CN108149201A - A kind of Mo-Si-X-C complex phase ceramic coatings and preparation method - Google Patents
A kind of Mo-Si-X-C complex phase ceramic coatings and preparation method Download PDFInfo
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- CN108149201A CN108149201A CN201810019151.XA CN201810019151A CN108149201A CN 108149201 A CN108149201 A CN 108149201A CN 201810019151 A CN201810019151 A CN 201810019151A CN 108149201 A CN108149201 A CN 108149201A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0635—Carbides
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Abstract
A kind of Mo Si X C complex phase ceramic coatings and preparation method, the coating are uniformly mixed by the powder of Mo, Si, X and are placed on carbon base body, are heated to 1,500 1600 DEG C and are obtained by the reaction;The X is selected from metal Al and/or Ti;Preparation method is using hot evaporation and in-situ chemical reaction joint legal system Mo Si X (X=Al, Ti) multicomponent system coating.MoSi is reduced by alloying2Fusing point (2030 DEG C), Mo Si X C (X=Al, Ti) complex phase ceramic coating can be prepared under lower temperature conditions.Overcome prior art coating and basal body binding force is poor, prepares the problems such as cumbersome, provide carbon source by carbon matrix, reaction in-situ forms the good SiC internal layers of basal body binding force, and largely fills intrinsic silicon hole and hole, forms the composite coating with engaging structure.The present invention, which prepares multicomponent system coating, has the characteristics that the time is short, preparation process is simple, compactness is good.
Description
Technical field
The present invention relates to a kind of complex phase ceramic coating and preparation methods, in particular to a kind of Mo-Si-X-C complex phase ceramics to apply
Layer and preparation method;Belong to high temperature complex phase ceramic preparing technical field.
Background technology
The use material needs of hypersonic aircraft nose of wing and Aerodynamic Heating component are born under near space environment
High operating temperature, oxygen-enriched working environment and strong airflow scouring.Coating technology can assign engine components high temperature resistant, resist
The functional characteristics such as oxidation, corrosion-resistant, wear-resistant, heat-insulated, to meet the harsh such as higher temperature, higher abrasion, more deep-etching
Under the conditions of requirement.Therefore, coating technology plays an important role to the reliability and service life that improve parts,
It is one of core technology that near space hypersonic aircraft is promoted to greatly develop.
In recent years, the SiC and MoSi for the research of high-temperature oxydation coating2Deng intermetallic compound be mainly to study
One of direction.MoSi2The selective oxidation of Si can occur under high temperature oxidizing conditions for coating, i.e., in MoSi2Coating surface forms one
The fine and close SiO of layer2Oxidation film.This oxidation film can prevent further diffusion of the oxygen inside C/C matrices of composite materials.Meanwhile
The SiO generated in crackle2Self-healing can be played.
It is more that Mo-Si system antioxidant coating methods are prepared at present, such as Li He armies of Northwestern Polytechnical University and Li Kezhi are adopted
B is prepared with investment2O3、LaB6Modified SiC-MoSi2Composite coating, and on this basis development multistage embedding, prepare as
SiC-MoSi2-CrSi2/ Si multilayer complex phase ceramic coatings.Yellow sword cutting edge of a knife or a sword of northwest University of Science and Technology etc. is deposited using pulse arc discharge
Method prepares AlPO4-SiC-MoSi2Duplex heat treatment, Turin, Italy Polytechnics prepare SiC/MoSi using slurry process2/Y2O3Three
Layer duplex heat treatment.But these technologies face some row problems, and investment reaction temperature is higher, are limited by calandria volume, container
System, difficulty meets the coatings such as large scale, shaped piece and prepares demand, and the coating of the preparations such as slurry process also faces agglutinant volatilization and causes
The problem of coating and poor basal body binding force.
Hot evaporation-reaction in-situ combination method combines chemical reaction according to physical deposition techniques, can, abnormity structure large-scale in charcoal base
Prepare the fine and close and good ceramic coating of basal body binding force in part surface.But due to MoSi2Fusing point is up to 2030 DEG C, meanwhile, MoSi2
It is unstable C at 1900 DEG C to 2030 DEG C40Hexagonal crystallographic texture.When using Si and Mo or MoSi2During as constituent element hot evaporation,
A series of problems, such as excessive temperature is likely to result in particle in coating and excessively grows up, and material internal damages.
