CN112708916B - Method for improving surface quality of super-hard aluminum alloy part after sulfuric acid anodization - Google Patents
Method for improving surface quality of super-hard aluminum alloy part after sulfuric acid anodization Download PDFInfo
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- CN112708916B CN112708916B CN202011420064.9A CN202011420064A CN112708916B CN 112708916 B CN112708916 B CN 112708916B CN 202011420064 A CN202011420064 A CN 202011420064A CN 112708916 B CN112708916 B CN 112708916B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/16—Pretreatment, e.g. desmutting
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- 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
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
- C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
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Abstract
The invention discloses a method for improving the surface quality of an ultra-hard aluminum alloy after sulfuric acid anodization; the method comprises the following steps: A. selecting a superhard aluminum alloy with a heat treatment state being an annealing state, and reserving the rest for rough machining; B. then carrying out 460-475 ℃ solution treatment, wherein the heat preservation time is determined according to the thickness of the material, then cooling to room temperature by water, and the requirement of the solution transfer time is less than 15 s; C. carrying out complete artificial aging treatment, wherein the artificial aging temperature is 135-145 ℃, and the heat preservation is carried out for 8-16 h, wherein the time interval between solid solution and artificial aging is less than 4(h) or more than 48 (h); D. then finish machining is carried out to ensure that the size is in place; E. then carrying out surface treatment of sulfuric acid anodic oxidation; F. and (5) checking the dimension and appearance quality after surface treatment. The method can ensure that the surface of the part is bright silvery white after the super-hard aluminum alloy product is subjected to the anodic oxidation by the natural-color sulfuric acid, and an oxidation film after the surface treatment has good integrity and has no obvious black spots and miscellaneous stripes. The surface quality of the part is greatly improved.
Description
Technical Field
The invention belongs to the technical field of metal material processing, heat treatment and surface treatment, and relates to a method for improving the surface quality of an ultra-hard aluminum alloy part after sulfuric acid anodization; in particular to a method for improving the surface quality of an Al-Zn-Mg-Cu series superhard aluminum alloy part after sulfuric acid anodization.
Background
The super hard aluminum is mainly 7A04 and 7A09 alloys of Al-Zn-Mg-Cu series, and belongs to aluminum alloy capable of being strengthened by heat treatment. The strength is higher in the existing aluminum alloy, and the tensile strength can reach 510 MPa-530 MPa. The composite material is mainly used as an important stressed member in aviation and aerospace products. However, these alloys have low plasticity, high notch sensitivity and stress corrosion sensitivity in the solid solution and fully artificially aged state, and require surface treatment to reduce the corrosion effect of the parts. The surface treatment measure adopted by the aluminum alloy is to carry out sulfuric acid anodizing on Al/Et.A (S) S, but after the surface treatment of sulfuric acid anodizing on the aluminum alloy, the surface of a part has obvious stripe and dot stripes, and the whole color is changed from bright silvery white to dark grayish black, so that the delivery quality of the product is influenced.
Therefore, the development of a reasonable, effective and feasible process method and the process method for remarkably improving the surface quality of the super-hard aluminum alloy part after sulfuric acid anodization have important significance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for improving the surface quality of the super-hard aluminum alloy after being anodized by sulfuric acid.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for improving the surface quality of an ultra-hard aluminum alloy part after sulfuric acid anodization, which comprises the following steps:
A. selecting a superhard aluminum alloy part in a specific heat treatment state, and reserving the rest for rough machining;
B. carrying out solution treatment on the roughly processed part, and then cooling the part to room temperature by water, wherein the requirement on the solution transfer time is less than 15 s;
C. carrying out complete artificial aging treatment on the part subjected to solid solution;
D. performing finish machining on the part subjected to the artificial aging treatment;
E. and carrying out sulfuric acid anodic oxidation surface treatment on the finished parts.
As an embodiment of the present invention, in the step a, the specific heat treatment state is an O (annealed) state.
In step B, the rough machined part is subjected to solution treatment in an air circulating furnace.
In the step B, the solid solution temperature is 460-475 ℃, and the holding time is determined according to the thickness of the material.
