CN112921317A - Method for preparing ternary layered MAX phase ceramic coating through laser cladding - Google Patents
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- CN112921317A CN112921317A CN202110103890.9A CN202110103890A CN112921317A CN 112921317 A CN112921317 A CN 112921317A CN 202110103890 A CN202110103890 A CN 202110103890A CN 112921317 A CN112921317 A CN 112921317A
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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
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- 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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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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Abstract
The invention provides a method for preparing a ternary layered MAX phase ceramic coating by laser cladding, and relates to the technical field of ceramic coatings. The method for preparing the ternary layered MAX phase ceramic coating through laser cladding comprises the steps of ball-milling and uniformly mixing M, A, X element powder or a mixture of binary compound powder and ternary compound powder of the element powder in a certain molar ratio, then carrying out laser cladding on the surface of a substrate, and finally carrying out subsequent heat treatment to obtain the MAX phase ceramic coating. MAX phase chemical formula Mn+1AXnM is a transition metal element; a is main group element, mainly refers to IIIA and IVA group element; x is C or N element; n is an integer of 1 to 6. The specific method comprises the following steps: preparation of a base material, preparation of powder, a preparation process of a coating and post-heat treatment of the coating. The method for preparing the ternary layered MAX phase ceramic coating by laser cladding can effectively solve the problem of unclear thermal decomposition and in-situ synthesis mechanism.
Description
Technical Field
The invention relates to the technical field of ceramic coatings, in particular to a method for preparing a ternary layered MAX-phase ceramic coating by laser cladding.
Background
The MAX phase is a general name of a novel ternary compound with a micro-layered structure, and the chemical formula can be expressed as Mn+ 1AXn, wherein M is a transition metal element; a is main group element, mainly refers to IIIA and IVA group element; x is C or N element; n is an integer of 1 to 6. The MAX phase has a special nano-layered structure and bonding types, so that the MAX phase not only has excellent electric and thermal conductivity, machinability, thermal shock resistance, damage tolerance and other properties of a metal material, but also has the high elastic modulus and excellent high-temperature, oxidation resistance, corrosion resistance, wear resistance and other properties of a ceramic material.
In particular, the MAX phase is regarded as a coating material. This is because the unique layered structure and electron density of state distribution of MAX phase can provide multiple energy absorption mechanisms, and is a protective coating material with great potential for application. In a MAX phase system, Ti3AlC2、Ti2AlC、Ti2AlN、Cr2AlC and the like can be selectively oxidized to form Al on the surface2O3The film has excellent high-temperature oxidation resistance and Ti2AlN also has excellent wear resistance; on the other hand, the MAX phases have the thermal expansion coefficient similar to that of metal, so that the MAX phases have great application prospects as high-temperature corrosion resistant protective coating materials for metal surfaces. In addition, the MAX phase has great development potential as a coating material in the aspects of friction and wear resistance, high-strength conductivity, special medium corrosion resistance and the like.
In the current research on the preparation of MAX phase coatings, various composite magnetron sputtering processes are generally adopted to prepare thin coatings, and spraying processes are adopted to prepare thick coatings. The MAX phase coating prepared by sputtering usually faces the problems of functional size and substrate selection, etc., while the MAX phase coating prepared by cold and hot spraying techniques respectively needs to solve the problems of density and thermal decomposition.
Disclosure of Invention
Solves the technical problem
Aiming at the defects of the prior art, the invention provides a method for preparing a ternary layered MAX phase ceramic coating by laser cladding, which can efficiently, simply and conveniently prepare a dense MAX phase thick coating with higher purity so as to promote the large-scale industrial application of the MAX phase coating.
Technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme: a method for preparing a ternary laminar MAX phase ceramic coating through laser cladding comprises the steps of carrying out ball milling and mixing on M, A, X element powder or a mixture of binary compound powder and ternary compound powder of the element powder in a certain molar ratio uniformly, carrying out laser cladding on the surface of a substrate, and carrying out heat treatment to obtain the MAX phase ceramic coating. MAX phase chemical formula Mn+1AXnM is a transition metal element; a is main group element, mainly refers to IIIA and IVA group element; x is C or N element; n is an integer of 1-6, and the specific method comprises the following steps: preparation of a base material, preparation of powder, a preparation process of a coating and post-heat treatment of the coating.
Preferably, the raw material may be M, A, X element powder or a mixture of binary and ternary compound powders thereof.
Preferably, the base material can be titanium alloy, zirconium alloy, copper alloy and various common steel materials. The substrate was cut to a desired size using a wire electric discharge machine, and after a surface oxide layer was polished off using 100# SiC abrasive paper, it was washed with acetone and absolute ethanol, and dried in hot air.
Preferably, the powder is prepared by adopting M, A, X element powder or a mixture of binary compound powder and ternary compound powder thereof, taking the molar ratio of M, A, X ═ (n +1):1: n as a basic proportion, mixing the raw material powder for 2 hours in vacuum by a physical mechanical ball milling method, sieving, and drying for 1 hour at 100 ℃ in vacuum.
Preferably, the preparation process of the coating is to adopt laser cladding in-situ synthesis of the coating, and use a self-made mold to directly lay the mixed powder on the surface of the treated substrate. The thickness of the powder is 1-2 mm. The optical fiber laser system with the argon cabin is adopted, and the main technological parameters are as follows: the laser power is 1.8-3.5kW, and the laser spot size is 10 multiplied by 2mm2The scanning speed is 60-240mm/min, and the argon flow is 10L/min.
Preferably, the coating is post-heat treated to produce a coating of ≤ 1.0 × 10-1Heat treatment is carried out in Pa vacuum or Ar protective atmosphere, the temperature is 700-1200 ℃, the treatment time is 1-10h, and the coating taking MAX phase ceramic as the main phase is obtained after the treatment.
Preferably, in the preparation of the powder, the powder used for cladding coating comprises the following main components: m, A, X, but it can be element powder or the mixture of binary and ternary compound powder, it is not necessary to be consistent with the cladding coating, the molar ratio of M, A, X in the mixed powder is adjusted on the basis of the basic proportion of (n +1):1: n according to the loss degree of different elements in the coating cladding process.
Preferably, the preparation process of the coating does not need to additionally heat the substrate during the laser cladding coating process, but the preparation process needs to be carried out in an argon chamber.
Preferably, in the post-heat treatment of the coating, the treatment conditions for performing the final heat treatment on the clad coating are as follows: 1.0X 10-3Pa-1.0×10-2Pa vacuum or Ar protective atmosphere, the treatment temperature is 700-1000 ℃, and the treatment time is 1-10 h.
Advantageous effects
The invention provides a method for preparing a ternary layered MAX phase ceramic coating by laser cladding. The method has the following beneficial effects:
the method for preparing the ternary layered MAX-phase ceramic coating by the novel laser cladding can effectively avoid the problems of thermal decomposition and unclear in-situ synthesis mechanism, and can ensure that the preparation quality of the ceramic coating is better.
Drawings
FIG. 1 shows XRD patterns of a laser cladding coating and the coating annealed at 1000 ℃ for 1 hour;
FIG. 2 SEM topography of laser cladding coatings;
FIG. 3 SEM morphology after annealing of the laser cladding coating at 1000 ℃ for 1 h.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely 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.
Example (b):
the embodiment of the invention provides a method for preparing a ternary layered MAX phase ceramic coating by laser cladding, which comprises the steps of carrying out ball milling and mixing uniformly on M, A, X element powder or a mixture of binary compounds and ternary compounds of the element powder in a certain molar ratio, carrying out laser cladding on the surface of a substrate, and carrying out heat treatment to obtain the MAX phase ceramic coating. MAX phase chemical formula Mn+1AXnM is a transition metal element; a is main group element, mainly refers to IIIA and IVA group element; x is C or N element; n is an integer of 1-6, and the specific method comprises the following steps: preparation of a base material, preparation of powder, a preparation process of a coating and post-heat treatment of the coating.