Goal of the invention
The present invention prepares deficiency existing for Mo-Si system anti-yaw damper coating process for the prior art in charcoal primary surface, carries
For a kind of reasonable mixture ratio of components, the Mo-Si complex phase ceramic coatings that preparation process is simple, preparation temperature is low.
Another object of the present invention is to provide it is a kind of it is simple for process, technological process is short, prepare complex phase ceramic coating with
The preparation method of the compact Mo-Si complex phase ceramic coatings of matrix.
A kind of Mo-Si-X-C complex phase ceramic coatings of the present invention, the coating are uniformly mixed by the powder of Mo, Si, X and are placed on
On carbon base body, it is heated to 1500-1600 DEG C and is obtained by the reaction;The X is selected from metal Al and/or Ti.
A kind of Mo-Si-X-C complex phase ceramic coatings of the present invention, described Mo, Si, X are formed by following mass ratio:
Mo:Si:X=(20-30):(40-60):(20-30).
A kind of Mo-Si-X-C complex phase ceramic coatings of the present invention, in component X, metal Al, Ti mixture in any proportion.
A kind of Mo-Si-X-C complex phase ceramic coatings of the present invention, purity >=99.9% of metal Mo, the mesh of granularity≤300;
Purity >=99.9% of Si, the mesh of granularity≤300;
Purity >=99.5% of metal Ti, granularity are≤500 mesh;
Purity >=99.7% of metal Al, granularity are≤300 mesh.
A kind of preparation method of Mo-Si-X-C complex phase ceramic coatings of the present invention, includes the following steps:
Step 1
Mo, Si, Ti, Al component proportion by design is uniformly mixed, is mixed with Mo powder, Si powder, Ti powder, Al powder is taken
Powder;
Step 2
The mixed-powder that step 1 obtains is placed in vacuum sintering furnace, carbon base body is placed in above mixed-powder, is heated to
1500-1800 DEG C, at least 2 hours are kept the temperature, mixed-powder is deposited to carbon base body, then, dropped with the speed of 6-15 DEG C/min
Temperature is to 800-1000 DEG C, furnace cooling.
A kind of preparation method of Mo-Si-X-C complex phase ceramic coatings of the present invention, in step 1, mixed-powder uses wet type ball
Mill is uniformly mixed, and is sieved after the drying of uniformly mixed powder.
A kind of preparation method of Mo-Si-X-C complex phase ceramic coatings of the present invention, wet ball-milling use planetary ball mill, ball
Grinding media is alcohol, wet ball-milling time 5-8h, ratio of grinding media to material 5:1-8:1, drum's speed of rotation 200-350 turns/min.
A kind of preparation method of Mo-Si-X-C complex phase ceramic coatings of the present invention, in step 1, Mo, Si, Ti, Al of design
Component proportion is:
Mo:Si:X=(20-30):(40-60):(20-30).
A kind of preparation method of Mo-Si-X-C complex phase ceramic coatings of the present invention, in step 1,
Purity >=99.9% of metal Mo, the mesh of granularity≤300;
Purity >=99.9% of Si, the mesh of granularity≤300;
Purity >=99.5% of metal Ti, granularity are≤500 mesh;
Purity >=99.7% of metal Al, granularity are≤300 mesh.
A kind of preparation method of Mo-Si-X-C complex phase ceramic coatings of the present invention, in step 2, vacuum degree in vacuum sintering furnace
≤ 10Pa, the protection of temperature-rise period argon gas atmosphere;5-10 DEG C of heating rate/min;Soaking time 2-3h.
A kind of preparation method of Mo-Si-X-C complex phase ceramic coatings of the present invention, in step 2, mixed-powder is placed in graphite tank
In, carbon matrix is placed in 2-4cm positions above graphite tank, and carbon base body and graphite tank are that high purity graphite is formed, and graphite purity >=
99.99%;Density is 1.72g/cm3。
Carbon base body polishes smooth rear alcohol ultrasonic cleaning 30min with sand paper, and rear 120 DEG C of drying 2h is spare.
