CN109023220B - Method for preparing Ti-SiC-C composite coating by reactive plasma spraying - Google Patents

Method for preparing Ti-SiC-C composite coating by reactive plasma spraying Download PDF

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CN109023220B
CN109023220B CN201811117684.8A CN201811117684A CN109023220B CN 109023220 B CN109023220 B CN 109023220B CN 201811117684 A CN201811117684 A CN 201811117684A CN 109023220 B CN109023220 B CN 109023220B
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powder
sic
spraying
coating
plasma spraying
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CN109023220A (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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    • 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 invention relates to a method for preparing a Ti-SiC-C composite coating by plasma spraying. The method comprises the following steps: adding deionized water, gel and a dispersing agent into Ti powder, SiC powder and graphite powder to obtain mixed slurry; preparing agglomerated composite powder from the mixed slurry by a spray drying method; spraying the mixture on the bonding layer through a plasma spraying device, and then carrying out annealing heat treatment in a vacuum or atmosphere protection furnace; the annealing heat treatment temperature is 400-1400 ℃, the heating time is 0.5-4 hours, and the furnace is heated and cooled. The coating prepared by the invention is more uniform in whole, the density is improved, the porosity is reduced, the whole operation process is simple, the process flow is simplified, and the cost is relatively low.

Description

Method for preparing Ti-SiC-C composite coating by reactive plasma spraying
Technical Field
The invention relates to a method for preparing a spray coating and optimizing the quality of the coating, in particular to a method for preparing and optimizing a plasma spray coating with high hardness, high wear resistance and high-temperature oxidation resistance.
Background
The titanium and titanium compound coating is prepared on the surface of a common material, so that the titanium and titanium compound coating becomes a special material for material protection and becomes an important research content of the current surface scientific engineering. For example, TiC cermet material is a heterogeneous composite material composed of metal or alloy and TiC ceramic phase, which not only maintains the characteristics of high strength, high hardness, wear resistance, high temperature resistance, oxidation resistance and chemical stability of ceramic, but also has better metal toughness, and the high temperature oxidation resistance is only lower than that of silicon carbide [ Chenyiyuan ] Yanghuang. 5-9], which is an important raw material for cemented carbide, and thus has been widely used as a hard phase in structural materials for manufacturing wear-resistant materials, cutting tool materials, machine parts, etc., and titanium carbide-based cermets have been attracting attention due to their excellent physicochemical properties.
The SiC ceramic is prepared by using silicon carbide powder and a powder metallurgy method through a reaction sintering or hot-pressing sintering process. The SiC ceramic has the biggest characteristics of high-temperature strength, good thermal stability, good wear resistance and creep resistance. The method is suitable for parts such as throat nozzles for pouring metal, thermocouple sleeves, blades of gas turbines, bearings and the like. Meanwhile, the heat transfer performance is high, so that the heat exchanger is also suitable for heat exchanger materials under high temperature conditions, and can also be used for manufacturing sealing rings of various pumps.
The plasma spraying has the characteristics of simple process, flexibility and convenience, and no need of redesigning workpieces. The reactive plasma spraying integrates the plasma spraying and the self-propagating technology, has high preparation efficiency and low cost, and is suitable for the surfaces of parts with various sizes. Therefore, powder which contains Ti, SiC and C and is suitable for spraying is prepared, the composite powder is fed into plasma flame flow, and self-propagating reaction among the Ti, the C and the SiC is ignited by the high temperature of the flame flow to form products such as TiC, SiC, Ti3SiC2, Ti5Si3 and the like to form a coating. The composite structures of nano-crystalline TiC, SiC, Ti3SiC2 and the like with different contents are obtained by regulating and controlling the component proportion of the composite powder, the powder preparation process and the spraying process, the tissue regulation of the coating is realized, and the composite coating has certain performance advantages of strength, plastic toughness, high temperature oxidation resistance and the like simultaneously by the plasma spraying technology, thereby becoming the primary key point of the experiment.
