CN105924234A - Carbon/carbon (C/C) composite material surface low-porosity complex-phase ceramic coating and preparation method thereof - Google Patents
Carbon/carbon (C/C) composite material surface low-porosity complex-phase ceramic coating and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a carbon/carbon (C/C) composite material surface low-porosity complex-phase ceramic coating and a preparation method thereof. The preparation method comprises the following steps: previously carrying out sintering heat treatment on a ZrB2-SiC powder mixture for ultrasonic plasma spraying in a protective atmosphere, preparing a SiC inner coating and a ZrB2-SiC complex-phase ceramic coating respectively by an embedding process and an ultrasonic plasma spraying two-step process, and carrying out sintering heat treatment on the powder for spraying to sufficiently diffuse molecules so as to form a partial solid solution, thereby preparing the complex-phase ceramic coating with uniform phase distribution and lower porosity. After the ZrB2-SiC powder mixture is subjected to sintering heat treatment in the reducing protective atmosphere, the partial solid solution is formed in the sintering heat treatment process, and the solid solution can not easily shrink in the cooling process, thereby lowering the pores generated in the cooling process after coating spraying and further forming the low-porosity coating. Besides, in the sintering heat treatment process, the molecules interdiffuse, so that the finally prepared complex-phase ceramic coating has more uniform phase distribution.
Description
Technical field
The present invention relates to a kind of carbon/carbon C/C composite material surface low porosity complex phase ceramic coating and preparation method, especially
Relate to the preparation method of carbon/carbon compound material (hereinafter referred to as C/C composite) surface low porosity complex phase ceramic coating,
Particularly raw powder's production technology used by Supersonic Plasma Spraying complex phase ceramic coating.
Background technology
C/C composite has low-density, Gao Biqiang, Gao Bimo, ablation high temperature resistant, resistance to and the high-temperature mechanics of excellence
Many excellent specific properties such as performance, have a wide range of applications in national defence such as Aero-Space as heat structure thermally protective materials
Prospect.But the actual application of the high temperature oxidizable C/C of being composite is most difficult to the bottleneck broken through, superhigh temperature ceramics coating
Technology is to improve the most effective means of this material at high temperature antioxygenic property.Supersonic Plasma Spraying (hereinafter referred to as SAPS)
Coating technology not only manufacturing cycle is short, coating layer thickness is controlled in preparation, and less to matrix damage, thus super in preparation
Gain great popularity during high-temperature ceramics.But, coating prepared by SAPS is during high temperature cooling, and coating shrinkage produces hole
Gap, seriously reduces the compactness of coating, and then also reduces the antioxidation of coating, anti-yaw damper performance.So how
Improve SAPS and prepare the compactness of coating, reduce its porosity, cause the very big of domestic and international research worker and pay close attention to:
Document 1 " Ablation Behavior of ZrB2-Based Coating Prepared by Supersonic Plasma
Spraying for SiC-Coated C/C Composites Under Oxyacetylene Torch.Yao Xi-Yuan, Zhang
Yu-Lei, Li Ke-Zhi.Journal of Thermal Spray Technology, 2013,22 (4): 531-537 " open
Investment prepares SiC undercoating, and Supersonic Plasma Spraying method prepares ZrB2The preparation technology of-SiC external coating.Should
ZrB2-SiC coating prepares in atmospheric environment, and spray power is at 38.5kW～53.9kW, owing to, in spraying process, melting
The powder particles melting state sprays to the speed of matrix surface quickly, the coating relative atmospheric plasma spraying prepared
Coating prepared by technique is comparatively dense, but yet suffers from some unavoidable holes in coating.Due to spraying process
In, under high temperature, powder particles is in molten condition all the time, forms lamellar structure, spraying knot after being sprayed onto on matrix
After bundle, temperature is rapidly decreased to room temperature, shrinks and form space in coating between each lamella.These are formed because of contraction
Hole brings the biggest resistance to the raising of the antioxidation of coating, anti-yaw damper performance.