A kind of preparation method of Mo-Si-X-C complex phase ceramic coatings of the present invention, the Mo-Si-X-C ceramic coatings being prepared
Surface is by high-melting-point, the MoSi of resistance to ablation2It is formed with SiC, internal layer is the multilayer complex phase of SiC compositions combined closely with carbon base body
Structure, coating and matrix metallurgical binding.
The present invention adds alloy element Al, Ti in hot evaporation Mo-Si system coatings, utilizes Ti, Al atomic substitutions
MoSi2Middle part atom site, and form (Mo, Ti) Si compared with low melting point2Or Mo (Si, Al)2;On the one hand, alloying can be realized
Hot evaporation constituent element volatilizees in lower temperature section and spreads, the high-melting-point TiO formed after another aspect ablation2、Al2O3Be also beneficial to
Imperial flame impingement, improves coating Burning corrosion resistance energy.So as to overcome prior art reaction temperature height, coating and basal body binding force
The problem of poor.
The advantages of invention and good effect
The preparation method of alloying Mo-Si-X (X=Al, Ti) multicomponent system coating of the present invention, with reference to hot evaporation and original position
Joint legal system Mo-Si-X (X=Al, Ti) multicomponent system coating is chemically reacted, is mainly used in the work(of the requirements such as high temperature, resistance to ablation
It can structural elements surfacecti proteon.
Compared with prior art, the advantages and positive effects of the present invention are embodied in:
(1) MoSi is reduced by alloying2Fusing point (2030 DEG C), Mo-Si- can be prepared under lower temperature conditions
X-C (X=Al, Ti) complex phase ceramic coating.
(2) overcome prior art coating and basal body binding force be poor, prepares the problems such as cumbersome, carbon source is provided by carbon matrix,
Reaction in-situ forms the good SiC internal layers of basal body binding force, and largely fills intrinsic silicon hole and hole, and being formed has engagement knot
The composite coating of structure.
(3) present invention, which prepares multicomponent system coating, has the characteristics that the time is short, preparation process is simple, compactness is good.
Description of the drawings
Attached drawing 1 is 1 face coat XRD diffracting spectrums of embodiment.
Attached drawing 2 is the stereoscan photograph (x 100) of one coating morphology of embodiment.
Attached drawing 3 is the big multiplying power electron scanning electromicroscopic photograph (x5000) of attached drawing 2.
Attached drawing 4 is the matrix cross-sectional internal photo (x1000) of ZrC-SiC coatings in embodiment 1.
Attached drawing 5 is one ablation 60s rear surface pattern secondary electron stereoscan photographs of embodiment.
Attached drawing 6 is the coating X ray diffracting spectrum of embodiment 2.Scanning electricity of the attached drawing 7 for two coating morphology of embodiment
Mirror photo.
Attached drawing 8a is that 1000 times of photos are amplified in subregion in Fig. 7.
Attached drawing 8b is the energy spectrum analysis figure at attached drawing 8a midpoints 1.
Attached drawing 8c is the energy spectrum analysis figure at attached drawing 8a midpoints 2.
Attached drawing 8d is the energy spectrum analysis figure at attached drawing 8a midpoints 3.
Attached drawing 9 is the stereoscan photograph of two coating cross sections of embodiment.
Attached drawing 10 is two coating ablation 60s rear surface stereoscan photographs of embodiment.It can be seen that from attached drawing 1:Coating by
Simple substance Si, SiC and (Ti0.8Mo0.2)Si2Object phase composition.
Attached drawing 11a is embodiment Three coating surface scan electromicroscopic photograph.
Attached drawing 11b is the energy spectrum analysis figure at attached drawing 11a midpoints 1.
Attached drawing 11c is the energy spectrum analysis figure at attached drawing 11a midpoints 2.
It can be seen that from attached drawing 2:Coating surface is mainly made of white molybdenum silicide and black SiC.
It can be seen that from attached drawing 3:Coating surface is not completely fine and close, there are still tiny microvoid, white molybdenum silicide
It is scattered to be distributed on the SiC particulate of black polygon accumulation.
It can be seen that from attached drawing 4:Molybdenum silicide is mainly gathered in the superficial layer of coating, and internal layer is mainly by the SiC groups of grey
Into SiC penetrates into the hole and hole of intrinsic silicon, and forms metallurgical engagement.
