CN117107192A - Preparation method of GH4698 superalloy surface aluminizing protective coating - Google Patents
Preparation method of GH4698 superalloy surface aluminizing protective coating Download PDFInfo
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- CN117107192A CN117107192A CN202311025688.4A CN202311025688A CN117107192A CN 117107192 A CN117107192 A CN 117107192A CN 202311025688 A CN202311025688 A CN 202311025688A CN 117107192 A CN117107192 A CN 117107192A
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- 238000005269 aluminizing Methods 0.000 title claims abstract description 65
- 229910000601 superalloy Inorganic materials 0.000 title claims abstract description 26
- 239000011253 protective coating Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 76
- 239000000463 material Substances 0.000 claims abstract description 59
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000000843 powder Substances 0.000 claims abstract description 46
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 26
- CYUOWZRAOZFACA-UHFFFAOYSA-N aluminum iron Chemical compound [Al].[Fe] CYUOWZRAOZFACA-UHFFFAOYSA-N 0.000 claims abstract description 25
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 25
- 238000009792 diffusion process Methods 0.000 claims abstract description 25
- 238000000137 annealing Methods 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 21
- 230000000149 penetrating effect Effects 0.000 claims abstract description 21
- 230000003213 activating effect Effects 0.000 claims abstract description 10
- 238000004806 packaging method and process Methods 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- KCZFLPPCFOHPNI-UHFFFAOYSA-N alumane;iron Chemical class [AlH3].[Fe] KCZFLPPCFOHPNI-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000007689 inspection Methods 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims description 32
- 238000001994 activation Methods 0.000 claims description 14
- 230000004913 activation Effects 0.000 claims description 13
- 238000007599 discharging Methods 0.000 claims description 12
- 238000004321 preservation Methods 0.000 claims description 9
- 230000007480 spreading Effects 0.000 claims description 9
- 238000003892 spreading Methods 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 7
- 230000003647 oxidation Effects 0.000 claims description 6
- 238000007254 oxidation reaction Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 230000002045 lasting effect Effects 0.000 claims description 4
- 229910000838 Al alloy Inorganic materials 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 3
- 239000002932 luster Substances 0.000 claims description 3
- 238000005192 partition Methods 0.000 claims description 3
- 230000009467 reduction Effects 0.000 claims description 3
- 238000012856 packing Methods 0.000 claims description 2
- 239000010410 layer Substances 0.000 abstract description 20
- 239000011241 protective layer Substances 0.000 abstract description 4
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical group [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 10
- 229910052782 aluminium Inorganic materials 0.000 description 9
- 239000000956 alloy Substances 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 3
- 239000002344 surface layer Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010587 phase diagram Methods 0.000 description 2
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 229910015372 FeAl Inorganic materials 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
-
- C—CHEMISTRY; METALLURGY
- 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
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
-
- 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
Abstract
A preparation method of a GH4698 superalloy surface aluminizing protective coating comprises the following steps: s1, pretreatment of materials: carrying out standard heat treatment on the GH4698 material and detecting mechanical properties; s2, ammonium chloride drying; s3, activating aluminum iron powder; s4, preparing a penetrating agent: the penetrating agent is formed by uniformly stirring activated aluminum iron powder and 0.5 to 4.0wt.% of activating agent ammonium chloride; s5, packaging; s6, aluminizing: the aluminizing bag is placed into a heating furnace for aluminizing; s7, unpacking; s8, diffusion annealing: placing the GH4698 material after cleaning and drying into a heating furnace for diffusion annealing; s9, quality inspection of aluminizing: the thickness of the aluminized layer is detected by a metallographic method, and the thickness of the aluminized layer is required to be 20-70 mu m. According to the invention, the activating agent ammonium chloride is added into the aluminum-iron powder, and reacts with the aluminum-iron powder to separate out aluminum atoms in a heating state, so that a material is provided for an aluminized layer, and the formation of an aluminized protective layer is quickened.