The annealing heat treatment can improve or eliminate various tissue defects and residual stress caused by the steel in the casting, forging, rolling and welding processes, and prevent the deformation and cracking of the workpiece; softening the workpiece for cutting; grain formation, and improved structure to improve mechanical properties of the workpiece. The coating is subjected to heat treatment at a proper temperature and under proper conditions, so that the problems of non-uniformity, insufficient hole density and the like of the plasma spraying coating can be solved, the stress release in the coating is facilitated, the ductility and toughness of the coating are increased, and a special microstructure is generated, so that the quality and performance of the coating are improved.
Although the SiC ceramic material can be prepared by various modes, the characteristics of poor SiC toughness and high brittleness cannot be changed, and the SiC ceramic material cannot be used for sintering complex parts, so that the application range of the SiC ceramic material is greatly restricted. The preparation of various composite structures for improving SiC materials, particularly TiC and SiC composite materials, is now receiving great attention. The technical purpose of the invention is to obtain a multi-term composite ceramic coating by reactive plasma spraying aiming at respective defects of TiC and SiC coatings, but the coating is influenced by a spraying process, so that a large number of pores or holes inevitably exist in the coating, and the performance quality and the like of the coating are greatly influenced.
Disclosure of Invention
The invention aims to provide a method for preparing a titanium-silicon carbide-carbon ceramic composite coating by plasma spraying, aiming at the defects of the prior art. The preparation method comprises the steps of mixing SiC powder, graphite powder and Ti powder, and granulating by a spray drying method to obtain graphite powder-coated SiC and Ti agglomerated powder; the multinomial composite ceramic coating prepared by reactive plasma spraying has higher hardness, good wear resistance and high-temperature oxidation resistance, and better density and porosity; and the defects of insufficient uniformity, more holes and low density of the plasma spraying coating can be overcome through vacuum annealing heat treatment, and the quality and the performance of the coating are further improved.
The technical scheme of the invention is as follows:
a method for preparing a Ti-SiC-C composite coating by plasma spraying comprises the following steps:
weighing raw material powder according to mass percentage, wherein the raw material powder comprises the following components in percentage by mass: 50-85% of Ti powder, 10-45% of SiC powder and 5-15% of graphite powder;
step two, adding deionized water, gel and a dispersing agent into the weighed raw material powder, and mechanically stirring for 3-5 hours to obtain mixed slurry;
the gel is prepared by mixing deionized water and sodium carboxymethylcellulose, and the mass ratio of the deionized water to the sodium carboxymethylcellulose is as follows: sodium carboxymethylcellulose is 70-120: 1; the dispersant is PVP; the mass ratio of the raw material powder is as follows: deionized water: gel 2: 0.8-3.0: 1, adding 0.5 to 3.5 percent of dispersant PVP (polyvinyl pyrrolidone) by mass based on the total mass of the raw material powder;
step three, preparing the agglomerated composite powder from the mixed slurry by a spray drying method; wherein the inlet temperature of the spray granulator is 260-290 ℃, and the outlet temperature is 110-125 ℃;
drying and screening the agglomerated composite powder to obtain 100-300-mesh agglomerated particles serving as plasma spraying feeding powder;
step five, roughening the surface of the matrix;
step six, spraying Ni-10 wt% of Al self-fluxing alloy powder on the roughened surface of the substrate in advance to obtain a bonding layer with the thickness of 50-120 mu m;
and step seven, adding the spraying feeding powder obtained in the step four into a plasma spraying device, and spraying the powder on the bonding layer to obtain the titanium-silicon carbide-carbon composite coating with the thickness of 200-300 microns.
Step eight, annealing and heat treating the composite coating prepared in the step seven in a vacuum or atmosphere protective furnace; the annealing heat treatment temperature is 400-1400 ℃, the heating time is 0.5-4 hours, and the furnace is heated and cooled.
In the first step, the granularity of Ti powder is 325-500 meshes, the granularity of SiC powder is 300-600 meshes, and the granularity of graphite powder is 8000-15000 meshes.
The matrix roughening treatment in the fifth step is specifically as follows: sanding with sand paper and then surface blasting.
