CN112795914A - Method for preparing in-situ synthesized TiC/NiCrBSi composite coating on surface of die steel - Google Patents
Method for preparing in-situ synthesized TiC/NiCrBSi composite coating on surface of die steel Download PDFInfo
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- 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
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- C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
- C23C24/103—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
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Abstract
The invention discloses a method for preparing a TiC/NiCrBSi composite coating on the surface of die steel, which comprises the following steps: mixing Ti powder, graphite powder and NiCrBSi alloy powder; cutting the die steel and performing surface pretreatment; using a water glass colloid as a binder, uniformly stirring the mixed powder in the first step and water glass to prepare a paste, and coating the paste on the surface of the die steel; placing the coated substrate in a forced air drying oven to fully volatilize the binder; putting the dried sample into a hollow graphite base; placing the die steel and the graphite base together under an induction coil for induction cladding; putting the die steel subjected to cladding into a vacuum tube furnace, and carrying out solid solution treatment; and putting the die steel into a vacuum tube furnace, vacuumizing and carrying out artificial aging treatment. The composite material prepared on the surface of the die steel has excellent surface hardness, friction resistance and wear resistance, and good high-temperature performance, prolongs the service life of the die steel, and enlarges the application range.
Description
Technical Field
The invention relates to a method for preparing an in-situ synthesized TiC/NiCrBSi composite coating on the surface of die steel, belonging to the technical field of die material surface engineering.
Background
The die steel may be classified into hot-work die steel, cold-work die steel, and plastic die steel according to the working state. Wherein the cold-work die steel is die steel used for metal deformation in a cold state. Cold forming is generally the drawing, stamping, cold heading or cold extrusion of a sheet or rod using dies such as cold punching, cold extrusion, blanking and drawing. Although the specific service conditions of the die are different for different types of cold deformation, the die has the following common characteristics: the working temperature is not high, the high pressure or impact force is mainly borne, and the metal has violent friction. Therefore, the cold-work die steel is required to have high hardness and wear resistance, and also to have certain toughness. The process requires sufficient hardenability and small quenching deformation. With the rapid development of the processing industry in China, the load of the die is continuously increased, and the requirement is higher and higher, so that the die is required to be manufactured by adopting more durable materials and a novel process. The current research mainly focuses on adjusting and controlling the microstructure of the die steel by changing alloy components and carrying out a proper heat treatment process, so as to achieve the aims of strengthening the strength, hardness, wear resistance and toughness of the die steel and further prolonging the service life of the die steel.
Through the literature search of the prior art, Chinese patent CN110983202A discloses a preparation method of heat fatigue resistant die-casting die steel. Proportioning according to fixed chemical components, placing the raw materials into an electric arc furnace for smelting after removing rust and oil stains on the surfaces, then carrying out vacuum refining, controlling the temperature at 1600 ℃ and the vacuum degree at 10Pa during the refining, and then placing the raw materials into an argon-protected electroslag furnace for electroslag remelting. And after the smelting is finished, performing 3D forging by using a hydraulic press and a precision forging machine, and finally homogenizing the forged material to obtain the die steel. The die steel obtained by the method has uniform components and compact structure, eliminates various macroscopic and microscopic defects, improves the toughness and plasticity of the die steel, and has the impact property reaching the average value of 330J.
Chinese patent CN111041176A discloses a heat treatment process for hot work die steel. The electroslag ingot which is in a red hot state after being remelted by electroslag is put into a heating furnace for high-temperature homogenization treatment, and is heated to 120 ℃ below a solidus line for heat preservation. And adjusting the temperature to below 200 ℃ of the solidus line, preserving the heat for 2-4 h, and discharging from the furnace for direct forging. And then carrying out a series of heat treatment processes of grain refining, ultra-fining, spheroidizing annealing and quenching and tempering to finally obtain the die steel. After the process is adopted, the metallographic structure of the hot work die steel is uniform and fine, and the carbide is in a spherical shape and is finely dispersed and separated out. Under the condition of the same hardness, the unnotched impact energy of the sample of the tool and die body is more than or equal to 350J, and the notched impact energy is more than or equal to 20J; the equal directional performance is more than or equal to 0.85, and the equal directional performance, the toughness, the impact performance, the service life and other important indexes of the tool and the die are obviously improved.