Document 2 " Effect of pre-oxidation on the ablation resistance of ZrB2-SiC coating for
SiC-coated carbon/carbon composites,Zhang YuLei,Hu Zhixiong,Yang Boying,Jincui
Ren, Li Hejun.Ceramics International 2015, (41): 2582-2589 " disclose a kind of employing at pre-oxidation
ZrB prepared by reason Supersonic Plasma Spraying2The method of-SiC coating.The method is that coating spraying prepared is placed
Under 1100 DEG C of atmospheric environments, aoxidize a period of time, reach by producing one layer of fine and close oxide skin(coating) at coating surface
The purpose of sealing of hole.Although this technology improves the anti-yaw damper performance of coating to a certain extent, but pre-oxidation treatment
During, sample sustains damage unavoidably, and the oxide skin(coating) ratio generated is relatively thin, for improving the long-time anti-of coating
Ablative help is the most little.
ZrB2-SiC complex phase ceramic is as a kind of superhigh temperature ceramics, in extreme harsh superhigh temperature oxide etch environment still
Have good chemical stability and thermal shock resistance, thus it is not only a kind of preferably high-temperature structural material, the most usually
It is chosen as coating material and protects the most oxidized matrix.ZrB2After-SiC ceramic sintering, molecule mutually diffuses to form portion
Divide solid solution, and the solid solution formed be distorted because of lattice, be unfavorable for the motion of dislocation, thus elastic modelling quantity increases,
Plasticity reduces, and this can hinder ceramic coating to the contraction of low-temperature transformation process and then being reduced the hole in coating by high temperature
Rate.
Summary of the invention
Solve the technical problem that
In place of the deficiencies in the prior art, the present invention proposes a kind of carbon/carbon C/C composite material surface low porosity
Complex phase ceramic coating and preparation method, solve complex phase ceramic coating hole prepared by existing Supersonic Plasma Spraying method
Rate technical problem high, mutually pockety.
Technical scheme
A kind of carbon/carbon C/C composite material surface low porosity complex phase ceramic coating, including SiC undercoating and
ZrB2The external coating of-SiC complex phase ceramic；It is characterized in that: described ZrB2The powder that the external coating of-SiC complex phase ceramic uses
Body is SiC powder body and the ZrB of 70%～90% of 10%～30%2Powder body diffuses to form partial solid solution through high-temperature-phase
Spraying powder body.
A kind of ZrB prepared in described C/C composite material surface complex phase ceramic coating2The external coating spray of-SiC complex phase ceramic
The method of painting powder body, it is characterised in that: described ZrB2The preparation process of the external coating of-SiC complex phase ceramic is:
Step 1): volume fraction is respectively SiC powder body and the ZrB of 70%～90% of 10%～30%2Powder body is at corundum
Stirring mixing in mortar；
Step 2): mixed powder is put in the hot pressing vacuum response stove that graphite is heater, vacuum drying oven is carried out
Application of vacuum, furnace temperature, to normal pressure, is risen to 1800～2200 DEG C from room temperature with the programming rate of 5～10 DEG C/min by logical Ar gas,
It is incubated 2～4 hours；Close power supply and naturally cool to room temperature, whole during logical Ar gas shielded, obtain densified sintering product
ZrB2-SiC ceramic block；
Step 3): use disintegrating machine by ZrB2-SiC ceramic block is broken into particulate ceramic, particulate ceramic is put in equipped with
The high-energy planetary ball mill tank of agate ball obtains after ball milling the powder body of mobility, utilizes screen cloth to filter out particle diameter and exist
Ceramic particle between 40～70 μm is as the powder body of spraying complex phase ceramic.
