CN113073290B - Preparation method of metal-based material coated with multi-component composite coating - Google Patents
Preparation method of metal-based material coated with multi-component composite coating Download PDFInfo
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- CN113073290B CN113073290B CN202110326113.0A CN202110326113A CN113073290B CN 113073290 B CN113073290 B CN 113073290B CN 202110326113 A CN202110326113 A CN 202110326113A CN 113073290 B CN113073290 B CN 113073290B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C12/00—Solid state diffusion of at least one non-metal element other than silicon and at least one metal element or silicon into metallic material surfaces
- C23C12/02—Diffusion in one step
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/18—Hardening; Quenching with or without subsequent tempering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F17/00—Multi-step processes for surface treatment of metallic material involving at least one process provided for in class C23 and at least one process covered by subclass C21D or C22F or class C25
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Abstract
The invention discloses a preparation method of a metal-based material coated with a multi-element composite coating, and relates to the technical field of metal surface treatment. The invention discloses a preparation method of a metal-based material coated with a multi-element composite coating, which comprises the following steps: pretreating the surface of the metal-based material, then adding the metal-based material into a mixture of a co-penetrating agent and a composite borate in a nitrogen atmosphere, and preserving heat to obtain the metal-based material coated with the multi-element composite coating; wherein the compound borate is prepared by compounding diboron trioxide, zinc borate and sodium borate. The coated metal-based material has excellent wear resistance, corrosion resistance, tensile damage resistance, high hardness and high strength, the composite borate has good fluidity and lower melting point in the preparation process, the decomposed product is not easy to corrode equipment, the coating is uniform, the binding force between the coating and the metal-based material is strong, the qualification rate of the metal-based material is improved, the service life of the metal-based material is prolonged, and the production cost is saved.
Description
Technical Field
The invention belongs to the technical field of metal surface treatment, and particularly relates to a preparation method of a metal-based material coated with a multi-component composite coating.
Background
With the rapid development of metal processing industry, railway manufacturing industry, automobiles, aerospace and other industries, the quality requirements for producing various metal products are higher and higher, however, in the long-term use process of the metal products, failure modes such as friction wear, oxidation corrosion, fatigue fracture and the like are easy to occur under the influence of the external environment, so that the service life of the metal base material is influenced, and a large amount of waste of metal materials is caused. The surface is the interface of metal material and its products and environment, the surface engineering technology is to change the chemical composition of the surface of the base material or to adopt some processes to change the organization structure of the base surface and obtain the corresponding properties of wear resistance, corrosion resistance, pull resistance, high strength, etc., so as to improve the surface performance of the base material, and also to make the common and cheap metal material have special properties, which not only can improve the service life of the metal base material, but also can improve the labor productivity and reduce the production cost.
In order to meet the high requirements of the metal material surface special performance which is developing rapidly, a plurality of new methods for surface treatment have been developed, wherein the widely applied metal surface strengthening treatment technologies include methods of vapor deposition, laser surface strengthening, electron beam surface strengthening, thermal spraying, chemical heat treatment and the like.
Vapor deposition techniques include chemical vapor deposition and physical vapor deposition, which can obtain a coating film with high hardness and high melting point, but cannot be applied locally, have high running cost and environmental pollution, and are not suitable for large-scale industrialization. The laser surface strengthening method is characterized in that laser energy is absorbed by a treated surface to generate height in a short time and then is rapidly cooled to achieve the purpose of surface strengthening. The electron beam surface strengthening method is similar to the laser surface strengthening, except for a heat source, the electron beam is adopted for processing, the strengthening technology is used for local surface modification, the deformation is small, the surface has high hardness, high wear resistance and excellent corrosion resistance, but the strengthening treatment is completed in a vacuum chamber, the industrialization cannot be realized, the flexibility is poor, and the equipment and the cost are expensive. The thermal spraying is to heat, melt or soften and accelerate the solid material, and spray the solid material onto the surface of the substrate to form a special coating, but the bonding strength of the coating and the substrate is low, the porosity of the coating is high, and the uniformity of the coating is poor.
