CN111962063B - Preparation method of high-temperature protective coating - Google Patents
Preparation method of high-temperature protective coating Download PDFInfo
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- CN111962063B CN111962063B CN202010727564.0A CN202010727564A CN111962063B CN 111962063 B CN111962063 B CN 111962063B CN 202010727564 A CN202010727564 A CN 202010727564A CN 111962063 B CN111962063 B CN 111962063B
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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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- 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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/24—Nitriding
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Abstract
The invention belongs to the technical field of preparation of high-temperature protective coatings, and particularly relates to a preparation method of a high-temperature protective coating. The TiAlN coating is obtained by directly melting and depositing Ti3Al powder which is sold in the market as a raw material on a preheated forming substrate by using laser as an energy source and utilizing powder-feeding type laser rapid forming equipment and setting reasonable process parameters, and the obtained TiAlN coating is compact and free of defects, and nitrides in the coating mainly exist in a dendritic form. The TiAlN coating prepared by the method does not need a die, and has good coating forming quality, uniform structure and better comprehensive mechanical property.
Description
Technical Field
The invention belongs to the technical field of preparation of high-temperature protective coatings, relates to a powder feeding type laser rapid prototyping technology, in particular to a preparation method of a high-temperature protective coating, and particularly relates to a preparation method of a TiAlN high-temperature protective coating.
Background
In order to meet the requirement of aerospace related materials on service at high temperature, high-temperature protective coatings are widely applied in the field. The nitride hard film layer has the potential of high hardness, high wear resistance, high melting point, good thermal stability, excellent high-temperature strength, excellent chemical inertness and the like, and thus has become a hot point of research at home and abroad. The nitride hard coating which is currently formed into industrialization and widely used is a TiN coating. The coating has good wear resistance and mechanical property, but when the using temperature reaches the critical oxidation temperature, the coating can be rapidly oxidized and failed, and then the protective capability is lost. Compared with a TiN coating, the TiAlN coating has higher oxidation temperature, thermosetting property and high-temperature wear resistance, is expected to partially or completely replace the TiN coating in the field of aerospace, and has wide application prospect.
The patent (CN00136042.6) adopts a cathodic arc ion plating method to prepare a TiAlN coating for a compressor blade of a naval aircraft engine. The patent (CN200510046367.8) adopts a multi-arc ion plating method to prepare a multilayer TiAlN/TiN protective coating. The principle of the cathode arc ion plating is that under a vacuum environment, the electric arcs of a cathode and an anode enable the surface of the cathode to be evaporated, if reaction gas is introduced, plasma generated by the cathode enables the cathode to be ionized and react, and ions are deposited on the surface of a workpiece under the action of an external magnetic field and an electric field to form a coating. The method has the advantages of high metal ionization rate and high deposition rate, but the method is limited by a closed environment, the shape and the size of a workpiece are limited, the thickness of the prepared coating is thin, the service life is short, and the surface roughness of the coating is high.
Therefore, it is necessary to develop a method for preparing a TiAlN high-temperature protective coating that can solve the above problems.
Disclosure of Invention
Aiming at the problems, the invention provides a method for preparing a TiAlN high-temperature protective coating by taking a high-energy laser beam as a heat source.
In order to solve the technical problem, the technical scheme of the invention is as follows:
a preparation method of a high-temperature protective coating takes Ti3Al powder as a raw material, adopts a powder-feeding laser rapid technology to prepare the TiAlN high-temperature protective coating, nitrides in the coating mainly exist in a dendritic crystal form, and the preparation process comprises the following steps:
(1) sieving the commercially available Ti3Al powder through a metal sieve to obtain Ti3Al powder with uniform particle size;
step one, placing Ti3Al powder with uniform particle size in a powder feeder of a laser rapid prototyping system, and taking mixed gas of nitrogen and argon in a certain proportion as powder carrying gas and protective gas;
step two, preheating the substrate;
and step three, coaxially delivering the laser and the powder, synchronously moving, scanning for one pass in one direction only, and melting the Ti3Al powder on the forming substrate to form a molten pool under the action of the laser and reacting with the nitrogen. The molten pool is solidified along with the forward movement of the powder and the laser to form a coating;
fourthly, the coaxial heads of the powder and the laser move for one pass interval along the coating direction vertical to the third step, and the third step is repeated to obtain another pass of coating;
step five, repeating the step four until a TiAlN coating with a required area is prepared;
moving the coaxial heads of the powder and the laser to an initial point, moving the coaxial heads to a position between the first pass and the second pass of the first layer of coating along a direction perpendicular to the first pass of the first layer of coating, and repeating the step three;
step seven, moving the coaxial heads of the powder and the laser by one pass interval along the coating direction vertical to the step six, and repeating the step three to obtain another pass of coating;
and step eight, repeating the step seven until the preparation of the TiAlN coating with the area required by the second layer is finished, and taking out the TiAlN coating and the substrate after the temperature of the coating and the substrate is reduced to room temperature to obtain the alloy with the TiAlN coating on the surface.
