CN104130022B - Carbon/carbon compound material ZrO 2the preparation method of particle and SiC whisker coordination plasticizing mullite compound coating - Google Patents
Carbon/carbon compound material ZrO 2the preparation method of particle and SiC whisker coordination plasticizing mullite compound coating Download PDFInfo
- Publication number
- CN104130022B CN104130022B CN201410328344.5A CN201410328344A CN104130022B CN 104130022 B CN104130022 B CN 104130022B CN 201410328344 A CN201410328344 A CN 201410328344A CN 104130022 B CN104130022 B CN 104130022B
- Authority
- CN
- China
- Prior art keywords
- carbon
- powder
- sic whisker
- mullite
- zro
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The invention provides a kind of carbon/carbon compound material ZrO
2the preparation method of particle and SiC whisker coordination plasticizing mullite compound coating: by mullite powder, SiC whisker and ZrO
2powder is scattered in butanols, stirs after ultrasonic vibration, heats to obtain suspending liquid A in stirring simultaneously; In suspending liquid A, add iodine, in stirring, heat to obtain suspension B simultaneously; Suspension B is poured into one be anode with Graphite Electrodes, in the conducting base water heating kettle that is negative electrode, carry out electromagnetic induction heating two pulse water heat electrophoresis deposition, take out samples dried; Carbon/carbon compound material ZrO prepared by the present invention
2particle and SiC whisker coordination plasticizing mullite compound external coating (EC) surface flawless, greatly, preparation technology is simple, and easy to operate, reaction time is short, and raw material is easy to get, and preparation cost is lower, has vast potential for future development for coating and substrate combinating strength.
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 a kind of electromagnetic induction heating-two pulse water heat electrophoresis deposition and prepare the non-microcracked generation of surface uniform, and the homogeneous carbon/carbon compound material ZrO produced without penetrability hole and crackle of thickness
2the method of particle and SiC whisker coordination plasticizing mullite compound external coating (EC).
Background technology
C/C matrix material take carbon fiber as the C-base composte material of wild phase, because it is made up of single carbon, not only there is the ablation resistance of carbon and graphite material excellence, the advantages such as low density, thermal expansivity are low, and also have excellent mechanical property under high temperature, as high strength, high-modulus, good fracture toughness property and wear resisting property.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.SiC coating is due to fabulous antioxidant property and good and generally to use as transition layer with the physics of C/C matrix material, chemical compatibility; 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 external coating (EC) of preparation has a variety of, such as Mullite-Al
2o
3-SiC coating [Huang Jian-Feng, Zeng Xie-Rong, Li He-Jun, Xiong Xin-Bo, Huang Min, Mullite-Al2O3-SiC oxidation protective coating for carbon/carbon composites.Carbon, 2003,41,2825-2829.], the crystal whisker toughened MoSi of SiC
2-SiC-Si coating [Fu Qian-Gang, Li He-Jun, Li Ke-Zhi, Shi Xiao-Hong, Hu Zhi-Biao, Huang Min, SiC whisker-toughened MoSi
2-SiC-Si coating to protect carbon/carbon composites against oxidation, Carbon.2006,44,1866.], MoSi
2/ SiC coating [Huang J F, Wang B, Li H J, et al.A MoSi
2/ SiC oxidation protective coating for carbon/carbon composites.Corrosion Science, 2011,2 (53): 834-839.] 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, in addition with ZrO
2the phase transformation coordination plasticizing of particle becomes 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, to sum up, ZrO
2particle and SiC whisker coordination plasticizing mullite oxidation resistant coating have good application prospect.
