CN102409383A - Anodic oxidation method for magnesium alloy - Google Patents
Anodic oxidation method for magnesium alloy Download PDFInfo
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- CN102409383A CN102409383A CN2011103600672A CN201110360067A CN102409383A CN 102409383 A CN102409383 A CN 102409383A CN 2011103600672 A CN2011103600672 A CN 2011103600672A CN 201110360067 A CN201110360067 A CN 201110360067A CN 102409383 A CN102409383 A CN 102409383A
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Abstract
The invention discloses an anodic oxidation method for a magnesium alloy. A used electrolyte consists of 10-100 g/L of sodium hydroxide or potassium hydroxide, 20-200 g/L of sodium silicate or potassium silicate, 20-150 g/L of sodium tetraborate or potassium tetraborate, saccharides and derivative additives thereof, and water. The method comprises the following steps of: (1) pretreating the magnesium alloy; and (2) performing anodic oxidation on the magnesium alloy: performing constant-current anodic oxidation under the stirring condition for 10-50 minutes, wherein a pulse power supply is taken as a power supply, and the temperature of an electrolyte is controlled at 5-40 DEG C. Due to the adoption of the components in the electrolyte, a solution is free from chromium, phosphorus and fluorine, and is environmentally-friendly. Saccharide substances serving as additives are added into a basic electrolyte, so that the reaction rate of magnesium with oxygen can be lowered, the growing speed of an oxide film can be lowered, the surface pore space of the oxide film of the magnesium alloy is reduced, the surface finish is enhanced, and the corrosion resistance of a magnesium alloy oxide film layer is enhanced.
Description
Technical field
The present invention relates to a kind of anodic oxidation of magnetism alloy method, belong to metal surface treatment technology.
Background technology
Advantages such as magnesiumalloy has that density is little, specific tenacity is high, specific rigidity is high, damping property is good, electromagnetic shielding and capability of resistance to radiation are strong have become novel material research and the focus that uses.Yet the solidity to corrosion of magnesiumalloy is minimum in the common metal structured material, is prone to galvanic corrosion take place and the accelerate dissolution corrosion, has restricted the widespread use of magnesiumalloy.Magnesiumalloy is carried out the corrosion resistance nature that surface treatment can effectively promote alloy material.Can form the sull that one deck electrical insulating property is good, bonding force is strong, solidity to corrosion is good at material surface in the anodic oxidation of magnetism alloy technology, be the magnesium alloy surface treatment of tool industrial applications prospect.
At present, mostly contain harmful elements such as Cr, P and F in the electrolyte solution that used Mg alloy surface is handled in the industrial production, environmental pollution is serious, and the processing cost of waste liquid is high, does not meet the requirement of Sustainable development.Therefore, no Cr, the environment protection electrolytic solution of harmful elements such as P and F and technology thereof become the emphasis of anodic oxidation of magnetism alloy research now.The environment protection electrolytic solution system mainly contains KOH-Na
2SiO
3-NaAlO
2, NaOH-Al (OH)
3-Na
2SiO
3, NaOH-Na
2SiO
3-Na
2B
4O
7Deng electrolyte system; Yet the sull surfaceness that is obtained by the environment protection electrolytic solution that inorganic salt are formed is big, and micropore skewness, aperture are bigger, cause corrosion resisting property relatively poor; And sticking power is not strong; Film forming is inhomogeneous, is prone to crack, and problems such as processes voltage is wayward, the local ablation of easy generation.
Summary of the invention
The present invention is intended to propose a kind of anodic oxidation of magnetism alloy method; Can generate the sull that micropore is evenly distributed, the aperture is tiny, roughness is little, solidity to corrosion is good at Mg alloy surface, and electrolytic solution satisfies environmental requirement, can not cause environmental pollution; It is simple that magnesiumalloy is carried out process of surface treatment; Film forming is easy to control, and raw material is easy to get, low price, is suitable for suitability for industrialized production.
This anodic oxidation of magnetism alloy method; Earlier with the magnesiumalloy pre-treatment; Put into electrolytic solution then and carry out anodic oxidation; Consisting of of wherein used electrolytic solution: sodium hydroxide or Pottasium Hydroxide 10-100g/L, water glass or potassium silicate 20-200g/L, sodium tetraborate or potassium tetraborate 20-150g/L, additive and water, described additive are one or both in carbohydrate and verivate glucose, lactose, sucrose, SANMALT-S, starch, dextrin, sorbyl alcohol and the Xylitol.