Description
Technical Field
The invention relates to an aerospace hot end part surface coating and a matrix material mechanical property improvement providing method thereof, in particular to a preparation method of an GH4698 superalloy surface aluminizing protective coating.
Background
The GH4698 superalloy is a novel superalloy formed by improving the content of Al and Ti and reducing the content of Cr on the basis of the GH4033 superalloy. The alloy has high lasting strength and tensile strength in the temperature range of 550-800 ℃ and good plasticity and comprehensive performance, and is widely applied to components such as turbine discs of aeroengines. However, due to the high-temperature oxidation and corrosion effects, an aluminizing protective coating is generally prepared on the surface of the GH4698 material to improve the oxidation resistance and corrosion resistance of the GH4698 material.
The powder embedding method aluminizing is a mature and stable high-temperature coating preparation technology and has the advantages of low equipment requirement, simple operation and low cost. However, in the powder embedding method aluminizing technology, many factors influencing the quality of the aluminized coating, such as aluminizing temperature, time, powder activity and the like, are included. The powder embedding method for aluminizing is to prepare the aluminizing coating at the high temperature of 900-1000 ℃, so that the quantity and distribution state of the organization structure of the GH4698 material are changed, and the mechanical property is reduced.
Disclosure of Invention
The invention mainly aims to provide a preparation method of an GH4698 superalloy surface aluminizing protective coating, which aims to solve the technical problems.
In order to achieve the aim, the invention provides a preparation method of a GH4698 superalloy surface aluminizing protective coating, which comprises the following steps:
s1, pretreatment of materials: carrying out standard heat treatment on the GH4698 material and detecting mechanical properties;
s2, ammonium chloride drying: drying ammonium chloride, grinding into powder, and sieving;
s3, activating treatment of aluminum iron powder: uniformly stirring the sieved aluminum iron powder and the dried ammonium chloride powder, and filling the mixture into an aluminizing bag for activation treatment;
s4, preparing a penetrating agent: the penetrating agent is formed by uniformly stirring activated aluminum iron powder and 0.5 to 4.0wt.% of activating agent ammonium chloride;
s5, packaging: packaging GH4698 material and a penetrating agent to obtain an aluminized package;
s6, aluminizing: the aluminizing bag is placed into a heating furnace for aluminizing;
s7, unpacking: taking out GH4698 material from the aluminized bag, cleaning surface powder, and then drying to ensure that the surface of the material is free of stains and moisture;
s8, diffusion annealing: placing the GH4698 material after cleaning and drying into a heating furnace for diffusion annealing;
s9, quality inspection of aluminizing: the thickness of the aluminized layer is detected by a metallographic method, and the thickness of the aluminized layer is required to be 20-70 mu m.
Preferably, in step S1, the parameters of standard heat treatment of the GH4698 material are: heat preservation is carried out for 8 hours at 1120 ℃, air cooling is carried out to 1000 ℃ and heat preservation is carried out for 4 hours, air cooling is carried out to 775 ℃ and heat preservation is carried out for 16 hours, then air cooling is carried out to room temperature, and the surface to be aluminized is required to have obvious metallic luster after standard heat treatment, and the surface is free from rust, dirt and oxidation.
Preferably, in step S1, the GH4698 material is subjected to standard heat treatment to the desired levelThe mechanical properties are as follows: tensile Strength R at room temperature m Elongation strength R at not less than 1130MPa and non-proportional elongation of 0.2% is specified p0.2 705Mpa, elongation after break A not less than 17%, reduction of area Z not less than 19%, impact energy not less than 40, hardness 3.55-3.30; tensile Strength R at 750 ℃ m The elongation after fracture A is more than or equal to 5 percent, the area shrinkage Z is more than or equal to 8 percent, and the lasting strength sigma is 412Mpa.
Preferably, in step S2, the method for drying ammonium chloride is as follows: drying at 90-160 deg.c for over 1 hr, cooling in air or with furnace, grinding into powder, and sieving with 50-150 mesh sieve.
