CN109023220A - A kind of method that reaction and plasma spraying prepares Ti-SiC-C composite coating - Google Patents

A kind of method that reaction and plasma spraying prepares Ti-SiC-C composite coating Download PDF

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CN109023220A
CN109023220A CN201811117684.8A CN201811117684A CN109023220A CN 109023220 A CN109023220 A CN 109023220A CN 201811117684 A CN201811117684 A CN 201811117684A CN 109023220 A CN109023220 A CN 109023220A
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powder
sic
composite coating
coating
mesh
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CN109023220B (en
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章凡勇
李超
闫姝
何继宁
殷福星
丁一
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Hebei University of Technology
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Hebei University of Technology
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C4/00Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/12Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
    • C23C4/134Plasma spraying
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C4/00Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/04Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
    • C23C4/06Metallic material
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C4/00Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/18After-treatment

Abstract

The present invention is a kind of method that plasma spraying prepares Ti-SiC-C composite coating.Method includes the following steps: deionized water, gel, dispersing agent are added into Ti powder, SiC powder, graphite powder, mixed slurry is obtained;Mixed slurry is prepared to the composite granule of reunion by spray drying process;By being sprayed on above adhesive layer in plasma spray apparatus, then annealing heat-treatment is carried out in vacuum or atmosphere protection stove;Annealing heat-treatment temperature is 400 DEG C -1400 DEG C, and heating time is 0.5-4 hours, cooling with stove heating.Coating prepared by the present invention, whole more uniform, consistency improves, porosity reduces, and whole operation process is simple, simplifies process flow, and cost is relatively low.

Description

A kind of method that reaction and plasma spraying prepares Ti-SiC-C composite coating
Technical field
The present invention relates to the methods that a kind of preparation of spray-on coating and coating quality optimize, more particularly to one kind to have height hard Degree, high-wearing feature, resistance to high temperature oxidation plasma spraying coating prepare optimization method.
Background technique
The compound coat of titanium and titanium is prepared on common material surface, the special type material of material protection is made, becomes The important research content of Surface Science engineering at present.Such as TiC cermet material, it is that one kind is made pottery by metal or alloy with TiC Heterogeneous composite material composed by porcelain phase, it had both maintained the high intensity of ceramics, high rigidity, wear-resistant, high temperature resistant, antioxygen The characteristics such as change and chemical stability, and have preferable metal toughness, high-temperature oxidation resistance is only below silicon carbide [Chen Yi member Zou Positive light dragon flies the synthesis and its application study status Ti industry progress of TiC-based cermet, 2007,24 (3): 5-9], It is the important source material of hard alloy, therefore is widely used in making wear-resistant material, cutting as hard phase in structural material Cutter material, machine components etc. make TiC-based cermet by pass just because of these excellent physical and chemical performances Note.
SiC ceramic is to use carborundum powder, is made of the reacted sintering of powder metallurgic method or hot-pressing sintering technique.SiC ceramic Maximum feature is that elevated temperature strength is big, thermal stability is good, wear-resisting creep resistance is good.Larynx mouth, thermocouple suitable for casting metal The parts such as casing, the blade of gas turbine, bearing.Simultaneously because its capacity of heat transmission is high, apply also under hot conditions Heat exchanger material, it can also be used to make the sealing ring of various pumps.
Plasma spraying has the characteristics that simple process, flexible and convenient, workpiece without redesigning.Reaction and plasma spraying Integrate plasma spraying and self- propagating technology, preparation efficiency height is at low cost, is suitable for various sizes piece surface.Therefore The powder for the suitable spraying that one kind contains Ti, SiC and C is prepared, composite powder is sent into plasma flame flow, by flame stream High temperature is lighted and forms the products such as TiC, SiC, Ti3SiC2, Ti5Si3 formation coating from climing combustion reaction between Ti, C, SiC.Pass through tune Composite powder composition proportion, powder process and spraying process are controlled, nanocrystalline TiC, SiC, Ti3SiC2 of different content etc. are obtained Complex tissue realizes the tissue modulation of coating, make composite coating both by plasma spraying technology and meanwhile have both certain intensity, The feature performance benefits such as plasticity and toughness, high temperature oxidation resisting become the primary emphasis of experiment.