Chemical heat treatment is a heat treatment technique for infiltrating alloy elements into a metal surface layer by utilizing diffusion of elements, and is usually a carburization, nitridation, boriding, carbonitriding, TD treatment technique and the like. Insufficient carburization wear resistance; the nitriding layer has long production period and thin nitriding layer, and is not suitable for application under high stress and impact load; the boronized layer has poor compactness, discontinuity, undesirable impact and fatigue properties and is easy to peel off during working. The TD treatment technology is a general term for diffusion surface hardening treatment by a molten salt soaking method, an electrolysis method and a powder method, the technology which is most applied is the technology for forming superhard coating layers such as VC, NbC, VB, Fe2B and the like on the metal surface by the molten salt soaking method, the technology is an excellent surface modification technology, and a film layer obtained by treatment has excellent wear resistance, corrosion resistance and high hardness, and the service life is greatly prolonged. However, the existing TD treatment technology is more suitable for steel with carbon content higher than 0.3%, and has poor surface modification effect on low-carbon steel. The TD treatment technology belongs to high temperature treatment, generally 900-. The fused salt commonly used in the TD treatment technology at present is borax-based salt, has high melting point and poor fluidity, is easy to cause uneven seeping layer and influences the use effect; the catalyst is decomposed at high temperature, and decomposition products have strong corrosivity, are easy to corrode equipment and fixtures, are difficult to clean residues and the like, so that the catalyst is difficult to use on a large scale in the practical application process.
Therefore, a metal-based material with good molten salt component fluidity, uniform coating, strong coating bonding force, high wear resistance, corrosion resistance and high hardness needs to be developed.
Disclosure of Invention
The invention aims to provide a preparation method of a metal-based material coated with a multi-element composite coating, the coated metal-based material prepared by the method has excellent wear resistance, corrosion resistance, tensile damage resistance, high hardness and high strength, the composite borate has good fluidity and lower melting point in the preparation process of the coating of the metal-based material, the decomposed product is not easy to corrode equipment, the coating is uniform, the binding force between the coating and the metal-based material is strong, the qualification rate of the metal-based material is improved, the service life of the metal-based material is prolonged, and the production cost is saved.
In order to realize the aim of the invention, the invention provides a preparation method of a metal-based material coated with a multi-component composite coating, which specifically comprises the following steps:
(1) pretreatment of the metal-based material: cleaning the surface of the metal-based material, polishing, cleaning with a solvent, and then placing the metal-based material at the temperature of 100-120 ℃ for 0.5-3 h.
(2) Under the atmosphere of nitrogen, adding the pretreated metal-based material into a mixture of a co-permeation agent and a composite borate at the temperature of 600-720 ℃, preserving heat for 1-3 h, then raising the temperature of the mixture to 780-900 ℃, and preserving heat for 2-5 h to obtain the metal-based material coated with the multi-component composite coating. The composite borate is prepared by compounding diboron trioxide, zinc borate and sodium borate.
The co-permeation agent comprises the following components: the titanium dioxide reducing agent comprises vanadium pentoxide, boron carbide, chromium powder, yttrium oxide, a reducing agent and an activating agent, wherein the reducing agent comprises aluminum powder and titanium powder, and the activating agent comprises ammonium chloride and nickel chloride.
Furthermore, the multi-element composite coating is a coating taking boron, vanadium and chromium as main components.
Further, the mass ratio of the composite borate to the co-permeation agent is (2.5-4.1): 1.
further, the composite borate is prepared from the following raw materials in percentage by mass: 20-40% of diboron trioxide, 30-50% of zinc borate and 10-30% of sodium borate.
Further, the composite borate is prepared from boron trioxide, zinc borate and sodium borate according to a mass ratio of 3: 4: 3 is prepared by compounding.
