CN115233137B - Low-friction supersonic flame spraying wear-resistant coating material, preparation method and application - Google Patents
Low-friction supersonic flame spraying wear-resistant coating material, preparation method and application Download PDFInfo
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- CN115233137B CN115233137B CN202210927401.6A CN202210927401A CN115233137B CN 115233137 B CN115233137 B CN 115233137B CN 202210927401 A CN202210927401 A CN 202210927401A CN 115233137 B CN115233137 B CN 115233137B
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- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/06—Metallic material
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/026—Spray drying of solutions or suspensions
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- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
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- C22C29/067—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds comprising a particular metallic binder
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- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/08—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds based on tungsten carbide
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1635—Composition of the substrate
- C23C18/1639—Substrates other than metallic, e.g. inorganic or organic or non-conductive
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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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
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- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/129—Flame spraying
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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Abstract
The invention discloses a low-friction supersonic flame spraying wear-resistant coating material, a preparation method and application thereof, wherein the coating comprises the following raw materials in percentage by mass: co powder 5-20wt%, mo 2 0.5-8wt% of C powder, 0.3-1.0wt% of VC powder and Cr 3 C 2 0.1-5wt% of powder, 1-5wt% of solid lubricating phase and the balance of WC powder; the solid lubricating phase is Ni-coated graphite particles and/or Ni-coated MoS 2 And (3) particles. The invention introduces graphite and MoS into WC-Co based coating 2 Solid lubricating phase such as particles, etc. is formed by graphite and MoS 2 The chemical plating Ni treatment on the particle surface obviously reduces the friction coefficient of the coating under the condition of not reducing the hardness, the binding force, the compactness and the like of the coating, thereby improving the wear resistance of the coating.
Description
Technical Field
The invention belongs to the technical field of supersonic flame spraying materials, and particularly relates to a low-friction supersonic flame spraying wear-resistant coating material and a preparation method thereof.
Background
The supersonic flame spraying is a novel thermal spraying technology developed on the basis of common flame spraying. The spray powder is fed into high-temperature high-speed flame which is burnt by mixing oxygen (air) with kerosene, propane, acetylene and other fuels in proportion, heated to a molten or semi-molten state and sprayed onto the surface of a substrate at high speed through a compression-expansion nozzle, so that a coating with high bonding strength, high hardness, wear resistance, corrosion resistance and compactness and high quality is obtained. The supersonic flame spraying has the advantages of high particle flight speed, high deposition speed, high bonding strength, high density and the like, and the high cooling speed can effectively limit element segregation, inhibit nucleation and growth of intermetallic compounds and is beneficial to forming solid solution. Therefore, the supersonic flame spraying is very suitable for preparing the alloy or alloy carbide series metal ceramic wear-resistant coating, and has been rapidly developed and widely applied in recent years.
The first prior art discloses a WC-Co coating with a high-compactness quasi-nanostructure and a preparation method thereof, and relates to nano WC-Co composite powder and Cr 3 C 2 Mixing with VC powder, ball milling, mixing, granulating, heat treating, sieving, and spray-coating with supersonic speed flame. The second prior art discloses a WC-Co cermet coating with multi-scale WC grains and a preparation method, and the supersonic flame spraying wear-resistant WC-Co coating with high hardness and high toughness is obtained through partial nanocrystallization of the WC grains. The third prior art discloses a wear-resistant screw with a nano ceramic coating, and relates to a supersonic flame-sprayed WC-Co ceramic coating with a nano structure, wherein the prepared coating has high hardness, high bonding strength and high compactness. The fourth prior art discloses a preparation method of a WC-Co coating with low porosity, which inhibits decarburization of WC in the spray process of supersonic spraying by adding Al element, thereby reducing the porosity of the coating, increasing the hardness and fracture toughness and increasing the wear resistance of the coating. It can be seen that the current relevant supersonic flame-sprayed material patent is mainly made up by partial nanocrystallization and composition of WC grainsOr optimizing the process, and the like, to improve the hardness, toughness, compactness, and the like of the supersonic flame-sprayed WC-Co coating, thereby improving the wear resistance of the coating material, but the problem of improving the lubrication condition of a friction interface of the coating under the friction and wear condition is not related.
Meanwhile, the existing supersonic flame spraying WC-Co-based hard coating is mainly prepared by mixing WC, co and other component powders in proportion, preparing the mixed powder into suspension slurry, atomizing to prepare powder, sintering, and then performing supersonic flame spraying. The traditional WC-Co-based hard coating is required to have high hardness and high compactness, and the wear resistance of the coating is improved by increasing the hardness of the coating, so that a lubricating phase for improving friction conditions is not added in the design process of a matrix component. Although the coating has higher hardness through the coating composition and process optimization, the friction coefficient of the coating is higher due to the existence of a large amount of hard ceramic phase in the coating. Therefore, serious abrasion and strain are caused on the surface of the friction pair in the dry friction process of the coating, and particularly in heavy-load friction and high-temperature oxidation environments, the damage to the friction pair is obviously aggravated due to insufficient lubrication conditions of a friction interface.