The above-mentioned patents are all that the microstructure of the die steel is regulated and controlled by controlling alloying elements or changing heat treatment process, so as to achieve the effect of improving performance. However, this approach has limited room for improvement in the properties of the die steel and is accompanied by some sacrifice in properties. Particularly, under the condition that a plurality of alloying elements are mixed and added, the conditions of increased cost, increased smelting difficulty and difficult control of components can occur. This results in a limited range of applications for the die steel.
The composite material coating is prepared on the surface of the die steel, and the improvement of the hardness, the friction and wear resistance and the corrosion resistance is mainly reflected in order to greatly improve the performance of the surface of the die steel. Ni-based alloys, especially NiCrBSi alloys, have high fracture toughness, high bond strength and excellent wear resistance. Due to these characteristics, they are widely used in various industries as coating materials produced by thermal spraying and induction cladding. However, the die steel is in a severe working environment, the performance requirement on the surface coating is higher and higher, and the performance of a single alloy coating cannot meet the higher requirement under the working environment with serious abrasion. Therefore, ceramic particles with high hardness are added into alloy powder, and a composite coating with uniform components and compact structure can be obtained by a cladding technology, so that the hardness and the wear resistance of the coating are improved.
At present, the method for preparing the composite material coating on the surface of the matrix by using the high-frequency induction cladding technology tends to be mature, but still has some problems to restrict the application range of the composite material coating. The composite coating added with the ceramic particles has the defects of cracks, air holes and the like because the ceramic particles and the coating are in mosaic combination. In addition, high frequency induction heating is a rapid heating and cooling process, and this particular thermal cycle can cause the structure of the cladding layer to be unstable. The non-uniform distribution of eddy currents results in non-uniform local heat input and residual stresses in the cladding layer. Although the existence of residual stress can increase the dislocation density and improve the strength of the coating to a certain extent, the existence of the residual stress can increase the speed of crack propagation in the coating, and the performance of the coating is extremely unstable during the use process, so that the hardness and the wear resistance of the coating are greatly changed along with the prolonging of service time.
Disclosure of Invention
The invention aims to provide a method for preparing an in-situ synthesized TiC/NiCrBSi composite coating on the surface of die steel, which improves the surface hardness, the frictional wear resistance and the high-temperature performance of the die steel, prolongs the service life and prolongs the application range; meanwhile, the problems of insufficient bonding strength, uneven structure, insufficient stability and the like of a coating prepared by high-frequency induction cladding are solved.
The in-situ synthesized TiC/NiCrBSi composite material coating is prepared on the surface of the die steel by adopting Ti powder, graphite powder and NiCrBSi alloy powder. In the current research at home and abroad, in order to improve the surface hardness, wear resistance and corrosion resistance of materials, the alloy powder subjected to surface cladding mainly comprises Fe-based alloy powder, Ni-based alloy powder and Co-based alloy powder. NiCrBSi alloy powder belongs to Ni-based alloy powder, has hardness and wear resistance second to Co-based alloy powder, and has good self-fluxing property and fluidity and low price, so that the NiCrBSi alloy powder is widely used. Compared with the direct addition of TiC particles, the in-situ synthesized TiC ceramic particle reinforced phase in the alloy is a thermodynamic stable phase which is formed by in-situ nucleation and growth in a matrix, the surface of the reinforced body is free of pollution, the wettability with the matrix is good, the problem of poor compatibility with the matrix is avoided, the interface bonding strength is high, the reinforced particles are fine and uniformly distributed, and the reinforcing effect on the matrix is greatly improved.
The invention provides a method for preparing an in-situ synthesized TiC/NiCrBSi composite coating on the surface of die steel, which comprises the following steps:
the method comprises the following steps: mixing Ti powder (with particle size of 10-25 mu m and purity of 99.9%) and graphite powder (with particle size of 5-50 mu m and purity of 99.99%) in a molar ratio of 1:1, and putting the mixture and NiCrBSi alloy powder into a planetary ball mill for mixing, wherein the mass ratio of the Ti/graphite mixed powder to the NiCrBSi alloy powder is 5-25: 75-95;
stainless steel balls in a stainless steel tank are used for ball milling, the ball-material ratio is 3:1, the rotating speed is 100-120 r/min, and the ball milling time is 3-4 h.