Further, the co-permeation agent is prepared from the following raw materials in percentage by mass: 15-25% of vanadium pentoxide, 15-20% of boron carbide, 10-16% of chromium powder, 10-15% of yttrium oxide, 6-12% of reducing agent and 23-30% of activating agent.
Further, the reducing agent is aluminum powder and titanium powder, and the mass ratio of the aluminum powder to the titanium powder is (1-2): (0.2-0.5) by compounding.
Further, the activating agent is ammonium chloride and nickel chloride, and the mass ratio of the ammonium chloride to the nickel chloride is 4: 1 are mixed.
Further, the composite borate and the co-permeation agent are pretreated before use, and the pretreatment process is drying at the temperature of 120-140 ℃ for 3-4 h.
A preparation method of a metal-based material covered with a multi-component composite coating further comprises the following steps: and (3) taking out the metal-based material coated with the multi-component composite coating in the step (2), naturally cooling, cleaning with acetic acid-containing boiling water, quenching with water or oil, and finally tempering at the temperature of 200-.
The invention achieves the following beneficial effects:
1. the composite borate is prepared by compounding boron trioxide, zinc borate and sodium borate, has a low melting point, enables a metal-based material to achieve an excellent coating effect below 900 ℃, has short heat preservation time and saves energy; the composite borate has good fluidity, can ensure that the co-penetrating agent is uniformly dispersed in the molten salt, so that the components in the coating are uniformly distributed on the surface of the metal-based material, has excellent performances of high hardness, high wear resistance, high corrosion resistance, high tensile damage resistance and the like, and greatly prolongs the service life of the metal-based material; under the action of a reducing agent, zinc borate is reduced into zinc atoms and permeates into the surface of the metal base to be combined with the metal base, so that the coating contains zinc and has excellent corrosion resistance; the composite borate is decomposed at high temperature, the decomposed residual products are less, the equipment and the clamp are not easy to corrode, the service life of salt bath equipment is effectively prolonged, and the energy loss is reduced.
2. Under the action of a reducing agent and an activating agent, vanadium pentoxide, chromium powder and boron nitride in the co-permeation agent provide vanadium, chromium and boron elements for the coating, so that the vanadium, chromium and boron elements form a carbide or alloy matrix with carbon and iron elements under the action of high temperature, the binding force of the coating and the metal matrix is improved, and a compact coating is formed.
3. The addition of the yttrium oxide improves the binding force between the metal substrate and the coating, greatly improves the permeation speed of the co-permeation agent, and the co-permeation agent permeates into the coating, improves the wear resistance and hardness of the coating, reduces the brittleness of the coating and improves the thickness of the coating. The titanium powder is used as a reducing agent, has high chemical activity at high temperature, is easy to react with carbon in a metal matrix, and improves the binding force between a coating and the metal matrix; titanium also reacts readily with Al, N, etc., thereby increasing the hardness and strength of the coating. The invention uses ammonium chloride and nickel chloride with two different activation mechanisms as activating agents, improves the permeation rate of the co-permeation agent, saves the production time, improves the production efficiency, and has NH4 in the activating agent+The nitrogen element in the coating can be increased to react with the metal element in the coating to generate nitride, so that the hardness, the wear resistance, the corrosion resistance and the toughness of the coating are improved.
4. The preparation method has the advantages of simple process flow, small corrosion of the composite borate to equipment, low preparation temperature, short impregnation time, difficult deformation or cracking of the metal substrate, high qualification rate of more than 90 percent, thick and uniform surface film layer of the metal substrate, reduction of production cost, improvement of generation efficiency and contribution to industrial production.
5. The multi-component composite coating prepared on the surface of the metal substrate material is compact and uniform in thickness, has strong binding force with a metal matrix, obviously improves the surface performance of the metal matrix material, has excellent performances of high hardness, high strength, high wear resistance, high tensile damage resistance, high temperature oxidation resistance, environmental corrosion resistance and the like, greatly prolongs the service life of a metal member, and widens the industrial application range of the metal material.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the following examples, the metal-based material was composed of gray iron material (commercially available HT150, carbon content of 3.2-3.5%, average hardness of HV265), Cr12MoV (commercially available, carbon content of 1.45-1.70%, average hardness of HV622), and 2Cr13 martensitic stainless steel material (commercially available, carbon content of 0.16-0.25%, average hardness of HV458), respectively.