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 Bemeburg P L of preparation cycle, Krukonis V J.Processing of carbon/carbon composites using supercritical fluid technology [P] .United States Patent US5035921, 1991], the coating adopting formed in situ legal system standby needs pyroprocessing at 1500 DEG C, and once can not prepare [Huang Jian-Feng, Li He-Jun, Zeng Xie-Rong, Li Ke-Zhi.Surf.coat.Technol.2006, 200, 5379.], easily ftracture and coat-thickness deficiency [Huang Jian-Feng in the external coating (EC) surface adopting sol-gel method to prepare, Zeng Xie-Rong, Li He-Jun, Xiong Xin-Bo, Sun Guo-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 further will be improved [Terentieva V S, Bogachkova O P, Goriatcheva E V.Method for protecting products made of a refractory material against oxidation, and resulting products [p] .US5677060, 1997.].And adopt electromagnetic induction heating-two pulse water heat electrophoresis deposition method to prepare ZrO
2the method of particle and SiC whisker coordination plasticizing mullite compound external coating (EC) have not been reported.
Summary of the invention
The object of the present invention is to provide a kind of carbon/carbon compound material ZrO
2the preparation method of particle and SiC whisker coordination plasticizing mullite compound coating.
For achieving the above object, present invention employs following technical scheme:
1) by mullite powder, SiC whisker and ZrO
2the mixed powder of powder composition is scattered in 80 ~ 100mL butanols and is mixed with the suspending liquid A 1 that mixed powder concentration is 8 ~ 20g/L, and in mixed powder, the massfraction of mullite powder is the massfraction of 40 ~ 60%, SiC whisker is 20 ~ 50%, ZrO
2the massfraction of powder is 10 ~ 30%, and by suspending liquid A 1 ultrasonic vibration 10 ~ 20min, then on magnetic stirring apparatus, stir 36 ~ 48h, heat in stirring, heating and temperature control, at 40 ~ 60 DEG C, obtains suspending liquid A simultaneously;
2) in suspending liquid A, add iodine and obtain mixture, in mixture, the concentration of iodine is 0.2 ~ 0.5g/L, mixture is stirred 0.5 ~ 1h on magnetic stirring apparatus, heats in stirring simultaneously, and heating and temperature control, at 80 ~ 100 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 water heat electrophoresis deposition, in deposition process, the heating current of electromagnetic induction heater controls at 150 ~ 250A, the insulation power current of electromagnetic induction heater controls 100 ~ 150A (making hydrothermal temperature control at 100 ~ 150 DEG C), pulse power voltage is 220V, pulse power periodic Control is at 2000 ~ 2400ms, pulse power peak value comparison method is at 30 ~ 40A, pulse power direct impulse working time control is at 1800 ~ 2000ms, pulse power reverse impulse working time control is at 200 ~ 400ms, pulse power direct impulse width control system is at 150 ~ 300 μ s, pulse power reverse impulse width control system is at 100 ~ 200 μ s, pulse power group working time control is at 12 ~ 15min, pulse power net cycle time controls at 15 ~ 35min, room temperature is naturally cooled to after deposition terminates,
4) through step 3) after, open described 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 median size of described mullite powder controls at 100 ~ 200nm, ZrO
2the median size of powder controls at 1 ~ 3 μm, and the length-to-diameter ratio of SiC whisker is 50 ~ 100, purity>=99.7% of iodine, purity>=99.8% of butanols.
The ultrasonic power of described ultrasonic vibration is 500 ~ 1000W.
The compactedness of described water heating kettle controls 50 ~ 63%.
Beneficial effect of the present invention is embodied in:
1) the carbon/carbon compound material ZrO for preparing of the present invention
2particle and SiC whisker coordination plasticizing mullite compound external coating (EC) thickness are evenly, without through-wall crack and micropore, be combined closely with SiC undercoat.
2) the present invention can obtain structure-controllable and carbon/carbon compound material ZrO of good performance at low temperatures
2particle and SiC whisker coordination plasticizing mullite compound external coating (EC).
3) the present invention adopts the method for electromagnetic induction heating, and rate of heating is fast, and efficiency is high, and homogeneous temperature.
4) the present invention adopts dual-pulse power supply (positive back pulse), and the coatingsurface of preparation is smooth, and thickness is even.