In the electrolytic solution in this anodic oxidation of magnetism alloy method, oxyhydroxide is mainly used in regulator solution resistance and pH value; Silicate is main membrane-forming agent, participates in the anodic oxidation of magnetism alloy reaction, forms insoluble compound, makes the refinement of sull rete, densification, improves homogeneity, can significantly improve the solidity to corrosion of sull; Borate is mainly used in increases the sull film forming speed, shortens the reaction times; Additive carbohydrate and verivate thereof are biological polyvalent alcohol; Contain a plurality of hydroxyls in its unit molecule structure; And the lone-pair electron that have on the hydroxyl can combine with the magnesium atom unoccupied orbital, thereby can be adsorbed in Mg alloy surface effectively, play shielding effect at Mg alloy surface; Thereby slow down the speed of reaction and the oxide growth speed of magnesium and oxygen, make compactness, homogeneity and the solidity to corrosion of sull be significantly increased.
Anodic oxidation of magnetism alloy method of the present invention mainly contains following advantage compared with prior art:
(1) environmental protection.Objectionable impuritiess such as Chrome-free, fluorine, phosphorus in the electrolytic solution of the present invention, waste liquid is prone to handle simultaneously, and environmentally safe belongs to the environmental type prescription.
(2) additive is carbohydrate and verivate thereof, is the biomass compound, and is pollution-free to human body and physical environment, and is prone to by microbiological degradation.
(3) can obtain the good sull of solidity to corrosion.Can obtain with method of the present invention smooth, densification, evenly and the good anodic oxidation of magnetism alloy film of solidity to corrosion, the simultaneous oxidation membrane micropore is evenly distributed, the aperture is tiny.
Description of drawings
Fig. 1 is the Tafel polarization curve that carries out surface-treated AZ31 magnesium alloy sample and AZ31 magnesium alloy substrate through method of the present invention, and among the figure, a is without anodised magnesium alloy sample curve, and b representes the magnesium alloy sample curve after the inventive method is handled;
Fig. 2 is with starch during as additive, AZ31 anodic oxidation of magnetism alloy film surface topography SEM photo;
Fig. 3 is with starch during as additive, AZ31 anodic oxidation of magnetism alloy film cross section pattern SEM photo.
Embodiment
Consisting of of the electrolytic solution that this anodic oxidation of magnetism alloy method is used: sodium hydroxide or Pottasium Hydroxide 10-100g/L, water glass or potassium silicate 20-200g/L, sodium tetraborate or potassium tetraborate 20-150g/L, additive and water, described additive are one or both in carbohydrate and verivate glucose, lactose, sucrose, SANMALT-S, starch, dextrin, sorbyl alcohol and the Xylitol.
When additive was glucose, add-on can be 5-40g/L.
When additive was lactose, add-on can be 5-60g/L.
When additive was sucrose, add-on can be 10-40g/L.
When additive was SANMALT-S, add-on can be 10-50g/L.
When additive was dextrin, add-on can be 5-50g/L.
When additive was starch, add-on can be 5-50g/L.
When additive was sorbyl alcohol, add-on can be 10-40g/L.
When additive was Xylitol, add-on can be 5-30g/L.
When magnesiumalloy being carried out anodic oxidation, can adopt the pulse power with above-mentioned electrolytic solution, the continuous current pattern, concrete steps are following:
(1) magnesiumalloy pre-treatment: polishing, boring, zero(ppm) water cleaning, acetone ultrasonic cleaning, zero(ppm) water clean, dry up.
(2) anodic oxidation of magnetism alloy: use stainless steel to be negative electrode, magnesiumalloy is an anode, under agitation condition, and the constant current anodic oxidation, electrolyte temperature is controlled at 5～40 ℃, and the time is 10～50min.Used power supply is the pulse power, and its pulse-repetition and dutycycle are adjustable continuously, and current density is 5mA/cm
2～40mA/cm
2, range of frequency is 100Hz～500Hz, dutycycle is 10%～30%.
Embodiment 1
Magnesium alloy materials: AZ31 magnesium alloy plate
Magnesium alloy materials is processed sample respectively through following pre-treatment: polishing, boring, zero(ppm) water clean, acetone is ultrasonic, zero(ppm) water cleans, dries up.
With above-mentioned magnesium alloy sample (having 7 samples) anodic oxidation in the electrolytic solution described in the table 1, anodic oxidation condition is: the pulse power, continuous current pattern, current density 10mA/cm
2, anodizing time 15min, pulse-repetition 100Hz, dutycycle 10%, temperature be controlled at 10-30 ℃.Whole anode oxidation process carries out under stirring condition.