The matrix in the fifth step is made of metal materials such as carbon steel, titanium alloy, high-temperature alloy and the like.
And seventhly, adopting the agglomerated powder screened in the fourth step as a spraying feed, and preparing the titanium-silicon carbide-carbon ceramic composite coating on the surface of the substrate by using plasma spraying, wherein the plasma spraying process parameters comprise that the working voltage is 55-75V, the working current is 400-500A, the argon flow is 20-40L/min, the hydrogen flow is 20-30L/min, the powder feeding speed is 2-5L/min, the spraying distance is 80-120 mm, and argon is simultaneously used as the powder feeding gas and the protective gas.
The invention has the substantive characteristics that:
according to the invention, SiC powder is used as a silicon source, graphite powder is used as a carbon source, and is mixed with Ti powder in different proportions and then granulated by a spray drying method to obtain graphite powder coated SiC and Ti agglomerated powder, the particle size is proper, the coating uniformity is good, the graphite powder coated SiC and Ti agglomerated powder is very suitable for being used as plasma spraying feeding, the problem of powder nonuniformity caused by traditional direct mechanical mixing is solved, and the full reaction of the powder in the plasma spraying process is facilitated; the multiphase composite ceramic coating prepared by reactive plasma spraying has higher hardness, good wear resistance and high-temperature oxidation resistance, and better density and porosity; the vacuum annealing heat treatment can make up the defects of insufficient uniformity, more holes and low density of the plasma spraying coating, and further improve the quality and performance of the coating.
The invention has the beneficial effects that:
(1) the Ti-SiC-C coating mainly comprises TiC, Ti5Si3 and Ti3SiC2, wherein a high-hardness TiC phase is taken as a matrix, a Ti5Si3 phase is taken as a composite reinforcing phase, and Ti3SiC2 is taken as a toughening and wear-reducing phase, so that the coating is high in hardness and good in wear resistance.
(2) By adopting the high-heat-value exothermic reaction of plasma spraying and self-propagating in-situ synthesis of the Ti-SiC-C composite coating, a more uniform structure than that of a cladding coating can be obtained, and the crystal grains are finer.
(3) The Ti powder, the SiC powder and the graphite powder are subjected to mechanical stirring and spray granulation to obtain the agglomerated powder, so that the full reaction of each element powder in the spraying flame flow is facilitated, and the residual of metal Ti is avoided.
(4) The agglomeration powder contains SiC, has high chemical stability, is high-temperature resistant and antioxidant, is beneficial to improving the high-temperature resistance of the coating, and is an economic and environment-friendly raw material.
(5) The coating preparation technology provided by the invention is simple to operate, high in production efficiency and easy to control the coating thickness.
(6) The invention carries out vacuum annealing heat treatment on the coating, so that the coating has the advantages of reducing the size of holes, improving the density, optimizing the quality of the coating, greatly improving the hardness, improving the toughness and improving the wear resistance.
In conclusion, the powder for plasma spraying prepared by the Ti-SiC-C ceramic composite coating prepared by the invention has the characteristics of uniform particle size, high sphericity and strong fluidity, and is suitable for plasma spraying, and the prepared Ti-SiC-C ceramic composite coating has higher hardness, higher toughness and better wear resistance than the original coating after annealing heat treatment, is more uniform in the whole coating, improved in density, reduced in porosity, simple in the whole operation process, simplified in process flow and relatively lower in cost.
Drawings
FIG. 1 is an SEM photograph of the powder after spray granulation in example 2 of the present invention;
FIG. 2 is an XRD pattern of the Ti-SiC-C ceramic composite coating on the surface of the 45# steel substrate in example 2 of the invention;
FIG. 3 is an SEM image of the surface of the Ti-SiC-C ceramic composite coating on the surface of a 45# steel substrate in example 2 of the invention;
FIG. 4 is a SEM image of the cross section of the Ti-SiC-C ceramic composite coating on the surface of a 45# steel substrate in example 2 of the invention;
FIG. 5 is the average value of the microhardness of the Ti-SiC-C ceramic composite coating on the surface of the 45# steel substrate in the examples 1 and 2 of the invention before and after heat treatment under HV0.2 load.