Annealing heat-treatment can improve or eliminate steel in casting, forging and stamping, rolling and welding process caused by it is various Tissue defects and residual stress prevent workpiece deformation, cracking;Soften workpiece to carry out machining;Change crystal grain, improvement group It knits to improve mechanical performance of workpiece etc..Temperature appropriate and under the conditions of coating is heat-treated, plasma can be made up The problems such as spray-on coating is uneven, hole consistency is insufficient facilitates coat inside release stress, increases its ductility and tough Property, generate special microstructure, to promote coating quality and performance.
Although SiC ceramic material can be prepared there are many mode, but still it can not change SiC poor toughness, the high feature of brittleness, and It cannot be used for the sintering of complex parts, greatly constrain the application range of SiC ceramic.Multinomial composite construction preparation improves SiC Nowadays material especially TiC and SiC ceramic matrix composite material have attracted much attention.Technical purpose of the invention is for TiC and SiC coating respectively Deficiency, a kind of multinomial composite ceramic coat is made by reaction and plasma spraying, but is influenced by spraying process, coating In unavoidably there is a large amount of hole or hole, the performance quality etc. of coating is produced bigger effect.
Summary of the invention
It is an object of the present invention in view of the deficiencies of the prior art, provide a kind of plasma spraying to prepare titanium-silicon carbide-carbon The method of ceramic composite coating.The present invention is granulated acquisition stone by spray drying process using after SiC powder, graphite powder, the mixing of Ti powder The reunion powder of ink powder coated Si/C and Ti;The multinomial composite ceramic coat as made from reaction and plasma spraying is with higher hard Degree, good wearability and high temperature oxidation resistance, consistency, porosity are preferable;It is heat-treated, can make up using vacuum annealing The disadvantage that plasma spraying coating uniformity is inadequate, hole is more, consistency is low further promotes the quality and performance of coating.
The technical solution of the present invention is as follows:
A kind of method that plasma spraying prepares Ti-SiC-C composite coating, comprising the following steps:
Step 1: weighing raw material powder by mass percentage, wherein the ratio of each component in raw material powder are as follows: 50%~ 85% is Ti powder, and 10%~45 is SiC powder, and 5%~15% is graphite powder;
Step 2: deionized water, gel, dispersing agent are added into load weighted raw material powder, after mechanical stirring 3~5 hours Obtain mixed slurry;
Wherein, gel is mixed to prepare by deionized water and sodium carboxymethylcellulose, and mass ratio is deionized water: carboxymethyl is fine Tie up element sodium=70~120:1;, dispersing agent used is PVP;Mass ratio is raw material powder: deionized water: gel=2:0.8~3.0: 1, the dispersing agent PVP mass of addition is the 0.5%-3.5% of raw material powder gross mass;
Step 3: mixed slurry to be prepared to the composite granule of reunion by spray drying process;Wherein, mist projection granulating device Inlet temperature is 260~290 DEG C, and outlet temperature is 110~125 DEG C;
Step 4: the composite granule of reunion is dried, sub-sieve, 100 mesh~300 mesh agglomerated particle is obtained, as Plasma spraying feeding powder;
Step 5: carrying out roughening treatment to matrix surface;
Step 6: the matrix surface in roughening sprays Ni-10wt%Al self-fluxing alloyed powder in advance, obtain with a thickness of 50 ~120 μm of adhesive layer;
Step 7: the spraying feedstock powder obtained in step 4 is added in plasma spray apparatus, it is sprayed on adhesive layer Above, titanium-silicon carbide-carbon composite coating is obtained, with a thickness of 200~300 μm.
Step 8: composite coating obtained in step 7 is carried out annealing heat-treatment in vacuum or atmosphere protection stove;It moves back Heat treat temperatures are 400 DEG C -1400 DEG C, and heating time is 0.5-4 hours, cooling with stove heating.
The granularity of Ti powder is 325 mesh~500 mesh in the step 1, and the granularity of SiC powder is 300~600 mesh, graphite powder Granularity is 8000 mesh~15000 mesh.
