven with forced convection at 60 DEG C dry 4h, obtain carbon/carbon compound material SiC crystal whisker toughened mullite compound external coating (EC).
Embodiment 4:
1) commercially available SiC whisker (length-to-diameter ratio is 50 ~ 100) is selected, (commercially available mullite powder is through dry ball milling about 45h for mullite powder, median size controls at about 100nm), iodate carbon (purity >=99.7%), and butanols (purity >=99.8%) is raw material;
2) first the mixed powder of mullite powder and SiC whisker composition is scattered in 70mL butanols, be mixed with the suspending liquid A 1 that mixed powder concentration is 35g/L, in mixed powder, the massfraction of SiC whisker is 40%, the massfraction of mullite powder is 60%, and by suspending liquid A 1 ultrasonic vibration 6min, ultrasonic power is 800W, then be placed on magnetic stirring apparatus and stir 2h, heat in stirring, heating and temperature control, at 60 DEG C, obtains suspending liquid A 2 simultaneously;
3) in suspending liquid A 2, add iodate carbon and obtain mixture, in mixture, the concentration of iodate carbon is 1.0g/L, is placed on by mixture on magnetic stirring apparatus and stirs 2h, heat in stirring simultaneously, and heating and temperature control, at 60 DEG C, obtains suspension B;
4) pouring suspension B into one with Graphite Electrodes is anode, conducting base is in the water heating kettle of negative electrode, compactedness is 70%, C/C composite sample with SiC coating is clipped in (sample floods into suspension B) on the negative electrode in this water heating kettle, then electromagnetic induction heater is put into after being sealed by this water heating kettle, then negative and positive the two poles of the earth of this water heating kettle are connected to SMD-P type intelligence corresponding the two poles of the earth of multipulse electroplating power supply and carry out electromagnetic induction heating two pulse electrophoretic deposition: the heating current of electromagnetic induction heater controls at 260A, insulation power current controls at 260A, hydrothermal temperature controls at 210 DEG C.Pulse power voltage is 220V, periodic Control is at 2000ms, peak value comparison method is at 55A, direct impulse working time control is at 600ms, reverse impulse working time control is at 200ms, and positive and negative pulse width control is at 200 μ s, and group working time control is at 8min, net cycle time controls at 25min, naturally cools to room temperature after deposition terminates;
5) through step 4) after, open above-mentioned water heating kettle, take out sample, then by take out sample in electric drying oven with forced convection at 60 DEG C dry 4h, obtain carbon/carbon compound material SiC crystal whisker toughened mullite compound external coating (EC).
Embodiment 5:
1) commercially available SiC whisker (length-to-diameter ratio is 50 ~ 100) is selected, (commercially available mullite powder is through dry ball milling about 45h for mullite powder, median size controls at about 100nm), iodate carbon (purity >=99.7%), and butanols (purity >=99.8%) is raw material;
2) first the mixed powder of mullite powder and SiC whisker composition is scattered in 80mL butanols, be mixed with the suspending liquid A 1 that mixed powder concentration is 40g/L, in mixed powder, the massfraction of SiC whisker is 25%, the massfraction of mullite powder is 75%, and by suspending liquid A 1 ultrasonic vibration 5min, ultrasonic power is 1000W, then be placed on magnetic stirring apparatus and stir 2h, heat in stirring, heating and temperature control, at 80 DEG C, obtains suspending liquid A 2 simultaneously;
3) in suspending liquid A 2, add iodate carbon and obtain mixture, in mixture, the concentration of iodate carbon is 1.0g/L, is placed on by mixture on magnetic stirring apparatus and stirs 2h, heat in stirring simultaneously, and heating and temperature control, at 80 DEG C, obtains suspension B;
4) pouring suspension B into one with Graphite Electrodes is anode, conducting base is in the water heating kettle of negative electrode, compactedness is 80%, C/C composite sample with SiC coating is clipped in (sample floods into suspension B) on the negative electrode in this water heating kettle, then electromagnetic induction heater is put into after being sealed by this water heating kettle, then negative and positive the two poles of the earth of this water heating kettle are connected to SMD-P type intelligence corresponding the two poles of the earth of multipulse electroplating power supply and carry out electromagnetic induction heating two pulse electrophoretic deposition: the heating current of electromagnetic induction heater controls at 300A, insulation power current controls at 300A, hydrothermal temperature controls at 250 DEG C.Pulse power voltage is 220V, periodic Control is at 3000ms, peak value comparison method is at 60A, direct impulse working time control is at 800ms, reverse impulse working time control is at 300ms, and positive and negative pulse width control is at 300 μ s, and group working time control is at 12min, net cycle time controls at 25min, naturally cools to room temperature after deposition terminates;
5) through step 4) after, open above-mentioned water heating kettle, take out sample, then by take out sample in electric drying oven with forced convection at 80 DEG C dry 2h, obtain carbon/carbon compound material SiC crystal whisker toughened mullite compound external coating (EC).
As can be seen from Fig. 1 and Fig. 2, external coating (EC) prepared by the present invention consists of mullite (3Al
2o
3siO
2) and SiC, surfacing is even, comparatively fine and close, surperficial flawless.