The NiCrBSi alloy powder consists of the following substances in percentage by mass: 15-20% of Cr, 3.0-4.5% of Si, 3.5-5.5% of B, 0.5-1.1% of C, 3.5-5.0% of Fe and the balance of Ni.
Step two: cutting the die steel into a cylindrical shape with the diameter of 15mm multiplied by 10mm, performing surface pretreatment, performing ultrasonic cleaning on the surface by using acetone to remove oil stains on the surface, and then performing sand blasting to remove a surface oxide layer and simultaneously keep the surface roughness at Ra4.5-12.5 mu m, so that the bonding capacity of a matrix and a coating can be properly improved.
Step three: using a sodium silicate colloid as a binder, uniformly stirring the powder mixed by the ball milling machine in the first step and the sodium silicate to prepare a paste, and then coating the paste on the surface of the die steel, wherein the coating thickness is 1 mm-1.5 mm;
the mass ratio of the water glass to the powder is 8-12% and is 8-12: 100.
Step four: and (3) placing the coated substrate in a blast drying oven, keeping the temperature at 100-120 ℃ for 3-4 h, and fully volatilizing the binder.
Step five: the dried sample is placed into a hollow graphite base suitable for the size of the sample, so that two sides of the coated die steel are tightly wrapped by the graphite pipe wall, air is isolated to the maximum extent, and the coating and a matrix are prevented from being seriously oxidized in the induction heating process.
The hollow graphite base is a cylindrical hollow graphite pipe, the bottom end of the hollow graphite base is fixed by the base, die steel with the diameter of phi 15mm can be put down just by the diameter of the hollow graphite base, and a coated sample is put into the die steel for induction cladding so as to avoid oxidation.
Step six: and placing the die steel and the graphite base together under the induction coil for induction cladding. A gradient heating method is adopted, wherein the first stage is a preheating stage, the heating temperature is 500-600 ℃, the current is 20-30A, and the heating time is 60-80 s. The second stage is a melting stage, the heating temperature is 1100-1200 ℃, the current is 280-320A, and the heating time is 20-30 s. And after the powder is melted, cooling in the air, and solidifying to obtain a cladding layer.
Step seven: and (4) putting the die steel subjected to cladding into a vacuum tube furnace, vacuumizing the vacuum tube, and performing solid solution treatment. The temperature of the solution treatment is 920-950 ℃, and the solution treatment is carried out after heat preservation for 1h and then water cooling is carried out.
Step eight: and putting the die steel into the vacuum tube furnace again, vacuumizing and carrying out artificial aging treatment. The aging temperature is 510-540 ℃, the heat preservation time is 4-8 h, and the cooling mode is air cooling. And when the sample is cooled to room temperature, the TiC/NiCrBSi composite coating is obtained on the surface of the die steel.
The in-situ synthesized TiC/NiCrBSi composite material coating is prepared on the surface of the die steel by adopting Ti powder, graphite powder and NiCrBSi alloy powder. In the current research at home and abroad, in order to improve the surface hardness, wear resistance and corrosion resistance of materials, the alloy powder subjected to surface cladding mainly comprises Fe-based alloy powder, Ni-based alloy powder and Co-based alloy powder. NiCrBSi alloy powder belongs to Ni-based alloy powder, has hardness and wear resistance second to Co-based alloy powder, and has good self-fluxing property and fluidity and low price, so that the NiCrBSi alloy powder is widely used. Compared with the direct addition of TiC particles, the in-situ synthesized TiC ceramic particle reinforced phase in the alloy is a thermodynamic stable phase which is formed by in-situ nucleation and growth in a matrix, the surface of the reinforced body is free of pollution, the wettability with the matrix is good, the problem of poor compatibility with the matrix is avoided, the interface bonding strength is high, the reinforced particles are fine and uniformly distributed, and the reinforcing effect on the matrix is greatly improved.
The mixed powder after mechanical ball milling needs to be added with proper binder for preparing a coating, and the reason for selecting the water glass is as follows: the research shows that the water glass has no obvious influence on the structure and the performance of the coating, and when the water glass is used for prefabricating the coating, the coating with good forming and excellent performance can be obtained.