A kind of employing ZrB2The external coating spraying powder body of-SiC complex phase ceramic prepares described C/C composite material surface complex phase
The method of ceramic coating, it is characterised in that step is as follows:
Step 1, preparation SiC undercoating: by ultrasonic cleaning after C/C composite sanding and polishing and dry, then put
In the mixed powder of graphite crucible；Graphite crucible is put in the hot pressing vacuum response stove with graphite as heater, right
Vacuum drying oven carries out application of vacuum, makes vacuum reach-0.09MPa, and logical Ar gas is to normal pressure, with the liter of 5～10 DEG C/min
Furnace temperature is risen to 1800～2000 DEG C from room temperature by temperature speed, is incubated 1～3 hour；Close power supply and naturally cool to room temperature,
During whole, logical Ar gas shielded, makes SiC undercoating at carbon/carbon C/C composite material surface；
Described mixed powder is: by Si powder, C powder and Al2O3Powder by mass percentage 60%～90%, 10%～30%,
Ball milling after 3%～15% mixing, makes powder body mix homogeneously；
Step 2, preparation ZrB2-SiC complex phase ceramic coating: utilize Supersonic Plasma Spraying equipment to be made pottery by spraying complex phase
The powder spray of porcelain is coated onto prepared being embedded with on SiC internally coated C/C matrix of step 1, prepares low-porosity
ZrB2-SiC complex phase ceramic coating；Plasma spray coating process parameter is: spraying DC current: 350～450A；Spraying is straight
Stream voltage: 120～150V；Main gas argon flow amount: 75～85L/min；Auxiliary gas hydrogen flowing quantity: 4.5～5.5L/min；Send
Powder speed: 20～40g/min；Spray distance: 80～150mm；Circulation spraying is repeatedly to meet the outer painting that design is wanted
Layer thickness.
Spraying number of times repeatedly described in step 2 is 8～15.
Beneficial effect
A kind of carbon/carbon C/C composite material surface low porosity the complex phase ceramic coating of present invention proposition and preparation method,
ZrB to Supersonic Plasma Spraying in protective atmosphere2It is sintered heat treatment in advance with SiC mixed powder, then adopts
SiC undercoating and ZrB is prepared respectively by investment and Supersonic Plasma Spraying two-step method2-SiC complex phase ceramic coating,
By making molecule fully spread spraying powder sintering heat treatment, forming part solid solution, thus preparation distribution mutually is all
The complex phase ceramic coating that the even and porosity is relatively low.In order to compare, utilize the ZrB not doing heat treatment2With SiC mixed powder
Material uses same process to prepare ZrB2-SiC complex phase ceramic coating.
The invention has the beneficial effects as follows: to ZrB in reduction protection atmosphere2It is sintered heat treatment with SiC mixed powder
After, utilize Supersonic Plasma Spraying legal system to obtain ZrB2-SiC complex phase ceramic coating.Sintering heat treatment process defines
Partial solid solution (such as Fig. 1), is difficult in solid solution cooling procedure shrink, and produces after reducing coating spraying in cooling procedure
Raw hole, thus form low porosity coating such as Fig. 2 and Fig. 3.It addition, in sintering heat treatment process, molecule phase
Counterdiffusion, makes the final complex phase ceramic coating prepared also be distributed mutually more uniform, such as Fig. 4.
Accompanying drawing explanation
Fig. 1 is the back scattering electron microscopic picture of the spraying powder that the sintered heat treatment of embodiment 1 prepares.
Fig. 2 is the ZrB of embodiment 1 preparation2-SiC complex phase ceramic coating cross section back scattering electromicroscopic photograph.
Fig. 3 is to prepare with spraying powder (a) not dealt with spraying powder (b) of sintering heat treatment respectively
ZrB2-SiC complex phase ceramic coating cross-sectional scans electromicroscopic photograph.
Fig. 4 is to prepare with spraying powder (a) not dealt with spraying powder (b) of sintering heat treatment respectively
ZrB2-SiC complex phase ceramic coating cross section back scattering electromicroscopic photograph.
Detailed description of the invention
In conjunction with embodiment, accompanying drawing, the invention will be further described:
Embodiment 1:
Step 1: preparation SiC undercoating.Its detailed process is:
1) C/C composite is used anhydrous second after the sand paper sanding and polishing successively of No. 400, No. 800 and No. 1000
Alcohol supersound washing is clean, dry for standby in baking oven.Drying temperature is 80 DEG C.