The raw material powder for cladding can be M, A, X element powder or a mixture of binary compound powder and ternary compound powder thereof. The base material is prepared by coating titanium alloy, zirconium alloy, copper alloy or various steel materials. The substrate was cut to a desired size using a wire electric discharge machine, and after a surface oxide layer was polished off using 100# SiC abrasive paper, it was washed with acetone and absolute ethanol, and dried in hot air. The powder is prepared by adopting M, A, X element powder or a mixture of binary and ternary compound powder thereof, taking the molar ratio of M, A, X ═ n + 1: n as a basic proportion, mixing the raw material powder for 2 hours in vacuum by a physical mechanical ball milling method, sieving, and drying for 1 hour at 100 ℃ in vacuum.
The preparation process of the coating is to adopt laser cladding in-situ synthesis coating, and use a self-made mould to directly lay the mixed powder on the surface of the treated substrate. The thickness of the powder is 1-2 mm. The optical fiber laser system with the argon cabin is adopted, and the main technological parameters are as follows: the laser power is 1.8-3.5kW, and the laser spot size is 10 multiplied by 2mm2The scanning speed is 60-240mm/min, and the argon flow is 10L/min. The post-heat treatment of the coating is to make the prepared coating be less than or equal to 1.0 multiplied by 10-1Heat treatment is carried out in Pa vacuum or Ar protective atmosphere, the temperature is 700-1200 ℃, the treatment time is 1-10h, and the coating taking MAX phase ceramic as the main phase is obtained after the treatment.
In the preparation of the powder, the main component of the powder used for cladding the coating is M, A, X, but the raw material can be element powder or a mixture of binary and ternary compounds thereof, the raw material is not required to be consistent with the cladding coating, and the molar ratio of M, A, X in the mixed powder is adjusted on the basis of the basic proportion of (n +1):1: n according to the loss degree of different elements in the cladding process of the coating.
In the preparation process of the coating, the substrate does not need to be heated additionally in the process of laser cladding coating, but the heating is carried out in an argon chamber. In the post-heat treatment of the coating, the treatment conditions for carrying out the final heat treatment on the cladded coating are as follows: 1.0X 10- 3Pa-1.0×10-2Pa vacuum or Ar protective atmosphere, the treatment temperature is 700-1000 ℃, and the treatment time is 1-10 h.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. A method for preparing a ternary layered MAX phase ceramic coating by laser cladding is characterized by comprising the following steps: the M, A, X element powder or the mixture of binary and ternary compound powder thereof with a certain molar ratio is ball-milled and evenly mixed, laser cladding is carried out on the surface of a substrate, and the MAX coating is obtained through heat treatment. MAX phase chemical formula Mn+1AXnM is a transition metal element; a is main group element, mainly refers to IIIA and IVA group element; x is C or N element; n is an integer of 1 to 6, specifically including Ti2AlC、Ti2AlN、Cr2AlC、V2AlC、Ti3AlC、Ti3AlC2And the like. The specific method comprises the following steps: preparation of a base material, preparation of powder, a preparation process of a coating and post-heat treatment of the coating.
2. The method for preparing the ternary layered MAX phase ceramic coating by laser cladding according to claim 1, wherein the method comprises the following steps: the powder mixture for laser cladding can be M, A, X element powder mixture or mixture of binary and ternary compound powder thereof.
3. The method for preparing the ternary layered MAX phase ceramic coating by laser cladding according to claim 1, wherein the method comprises the following steps: the base material is titanium alloy, zirconium alloy, copper alloy or common steel materials. The substrate was cut to a desired size using a wire electric discharge machine, and after a surface oxide layer was polished off using 100# SiC abrasive paper, it was washed with acetone and absolute ethanol, and dried in hot air.