Table 1 electrolytic solution is formed
| Specimen coding | 1 | 2 | 3 | 4 | 5 | 6 | 7 |
| NaOH(g/L) | 45 | 45 | 45 | 45 | 45 | 45 | 45 |
| Na 2SiO 3(g/L) | 70 | 70 | 70 | 70 | 70 | 70 | 70 |
| Na 2B 4O 7(g/L) | 90 | 90 | 90 | 90 | 90 | 90 | 90 |
| Glucose (g/L) | 10 | ? | ? | ? | ? | ? | ? |
| Sucrose (g/L) | ? | 10 | ? | ? | ? | ? | ? |
| SANMALT-S | ? | ? | ? | ? | 15 | ? | ? |
| Dextrin (g/L) | ? | ? | 20 | ? | ? | ? | ? |
| Lactose (g/L) | ? | ? | ? | 15 | ? | ? | ? |
| Sorbyl alcohol (g/L) | ? | ? | ? | ? | ? | 15 | ? |
| Xylitol (g/L) | ? | ? | ? | ? | ? | ? | 20 |
The performance evaluation of anodic oxidation of magnetism alloy film: see table 2.
Table 2 anodic oxidation of magnetism alloy film properties
Salt-fog test is undertaken by ASTMB117 and ASTMB398 standard.Test temperature is 35.5 ± 0.5 ℃, and used corrosive medium is the 5%NaCl solution of pH=7.Hot spot appears in the AZ31 magnesiumalloy salt fog 8h without anodize; This programme is handled its salt fog of AZ31 magnesiumalloy 130h, and hot spot does not all appear in specimen surface.
Embodiment 2
Magnesium alloy materials: AZ31 magnesium alloy plate
Magnesium alloy materials is processed sample respectively through following pre-treatment: polishing, boring, zero(ppm) water clean, acetone is ultrasonic, zero(ppm) water cleans, dries up.
Electrolytic solution is formed:
NaOH：45g/L，
Na
2SiO
3：50g/L，
Na
2B
4O
7：70g/L，
Glucose: 15g/L.
Magnesium alloy sample carries out anodic oxidation in above-mentioned electrolytic solution, the pulse power, and the continuous current pattern adopts 5 kinds of different anode oxidation process conditions as shown in table 3, carries out anodic oxidation.
Table 3 anodic oxidation of magnetism alloy processing condition
| Specimen coding | 1 | 2 | 3 | 4 | 5 |
| Current density (mA/cm 2) | 5 | 10 | 10 | 20 | 40 |
| Oxidization time (min) | 25 | 15 | 20 | 10 | 10 |
| Pulse-repetition (Hz) | 100 | 100 | 200 | 500 | 100 |
| Dutycycle (%) | 20 | 10 | 10 | 30 | 10 |
The performance evaluation of the anodic oxidation of magnetism alloy film of gained is seen table 4.
Table 4 anodic oxidation of magnetism alloy film properties
Salt-fog test is undertaken by ASTMB117 and ASTMB398 standard.Test temperature is 35.5 ± 0.5 ℃, and used corrosive medium is the 5%NaCl solution of pH=7.Hot spot appears in the AZ31 magnesiumalloy salt fog 8h without anodize; This programme is handled its salt fog of AZ31 magnesiumalloy 120h, and hot spot does not all appear in specimen surface
Embodiment 3
Magnesium alloy materials: AZ31 magnesium alloy plate
Magnesium alloy materials is processed sample respectively through following pre-treatment: polishing, boring, zero(ppm) water clean, acetone is ultrasonic, zero(ppm) water cleans, dries up.
Electrolytic solution is formed:
NaOH：45g/L，
Na
2SiO
3：50g/L，
Na
2B
4O
7：70g/L，
Zulkovsky starch: 15g/L.
Magnesium alloy sample is carried out anodic oxidation in above-mentioned electrolytic solution.Anodic oxidation condition is: the pulse power, continuous current pattern, current density 10mA/cm
2, anodizing time 20min, pulse-repetition 200Hz, dutycycle 10%, temperature be controlled at 5-40 ℃ of whole anode oxidation process and under stirring condition, carry out.
Sull outward appearance and performance: the anodic oxidation of magnetism alloy film is pearl, and is smooth, even, fine and close; Thicknesses of layers 15-17 μ m, roughness 0.326 μ m.
To and in 3.5% sodium chloride solution, do the Tafel polarization curve through the magnesiumalloy of anodize and carry out corrosion evaluation without anodised magnesiumalloy, the result be as shown in Figure 1.A representes without anodised magnesium alloy sample among the figure, and b representes the magnesium alloy sample after the inventive method is handled.The a corrosion potential is-1.496V, is 338.84 μ A/cm from corrosion electric current density
2, the AZ31 magnesiumalloy sull corrosion potential of optimization process is-1.215V, the corrosion potential 0.281V that shuffled is 0.14 μ A/cm from corrosion electric current density
2Magnesium alloy work-piece surface and cross section pattern such as Fig. 2, shown in Figure 3 can know that sull is even, densification by figure.