2) the Si powder of 80g is weighed respectively, the C powder of 30g, and the Al of 5g2O3Powder, is placed in Colophonium ball grinder,
Take the agate ball of varying number different-diameter to put into ball milling mixed processing in ball grinder and obtain mixed powder in 2 hours, dry
Standby as investment.
3) the mixed powder half of preparation is put in graphite crucible, then the C/C composite after cleaning, drying is tried
Sample is placed on above powder, is subsequently placed into second half embedding powder and is covered by C/C composite sample.
Above-mentioned graphite crucible is put into graphite as in the hot pressing vacuum response stove of heater.Evacuation makes after 30 minutes very
Reciprocal of duty cycle reaches-0.09MPa, empty 30 minutes of fidelity, observes whether vacuum meter registration changes, as unchanged, system is described
Air-tightness is intact.Logical argon is to normal pressure.This process is in triplicate.Afterwards furnace temperature rising to 2000 DEG C, heating rate is
10 DEG C/min, then insulation 2.5 hours.Be then turned off power supply and naturally cool to room temperature, whole during logical argon protect
Protect.Taking out graphite crucible subsequently, cleaning embedding powder obtains the C/C composite containing SiC coating.
Step 2, the preparation spraying powder containing partial solid solution.Detailed process is:
1) by 10g SiC powder body and 90g ZrB2Powder body is put in corundum mortar, stirs and makes its mix homogeneously in 2 hours；
2) putting in graphite crucible by mixed powder, artificially pressurize, make powder closely knit, graphite crucible is put into graphite is
In the hot pressing vacuum response stove of heater.Evacuation makes vacuum reach-0.09MPa after 30 minutes, empty 30 points of fidelity
Clock, observes whether vacuum meter registration changes, and as unchanged, illustrates that system air-tightness is intact.Logical argon is to normal pressure.This
Process is in triplicate.With 10 DEG C/min programming rate, furnace temperature is risen to 2100 DEG C from room temperature, be incubated 2 hours；Close
Power supply naturally cools to room temperature, whole during logical Ar gas shielded, obtain the ZrB of densified sintering product2-SiC ceramic block.
3) with disintegrating machine, block ceramic is broken into small-particle ceramic porcelain, small-particle ceramic porcelain is put in the high energy equipped with agate ball
Ball milling 4 hours in planetary ball mill tank, it is thus achieved that the preferable powder body of mobility, cross 200 mesh and 400 mesh respectively by this powder body
Screen cloth, takes intermediate layer powder as spraying powder, and particle diameter is in 40～70 μm.
Step 3: preparation ZrB2-SiC complex phase ceramic coating
The surface obtained in step 1 is contained SiC internally coated C/C composite be placed in specimen holder, will step
Rapid 2 spray coating powders prepared load powder feeder, open Supersonic Plasma Spraying equipment, and whether inspection equipment leaks, leaks
Gas.After confirming Plant in good condition, adjust device parameter: spray DC current 350A, spray DC voltage 120V, main
Gas (argon) flow 75L/min, auxiliary gas (hydrogen) flow 4.5L/min, powder feeding rate 20g/min, spray gun and sample
Distance is 150mm.According to above parameter, spraying powder is sprayed on sample, circulation spraying 10 times.
Through above step, prepare the spraying powder containing partial solid solution, as it is shown in figure 1, wherein there are three kinds of phases
Coexist, be the ZrB of white respectively2Phase, the SiC phase of black and color solid solution phase therebetween.Utilizing should
The ZrB of low-porosity is prepared in powder spraying2-SiC complex phase ceramic coating, as in figure 2 it is shown, coating cross sections is without big hole
System and crackle, and be tightly combined with SiC undercoating.
