CN112210748A - Method for preparing diffusion barrier layer by embedding aluminizing-preoxidation - Google Patents
Method for preparing diffusion barrier layer by embedding aluminizing-preoxidation Download PDFInfo
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- CN112210748A CN112210748A CN202011094516.9A CN202011094516A CN112210748A CN 112210748 A CN112210748 A CN 112210748A CN 202011094516 A CN202011094516 A CN 202011094516A CN 112210748 A CN112210748 A CN 112210748A
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- aluminizing
- preoxidation
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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
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
- C23C10/34—Embedding in a powder mixture, i.e. pack cementation
- C23C10/36—Embedding in a powder mixture, i.e. pack cementation only one element being diffused
- C23C10/48—Aluminising
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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
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/60—After-treatment
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Abstract
The invention provides a method for preparing a diffusion barrier layer by embedding aluminizing-preoxidation, which comprises the following steps: preparing an aluminizing agent according to a certain proportion, and roasting the aluminizing agent for multiple times to activate the aluminizing agent; aluminizing by adopting a solid powder method under atmospheric conditions to obtain an aluminized layer on the surface of the high-temperature alloy workpiece; an aluminum oxide film is generated on the surface of the aluminized layer through high-temperature pre-oxidation, and the aluminum oxide film can be used as a diffusion barrier layer and can effectively prevent the interdiffusion of the high-temperature alloy substrate and the coating surface layer on the outer surface of the aluminum oxide film.
Description
Technical Field
The invention belongs to the field of metal surface processing by chemical heat treatment, and particularly relates to a method for preparing a diffusion barrier layer by embedding aluminizing and pre-oxidation.
Background
The K424, GH536 and GH3128 alloys are high-temperature alloys widely used in aircraft engines, have high-temperature specific strength, the maximum working temperature can reach over 1000 ℃, certain coatings of the high-temperature alloys need to maintain the functionality of the coatings in the high-temperature service process, but under the condition of high temperature and long time, mutual diffusion can occur between the coatings and a base material, so that the surface coatings fail. Therefore, a diffusion barrier layer needs to be prepared between the base material and the surface coating, so that mutual diffusion between the coating and the base is effectively prevented, and the performance of the coating is ensured. At present, the diffusion impervious layer can be directly prepared by adopting methods such as spraying, electroplating and the like, but the diffusion impervious layer prepared by directly adopting the methods of spraying and electroplating has general bonding strength with an alloy matrix and poor diffusion resistance. The diffusion barrier layer is prepared by adopting indirect reaction, and the prepared diffusion barrier layer not only has excellent diffusion resistance effect, but also has good bonding strength.
Disclosure of Invention
The invention aims at the defects of the prior art and provides a method for preparing a diffusion barrier layer by embedding aluminizing-preoxidation.
The technical scheme adopted by the invention for solving the technical problems is as follows: a method for preparing a diffusion barrier layer by embedding aluminizing-preoxidation comprises the following steps:
(1) preparing an aluminizing agent: preparing an aluminizing agent from aluminum iron powder and ammonium chloride powder according to the following mass percentage, wherein the aluminum iron powder accounts for 95-98% of the aluminizing agent, and the balance is ammonium chloride powder;
(2) embedding aluminizing: embedding the test piece into an aluminizing agent for aluminizing treatment, wherein the aluminizing temperature is 870-950 ℃, and the heat preservation time is 2-8 hours;
(3) a pre-oxidation procedure: and carrying out high-temperature preoxidation treatment on the aluminized test piece to generate an alumina film layer on the aluminized layer surface of the test piece to be used as a diffusion barrier layer.
Further, the particle size of the aluminum-iron powder in the step (1) is smaller than 30 meshes, wherein the mass fraction of the iron powder is 42% -50%, and the balance is aluminum.
Further, the aluminizing agent used in the step (1) needs to be roasted for at least five times for aluminizing the cavity; the temperature of the roasting process is 920-980 ℃, and the roasting time is 2-4 h.
Further, when the single test piece or the single-layer test piece is subjected to aluminizing embedding in the step (2), the thickness of the aluminizing agent above and below the test piece is 60-80 mm, and when the multi-layer test piece is subjected to aluminizing embedding, the thickness of the aluminizing agent above the uppermost test piece and below the lowermost test piece is 60-80 mm.