Matrix roughening treatment in the step 5 specifically: first polished with sand paper, then carry out surface sand-blasting.
The step 5 matrix is specially the metal materials such as carbon steel, titanium alloy, high temperature alloy.
Matrix table is coated in using plasma spray as spraying feedstock using the reunion powder of step 4 screening in the step 7 Wheat flour is for titanium-silicon carbide-carbon ceramic composite coating, wherein plasma spray coating process parameter are as follows: operating voltage is 55~75V, work Make electric current be 400~500A, argon flow be 20~40L/min, hydrogen flowing quantity be 20~30L/min, powder feed rate be 2~ 5L/min, spray distance are 80~120mm, and wherein argon gas is used as powder feeding gas and protection gas simultaneously.
Substantive distinguishing features of the invention are as follows:
The present invention is using SiC powder as silicon source, and graphite powder is as carbon source, by spraying after mixing in varing proportions with Ti powder Seasoning is granulated the reunion powder for obtaining graphite powder coated Si/C and Ti, and granularity is suitable, and being evenly coated property is good, is highly suitable as Plasma spray feeding overcomes traditional directly mechanical mixture bring powder non-uniformity problem, is conducive to powder in plasma It is sufficiently reacted in spraying process;Multiphase composite coating hardness with higher, good as made from reaction and plasma spraying Good wearability and high temperature oxidation resistance, consistency, porosity is preferable;Vacuum annealing heat treatment, can make up plasma spraying The disadvantage that coating uniformity is inadequate, hole is more, consistency is low further promotes the quality and performance of coating.
The invention has the benefit that
(1) Ti-SiC-C coating of the invention is mainly made of TiC, Ti5Si3 and Ti3SiC2, wherein high hard TiC phase is Matrix, Ti5Si3 phase are used as composite strengthening phase, and Ti3SiC2 is as toughening anti-attrition phase, and the hardness of coating is high, wearability is good.
(2) the high heating value exothermic reaction of plasma spraying is used, self- propagating fabricated in situ Ti-SiC-C composite coating can obtain The tissue more more uniform than cladding coating is obtained, and crystal grain is more tiny.
(3) present invention is by Ti powder, and SiC powder and graphite powder obtain reunion powder by mechanical stirring and mist projection granulating mode, has Help abundant reaction of each element powder in spraying flame stream, avoids the residual of metal Ti.
(4) the reunion powder in the present invention contains SiC, and chemical stability is high, and fire-resistant oxidation resistant helps to improve coating High temperature resistance is a kind of economic and environment-friendly original material.
(5) coat preparing technology of the invention is easy to operate, high production efficiency, and coating layer thickness is easy to control.
(6) present invention carries out vacuum annealing heat treatment to coating, so that coating hole reduces reduction, consistency improves coating Quality is optimised, and hardness significantly increases, and toughness improves, and wearability enhancement can be promoted.
In conclusion Ti-SiC-C ceramic composite coating prepared by the present invention, powder used for plasma spraying obtained has Particle size uniformity, sphericity is high, the strong feature of mobility, and suitable plasma spraying uses, and Ti-SiC- obtained C ceramic composite coating has hardness more higher than former coating, higher toughness and more preferable wearability after annealing heat-treatment, applies Layer is whole more uniform, and consistency improves, porosity reduces, and whole operation process is simple, simplifies process flow, cost also phase To lower.
Detailed description of the invention
Fig. 1 is the SEM figure of powder after mist projection granulating in the embodiment of the present invention 2;
Fig. 2 is the XRD spectrum of 45# steel matrix surface Ti-SiC-C ceramic composite coating in the embodiment of the present invention 2;
Fig. 3 is that 45# steel matrix surface Ti-SiC-C ceramic composite coating surface SEM schemes in the embodiment of the present invention 2;
Fig. 4 is that 45# steel matrix surface Ti-SiC-C ceramic composite coating section SEM schemes in the embodiment of the present invention 2;
Fig. 5 be in the embodiment of the present invention 1,2 45# steel matrix surface Ti-SiC-C ceramic composite coating under HV0.2 load Heat treatment front and back microhardness average value.