Disclosure of Invention
The invention aims to provide a low-friction supersonic flame spraying wear-resistant coating material and a preparation method thereof, wherein graphite and MoS coated by chemical plating Ni are introduced into a WC-Co-based hard coating sprayed by a traditional supersonic flame 2 The particles are used as a solid friction lubrication phase, and under the conditions of ensuring high hardness, high compactness and high binding force of the supersonic flame coating, the lubrication condition of the friction pair of the spray coating WC-Co coating is obviously improved, so that the friction coefficient of the coating is obviously reduced, and the abrasion resistance of the coating is improved.
In order to achieve the purpose, the invention provides a low-friction supersonic flame spraying wear-resistant coating material, which comprises the following raw materials in percentage by mass: co powder 5-20wt%, mo 2 0.5-8wt% of C powder, 0.3-1.0wt% of VC powder and Cr 3 C 2 0.1-5wt% of powder, 1-5wt% of solid lubricating phase and the balance of WC powder; the solid lubricating phase is Ni-coated graphite particles and/or Ni-coated MoS 2 And (3) particles.
The friction coefficient of the low-friction supersonic flame spraying wear-resistant coating material prepared by the invention is lower than 0.48, and the wear rate is lower than 6.5x10 -8 mm 3 /m。
Further, co powder, mo 2 C powder, VC powder, cr 3 C 2 The particle size of the powder and WC powder is 1-2.5 μm.
The invention also provides a preparation method of the low-friction supersonic flame spraying wear-resistant coating material, which comprises the following steps:
(1) Preparation of solid lubricating phase by chemical nickel plating
By granulating graphite or MoS 2 The particles are sequentially deoiled, coarsened, activated and chemically plated with nickel to prepare a solid lubricating phase, and the medium of the chemically plated nickel is 20-40g/L NiSO 4 ·6H 2 O, naH 15-30g/L 2 PO 2 ·H 2 O, na of 20-30g/L 3 C 5 H 5 O 7 ·2H 2 O, CH of 10-20g/L 3 COONa·3H 2 O, 20-25mL/L lactic acid, 15-20mL/L acetic acid and 0.05-0.08g/L thiourea, wherein the pH value of the medium is 4.5-6.0, the temperature of the electroless nickel plating is controlled to be 50-75 ℃, and the time is 60-120min;
(2) Mixing and granulating
Ball milling the raw materials to prepare mixed powder;
heating and stirring polyvinyl alcohol and deionized water to prepare concentrated glue, diluting the concentrated glue to prepare a polyvinyl alcohol solution, mixing the polyvinyl alcohol solution with mixed powder, and ball-milling to prepare suspension;
spraying and granulating the suspension to obtain spherical powder;
(3) Powder heat treatment
Drying the spherical powder, heating up and sintering in a gradient way, and cooling to obtain mixed powder;
(4) Spraying
And spraying the mixed powder on the surface of the pretreated substrate by adopting a supersonic flame spraying technology, so as to obtain the low-friction supersonic flame spraying wear-resistant coating material.
Further, the preparation of the concentrated glue comprises the following steps: mixing polyvinyl alcohol powder with deionized water according to a mass ratio of 1:4-8, heating to 65-85 ℃ in a water bath, and stirring for 12-24 hours to obtain the concentrated glue.
Further, the preparation of the suspension comprises the following steps: adding deionized water into the concentrated glue, so that the mass ratio of polyvinyl alcohol to deionized water is 1:1.35-1.55, mixing and ball milling with mixed powder according to the mass ratio of 3-5:1, controlling the ball-material ratio to be 5-10:1, and the ball milling time to be 12-24h and the rotating speed to be 120-180r/min, thus obtaining suspension.
Further, the parameters of spray granulation are: the inlet temperature is 200-380 ℃, the outlet temperature is 100-200 ℃, the feeding speed is 30-50r/min, the rotating speed of the atomizing disk is 12000-18000r/min, the drying atmosphere is nitrogen, and the pressure is 0.5-1.5Mpa.
Further, the matrix preheating temperature of the supersonic flame spraying technology is 80-120 ℃, the compressed air pressure of the combustion improver is 0.5-0.85MPa, the flow rate is 750-1200SL/min, the fuel is propane or kerosene, the fuel pressure is 0.55-0.85MPa, the fuel flow rate is 10-20 SL/h, the combustion pressure of the combustion chamber is 0.6-1.0 MPa, the powder feeding rate is 60-100g/min, the moving speed of the spray gun is 400-900mm/min, the spraying distance is 200-500mm, the cooling medium is compressed air, and the flow rate is 2-5SL/min.