FIG. 6 is a comparison of the average values of fracture toughness before and after heat treatment of the Ti-SiC-C ceramic composite coating on the surface of the 45# steel substrate in example 2 of the present invention.
Detailed Description
The invention will be described in further detail with reference to the following examples of the drawings, which are intended to facilitate the understanding of the invention and are not intended to limit it in any way
Example 1:
the embodiment is a method for preparing and optimizing a Ti-SiC-C ceramic composite coating based on plasma spraying, and the method comprises the following steps:
step one, weighing raw materials according to 81.8 wt% of Ti powder, 11.4 wt% of SiC powder and 6.8 wt% of graphite powder, wherein the purity is 99.9%; wherein, the granularity of Ti powder is 325-500 meshes, the granularity of SiC powder is 300-600 meshes, and the granularity of graphite powder is 8000-15000 meshes.
Step two, adding deionized water and gel (the gel is obtained by mixing water and sodium carboxymethylcellulose in a mass ratio of 100: 1. the gel composition in the following examples is the same), adding 1% of PVP (polyvinyl pyrrolidone) serving as a dispersing agent in the total mass of the raw material powder, mixing, and mechanically stirring for 3 hours to obtain slurry; wherein, the mass ratio of the original powder to the deionized water is 2: 2: 1;
step three, spray drying: spraying the mixed slurry into a drying chamber for atomization, and rapidly drying to form agglomerated particles, wherein the inlet temperature of a spray dryer is 260 ℃ and the outlet temperature of the spray dryer is 110 ℃;
step four, selecting agglomerated particles with the size of 100-300 meshes by using a sieve as spraying feed;
step five, polishing the 45# steel substrate by using sand paper, then carrying out sand blasting roughening treatment, and fixing on a workbench;
step six, spraying Ni-10 wt% of Al as a bonding layer on the coarsened 45 steel substrate by using plasma spraying, wherein the thickness is controlled to be 50-120 mu m;
and seventhly, feeding and spraying the screened agglomerated composite powder on the bonding layer to obtain the Ti-SiC-C ceramic composite coating with the thickness of 200-300 mu m.
The plasma spraying parameters comprise that the working voltage is 70V, the working current is 500A, the argon flow is 30L/min, the hydrogen flow is 20L/min, the powder feeding speed is 2L/min, the spraying distance is 100mm, and argon is simultaneously used as the powder feeding gas and the protective gas.
And step eight, carrying out annealing heat treatment on the composite coating prepared in the step seven in an argon atmosphere protective furnace, heating at 800 ℃ for 1 hour, and heating and cooling along with the furnace.
The SEM image of the powder after spray granulation obtained above is similar to that shown in FIG. 1. It can be seen that after spray granulation, the powder has obvious agglomeration effect, basically presents a spherical or ellipsoidal shape and has better fluidity.
The XRD pattern of the Ti-SiC-C ceramic composite coating on the surface of the 45# steel substrate prepared by the method is similar to that shown in figure 2. It can be seen that the main phases are TiN and Ti5Si3, and a certain amount of Ti3SiC2 is contained, and no elemental phase and SiC phase are detected, which indicates that the agglomerate powder prepared by the present invention is suitable for spray coating and has sufficient reaction.
The surface SEM image of the Ti-SiC-C ceramic composite coating on the surface of the 45# steel substrate prepared in the way is similar to that shown in FIG. 3. It can be seen that the coating surface is denser with a few holes.
The SEM image of the cross section of the Ti-SiC-C ceramic composite coating on the surface of the 45# steel substrate prepared in the way is similar to that shown in the figure 4. The coating is composed of a gray Ti-SiC-C coating on the outer side and a white NiAl transition layer on the inner layer, the Ti-SiC-C coating is obviously combined in a lamellar manner, and the density between layers is high.