As an embodiment of the present invention, the incubation time is:
| thickness of material mm | Holding time min |
| 2.0～3.0 | 15～30 |
| 3.0～5.0 | 20～45 |
| 5.0～10.0 | 30～50 |
| 0.0～20.0 | 35～55 |
| 20.0～30.0 | 40～60 |
| 30.0～50.0 | 60～120 |
| 50.0～75.0 | 120～180 |
| 75.0～100.0 | 180～240 |
| 100.0～150.0 | 240～300 |
。
In one embodiment of the invention, in the step C, the time interval between the solution treatment and the artificial aging treatment is <4h or >48 h.
In the step C, the temperature of the artificial aging is 135-145 ℃, and the heat preservation time is 8-16 hours.
As an embodiment of the present invention, the step E further includes a step of checking the size and appearance quality after the surface treatment.
As an embodiment of the present invention, the super hard aluminum alloy is an Al-Zn-Mg-Cu series super hard aluminum alloy.
The traditional solid solution aging is carried out at the stage of a part blank, the main purpose of the traditional solid solution aging is to improve the strength and the hardness of a material, and a heat treatment mode of stress relief annealing is mainly used after rough machining to remove machining stress. The purpose of the surface treatment is mainly to protect the material from oxidation corrosion caused by contact with foreign substances, and the two are not necessarily related to each other. According to the invention, after the solution aging is applied to the rough machining of the part, the traditional stress relief annealing treatment is replaced, so that the strength of the final state of the part is ensured to meet the requirement, and the adverse effect on the part caused by the solution aging treatment is reduced. That is, through the process flow of the invention, the strength and hardness of the material after the solid solution aging treatment can be achieved, meanwhile, the harm caused by the solid solution aging treatment is reduced, and the surface quality of the material after the anode oxidation is improved.
In addition, the invention needs to improve the surface performance of the material after sulfuric acid anodizing. The aim of the solution aging treatment is to improve the strength and hardness of the material, but the processing of parts is affected, so that the surface quality of the aluminum alloy after anodic oxidation is poor. The process flow specified by the invention can not only meet the strength requirement of the material, but also improve the surface performance of the material.
Specifically, compared with the prior art, the invention has the following beneficial effects:
1) according to the invention, the O (annealed) state superhard aluminum alloy is adopted to replace the traditional T6 state as a blank material for processing, the internal structure of the material is optimized, the grain refinement is facilitated, the internal defects of the raw material are reduced, the possibility of processing cracking caused by cracks generated by internal stress of the material in the rough machining process is reduced, the material strength is reduced, the plasticity of the material is improved, the part is easier to cut and process, and the tool wear is reduced;
2) the invention adopts a heat treatment mode of solid solution-artificial aging to replace the traditional heat treatment mode of stress relief, ensures that the strengthening phase of the superhard aluminum alloy is fully solid-dissolved, simultaneously eliminates the processing stress generated in mechanical processing, and meets the requirement of the use strength and hardness;
3) after the superhard aluminum alloy product is subjected to anodic oxidation by the natural-color sulfuric acid, the surface of the part is bright silvery white, and no obvious black spots or mottles are generated; the integrity of the oxide film is good, and the thickness of the film layer is about 7-8 mu m; only normal uniform punctiform pits exist on the surface of the part under observation in a microscopic state, and no obvious large-size corrosion pits exist; parts processed by the traditional process method are dark black, and black stripes exist on the surfaces of the parts; part of the oxide film is corroded to the inside of the matrix, and the thickness of the film layer is about 3-4 mu m; observing the existence of obvious large-size corrosion pits on the surface of the part under a microscopic state; therefore, the process method has remarkable advantages.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a flow chart of a method of machining an ultrahard aluminum alloy part;
FIG. 2 is a specimen sampling position;
FIG. 3 is a plot of the macro topography of the surface treated test pieces 7A04 of example 1 and comparative example 1, where the (right) sample labeled S is example 1 and the (left) sample labeled D is comparative example 1;
FIG. 4 is a plot of the macro topography of the surface treated test pieces 7A09 of example 2 and comparative example 2, where the sample labeled S (right) is example 3 and the sample labeled D (left) is comparative example 2;
FIG. 5 is a surface microtopography photograph of the test piece of example 1; wherein (a) is 200 μm, (b) is 30 μm;
FIG. 6 is a cross-sectional microscopic morphology photograph of a test piece of example 1;
FIG. 7 is a surface microtopography photograph of the test piece of comparative example 1; wherein (a) is 200 μm, (b) is 30 μm;
FIG. 8 is a cross-sectional microscopic morphology photograph of the test piece of comparative example 1;
FIG. 9 is a surface microtopography photograph of the test piece of example 2; wherein (a) is 200 μm, (b) is 30 μm;
FIG. 10 is a cross-sectional microtopography photograph of the test piece of example 2;
FIG. 11 is a surface microtopography photograph of the test piece of comparative example 2; wherein (a) is 200 μm, (b) is 30 μm;
FIG. 12 is a cross-sectional microscopic morphology photograph of the test piece of comparative example 2.