Preferably, in step S3, the components of the aluminum-iron powder used include:
Fe：40～52wt.％；
Si：≤4.0wt.％；
Mn：≤2.0wt.％；
cu: less than or equal to 6.0wt.%; the balance being Al.
Preferably, in step S3, the unused fine aluminum powder after being sieved by a 50-150 mesh sieve is uniformly stirred with 0.5-2.0 wt.% of dry ammonium chloride powder, and is put into an aluminizing bag for activation treatment, wherein the parameters of the activation treatment are as follows: feeding the materials into a furnace at the temperature of less than or equal to 500 ℃, heating to 500+/-30 ℃ along with the furnace, preserving heat for 1-2 h, heating to 950+/-10 ℃ along with the furnace, preserving heat for 1-4 h, discharging and air cooling to room temperature.
Preferably, in step S5, the method of packaging is as follows: uniformly spreading a layer of penetrating agent on the aluminized ladle bottom, wherein the thickness is more than 40mm, and sequentially placing GH4698 materials on the penetrating agent, wherein the distances between GH4698 materials and the ladle wall are required to be more than 20 mm; spreading a penetrating agent, placing a partition plate above GH4698 material, uniformly spreading aluminum-iron powder with the thickness of not less than 40mm to isolate air, and covering a cover; and (5) vibrating the aluminized bag until no obvious gas is discharged.
Preferably, in step S6, the aluminizing parameters are as follows: feeding the aluminum alloy into a furnace at the temperature of less than or equal to 500 ℃, heating to 500+/-30 ℃ along with the furnace, preserving heat for 1-2 hours, then heating to 850+/-10 ℃ along with the furnace, preserving heat for 1-2 hours, heating to 960+/-10 ℃ along with the furnace, preserving heat for 6-8 hours, and finally discharging from the furnace along with an aluminizing bag for air cooling.
Preferably, in step S8, parameters of diffusion annealing are: feeding the materials into a furnace at the temperature of less than or equal to 1000 ℃, heating the materials to 1000+/-10 ℃ along with the furnace, preserving heat for 3-6 h, and finally discharging the materials from the furnace for air cooling to the room temperature.
Preferably, in step S8, after the diffusion annealing is completed, a heat treatment is performed, and the heat treatment parameters are as follows: charging into furnace at 775 deg.C, heating to 775+ -10 deg.C, maintaining for 12-17 h, air cooling, and detecting mechanical property after heat treatment.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
(1) According to the invention, the activating agent ammonium chloride is added into the aluminum-iron powder, and reacts with the aluminum-iron powder to separate out aluminum atoms in a heating state, so that a material is provided for an aluminized layer, and the formation of an aluminized protective layer is quickened.
(2) In the aluminizing process, the temperature difference in the aluminizing bag is reduced through gradient temperature rise, and the thickness uniformity of the aluminizing protective layer is ensured. Meanwhile, the aluminized coating consists of an outer surface layer and an alloy layer, wherein the outer surface layer mainly consists of aluminum, and the alloy layer mainly consists of an aluminum-iron compound (Fe 2Al5 and the like) with high aluminum content. Pure aluminum has poor corrosion resistance, and aluminum-iron compounds with high aluminum content have high brittleness and are easy to separate from a matrix, so that the use requirement cannot be met. After diffusion, pure aluminum on the outer surface layer forms an Al2O3 film, the aluminum-iron compound with high aluminum content is gradually converted into an aluminum-iron compound with low aluminum content (FeAl, fe3Al and the like), the combination property of the aluminized layer and a matrix is improved, and meanwhile, the oxidation resistance and the corrosion resistance of the aluminized layer are also enhanced.