Further, when the plurality of test pieces are aluminized in the step (2), the distance between the test pieces is not less than 15mm, and the distance between the test pieces and the aluminized wrapping wall is not less than 20 mm.
Further, when the multilayer test piece is aluminized in the step (2), the thickness of the interlayer aluminizing agent is 30-50 mm.
Further, the high-temperature pre-oxidation treatment in the step (3) comprises two modes of vacuum pre-oxidation or atmospheric pre-oxidation:
vacuum pre-oxidation: placing the test piece in a vacuum furnace, preserving heat for 1-4 h at 900-1070 ℃, and then filling argon for cooling;
atmospheric pre-oxidation: and (3) placing the test piece in an air furnace, preserving the heat for 3-6 h at 760-950 ℃, and then air cooling.
Further, during the vacuum pre-oxidation in the step (3), the vacuum pressure is controlled to be 100-220 Pa in the processes of temperature rise and heat preservation at the temperature of more than 800 ℃.
Further, the test piece in the step (2) is pretreated to remove oxides and dirt on the surface of the test piece before the embedding aluminizing process; and (4) before the pre-oxidation process in the step (3), blowing sand to clean the surface of the aluminized test piece, and removing the attachments on the surface of the test piece.
The principle of the invention is as follows: preparing an aluminizing agent according to a proportion, and roasting the aluminizing agent for multiple times to activate the aluminizing agent; under the atmospheric condition, aluminizing by adopting a solid powder method to obtain an aluminized layer on the surface of the high-temperature alloy part; and then, a layer of aluminum oxide film is generated on the surface of the aluminized layer through high-temperature pre-oxidation, namely a diffusion barrier layer, and the aluminum oxide film can be used as a bonding layer of the surface layer of the substrate and the surface layer of the substrate, and can effectively prevent the interdiffusion of the high-temperature alloy substrate and the surface layer coated on the outer surface of the aluminum oxide film. The diffusion barrier layer of the high-temperature alloy material prepared by the invention effectively prevents the mutual diffusion between the base material and the surface coating, keeps the functionality of the surface coating, can improve the oxidation resistance, corrosion resistance, hardness, wear resistance and the like of the surface of the material, and has wide value in the field of protective coatings of high-temperature alloy workpieces.
Compared with the prior art, the invention has the beneficial effects that:
1. the alumina barrier layer formed by the method is complete, continuous and compact and stably exists at high temperature for a long time;
2. the prepared alumina barrier layer can effectively prevent the mutual diffusion between the surface coating and the matrix material, and the surface coating is still intact after the heat resistance test of heat preservation at 900 ℃ for 300h, so that the characteristics of the surface coating are kept;
3. the chemical heat treatment and vacuum or conventional heat treatment methods related by the invention are not limited by the shape and structure of the workpiece, and the process adaptability is strong;
4. the method can also realize the local preparation of the diffusion barrier layer of the workpiece, and the method has the advantages of low cost of raw materials, simple process and high production efficiency.