Detailed Description
The present invention will be described in detail with reference to examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be apparent to those skilled in the art that several modifications and improvements can be made without departing from the inventive concept. All falling within the scope of the present invention. The test methods described in the following examples are conventional methods unless otherwise specified. The reagents and materials are commercially available, unless otherwise specified.
In the following examples, the holding time for the solution treatment step is determined based on the thickness of the material, and the specific examples of the present invention are described above. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
TABLE 1 aluminium alloy solid solution heat preservation time table
Example 1
1) Test piece material
Material designation: 7A04, material heat treatment state: o, test piece blank size: 55mm by 55 mm.
2) Scheme flow
Taking a test piece, rough machining, solution treatment, complete artificial aging, finish machining, surface treatment (Al/Et.A (S) S), and inspecting (size, appearance and microscopic appearance); as in fig. 1.
3) Parameters of heat treatment process
TABLE 2 Heat treatment Process parameters Table for example 1
Wherein: the time interval between the solution treatment and the artificial aging treatment is 50 h.
4) Macroscopic and microscopic morphology
The macro topography of the test piece of this example after the sulfuric acid anodizing surface treatment is shown by a mark S in fig. 3, the sampling position of the test piece is shown in fig. 2, the surface micro-topography is shown in fig. 5, and the cross-sectional micro-topography is shown in fig. 6.
Comparative example 1
1) Test piece material
Material designation: 7A04, material heat treatment state: t6, test piece blank size: 55mm by 55 mm.
2) Scheme flow
Taking a test piece, rough machining, stress relief treatment, finish machining, surface treatment (Al/Et.A (S). S), and checking (size, appearance and microscopic morphology).
3) Parameters of heat treatment process
Table 3, heat treatment process parameter table of comparative example 1
4) Macroscopic and microscopic morphology
The macro-morphology of the test piece of the present comparative example after the sulfuric acid anodizing surface treatment is shown by a mark D in fig. 3, the surface micro-morphology is shown in fig. 7, and the cross-sectional micro-morphology is shown in fig. 8.
In this comparative example, it should be noted that the preparation method of the green stock of the T6 temper is not suitable for solution aging to be performed many times, so it corresponds to the conventional preparation process of the subsequent parts (i.e. the processing scheme of this comparative example).
Example 2
1) Test piece material
Material designation: 7A09, material heat treatment state: o, test piece blank size: 55mm by 55 mm.
2) Scheme flow
Taking a test piece, rough machining, solution treatment, complete artificial aging, finish machining, surface treatment (Al/Et.A (S) S), and inspecting (size, appearance and microscopic morphology).
3) Parameters of heat treatment process
TABLE 4 Heat treatment process parameter Table of example 2
Wherein: the time interval between the solution treatment and the artificial aging treatment is 50 h.
4) Macroscopic and microscopic morphology
The macro topography of the test piece of this example after the sulfuric acid anodizing surface treatment is shown as a mark S in fig. 4, the surface micro-topography is shown as fig. 9, and the cross-sectional micro-topography is shown as fig. 10.
Comparative example 2
1) Test piece material
Material designation: 7A09, material heat treatment state: t6, test piece blank size: 55mm by 55 mm.
2) Scheme flow
Taking a test piece, rough machining, stress relief treatment, finish machining, surface treatment (Al/Et.A (S). S), and checking (size, appearance and microscopic morphology).