It can be seen that from attached drawing 5:It is observed that coating surface is fine and close after ablation, without apparent hole and hole.From
Attached drawing 6 is observed that:Coating surface is mainly by MoSi2、SiC、Mo(Si,Al)2It is formed with Si.MoSi2For the most strong diffraction of coating
Peak.
From attached drawing 7 it is observed that coating surface structure is complicated, ribbon white phase and black particle are attached to grey form and aspect
On;With reference to the energy spectrum diagram attached drawing 8b at attached drawing 8a midpoints 1,2,3;Attached drawing 8c;Attached drawing 8d can be seen that:Black particle is containing Al's
SiC, grey form and aspect are SiC, and ribbon white phase is MoSiAlC solid solution.
It is observed that from attached drawing 9:Coating surface molybdenum silicide is also gathered in coating surface layer substantially, and inside is based on SiC
Composite construction.
It is observed that from attached drawing 10:After coating ablation, surface has more apparent particle packing pattern, and surface exists
More apparent hole and hole.
From attached drawing 11 it is observed that coating surface structure is complicated, black particle is attached in canescence " cloud wadding " phase;Knot
Close the energy spectrum diagram attached drawing 11b at attached drawing 11a midpoints 1,2;Attached drawing 11c;It can be seen that:Greyish white form and aspect are MoSiAlTi phases.
Specific embodiment
Embodiment one
Using density as 1.72g/cm3High purity graphite as matrix, polish smooth rear alcohol ultrasonic cleaning with sand paper
30min, rear 120 DEG C of drying 2h are spare.
By the Mo powder, Si powder, Ti powder of different proportion, respectively according to 20:60:20 mass ratioes alcohol on planetary ball mill
Wet-milling 8h takes out drying, mixed powder is obtained after sieving.
It is evenly laid out in graphite pot bottom that powder will be mixed, graphite tank is placed in vacuum sintering furnace.It is evacuated to 10- 3Pa is passed through Ar gases, and heating rate is 8-10 DEG C/min, is warming up to 1600 DEG C;2h is kept the temperature, mixed powder is made to be deposited to graphite
On matrix, then 1000 DEG C are cooled to the speed of 10 DEG C/min.Powered-down source cooled to room temperature.
Referring to attached drawing 1-5, one coating surface of embodiment by white (Ti0.8Mo0.2)Si2Mutually with the SiC phases of grey and less
Measure Si compositions.Coating is fine and close, and surface is without apparent crackle.Coating layer thickness is about 100 μm, and inside is mainly made of SiC, and coating penetrates into
Graphite matrix is deeper, and the hole and hole of fabulous filling graphite surface have metallurgical binding feature.
According to GJB323A-96,2500 DEG C carry out ablation test to sample and calculate ablating rate, and the ablation time is 30s,
60s, ablation center temperature are 2500 DEG C.Coating test coating after 60s ablations keeps compact and complete, does not come off, quality
Ablating rate is 0.01mg/s, and linear ablative rate is 2 μm/s.
Embodiment two
Density is 1.72g/cm3High purity graphite as matrix, polish smooth rear alcohol ultrasonic cleaning with sand paper
30min, rear 120 DEG C of drying 2h are spare.
By the Mo powder, Si powder, Al powder of different proportion respectively according to 30:50:20 mass ratioes alcohol on planetary ball mill
Wet-milling 6h takes out drying, mixed powder is obtained after sieving.
It is evenly laid out in graphite pot bottom that powder will be mixed, graphite tank is placed in vacuum sintering furnace.It is evacuated to 10- 3Pa is passed through Ar gases, and heating rate is 10min/ DEG C, is warming up to 1600 DEG C.Sample is kept the temperature into 2h at 1600 DEG C, then with 10
DEG C speed be cooled to 1000 DEG C, stopping is passed through Ar gases.Powered-down source cooled to room temperature.
Two coating of embodiment is observed it is found that coating surface is by white MoSi2, Mo (Al, Si)2The SiC of mixed phase and black
Phase and the Si phase compositions containing Al.Coating is fine and close, and surface is without apparent crackle.Coating layer thickness is about 100 μm, and inside is mainly by SiC groups
Into coating infiltration graphite matrix is deeper, and the hole and hole of fabulous filling graphite surface have metallurgical binding feature.