The hardness of the Ti-SiC-C ceramic composite coating on the surface of the 45# steel substrate prepared by the method is tested by a microhardness tester, the applied load time of the experiment is 15s, and 200g of load is selected, and for comparison, the Ti-SiC-C ceramic composite coating on the surface of the 45# steel substrate prepared before and after heat treatment in example 1 is subjected to the experiment completely identical to that in example 2. The average hardness of the obtained coating is 1700HV 0.2.
The fracture toughness detection of the Ti-SiC-C ceramic composite coating on the surface of the 45# steel substrate prepared in the way is similar to that shown in FIG. 6. The measurement results show that the toughness of the coating surface is improved by about sixty percent after heat treatment.
Example 2:
the embodiment is a method for preparing and optimizing a Ti-SiC-C ceramic composite coating based on plasma spraying, and the method comprises the following steps:
step one, weighing raw materials according to 74 wt% of Ti powder, 20 wt% of SiC powder and 6 wt% of graphite powder, wherein the purity is 99.9%; wherein, the granularity of Ti powder is 325-500 meshes, the granularity of SiC powder is 300-600 meshes, and the granularity of graphite powder is 8000-15000 meshes.
Step two, adding deionized water and gel (the gel is obtained by mixing water and sodium carboxymethylcellulose in a mass ratio of 100: 1. the gel composition in the following examples is the same), adding 1% of PVP (polyvinyl pyrrolidone) serving as a dispersing agent in the total mass of the raw material powder, mixing, and mechanically stirring for 3 hours to obtain slurry; wherein, the mass ratio of the original powder to the deionized water is 2: 2: 1;
step three, spray drying: spraying the mixed slurry into a drying chamber for atomization, and rapidly drying to form agglomerated particles, wherein the inlet temperature of a spray dryer is 260 ℃ and the outlet temperature of the spray dryer is 110 ℃;
step four, selecting agglomerated particles with the size of 100-300 meshes by using a sieve as spraying feed;
step five, polishing the 45# steel substrate by using sand paper, then carrying out sand blasting roughening treatment, and fixing on a workbench;
step six, spraying Ni-10 wt% of Al as a bonding layer on the coarsened 45 steel substrate by using plasma spraying, wherein the thickness is controlled to be 50-120 mu m;
and seventhly, feeding and spraying the screened agglomerated composite powder on the bonding layer to obtain the Ti-SiC-C ceramic composite coating with the thickness of 200-300 mu m.
The plasma spraying parameters comprise that the working voltage is 70V, the working current is 500A, the argon flow is 30L/min, the hydrogen flow is 20L/min, the powder feeding speed is 2L/min, the spraying distance is 100mm, and argon is simultaneously used as the powder feeding gas and the protective gas.
And step eight, carrying out annealing heat treatment on the composite coating prepared in the step seven in an argon atmosphere protective furnace, heating at 800 ℃ for 1 hour, and heating and cooling along with the furnace.
The SEM image of the spray-granulated powder obtained above is shown in FIG. 1. It can be seen that after spray granulation, the powder is integrally formed into Ti and SiC particles with larger surface C coating particle size, the coating effect is obvious, the sphericity is high, and the powder fluidity is better.
The XRD pattern of the Ti-SiC-C ceramic composite coating on the surface of the 45# steel substrate prepared in the way is shown in figure 2. It can be seen that, in addition to the main phase of TiC and TiN, the peak values of the phases of Ti3SiC2 and Ti5Si3 are high, indicating that the reaction is sufficient and that the type of the phase does not change before and after the vacuum heat treatment.
The surface SEM image of the Ti-SiC-C ceramic composite coating on the surface of the 45# steel substrate prepared in the way is shown in FIG. 3. Compared with the surface which is not subjected to vacuum heat treatment, the surface of the coating after treatment has small holes, the number of the holes is reduced, the surface density is improved, and the overall quality of the coating is improved.
The SEM image of the cross section of the Ti-SiC-C ceramic composite coating on the surface of the 45# steel substrate prepared in the way is shown in FIG. 4. It can be seen that although some holes exist in the cross section, the whole layer is combined compactly, and different elements are distributed uniformly.
