CN110093608B - Surface polishing solution for additive manufacturing of aluminum alloy and application - Google Patents
Surface polishing solution for additive manufacturing of aluminum alloy and application Download PDFInfo
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- CN110093608B CN110093608B CN201910457147.6A CN201910457147A CN110093608B CN 110093608 B CN110093608 B CN 110093608B CN 201910457147 A CN201910457147 A CN 201910457147A CN 110093608 B CN110093608 B CN 110093608B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
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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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F3/00—Brightening metals by chemical means
- C23F3/02—Light metals
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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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G3/00—Apparatus for cleaning or pickling metallic material
Abstract
The invention belongs to the field of surface treatment of aluminum alloy, and discloses a surface polishing solution for additive manufacturing of aluminum alloy and application thereof. The surface polishing solution mainly comprises 100-150 g.L‑1Potassium hydroxide, 20-60 g.L‑1Sodium acetate, 20-40 g.L‑1Sodium sulfide, 15-30 g.L‑1Potassium borate, 5-10 g.L‑1Magnetic abrasive and 5-10 g.L‑1Sodium tripolyphosphate, 3-8 g.L‑1Magnesium dodecyl sulfate and 5-10 mL. L‑1Glycerol as an additive. The polishing process comprises the following steps: pretreatment → arrangement of surface polishing liquid → chemical polishing → neutralization treatment → post-treatment. The polishing process can be used for aluminum alloy workpieces with regular shapes and complex aluminum alloy products containing pipelines, apertures, curved surfaces and internal flows in additive manufacturing. After the aluminum alloy product is treated by the method, the surface roughness is reduced by 50-60%, and the weight loss rate is about 7-8%. The surface polishing solution has stable quality, easily obtained formula materials, low cost and good conductivity, and is not limited by the shape of a polishing product. The polishing process is safe and environment-friendly, the surface brightness and the flatness of the processed aluminum alloy are good, and the quality is improved.
Description
Technical Field
The invention belongs to the technical field of surface treatment in the field of metal treatment, and particularly relates to an additive manufacturing aluminum alloy surface polishing process which is difficult to perform surface treatment through traditional mechanical polishing.
Background
The additive manufacturing has the advantages of high flexibility, no mold, short period, diversified manufactured products, unlimited design space and the like, and is widely applied to the industries of aerospace, biomedical, automobile industry, mechanical electronics and the like. As the additive manufacturing technology develops toward high efficiency and low cost, the additive manufacturing becomes more and more important. Aluminum alloys have been rapidly developed in the field of additive manufacturing in recent years due to their unique properties, such as low density, high corrosion resistance, good electrical conductivity, thermal conductivity and light reflectance, easy workability and relatively low cost. In order to improve the surface flatness of the additive manufacturing aluminum alloy and expand the practical application range, the surface of the aluminum alloy is usually required to be subjected to finish machining and polishing. The most common polishing processes are mechanical polishing, chemical polishing, electrochemical polishing, and the like.
Mechanical polishing is a polishing method in which the convex part of a polished member is removed by cutting and plastic deformation of the material surface to obtain a smooth surface. Chemical polishing is to make the microscopically protruding part of the material surface dissolve in a chemical medium preferentially than the concave part, so as to obtain a smooth surface. Electropolishing is a finishing process in which a metal article is anodized in a specific composition of electrolyte to obtain a smooth, bright surface. Aiming at the problems of higher surface roughness, more complex shape and the like of an additive manufacturing aluminum alloy product, the surface of the aluminum alloy is treated by utilizing two technologies of chemical polishing and electrolytic polishing, and the method is the most efficient method for reducing the surface roughness and improving the aesthetic property. In contrast, electropolishing is costly, requires complex equipment and is complicated to implement. The chemical polishing operation process is relatively simple, complex equipment is not needed, the practicability is high, and the special-shaped workpiece which has a complex aperture, a complex pipeline and a complex inner flow passage and is difficult to carry out surface treatment through electrolytic polishing can be polished, so that the chemical polishing process is the simplest and most efficient surface treatment process. At present, the chemical polishing process of the aluminum alloy mainly comprises two main types of acid polishing and alkaline polishing. Although the acidic polishing has good stability, short treatment time and remarkable polishing effect, in industrial production, toxic gas is generated due to the existence of a large amount of nitric acid in the polishing solution, and the toxic gas is harmful to the atmospheric environment, water quality and human health, so that the strong development of alkaline polishing solution becomes a great trend of the chemical polishing method for surface treatment of the additive manufacturing aluminum alloy at present.
Disclosure of Invention
The invention aims to solve the surface quality problem of the existing additive manufacturing aluminum alloy, and provides an additive manufacturing aluminum alloy surface polishing process which is low in configuration cost, strong in stability, easy to control in reaction speed, simple and convenient to operate, and high in efficiency.