5) the present invention once completes in water heating kettle, does not need Post isothermal treatment, and preparation technology is simple, and easy to operate, reaction time is short, and raw material is easy to get, and preparation cost is lower, has vast potential for future development.
Accompanying drawing explanation
Fig. 1 is carbon/carbon compound material ZrO prepared by embodiment 3
2the surperficial SEM photo of particle and SiC whisker coordination plasticizing mullite compound external coating (EC).
Fig. 2 is carbon/carbon compound material ZrO prepared by embodiment 3
2the XRD figure spectrum of particle and SiC whisker coordination plasticizing mullite compound external coating (EC).
Embodiment
Below in conjunction with drawings and Examples, the present invention is elaborated.
Embodiment 1:
1) mullite powder (through dry ball milling about 45h, median size controls at about 150nm commercially available mullite powder) is selected, ZrO
2powder (commercially available ZrO
2powder is through dry ball milling about 45h, and median size controls at about 2 μm), commercially available SiC whisker (length-to-diameter ratio is 50 ~ 100), iodine (purity>=99.7%), and butanols (purity>=99.8%) is raw material;
2) first by mullite powder, SiC whisker and ZrO
2the mixed powder of powder composition is scattered in 80mL butanols, and be mixed with the suspending liquid A 1 that mixed powder concentration is 16g/L, in mixed powder, the massfraction of mullite powder is the massfraction of 50%, SiC whisker is 40%, ZrO
2the massfraction of powder is 10%, and by suspending liquid A 1 ultrasonic vibration 10min, ultrasonic power is 1000W, is then placed on magnetic stirring apparatus and stirs 36h, heat in stirring simultaneously, and heating and temperature control, at 60 DEG C, obtains suspending liquid A;
3) in suspending liquid A, add iodine and obtain mixture, in mixture, the concentration of iodine is 0.5g/L, is placed on by mixture on magnetic stirring apparatus and stirs 1h, heat in stirring simultaneously, and Heating temperature is 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 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 water heat electrophoresis deposition: the heating current of electromagnetic induction heater controls at 250A, insulation power current controls at 150A, hydrothermal temperature controls at 150 DEG C, pulse power voltage is 220V, periodic Control is at 2000ms, peak value comparison method is at 30A, direct impulse working time control is at 1800ms, and reverse impulse working time control is at 200ms, and direct impulse width control system is at 200 μ s, reverse impulse width control system is at 100 μ s, group working time control is at 12min, and 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 the sample of taking-up in electric drying oven with forced convection at 50 DEG C dry 4h namely obtain carbon/carbon compound material ZrO
2particle and SiC whisker coordination plasticizing mullite compound external coating (EC).
Embodiment 2:
1) mullite powder (through dry ball milling about 45h, median size controls at about 150nm commercially available mullite powder) is selected, ZrO
2powder (commercially available ZrO
2powder is through dry ball milling about 45h, and median size controls at about 2 μm), commercially available SiC whisker (length-to-diameter ratio is 50 ~ 100), iodine (purity>=99.7%), and butanols (purity>=99.8%) is raw material;
2) first by mullite powder, SiC whisker and ZrO
2the mixed powder of powder composition is scattered in 90mL butanols, and be mixed with the suspending liquid A 1 that mixed powder concentration is 10g/L, in mixed powder, the massfraction of mullite powder is the massfraction of 55%, SiC whisker is 35%, ZrO
2the massfraction of powder is 10%, and by suspending liquid A 1 ultrasonic vibration 15min, ultrasonic power is 800W, is then placed on magnetic stirring apparatus and stirs 36h, heat in stirring simultaneously, and heating and temperature control, at 60 DEG C, obtains suspending liquid A;
3) in suspending liquid A, add iodine and obtain mixture, in mixture, the concentration of iodine is 0.5g/L, is placed on by mixture on magnetic stirring apparatus and stirs 1h, heat in stirring simultaneously, and Heating temperature is 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 57%, 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 water heat electrophoresis deposition: the heating current of electromagnetic induction heater controls at 150A, insulation power current controls at 150A, hydrothermal temperature controls at 120 DEG C, pulse power voltage is 220V, periodic Control is at 2200ms, peak value comparison method is at 30A, direct impulse working time control is at 1900ms, and reverse impulse working time control is at 300ms, and direct impulse width control system is at 150 μ s, reverse impulse width control system is at 100 μ s, group working time control is at 12min, and net cycle time controls at 15min, naturally cools to room temperature after deposition terminates,
5) through step 4) after, open above-mentioned water heating kettle, take out sample, then by the sample of taking-up in electric drying oven with forced convection at 50 DEG C dry 5h namely obtain carbon/carbon compound material ZrO
2particle and SiC whisker coordination plasticizing mullite compound external coating (EC).