Fig. 6 is that 45# steel matrix surface Ti-SiC-C ceramic composite coating heat treatment front and back fracture is tough in the embodiment of the present invention 2 Property mean value compares.
Specific embodiment
Present invention is further described in detail for embodiment with reference to the accompanying drawing, it should be pointed out that implementation as described below Example is intended to convenient for the understanding of the present invention, and does not play any restriction effect to it
Embodiment 1:
A kind of method that the present embodiment prepared based on plasma spraying and optimized Ti-SiC-C ceramic composite coating, including with Lower step:
Step 1: weighing raw material, purity respectively according to Ti powder 81.8wt%, SiC powder 11.4wt%, graphite powder 6.8wt% It is 99.9%;Wherein, the granularity of Ti powder is 325 mesh~500 mesh, and the granularity of SiC powder is 300~600 mesh, the granularity of graphite powder For 8000 mesh~15000 mesh.
Step 2: be added into raw material powder deionized water and gel (gel is according to quality than water: carboxycellulose sodium= 100:1 is obtained by mixing.Gel composition is same in following embodiment), the 1%PVP for adding raw material powder gross mass is dispersing agent, is carried out Mixing, mechanical stirring 3h obtain slurry;Wherein, the original powder of mass ratio, deionized water, gel=2:2:1;
Step 3: spray drying: mixed slurry penetrating hothouse is atomization, and drying forms agglomerated particle rapidly, wherein The inlet temperature of spray dryer is 260 DEG C, and outlet temperature is 110 DEG C;
Step 4: using sieve select scale 100 mesh~300 agglomerated particle as spraying feedstock;
Step 5: clean, then progress sandblasting roughening treatment that 45# steel matrix is polished with sand paper, and it is fixed on workbench On;
Step 6: being coated in No. 45 steel matrix spraying Ni-10wt%Al of roughening as adhesive layer, thickness using plasma spray Control is at 50~120 μm;
Step 7: the reunion composite granule feeding screened is sprayed on adhesive layer again, obtain with a thickness of 200~300 μ The Ti-SiC-C ceramic composite coating of m.
The Plasma Spray Parameters are as follows: operating voltage 70V, operating current 500A, argon flow 30L/ Min, hydrogen flowing quantity 20L/min, powder feed rate 2L/min, spray distance 100mm are sent wherein being used as simultaneously using argon gas Powder gas and protection gas.
Step 8: composite coating obtained in step 7 is carried out annealing heat-treatment in argon atmosphere protection stove, heat Temperature is 800 DEG C, and heating time is 1 hour, cooling with stove heating.
It is similar to Figure 1 to the SEM figure obtained above for stating powder after mist projection granulating.It can be seen that passing through mist projection granulating Afterwards, powder reuniting effect is obvious, and basic presentation is spherical or spheroid shape, mobility are preferable.
It is similar to Figure 2 to the XRD spectrum of 45# steel matrix obtained above surface Ti-SiC-C ceramic composite coating.It can To find out, main object is mutually that containing a certain amount of Ti3SiC2 simple substance object phase and SiC phase is not detected in TiN and Ti5Si3, this says Bright reunion powder prepared by the present invention is suitble to spray, and reacts abundant.
It is similar to Figure 3 to the surface SEM figure of 45# steel matrix obtained above surface Ti-SiC-C ceramic composite coating. As can be seen that coating surface is comparatively dense, there are a small amount of holes.
Shown in section SEM figure similar 4 to 45# steel matrix obtained above surface Ti-SiC-C ceramic composite coating.It can To find out, coating is made of the NiAl transition zone of Ti-SiC-C coating and the internal layer white of outside grey, and Ti-SiC-C coating is in Now apparent lamellar combines, and consistency between layers is higher.
Hardness survey is carried out with microhardness tester to 45# steel matrix obtained above surface Ti-SiC-C ceramic composite coating Examination, it is 15s that this experiment, which applies load-time, and magnitude of load selects 200g, for the sake of comparing, before being heat-treated in embodiment 1 45# steel matrix obtained surface Ti-SiC-C ceramic composite coating carries out and the identical experiment of embodiment 2 afterwards.Obtained painting Layer hardness average mean is 1700HV0.2.