In the invention, a sample is placed in a hollow graphite base and is placed in a coil together, and a gradient induction heating method is adopted. The purpose of using a hollow graphite tube to wrap the sample is to minimize air contact with the coating and substrate, and to reduce the formation of brittle oxides that can lead to impaired coating performance. The method adopts a gradient heating method, the highest temperature is accurately controlled, the temperature of the matrix and the alloy powder is slowly increased from room temperature to 500-600 ℃ in the preheating stage, and the defects of crack generation and the like caused by too fast temperature rise are avoided. The melting stage is a process of melting alloy powder and forming metallurgical bonding with a substrate, the temperature is required to reach 1100-1200 ℃ rapidly, and the alloy powder stays for a proper time to avoid coating entrainment.
The invention carries out the heat treatment process of solid solution and aging on the composite material coating obtained by high-frequency induction cladding, and aims to improve the bonding strength of the coating and obtain the coating with high compactness and low residual stress. On the other hand, as the high-frequency induction cladding is an unbalanced process of rapid heating and cooling, the diffusion of elements in a molten pool on the surface of a substrate is inhibited, and the internal structure of a cladding layer is easy to form supersaturated unbalanced metastable phase solid solution after the cladding is finished. Through heat treatment, the diffusion effect among atoms is intensified, so that a new phase is precipitated from a supersaturated solid solution and is simultaneously converted to a stable state, the tissue in the coating is more uniform and stable, and the comprehensive mechanical property of the cladding layer is obviously improved.
The invention has the beneficial effects that:
(1) the in-situ synthesized TiC reinforced NiCrBSi alloy is adopted, the surface of the obtained reinforcement body is pollution-free, the wettability with the matrix is good, the problem of poor compatibility with the matrix is avoided, the interface bonding strength is high, and TiC reinforced particles are fine and uniformly distributed.
(2) The hollow graphite tube is introduced in the high-frequency induction cladding process, so that partial air can be effectively isolated, and the damage of oxide generated by oxidation of the coating and a die steel substrate to the comprehensive performance of the coating is avoided. The method has low cost and can be repeatedly used, and the economic benefit is greatly improved.
(3) A gradient heating method is adopted in the high-frequency induction cladding process, the temperature is accurately controlled, and the situations of excessive heating and insufficient heating are avoided. The preheating stage avoids the defects of cracks and the like caused by too fast temperature rise, and the powder and the matrix form good metallurgical bonding in the melting stage.
(4) The solid solution treatment is utilized to achieve the effect of solid solution strengthening, the defects of pores, cracks and the like in the coating are obviously reduced, and the structure is uniform and compact; the distribution of alloy elements is more uniform; the strengthening effect of the gamma-Ni solid solution is enhanced, a new phase is precipitated from the coating, and a small amount of oxide exists (the small amount of oxide exists because the induction cladding is carried out in the air, and the graphite base can not completely isolate the air to prevent oxidation).
(5) During the aging treatment, the gamma-Ni solid solution is gradually decomposed, the hardness of the coating is slightly reduced, and the coating still shows higher high-temperature stability.
Detailed Description
The present invention is further illustrated by, but is not limited to, the following examples.
Example 1:
the first step is as follows: mixing Ti powder and graphite powder in a molar ratio of 1:1, and putting the Ti powder and the graphite powder into a planetary ball mill to mix with NiCrBSi alloy powder with the mass percent of 16.68% of Cr, 3.47% of Si, 3.76% of B, 0.58% of C, 3.97% of Fe and the balance of Ni, wherein the ratio (mass fraction) of the Ti/graphite mixed powder to the NiCrBSi alloy powder is 10%. The ball milling parameters are that the ball-material ratio is 3:1, the rotating speed is 100r/min, and the ball milling time is 4 h.
The second step is that: the die steel was cut into a cylindrical shape of phi 15mm × 10mm and subjected to surface pretreatment, the surface was ultrasonically cleaned with acetone to remove oil stains on the surface, and then subjected to sand blasting.
The third step: and (3) using water glass as a binder, uniformly stirring the powder mixed by the ball milling machine in the first step and the water glass to prepare paste, and coating the paste on the surface of the die steel, wherein the coating thickness is 1 mm.
The fourth step: and (3) placing the coated substrate in a forced air drying oven, drying for 4 hours at the temperature of 100 ℃ to fully volatilize the binder.
The fifth step: and putting the dried sample into a hollow graphite base with a size suitable for the sample, so that two sides of the coated die steel are tightly wrapped by the graphite pipe wall, and air is isolated to the greatest extent.