Embodiment 3:
1) mullite powder (through dry ball milling about 45h, median size controls at about 150nm commercially available mullite powder) is selected, ZrO
2powder (commercially available ZrO
2powder is through dry ball milling about 45h, and median size controls at about 2 μm), commercially available SiC whisker (length-to-diameter ratio is 50 ~ 100), iodine (purity>=99.7%), and butanols (purity>=99.8%) is raw material;
2) first by mullite powder, SiC whisker and ZrO
2the mixed powder of powder composition is scattered in 100mL butanols, and be mixed with the suspending liquid A 1 that mixed powder concentration is 15g/L, in mixed powder, the massfraction of mullite powder is the massfraction of 60%, SiC whisker is 20%, ZrO
2the massfraction of powder is 20%, and by suspending liquid A 1 ultrasonic vibration 20min, ultrasonic power is 500W, is then placed on magnetic stirring apparatus and stirs 40h, heat in stirring simultaneously, and heating and temperature control, at 50 DEG C, obtains suspending liquid A;
3) in suspending liquid A, add iodine and obtain mixture, in mixture, the concentration of iodine is 0.2g/L, is placed on by mixture on magnetic stirring apparatus and stirs 0.8h, heat in stirring simultaneously, and Heating temperature is 90 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 63%, 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 water heat electrophoresis deposition: the heating current of electromagnetic induction heater controls at 250A, insulation power current controls at 120A, hydrothermal temperature controls at 120 DEG C, pulse power voltage is 220V, periodic Control is at 2400ms, peak value comparison method is at 35A, direct impulse working time control is at 2000ms, and reverse impulse working time control is at 400ms, and direct impulse width control system is at 180 μ s, reverse impulse width control system is at 180 μ s, group working time control is at 15min, and 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 the sample of taking-up in electric drying oven with forced convection at 60 DEG C dry 3h namely obtain carbon/carbon compound material ZrO
2particle and SiC whisker coordination plasticizing mullite compound external coating (EC).
