CN101016627A - Method of treating magnesium alloy work-piece surface - Google Patents
Method of treating magnesium alloy work-piece surface Download PDFInfo
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- CN101016627A CN101016627A CN 200710078179 CN200710078179A CN101016627A CN 101016627 A CN101016627 A CN 101016627A CN 200710078179 CN200710078179 CN 200710078179 CN 200710078179 A CN200710078179 A CN 200710078179A CN 101016627 A CN101016627 A CN 101016627A
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Abstract
The invention discloses a surface disposing method of electron alloys work piece, which is characterized by the following: including work piece fore treatment, chemical transformation treatment, drying treatment and washing treatment of each interprocess; dipping electron alloys work piece into inverting liquid of main filming matter and assistance filming matter as chemical transformation treatment; setting main filming matter as one or several zircon salt, manganic salt, molybdate and tungstate and so on transient metal salt; converting to Na2MoO4.2H2O content with density at 5-150g/L; setting the assistance filming matter as one or several nitrate and sulfate of lithium, sodium and potassium alkali metal; converting to LiNO3 content with density at 0.5-20g/L and pH value of inverting liquid at 2-6; controlling the disposing temperature at 10-90 deg.c and disposing time at 5-30 min. This surface film possesses properties of protection and decoration.
Description
Technical field
The present invention relates to technical field of magnesium alloy surface treatment, be specifically related to a kind of environment-friendly type preparation method of magnesium alloy work-piece surface protected decoration film.
Background technology
Magnesium alloy is little because of density, specific tenacity is high, processing welding and damping capacity is good and dimensional stabilizing, advantage such as cheap, easy to be recycled are described as " 21 century green engineering material ", and application is more widely arranged in fields such as machinofacture, automobile making, aerospace, electronics, military affairs, communication, opticinstrument, computers.But the corrosion resisting property of magnesium alloy is very poor, all corrodes easily in moist atmosphere or acidity, neutrality, weakly alkaline solution, and this has hindered applying of magnesium alloy to a great extent.In addition, along with the development of society, people not only require magnesium alloy workpiece not perishable, but also require it to have certain color and luster, as electronic product shell such as the notebook computer made for magnesium alloy materials, mobile phone, extremely people's the favor of bright-coloured color and luster; And be used for the magnesium alloy materials of military aircraft or other defence product, then require the color and luster of material darker and not reflective.Therefore, adopt suitable surface treatment when improving the magnesium alloy workpiece corrosion resisting property, to give its certain color and luster, promptly prepare the ornamental rete of magnesium alloy surface protective, for promoting that Application of Magnesium is significant.
The preparation method of the ornamental rete of existing magnesium alloy surface protective is mainly after the anodic oxidation electrolytic coloring again, and (as publication number is CN 1632179A, application number is 200410067814.3 " two-step pigmenting method for green oxidation film layer on magnesium alloy surface ") or anodic oxidation after chemical staining (as publication number is CN 1405362A, and application number is 02142663.5 " colorize method of magnesium material and utilize this painted magnesium material shell ") again.Can have protection and decorate properties concurrently by the painted anodic film of these prepared, but these technologies can't be handled complex-shaped workpiece on the one hand, more thereby have shortcomings such as treatment process complexity, cost height, cycle are long because relate to step on the other hand.Therefore, exploitation is more easy, can to form the preparation technology of protected decoration film at the different shape magnesium alloy work-piece surface very necessary and urgent.
Chemical conversion is handled as the etch-proof a kind of important method of Mg alloy surface, can magnesium alloy workpiece be contacted with conversion fluid by methods such as dipping, sprays, because matrix metal and conversion fluid generation chemical reaction, can generate the passive film that constitutes by oxide compound or metal-salt at workpiece surface, thereby improve the antiseptic property of workpiece.This method can be handled complex-shaped workpiece, and treatment process is very easy.But contain heavy metal ion Cr usually in traditional magnesium alloy chemical conversion treating solution
6+, toxicity is big, and environmental pollution is serious.Though number being " a kind of surface treatment method of Mg alloy " (publication number is CN 1632169A) of 200510200038.4, recent disclosed Chinese patent application provide a kind of conversion fluid to realize not containing deleterious Cr
6+, but remain that the superficial film color and luster that makes at it is single, decorate properties is strong, in problems such as application facet are subject to many limitations.