(3) In the present invention, in step S8, after the diffusion is completed, heat treatment is performed, and the following heat treatment parameters are adopted: charging into a furnace at the temperature of less than or equal to 775 ℃, heating to 775+/-10 ℃ along with the furnace, preserving heat for 12-17 hours, and then air-cooling, so that the GH4698 material after aluminizing can meet the performance index requirements.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to the structures shown in these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram showing the heating curve of the activation treatment of fine aluminum powder
FIG. 2 is a schematic diagram of an aluminizing heating curve;
FIG. 3 is a schematic illustration of a diffusion annealing heating curve;
FIG. 4 is a schematic view of a heating curve of the heat treatment after the diffusion annealing is completed;
FIG. 5 is a phase diagram of a GH4698 superalloy and aluminized layer prepared in accordance with the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The embodiment provides a preparation method of a GH4698 high-temperature alloy surface aluminizing protective coating, which is characterized in that GH4698 alloy materials are embedded in an aluminum-iron alloy penetrating agent, and after high-temperature aluminizing and diffusion annealing, a layer of continuous and uniform aluminum protective layer with the thickness of 20-70 mu m can be formed on the surface of the GH4698 alloy material. Finally, the mechanical properties of the GH4698 superalloy are improved by heat treatment, and the method specifically comprises the following steps:
step S1, pretreatment of materials: carrying out standard heat treatment on the GH4698 material and detecting mechanical properties; the parameters of standard heat treatment are: heat preservation is carried out for 8 hours at 1120 ℃, air cooling is carried out to 1000 ℃ and heat preservation is carried out for 4 hours, air cooling is carried out to 775 ℃ and heat preservation is carried out for 16 hours, then air cooling is carried out to room temperature, and the surface to be aluminized is required to have obvious metallic luster after standard heat treatment, and the surface is free from rust, dirt and oxidation. Specifically, the mechanical properties required to be achieved after the GH4698 material is subjected to standard heat treatment are as follows: at room temperature, the tensile strength Rm is more than or equal to 1130Mpa, the elongation strength Rp0.2 when the non-proportional elongation is 0.2% is 705Mpa, the elongation after fracture A is more than or equal to 17%, the area shrinkage Z is more than or equal to 19%, the impact energy is more than or equal to 40, and the hardness is 3.55-3.30; at 750 ℃, the tensile strength Rm is more than or equal to 740Mpa, the elongation after break A is more than or equal to 5%, the area shrinkage Z is more than or equal to 8%, and the lasting strength sigma is 412Mpa.
Specifically, the standard heat treatment index requirement of the GH4698 superalloy and the mechanical property detection result after standard heat treatment are shown in table 1:
TABLE 1 standard heat treatment index requirement for GH4698 superalloy and mechanical property detection result after standard heat treatment
Step S2, ammonium chloride drying: drying ammonium chloride, grinding into powder, and sieving; specifically, the method for drying ammonium chloride comprises the following steps: drying at 90-160 deg.c for over 1 hr, cooling in air or with furnace, grinding into powder, sieving with 50-150 mesh sieve, and other steps. Preferred specific parameters are: drying ammonium chloride at 100deg.C for 2 hr, discharging, air cooling or cooling with furnace, cooling to room temperature, grinding into powder, and sieving with 80 mesh sieve.
Step S3, activating treatment of aluminum iron powder: uniformly stirring the sieved aluminum iron powder and the dried ammonium chloride powder, and filling the mixture into an aluminizing bag for activation treatment. Specifically, the unused aluminum iron powder after being sieved by a 50-150-mesh sieve is uniformly stirred with 0.5-2.0 wt.% of dry ammonium chloride powder, and is filled into an aluminizing bag for activation treatment, wherein the parameters of the activation treatment are as follows: feeding the materials into a furnace at the temperature of less than or equal to 500 ℃, heating to 500+/-30 ℃ along with the furnace, preserving heat for 1-2 h, heating to 950+/-10 ℃ along with the furnace, preserving heat for 1-4 h, discharging and air cooling to room temperature. The activation treatment heating curve of the fine aluminum iron powder is shown in fig. 1.