And a sixth step: and placing the die steel and the graphite base together under the induction coil for induction cladding. Gradient heating is adopted, the preheating stage is carried out, the heating temperature is 520 ℃, the current is 20A, and the heating time is 74 s. And in the melting stage, the heating temperature is 1150 ℃, the current is 282A, and the heating time is 28 s. And after the powder is melted, cooling in the air, and solidifying to obtain a cladding layer.
The seventh step: and (4) putting the die steel subjected to cladding into a vacuum tube furnace, vacuumizing the vacuum tube, and performing solid solution treatment. The temperature of the solution treatment is 920 ℃, and the solution treatment is carried out by water cooling after heat preservation for 1 h.
Eighth step: and putting the die steel into the vacuum tube furnace again, vacuumizing and carrying out artificial aging treatment. The aging temperature is 510 ℃, the heat preservation time is 8h, and the cooling mode is air cooling. And cooling the sample to room temperature to prepare the TiC/NiCrBSi composite material on the surface of the die steel.
The results show that: the in-situ synthesized TiC reinforced NiCrBSi alloy composite material coating prepared on the surface of the die steel has uniform and compact structure, no obvious defects of air holes, cracks and the like, and good metallurgical bonding with a matrix. The microstructure of the coating mainly takes gamma-Ni solid solution as a matrix, and Ni3Si and Ni4B3The eutectic structure is distributed on the substrate in a tree shape, and simultaneously, a large amount of nano-scale carbide (Fe, Ni) is dispersed and precipitated on the substrate23C6With TiC, SiB6Equal hard phase particles, carbo-chromide and borochromide precipitated at the grain boundary of gamma-Ni, and Fe-Cr series delta phase particles. The average hardness of the coating reaches 932.3HV0.2The abrasion loss was reduced by 62.3% relative to the substrate.
Example 2:
the first step is as follows: mixing Ti powder and graphite powder in a molar ratio of 1:1, and putting the Ti powder and the graphite powder into a planetary ball mill to mix, wherein the NiCrBSi alloy powder comprises 17.34% of Cr, 3.56% of Si, 3.96% of B, 0.55% of C, 4.13% of Fe and the balance of Ni by mass percentage, and the ratio (mass fraction) of the Ti/graphite mixed powder to the 90% NiCrBSi alloy powder. The ball milling parameters are that the ball-material ratio is 3:1, the rotating speed is 120r/min, and the ball milling time is 3.5 h.
The second step is that: the die steel was cut into a cylindrical shape of phi 15mm × 10mm and subjected to surface pretreatment, the surface was ultrasonically cleaned with acetone to remove oil stains on the surface, and then subjected to sand blasting.
The third step: and (3) using water glass as a binder, uniformly stirring the powder mixed by the ball milling machine in the first step and the water glass to prepare paste, and coating the paste on the surface of the die steel, wherein the coating thickness is 1.2 mm.
The fourth step: and (3) placing the coated substrate in a forced air drying oven, drying for 4 hours at the temperature of 100 ℃ to fully volatilize the binder.
The fifth step: and putting the dried sample into a hollow graphite base with a size suitable for the sample, so that two sides of the coated die steel are tightly wrapped by the graphite pipe wall, and air is isolated to the greatest extent.
And a sixth step: and placing the die steel and the graphite base together under the induction coil for induction cladding. Gradient heating is adopted, the preheating stage is carried out, the heating temperature is 560 ℃, the current is 23A, and the heating time is 68 s. And in the melting stage, the heating temperature is 1200 ℃, the current is 316A, and the heating time is 22 s. And after the powder is melted, cooling in the air, and solidifying to obtain a cladding layer.
The seventh step: and (4) putting the die steel subjected to cladding into a vacuum tube furnace, vacuumizing the vacuum tube, and performing solid solution treatment. The temperature of the solution treatment is 930 ℃, and the solution treatment is carried out by water cooling after heat preservation for 1 h.
Eighth step: and putting the die steel into the vacuum tube furnace again, vacuumizing and carrying out artificial aging treatment. The aging temperature is 520 ℃, the heat preservation time is 6h, and the cooling mode is air cooling. And cooling the sample to room temperature to prepare the TiC/NiCrBSi composite material on the surface of the die steel.