The preparation method of the metal-based material coated with the multi-component composite coating according to the present invention is described below with reference to specific examples.
Example 1
A preparation method of a gray iron material covered with a multi-component composite coating specifically comprises the following steps: cleaning the surface of the gray iron material, polishing, cleaning with a solvent, and then placing the gray iron material at the temperature of 100 ℃ and 120 ℃ for 0.5-3 h; and (3) under the nitrogen atmosphere, adding the pretreated gray iron material into a mixture of a co-penetrating agent and a composite borate at the temperature of 600 ℃, preserving heat for 3 hours, then heating the mixture to 780 ℃, and preserving heat for 3 hours to obtain the gray iron material covered with the multi-component composite coating. Wherein the mass ratio of the composite borate to the co-permeation agent is 4.1: the multi-element composite coating is a coating taking boron, vanadium and chromium as main components.
The composite borate is prepared by compounding 20 wt% of diboron trioxide, 50 wt% of zinc borate and 30 wt% of sodium borate.
The co-permeation agent comprises the following components: 25 wt% of vanadium pentoxide, 15 wt% of boron carbide, 10 wt% of chromium powder, 15 wt% of yttrium oxide, 12 wt% of reducing agent and 23 wt% of activating agent. Wherein the reducing agent is prepared from the following components in a mass ratio of 2: 1, and an activating agent is aluminum powder and titanium powder, wherein the mass ratio of the activating agent is 4: 1 ammonium chloride and nickel chloride.
And (3) taking out the gray iron material after the surface of the gray iron material is coated with the multi-element composite coating, naturally cooling, cleaning by using boiling water containing acetic acid, quenching by using water or oil, finally tempering for 3 times at the temperature of 200-600 ℃, and polishing the working surface to ensure that the roughness of the working surface is lower than 0.4, thus obtaining the gray iron material with the required coating.
The composite borate and the co-permeation agent in the embodiment are pretreated before use, and the pretreatment process is drying for 3-4 h at the temperature of 120-140 ℃. The complex borate and the co-permeation agent in all the following examples need to be pretreated before use, and the method is the same as that in example 1, which will not be described again.
Example 2
A preparation method of Cr12MoV coated with a multi-component composite coating specifically comprises the following steps: cleaning the surface of Cr12MoV, polishing, cleaning with a solvent, and then placing the surface at the temperature of 100 ℃ and 120 ℃ for 0.5-3 h; under the nitrogen atmosphere, adding the pretreated Cr12MoV into a mixture of a co-permeation agent and a composite borate at the temperature of 720 ℃, preserving heat for 1h, then raising the temperature of the mixture to 900 ℃, and preserving heat for 2h to obtain the Cr12MoV coated with the multi-element composite coating. Wherein the mass ratio of the composite borate to the co-permeation agent is 2.5: the multi-element composite coating is a coating taking boron, vanadium and chromium as main components.
The composite borate is prepared by compounding 40 wt% of diboron trioxide, 50 wt% of zinc borate and 10 wt% of sodium borate.
The co-permeation agent comprises the following components: 15 wt% of vanadium pentoxide, 20 wt% of boron carbide, 16 wt% of chromium powder, 13 wt% of yttrium oxide, 6 wt% of reducing agent and 30 wt% of activating agent. Wherein the reducing agent is prepared from the following components in a mass ratio of 4: 1, and an activating agent is aluminum powder and titanium powder, wherein the mass ratio of the activating agent is 4: 1 ammonium chloride and nickel chloride.
And (2) covering the surface of the Cr12MoV with a multi-component composite coating, taking out, naturally cooling, cleaning with acetic acid-containing boiling water, quenching with water or oil, and finally tempering at the temperature of 200-.