4. The method for preparing the ternary layered MAX phase ceramic coating by laser cladding according to claim 1, wherein the method comprises the following steps: the powder is prepared by taking M, A, X element powder or binary and ternary compound powder thereof as raw material powder, taking M, A, X molar ratio (n +1):1: n as a basic proportion, mixing the raw material powder for 2 hours by a physical mechanical ball milling method, sieving, and drying for 1 hour at 100 ℃ in vacuum.
5. The method for preparing the ternary layered MAX phase ceramic coating by laser cladding according to claim 1, wherein the method comprises the following steps: the preparation process of the coating adopts a laser cladding method, and a self-made mould is used for directly laying the mixed powder on the surface of the treated substrate. The thickness of the powder is 1-2 mm. The optical fiber laser system with the argon cabin is adopted, and the main technological parameters are as follows: the laser power is 1.8-3.5kW, and the laser spot size is 10 multiplied by 2mm2The scanning speed is 60-240mm/min, and the argon flow is 10L/min.
6. The method for preparing the ternary layered MAX phase ceramic coating by laser cladding according to claim 1, wherein the method comprises the following steps: the post-heat treatment of the coating is to heat the prepared coating to less than or equal to 1.0 multiplied by 10-1Heat treatment is carried out in Pa vacuum or Ar protective atmosphere, the temperature is 700-1200 ℃, the treatment time is 1-10h, and the coating taking MAX phase ceramic as the main phase is obtained after the treatment.
7. The method for preparing the ternary layered MAX phase ceramic coating by laser cladding according to claim 1, wherein the method comprises the following steps: in the preparation of the powder, the powder used for cladding coating comprises the following main components: m, A, X element powder mixture or mixture of binary and ternary compounds thereof, which is not required to be consistent with the cladding coating, the molar ratio of M, A, X in the mixed powder is adjusted on the basis of the basic proportion of (n +1):1: n according to the loss degree of different elements in the cladding process of the coating.
8. The method for preparing the ternary layered MAX phase ceramic coating by laser cladding according to claim 1, wherein the method comprises the following steps: in the preparation process of the coating, the substrate does not need to be heated additionally in the process of laser cladding, but the heating is carried out in an argon chamber.
9. The method for preparing the ternary layered MAX phase ceramic coating by laser cladding according to claim 1, wherein the method comprises the following steps: in the post-heat treatment of the coating, the treatment conditions for carrying out the final heat treatment on the cladded coating are as follows: 1.0X 10-3Pa-1.0×10-2Pa vacuum or Ar protective atmosphere, the treatment temperature is 700-1000 ℃, and the treatment time is 1-10 h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114032542A (en) * | 2021-11-02 | 2022-02-11 | 贵州大学 | Method for preparing MAX phase coating by using two-step method of laser technology |
| CN114262239A (en) * | 2021-12-28 | 2022-04-01 | 江苏大学 | Preparation method of carbon/carbon composite material high-temperature oxidation-resistant coating |
| CN114315420A (en) * | 2021-12-28 | 2022-04-12 | 江苏大学 | Method for preparing carbon/carbon composite material high-temperature oxidation-resistant coating through in-situ reaction |
| CN114657551A (en) * | 2021-12-28 | 2022-06-24 | 江苏大学 | Repairing method of high-temperature oxidation-resistant coating |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114032542A (en) * | 2021-11-02 | 2022-02-11 | 贵州大学 | Method for preparing MAX phase coating by using two-step method of laser technology |
| CN114262239A (en) * | 2021-12-28 | 2022-04-01 | 江苏大学 | Preparation method of carbon/carbon composite material high-temperature oxidation-resistant coating |
| CN114315420A (en) * | 2021-12-28 | 2022-04-12 | 江苏大学 | Method for preparing carbon/carbon composite material high-temperature oxidation-resistant coating through in-situ reaction |
| CN114657551A (en) * | 2021-12-28 | 2022-06-24 | 江苏大学 | Repairing method of high-temperature oxidation-resistant coating |
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