Salt-fog test is undertaken by ASTMB117 and ASTMB398 standard.Test temperature is 35.5 ± 0.5 ℃, and used corrosive medium is the 5%NaCl solution of pH=7.Hot spot appears in the AZ31 magnesiumalloy salt fog 8h without anodize; This programme is handled its salt fog of AZ31 magnesiumalloy 150h, and hot spot does not appear in specimen surface.
Magnesium alloy materials: AZ31 magnesium alloy plate.
Magnesium alloy materials is processed sample respectively through following pre-treatment: polishing, boring, zero(ppm) water clean, acetone is ultrasonic, zero(ppm) water cleans, dries up.
Electrolytic solution is formed:
NaOH：45g/L，
Na
2SiO
3：50g/L，
Na
2B
4O
7：70g/L，
Zulkovsky starch: 15g/L.
Anode oxidation process: the pulse power, continuous current pattern, current density 25mA/cm
2, anodizing time 25min, pulse-repetition 100Hz, dutycycle 10%.
Obtain grey black, even sull, its thicknesses of layers 55-70 μ m.
To and in 3.5% sodium chloride solution, do the Tafel polarization curve through the magnesiumalloy of anodize and carry out corrosion evaluation without anodised magnesiumalloy, the magnesium alloy substrate corrosion potential be-1.496V, is 338.84 μ A/cm from corrosion electric current density
2, magnesiumalloy black oxide film corrosion potential is-1.284V, the corrosion potential 0.112V that shuffled is 0.32 μ A/cm from corrosion electric current density
2
Salt-fog test is undertaken by ASTMB117 and ASTMB398 standard.Test temperature is 35.5 ± 0.5 ℃, and used corrosive medium is the 5%NaCl solution of pH=7.Hot spot appears in the AZ31 magnesiumalloy salt fog 8h without anodize; This programme is handled its salt fog of AZ31 magnesiumalloy 130h, and hot spot does not appear in specimen surface.
Embodiment 5
According to table 5 preparing electrolyte, carry out anodize at the AZ31 Mg alloy surface.
Table 5 electrolyte prescription
| Specimen coding | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 |
| NaOH(g/L) | 20 | 20 | 45 | 45 | 30 | 25 | ? | ? | ? |
| KOH(g/L) | ? | 50 | ? | ? | 30 | 40 | 65 | 65 | 100 |
| Na 2SiO 3(g/L) | ? | 70 | ? | 30 | 70 | ? | 50 | 100 | ? |
| K 2SiO 3(g/L) | 100 | ? | 80 | 60 | ? | 90 | 40 | ? | 200 |
| Na 2B 4O 7(g/L) | ? | 80 | 60 | 20 | 90 | 40 | 90 | 90 | ? |
| K 2B 4O 7(g/L) | 150 | ? | 20 | 70 | ? | 60 | ? | ? | 70 |
| Glucose (g/L) | 5 | ? | 40 | ? | ? | ? | ? | ? | ? |
| Sucrose (g/L) | ? | 40 | ? | 5 | ? | 15 | ? | ? | ? |
| SANMALT-S (g/L) | ? | ? | ? | ? | 10 | ? | ? | 50 | ? |
| Lactose (g/L) | ? | 5 | ? | 40 | ? | ? | ? | ? | ? |
| Starch (g/L) | ? | ? | 5 | ? | ? | ? | ? | ? | 60 |
| Dextrin (g/L) | 50 | ? | ? | ? | ? | 10 | ? | ? | 5 |
| Sorbyl alcohol (g/L) | ? | ? | ? | ? | 40 | ? | 10 | ? | ? |
| Xylitol (g/L) | ? | ? | ? | ? | ? | ? | 30 | 5 | ? |
The performance evaluation of the anodic oxidation of magnetism alloy film of gained is seen table 6
Table 6 anodic oxidation of magnetism alloy film properties
Salt-fog test is undertaken by ASTMB117 and ASTMB398 standard.Test temperature is 35.5 ± 0.5 ℃, and used corrosive medium is the 5%NaCl solution of pH=7.Hot spot appears in the AZ31 magnesiumalloy salt fog 8h without anodize; This programme is handled its salt fog of AZ31 magnesiumalloy 110h, and hot spot does not all appear in specimen surface.