The invention also provides application of the low-friction supersonic flame spraying wear-resistant coating material, which comprises application in an atmosphere environment below 650 ℃ or application in a vacuum environment below 450 ℃.
Preferably, the solid lubricating phase is Ni coated graphite particles, and the low-friction supersonic flame-sprayed wear-resistant coating material is used in the atmosphere environment below 650 ℃.
Preferably, the solid lubricating phase is Ni-coated MoS 2 The particle, low friction supersonic flame spray wear-resistant coating material is used in vacuum environment below 450 ℃.
In summary, the invention has the following advantages:
1. the invention provides a low-friction supersonic flame spraying wear-resistant coating material, graphite and MoS are introduced into WC-Co based coating 2 Solid lubricating phase such as particles, etc. is formed by graphite and MoS 2 The chemical plating Ni treatment on the particle surface obviously reduces the friction coefficient of the coating under the condition of not reducing the hardness, the binding force, the compactness and the like of the coating, thereby improving the wear resistance of the coating.
2. The invention uses chemical plating method to deposit graphite and MoS 2 Plating Ni on the surface of the particles to prepare graphite and MoS with uniform Ni coating 2 Is composed of Ni-coated shell layer, graphite core and MoS 2 The core bonding force is good and the thickness is uniform. In graphite and Mo 2 Compared with Physical Vapor Deposition (PVD), chemical Vapor Deposition (CVD), electroplating and other processes, the process for coating the metal Ni on the surfaces of the solid lubricating particles such as S and the like by using the chemical plating method has the advantages of uniform and controllable thickness, good bonding effect, simple process, easy operation, no need of complex and expensive equipment (such as a vacuum coating machine, various power supply equipment and the like) and good particle dispersibility after coating.
Drawings
FIG. 1 is a schematic illustration of the preparation process of the present invention.
Detailed Description
In the prior art, the high-temperature lubricating phase Ni adopted is coated with BN (boron nitride), and harmful Ni can be formed in the chemical plating layer 3 P and Ni 3 And B, substances which are harmful to the lubricating property and the wear resistance of the coating material. WS on the other hand 2 Is used as a medium-low temperature solid lubricating phase, but in the process of preparing composite powder by spheroidization and supersonic flame spraying, W is introduced to change the balance of a W-Co-C ternary system in the material, so that the material is subjected to C removal to form brittle eta phase (W 3 Co 3 C, etc.), reducing the wear resistance of the coating material. Based on the reasons, the invention adopts Ni-coated graphite and Ni-coated MoS 2 As a solid lubricating phase.
The supersonic spraying coating material containing Ni coated graphite core-shell structure is mainly used in the atmospheric environment, can be applied to the temperature below 650 ℃ and contains Ni coated MoS 2 The supersonic spraying coating material with the core-shell structure is mainly suitable for vacuum environment and has good lubrication effect below 450 ℃.
Due to the existence of Ni coating layerThe relative graphite and MoS of the metal Co in the powder sintering and spraying process are obviously improved 2 The wettability of the particles is not due to graphite and MoS 2 The introduction of particles reduces the compactness of the coating. Coating graphite with Ni and MoS 2 Core/shell particles of (C), and WC, co, VC and Cr 3 C 2 The powder is evenly mixed, and spherical powder with even components, high sphericity and even grain size distribution is prepared by an atomization pulverizing process. Due to VC and Cr in the mixed powder 3 C 2 The addition of the powder can effectively inhibit the growth of WC crystal grains in the heat treatment and spraying processes of the spherical powder, compensate the reduction of the hardness of the coating caused by the addition of the lubricating oil, thereby improving the hardness and the strength of the coating, and Cr 3 C 2 The addition of (c) can improve the corrosion resistance of the coating. Mo in coating 2 The addition of the powder C can improve the toughness of the coating, improve the binding force and the lubrication condition of the coating in a high-temperature oxidation friction environment, thereby improving the wear resistance of the coating.
The principles and features of the present invention are described below in connection with the following examples, which are set forth to illustrate, but are not to be construed as limiting the scope of the invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
The embodiment provides a preparation method of a low-friction supersonic flame-spraying wear-resistant coating material (Ni-coated graphite), which comprises the following steps:
(1) Electroless plating
Deoiling, sequentially carrying out ultrasonic treatment on graphite particles with the average particle size of 1.0 mu m in 8wt% NaOH solution for 30min, carrying out ultrasonic treatment in acetone for 10min, and then washing with deionized water to be neutral;
coarsening, namely performing ultrasonic treatment on graphite in 8wt% of dilute nitric acid solution for 20min, boiling in 15wt% of silver nitrate solution for 20min, and then washing with deionized water to be neutral;
activating graphite with 0.2g/L PdCl 2 And 10mL/L HCStirring the solution (water is used as a solvent, water is used as a solvent in the following examples) for 5min, and then washing the solution with deionized water to be neutral;
electroless nickel plating, which is to chemically plate activated graphite with 30g/L NiSO of electroless plating medium (water as solvent, same in the following examples) 4 ·6H 2 O，30g/L NaH 2 PO 2 ·H 2 O，20g/LNa 3 C 5 H 5 O 7 ·2H 2 O，20g/L CH 3 COONa·3H 2 O,20mL/L lactic acid, 20mL/L acetic acid, 0.08g/L thiourea, the pH value of the solution is 4.5-5.0, the temperature is controlled to be 75 ℃, ultrasonic stirring is carried out, and the plating time is 90min;
and (3) after plating, washing graphite with absolute ethyl alcohol, placing the graphite in a vacuum drying oven, heating to 80 ℃ under vacuum condition, and preserving heat for 2 hours, wherein the vacuum degree is 0.5Pa.