Summary of the invention
At the deficiency that above-mentioned prior art exists, the purpose of this invention is to provide a kind of method for the treatment of magnesium alloy work-piece surface different shape magnesium alloy workpiece, that treatment process is simple and cost is low, the gained rete has protection and decorate properties concurrently of handling.
The object of the present invention is achieved like this: a kind of method for the treatment of magnesium alloy work-piece surface, technical process comprise workpiece pretreatment procedure, chemical conversion treatment process and drying process, and the washing step of each inter process, pure water are washed operation; Its key feature is: the chemical conversion treatment process is that magnesium alloy workpiece is immersed with transition metal salt is that main filmogen, an alkali metal salt are to carry out in the conversion fluid of auxiliary film forming matter, conversion fluid pH value is controlled at 2～6, treatment temp is controlled at 10～90 ℃, and the treatment time is 5～30 minutes; Transition metal salt is one or more in zirconates, manganese salt, molybdate, the tungstate, is converted into Na
2MoO
42H
2O content, main filmogen concentration is 5～150g/L; An alkali metal salt is one or more in lithium nitrate, Lithium Sulphate, SODIUMNITRATE, sodium sulfate, saltpetre, the vitriolate of tartar, is converted into LiNO
3Content, auxiliary film forming matter concentration are 0.5～20g/L; Conversion fluid pH value is regulated by phosphoric acid or sulfuric acid, potassium hydroxide or sodium hydroxide.
Its feature also comprises:
1. pretreatment procedure is washed operation, caustic wash process, Warm Wash operation, washing step, pure water by degreasing process, washing step, pure water and is washed operation, pickling process, washing step, pure water and wash operation and constitute, wherein degreasing fluid consists of: commercial metal cleaner 3-5wt%, and all the other are pure water; Skimming temp is controlled at 20～60 ℃, and degreasing time was controlled at 1～20 minute; Alkaline wash consists of: sodium hydroxide 5～50g/L, yellow soda ash 1～50g/L, sodium bicarbonate 1～50g/L, and all the other are pure water; The alkali cleaning temperature is controlled at 40～60 ℃, and the alkali cleaning time was controlled at 3～20 minutes; Pickle solution consists of: nitric acid 1～50g/L, and all the other are pure water; Pickling temperature is controlled at 15～35 ℃, and the pickling time was controlled at 1～50 second;
2. drying process adopts freezing air to dry up, and temperature is 10～25 ℃, and the time is 2～20 minutes;
3. washing step is 1 road, and except that the Warm Wash process temperature after the alkali cleaning is 40～60 ℃, other washing step temperature all are controlled at 10～30 ℃.
Rete decorate properties of the present invention is meant its color and luster; The regulation and control of rete color and luster are based on filmogen and magnesium alloy workpiece generation chemical reaction in the conversion fluid, can obtain having transition metal hydroxide, oxide compound, the salt of certain color under different pH values, thereby make rete show specific color and luster.
Being used for surface-treated magnesium alloy of the present invention is AZ series magnesium alloy die casting, but can be not limited thereto series, this form magnesium alloy.
The beneficial effect that the present invention reached is: the magnesium alloy work-piece surface rete of preparation has protection and decorate properties concurrently, and its solidity to corrosion reaches with the paint film bonding force and is not less than through containing Cr
6+Conversion fluid handle the rete obtain, various and color and luster homogeneity of its color and luster and durability degree are not inferior to the rete that obtains through electrolytic coloring or chemical staining.This has realized the combination of magnesium alloy work-piece surface antiseptic property and decorate properties on environmental friendliness, resource-effective basis, widened the Application of Magnesium field greatly.Its concrete advantage is as follows:
1, handle the conversion film obtain having good corrosion resistance, good combination power concurrently and to have different color and lusters such as silver color, grey, golden yellow, purple, brown, brown by a step chemical conversion, and the rete color and luster is even, weather resistance is good;
2, do not contain Cr in the treatment solution
6+Deng harmful metal ion, environment protecting is good;
3, the conversion fluid composition is simple, and required equipment is simple and easy, and to the no requirement (NR) of workpiece shape, treatment process is easy;
4, treatment temp is moderate, and the treatment time is short, and energy consumption is little.