3) Parameters of heat treatment process
Table 5, heat treatment process parameter table of comparative example 2
4) Macroscopic and microscopic morphology
The macro-morphology of the test piece of this comparative example after the sulfuric acid anodizing surface treatment is shown by a mark D in fig. 4, the surface micro-morphology is shown in fig. 11, and the cross-sectional micro-morphology is shown in fig. 12.
In the above examples and comparative examples, two grades of superhard aluminum alloy are adopted, two blanks are in heat treatment state, after rough machining, different heat treatment methods are carried out, and the test is carried out on the part formed by finish machining, and the obtained macro morphology and the micro morphology are compared. Further clarifies that the process method of the invention has the best effect of improving the surface quality of the super-hard aluminum alloy after being anodized by sulfuric acid.
Comparing fig. 3 and fig. 4, the superhard aluminum alloy test pieces of example 1 and example 3 using the process of the present invention still have silvery white appearance, glossy surface and no black spots after sulfuric acid anodizing, while the superhard aluminum alloy test pieces of comparative example 1 and comparative example 2 using the conventional process have dull black color after sulfuric acid anodizing, wherein the surface of the test piece of comparative example 1 even has a large number of black stripes. Therefore, the invention can improve the appearance performance of the ultra-hard aluminum alloy after surface treatment and meet the requirement of part processing.
Comparing fig. 5 and 9 with fig. 7 and 11, it can be seen that the black dot-shaped pits exist on the surface of the oxide film of the test piece adopting various process schemes under microscopic conditions, but the size of the pits on the surface of the test piece adopting the process method of the present invention is obviously smaller than that of the test piece adopting the conventional process method, and the number of the pits is also obviously reduced. Therefore, the invention can reduce the number of pits on the surface of the superhard aluminum alloy and optimize the quality of the pits.
Comparing fig. 6, 10 with fig. 8, 12, it can be seen that the oxide film on the surface of the test piece of the process of the present invention is more complete and continuous and has uniform thickness, wherein the oxide film thickness of example 1 is about 7.5 μm-8.0 μm, and the oxide film thickness of example 2 is about 7.9 μm-8.2 μm, while the oxide film on the surface of the test piece of the conventional process has corroded into the substrate, and the thickness of the oxide film at this position is thinner than that of the normal region, wherein the oxide film thickness of comparative example 1 is about 4.1 μm-4.3 μm, and the oxide film thickness of comparative example 2 is about 2.3 μm-3.6 μm, so that the present invention can ensure the integrity of the oxide film, and at the same time, the thickness of the oxide film is properly increased.
Compared with the superhard aluminum alloy part prepared by the traditional process method, the superhard aluminum alloy part prepared by the process method has the advantages that the surface quality of the part is obviously improved after the part is anodized by sulfuric acid, the integrity of an oxidation film is ensured, the aesthetic property of the part is improved, and the surface corrosion resistance is improved.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (4)
1. A method of improving the surface quality of a superhard aluminum alloy part after sulfuric acid anodization, the method comprising the steps of:
A. selecting an Al-Zn-Mg-Cu series superhard aluminum alloy part with an annealing state as a heat treatment state, and reserving the rest for rough machining;
B. carrying out solid solution treatment on the rough-machined part, wherein the solid solution temperature is 460-475 ℃, the heat preservation time is determined according to the thickness of the material, then, cooling the part to room temperature by water, and the requirement on the solid solution transfer time is less than 15 s;
C. carrying out complete artificial aging treatment on the part subjected to solid solution; the time interval between the solid solution treatment and the artificial aging treatment is less than 4 hours or more than 48 hours, the temperature of the artificial aging treatment is 135-145 ℃, and the heat preservation time is 8-16 hours;
D. performing finish machining on the part subjected to the artificial aging treatment;
E. and carrying out sulfuric acid anodic oxidation surface treatment on the finished parts.
2. The method for improving the surface quality of an ultrahard aluminum alloy part after sulfuric acid anodization as recited in claim 1, wherein in the step B, the rough-machined part is subjected to solution treatment in an air circulation furnace.
3. The method of improving the surface quality of a superhard aluminum alloy part after sulfuric acid anodization of claim 1, wherein the holding time is:
。
4. The method for improving the surface quality of a superhard aluminum alloy part after sulfuric acid anodization of claim 1, further comprising a step of checking the dimension and appearance quality after surface treatment after the step E.
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