Drawings
FIG. 1 is a cross-sectional view of a test piece of example 1 after aluminizing and pre-oxidation;
FIG. 2 is a surface topography of the alumina barrier layer of the test piece of example 1 after a heat resistance test.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A method for preparing a diffusion barrier layer by embedding aluminizing-preoxidation comprises the following steps:
(1) dry blowing sand: corundum sand is adopted to blow off oxide and dirt on the surfaces of a workpiece and a test piece, wherein the wind pressure is not more than 0.3 MPa;
(2) preparing and roasting an aluminizing agent: proportioning according to the mass percentage, wherein the aluminum-iron powder in the aluminizing agent accounts for 98 percent, and the ammonium chloride powder accounts for 2 percent; the powder granularity of the aluminum iron powder (the mass fraction of the iron powder is 45 percent, and the balance is aluminum) is less than 30 meshes, and the ammonium chloride powder is a commercially available analytical reagent; roasting the aluminizing agent for 5 times after the preparation is finished, wherein the roasting temperature is 950 ℃, and the roasting time is 2 hours each time;
(3) embedding aluminizing: filling the prepared aluminizing agent into an aluminizing bag, embedding the test piece into the roasted aluminizing agent, placing the aluminizing bag in a resistance furnace, heating to 920 ℃, and preserving heat for 2.5 hours;
the specific embedding operation of the multilayer test piece was: uniformly spreading a layer of aluminizing agent with the thickness of 70mm on the bottom of the aluminizing bag, putting a layer of test piece on the aluminizing agent, wherein the distance between the test pieces is 15mm, the distance between the test piece and the bag wall is 20mm, uniformly spreading a layer of aluminizing agent with the thickness of 40mm on the layer of test piece, putting a second layer of test piece …, assembling the test pieces layer by layer, and tamping the aluminizing agent layer by layer (paying attention to not damage the test pieces) so as to avoid generating an air cavity; uniformly scattering a layer of aluminizing agent with the thickness of 70mm on the uppermost layer of test piece, lightly tamping, then putting an upper aluminizing bag lower cover, uniformly scattering a layer of waste aluminum-iron alloy powder with the thickness of 60mm on the lower cover, lightly compacting, then putting an upper aluminizing bag upper cover, and lightly tapping the packed outer wall to further compact the aluminizing agent;
(4) liquid sand blowing: after aluminizing is finished, cooling the temperature in the furnace to room temperature, taking out the test piece, blowing sand to clean the surface of the test piece, and removing surface attachments;
(5) vacuum pre-oxidation: drying the test piece, placing the test piece in a vacuum furnace, preserving the heat for 2 hours at 1050 ℃, and then filling argon for cooling; and during vacuum pre-oxidation, controlling the vacuum pressure to be 150-180 Pa in the processes of temperature rise and heat preservation at the temperature of over 800 ℃.
Wherein, FIG. 1 shows the cross-sectional morphology of the sample of this example after aluminizing-pre-oxidation, the depth of the aluminized layer is 0.02 mm-0.04 mm, and an aluminum oxide film is formed on the surface thereof by Raman detection, and the thickness of the aluminum oxide film is 0.5 μm-2 μm according to calculation; FIG. 2 shows that the surface of the aluminum oxide barrier layer of the test piece is coated with a surface layer, and after the test at 900 ℃ for 300h, the surface still presents the metallic silvery white of the surface layer coating, and the surface has no phenomena of scratch, wrinkling, bubbling, cracking, peeling, shedding and the like, which indicates that the base material and the surface layer do not diffuse mutually.
Example 2
A method for preparing a diffusion barrier layer by embedding aluminizing-preoxidation comprises the following steps:
(1) dry blowing sand: corundum sand is adopted to blow off oxide and dirt on the surfaces of a workpiece and a test piece, wherein the wind pressure is not more than 0.3 MPa;
(2) preparing and roasting an aluminizing agent: proportioning according to the mass percentage, wherein the aluminum-iron powder in the aluminizing agent accounts for 95 percent, and the ammonium chloride powder accounts for 5 percent; the particle size of the aluminum iron powder (the mass fraction of the iron powder is 45 percent, and the balance is aluminum) is less than 30 meshes; roasting the aluminizing agent for 5 times after the preparation is finished, wherein the roasting temperature is 920 ℃, and the roasting time is 4 hours each time;
(3) embedding aluminizing: filling the prepared aluminizing agent into an aluminizing bag, embedding a single test piece into the roasted aluminizing agent, tamping the aluminizing agent, putting the aluminizing bag into a resistance furnace, heating to 900 ℃, and preserving heat for 5 hours, wherein the thickness of the aluminizing agent on the upper surface and the lower surface of the test piece in the aluminizing bag is 75mm, and the rest embedding operations are the same as those in the embodiment 1;
(4) liquid sand blowing: after aluminizing is finished, cooling the temperature in the furnace to room temperature, taking out the test piece, blowing sand to clean the surface of the test piece, and removing surface attachments;
(5) atmospheric pre-oxidation: and drying the test piece, placing the test piece in an air furnace, preserving the heat for 4 hours at 850 ℃, and then air-cooling.