Fracture toughness is carried out to 45# steel matrix obtained above surface Ti-SiC-C ceramic composite coating and detects similar Fig. 6 It is shown.Coating surface toughness improves 60 or so percent after measurement result display heat treatment.
Embodiment 2:
A kind of method that the present embodiment prepared based on plasma spraying and optimized Ti-SiC-C ceramic composite coating, including with Lower step:
Step 1: weighing raw material respectively according to Ti powder 74wt%, SiC powder 20wt%, graphite powder 6wt%, purity is 99.9%;Wherein, the granularity of Ti powder is 325 mesh~500 mesh, and the granularity of SiC powder is 300~600 mesh, and the granularity of graphite powder is 8000 mesh~15000 mesh.
Step 2: be added into raw material powder deionized water and gel (gel is according to quality than water: carboxycellulose sodium= 100:1 is obtained by mixing.Gel composition is same in following embodiment), the 1%PVP for adding raw material powder gross mass is dispersing agent, is carried out Mixing, mechanical stirring 3h obtain slurry;Wherein, the original powder of mass ratio, deionized water, gel=2:2:1;
Step 3: spray drying: mixed slurry penetrating hothouse is atomization, and drying forms agglomerated particle rapidly, wherein The inlet temperature of spray dryer is 260 DEG C, and outlet temperature is 110 DEG C;
Step 4: using sieve select scale 100 mesh~300 agglomerated particle as spraying feedstock;
Step 5: clean, then progress sandblasting roughening treatment that 45# steel matrix is polished with sand paper, and it is fixed on workbench On;
Step 6: being coated in No. 45 steel matrix spraying Ni-10wt%Al of roughening as adhesive layer, thickness using plasma spray Control is at 50~120 μm;
Step 7: the reunion composite granule feeding screened is sprayed on adhesive layer again, obtain with a thickness of 200~300 μ The Ti-SiC-C ceramic composite coating of m.
The Plasma Spray Parameters are as follows: operating voltage 70V, operating current 500A, argon flow 30L/ Min, hydrogen flowing quantity 20L/min, powder feed rate 2L/min, spray distance 100mm are sent wherein being used as simultaneously using argon gas Powder gas and protection gas.
Step 8: composite coating obtained in step 7 is carried out annealing heat-treatment in argon atmosphere protection stove, heat Temperature is 800 DEG C, and heating time is 1 hour, cooling with stove heating.
As indicated with 1 to the SEM figure obtained above for stating powder after mist projection granulating.It can be seen that after mist projection granulating, powder Body overall structure is the biggish Ti of surface C coated granularity, SiC particulate, and covered effect is obvious, and sphericity is high, powder fluidity compared with It is good.
It is as shown in Figure 2 to the XRD spectrum of 45# steel matrix obtained above surface Ti-SiC-C ceramic composite coating.It can be with To find out, outside main phase TiC, TiN substance, the object phase peak value of Ti3SiC2, Ti5Si3 are higher, illustrate that reaction is more abundant, and Compound type does not change before and after vacuum heat treatment.
It is as shown in Figure 3 to the surface SEM figure of 45# steel matrix obtained above surface Ti-SiC-C ceramic composite coating.It can To find out, compared with non-vacuum heat treatment surface, coating surface hole becomes smaller after processing, and pore quantity is reduced, and surface causes Density is promoted, and coating total quality makes moderate progress.
It is as shown in Figure 4 to the section SEM figure of 45# steel matrix obtained above surface Ti-SiC-C ceramic composite coating.It can To find out, although section, there are certain hole, integral layer is fine and close in conjunction with layer, different Elemental redistributions are uniform.
Hardness survey is carried out with microhardness tester to 45# steel matrix obtained above surface Ti-SiC-C ceramic composite coating Examination, for the sake of comparing, to 45# steel matrix surface Ti-SiC-C ceramic composite coating made from heat treatment front and back in embodiment 2 It carries out and the identical experiment of embodiment 1.As shown in figure 5, the coating hardness average value for measuring embodiment 2 is 1543HV0.2, It is substantially improved compared with non-vacuum annealing process.