In order to achieve the object of the present invention and achieve the desired effects, the inventors have diligently made efforts through a large number of trial and error tests to obtain the following technical solutions.
A surface polishing solution for additive manufacturing of aluminum alloy comprises the following substances in percentage by weight: 100-150 g.L-1Potassium hydroxide, 20-60 g.L-1Sodium acetate, 20-40 g.L-1Sodium thiosulfate 15-30 g.L-1Potassium silicate, 5-10 g.L-1Magnetic abrasives and additives; the content of each substance of the additive in the polishing solution is as follows: 5-10 g.L-1Sodium tripolyphosphate, 3-8 g.L-1Dodecyl magnesium sulfate or 5-10 mL. L-1One or more of glycerin.
The magnetic abrasive in the polishing solution is one of an aluminum-nickel-cobalt permanent magnet alloy, an iron-chromium-cobalt permanent magnet alloy, a permanent magnetic ferrite, a rare earth permanent magnet material or a composite permanent magnet material.
The surface polishing process for additive manufacturing of the aluminum alloy by adopting the surface polishing solution comprises the following steps:
(1) chemical oil removal: the degreasing liquid prepared by a metal detergent is adopted, and a sample is put into the degreasing liquid at the temperature of 85-95 ℃ for 15-30 min for ultrasonic cleaning and degreasing;
(2) acid washing/alkali washing: using 15-25 mL. L-1HNO of (2)3The pickling solution reacts for 1-3 min or 35-45 g.L at room temperature-1Reacting the NaOH alkaline solution at room temperature for 3-8 min to further clean the surface of the aluminum alloy workpiece, and then washing and drying the aluminum alloy workpiece by using deionized water;
(3) chemical polishing: dipping the aluminum alloy product obtained in the step (2) into surface polishing solution heated to 80-90 ℃ for surface polishing treatment, wherein magnetic stirring is assisted in the polishing process, and the temperature is kept for 30-300 s;
(4) neutralizationAnd (3) treatment: taking out the polished aluminum product for neutralization treatment, wherein the content of each substance in the treatment liquid is 75-85 g.L-1Citric acid, 15-25 g.L-1Oxalic acid, 240-260mL & L--1Phosphoric acid and 4-6 mL. L-1Glycerol, wherein the treatment temperature is 80-85 ℃, and the neutralization time is 15-30 s; since alkaline compounds are generated on the surface of the sample after polishing with alkali solution, and the compounds are black in color and difficult to wash away, neutralization treatment is required to wash away black substances and improve the surface brightness of the sample.
(5) And (3) post-treatment: and taking out the neutralized aluminum alloy sample, washing with water, and drying.
Further, the neutralization treatment in the step (4) is preferable: the content of each substance in the treating solution was 80 g.L-1Citric acid, 20 g.L-1Oxalic acid, 250 mL. L-1Phosphoric acid and 5 mL. L-1And (3) glycerol.
Further, it is preferable that the magnetic stirring speed in the above step (3) is 50 to 70 rpm.
Further, it is preferable that the polishing time in the above step (3) is 60s to 180 s.
When the polishing temperature is lower than 80 ℃, the required polishing time is long, and the surface color of the polished aluminum alloy is dark; when the polishing temperature is higher than 90 ℃, the over-corrosion phenomenon is easy to occur on the surface of the aluminum alloy, and the roughness is larger. And the time required for polishing is closely related to the concentration of each component of the polishing solution. The surface oxide of the aluminum alloy sample can not be completely stripped by the alkaline corrosion if the polishing time is too short, and the performance and the subsequent application of the product are adversely affected; the polishing time is too long, so that the risk of over-corrosion exists, the weight loss rate is increased and the cost is increased due to the fact that the surface roughness of the sample is increased.
The invention has the advantages that:
1. the chemical polishing solution used in the aluminum alloy surface polishing process has the advantages of low cost, stable property, good conductivity and high efficiency, and can be recycled for many times on the premise of replenishing the mother solution.
2. According to the aluminum alloy surface polishing process, the magnetic grinding material is added for stirring, so that floating powder on the surface of the additive manufacturing aluminum alloy is removed in the polishing process, the reaction speed can be effectively controlled, and the generation of flow marks is prevented.
3. The aluminum alloy surface polishing process disclosed by the invention is simple in implementation process and wide in application range, is suitable for additive manufacturing of aluminum alloy products with regular shapes, and is still suitable for complex aluminum alloy products with pipelines, inner holes or inner flow passages with different diameters. By using the surface polishing process to perform surface treatment on the additive manufactured aluminum alloy product, the sample weight loss rate is low on the premise of effectively reducing the surface roughness of the aluminum alloy, and the high-quality aluminum alloy surface can be obtained.