The results show that: the in-situ synthesized TiC reinforced NiCrBSi alloy composite material coating prepared on the surface of the die steel has uniform and compact structure, no obvious defects of air holes, cracks and the like, and good metallurgical bonding with a matrix. The microstructure of the coating mainly takes gamma-Ni solid solution as a matrix, and Ni3Si and Ni4B3The eutectic structure is distributed on the substrate in a tree shape, and simultaneously, a large amount of nano-scale carbide (Fe, Ni) is dispersed and precipitated on the substrate23C6With TiC, SiB6Equal hard phase particles, carbo-chromide and borochromide precipitated at the grain boundary of gamma-Ni, and Fe-Cr series delta phase particles. The average hardness of the coating reaches 916.5HV0.2The abrasion loss was reduced by 62.1% relative to the substrate.
Example 3:
the first step is as follows: mixing Ti powder and graphite powder in a molar ratio of 1:1, and putting the Ti powder and the graphite powder into a planetary ball mill to mix with NiCrBSi alloy powder with the mass percent of 16.74% of Cr, 3.67% of Si, 4.06% of B, 0.50% of C, 3.62% of Fe and the balance of Ni, wherein the ratio (mass fraction) of the Ti/graphite mixed powder to the NiCrBSi alloy powder is 10%. The ball milling parameters are that the ball-material ratio is 3:1, the rotating speed is 110r/min, and the ball milling time is 4 h.
The second step is that: the die steel was cut into a cylindrical shape of phi 15mm × 10mm and subjected to surface pretreatment, the surface was ultrasonically cleaned with acetone to remove oil stains on the surface, and then subjected to sand blasting.
The third step: and (3) using water glass as a binder, uniformly stirring the powder mixed by the ball milling machine in the first step and the water glass to prepare paste, and coating the paste on the surface of the die steel, wherein the coating thickness is 1.1 mm.
The fourth step: and (3) placing the coated substrate in a forced air drying oven, drying for 4 hours at the temperature of 100 ℃ to fully volatilize the binder.
The fifth step: and putting the dried sample into a hollow graphite base with a size suitable for the sample, so that two sides of the coated die steel are tightly wrapped by the graphite pipe wall, and air is isolated to the greatest extent.
And a sixth step: and placing the die steel and the graphite base together under the induction coil for induction cladding. Gradient heating is adopted, the preheating stage is carried out, the heating temperature is 580 ℃, the current is 26A, and the heating time is 66 s. And in the melting stage, the heating temperature is 1180 ℃, the current is 312A, and the heating time is 25 s. And after the powder is melted, cooling in the air, and solidifying to obtain a cladding layer.
The seventh step: and (4) putting the die steel subjected to cladding into a vacuum tube furnace, vacuumizing the vacuum tube, and performing solid solution treatment. The temperature of the solution treatment is 950 ℃, and the solution treatment is carried out by water cooling after heat preservation for 1 hour.
Eighth step: and putting the die steel into the vacuum tube furnace again, vacuumizing and carrying out artificial aging treatment. The aging temperature is 540 ℃, the heat preservation time is 4h, and the cooling mode is air cooling. And cooling the sample to room temperature to prepare the TiC/NiCrBSi composite material on the surface of the die steel.
The results show that: the in-situ synthesized TiC reinforced NiCrBSi alloy composite material coating prepared on the surface of the die steel has uniform and compact structure, no obvious defects of air holes, cracks and the like, and good metallurgical bonding with a matrix. The microstructure of the coating mainly takes gamma-Ni solid solution as a matrix, and Ni3Si and Ni4B3The eutectic structure is distributed on the substrate in a tree shape, and simultaneously, a large amount of nano-scale carbide (Fe, Ni) is dispersed and precipitated on the substrate23C6With TiC, SiB6Equal hard phase particles, carbo-chromide and borochromide precipitated at the grain boundary of gamma-Ni, and Fe-Cr series delta phase particles. The average hardness of the coating reaches 928.2HV0.2The abrasion loss was reduced by 61.5% relative to the substrate.