Hardness tests were conducted on the Ti-SiC-C ceramic composite coatings on the surfaces of the 45# steel substrates prepared as described above using a microhardness tester, and for comparison, the Ti-SiC-C ceramic composite coatings on the surfaces of the 45# steel substrates prepared before and after the heat treatment in example 2 were subjected to the same experiment as in example 1. As shown in fig. 5, the average hardness of the coating of example 2 was 1543HV0.2, which is significantly improved compared to the non-vacuum annealed coating.
The fracture toughness test of the Ti-SiC-C ceramic composite coating on the surface of the 45# steel substrate prepared in the above way is shown in FIG. 6. The surface toughness of the coating is determined by the fracture toughness numerical index KICCharacterization by measurement and calculation, the original coating KICAbout 1.48, and K after vacuum heat treatmentICIs 2.48, an improvement of nearly seventy percent.
Example 3:
the embodiment is a method for preparing and optimizing a Ti-SiC-C ceramic composite coating based on plasma spraying, and the method comprises the following steps:
step one, weighing raw materials according to 66.7 wt% of Ti powder, 27.8 wt% of SiC powder and 5.5 wt% of graphite powder, wherein the purity is 99.9%; wherein, the granularity of Ti powder is 325-500 meshes, the granularity of SiC powder is 300-600 meshes, and the granularity of graphite powder is 8000-15000 meshes.
Step two, adding deionized water and gel (the gel is obtained by mixing water and sodium carboxymethylcellulose in a mass ratio of 100: 1. the gel composition in the following examples is the same), adding 1% of PVP (polyvinyl pyrrolidone) serving as a dispersing agent in the total mass of the raw material powder, mixing, and mechanically stirring for 3 hours to obtain slurry; wherein, the mass ratio of the original powder to the deionized water is 2: 2: 1;
step three, spray drying: spraying the mixed slurry into a drying chamber for atomization, and rapidly drying to form agglomerated particles, wherein the inlet temperature of a spray dryer is 260 ℃ and the outlet temperature of the spray dryer is 110 ℃;
step four, selecting agglomerated particles with the size of 100-300 meshes by using a sieve as spraying feed;
step five, polishing the 45# steel substrate by using sand paper, then carrying out sand blasting roughening treatment, and fixing on a workbench;
step six, spraying Ni-10 wt% of Al as a bonding layer on the coarsened 45 steel substrate by using plasma spraying, wherein the thickness is controlled to be 50-120 mu m;
and seventhly, feeding and spraying the screened agglomerated composite powder on the bonding layer to obtain the Ti-SiC-C ceramic composite coating with the thickness of 200-300 mu m.
The plasma spraying parameters comprise that the working voltage is 70V, the working current is 500A, the argon flow is 30L/min, the hydrogen flow is 20L/min, the powder feeding speed is 2L/min, the spraying distance is 100mm, and argon is simultaneously used as the powder feeding gas and the protective gas.
And step eight, carrying out annealing heat treatment on the composite coating prepared in the step seven in an argon atmosphere protective furnace, heating at 800 ℃ for 1 hour, and heating and cooling along with the furnace.
The SEM image of the powder after spray granulation obtained above is similar to that shown in FIG. 1. It can be seen that after spray granulation, the powder has obvious agglomeration effect, basically presents a spherical or ellipsoidal shape and has better fluidity.
The XRD pattern of the Ti-SiC-C ceramic composite coating on the surface of the 45# steel substrate prepared by the method is similar to that shown in figure 2. It can be seen that the main phases are TiC, TiN and Ti5Si3, and a certain amount of Ti3SiC2 is contained, so that the reaction is relatively sufficient.
The surface SEM image of the Ti-SiC-C ceramic composite coating on the surface of the 45# steel substrate prepared in the way is similar to that shown in FIG. 3. It can be seen that the surface of the coating is relatively dense, a small number of holes exist, and the compactness can be further improved by improving the process.
