CN111893538A - Hard anodizing process method for 3D printing forming AlSi10Mg aluminum alloy material - Google Patents
Hard anodizing process method for 3D printing forming AlSi10Mg aluminum alloy material Download PDFInfo
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- CN111893538A CN111893538A CN202010626089.8A CN202010626089A CN111893538A CN 111893538 A CN111893538 A CN 111893538A CN 202010626089 A CN202010626089 A CN 202010626089A CN 111893538 A CN111893538 A CN 111893538A
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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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- 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
- C25D11/024—Anodisation under pulsed or modulated current or potential
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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
- C25D11/10—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing organic acids
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The invention relates to the technical field of metal surface treatment protection engineering, in particular to a hard anodizing process method for a 3D printing forming AlSi10Mg aluminum alloy material. The formula of the bath solution is improved, the indexes of film thickness, hardness and wear resistance are improved, the part meets the requirement of a hard anodizing process, and the problem that the electrochemical dissolution is aggravated in the film forming process due to the fact that the conductivity is obviously influenced and the local current density is overlarge in the treatment process of an aluminum alloy workpiece containing high silicon and magnesium in the conventional hard anodizing process is solved. The hard anodization process is carried out by selecting a sulfuric acid + functional organic acid process, the thickness of the formed anodized film layer can reach more than 30 micrometers, the hardness of the film layer reaches 340HV, the optimized hard anodization process is adopted for 3D printing of AlSi10Mg aluminum alloy parts, the process stability is good, the film forming efficiency is high, the actual film layer thickness is more than 30 micrometers, the film layer hardness reaches 340HV, and the traditional hard anodization performance is completely met.
Description
Technical Field
The invention relates to the technical field of metal surface treatment protection engineering, in particular to a hard anodizing process method for a 3D printing forming AlSi10Mg aluminum alloy material.
Background
In the traditional hard anodizing process, because the bath solution has simple components and the process is stable and mature, a layer of oxide film with good wear resistance, electrical insulation, corrosion resistance and heat resistance is obtained on the surface. Has little influence on the fatigue performance of the aluminum alloy material. The corrosion resistance of the film is good, and the like, and the film is widely applied to aerospace, aviation and navy parts.
The metal structure is a 3D printed (selective laser melting forming) AlSi10Mg aluminum alloy product, and as the selective laser melting forming (SLM) is a rapid melting and rapid solidification process, the spot diameter of laser is very small (0.1mm), a small molten pool is generated in the forming process, and the cooling rate of the molten pool is high, so that the material can obtain an ultrafine eutectic structure in the SLM forming process. The size of the alpha-Al matrix phase reaches the micron level, the size of the granular Si reaches the nanometer level, and the structure of the alpha-Al matrix phase is greatly different from that of common wrought aluminum alloys and cast aluminum alloys, so that the electrochemical behavior in the anodization film forming process has certain specificity. The conventional hard anodizing process needs to be improved.
The process aims at solving the problem that the electrochemical dissolution is aggravated in the film forming process due to the fact that the conductivity is obviously influenced in the processing process of the aluminum alloy workpiece with high silicon and magnesium contents and the local current density is overlarge in the conventional hard anodization process. The alloy can be successfully applied to military product parts of aerospace, aviation, navy and the like.
Disclosure of Invention
The invention is characterized in that the traditional hard anodization process is improved to be suitable for 3D printing (selective laser melting forming) AlSi10Mg aluminum alloy workpieces, sulfuric acid solution is selected as basic solution, proper additives are added to improve bath solution components, and low-temperature process is adopted to improve processing performance, so that the 3D printing AlSi10Mg aluminum alloy workpieces with superfine eutectic structures can more easily form an anodized film layer.
The process is characterized in that the wear resistance and the thickness of the film layer meet the requirements, the subsequent machining process can be carried out, and the process is suitable for parts with high requirements on wear resistance and dimensional accuracy.
Technical scheme
The hard anodizing process for the 3D printing forming AlSi10Mg aluminum alloy material comprises the following steps of:
(1) removing oil by using a weak base water-based solvent;
1/3 volumes of deionized water were added to the tank, and 21g/L of Na was added in that order3PO42.5g/L of C6H15O3N, 3.1g/L Na2B4O710H2And after the O is completely dissolved, adding deionized water to the liquid level height, and heating to 55 ℃.