Claims (9)
1. A method for preparing an in-situ synthesized TiC/NiCrBSi composite coating on the surface of die steel is characterized by comprising the following steps:
the method comprises the following steps: mixing Ti powder and graphite powder in a molar ratio of 1:1, and putting the Ti powder and NiCrBSi alloy powder into a planetary ball mill for mixing, wherein the mass ratio of the Ti/graphite mixed powder to the NiCrBSi alloy powder is 5-25: 75-95;
the NiCrBSi alloy powder consists of the following substances in percentage by mass: 15-20% of Cr, 3.0-4.5% of Si, 3.5-5.5% of B, 0.5-1.1% of C, 3.5-5.0% of Fe and the balance of Ni;
step two: cutting the die steel into cylinders with the diameter of 15mm multiplied by 10mm, performing surface pretreatment, performing ultrasonic cleaning on the surface by using acetone to remove oil stains on the surface, and then performing sand blasting treatment to remove a surface oxide layer and keep the surface rough so as to improve the bonding capacity of a matrix and a coating;
step three: using a water glass colloid as a binder, uniformly stirring the mixed powder subjected to ball milling in the first step and water glass to prepare a paste, and then coating the paste on the surface of the die steel, wherein the coating thickness is 1 mm-1.5 mm;
step four: placing the substrate coated in the third step in a blast drying oven, keeping the temperature at 100-120 ℃ for 3-4 h, and fully volatilizing the binder;
step five: putting the dried sample into a hollow graphite base with corresponding size, so that two sides of the coated die steel are tightly wrapped by the graphite pipe wall to isolate air, and the coating and the matrix are prevented from being seriously oxidized in the induction heating process;
step six: placing the die steel and the graphite base together under an induction coil for induction cladding; a gradient heating method is adopted, the first stage is a preheating stage, the second stage is a melting stage, after the powder is melted, the powder is cooled in the air, and a cladding layer is obtained after solidification;
step seven: putting the die steel subjected to cladding into a vacuum tube furnace, vacuumizing a vacuum tube, and performing solid solution treatment;
step eight: putting the die steel into a vacuum tube furnace again, vacuumizing and carrying out artificial aging treatment; and when the sample is cooled to room temperature, the TiC/NiCrBSi composite coating is obtained on the surface of the die steel.
2. The method of claim 1 for the preparation of in situ authigenic TiC/NiCrBSi composite coatings on the surface of die steel, characterized in that: the particle size of the Ti powder is 10-25 mu m, and the purity is 99.9%; the particle size of the graphite powder is 5-50 mu m, and the purity is 99.99%.
3. The method of claim 1 for the preparation of in situ authigenic TiC/NiCrBSi composite coatings on the surface of die steel, characterized in that: stainless steel balls in a stainless steel tank are used for ball milling, the ball-material ratio is 3:1, the rotating speed is 100-120 r/min, and the ball milling time is 3-4 h.
4. The method of claim 1 for the preparation of in situ authigenic TiC/NiCrBSi composite coatings on the surface of die steel, characterized in that: and in the second step, the roughness of the surface of the die steel is kept at Ra4.5-12.5 mu m.
5. The method of claim 1 for the preparation of in situ authigenic TiC/NiCrBSi composite coatings on the surface of die steel, characterized in that: in the third step, the mass ratio of the water glass to the powder is 8-12: 100.
6. The method of claim 1 for the preparation of in situ authigenic TiC/NiCrBSi composite coatings on the surface of die steel, characterized in that: and fifthly, the hollow graphite base is a cylindrical hollow graphite pipe, the bottom end of the hollow graphite pipe is fixed by the base, die steel with the diameter of phi 15mm can be put down just, and the coated sample is put into the hollow graphite pipe for induction cladding so as to avoid oxidation.
7. The method of claim 1 for the preparation of in situ authigenic TiC/NiCrBSi composite coatings on the surface of die steel, characterized in that: in the induction cladding process, the heating temperature in the preheating stage is 500-600 ℃, the current is 20-30A, and the heating time is 60-80 s; the heating temperature in the melting stage is 1100-1200 ℃, the current is 280-320A, and the heating time is 20-30 s.
8. The method of claim 1 for the preparation of in situ authigenic TiC/NiCrBSi composite coatings on the surface of die steel, characterized in that: the temperature of the solution treatment is 920-950 ℃, and the solution treatment is carried out after heat preservation for 1h and then water cooling is carried out.
9. The method of claim 1 for the preparation of in situ authigenic TiC/NiCrBSi composite coatings on the surface of die steel, characterized in that: the temperature of the aging treatment is 510-540 ℃, the heat preservation time is 4-8 h, and the cooling mode is air cooling.
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