(2) Ball milling mixing material
3wt% of prepared Ni-coated graphite particles, 10wt% of Co powder (2.0 mu m), and Mo 2 5wt% of C powder (2.0 μm), 0.6wt% of VC powder (2.0 μm), cr 3 C 2 Powder (2.0 μm) 2wt%, WC powder (2.0 μm) as the balance, and powder raw materials were mixed. Ball milling and mixing are carried out on the mixture by adopting a planetary ball mill, the ball-material ratio is 8:1, the rotating speed is 200r/min, and the ball milling time is 6h.
(3) Spray granulation
Mixing polyvinyl alcohol (PVA) powder with deionized water according to a mass ratio of 1:8, heating to 85 ℃ by adopting water bath, and stirring for 12 hours to prepare concentrated glue;
adding deionized water into the prepared concentrated glue to further dilute PVA, wherein the mass ratio of PVA to deionized water is 1:50, and the PVA is ensured to be completely dissolved in water;
mixing the mixed powder and PVA solution according to a mass ratio of 1:5, adding the mixed powder and PVA solution into a planetary ball milling tank, controlling the ball-material ratio to be 5:1, and after ball milling for 24 hours, uniformly mixing the slurry at a rotating speed of 120r/min to reach a stable state, and preparing a stable material suspension;
spray granulation is carried out by adopting a spray dryer, the inlet speed is controlled to be 350 ℃, the outlet temperature is controlled to be 150 ℃, the feeding speed is controlled to be 30r/min, the rotating speed of an atomizing disc is 15000r/min, the drying atmosphere is nitrogen, and the pressure is 1.5MPa, so that spherical powder is obtained.
(4) Powder heat treatment
Drying the mixed powder in a vacuum drying oven for 12 hours at the temperature of 100 ℃ and the vacuum degree of 0.5Pa, and discharging excessive water;
loosely sintering the powder dried by the vacuum drying oven in a vacuum sintering furnace, heating to 150 ℃ at 5 ℃/min, and preserving heat for 1h, wherein the vacuum degree is 0.5Pa so as to remove adsorbed gas and moisture;
further heating to 550 ℃ at a speed of 5 ℃/min, and preserving heat for 3 hours, wherein the vacuum degree is 0.1Pa so as to ensure that the forming agent PVA is completely removed;
heating to a set sintering temperature of 1320 ℃ at 5 ℃/min, preserving heat and sintering for 1.5 hours, and cooling along with a furnace, wherein the vacuum degree is 0.01Pa;
then vibration screening is carried out by utilizing a screen mesh to obtain mixed powder with the particle size of 20-55 mu m.
(5) Spraying
Firstly, carrying out oil removal and cleaning treatment on the surface of a spraying substrate, carrying out ultrasonic treatment on the substrate material in 8wt% NaOH solution for 30min, carrying out ultrasonic cleaning in acetone for 10min, and drying;
carrying out sand blasting treatment on the surface of a spraying substrate, wherein white corundum sand with the particle size of 24-48 meshes, the sand blasting pressure of 0.6MPa and the sand blasting distance of 100mm are adopted, and the surface roughness after treatment is Ra5-10 mu m;
then, a supersonic flame spraying technology is adopted to prepare a coating, a spray gun is kept vertical to a sample during spraying, the preheating temperature of a matrix is 80 ℃, combustion improver compresses air, the pressure is 0.75MPa, the flow rate is 950SL/min, fuel is propane, the pressure is 0.7MPa, the fuel flow rate is 12SL/h, the combustion pressure of a combustion chamber is 0.8MPa, the powder feeding rate is 80g/min, the moving speed of the spray gun is 750mm/min, and the spraying distance is 320mm. The cooling medium was compressed air with a flow rate of 4SL/min.
The hardness of the coating prepared by the invention is 1200Hv, the void ratio is 0.6%, the bonding strength is 90MPa, and the friction coefficient is 0.45.