Description of drawings:
Fig. 1 is a process flow sheet of the present invention.
Embodiment
A kind of method for the treatment of magnesium alloy work-piece surface proposed by the invention, its technical process comprises workpiece pretreatment procedure, chemical conversion treatment process and drying process, and the washing step of each inter process, pure water are washed operation.
Pretreatment procedure is washed operation, caustic wash process, Warm Wash operation, washing step, pure water by degreasing process, washing step, pure water and is washed operation, pickling process, washing step, pure water and wash operation;
Wherein, degreasing fluid consists of: commercial metal cleaner (as the spring river board metal cleaner of chemical plant, the Changjiang river, Shanghai production) 3-5wt%, and all the other are pure water; Skimming temp is controlled at 20～60 ℃; Degreasing time was controlled at 1～20 minute;
Alkaline wash consists of: sodium hydroxide 5～50g/L, yellow soda ash 1～50g/L, sodium bicarbonate 1～50g/L, and all the other are pure water; The alkali cleaning temperature is controlled at 40～60 ℃; The alkali cleaning time was controlled at 3～20 minutes;
Pickle solution consists of: nitric acid 1～50g/L, and all the other are pure water; Pickling temperature is controlled at 15～35 ℃; The pickling time was controlled at 1～50 second.
Committed step of the present invention is the chemical conversion treatment process, and being about to the magnesium alloy workpiece immersion is that main filmogen, an alkali metal salt are to carry out in conversion fluid auxiliary film forming matter, certain pH value with transition metal salt.
Contain transition metal salt and an alkali metal salt in the used conversion fluid of chemical conversion treatment process, conversion fluid pH value is controlled at 2～6, and treatment temp is controlled at 10～90 ℃, and the treatment time is 5～30 minutes.Transition metal salt is one or more in zirconates, manganese salt, molybdate and the tungstate, is converted into Na
2MoO
42H
2O content, main filmogen concentration is 5～150g/L.An alkali metal salt is one or more in lithium nitrate, Lithium Sulphate, SODIUMNITRATE, sodium sulfate, saltpetre, the vitriolate of tartar, is converted into LiNO
3Content, auxiliary film forming matter concentration are 0.5～20g/L.Conversion fluid pH value is regulated by phosphoric acid or sulfuric acid, potassium hydroxide or sodium hydroxide.
Drying process adopts freezing air to dry up, and temperature is 10～25 ℃, and the time is 2～20 minutes.
Washing step is 1 road, and except that the Warm Wash process temperature after the alkali cleaning is 40～60 ℃, other washing step temperature all are controlled at 10～30 ℃.
(1) film quality check
A. visual testing visual inspection rete whether complete, continuous, have zero defect, color and luster whether even.
B. spot test check membranous layer corrosion resistance energy is adopted in solidity to corrosion check, and the drop time is long more to show that anti-corrosion effect is good more.The point dropping liquid consists of: potassium permanganate 0.05g, concentrated nitric acid (1mL of ρ=1.42g/mL), pure water 100mL; The endpoint condition is: some dropping liquid red-purple disappears; The drop temperature is controlled at 25 ℃; Parallel laboratory test 3 times.
C. paint film bonding force check
Adopt cross-hatching to measure the bonding force of conversion film and paint film.Promptly handling the specimen surface japanning and drying.Be divided into 100 little lattice with pocket knife at interval with 1mm, press sticking cellophane tape thereon, and then adhesive tape is uncovered, observe the little lattice of residue paint film on sample, represent with percentage ratio.Percentage ratio is big more to show that the bonding force of conversion film and paint film is good more.
D. weather resistance check is placed certain hour with the film forming workpiece in room air, and visual inspection rete color and luster has no change, rete to have or not to come off and corrodes.