Example 3
A preparation method of 2Cr13 coated with a multi-component composite coating specifically comprises the following steps: cleaning the surface of 2Cr13, polishing, cleaning with a solvent, and then placing the 2Cr13 at the temperature of 100 ℃ and 120 ℃ for 0.5-3 h; under the nitrogen atmosphere, adding the pretreated 2Cr13 into a mixture of an co-penetrating agent and a composite borate at the temperature of 630 ℃, preserving heat for 3 hours, then raising the temperature of the mixture to 810 ℃, and preserving heat for 5 hours to obtain the 2Cr13 coated with the multi-component composite coating. Wherein the mass ratio of the composite borate to the co-permeation agent is 3: the multi-element composite coating is a coating taking boron, vanadium and chromium as main components.
The composite borate is prepared by compounding 30 wt% of diboron trioxide, 40 wt% of zinc borate and 30 wt% of sodium borate.
The co-permeation agent comprises the following components: 21 wt% of vanadium pentoxide, 18 wt% of boron carbide, 15 wt% of chromium powder, 10 wt% of yttrium oxide, 10 wt% of reducing agent and 26 wt% of activating agent. Wherein the reducing agent is prepared from the following components in percentage by mass: 1, and an activating agent is aluminum powder and titanium powder, wherein the mass ratio of the activating agent is 4: 1 ammonium chloride and nickel chloride.
And (2) taking out the 2Cr13 surface coated with the multi-component composite coating, naturally cooling, cleaning by using acetic acid-containing boiling water, quenching by using water or oil, and finally tempering at the temperature of 200-600 ℃ to obtain the 2Cr13 of the required coating.
Example 4
A preparation method of Cr12MoV coated with a multi-component composite coating specifically comprises the following steps: cleaning the surface of Cr12MoV, polishing, cleaning with a solvent, and then placing the surface at the temperature of 100 ℃ and 120 ℃ for 0.5-3 h; and (2) under the nitrogen atmosphere, adding the pretreated Cr12MoV into a mixture of a co-permeation agent and a composite borate at the temperature of 650 ℃, preserving heat for 2 hours, then heating the mixture to 820 ℃, and preserving heat for 3 hours to obtain the Cr12MoV coated with the multi-element composite coating. Wherein the mass ratio of the composite borate to the co-permeation agent is 3.2: the multi-element composite coating is a coating taking vanadium-boron-chromium as a main component, and the thickness of the coating can be adjusted according to the content of each component of the composite borate and the co-penetrating agent and can also be controlled according to the heat preservation time and the temperature.
The composite borate is prepared by compounding 30 wt% of diboron trioxide, 40 wt% of zinc borate and 30 wt% of sodium borate.
The co-permeation agent comprises the following components: 22 wt% of vanadium pentoxide, 17 wt% of boron carbide, 13 wt% of chromium powder, 12 wt% of yttrium oxide, 8 wt% of reducing agent and 28 wt% of activating agent. Wherein the reducing agent is prepared from the following components in a mass ratio of 3: 1, and an activating agent is aluminum powder and titanium powder, wherein the mass ratio of the activating agent is 4: 1 ammonium chloride and nickel chloride.
And (2) covering the surface of the Cr12MoV with a multi-component composite coating, taking out, naturally cooling, cleaning with acetic acid-containing boiling water, quenching with water or oil, and finally tempering at the temperature of 200-.
Comparative example 1
The preparation method of Cr12MoV coated with a multi-component composite coating comprises the following specific steps of example 4, except that the composite borate in the comparative example is prepared from the following components in a mass ratio of 1: 1 of diboron trioxide and sodium borate.
Comparative example 2
The preparation method of Cr12MoV coated with the multi-component composite coating is the same as that in example 4, except that the reducing agent is aluminum powder.
Comparative example 3
The preparation method of the Cr12MoV coated with the multi-component composite coating is the same as that in the embodiment 4, except that chromium powder is not contained in the preparation method.