Embodiment 2:
Step 1: preparation SiC undercoating.Its detailed process is:
1) C/C composite is used anhydrous second after the sand paper sanding and polishing successively of No. 400, No. 800 and No. 1000
Alcohol supersound washing is clean, dry for standby in baking oven.Drying temperature is 80 DEG C.
2) the Si powder of 80g is weighed respectively, the C powder of 30g, and the Al of 5g2O3Powder, is placed in Colophonium ball grinder,
Take the agate ball of varying number different-diameter to put into ball milling mixed processing in ball grinder and obtain mixed powder in 2 hours, dry
Standby as investment.
3) the mixed powder half of preparation is put in graphite crucible, then the C/C composite after cleaning, drying is tried
Sample is placed on above powder, is subsequently placed into second half embedding powder and is covered by C/C composite sample.
Above-mentioned graphite crucible is put into graphite as in the hot pressing vacuum response stove of heater.Evacuation makes after 30 minutes very
Reciprocal of duty cycle reaches-0.09MPa, empty 30 minutes of fidelity, observes whether vacuum meter registration changes, as unchanged, system is described
Air-tightness is intact.Logical argon is to normal pressure.This process is in triplicate.Afterwards furnace temperature rising to 2000 DEG C, heating rate is
10 DEG C/min, then insulation 2.5 hours.Be then turned off power supply and naturally cool to room temperature, whole during logical argon protect
Protect.Taking out graphite crucible subsequently, cleaning embedding powder obtains the C/C composite containing SiC coating.
Step 2, the preparation spraying powder containing partial solid solution.Detailed process is:
1) by 11g SiC powder body and 88g ZrB2Powder body is put in corundum mortar, stirs and makes its mix homogeneously in 2 hours；
2) putting in graphite crucible by mixed powder, artificially pressurize, make powder closely knit, graphite crucible is put into graphite is
In the hot pressing vacuum response stove of heater.Evacuation makes vacuum reach-0.09MPa after 30 minutes, empty 30 points of fidelity
Clock, observes whether vacuum meter registration changes, and as unchanged, illustrates that system air-tightness is intact.Logical argon is to normal pressure.This
Process is in triplicate.With 10 DEG C/min programming rate, furnace temperature is risen to 2200 DEG C from room temperature, be incubated 2 hours；Close
Power supply naturally cools to room temperature, whole during logical Ar gas shielded, obtain the ZrB of densified sintering product2-SiC ceramic block.
3) with disintegrating machine, block ceramic is broken into small-particle ceramic porcelain, small-particle ceramic porcelain is put in the high energy equipped with agate ball
Ball milling 4 hours in planetary ball mill tank, it is thus achieved that the preferable powder body of mobility, cross 200 mesh and 400 mesh respectively by this powder body
Screen cloth, takes intermediate layer powder as spraying powder, and particle diameter is in 40～70 μm.
Step 3: preparation ZrB2-SiC complex phase ceramic coating
The surface obtained in step 1 is contained SiC internally coated C/C composite be placed in specimen holder, will step
Rapid 2 spray coating powders prepared load powder feeder, open Supersonic Plasma Spraying equipment, and whether inspection equipment leaks, leaks
Gas.After confirming Plant in good condition, adjust device parameter: spray DC current 350A, spray DC voltage 120V, main
Gas (argon) flow 75L/min, auxiliary gas (hydrogen) flow 4.5L/min, powder feeding rate 20g/min, spray gun and sample
Distance is 150mm.According to above parameter, spraying powder is sprayed on sample, spray 10 times.
Through above step, prepare SiC/ZrB at C/C composite material surface2-SiC ceramic coating is permissible by Fig. 3 b
Find out the ZrB that the method is prepared2-SiC complex phase ceramic coating is compared to the coating utilizing the powder body not processed to prepare
(Fig. 3 a), cross section porosity significantly reduces.
Embodiment 3:
Step 1: preparation SiC undercoating.Its detailed process is:
1) C/C composite is used anhydrous second after the sand paper sanding and polishing successively of No. 400, No. 800 and No. 1000
Alcohol supersound washing is clean, dry for standby in baking oven.Drying temperature is 80 DEG C.