(2) Washing with water;
(3) acid deoxidation; washing with water
(4)3D printing (selective laser melting forming) AlSi10Mg aluminum alloy hard anodizing process method:
1/3 volumes of deionized water were added to the tank, and H was slowly added to the tank2SO4Deionized water was added to 2/3 volumes and the compressed air was turned on and stirred. And dissolving the functional organic acid by using deionized water at the temperature of 90-100 ℃, increasing the temperature of the bath solution during processing, and adding the dissolved functional organic acid solution into the bath solution to form a brown surface. Adding deionized water to the liquid level of the bath solution, and stirring with compressed air. The stirring temperature of the bath solution is-2 to 2 ℃.
Anodizing the workpiece after the workpiece is placed in the tank according to the following parameters:
pulse duty 27: 9
The current density is 2.5-3A/dm2
The processing temperature is-2 to +2 ℃.
The required time is adjusted according to the requirement of the thickness of the film layer;
(5) washing with water;
(6) and (5) drying.
The deionized water has the silicon content (SiO2) less than or equal to 1ppm, the resistivity (25 ℃) more than or equal to 100000 omega-cm and the PH value of 5.5-7.
The anodizing treatment time is delayed for 10-20 minutes.
The anodizing time is 70 +/-10 minutes except the delay time;
current/voltage fluctuations caused by equipment precision during machining are normal phenomena.
The water washing of (2) and (5) comprises flowing cold water washing and hot water washing.
And the water washing in the step (3) is only flowing cold water washing.
And (2) and (3) need to be subjected to oil removal and washing effect inspection.
And the drying (6) is specifically drying at the temperature of less than or equal to 60 ℃, or blowing by compressed air.
Technical effects
Experiments prove that: the hard anodization process is carried out by selecting a sulfuric acid + functional organic acid process, the thickness of an anodized film layer formed by 3D printing (selective laser melting forming) AlSi10Mg aluminum alloy workpieces can reach more than 30 micrometers, the film hardness reaches 340HV, the 3D printing (selective laser melting forming) AlSi10Mg aluminum alloy workpieces are processed by adopting the optimized hard anodization process, the process stability is good, the film forming efficiency is high, the actual film thickness is more than 30 micrometers, and the film hardness reaches 340HV, so that the traditional hard anodization performance is completely met. The process meets the requirement of hard anodizing of 3D printed (selective laser melting forming) AlSi10Mg aluminum alloy workpieces, and is successfully applied to 3D printed AlSi10Mg parts of our company.
Detailed Description
The present technical solution is further illustrated by the following examples.
The hard anodizing process for the 3D printing forming AlSi10Mg aluminum alloy material comprises the following steps of:
(1) removing oil by using a weak base water-based solvent;
1/3 volumes of deionized water were added to the tank, and 21g/L of Na was added in that order3PO42.5g/L of C6H15O3N, 3.1g/L Na2B4O710H2And after the O is completely dissolved, adding deionized water to the liquid level height, and heating to 55 ℃.
(2) Washing with water;
(3) acid deoxidation; washing with water
(4)3D printing (selective laser melting forming) AlSi10Mg aluminum alloy hard anodizing process method:
1/3 volumes of deionized water were added to the tank, and H was slowly added to the tank2SO4Adding deionized water to 2/3 volume,the compressed air agitation was turned on. And dissolving the functional organic acid by using deionized water at the temperature of 90-100 ℃, increasing the temperature of the bath solution during processing, and adding the dissolved functional organic acid solution into the bath solution to form a brown surface. Adding deionized water to the liquid level of the bath solution, and stirring with compressed air. The stirring temperature of the bath solution is-2 to 2 ℃.
Anodizing the workpiece after the workpiece is placed in the tank according to the following parameters:
pulse duty 27: 9
The current density is 2.5-3A/dm2
The processing temperature is-2 to +2 ℃.
The required time is adjusted according to the requirement of the thickness of the film layer;
(5) washing with water;
(6) and (5) drying.
The deionized water has the silicon content (SiO2) less than or equal to 1ppm, the resistivity (25 ℃) more than or equal to 100000 omega-cm and the PH value of 5.5-7.
The anodizing treatment time is delayed for 10-20 minutes.
The anodizing time is 70 +/-10 minutes except the delay time;
current/voltage fluctuations caused by equipment precision during machining are normal phenomena.
The water washing of (2) and (5) comprises flowing cold water washing and hot water washing. This step is a conventional water wash.