Embodiment 4:
1) mullite powder (through dry ball milling about 45h, median size controls at about 150nm commercially available mullite powder) is selected, ZrO
2powder (commercially available ZrO
2powder is through dry ball milling about 45h, and median size controls 2
μabout m), commercially available SiC whisker (length-to-diameter ratio is 50 ~ 100), iodine (purity>=99.7%), and butanols (purity>=99.8%) is raw material;
2) first by mullite powder, SiC whisker and ZrO
2the mixed powder of powder composition is scattered in 90mL butanols, and be mixed with the suspending liquid A 1 that mixed powder concentration is 18g/L, in mixed powder, the massfraction of mullite powder is the massfraction of 40%, SiC whisker is 30%, ZrO
2the massfraction of powder is 30%, and by suspending liquid A 1 ultrasonic vibration 20min, ultrasonic power is 500W, is then placed on magnetic stirring apparatus and stirs 40h, heat in stirring simultaneously, and heating and temperature control, at 45 DEG C, obtains suspending liquid A;
3) in suspending liquid A, add iodine and obtain mixture, in mixture, the concentration of iodine is 0.3g/L, is placed on by mixture on magnetic stirring apparatus and stirs 0.5h, heat in stirring simultaneously, and Heating temperature is 100 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 57%, 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 water heat electrophoresis deposition: the heating current of electromagnetic induction heater controls at 180A, insulation power current controls at 120A, hydrothermal temperature controls at 100 DEG C, pulse power voltage is 220V, periodic Control is at 2200ms, peak value comparison method is at 35A, direct impulse working time control is at 2000ms, and reverse impulse working time control is at 200ms, and direct impulse width control system is at 200 μ s, reverse impulse width control system is at 150 μ s, group working time control is at 15min, and net cycle time controls at 35min, naturally cools to room temperature after deposition terminates,
5) through step 4) after, open above-mentioned water heating kettle, take out sample, then by the sample of taking-up in electric drying oven with forced convection at 70 DEG C dry 2h namely obtain carbon/carbon compound material ZrO
2particle and SiC whisker coordination plasticizing mullite compound external coating (EC).
Embodiment 5:
1) mullite powder (through dry ball milling about 45h, median size controls at about 150nm commercially available mullite powder) is selected, ZrO
2powder (commercially available ZrO
2powder is through dry ball milling about 45h, and median size controls at about 2 μm), commercially available SiC whisker (length-to-diameter ratio is 50 ~ 100), iodine (purity>=99.7%), and butanols (purity>=99.8%) is raw material;
2) first by mullite powder, SiC whisker and ZrO
2the mixed powder of powder composition is scattered in 100mL butanols, and be mixed with the suspending liquid A 1 that mixed powder concentration is 20g/L, in mixed powder, the massfraction of mullite powder is the massfraction of 60%, SiC whisker is 30%, ZrO
2the massfraction of powder is 10%, and by suspending liquid A 1 ultrasonic vibration 15min, ultrasonic power is 800W, is then placed on magnetic stirring apparatus and stirs 45h, heat in stirring simultaneously, and heating and temperature control, at 55 DEG C, obtains suspending liquid A;
3) in suspending liquid A, add iodine and obtain mixture, in mixture, the concentration of iodine is 0.5g/L, is placed on by mixture on magnetic stirring apparatus and stirs 0.5h, heat in stirring simultaneously, and Heating temperature is 95 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 63%, 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 water heat electrophoresis deposition: the heating current of electromagnetic induction heater controls at 180A, insulation power current controls at 120A, hydrothermal temperature controls at 150 DEG C, pulse power voltage is 220V, periodic Control is at 2100ms, peak value comparison method is at 40A, direct impulse working time control is at 1800ms, and reverse impulse working time control is at 300ms, and direct impulse width control system is at 300 μ s, reverse impulse width control system is at 200 μ s, group working time control is at 15min, and net cycle time controls at 18min, naturally cools to room temperature after deposition terminates,
5) through step 4) after, open above-mentioned water heating kettle, take out sample, then by the sample of taking-up in electric drying oven with forced convection at 40 DEG C dry 5h namely obtain carbon/carbon compound material ZrO
2particle and SiC whisker coordination plasticizing 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), SiC and ZrO
2, surface particles proper alignment, comparatively dense uniform.
First electromagnetic induction heating-its feature of two pulse water heat electrophoresis 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, effectively reduces ZrO
2the Activation energy of particle, SiC whisker and mullite Multiphase suspended particles, makes it react in water heat electrophoresis deposition process more completely with abundant, thus obtains 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.The phase transformation that employing the method can be avoided adopting conventional high-temperature coating and cause 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 ZrO fine and close, that have micro-flaw, different thickness in controlled conditions
2particle and SiC whisker coordination plasticizing mullite coating.Electromagnetic induction heating-two pulse water heat electrophoresis deposition also has the features such as simple to operation, cost is low, depositing operation is easy to control.