2) the Si powder of 80g is weighed respectively, the C powder of 30g, and the Al of 5g2O3Powder, is placed in Colophonium ball grinder,
Take the agate ball of varying number different-diameter to put into ball milling mixed processing in ball grinder and obtain mixed powder in 2 hours, dry
Standby as investment.
3) the mixed powder half of preparation is put in graphite crucible, then the C/C composite after cleaning, drying is tried
Sample is placed on above powder, is subsequently placed into second half embedding powder and is covered by C/C composite sample.
Above-mentioned graphite crucible is put into graphite as in the hot pressing vacuum response stove of heater.Evacuation makes after 30 minutes very
Reciprocal of duty cycle reaches-0.09MPa, empty 30 minutes of fidelity, observes whether vacuum meter registration changes, as unchanged, system is described
Air-tightness is intact.Logical argon is to normal pressure.This process is in triplicate.Afterwards furnace temperature rising to 2000 DEG C, heating rate is
10 DEG C/min, then insulation 2.5 hours.Be then turned off power supply and naturally cool to room temperature, whole during logical argon protect
Protect.Taking out graphite crucible subsequently, cleaning embedding powder obtains the C/C composite containing SiC coating.
Step 2, the preparation spraying powder containing partial solid solution.Detailed process is:
1) by 10g SiC powder body and 90g ZrB2Powder body is put in corundum mortar, stirs and makes its mix homogeneously in 2 hours；
2) putting in graphite crucible by mixed powder, artificially pressurize, make powder closely knit, graphite crucible is put into graphite is
In the hot pressing vacuum response stove of heater.Evacuation makes vacuum reach-0.09MPa after 30 minutes, empty 30 points of fidelity
Clock, observes whether vacuum meter registration changes, and as unchanged, illustrates that system air-tightness is intact.Logical argon is to normal pressure.This
Process is in triplicate.With 8 DEG C/min programming rate, furnace temperature is risen to 2100 DEG C from room temperature, be incubated 3 hours；Close electricity
Source naturally cools to room temperature, whole during logical Ar gas shielded, obtain the ZrB of densified sintering product2-SiC ceramic block.
3) with disintegrating machine, block ceramic is broken into small-particle ceramic porcelain, small-particle ceramic porcelain is put in the high energy equipped with agate ball
Ball milling 4h in planetary ball mill tank, it is thus achieved that the preferable powder body of mobility, crosses 200 mesh and 400 eye mesh screens respectively by this powder body,
Taking intermediate layer powder as spraying powder, particle diameter is in 40～70 μm.
Step 3: preparation ZrB2-SiC complex phase ceramic coating
The surface obtained in step 1 is contained SiC internally coated C/C composite be placed in specimen holder, will step
Rapid 2 spray coating powders prepared load powder feeder, open Supersonic Plasma Spraying equipment, and whether inspection equipment leaks, leaks
Gas.After confirming Plant in good condition, adjust device parameter: spray DC current 350A, spray DC voltage 120V, main
Gas (argon) flow 75L/min, auxiliary gas (hydrogen) flow 4.5L/min, powder feeding rate 20g/min, spray gun and sample
Distance is 150mm.According to above parameter, spraying powder is sprayed on sample, spray 10 times.
Through above step, prepare SiC/ZrB at C/C composite material surface2-SiC ceramic coating, due to supersonic speed etc.
Plasma spray method prepares ZrB2The powder body of-SiC complex phase ceramic coating is through oversintering heat treatment, so the coating prepared is not
The only porosity is low, and by the contrast of Fig. 4 b and Fig. 4 a it is also seen that the distribution mutually of coating is the most uniform.