Comparative example 4
The preparation method of the Cr12MoV coated with the multi-component composite coating comprises the same specific steps as the example 4, except that the yttrium oxide is not contained in the invention.
Comparative example 5
The preparation method of Cr12MoV coated with a multi-element composite coating is the same as that in example 4, except that the activating agent is nickel chloride.
The surface coatings of the metal-based materials prepared in the above examples 1 to 4 and comparative examples 1 to 5 were subjected to tests of coating thickness, hardness, surface bonding force, abrasion resistance and scratch resistance, and the test results are shown in table 1.
Coating thickness: and (3) performing thickness test on 6 different points on the surface of the metal base material coated with the multi-element composite coating, and taking an average value.
Hardness: the surface hardness was measured by using a Vickers hardness tester model HV-1000 with a test force of 100gf, a square pyramid diamond indenter, and 6 points at different positions were randomly detected, and the average of the values from which a maximum value and a minimum value were removed was taken as the surface hardness.
Surface bonding force: the surface performance of the multifunctional material is measured by an MFT-4000 tester, the load is 100N, the loading rate is 100N/min, the scratch length is set to be 5mm, and the taper angle and the tip radius R of the diamond indenter are set to be 0.2 mm.
And (3) friction resistance: and (3) detecting by a high-temperature friction and wear tester, wherein the load is 20N, and the counter friction ball is SiC under the dry grinding condition.
The tensile damage resistance performance is as follows: the Cr12MoV is used as a die insert of a chassis part of a heavy truck, and after the die insert is used for 10000 times, the surface condition of the die is checked.
TABLE 1 test results of surface coating properties of metal-based materials
The test results in table 1 show that the coating of the present invention is relatively thick, has high hardness, excellent surface bonding force, excellent wear resistance and excellent tensile damage resistance. The zinc borate is added into the composite borate, so that the thickness, hardness, surface bonding force, wear resistance and tensile damage resistance of the coating are obviously improved; the co-permeation agent is added with chromium powder, so that the hardness and the wear resistance of the coating are improved; the titanium powder is added into the reducing agent, so that the thickness, hardness and surface binding force of the coating are obviously improved; the yttrium oxide is added into the co-permeation agent, so that the hardness, the surface bonding force and the wear resistance of the coating are improved; the activating agent of the invention uses the combination of ammonium chloride and nickel chloride, thus improving the hardness, surface bonding force and wear resistance of the coating.
The technical features of the embodiments described above can be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (10)
1. A preparation method of a metal-based material coated with a multi-component composite coating is characterized by comprising the following steps:
(1) pretreatment of the metal-based material: cleaning the surface of the metal-based material, polishing, cleaning with a solvent, and then placing the metal-based material at the temperature of 100-120 ℃ for 0.5-3 h;
(2) under the nitrogen atmosphere, adding the pretreated metal-based material into a mixture of a co-permeation agent and a composite borate at the temperature of 600-720 ℃, preserving heat for 1-3 h, then raising the temperature of the mixture to 780-900 ℃, and preserving heat for 2-5 h to obtain the metal-based material coated with the multi-component composite coating;
the composite borate is prepared by compounding diboron trioxide, zinc borate and sodium borate;
the co-permeation agent comprises the following components: the titanium dioxide reducing agent comprises vanadium pentoxide, boron carbide, chromium powder, yttrium oxide, a reducing agent and an activating agent, wherein the reducing agent comprises aluminum powder and titanium powder, and the activating agent comprises ammonium chloride and nickel chloride.
2. The method for preparing a metal-based material coated with a multi-component composite coating according to claim 1, wherein the multi-component composite coating is a coating mainly containing boron, vanadium and chromium.
3. The method for preparing the multi-element composite coated metal-based material according to claim 1, wherein the mass ratio of the composite borate to the co-permeation agent is (2.5-4.1): 1.