Example 2
The embodiment provides a low-friction supersonic flame spraying wear-resistant coatingLayer material (Ni coated MoS) 2 ) The preparation method of (2) comprises the following steps:
(1) Electroless plating
Deoiling, and subjecting MoS with average particle size of 2 μm to 2 Respectively carrying out ultrasonic treatment on the particles in an 8wt.% NaOH solution for 30min, carrying out ultrasonic treatment in acetone for 10min, and then washing with deionized water to be neutral;
coarsening MoS 2 After the particles are treated by ultrasonic in 8wt% of dilute nitric acid solution for 20min, the particles are boiled in 15wt% of silver nitrate solution for 20min and then washed to be neutral by deionized water;
activating, moS 2 The granules contain 0.2g/L PdCl 2 Stirring in 10mL/L HCl solution for 5min, and then washing with deionized water to neutrality;
electroless nickel plating, activating the MoS 2 The particles are subjected to chemical plating, and the chemical plating medium is 30g/LNiSO 4 ·6H 2 O，30g/L NaH 2 PO 2 ·H 2 O，20g/L Na 3 C 5 H 5 O 7 ·2H 2 O，20g/LCH 3 COONa·3H 2 O,20mL/L lactic acid, 20mL/L acetic acid, 0.08g/L thiourea, the pH value of the solution is 4.5-5.0, the temperature is controlled to be 75 ℃, ultrasonic stirring is carried out, and the plating time is 90min;
washing MoS with absolute ethanol after plating 2 The granules are placed in a vacuum drying oven, heated to 80 ℃ under vacuum condition, and kept for 2 hours, wherein the vacuum degree is 0.5Pa.
(2) Ball milling mixing material
Ni-coated MoS prepared 2 3wt% of particles, 10wt% of Co powder (2.0 mu m), and Mo 2 5wt% of C powder (2.0 μm), 0.5wt% of VC powder (2.0 μm), cr 3 C 2 Powder (2.0 μm) 1.5wt% of WC powder (2.0 μm) as the balance, and powder raw materials were mixed. Ball milling and mixing are carried out on the mixture by adopting a planetary ball mill, the ball-material ratio is 8:1, the rotating speed is 200r/min, and the ball milling time is 6h.
(3) Spray granulation
Mixing polyvinyl alcohol (PVA) powder with deionized water according to a mass ratio of 1:8, heating to 85 ℃ by adopting water bath, and stirring for 12 hours to prepare concentrated glue;
adding deionized water into the prepared concentrated glue to further dilute PVA, wherein the mass ratio of PVA to deionized water is 1:50, and the PVA is ensured to be completely dissolved in water;
mixing the mixed powder and PVA solution according to a mass ratio of 1:5, adding the mixed powder and PVA solution into a planetary ball milling tank, controlling the ball-material ratio to be 5:1, and after ball milling for 24 hours, uniformly mixing the slurry at a rotating speed of 120r/min to reach a stable state, and preparing a stable material suspension;
spray granulation is carried out by adopting a spray dryer, the inlet speed is controlled to be 350 ℃, the outlet temperature is controlled to be 150 ℃, the feeding speed is controlled to be 30r/min, the rotating speed of an atomizing disc is 15000r/min, the drying atmosphere is nitrogen, and the pressure is 1.5MPa, so that spherical powder is obtained.
(4) Powder heat treatment
Drying the mixed powder in a vacuum drying oven for 12 hours at the temperature of 100 ℃ and the vacuum degree of 0.5Pa, and discharging excessive water;
loosely sintering the powder dried by the vacuum drying oven in a vacuum sintering furnace, heating to 150 ℃ at 5 ℃/min, and preserving heat for 1h, wherein the vacuum degree is 0.5Pa so as to remove adsorbed gas and moisture;
further heating to 550 ℃ at a speed of 5 ℃/min, and preserving heat for 3 hours, wherein the vacuum degree is 0.1Pa so as to ensure that the forming agent PVA is completely removed;
heating to a set sintering temperature of 1320 ℃ at 5 ℃/min, preserving heat and sintering for 1.5 hours, and cooling along with a furnace, wherein the vacuum degree is 0.01Pa;
then vibration screening is carried out by utilizing a screen mesh to obtain mixed powder with the particle size of 20-55 mu m.
(5) Spraying
Firstly, carrying out oil removal and cleaning treatment on the surface of a spraying substrate, carrying out ultrasonic treatment on the substrate material in 8wt% NaOH solution for 30min, carrying out ultrasonic cleaning in acetone for 10min, and drying;
carrying out sand blasting treatment on the surface of a spraying substrate, wherein white corundum sand with the particle size of 24-48 meshes, the sand blasting pressure of 0.6MPa and the sand blasting distance of 100mm are adopted, and the surface roughness after treatment is Ra5-10 mu m;
then, a supersonic flame spraying technology is adopted to prepare a coating, a spray gun is kept vertical to a sample during spraying, the preheating temperature of a matrix is 80 ℃, combustion improver compresses air, the pressure is 0.7MPa, the flow rate is 900SL/min, fuel is propane, the pressure is 0.65MPa, the fuel flow rate is 11SL/h, the combustion pressure of a combustion chamber is 0.8MPa, the powder feeding rate is 90g/min, the moving speed of the spray gun is 800mm/min, and the spraying distance is 380mm. The cooling medium was compressed air with a flow rate of 4SL/min.