According to GJB323A-96, ablation test is carried out to sample and calculates ablating rate, the ablation time is 30s, 60s, ablation
Center temperature is 2500 DEG C.Coating test coating after 60s ablations keeps complete, does not come off, but surface presence is more porous
Gap and hole, mass ablative rate 1.05mg/s, linear ablative rate are 9 μm/s.
Embodiment three
Density is 1.72g/cm3High purity graphite as matrix, polish smooth rear alcohol ultrasonic cleaning with sand paper
30min, rear 120 DEG C of drying 2h are spare.
By the Mo powder of different proportion, Si powder, Al powder and Ti powder respectively according to 30:50:10:10 mass ratioes are in planetary type ball-milling
Alcohol wet-milling 6h on machine takes out drying, mixed powder is obtained after sieving.
It is evenly laid out in graphite pot bottom that powder will be mixed, graphite tank is placed in vacuum sintering furnace.It is evacuated to 10- 3Pa is passed through Ar gases, and heating rate is 10min/ DEG C, is warming up to 1600 DEG C.Sample is kept the temperature into 2h at 1600 DEG C, then with 10
DEG C speed be cooled to 1000 DEG C, stopping is passed through Ar gases.Powered-down source cooled to room temperature.
Embodiment Three coating is observed it is found that coating surface canescence MoSiTiAl solid solution phases and black SiC phase compositions, coating
Densification, surface is without apparent crackle.
According to GJB323A-96, ablation test is carried out to sample and calculates ablating rate, the ablation time is 30s, 60s, ablation
Center temperature is 2500 DEG C.Coating test coating after 60s ablations keeps complete, does not come off, but surface presence is more porous
Gap and hole, mass ablative rate 0.65mg/s, linear ablative rate are 4.0 μm/s.Comparative example
Density is 1.72g/cm3High purity graphite as matrix, polish smooth rear alcohol ultrasonic cleaning with sand paper
30min, rear 120 DEG C of drying 2h are spare.
By the Mo powder of different proportion, Si powder respectively according to 50:50 mass ratioes alcohol wet-milling 6h on planetary ball mill, takes
Go out drying, mixed powder is obtained after sieving.
It is evenly laid out in graphite pot bottom that powder will be mixed, graphite tank is placed in vacuum sintering furnace.It is evacuated to 10- 3Pa is passed through Ar gases, and heating rate is 10min/ DEG C, is warming up to 1800 DEG C.Sample is kept the temperature into 2h at 1800 DEG C, then with 10
DEG C speed be cooled to 1000 DEG C, stopping is passed through Ar gases.Powered-down source cooled to room temperature.
According to GJB323A-96, ablation test is carried out to sample and calculates ablating rate, the ablation time is 30s, 60s, ablation
Center temperature is 2500 DEG C.Coating test coating after 60s ablations keeps complete, does not come off, but surface presence is more porous
Gap and hole, mass ablative rate 0.98mg/s, linear ablative rate are 9.0 μm/s.
The performance parameter of each embodiment and comparative example is understood in comparison sheet 1:After adding Ti, coating quality ablating rate and line are burnt
Erosion rate is decreased obviously.
Table 1
Claims (10)
1. a kind of Mo-Si-X-C complex phase ceramic coatings, the coating are uniformly mixed by the powder of Mo, Si, X and are placed on carbon base body
On, it is heated to 1500-1600 DEG C and is obtained by the reaction;The X is selected from metal Al and/or Ti.
2. a kind of Mo-Si-X-C complex phase ceramic coatings according to claim 1, it is characterised in that:Described Mo, Si, X press with
Lower mass ratio composition:
Mo:Si:X=(20-30):(40-60):(20-30).
3. a kind of Mo-Si-X-C complex phase ceramic coatings according to claim 2, it is characterised in that:In component X, metal Al,
Ti mixtures in any proportion.
4. a kind of Mo-Si-X-C complex phase ceramic coatings according to claim 1-3 any one, it is characterised in that:Metal
Purity >=99.9% of Mo, the mesh of granularity≤300;
Purity >=99.9% of Si, the mesh of granularity≤300;
Purity >=99.5% of metal Ti, granularity are≤500 mesh;
Purity >=99.7% of metal Al, granularity are≤300 mesh.