(2) specific embodiment
The magnesium alloy of selecting for use is the AZ91 die casting, and specification is 35mm * 20mm * 3.0mm magnesium sheet, respectively with waterproof abrasive paper polish step by step to 1000#, washing, pure water wash, acetone wiping, washing, pure water are washed, freezing air dries up.In degreasing fluid, handled 5 minutes down, carry out the washing of 1 road then, 1 road pure water is washed in 30 ℃; In alkaline wash, handled 10 minutes down again, carry out 1 road Warm Wash, the washing of 1 road, 1 road pure water then and wash in 60 ℃; In pickle solution, handled 15 seconds down again, carry out the washing of 1 road then, 1 road pure water is washed in 25 ℃; Carry out chemical conversion afterwards and handle, carry out the washing of 1 road then, 1 road pure water is washed; Last freezing air dries up.Among following 6 embodiment the pre-treating technology of all workpiece all as mentioned above, chemical conversion handles that used conversion fluid is formed and pH value, treatment condition and film quality assay are as follows:
Embodiment 1:
Conversion fluid is formed: Sodium orthomolybdate [Na
2MoO
42H
2O] 48g/L;
Lithium nitrate [LiNO
3] 5g/L.
Conversion fluid pH value is 4.
Treatment condition: 80 ℃ of temperature, 5 minutes time.
The film quality assay: rete be lilac, continuously, zero defect, spot test result 76 seconds, paint film bonding force 100%, workpiece is placed after 425 days color and luster no change, rete not to be had and comes off and corrosion phenomenon.
Embodiment 2:
Conversion fluid is formed: Sodium orthomolybdate [Na
2MoO
42H
2O] 150g/L;
SODIUMNITRATE [NaNO
3], Lithium Sulphate [Li
2SO
4H
2O] 20g/L (is converted into LiNO
3Content).
Conversion fluid pH value is 3.
Treatment condition: 60 ℃ of temperature, 15 minutes time.
The film quality assay: rete be brown, continuously, zero defect, spot test result 142 seconds, paint film bonding force 100%, workpiece is placed after 425 days color and luster no change, rete not to be had and comes off and corrosion phenomenon.
Embodiment 3:
Conversion fluid is formed: zirconium sulfate [ZrSO
44H
2O] 5g/L (is converted into Na
2MoO
42H
2The content of O);
Lithium Sulphate [Li
2SO
4H
2O] 1.5g/L (is converted into LiNO
3Content).
Conversion fluid pH value is 5.
Treatment condition: 40 ℃ of temperature, 10 minutes time.
The film quality assay: rete be silver gray, continuously, zero defect, spot test result 83 seconds, paint film bonding force 100%, workpiece is placed after 425 days color and luster no change, rete not to be had and comes off and corrosion phenomenon.
Embodiment 4:
Conversion fluid is formed: zirconium sulfate [ZrSO
44H
2O] 12g/L (is converted into Na
2MoO
42H
2The content of O);
Saltpetre [KNO
3] 0.5g/L (is converted into LiNO
3Content).
Conversion fluid pH value is 2.
Treatment condition: 10 ℃ of temperature, 30 minutes time.
The film quality assay: rete be light brown, continuously, zero defect, spot test result 107 seconds, paint film bonding force 100%, workpiece is placed after 425 days color and luster no change, rete not to be had and comes off and corrosion phenomenon.
Embodiment 5:
Conversion fluid is formed:
Sodium wolframate [Na
2WO
42H
2O], Sodium orthomolybdate 86g/L (is converted into Na
2MoO
42H
2The content of O);
Sodium sulfate [Na
2SO
4] 13g/L (is converted into LiNO
3Content).
Conversion fluid pH value is 6.
Treatment condition: 20 ℃ of temperature, 20 minutes time.
The film quality assay: rete is faint yellow, continuous, zero defect, spot test result 134 seconds, and paint film bonding force 100%, workpiece is placed after 425 days color and luster no change, rete not to be had and comes off and corrosion phenomenon.
Embodiment 6:
Conversion fluid is formed:
Manganous sulfate [MnSO
4H
2O], zirconium sulfate [ZrSO
44H
2O] 126g/L (is converted into Na
2MoO
42H
2The content of O);
Lithium Sulphate [Li
2SO
4H
2O], saltpetre [KNO
3] 7.2g/L (is converted into LiNO
3Content).