The hardness of the coating prepared by the invention is 1250Hv, the void ratio is lower than 0.54%, the bonding strength is 92MPa, and the friction coefficient is lower than 0.48.
Example 3
The embodiment provides a low-friction supersonic flame-sprayed wear-resistant coating material (Ni-coated MoS) 2 Ni coated graphite) comprising the steps of:
(1) Electroless plating
Deoiling, mixing graphite with average particle size of 1.0 μm and MoS with average particle size of 2 μm 2 Respectively carrying out ultrasonic treatment on the particles in 8wt.% NaOH solution for 30min, carrying out ultrasonic treatment in acetone for 10min, and then washing the particles with deionized water to be neutral;
coarsening graphite and MoS 2 After the particles are subjected to ultrasonic treatment in an 8wt% dilute nitric acid solution for 20min, the particles are boiled in a 15wt% silver nitrate solution for 20min and then washed to be neutral by deionized water;
activation of graphite and MoS 2 The granules contain 0.2g/L PdCl 2 Stirring in 10mL/L HCl solution for 5min, and then washing with deionized water to neutrality;
chemical nickel plating, and activating the graphite and MoS 2 The particles are subjected to chemical plating, and the chemical plating medium is 30g/LNiSO 4 ·6H 2 O，30g/L NaH 2 PO 2 ·H 2 O，20g/L Na 3 C 5 H 5 O 7 ·2H 2 O，20g/LCH 3 COONa·3H 2 O,20mL/L lactic acid, 20mL/L acetic acid, 0.08g/L thiourea, the pH value of the solution is 4.5-5.0, the temperature is controlled to be 75 ℃, ultrasonic stirring is carried out, and the plating time is 90min;
washing graphite and MoS with absolute ethanol after plating 2 The granules are placed in a vacuum drying oven, heated to 80 ℃ under vacuum condition, and kept for 2 hours, wherein the vacuum degree is that0.5Pa。
(2) Ball milling mixing material
2.5wt% of Ni-coated graphite particles prepared and Ni-coated MoS 2 2.5wt% of particles, 10wt% of Co powder (2.0 μm), mo 2 5wt% of C powder (2.0 μm), 0.8wt% of VC powder (2.0 μm), cr 3 C 2 Powder (2.0 μm) 2.5wt%, WC powder (2.0 μm) as the balance, and powder raw materials were mixed. Ball milling and mixing are carried out on the mixture by adopting a planetary ball mill, the ball-material ratio is 8:1, the rotating speed is 200r/min, and the ball milling time is 6h.
(3) Spray granulation
Mixing polyvinyl alcohol (PVA) powder with deionized water according to a mass ratio of 1:8, heating to 85 ℃ by adopting water bath, and stirring for 12 hours to prepare concentrated glue;
adding deionized water into the prepared concentrated glue to further dilute PVA, wherein the mass ratio of PVA to deionized water is 1:50, and the PVA is ensured to be completely dissolved in water;
mixing the mixed powder and PVA solution according to a mass ratio of 1:5, adding the mixed powder and PVA solution into a planetary ball milling tank, controlling the ball-material ratio to be 5:1, and after ball milling for 24 hours, uniformly mixing the slurry at a rotating speed of 120r/min to reach a stable state, and preparing a stable material suspension;
spray granulation is carried out by adopting a spray dryer, the inlet speed is controlled to be 350 ℃, the outlet temperature is controlled to be 150 ℃, the feeding speed is controlled to be 30r/min, the rotating speed of an atomizing disc is 15000r/min, the drying atmosphere is nitrogen, and the pressure is 1.5MPa, so that spherical powder is obtained.
(4) Powder heat treatment
Drying the mixed powder in a vacuum drying oven for 12 hours at the temperature of 100 ℃ and the vacuum degree of 0.5Pa, and discharging excessive water;
loosely sintering the powder dried by the vacuum drying oven in a vacuum sintering furnace, heating to 150 ℃ at 5 ℃/min, and preserving heat for 1h, wherein the vacuum degree is 0.5Pa so as to remove adsorbed gas and moisture;
further heating to 550 ℃ at a speed of 5 ℃/min, and preserving heat for 3 hours, wherein the vacuum degree is 0.1Pa so as to ensure that the forming agent PVA is completely removed;
heating to a set sintering temperature of 1320 ℃ at 5 ℃/min, preserving heat and sintering for 1.5 hours, and cooling along with a furnace, wherein the vacuum degree is 0.01Pa;
then vibration screening is carried out by utilizing a screen mesh to obtain mixed powder with the particle size of 20-55 mu m.