Claims (10)
1. anodic oxidation of magnetism alloy method; With the magnesiumalloy pre-treatment; Put into electrolytic solution then and carry out anodic oxidation; It is characterized in that consisting of of used electrolytic solution: sodium hydroxide or Pottasium Hydroxide 10-100g/L, water glass or potassium silicate 20-200g/L, sodium tetraborate or potassium tetraborate 20-150g/L, additive and water, described additive are one or both in carbohydrate and verivate glucose, lactose, sucrose, SANMALT-S, starch, dextrin, sorbyl alcohol and the Xylitol.
2. anodic oxidation of magnetism alloy method as claimed in claim 1 is characterized in that described additive is a glucose, and add-on is 5-40g/L.
3. anodic oxidation of magnetism alloy method as claimed in claim 1 is characterized in that described additive is a lactose, and add-on is 5-60g/L.
4. anodic oxidation of magnetism alloy method as claimed in claim 1 is characterized in that described additive is a sucrose, and add-on is 10-40g/L.
5. anodic oxidation of magnetism alloy method as claimed in claim 1 is characterized in that described additive is a SANMALT-S, and add-on is 10-50g/L.
6. anodic oxidation of magnetism alloy method as claimed in claim 1 is characterized in that described additive is a dextrin, and add-on is 5-50g/L.
7. anodic oxidation of magnetism alloy method as claimed in claim 1 is characterized in that described additive is a starch, and add-on is 5-50g/L.
8. anodic oxidation of magnetism alloy method as claimed in claim 1 is characterized in that described additive is a sorbyl alcohol, and add-on is 10-40g/L.
9. anodic oxidation of magnetism alloy method as claimed in claim 1 is characterized in that described additive is an Xylitol, and add-on is 5-30g/L.
10. anodic oxidation of magnetism alloy method as claimed in claim 1 is characterized in that described magnesiumalloy pre-treatment is: polishing, boring, zero(ppm) water clean, acetone is ultrasonic, zero(ppm) water cleans, dries up; Described anode oxidation process is: use stainless steel to be negative electrode, magnesiumalloy is an anode, under agitation condition, and the constant current anodic oxidation, used power supply is the pulse power, and its pulse-repetition and dutycycle have continuously adjustable, and current density is 5mA/cm
2～50mA/cm
2, range of frequency is 100Hz～500Hz, and dutycycle is 10%～30%, and electrolyte temperature is controlled at 5～40 ℃, and the time is 10～50min.
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| CN103938253A (en) * | 2013-01-23 | 2014-07-23 | 汉达精密电子(昆山)有限公司 | Magnesium alloy anodic oxidation electrolyte and method of processing magnesium alloy with the electrolyte |
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| CN105063721A (en) * | 2015-08-26 | 2015-11-18 | 华南理工大学 | Magnesium alloy anodizing electrolyte and method for preparing anodic oxide film by electrolyte |
| CN106906509A (en) * | 2017-04-10 | 2017-06-30 | 四川理工学院 | One kind improves the corrosion proof method of Anodic Film On Magnesium Alloy |
| CN107287641A (en) * | 2016-03-31 | 2017-10-24 | 比亚迪股份有限公司 | A kind of method of anodic oxidation of magnetism alloy liquid, preparation method and anodic oxidation of magnetism alloy |
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| CN107937965A (en) * | 2017-12-18 | 2018-04-20 | 嘉兴学院 | A kind of magnesium alloy anodic oxidation electrolyte and anodic oxidation method for magnesium alloy |
| CN108048893A (en) * | 2017-12-18 | 2018-05-18 | 嘉兴学院 | A kind of environmental-protection type magnesium alloy anodic oxidation electrolyte and anodic oxidation method for magnesium alloy |
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| CN102828218B (en) * | 2012-09-14 | 2015-04-15 | 戚威臣 | Electrolyte used for magnesium alloy anode oxidation treatment and treatment method |
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| CN108048893A (en) * | 2017-12-18 | 2018-05-18 | 嘉兴学院 | A kind of environmental-protection type magnesium alloy anodic oxidation electrolyte and anodic oxidation method for magnesium alloy |
| CN108048893B (en) * | 2017-12-18 | 2019-07-16 | 嘉兴学院 | A kind of environmental-protection type magnesium alloy anodic oxidation electrolyte and anodic oxidation method for magnesium alloy |
| CN107937965B (en) * | 2017-12-18 | 2019-07-23 | 嘉兴学院 | A kind of magnesium alloy anodic oxidation electrolyte and anodic oxidation method for magnesium alloy |
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| CN115537895A (en) * | 2022-10-14 | 2022-12-30 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of pure titanium surface colorful anodic oxide film |
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