Claims (4)
1. a carbon/carbon compound material ZrO
2the preparation method of particle and SiC whisker coordination plasticizing mullite compound coating, is characterized in that: comprise the following steps:
1) by mullite powder, SiC whisker and ZrO
2the mixed powder of powder composition is scattered in butanols and is mixed with the suspending liquid A 1 that mixed powder concentration is 8 ~ 20g/L, and in mixed powder, the massfraction of mullite powder is the massfraction of 40 ~ 60%, SiC whisker is 20 ~ 50%, ZrO
2the massfraction of powder is 10 ~ 30%, and by suspending liquid A 1 ultrasonic vibration 10 ~ 20min, then on magnetic stirring apparatus, stir 36 ~ 48h, heat in stirring, heating and temperature control, at 40 ~ 60 DEG C, obtains suspending liquid A simultaneously;
2) in suspending liquid A, add iodine and obtain mixture, in mixture, the concentration of iodine is 0.2 ~ 0.5g/L, mixture is stirred 0.5 ~ 1h on magnetic stirring apparatus, heats in stirring simultaneously, and heating and temperature control, at 80 ~ 100 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 water heat electrophoresis deposition, in deposition process, the heating current of electromagnetic induction heater controls at 150 ~ 250A, the insulation power current of electromagnetic induction heater controls at 100 ~ 150A, pulse power voltage is 220V, pulse power periodic Control is at 2000 ~ 2400ms, pulse power peak value comparison method is at 30 ~ 40A, pulse power direct impulse working time control is at 1800 ~ 2000ms, pulse power reverse impulse working time control is at 200 ~ 400ms, pulse power direct impulse width control system is at 150 ~ 300 μ s, pulse power reverse impulse width control system is at 100 ~ 200 μ s, pulse power group working time control is at 12 ~ 15min, pulse power net cycle time controls at 15 ~ 35min, room temperature is naturally cooled to after deposition terminates,
4) through step 3) after, open described 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. a kind of carbon/carbon compound material ZrO according to claim 1
2the preparation method of particle and SiC whisker coordination plasticizing mullite compound coating, is characterized in that: the median size of described mullite powder controls at 100 ~ 200nm, ZrO
2the median size of powder controls at 1 ~ 3 μm, and the length-to-diameter ratio of SiC whisker is 50 ~ 100, purity>=99.7% of iodine, purity>=99.8% of butanols.
3. a kind of carbon/carbon compound material ZrO according to claim 1
2the preparation method of particle and SiC whisker coordination plasticizing mullite compound coating, is characterized in that: the ultrasonic power of described ultrasonic vibration is 500 ~ 1000W.
4. a kind of carbon/carbon compound material ZrO according to claim 1
2the preparation method of particle and SiC whisker coordination plasticizing mullite compound coating, is characterized in that: the compactedness of described water heating kettle controls 50 ~ 63%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410328344.5A CN104130022B (en) | 2014-07-10 | 2014-07-10 | Carbon/carbon compound material ZrO 2the preparation method of particle and SiC whisker coordination plasticizing mullite compound coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410328344.5A CN104130022B (en) | 2014-07-10 | 2014-07-10 | Carbon/carbon compound material ZrO 2the preparation method of particle and SiC whisker coordination plasticizing mullite compound coating |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104130022A CN104130022A (en) | 2014-11-05 |
| CN104130022B true CN104130022B (en) | 2015-11-04 |
Family
ID=51802931
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410328344.5A Active CN104130022B (en) | 2014-07-10 | 2014-07-10 | Carbon/carbon compound material ZrO 2the preparation method of particle and SiC whisker coordination plasticizing mullite compound coating |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104130022B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105413603B (en) | 2015-11-09 | 2017-12-05 | 陕西科技大学 | It is effectively improved the composite preparation system and method for composite material interface combination |