The nitrogen in the mixed gas in the first step accounts for 20-80%.
Preferably, the average grain diameter of the Ti3Al powder in the first step is 50-100 μm.
Preferably, the flow rate of the powder carrying airflow in the first step is 5-10L/min, and the flow rate of the protective airflow is 10-30L/min.
Preferably, the preheating temperature of the substrate in the second step is 200 ℃.
Preferably, the powder feeding rate in the third step is 5-15 g/min.
Preferably, the laser power in the third step is 500-1500W, the laser is in a defocused state, the defocused distance is 3-15 mm, and the laser scanning speed is 800-1500 mm/min.
Preferably, the distance between the fourth passes in the step is 0.2-0.6 mm.
Preferably, the pass pitch in step seven is the same as the pass pitch in step four.
The beneficial effects of the invention are: the invention adopts a powder feeding type laser rapid forming technology to prepare the TiAlN high-temperature protective coating. The TiAlN coating is prepared by taking commercially available Ti3Al powder as a raw material, taking a mixed gas of nitrogen and argon in a certain proportion as a powder carrying gas and a protective gas, and reacting on the surface of a formed substrate through the action of laser. The substrate is subjected to preheating treatment, so that the problem of coating cracking caused by excessively high cooling speed of the coating is solved. Compared with other nitriding processes, the laser is used as a coating heat source, so that the bonding force between the coating and the surface of the substrate is enhanced, and the service life of the coating is prolonged; the depth of laser action is deep, and the nitride layer can reach hundreds of microns; the laser action area is small, the thermal deformation of the substrate is small, and the local nitridation of the component and the surface nitridation of the component with a complex shape can be realized; the nitride coatings with different thicknesses and different components can be obtained by adjusting the laser conditions (laser power, scanning speed and the like) and the gas conditions (gas flow rate, nitrogen proportion in mixed gas and the like); the process can be carried out in an atmospheric environment, and the preparation efficiency is high. According to the invention, two layers of coatings are coated on the surface of the substrate, wherein each pass of the second layer of coating is positioned between two adjacent passes of the first layer of coating, so that stress concentration generated between the passes is improved, and the cracking problem of the coating is relieved. The nitride in the coating mainly exists in a dendritic crystal form, is uniformly distributed, and has better comprehensive performance.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the embodiments described are only a few 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.
Features of various aspects of embodiments of the invention will be described in detail below. In the following detailed description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. It will be apparent, however, to one skilled in the art that the present invention may be practiced without these specific details. The following description of the embodiments is merely intended to provide a better understanding of the invention by illustrating examples thereof. The present invention is not limited to any particular arrangement or method provided below, but rather covers all product structures, any modifications, alterations, etc. of the method covered without departing from the spirit of the invention.
In the following description, well-known structures and techniques are not shown to avoid unnecessarily obscuring the present invention. The preparation method of the TiAlN high-temperature protective coating has the following specific embodiment:
example 1
(1) Sieving commercially available Ti3Al powder through a metal sieve to obtain Ti3Al powder with the average particle size of 80 μm;
(2) placing the Ti3Al powder obtained in the step (1) in a powder feeder of a laser rapid prototyping system, and taking a mixed gas of nitrogen and argon in a certain proportion as a powder carrying gas and a protective gas, wherein the nitrogen content in the mixed gas is 60%, the powder carrying gas flow rate is 8L/min, and the protective gas flow rate is 25L/min;
(3) preheating a base plate by using 100mm multiplied by 5mm TC4 titanium alloy as a forming base plate, wherein the preheating temperature is 200 ℃;
(4) the laser and the powder are coaxially sent out and synchronously move, scanning is carried out in one direction only for one pass, the powder feeding speed is 10g/min, the laser power is 600W, the laser is in a defocused state, the defocused distance is 5mm, the laser scanning speed is 900mm/min, and under the action of the laser, the Ti3Al powder is melted on a forming substrate to form a molten pool and reacts with nitrogen. The molten pool is solidified along with the forward movement of the powder and the laser to form a coating;
(5) moving the coaxial heads of the powder and the laser along the coating direction vertical to the step (4) for a certain distance (namely, the pass interval), wherein the pass interval is 0.4mm, and repeating the step (4) to obtain another pass of coating;
(6) repeating the step (5) until the TiAlN coating with the area of 100mm multiplied by 100mm is prepared;
(7) moving the coaxial heads of the powder and the laser to the starting point, moving the coaxial heads to the position between the first pass and the second pass of the first layer of coating along the direction vertical to the first pass of the first layer of coating, and repeating the step (4);
(8) moving the coaxial heads of the powder and the laser along the coating direction vertical to the step (7) for a certain distance (namely, the pass interval), wherein the pass interval is 0.4mm, and repeating the step (4) to obtain another pass of coating;
(9) and (5) repeating the step (8) until the preparation of the TiAlN coating with the area of the second layer of 100mm multiplied by 100mm is finished, and taking out after the temperature of the coating and the substrate is reduced to room temperature to obtain the TC4 titanium alloy with the TiAlN coating on the surface.