In step S3, the composition of the aluminum-iron powder used includes the following table:
| element(s) | Fe | Si | Mn | Cu | Al |
| Content/wt.% | 40～52 | ≤4.0 | ≤2.0 | ≤6.0 | Allowance of |
In this embodiment, specific parameters of the activation process are: the unused aluminum iron powder sieved by a 80-mesh sieve and 1.0wt.% of dry ammonium chloride powder are uniformly stirred, are filled into an aluminizing bag and are subjected to activation treatment, when in activation treatment, are put into a furnace at 400 ℃, are heated to 500 ℃ along with the furnace, are kept for 1.5 hours, are heated to 950 ℃ along with the furnace, are kept for 2.5 hours, and are discharged from the furnace and are air-cooled to room temperature.
Step S4, preparing a penetrating agent: the penetrating agent is formed by uniformly stirring activated aluminum iron powder and 0.5 to 4.0wt.% of activating agent ammonium chloride; specifically, the activator ammonium chloride specific gravity was 1.5wt.%.
S5, packaging: packaging GH4698 material and a penetrating agent to obtain an aluminized package; the specific packing method comprises the following steps: uniformly spreading a layer of penetrating agent on the aluminized ladle bottom, wherein the thickness is more than 40mm, and sequentially placing GH4698 materials on the penetrating agent, wherein the distances between GH4698 materials and the ladle wall are required to be more than 20 mm; spreading a penetrating agent, placing a partition plate above GH4698 material, uniformly spreading aluminum-iron powder with the thickness of not less than 40mm to isolate air, and covering a cover; and (5) vibrating the aluminized bag until no obvious gas is discharged. In this example, specific parameters were chosen such that the thickness of the infiltrant was chosen to be 50mm and the distance between the GH4698 materials and the containment wall was chosen to be 30mm.
S6, aluminizing: the aluminizing bag is placed into a heating furnace for aluminizing; the aluminizing parameters were as follows: feeding the aluminum alloy into a furnace at the temperature of less than or equal to 500 ℃, heating to 500+/-30 ℃ along with the furnace, preserving heat for 1-2 hours, then heating to 850+/-10 ℃ along with the furnace, preserving heat for 1-2 hours, heating to 960+/-10 ℃ along with the furnace, preserving heat for 6-8 hours, and finally discharging from the furnace along with an aluminizing bag for air cooling. The aluminizing heating curve is shown in fig. 2.
In this embodiment, specific parameters for aluminizing are selected as follows: 450 ℃ is put into a furnace, the temperature is raised to 500 ℃ along with the furnace, the heat is preserved for 1.5 hours, then the temperature is raised to 850 ℃ along with the furnace, the heat is preserved for 1.5 hours, and then the temperature is raised to 960 ℃ along with the furnace, and the heat is preserved for 6 hours and 20 minutes. Finally discharging the aluminum-impregnated bag from the furnace for air cooling.
Step S7, unpacking: and taking out the GH4698 material from the aluminized bag, cleaning the surface powder, and then drying to ensure that the surface of the material is free of stains and moisture.
Step S8, diffusion annealing: placing the GH4698 material after cleaning and drying into a heating furnace for diffusion annealing, wherein the parameters of the diffusion annealing are as follows: feeding the materials into a furnace at the temperature of less than or equal to 1000 ℃, heating the materials to 1000+/-10 ℃ along with the furnace, preserving heat for 3-6 h, and finally discharging the materials from the furnace for air cooling to the room temperature. The diffusion annealing heating curve is shown in fig. 3. After the diffusion annealing is finished, heat treatment is carried out, and the heat treatment parameters are as follows: charging into furnace at 775 deg.C, heating to 775+ -10 deg.C, preserving heat for 12-17 h, and air cooling. The heat treatment heating curve is shown in fig. 4.