4. the method for preparing the metal-based material coated with the multi-component composite coating according to claim 1, wherein the composite borate is prepared from the following raw materials in percentage by mass: 20-40% of diboron trioxide, 30-50% of zinc borate and 10-30% of sodium borate.
5. The method for preparing a metal-based material covered with a multi-element composite coating according to claim 1, wherein the composite borate is diboron trioxide, zinc borate and sodium borate in a mass ratio of 3: 4: 3 is prepared by compounding.
6. The method for preparing the metal-based material coated with the multi-element composite coating according to claim 1, wherein the co-permeation agent is prepared from the following raw materials in percentage by mass: 15-25% of vanadium pentoxide, 15-20% of boron carbide, 10-16% of chromium powder, 10-15% of yttrium oxide, 6-12% of reducing agent and 23-30% of activating agent.
7. The method for preparing the metal-based material covered with the multi-component composite coating according to claim 1 or 6, wherein the reducing agent is aluminum powder and titanium powder, and the mass ratio of the aluminum powder to the titanium powder is (1-2): (0.2-0.5) by compounding.
8. The method for preparing a metal-based material covered with a multi-component composite coating according to claim 1 or 6, wherein the activating agent is ammonium chloride and nickel chloride in a mass ratio of 4: 1 are mixed.
9. The method as claimed in claim 1, wherein the pre-treatment is carried out before the borate complex and the co-penetrant are used, and the pre-treatment is carried out by drying at 120-140 ℃ for 3-4 h.
10. The method of preparing a multi-component composite coated metal-based material of claim 1, further comprising: and (3) taking out the metal-based material coated with the multi-component composite coating in the step (2), naturally cooling, cleaning with acetic acid-containing boiling water, quenching with water or oil, and finally tempering at the temperature of 200-.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS5729570A (en) * | 1980-06-17 | 1982-02-17 | Hitachi Metals Ltd | Surface treating method |
| JPS5825470A (en) * | 1981-08-10 | 1983-02-15 | Toyota Central Res & Dev Lab Inc | Indirect heating furnace for surface treatment of metal or the like using boride bath |
| CN1092819A (en) * | 1993-03-19 | 1994-09-28 | 福建省冶金工业研究所 | Salt bath process for rare-earth-vanadium-boron co-diffusion |
| CN102268635A (en) * | 2011-08-12 | 2011-12-07 | 李华平 | Rare earth-boron-vanadium carburizing agent |
| CN103526154A (en) * | 2013-10-30 | 2014-01-22 | 重庆理工大学 | Chrome alum rare earth multicomponent cementation borax salt bath penetration metal penetrating agent and application method thereof |
| CN107385386A (en) * | 2017-08-07 | 2017-11-24 | 江苏大学 | A kind of high rigidity, high infiltration rate and big infiltration layer salt bath B-V co-penetrant and co-penetration technology |
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2021
- 2021-03-26 CN CN202110326113.0A patent/CN113073290B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5729570A (en) * | 1980-06-17 | 1982-02-17 | Hitachi Metals Ltd | Surface treating method |
| JPS5825470A (en) * | 1981-08-10 | 1983-02-15 | Toyota Central Res & Dev Lab Inc | Indirect heating furnace for surface treatment of metal or the like using boride bath |
| CN1092819A (en) * | 1993-03-19 | 1994-09-28 | 福建省冶金工业研究所 | Salt bath process for rare-earth-vanadium-boron co-diffusion |
| CN102268635A (en) * | 2011-08-12 | 2011-12-07 | 李华平 | Rare earth-boron-vanadium carburizing agent |
| CN103526154A (en) * | 2013-10-30 | 2014-01-22 | 重庆理工大学 | Chrome alum rare earth multicomponent cementation borax salt bath penetration metal penetrating agent and application method thereof |
| CN107385386A (en) * | 2017-08-07 | 2017-11-24 | 江苏大学 | A kind of high rigidity, high infiltration rate and big infiltration layer salt bath B-V co-penetrant and co-penetration technology |
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| CN113073290A (en) | 2021-07-06 |
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