The SEM image of the cross section of the Ti-SiC-C ceramic composite coating on the surface of the 45# steel substrate prepared in the way is similar to that shown in the figure 4. The coating is composed of a gray Ti-SiC-C coating on the outer side and a white NiAl transition layer on the inner layer, the Ti-SiC-C coating is obviously combined in a lamellar manner, and the density between layers is high.
The Ti-SiC-C ceramic composite coating on the surface of the 45# steel substrate prepared by the method is subjected to microhardness test in example 2, and the average hardness of the obtained coating is 1414HV 0.2.
Fracture toughness detection of the Ti-SiC-C ceramic composite coating on the surface of the 45# steel substrate is similar to that shown in FIG. 6, and the measurement result shows that the toughness of the coating surface is improved by about fifty percent after heat treatment.
The embodiments described above are intended to illustrate the technical solutions of the present invention in detail, and it should be understood that the above-mentioned embodiments are only specific embodiments of the present invention, and are not intended to limit the present invention, and any modification, supplement or similar substitution made within the scope of the principles of the present invention should be included in the protection scope of the present invention.
The invention is not the best known technology.

Claims (2)

1. A method for preparing a Ti-SiC-C composite coating by plasma spraying is characterized by comprising the following steps:
weighing raw material powder according to mass percentage, wherein the raw material powder comprises the following components in percentage by mass: 50-85% of Ti powder, 10-45% of SiC powder and 5-15% of graphite powder;
step two, adding deionized water, gel and a dispersing agent into the weighed raw material powder, and mechanically stirring for 3-5 hours to obtain mixed slurry;
the gel is prepared by mixing deionized water and sodium carboxymethylcellulose, and the mass ratio of the deionized water to the sodium carboxymethylcellulose is as follows: sodium carboxymethylcellulose is 70-120: 1; the dispersant is PVP; the mass ratio of the raw material powder is as follows: deionized water: gel 2: 0.8-3.0: 1, adding 0.5 to 3.5 percent of dispersant PVP (polyvinyl pyrrolidone) by mass based on the total mass of the raw material powder;
step three, preparing the agglomerated composite powder from the mixed slurry by a spray drying method; wherein the inlet temperature of the spray granulator is 260-290 ℃, and the outlet temperature is 110-125 ℃;
drying and screening the agglomerated composite powder to obtain 100-300-mesh agglomerated particles serving as plasma spraying feeding powder;
step five, roughening the surface of the matrix;
step six, spraying Ni-10 wt% of Al self-fluxing alloy powder on the roughened surface of the substrate in advance to obtain a bonding layer with the thickness of 50-120 mu m;
step seven, adding the spraying feeding powder obtained in the step four into a plasma spraying device, and spraying the powder on the bonding layer to obtain a titanium-silicon carbide-carbon composite coating with the thickness of 200-300 microns;
step eight, annealing and heat treating the composite coating prepared in the step seven in a vacuum or atmosphere protective furnace; the annealing heat treatment temperature is 400-1400 ℃, the heating time is 0.5-4 hours, and the annealing heat treatment is heated and cooled along with the furnace;
in the first step, the granularity of Ti powder is 325-500 meshes, the granularity of SiC powder is 300-600 meshes, and the granularity of graphite powder is 8000-15000 meshes;
the matrix in the fifth step is carbon steel, titanium alloy or high-temperature alloy;
the method comprises the following steps of seven, adopting the agglomerated powder screened in the fourth step as a spraying feed, and preparing a titanium-silicon carbide-carbon ceramic composite coating on the surface of a substrate by using plasma spraying, wherein the plasma spraying process parameters comprise that the working voltage is 55-75V, the working current is 400-500A, the argon flow is 20-40L/min, the hydrogen flow is 20-30L/min, the powder feeding speed is 2-5L/min, the spraying distance is 80-120 mm, and argon is simultaneously used as the powder feeding gas and the protective gas;
the dispersant is PVP.
2. The method for preparing the Ti-SiC-C composite coating by plasma spraying according to claim 1, wherein the matrix roughening treatment in the fifth step is specifically: sanding with sand paper and then surface blasting.
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