(5) Spraying
Firstly, carrying out oil removal and cleaning treatment on the surface of a spraying substrate, carrying out ultrasonic treatment on the substrate material in 8wt% NaOH solution for 30min, carrying out ultrasonic cleaning in acetone for 10min, and drying;
carrying out sand blasting treatment on the surface of a spraying substrate, wherein white corundum sand with the particle size of 24-48 meshes, the sand blasting pressure of 0.6MPa and the sand blasting distance of 100mm are adopted, and the surface roughness after treatment is Ra5-10 mu m;
then, a supersonic flame spraying technology is adopted to prepare a coating, a spray gun is kept vertical to a sample during spraying, the preheating temperature of a matrix is 80 ℃, combustion improver compresses air, the pressure is 0.8MPa, the flow rate is 1000SL/min, fuel is propane, the pressure is 0.75MPa, the fuel flow rate is 12SL/h, the combustion pressure of a combustion chamber is 0.8MPa, the powder feeding rate is 80g/min, the moving speed of the spray gun is 800mm/min, and the spraying distance is 300mm. The cooling medium was compressed air with a flow rate of 4SL/min.
The hardness of the coating prepared by the invention is 1150Hv, the void ratio is 0.65%, the bonding strength is 85MPa, and the friction coefficient is lower than 0.42.
Test examples
1. Hardness: the microhardness of the surface of the thermal barrier coating was tested using an HV-1000 Vickers hardness tester. The hardness tester pressure head is a 136-degree diamond rectangular pyramid pressure head, the experimental loading load is 2.94N, and the loading time is 12s. Each coating sample was taken as 10 valid points, one maximum and one minimum were removed, and the average of the remaining 8 points was taken as the coating microhardness value.
2. Bond strength: the bond strength of the sprayed coating samples was tested by the cement tensile method using an Intron5500R electronic universal tester from Instron, with a loading rate of 1mm/min.
3. Porosity void: the true density of the coating material was tested at room temperature by stripping the coating and using archimedes' drainage. The porosity calculation formula is:
porosity= [1- (true density/theoretical density) ]x100%.
4. Coefficient of friction and wear rate: through the test of an HT1000 type ball-disc friction wear testing machine, a quenched high-chromium steel ball with the diameter of 6mm is used as a counter-grinding piece, the load is 15N, the rotating speed is 1000rpm, the rotating radius is 1mm, and the wear time is 30min.
The invention coats Ni with graphite and MoS 2 The particles are introduced and uniformly distributed in WC-Co based supersonic flame spraying material, so that the friction coefficient of the spraying coating material on steel is reduced from 0.65-0.75 to 0.4-0.48 and the wear rate is 4.5X10 under the condition of not reducing the hardness, compactness and binding force of the coating -7 mm 3 Reduced/m to 6.5X10 -8 mm 3 And/m, as shown in Table 1.
TABLE 1 results of physical parameters of coatings for different lubricating phases
As can be seen from Table 1, ni-coated BN and WS are added 2 Is a comparison of the above. Wherein, because the activation and electroplating effects of BN particles are not ideal, the Ni plating layer has poor binding force and is easy to fall off, and harmful Ni can be formed in the plating layer 3 P and Ni 3 Phase B, results in poor performance of the final coating material. While Ni-coated WS 2 In the processes of preparing composite powder by particle and supersonic flame spraying, W is introduced to change the balance of a W-Co-C ternary system in the material, so that the material is subjected to C removal to form brittle eta phase (W 3 Co 3 C, etc.), reducing the wear resistance of the coating material. Thus, the introduction of the lubricating phase significantly improves the lubrication conditions of the dry friction of the coating and significantly improves the wear resistance of the coating. However, as can be seen from table 1, the invention selects a proper lubricating phase, and simultaneously, the invention is assisted by a special supersonic flame spraying process, so that the hardness of the coating prepared by the invention is higher than 1100Hv, the void ratio is lower than 0.8%, the bonding strength is higher than 80MPa, and the friction coefficient is lower than 0.48.
While specific embodiments of the invention have been described in detail, it should not be construed as limiting the scope of the patent. Various modifications and variations which may be made by those skilled in the art without the creative effort are within the scope of the patent described in the claims.