5. a kind of preparation method of Mo-Si-X-C complex phase ceramic coatings, includes the following steps:
Step 1
Mo, Si, Ti, Al component proportion by design is uniformly mixed with Mo powder, Si powder, Ti powder, Al powder is taken, obtains mixed-powder;
Step 2
The mixed-powder that step 1 obtains is placed in vacuum sintering furnace, carbon base body is placed in above mixed-powder, is heated to 1500-
1800 DEG C, at least 2 hours are kept the temperature, mixed-powder is deposited to carbon base body, then, is cooled to the speed of 6-15 DEG C/min
800-1000 DEG C, furnace cooling.
6. a kind of preparation method of Mo-Si-X-C complex phase ceramic coatings according to claim 5, it is characterised in that:Step
In one, mixed-powder is uniformly mixed using wet ball-milling, is sieved after the drying of uniformly mixed powder;Wet ball-milling is using planetary
Ball mill, ball-milling medium are alcohol, wet ball-milling time 5-8h, ratio of grinding media to material 5:1-8:1, drum's speed of rotation 200-350 turns/min.
7. a kind of preparation method of Mo-Si-X-C complex phase ceramic coatings according to claim 5, it is characterised in that:Step
In one, Mo, Si, Ti, Al component proportion of design are:
Mo:Si:X=(20-30):(40-60):(20-30);
Purity >=99.9% of metal Mo, the mesh of granularity≤300;
Purity >=99.9% of Si, the mesh of granularity≤300;
Purity >=99.5% of metal Ti, granularity are≤500 mesh;
Purity >=99.7% of metal Al, granularity are≤300 mesh.
8. a kind of preparation method of Mo-Si-X-C complex phase ceramic coatings according to claim 5, it is characterised in that:Step
In two, vacuum degree≤10Pa in vacuum sintering furnace, the protection of temperature-rise period argon gas atmosphere;5-10 DEG C of heating rate/min;During heat preservation
Between 2-3h.
9. a kind of preparation method of Mo-Si-X-C complex phase ceramic coatings according to claim 5, it is characterised in that:Step
In two, mixed-powder is placed in graphite tank, and carbon matrix is placed in 2-4cm positions above graphite tank, and carbon base body and graphite tank are height
Pure graphite is formed, graphite purity >=99.99%.
10. a kind of preparation method of Mo-Si-X-C complex phase ceramic coatings according to claim 5-8 any one, special
Sign is:The Mo-Si-X-C ceramic coating surfaces being prepared are by high-melting-point, the MoSi of resistance to ablation2It is formed with SiC, internal layer is
The multilayer multiphase structure of SiC compositions combined closely with carbon base body, coating and matrix metallurgical binding.
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Cited By (5)
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CN111074190A (en) * | 2019-12-25 | 2020-04-28 | 江苏理工学院 | MoSi on steel surface2Composite coating and preparation method thereof |
CN112851358A (en) * | 2021-01-05 | 2021-05-28 | 北京动力机械研究所 | ZrB2-SiC-Mo(Six,Al1-x)2Zero ablation coating and hot pressing preparation method thereof |
CN112941486A (en) * | 2019-12-10 | 2021-06-11 | 中国科学院金属研究所 | Molybdenum-based thermal oxidation type anti-erosion ceramic coating and preparation method and application thereof |
CN113529012A (en) * | 2021-07-21 | 2021-10-22 | 国网天津市电力公司电力科学研究院 | MoSi for Al modification of surface of power transmission and transformation equipment2Preparation method of-SiC coating |
CN114478019A (en) * | 2020-10-23 | 2022-05-13 | 中南大学 | TiC modified MoSi2Base composite coating and preparation method thereof |
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CN114478019B (en) * | 2020-10-23 | 2023-03-03 | 中南大学 | TiC modified MoSi 2 Base composite coating and preparation method thereof |
CN112851358A (en) * | 2021-01-05 | 2021-05-28 | 北京动力机械研究所 | ZrB2-SiC-Mo(Six,Al1-x)2Zero ablation coating and hot pressing preparation method thereof |
CN113529012A (en) * | 2021-07-21 | 2021-10-22 | 国网天津市电力公司电力科学研究院 | MoSi for Al modification of surface of power transmission and transformation equipment2Preparation method of-SiC coating |
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