Specifically, in this embodiment, specific parameters of diffusion annealing are selected as follows: and (5) feeding the materials into a furnace at 950 ℃, heating to 1000 ℃ along with the furnace, preserving heat for 4 hours, and finally discharging and air cooling. The specific parameters of the heat treatment are selected as follows: feeding the materials into a furnace at 200 ℃, heating the materials to 775 ℃ along with the furnace, preserving heat for 16h, and then air-cooling.
In this step, the heat treatment is provided for the purpose of improving the mechanical properties of the GH4698 material after aluminizing, diffusion annealing.
S9, quality inspection of aluminizing: checking the aluminizing quality, wherein the surface of the GH4698 aluminizing layer has no corrosion pit, adhesive, oxide skin, protrusion or peeling of the aluminizing layer, and the thickness of the aluminizing layer is detected by adopting a metallographic method, and the thickness of the aluminizing layer is required to be 20-70 mu m. Specifically, in this example, the aluminized layer obtained by detection has a thickness of 40 μm, and the gold phase diagram of the GH4698 superalloy aluminized layer is shown in FIG. 5.
In this example, mechanical properties of GH4698 high-temperature alloy materials subjected to aluminizing and diffusion annealing were measured, and the results are shown in Table 2, in which the tensile strength, reduction of area, and hardness of high-temperature stretching do not meet the index requirements.
TABLE 2 mechanical property test results of GH4698 superalloy after aluminizing and diffusion annealing treatment
After diffusion annealing, the material is put into a furnace at 200 ℃, is heated to 775 ℃ along with the furnace, is preserved for 16 hours, is subjected to air cooling heat treatment, and is subjected to mechanical property detection, and the results are shown in table 3, wherein all indexes meet the requirements.
TABLE 3 mechanical property test results of GH4698 superalloy after heat treatment
The foregoing description is only of the preferred embodiments of the present invention, and is not intended to limit the scope of the invention, but rather, the equivalent structural changes made by the description of the present invention and the accompanying drawings or the direct/indirect application in other related technical fields are included in the scope of the invention.
Claims (10)
1. The preparation method of the GH4698 superalloy surface aluminizing protective coating is characterized by comprising the following steps:
s1, pretreatment of materials: carrying out standard heat treatment on the GH4698 material and detecting mechanical properties;
s2, ammonium chloride drying: drying ammonium chloride, grinding into powder, and sieving;
s3, activating treatment of aluminum iron powder: uniformly stirring the sieved aluminum iron powder and the dried ammonium chloride powder, and filling the mixture into an aluminizing bag for activation treatment;
s4, preparing a penetrating agent: the penetrating agent is formed by uniformly stirring activated aluminum iron powder and 0.5 to 4.0wt.% of activating agent ammonium chloride;
s5, packaging: packaging GH4698 material and a penetrating agent to obtain an aluminized package;
s6, aluminizing: the aluminizing bag is placed into a heating furnace for aluminizing;
s7, unpacking: taking out GH4698 material from the aluminized bag, cleaning surface powder, and then drying to ensure that the surface of the material is free of stains and moisture;
s8, diffusion annealing: placing the GH4698 material after cleaning and drying into a heating furnace for diffusion annealing;
s9, quality inspection of aluminizing: the thickness of the aluminized layer is detected by a metallographic method, and the thickness of the aluminized layer is required to be 20-70 mu m.
2. The method for preparing the GH4698 superalloy surface aluminizing protective coating according to claim 1, wherein in step S1, the parameters of standard heat treatment of the GH4698 material are: heat preservation is carried out for 8 hours at 1120 ℃, air cooling is carried out to 1000 ℃ and heat preservation is carried out for 4 hours, air cooling is carried out to 775 ℃ and heat preservation is carried out for 16 hours, then air cooling is carried out to room temperature, and the surface to be aluminized is required to have obvious metallic luster after standard heat treatment, and the surface is free from rust, dirt and oxidation.