The depth of the aluminized layer of the sample subjected to aluminizing and pre-oxidation is 0.02 mm-0.04 mm, an alumina film with the thickness of 0.5 mu m-2 mu m is formed on the surface of the sample, a surface layer is coated on the surface of the alumina barrier layer of the sample, and the surface of the sample subjected to a heat resistance test at 900 ℃ for 300 hours has no obvious color change, no scratch, no wrinkle, no bubbling, no cracking, no peeling, no mutual diffusion between the base material and the surface layer and the like.
The technical idea of the present invention is described in the above technical solutions, and the protection scope of the present invention is not limited thereto, and any changes and modifications made to the above technical solutions according to the technical essence of the present invention belong to the protection scope of the technical solutions of the present invention.
Claims (9)
1. A method for preparing a diffusion barrier layer by embedding aluminizing-preoxidation is characterized by comprising the following steps:
(1) preparing an aluminizing agent: preparing an aluminizing agent from aluminum iron powder and ammonium chloride powder according to the following mass percentage, wherein the aluminum iron powder accounts for 95-98% of the aluminizing agent, and the balance is ammonium chloride powder;
(2) embedding aluminizing: embedding the test piece into an aluminizing agent for aluminizing treatment, wherein the aluminizing temperature is 870-950 ℃, and the heat preservation time is 2-8 hours;
(3) a pre-oxidation procedure: and carrying out high-temperature preoxidation treatment on the aluminized test piece to generate an alumina film layer on the aluminized layer surface of the test piece to be used as a diffusion barrier layer.
2. The method for preparing a diffusion barrier layer by pack cementation-preoxidation as claimed in claim 1 wherein the particle size of the ferro-aluminum powder in step (1) is less than 30 mesh, wherein the mass fraction of the ferro-aluminum powder is 42-50%, and the balance is aluminum.
3. The method for preparing a diffusion barrier layer by embedding aluminizing-preoxidation according to claim 1, wherein the aluminizing agent used in the aluminizing cavity in the step (1) is roasted at least five times; the temperature of the roasting process is 920-980 ℃, and the roasting time is 2-4 h.
4. The method for preparing a diffusion barrier layer by pack aluminizing-preoxidation according to claim 1, wherein in the step (2), when the single specimen or the single-layer specimen in the step (2) is pack aluminized, the thickness of the aluminizing agent above and below the specimen is 60 to 80mm, and when the multi-layer specimen is pack aluminized, the thickness of the aluminizing agent above the uppermost specimen and below the lowermost specimen is 60 to 80 mm.
5. The method for preparing the diffusion barrier layer by pack aluminizing-preoxidation according to claim 1, wherein when a plurality of test pieces are aluminized in the step (2), the distance between the test pieces is not less than 15mm, and the distance between the test pieces and the aluminized bag wall is not less than 20 mm.
6. The method for preparing a diffusion barrier layer by pack aluminizing-preoxidation according to claim 1, wherein the thickness of the interlayer aluminizing agent is 30mm to 50mm when the multilayer test piece is aluminized in the step (2).
7. The method for preparing a diffusion barrier layer by pack cementation-preoxidation as claimed in claim 1, wherein the high temperature preoxidation treatment in step (3) comprises two modes of vacuum preoxidation or atmospheric preoxidation:
vacuum pre-oxidation: placing the test piece in a vacuum furnace, preserving heat for 1-4 h at 900-1070 ℃, and then filling argon for cooling;
atmospheric pre-oxidation: and (3) placing the test piece in an air furnace, preserving the heat for 3-6 h at 760-950 ℃, and then air cooling.
8. The method for preparing a diffusion barrier layer by embedding aluminizing-preoxidation according to claim 1, wherein during the vacuum preoxidation in the step (3), the vacuum pressure is controlled to be 100-220 Pa during the temperature rise and heat preservation process at the temperature of more than 800 ℃.
9. The method for preparing a diffusion barrier layer by pack aluminizing-preoxidation according to claim 1, wherein the test piece in the step (2) is pretreated to remove oxides and dirt on the surface of the test piece before the pack aluminizing process is carried out, and sand blasting is carried out to clean the surface of the test piece after aluminizing to remove attachments on the surface of the test piece before the preoxidation process in the step (3).
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Cited By (1)
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CN114622156A (en) * | 2022-03-01 | 2022-06-14 | 中国原子能科学研究院 | Stainless steel surface composite coating and preparation method thereof |
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