In all embodiments, the purity of described Si powder is 99.5%, granularity is 300 mesh, the purity of C powder is 99%,
Granularity is 300 mesh, Al2O3Powder be analytical pure (weight/mass percentage composition >=99.8%), granularity be 300 mesh, ZrB2Powder is pure
Degree is 99%, granularity is 800 mesh, and the purity of SiC powder is 99%, granularity is 800 mesh.
Claims (4)
1. carbon/carbon C/C composite material surface low porosity complex phase ceramic coating, including undercoating and the ZrB of SiC2-SiC
The external coating of complex phase ceramic；It is characterized in that: described ZrB2The powder body that the external coating of-SiC complex phase ceramic uses is
The SiC powder body of 10%～30% and the ZrB of 70%～90%2Powder body diffuses to form partial solid solution through high-temperature-phase
Spraying powder body.
2. the ZrB prepared in C/C composite material surface complex phase ceramic coating described in claim 12-SiC complex phase ceramic
The method of external coating spraying powder body, it is characterised in that: described ZrB2The system of the external coating of-SiC complex phase ceramic
Standby step is:
Step 1): volume fraction is respectively SiC powder body and the ZrB of 70%～90% of 10%～30%2Powder body is at corundum
Stirring mixing in mortar；
Step 2): mixed powder is put in the hot pressing vacuum response stove that graphite is heater, vacuum drying oven is carried out
Application of vacuum, furnace temperature, to normal pressure, is risen to 1800～2200 DEG C from room temperature with the programming rate of 5～10 DEG C/min by logical Ar gas,
It is incubated 2～4 hours；Close power supply and naturally cool to room temperature, whole during logical Ar gas shielded, obtain densified sintering product
ZrB2-SiC ceramic block；
Step 3): use disintegrating machine by ZrB2-SiC ceramic block is broken into particulate ceramic, particulate ceramic is put in equipped with
The high-energy planetary ball mill tank of agate ball obtains after ball milling the powder body of mobility, utilizes screen cloth to filter out particle diameter and exist
Ceramic particle between 40～70 μm is as the powder body of spraying complex phase ceramic.
3. the ZrB using claim 22The external coating spraying powder body of-SiC complex phase ceramic prepares claim 1 institute
The method stating C/C composite material surface complex phase ceramic coating, it is characterised in that step is as follows:
Step 1, preparation SiC undercoating: by ultrasonic cleaning after C/C composite sanding and polishing and dry, then put
In the mixed powder of graphite crucible；Graphite crucible is put in the hot pressing vacuum response stove with graphite as heater, right
Vacuum drying oven carries out application of vacuum, makes vacuum reach-0.09MPa, and logical Ar gas is to normal pressure, with the liter of 5～10 DEG C/min
Furnace temperature is risen to 1800～2000 DEG C from room temperature by temperature speed, is incubated 1～3 hour；Close power supply and naturally cool to room temperature,
During whole, logical Ar gas shielded, makes SiC undercoating at carbon/carbon C/C composite material surface；
Described mixed powder is: by Si powder, C powder and Al2O3Powder by mass percentage 60%～90%, 10%～30%,
Ball milling after 3%～15% mixing, makes powder body mix homogeneously；
Step 2, preparation ZrB2-SiC complex phase ceramic coating: utilize Supersonic Plasma Spraying equipment to be made pottery by spraying complex phase
The powder spray of porcelain is coated onto prepared being embedded with on SiC internally coated C/C matrix of step 1, prepares low-porosity
ZrB2-SiC complex phase ceramic coating；Plasma spray coating process parameter is: spraying DC current: 350～450A；Spraying is straight
Stream voltage: 120～150V；Main gas argon flow amount: 75～85L/min；Auxiliary gas hydrogen flowing quantity: 4.5～5.5L/min；Send
Powder speed: 20～40g/min；Spray distance: 80～150mm；Circulation spraying is repeatedly to meet the outer painting that design is wanted
Layer thickness.
The method preparing C/C composite material surface complex phase ceramic coating the most according to claim 3, it is characterised in that:
Spraying number of times repeatedly described in step 2 is 8～15.
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Application publication date: 20160907 |