Drawings
FIG. 1 is an SEM image of the surface topography of an aluminum alloy workpiece after pretreatment and before polishing in additive manufacturing according to example 2.
FIG. 2 is an SEM image of the surface topography of the additive manufactured aluminum alloy after polishing in example 2.
Detailed Description
The invention is further described with reference to specific examples.
Example 1
And performing surface polishing treatment on the additive manufacturing aluminum alloy tubular product with the length of 80mm and the inner and outer diameters of 15mm and 5mm respectively.
(1) Chemical oil removal: the degreasing liquid with the concentration of 10% prepared by a metal detergent is adopted, and a sample is placed into the degreasing liquid with the temperature of 85 ℃ for 30min for ultrasonic cleaning and degreasing.
(2) Acid washing: using 20 mL. L-1HNO of (2)3And reacting the pickling solution at room temperature for 2min to further clean the surface of the aluminum alloy workpiece, and then washing and drying the aluminum alloy workpiece by using deionized water.
(3) Preparing a polishing solution: the content of each substance in the prepared polishing solution is as follows: 120 g.L-1Potassium hydroxide, 30 g.L-1Sodium acetate, 35 g.L-1Sodium thiosulfate, 15 g.L-1Potassium silicate, 7 g.L-1Magnetic abrasive and 5 g.L-1Sodium tripolyphosphate, 4g, L-1Magnesium lauryl sulfate and 5 mL. L-1Glycerol as an additive.
(4) Chemical polishing: and (3) soaking the aluminum alloy product subjected to degreasing and cleaning in the chemical polishing solution heated to 80 ℃ for surface polishing treatment, wherein the magnetic stirring is carried out at the rotation speed of 70rpm in the polishing process, and the aluminum alloy product is kept at the temperature for 2 min.
(5) And (3) neutralization treatment: taking out the polished aluminum product for neutralization treatment, wherein the treatment liquid is 80 g.L-1Citric acid, 20 g.L-1Oxalic acid, 250 mL. L-1Phosphoric acid, 5 mL. L-1Preparing glycerol, treating at 80 deg.C for 20s
(6) And (3) post-treatment: and taking out the neutralized aluminum alloy sample, washing with water, and drying.
The roughness of the aluminum alloy surface is obviously reduced after polishing treatment, and the weight loss is less. The surface roughness is reduced from 15.696 mu m to 6.483 mu m, and the weight loss rate of the sample is 7.539%.
Example 2
The spherical additive manufacturing aluminum alloy product with the diameter of 25mm and the inner flow passage with the diameter of 3mm is subjected to surface polishing treatment.
(1) Chemical oil removal: the degreasing liquid with the concentration of 10% prepared by a metal detergent is adopted, and a sample is placed into the degreasing liquid with the temperature of 90 ℃ for 25min for ultrasonic cleaning and degreasing.
(2) Acid washing: using 20 mL. L-1HNO of (2)3And reacting the pickling solution at room temperature for 3min to further clean the surface of the aluminum alloy workpiece, and then washing and drying the aluminum alloy workpiece by using deionized water.
(3) Preparing a polishing solution: 135 g.L of-1Potassium hydroxide, 55 g.L-1Sodium acetate, 30 g.L-1Sodium thiosulfate, 25 g.L-1Potassium silicate, 5 g.L-1Magnetic abrasive and 10 g.L-1Sodium tripolyphosphate, 7 g.L-1Magnesium lauryl sulfate and 5 mL. L-1The additive composed of glycerol is mixed uniformly according to a proportion, and magnetic stirring is carried out to prepare the polishing solution.
(4) Chemical polishing: and (3) soaking the aluminum alloy product subjected to degreasing and cleaning in the chemical polishing solution heated to 85 ℃ for surface polishing treatment, wherein the magnetic stirring is carried out at the rotation speed of 60rpm in the polishing process, and the aluminum alloy product is kept at the temperature for 1 min.
(5) And (3) neutralization treatment: taking out the polished aluminum product for neutralization treatment, wherein the treatment liquid is 80 g.L-1Citric acid, 20 g.L-1Oxalic acid, 250 mL. L-1Phosphoric acid, 5 mL. L-1Preparing glycerol, wherein the treatment temperature is 80-85 ℃, and the neutralization time is 25 s.
(6) And (3) post-treatment: and taking out the neutralized aluminum alloy sample, washing with water, and drying.
The roughness of the aluminum alloy surface is obviously reduced after polishing treatment, and the weight loss is less. The surface roughness is reduced from 14.893 mu m to 6.067 mu m, and the weight loss rate of the sample is 7.019%.
Example 3
The additive manufacturing aluminum alloy product containing the grids, which is 70mm long, 20mm wide and 15mm high, is subjected to surface polishing treatment.