Fracture toughness detection is carried out such as Fig. 6 institute to 45# steel matrix obtained above surface Ti-SiC-C ceramic composite coating Show.Coating surface toughness is by fracture toughness numerical indication KICCharacterization, by survey calculation it is found that original coating KICFor 1.48 left sides The right side, its K after carrying out vacuum heat treatmentICIt is 2.48, promotes nearly 70 percent.
Embodiment 3:
A kind of method that the present embodiment prepared based on plasma spraying and optimized Ti-SiC-C ceramic composite coating, including with Lower step:
Step 1: weighing raw material, purity respectively according to Ti powder 66.7wt%, SiC powder 27.8wt%, graphite powder 5.5wt% It is 99.9%;Wherein, the granularity of Ti powder is 325 mesh~500 mesh, and the granularity of SiC powder is 300~600 mesh, the granularity of graphite powder For 8000 mesh~15000 mesh.
Step 2: be added into raw material powder deionized water and gel (gel is according to quality than water: carboxycellulose sodium= 100:1 is obtained by mixing.Gel composition is same in following embodiment), the 1%PVP for adding raw material powder gross mass is dispersing agent, is carried out Mixing, mechanical stirring 3h obtain slurry;Wherein, the original powder of mass ratio, deionized water, gel=2:2:1;
Step 3: spray drying: mixed slurry penetrating hothouse is atomization, and drying forms agglomerated particle rapidly, wherein The inlet temperature of spray dryer is 260 DEG C, and outlet temperature is 110 DEG C;
Step 4: using sieve select scale 100 mesh~300 agglomerated particle as spraying feedstock;
Step 5: clean, then progress sandblasting roughening treatment that 45# steel matrix is polished with sand paper, and it is fixed on workbench On;
Step 6: being coated in No. 45 steel matrix spraying Ni-10wt%Al of roughening as adhesive layer, thickness using plasma spray Control is at 50~120 μm;
Step 7: the reunion composite granule feeding screened is sprayed on adhesive layer again, obtain with a thickness of 200~300 μ The Ti-SiC-C ceramic composite coating of m.
The Plasma Spray Parameters are as follows: operating voltage 70V, operating current 500A, argon flow 30L/ Min, hydrogen flowing quantity 20L/min, powder feed rate 2L/min, spray distance 100mm are sent wherein being used as simultaneously using argon gas Powder gas and protection gas.
Step 8: composite coating obtained in step 7 is carried out annealing heat-treatment in argon atmosphere protection stove, heat Temperature is 800 DEG C, and heating time is 1 hour, cooling with stove heating.
It is similar to Figure 1 to the SEM figure obtained above for stating powder after mist projection granulating.It can be seen that passing through mist projection granulating Afterwards, powder reuniting effect is obvious, and basic presentation is spherical or spheroid shape, mobility are preferable.
It is similar to Figure 2 to the XRD spectrum of 45# steel matrix obtained above surface Ti-SiC-C ceramic composite coating.It can To find out, main object is mutually that TiC, TiN and Ti5Si3 react more abundant containing a certain amount of Ti3SiC2.
It is similar to Figure 3 to the surface SEM figure of 45# steel matrix obtained above surface Ti-SiC-C ceramic composite coating. As can be seen that coating surface is comparatively dense, there are a small amount of holes, can further increase consistency by improving technique.
Shown in section SEM figure similar 4 to 45# steel matrix obtained above surface Ti-SiC-C ceramic composite coating.It can To find out, coating is made of the NiAl transition zone of Ti-SiC-C coating and the internal layer white of outside grey, and Ti-SiC-C coating is in Now apparent lamellar combines, and consistency between layers is higher.
It is micro- in such as embodiment 2 with carrying out to 45# steel matrix obtained above surface Ti-SiC-C ceramic composite coating Hardness test, obtained coating hardness average mean are 1414HV0.2.
Fracture toughness is carried out to 45# steel matrix obtained above surface Ti-SiC-C ceramic composite coating and detects similar Fig. 6 Shown, coating surface toughness improves 50 or so percent after measurement result display heat treatment.