Conversion fluid pH value is 4.5.
Treatment condition: 90 ℃ of temperature, 8 minutes time.
The film quality assay: rete be golden yellow, continuously, zero defect, spot test result 156 seconds, paint film bonding force 100%, workpiece is placed after 425 days color and luster no change, rete not to be had and comes off and corrosion phenomenon.
As mentioned above, do not contain deleterious Cr in the used chemical conversion solution of the present invention
6+Plasma; Magnesium alloy workpiece corrosion resisting property after the processing reaches with the paint film bonding force and is not less than through containing Cr
6+The workpiece handled of conversion fluid; Magnesium alloy workpiece after the processing can have different color and lusters, and color and luster homogeneity and durability degree are not inferior to the workpiece through electrolytic coloring or chemical staining.
Claims (4)
1, a kind of method for the treatment of magnesium alloy work-piece surface, technical process comprises workpiece pretreatment procedure, chemical conversion treatment process and drying process, and the washing step of each inter process, pure water are washed operation; It is characterized in that:
1. pretreatment procedure is that degreasing process, washing step, pure water are washed operation, caustic wash process, Warm Wash operation, washing step, pure water and washed operation, pickling process, washing step and pure water and wash operation; Wherein degreasing fluid consists of: commercial metal cleaner 3-5wt%, and all the other are pure water; Skimming temp is controlled at 20～60 ℃, and degreasing time was controlled at 1～20 minute; Alkaline wash consists of: sodium hydroxide 5～50g/L, yellow soda ash 1～50g/L, sodium bicarbonate 1～50g/L, and all the other are pure water; The alkali cleaning temperature is controlled at 40～60 ℃, and the alkali cleaning time was controlled at 3～20 minutes; Pickle solution consists of: nitric acid 1～50g/L, and all the other are pure water; Pickling temperature is controlled at 15～35 ℃, and the pickling time was controlled at 1～50 second;
2. chemical conversion treatment process is that magnesium alloy workpiece is immersed with transition metal salt is that main filmogen, an alkali metal salt are to carry out in the conversion fluid of auxiliary film forming matter, conversion fluid pH value is controlled at 2～6, treatment temp is controlled at 10～90 ℃, and the treatment time is 5～30 minutes;
3. drying process adopts freezing air to dry up, and temperature is 10～25 ℃, and the time is 2～20 minutes;
4. washing step is 1 road, and except that the Warm Wash process temperature after the alkali cleaning is 40～60 ℃, other washing step temperature all are controlled at 10～30 ℃.
2, method for the treatment of magnesium alloy work-piece surface according to claim 1 is characterized in that, described conversion fluid master filmogen transition metal salt is one or more in zirconates, manganese salt, molybdate and the tungstate, is converted into Na
2MoO
42H
2O content, its concentration are 5～150g/L.
3, method for the treatment of magnesium alloy work-piece surface according to claim 1 is characterized in that, described conversion fluid auxiliary film forming matter an alkali metal salt is one or more in lithium nitrate, Lithium Sulphate, SODIUMNITRATE, sodium sulfate, saltpetre and the vitriolate of tartar, is converted into LiNO
3Content, its concentration are 0.5～20g/L.
4, method for the treatment of magnesium alloy work-piece surface according to claim 1 is characterized in that, described conversion fluid pH value is regulated by phosphoric acid or sulfuric acid, potassium hydroxide or sodium hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100781792A CN100507076C (en) | 2007-02-06 | 2007-02-06 | Method of treating magnesium alloy work-piece surface |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100781792A CN100507076C (en) | 2007-02-06 | 2007-02-06 | Method of treating magnesium alloy work-piece surface |
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| Publication Number | Publication Date |
|---|---|
| CN101016627A true CN101016627A (en) | 2007-08-15 |
| CN100507076C CN100507076C (en) | 2009-07-01 |
Family
ID=38725850
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|---|---|---|---|
| CNB2007100781792A Expired - Fee Related CN100507076C (en) | 2007-02-06 | 2007-02-06 | Method of treating magnesium alloy work-piece surface |
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