(1) Chemical oil removal: the degreasing liquid with the concentration of 10% prepared by a metal detergent is adopted, and a sample is put into the degreasing liquid with the temperature of 95 ℃ for 15min for ultrasonic cleaning and degreasing.
(2) Alkali washing: using 40 g.L-1The NaOH alkaline solution reacts for 6min at room temperature, the surface of the aluminum alloy workpiece is further cleaned, and then deionized water is used for washing and drying.
(3) Preparing a polishing solution: 105 g.L-1Potassium hydroxide, 40 g.L-1Sodium acetate, 25 g.L-1Sodium thiosulfate, 28 g.L-1Potassium silicate, 10 g.L-1Magnetic abrasive and 7.5 g.L-1Sodium tripolyphosphate, 3.5 g.L-1Magnesium lauryl sulfate and 6.5 mL. L-1The additive composed of glycerol is mixed uniformly according to a proportion, and magnetic stirring is carried out to prepare the polishing solution.
(4) Chemical polishing: and (3) soaking the aluminum alloy product subjected to degreasing and cleaning in the chemical polishing solution heated to 90 ℃ for surface polishing treatment, wherein the magnetic stirring is carried out at the rotation speed of 50rpm in the polishing process, and the aluminum alloy product is kept at the temperature for 3 min.
(5) And (3) neutralization treatment: taking out the polished aluminum product for neutralization treatment, wherein the treatment liquid is 80 g.L-1Citric acid, 20 g.L-1Oxalic acid, 250 mL. L-1Phosphoric acid, 5 mL. L-1Preparing glycerol, wherein the treatment temperature is 82 ℃, and the neutralization time is 25 s.
(6) And (3) post-treatment: and taking out the neutralized aluminum alloy sample, washing with water, and drying.
The roughness of the aluminum alloy surface is obviously reduced after polishing treatment, and the weight loss is less. The surface roughness is reduced from 19.837 mu m to 8.682 mu m, and the weight loss rate of the sample is 7.685%.
Claims (4)
1. The surface polishing process for manufacturing the aluminum alloy by the additive manufacturing by adopting the surface polishing solution is characterized by comprising the following steps of:
(1) chemical oil removal: the degreasing liquid prepared by a metal detergent is adopted, and a sample is put into the degreasing liquid at the temperature of 85-95 ℃ for 15-30 min for ultrasonic cleaning and degreasing;
(2) acid washing/alkali washing: using 15-25 mL. L-1HNO of (2)3The pickling solution reacts for 1-3 min or 35-45 g.L at room temperature-1Reacting the NaOH alkaline solution at room temperature for 3-8 min to further clean the surface of the aluminum alloy workpiece, and then washing and drying the aluminum alloy workpiece by using deionized water;
(3) chemical polishing: dipping the aluminum alloy product obtained in the step (2) into surface polishing solution heated to 80-90 ℃ for surface polishing treatment, wherein magnetic stirring is assisted in the polishing process, and polishing is carried out for 30-300 s at the temperature; the polishing solution comprises the following substances in percentage by weight: 100-150 g.L-1Potassium hydroxide, 20-60 g.L-1Sodium acetate, 20-40 g.L-1Sodium thiosulfate 15-30 g.L-1Potassium silicate, 5-10 g.L-1Magnetic abrasives and additives; the content of each substance of the additive in the polishing solution is as follows: 5-10 g.L-1Sodium tripolyphosphate, 3-8 g.L-1Dodecyl magnesium sulfate or 5-10 mL. L-1One or more of glycerin; the magnetic abrasive in the polishing solution is one of an aluminum-nickel-cobalt permanent magnet alloy, an iron-chromium-cobalt permanent magnet alloy, a permanent magnetic ferrite, a rare earth permanent magnet material or a composite permanent magnet material;
(4) and (3) neutralization treatment: taking out the polished aluminum product for neutralization treatment, wherein the content of each substance in the treatment liquid is 75-85 g.L-1Citric acid, 15-25 g.L-1Oxalic acid, 240-260mL & L--1Phosphoric acid and 4-6 mL. L-1Glycerol, wherein the treatment temperature is 80-85 ℃, and the neutralization time is 15-30 s;
(5) and (3) post-treatment: and taking out the neutralized aluminum alloy sample, washing with water, and drying.
2. The surface polishing process according to claim 1, wherein the step (4) of neutralizing treatment: the content of each substance in the treating solution was 80 g.L-1Citric acid, 20 g.L-1Oxalic acid, 250 mL. L-1Phosphoric acid and 5 mL. L-1And (3) glycerol.
3. The surface polishing process according to claim 1, wherein the magnetic stirring speed in the step (3) is 50 to 70 rpm.
4. The surface polishing process according to claim 1, wherein the polishing time in the step (3) is 30s to 300 s.
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