Technical solution of the present invention is described in detail in embodiment described above, it should be understood that the above is only For specific embodiments of the present invention, it is not intended to restrict the invention, all any modifications made in spirit of the invention, Supplement or similar fashion substitution etc., should all be included in the protection scope of the present invention.
Unaccomplished matter of the present invention is well-known technique.

Claims (6)

1. a kind of method that plasma spraying prepares Ti-SiC-C composite coating, it is characterized in that method includes the following steps:
Step 1: weighing raw material powder by mass percentage, wherein the ratio of each component in raw material powder are as follows: 50% ~ 85% is Ti powder, 10% ~ 45 is SiC powder, and 5% ~ 15% is graphite powder;
Step 2: deionized water, gel, dispersing agent are added into load weighted raw material powder, mechanical stirring is mixed after 3 ~ 5 hours Close slurry;
Wherein, gel is mixed to prepare by deionized water and sodium carboxymethylcellulose, and mass ratio is deionized water: carboxymethyl cellulose Sodium=70 ~ 120:1;, dispersing agent used is PVP;Mass ratio is raw material powder: deionized water: gel=2:0.8 ~ 3.0:1, addition Dispersing agent PVP mass is the 0.5%-3.5% of raw material powder gross mass;
Step 3: mixed slurry to be prepared to the composite granule of reunion by spray drying process;Wherein, the entrance of mist projection granulating device Temperature is 260 ~ 290 DEG C, and outlet temperature is 110 ~ 125 DEG C;
Step 4: the composite granule of reunion is dried, sub-sieve, 100 mesh ~ 300 mesh agglomerated particle is obtained, as plasma Spraying feedstock powder;
Step 5: carrying out roughening treatment to matrix surface;
Step 6: the matrix surface in roughening sprays Ni-10wt%Al self-fluxing alloyed powder in advance, obtain with a thickness of 50 ~ 120 μ The adhesive layer of m;
Step 7: the spraying feedstock powder obtained in step 4 is added in plasma spray apparatus, it is sprayed on above adhesive layer, Titanium-silicon carbide-carbon composite coating is obtained, with a thickness of 200 ~ 300 μm;
Step 8: composite coating obtained in step 7 is carried out annealing heat-treatment in vacuum or atmosphere protection stove;Annealing heat Treatment temperature is 400 DEG C -1400 DEG C, and heating time is 0.5-4 hours, cooling with stove heating.
2. the method that plasma spraying as described in claim 1 prepares Ti-SiC-C composite coating, it is characterized in that the step The granularity of Ti powder is 325 mesh ~ 500 mesh in one, and the granularity of SiC powder is 300 ~ 600 mesh, and the granularity of graphite powder is 8000 mesh ~ 15000 Mesh.
3. the method that plasma spraying as described in claim 1 prepares Ti-SiC-C composite coating, it is characterized in that the step Matrix roughening treatment in five specifically: first polished with sand paper, then carry out surface sand-blasting.
4. the method that plasma spraying as described in claim 1 prepares Ti-SiC-C composite coating, it is characterized in that the step Five matrixes are specially the metal materials such as carbon steel, titanium alloy, high temperature alloy.
5. the method that plasma spraying as described in claim 1 prepares Ti-SiC-C composite coating, it is characterized in that the step Matrix surface is coated in using plasma spray and prepares titanium-silicon carbide-as spraying feedstock using the reunion powder of step 4 screening in seven Carbon ceramics composite coating, wherein plasma spray coating process parameter are as follows: operating voltage be 55 ~ 75V, operating current be 400 ~ 500A, argon flow are 20 ~ 40L/min, and hydrogen flowing quantity is 20 ~ 30L/min, and powder feed rate is 2 ~ 5L/min, spray distance is 80 ~ 120mm, wherein argon gas is used as powder feeding gas and protection gas simultaneously.
6. the method that plasma spraying as described in claim 1 prepares Ti-SiC-C composite coating, it is characterized in that point Powder is PVP.
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CN111254376A (en) * 2020-03-15 2020-06-09 河北工业大学 Preparation method of high-entropy ceramic composite coating
CN111334742A (en) * 2020-03-15 2020-06-26 河北工业大学 Method for preparing ceramic composite coating of refractory transition metal compound
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