| 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 |
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 |
-
2014
- 2014-07-10 CN CN201410328344.5A patent/CN104130022B/en active Active
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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104130022A (en) | 2014-11-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103044086B (en) | Method for preparing carbon/carbon composite yttrium silicate whisker reinforced C-AlPO4-SiCn complex external coating | |
| CN103044075B (en) | Method for preparing carbon/carbon composite MoSi2-ZrSiO4-SiC gradient complex outer coating | |
| CN102674903B (en) | Preparation method of SiC/C-AlPO4-mullite antioxidation coating for C/C composite material | |
| CN101844936A (en) | Method for preparing C/C composite material nanometer silicon carbide-mullite-molybdenum disilicide composite external coating | |
| CN104130022B (en) | Carbon/carbon compound material ZrO 2the preparation method of particle and SiC whisker coordination plasticizing mullite compound coating | |
| CN104130013B (en) | The preparation method of the crystal whisker toughened mullite compound coating of a kind of carbon/carbon compound material SiC | |
| CN102674901B (en) | Preparation method of carbon/carbon material C-AlPO4-mullite-MoSi2 composite outer coating layer | |
| CN103601533B (en) | Preparation method of carbon/carbon composite material HfB2 anti-oxidation outer coating | |
| CN104130021B (en) | The preparation method of the crystal whisker toughened mullite compound coating of a kind of carbon/carbon composite mullite | |
| CN101838157B (en) | Method for preparing carbon/carbon composite material nanometer silicon carbide-mullite composite external coating | |
| CN104130019B (en) | The crystal whisker toughened C-AlPO of carbon/carbon composite mullite 4-MoSi 2the preparation method of compound coating | |
| CN105777207A (en) | Preparation method for carbon/carbon composite Yb2Si2O7 whisker toughened Yb2SiO5 composite coating | |
| CN103044076B (en) | Method for preparing carbon/carbon composite yttrium silicate whisker reinforced mullite-C-AlPO4 complex external coating | |
| CN104130012B (en) | Infrared Heating two pulse electrophoretic deposition prepares ZrSiO 4-SiO 2the method of compound coating | |
| CN102674891A (en) | Preparation method of SiCn-MoSi2-mullite composite overcoating for C/C composite material | |
| CN104130011B (en) | The preparation method of carbon/carbon compound material external coating (EC) | |
| CN104130016B (en) | A kind of preparation method of carbon/carbon compound material SiC nanowire plasticizing mullite-SiC compound coating | |
| CN104130014B (en) | Carbon/carbon compound material ZrO 2particle and mullite crystal whisker coordination plasticizing MoSi 2the preparation method of compound coating | |
| CN102875197B (en) | Method for preparing C-AlPO4-MoSi2 composite anti-oxidization coating layer | |
| CN101838836A (en) | Method for preparing carbon/carbon composite mullite and molybdenum disilicide composite outer coating | |
| CN104130017B (en) | The preparation method of the crystal whisker toughened zirconium silicate compound coating of carbon/carbon compound material SiC | |
| CN105777208B (en) | It is a kind of to use carbon/carbon compound material Yb2Si2O7Crystal whisker toughened Yb2Si2O7The preparation method of antioxidant coating | |
| CN104130015B (en) | A kind of preparation method of carbon/carbon compound material external coating (EC) | |
| CN102674900A (en) | Preparation method of C-AlPO4-mullite composite overcoating for C/C composite material | |
| CN106348790A (en) | Preparation method of carbon/carbon composite material SiCn-CrSi2 coating |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20201215 Address after: Floor 6, building 6, Xinlong Plaza, Xindu street, Chengnan New District, Yancheng City, Jiangsu Province, 224000 (CND) Patentee after: Yancheng julonghu Business Cluster Development Co.,Ltd. Address before: No. 1, Weiyang District university garden, Xi'an, Shaanxi Province, Shaanxi Patentee before: SHAANXI University OF SCIENCE & TECHNOLOGY |
|
| TR01 | Transfer of patent right |