First the feature of electromagnetic induction heating-two pulse electrophoretic deposition method is the sedimentation rate accelerating suspended particle under hydro-thermal supercritical environment, and suspended particle can be reacted at matrix surface rapidly.Electromagnetic induction heating technology is a kind of novel heating technique, it is according to electromagnetic induction principle, utilize the heat that in heated object, eddy current produces to carry out heating, compare with traditional type of heating, its heating efficiency is high, speed is fast, reliability is high, be easy to the heating realizing high temperature and local, and be widely used in industry heating field.Electromagnetic induction heating can make to produce localized hyperthermia and high pressure rapidly in reaction system simultaneously, the Activation energy of effective reduction SiC whisker and mullite Multiphase suspended particles, make it react in water heat electrophoresis deposition process more completely with abundant, thus obtain the coating of compact structure.Secondly, be under the positive and negative pulse power, the intermittence electric discharge of negative and positive the two poles of the earth, makes suspended particle be deposited on matrix surface, avoids the coating non-uniform phenomenon that the electric discharge of traditional continuous arcing produces, thus obtains the coating of compact structure.Adopt this method can avoid adopting conventional high-temperature coating and the phase transformation that causes and embrittlement, solve the thermal damage to matrix in coating preparation process to a certain extent; Simultaneously because deposition process is non-streamlined process, uniform settled layer can be formed at matrix surface that is complex-shaped or porous surface, and can accurately control coated component, thickness and porosity, make the heterogeneous compound coating of simple efficient preparation and gradient ceramic coating become possibility; Moreover electrophoretic deposition is the displacement of charged particle, can not because of the bonding force of a large amount of gases affect coating of producing during brine electrolysis solvent and matrix.In addition, direct impulse controls coated grains size and impurity level, and reverse impulse controls sedimentation velocity and thickness distribution, achieves and obtains the crystal whisker toughened mullite coating of SiC fine and close, that have micro-flaw, different thickness in controlled conditions.Electromagnetic induction heating-two pulse electrophoretic deposition also has the features such as simple to operation, cost is low, depositing operation is easy to control.
Claims (4)
1. a preparation method for the crystal whisker toughened mullite compound coating of carbon/carbon compound material SiC, is characterized in that: comprise the following steps:
1) first the mixed powder that mullite powder and SiC whisker form is scattered in butanols and is mixed with the suspending liquid A 1 that mixed powder concentration is 30 ~ 45g/L, in mixed powder, the massfraction of SiC whisker is 20 ~ 40%, the massfraction of mullite powder is 60 ~ 80%, by suspending liquid A 1 ultrasonic vibration 5 ~ 10min, then limit heating edge stirs 1 ~ 2h on magnetic stirring apparatus, obtain suspending liquid A 2, heating and temperature control is at 60 ~ 80 DEG C;
2) in suspending liquid A 2, add iodate carbon and obtain mixture, in mixture, the concentration of iodate carbon is 0.5 ~ 1.0g/L, mixture is stirred 1 ~ 2h on magnetic stirring apparatus, heats in stirring simultaneously, and heating and temperature control, at 60 ~ 80 DEG C, obtains suspension B;
3) pouring suspension B into one with Graphite Electrodes is anode, conducting base is in the water heating kettle of negative electrode, C/C composite sample with SiC coating is clipped on negative electrode, then electromagnetic induction heater is put into after being sealed by water heating kettle, then negative and positive the two poles of the earth of water heating kettle be connected with the pulse power and carry out electromagnetic induction heating two pulse electrophoretic deposition, in deposition process, the heating current of electromagnetic induction heater controls at 200 ~ 300A, the insulation power current of electromagnetic induction heater controls at 200 ~ 300A, pulse power voltage is 220V, pulse power periodic Control is at 1000 ~ 3000ms, pulse power peak value comparison method is at 40 ~ 60A, pulse power direct impulse working time control is at 400 ~ 800ms, pulse power reverse impulse working time control is at 100 ~ 300ms, the positive and negative pulse width control of the pulse power is at 100 ~ 300 μ s, pulse power group working time control is at 8 ~ 12min, pulse power net cycle time controls at 10 ~ 25min, room temperature is naturally cooled to after deposition terminates,
4) through step 3) after, open water heating kettle and take out sample, then by the sample that takes out in electric drying oven with forced convection at 40 ~ 80 DEG C dry 2 ~ 6h.
2. the preparation method of the crystal whisker toughened mullite compound coating of a kind of carbon/carbon compound material SiC according to claim 1, it is characterized in that: the length-to-diameter ratio of described SiC whisker is 50 ~ 100, the median size of mullite powder controls at 50 ~ 100nm, purity >=99.7% of iodate carbon, purity >=99.8% of butanols.
3. the preparation method of the crystal whisker toughened mullite compound coating of a kind of carbon/carbon compound material SiC according to claim 1, is characterized in that: the ultrasonic power of described ultrasonic vibration is 500 ~ 1000W.
4. the preparation method of the crystal whisker toughened mullite compound coating of a kind of carbon/carbon compound material SiC according to claim 1, is characterized in that: the compactedness of described water heating kettle controls 50 ~ 80%.
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| CN106478153B (en) * | 2016-09-28 | 2019-02-22 | 陕西科技大学 | A kind of carbon/carbon compound material β-Y2Si2O7Nanowire-toughened mullite/silicate glass coating preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4774209A (en) * | 1987-01-27 | 1988-09-27 | Corning Glass Works | Mullite ceramic whisker composite article exhibiting high-temperature strength |
| CN101885623A (en) * | 2010-06-11 | 2010-11-17 | 陕西科技大学 | Method for preparing carbon/carbon composite material mullite external coating by pulsed hydrothermal electrophoresis sedimentation method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4774209A (en) * | 1987-01-27 | 1988-09-27 | Corning Glass Works | Mullite ceramic whisker composite article exhibiting high-temperature strength |
| CN101885623A (en) * | 2010-06-11 | 2010-11-17 | 陕西科技大学 | Method for preparing carbon/carbon composite material mullite external coating by pulsed hydrothermal electrophoresis sedimentation method |
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