Claims (7)
1. The low-friction supersonic flame spraying wear-resistant coating material is characterized by comprising the following raw materials in percentage by mass: co powder 5-20wt%, mo 2 0.5-8wt% of C powder, 0.3-1.0wt% of VC powder and Cr 3 C 2 2-5wt% of powder, 1-5wt% of solid lubricating phase and the balance of WC powder; the solid lubricating phase is Ni-coated graphite particles and/or Ni-coated MoS 2 Particles
The average particle diameter of the graphite particles is 1 μm, and the MoS 2 The average particle diameter of the particles was 2. Mu.m;
the Co powder and Mo 2 C powder, VC powder, cr 3 C 2 The particle size of the powder and WC powder is 1-2.5 mu m;
the preparation of the low-friction supersonic flame spraying wear-resistant coating material comprises the following steps:
(1) Mixing and granulating
Ball milling the raw materials to prepare mixed powder;
heating and stirring polyvinyl alcohol and deionized water to prepare a polyvinyl alcohol solution, mixing the polyvinyl alcohol solution with mixed powder, and ball-milling to prepare a suspension;
spraying and granulating the suspension to obtain spherical powder;
(2) Powder heat treatment
Drying the spherical powder, heating up and sintering in a gradient way, and cooling to obtain mixed powder;
(3) Spraying
And spraying the mixed powder on the surface of the pretreated substrate by adopting a supersonic flame spraying technology, so as to obtain the low-friction supersonic flame spraying wear-resistant coating material.
2. The method of preparing a low friction, supersonic flame sprayed abrasion resistant coating material of claim 1, comprising the steps of:
(1) Preparation of solid lubricating phase by chemical nickel plating
By granulating graphite or MoS 2 The particles are sequentially subjected to degreasing, coarsening, activation and chemical nickel plating to prepare a solid lubricating phase, wherein the medium of the chemical nickel plating is 20-40g/L NiSO 4 ·6H 2 O, naH 15-30g/L 2 PO 2 ·H 2 O, na of 20-30g/L 3 C 5 H 5 O 7 ·2H 2 O, CH of 10-20g/L 3 COONa·3H 2 O, 20-25mL/L lactic acid, 15-20mL/L acetic acid and 0.05-0.08g/L thiourea, wherein the pH value of the medium is 4.5-6.0, the temperature of the electroless nickel plating is controlled to be 50-75 ℃, and the time is 60-120min;
(2) Mixing and granulating
Ball milling the raw materials to prepare mixed powder;
heating and stirring polyvinyl alcohol and deionized water to prepare a polyvinyl alcohol solution, mixing the polyvinyl alcohol solution with mixed powder, and ball-milling to prepare a suspension;
spraying and granulating the suspension to obtain spherical powder;
(3) Powder heat treatment
Drying the spherical powder, heating up and sintering in a gradient way, and cooling to obtain mixed powder;
(4) Spraying
And spraying the mixed powder on the surface of the pretreated substrate by adopting a supersonic flame spraying technology, so as to obtain the low-friction supersonic flame spraying wear-resistant coating material.
3. The method for preparing a low-friction, supersonic flame-sprayed, abrasion-resistant coating material according to claim 2, wherein the preparation of the polyvinyl alcohol solution comprises the steps of: mixing polyvinyl alcohol powder with deionized water according to a mass ratio of 1:4-8, heating to 65-85 ℃ in a water bath, and stirring for 12-24 hours to prepare concentrated glue; and diluting the concentrated gel with water to obtain the polyvinyl alcohol solution.
4. A method of preparing a low friction, supersonic flame sprayed abrasion resistant coating material according to claim 3, wherein the preparation of said suspension comprises the steps of: adding deionized water into the concentrated glue, mixing and ball milling the diluted polyvinyl alcohol solution and mixed powder according to the mass ratio of 3-5:1, controlling the ball-material ratio to be 5-10:1, the ball milling time to be 12-24h and the rotating speed to be 120-180r/min, and preparing the suspension.
5. The method for preparing a low-friction, supersonic flame-sprayed, wear-resistant coating material according to claim 2, wherein the parameters of spray granulation are: the inlet temperature is 200-380 ℃, the outlet temperature is 100-200 ℃, the feeding speed is 30-50r/min, the rotating speed of the atomizing disk is 12000-18000r/min, the drying atmosphere is nitrogen, and the pressure is 0.5-1.5Mpa.
6. The method for preparing the low-friction wear-resistant coating material sprayed by a supersonic flame according to claim 2, wherein the preheating temperature of a matrix of the supersonic flame spraying technology is 80-120 ℃, the compressed air pressure of a combustion improver is 0.5-0.85MPa, the flow rate is 750-1200SL/min, the fuel is propane or kerosene, the fuel pressure is 0.55-0.85MPa, the fuel flow rate is 10-20 SL/h, the combustion pressure of a combustion chamber is 0.6-1.0 MPa, the powder feeding rate is 60-100g/min, the moving speed of a spray gun is 400-900mm/min, the spraying distance is 200-500mm, the cooling medium is compressed air, and the flow rate is 2-5SL/min.
7. The use of a low friction, supersonic flame-sprayed wear resistant coating material of claim 1, wherein the low friction, supersonic flame-sprayed wear resistant coating material is used in an atmospheric environment below 650 ℃ or in a vacuum environment below 450 ℃.
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