Example 2
(1) Sieving commercial Ti3Al powder through a metal sieve to obtain Ti3Al powder with the average grain diameter of 90 mu m;
(2) placing the Ti3Al powder obtained in the step (1) in a powder feeder of a laser rapid prototyping system, and taking a mixed gas of nitrogen and argon in a certain proportion as a powder carrying gas and a protective gas, wherein the nitrogen content in the mixed gas is 40%, the powder carrying gas flow rate is 6L/min, and the protective gas flow rate is 20L/min;
(3) preheating a base plate by using 100mm multiplied by 5mm TC4 titanium alloy as a forming base plate, wherein the preheating temperature is 200 ℃;
(4) the laser and the powder are coaxially sent out and synchronously move, scanning is carried out in one direction only for one pass, the powder feeding speed is 7.5g/min, the laser power is 900W, the laser is in a defocusing state, the defocusing distance is 7mm, the laser scanning speed is 1000mm/min, and under the action of the laser, the Ti3Al powder is melted on a forming substrate to form a molten pool and reacts with nitrogen. The molten pool is solidified along with the forward movement of the powder and the laser to form a coating;
(5) moving the coaxial heads of the powder and the laser along the direction perpendicular to the coating obtained in the step (4) for a certain distance (namely, the pass interval), wherein the pass interval is 0.3mm, and repeating the step (4) to obtain another pass of coating;
(6) repeating the step (5) until the TiAlN coating with the area of 100mm multiplied by 100mm is prepared;
(7) moving the coaxial heads of the powder and the laser to the starting point, moving the coaxial heads to the position between the first pass and the second pass of the first layer of coating along the direction vertical to the first pass of the first layer of coating, and repeating the step (4);
(8) moving the coaxial heads of the powder and the laser along the direction perpendicular to the coating obtained in the step (7) for a certain distance (namely, the pass interval), wherein the pass interval is 0.3mm, and repeating the step (4) to obtain another pass of coating;
(9) and (5) repeating the step (8) until the preparation of the TiAlN coating with the area of the second layer of 100mm multiplied by 100mm is finished, and taking out after the temperature of the coating and the substrate is reduced to room temperature to obtain the TC4 titanium alloy with the TiAlN coating on the surface.
The method controls the depth of the nitride layer by changing the laser conditions (laser power, scanning speed and the like) and the gas conditions (nitrogen-argon ratio, gas flow rate and the like), can prepare the TiAlN coating with the thickness of 250 mu m in the embodiment, and has high coating preparation efficiency and better coating comprehensive performance (high strength, high film-substrate binding force and small crack sensitivity) compared with the prior art.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive various equivalent modifications or substitutions within the technical scope of the present invention, and these modifications or substitutions should be covered within the scope of the present invention.