The washing in (3) is only flowing cold water washing, the main component of deacidification oxygen is white powdery CaO, and because calcium oxide can emit a large amount of heat when meeting water, if with hot water washing, the heat propagation can be increased, the reaction is violent, and the experimental operation and the safety requirement are not facilitated.
And (2) and (3) need to be subjected to oil removal and washing effect inspection.
And the drying (6) is specifically drying at the temperature of less than or equal to 60 ℃, or blowing by compressed air.
The present invention will be described in detail with reference to examples, which further explain and illustrate the technical features of the present invention.
A protective hard anodizing process of AlSi10Mg, comprising the following steps:
example 1:
1. pre-treating a workpiece;
oil removal is carried out by adopting weak base water-based oil removal solvent
2. Washing with hot water and cold water;
acid deoxidation
3. Hard anodization (c):
59g/l sulfuric acid
Functional organic acid 2g/l
The temperature is-2 to 2 DEG C
The current density is 2.5-3A/dm2
Pulse duty 27: 9
The slow rising time is 10-20 minutes
The time is 70 +/-10 minutes
4. Washing with cold water;
5. washing with hot water, and drying.
Claims (8)
1. The hard anodizing process method for the 3D printing forming AlSi10Mg aluminum alloy material is characterized by comprising the following steps of:
degreasing by using a weak base water-based solvent;
1/3 volumes of deionized water were added to the tank, and 21g/L of Na was added in that order3PO42.5g/L of C6H15O3N, 3.1g/L Na2B4O710H2After the O is completely dissolved, adding deionized water to the liquid level height, and heating to 55 ℃;
step (2), washing with water;
acid deoxidation in the step (3); washing with water
Step (4), 3D printing, laser selective melting and forming AlSi10Mg aluminum alloy hard anodizing process:
1/3 volumes of deionized water were added to the tank, and H was slowly added to the tank2SO4Adding deionized water to 2/3 volume, and stirring by opening compressed air; dissolving functional organic acid by using deionized water at the temperature of 90-100 ℃, increasing the temperature of bath solution processing, and adding the dissolved functional organic acid solution into the bath solution to form a brown surface; adding deionized water to the liquid level of the bath solution, and stirring with compressed air; the stirring temperature of the bath solution is-2 to 2 ℃;
anodizing the workpiece after the workpiece is placed in the tank according to the following parameters:
pulse duty 27: 9
The current density is 2.5-3A/dm2
The processing temperature is-2 to +2 ℃;
the required time is adjusted according to the requirement of the thickness of the film layer;
step (5), washing with water;
and (6) drying.
2. The hard anodizing process method for the AlSi10Mg aluminum alloy material for 3D printing and forming according to claim 1, wherein the deionized water has a silicon content SiO2 of less than or equal to 1ppm, a resistivity of greater than or equal to 100000 Ω -cm at 25 ℃ and a pH value of 5.5-7.
3. The hard anodization process for 3D printing shaped AlSi10Mg aluminum alloy material as recited in claim 1, wherein the anodization time comprises a slow start time, and the slow start time is 10-20 minutes.
4. The hard anodizing process method for the 3D printed Al Si10Mg aluminum alloy material according to claim 3, wherein the anodizing time is stabilized for 70 ± 10 minutes except for the buffering time.
5. The hard anodizing process method for 3D printing of shaped AlSi10Mg aluminum alloy material according to claim 1, wherein the water washing in step (2) and step (5) comprises flowing cold water washing and hot water washing.
6. The hard anodizing process method for the 3D printed Al-Si 10Mg aluminum alloy material according to claim 1, wherein the water washing in step (3) is a flowing cold water washing.
7. The hard anodizing process method for the 3D printed and formed AlSi10Mg aluminum alloy material according to claim 1, wherein step (2) and step (3) need to be checked for degreasing and washing effects.
8. The hard anodizing process method for the 3D printing formed AlSi10Mg aluminum alloy material according to claim 1, wherein the step (6) drying is specifically drying in an environment of 60 ℃ or below, or blowing by compressed air.
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| CN202010626089.8A CN111893538A (en) | 2020-07-02 | 2020-07-02 | Hard anodizing process method for 3D printing forming AlSi10Mg aluminum alloy material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113981498A (en) * | 2021-09-30 | 2022-01-28 | 北京动力机械研究所 | 3D printing AlMgSc alloy surface anodic oxidation method |
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| CN113981498A (en) * | 2021-09-30 | 2022-01-28 | 北京动力机械研究所 | 3D printing AlMgSc alloy surface anodic oxidation method |
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