3. The method for preparing an aluminum-impregnated protective coating on a GH4698 superalloy surface as defined in claim 1, wherein in step S1, the GH4698 material is subjected to standard heat treatment to achieve mechanical propertiesThe method comprises the following steps: tensile Strength R at room temperature m Elongation strength R at not less than 1130MPa and non-proportional elongation of 0.2% is specified p0.2 705Mpa, elongation after break A not less than 17%, reduction of area Z not less than 19%, impact energy not less than 40, hardness 3.55-3.30;
tensile Strength R at 750 ℃ m The elongation after fracture A is more than or equal to 5 percent, the area shrinkage Z is more than or equal to 8 percent, and the lasting strength sigma is 412Mpa.
4. The method for preparing the GH4698 superalloy surface aluminizing protective coating according to claim 1, wherein in step S2, the method for drying ammonium chloride is as follows: drying at 90-160 deg.c for over 1 hr, cooling in air or with furnace, grinding into powder, and sieving with 50-150 mesh sieve.
5. The method for preparing the GH4698 superalloy surface aluminizing protective coating according to claim 1, wherein in step S3, the composition of the aluminum-iron powder used comprises:
Fe：40～52wt.％；
Si：≤4.0wt.％；
Mn：≤2.0wt.％；
cu: less than or equal to 6.0wt.%; the balance being Al.
6. The method for preparing the aluminum-impregnated protective coating on the surface of the GH4698 superalloy as claimed in claim 1, wherein in the step S3, unused aluminum iron powder screened by a 50-150 mesh sieve is uniformly stirred with 0.5-2.0 wt.% of dry ammonium chloride powder, and the aluminum-impregnated protective coating is put into an aluminum-impregnated bag for activation treatment, wherein the parameters of the activation treatment are as follows: feeding the materials into a furnace at the temperature of less than or equal to 500 ℃, heating to 500+/-30 ℃ along with the furnace, preserving heat for 1-2 h, heating to 950+/-10 ℃ along with the furnace, preserving heat for 1-4 h, discharging and air cooling to room temperature.
7. The method for preparing the GH4698 superalloy surface aluminizing protective coating according to claim 1, wherein in step S5, the packing method is as follows: uniformly spreading a layer of penetrating agent on the aluminized ladle bottom, wherein the thickness is more than 40mm, and sequentially placing GH4698 materials on the penetrating agent, wherein the distances between GH4698 materials and the ladle wall are required to be more than 20 mm; spreading a penetrating agent, placing a partition plate above GH4698 material, uniformly spreading aluminum-iron powder with the thickness of not less than 40mm to isolate air, and covering a cover; and (5) vibrating the aluminized bag until no obvious gas is discharged.
8. The method for preparing the GH4698 superalloy surface aluminizing protective coating according to claim 1, wherein in step S6, the aluminizing parameters are as follows: feeding the aluminum alloy into a furnace at the temperature of less than or equal to 500 ℃, heating to 500+/-30 ℃ along with the furnace, preserving heat for 1-2 hours, then heating to 850+/-10 ℃ along with the furnace, preserving heat for 1-2 hours, heating to 960+/-10 ℃ along with the furnace, preserving heat for 6-8 hours, and finally discharging from the furnace along with an aluminizing bag for air cooling.
9. The method for preparing a protective coating for surface aluminizing of a GH4698 superalloy as in claim 1, wherein in step S8, the parameters of diffusion annealing are: feeding the materials into a furnace at the temperature of less than or equal to 1000 ℃, heating the materials to (1000+/-10) DEG C along with the furnace, preserving the heat for 3-6 h, and finally discharging the materials from the furnace for air cooling to the room temperature.
10. The method for preparing the GH4698 superalloy surface aluminizing protective coating according to claim 1, wherein in step S8, after the diffusion annealing is finished, heat treatment is performed, and the heat treatment parameters are as follows: charging into furnace at 775 deg.C, heating to 775+ -10 deg.C, maintaining for 12-17 h, air cooling, and detecting mechanical property after heat treatment.
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