Claims (9)
1. A preparation method of a high-temperature protective coating is characterized by comprising the following steps: the preparation method of the high-temperature protective coating takes Ti3Al powder as a raw material, adopts a powder feeding type laser technology to prepare the TiAlN high-temperature protective coating, and comprises the following steps:
step one, placing Ti3Al powder with uniform particle size in a powder feeder of a laser rapid prototyping system, and taking mixed gas of nitrogen and argon as powder carrying gas and protective gas;
step two, preheating the substrate;
step three, coaxially sending out the laser and the powder, synchronously moving the laser and the powder, scanning the laser and the powder in one direction for one pass, melting the Ti3Al powder on a forming substrate to form a molten pool under the action of the laser, reacting the molten pool with nitrogen, and solidifying the molten pool along with the forward movement of the powder and the laser to form a coating;
fourthly, moving the coaxial heads of the powder and the laser by a pass interval along the coating direction vertical to the third step, and repeating the third step to obtain another pass of coating;
step five, repeating the step four until a TiAlN coating with a required area is prepared;
moving the coaxial heads of the powder and the laser to an initial point, moving the coaxial heads to a position between the first pass and the second pass of the first layer of coating along a direction perpendicular to the first pass of the first layer of coating, and repeating the step three;
step seven, moving the coaxial heads of the powder and the laser by a pass interval along the coating direction vertical to the step six, and repeating the step three to obtain another pass of coating;
and step eight, repeating the step seven until the preparation of the TiAlN coating with the area required by the second layer is finished, and taking out the TiAlN coating and the substrate after the temperature of the coating and the substrate is reduced to room temperature to obtain the alloy with the TiAlN coating on the surface.
2. The method for preparing a high temperature protective coating according to claim 1, wherein: in the first step, the average particle size of the Ti3Al powder is 50-100 μm.
3. The method for preparing a high temperature protective coating according to claim 1, wherein: in the first step, the nitrogen in the mixed gas accounts for 20-80%.
4. The method for preparing a high temperature protective coating according to claim 1, wherein: in the first step, the flow rate of the powder-carrying airflow is 5-10L/min, and the flow rate of the protective airflow is 10-30L/min.
5. The method for preparing a high temperature protective coating according to claim 1, wherein: the preheating temperature of the substrate in the second step is 200 ℃.
6. The method for preparing a high temperature protective coating according to claim 1, wherein: the powder feeding rate in the third step is 5-15 g/min.
7. The method for preparing a high temperature protective coating according to claim 1, wherein: in the third step, the laser power is 500-1500W, the laser is in an out-of-focus state, the out-of-focus distance is 3-15 mm, and the laser scanning speed is 800-1500 mm/min.
8. The method for preparing a high temperature protective coating according to claim 1, wherein: the fourth step is that the channel interval is 0.2-0.6 mm.
9. The method for preparing a high temperature protective coating according to claim 1, wherein: the channel interval in the step seven is the same as the channel interval in the step four.
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| CN101906631A (en) * | 2010-08-17 | 2010-12-08 | 华东理工大学 | Method for quickly preparing Ti3Al/TiN composite coating |
| CN102676982A (en) * | 2012-06-05 | 2012-09-19 | 华东理工大学 | Fast in-situ preparation method of TiN/Al composite coating |
| CN106947970A (en) * | 2017-03-23 | 2017-07-14 | 华东理工大学 | A kind of titanium or titanium alloy surface prepares fine grain Ti3The method and apparatus of Al/TiN gradient coatings |
| CN108044123A (en) * | 2017-11-14 | 2018-05-18 | 中国航发北京航空材料研究院 | A kind of Nb-Si-Ti alloy preparation methods with oriented freezing organization |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8541067B2 (en) * | 2010-10-05 | 2013-09-24 | King Fahd University Of Petroleum And Minerals | Method of laser treating ti-6AI-4V to form surface compounds |
| EP2940178A4 (en) * | 2012-12-26 | 2016-08-17 | Wu Shanghua | Method for preparing al2o2 coating on surface of silicon -nitride -cutting tool by using pvd,and composite coating method |
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Patent Citations (4)
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|---|---|---|---|---|
| CN101906631A (en) * | 2010-08-17 | 2010-12-08 | 华东理工大学 | Method for quickly preparing Ti3Al/TiN composite coating |
| CN102676982A (en) * | 2012-06-05 | 2012-09-19 | 华东理工大学 | Fast in-situ preparation method of TiN/Al composite coating |
| CN106947970A (en) * | 2017-03-23 | 2017-07-14 | 华东理工大学 | A kind of titanium or titanium alloy surface prepares fine grain Ti3The method and apparatus of Al/TiN gradient coatings |
| CN108044123A (en) * | 2017-11-14 | 2018-05-18 | 中国航发北京航空材料研究院 | A kind of Nb-Si-Ti alloy preparation methods with oriented freezing organization |
Non-Patent Citations (1)
| Title |
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| Large-sized TiAl/Ti3Al multilayer thin sheet: Microstructures,;Zaoyu Shen，et al.;《Journal of Alloys and Compounds》;20180210;102-107页 * |
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