CN102660736A - Magnesium alloy surface conversion treatment liquid and treatment method thereof - Google Patents
Magnesium alloy surface conversion treatment liquid and treatment method thereof Download PDFInfo
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- CN102660736A CN102660736A CN2012101537838A CN201210153783A CN102660736A CN 102660736 A CN102660736 A CN 102660736A CN 2012101537838 A CN2012101537838 A CN 2012101537838A CN 201210153783 A CN201210153783 A CN 201210153783A CN 102660736 A CN102660736 A CN 102660736A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 61
- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 14
- 239000007788 liquid Substances 0.000 title abstract description 7
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims abstract description 26
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims abstract description 19
- 235000002949 phytic acid Nutrition 0.000 claims abstract description 19
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000467 phytic acid Substances 0.000 claims abstract description 18
- 229940068041 phytic acid Drugs 0.000 claims abstract description 18
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 13
- HELHAJAZNSDZJO-OLXYHTOASA-L sodium L-tartrate Chemical compound [Na+].[Na+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O HELHAJAZNSDZJO-OLXYHTOASA-L 0.000 claims abstract description 13
- 239000001433 sodium tartrate Substances 0.000 claims abstract description 13
- 229960002167 sodium tartrate Drugs 0.000 claims abstract description 13
- 235000011004 sodium tartrates Nutrition 0.000 claims abstract description 13
- 238000005238 degreasing Methods 0.000 claims abstract description 7
- 238000009996 mechanical pre-treatment Methods 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 12
- 239000011734 sodium Substances 0.000 claims description 12
- 229960004418 trolamine Drugs 0.000 claims description 12
- 238000005554 pickling Methods 0.000 claims description 6
- 229910052708 sodium Inorganic materials 0.000 claims description 6
- 239000004576 sand Substances 0.000 claims description 2
- 238000004381 surface treatment Methods 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 abstract description 11
- 230000007797 corrosion Effects 0.000 abstract description 10
- 238000000576 coating method Methods 0.000 abstract description 8
- 239000011248 coating agent Substances 0.000 abstract description 7
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052804 chromium Inorganic materials 0.000 abstract description 4
- 239000011651 chromium Substances 0.000 abstract description 4
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 abstract description 3
- 238000005266 casting Methods 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 229910052731 fluorine Inorganic materials 0.000 abstract description 3
- 239000011737 fluorine Substances 0.000 abstract description 3
- 239000004615 ingredient Substances 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract 1
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 40
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 10
- 238000004512 die casting Methods 0.000 description 9
- 239000012530 fluid Substances 0.000 description 6
- 239000011780 sodium chloride Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 230000004580 weight loss Effects 0.000 description 5
- 244000137852 Petrea volubilis Species 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000005498 polishing Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000006025 fining agent Substances 0.000 description 3
- 238000005470 impregnation Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000003672 processing method Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 229910000600 Ba alloy Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- VZDYWEUILIUIDF-UHFFFAOYSA-J cerium(4+);disulfate Chemical compound [Ce+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VZDYWEUILIUIDF-UHFFFAOYSA-J 0.000 description 1
- 229910000355 cerium(IV) sulfate Inorganic materials 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910001430 chromium ion Inorganic materials 0.000 description 1
- 238000007739 conversion coating Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
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Abstract
The invention relates to magnesium alloy surface conversion treatment liquid and a treatment method thereof. The magnesium alloy surface conversion treatment liquid comprises the following components of: 5 to 45 g/l of phytic acid, 0.1 to 3 g/l of calcium nitrate, 0.1 to 5 g/l of sodium tartrate and 0.1 to 3 g/l of ammonium metavanadate. The magnesium alloy surface conversion treatment method comprises the following steps of: performing mechanical pretreatment; deoiling and degreasing; performing acid washing; converting; and drying. The magnesium alloy surface conversion treatment liquid does not contain environmental pollution ingredients of chromium, fluorine and the like, the treatment method is simple and high in efficiency, and the compactness of film layers and the corrosion resistance and adhesive force of magnesium alloy organic coatings can be improved. The magnesium alloy surface conversion treatment liquid can be widely applied to the surface coating pretreatment of magnesium alloy castings, section bars and magnesium alloy products.
Description
Technical field
The present invention relates to a kind of surface conversion treatment liquid and treatment process thereof, be specifically related to magnesiumalloy conversion treating solution and transformation processing method.
Background technology
Magnesiumalloy has specific tenacity and specific rigidity height, good casting property, electric shielding and characteristics such as damping capacity excellence and recyclable utilization, is widely used in fields such as aerospace, automobile and motorcycle, instrument, telecommunications, opticinstrument, computingmachine manufacturing.(2.36V), and volume ratio＜1 of natural oxide film and metal itself, be not enough to protect magnesium alloy substrate, corrosion resisting property is poor because the electropotential of magnesiumalloy is extremely negative.In order to improve the corrosion resisting property of Mg alloy surface, many protection processing methods are developed in succession, as: chemical conversion, anodic oxidation, differential arc oxidation, metal cover, vapour deposition and organic coating etc.Wherein chemical transformation have that technology is simple, with low cost, the influence that do not receive the workpiece shape and size and receive much concern with advantages such as the organic coating bonding force are strong.Chemical transformation can be divided into two kinds of chromate conversion method and Chrome-free conversion methods by whether containing chromium in the treatment solution.The chromate conversion technical maturity, the conversion film excellent property, but contain deleterious chromium ion in the treatment solution, human body and environment there are great harm.Therefore, the exploitation of environment-friendly type treatment solution and treatment process becomes the inexorable trend of chemical conversion treatment reason.
Because the magnesium alloy chemical activity is high; So far untappedly go out singlely to solve magnesiumalloy method of inhibiting corrosion under severe condition; Need further application or sealing of hole to handle after magnesiumalloy process chemical conversion or the anodize, significantly to improve the corrosion stability of magnesium alloy ability.Therefore, application pre-treatment film require to have good corrosion resisting property and with the bonding force of paint film.
The patent No. is 200710307863.3 patent of invention " a kind of film-forming soln of magnesium alloy chemical conversion film and the preparation method of this conversion film "; Adopt ceric sulfate 10～80g/l, sulfuric acid 3～60ml/l, phytic acid 1～10ml/l, inhibiter 0.5～5g/l and the formulated aqueous solution of buffer reagent 0.5～5g/l to prepare conversion film; It is good that this transforms rete compactness; Anti-corrosion and wear resisting property are good, and be higher with basic unit sticking power.But contain REE in this solution, cost is higher.
Publication number is that CN102268668A patent " preparation method of magnesium alloy surface conversion coating " employing concentration is the phytic acid conversion film of 1～25g/l formulations prepared from solutions trivalent and the above metal of trivalent; This technology agents useful for same all belongs to environmentally friendly, and conversion film and organic varnish binding force of membrane are good.Solution component has only phytic acid, influences the film forming efficiency and the stability of conversion fluid.
In addition, the phosphate conversion film corrosion resisting property that magnesiumalloy is commonly used is better, be good application bottom, but conversion film is prone to the phenomenon that crackle is roomy, crystal grain is thick.
Summary of the invention
The objective of the invention is to propose the magnesiumalloy conversion treating solution of a kind of Chrome-free, free-floride, is to add inhibiter, crystallization fining agent, promotor through phytic acid, can improve the solidity to corrosion and the sticking power of rete density and magnesiumalloy organic coating.
Another object of the present invention is simple, the efficient transformation processing method that proposes a kind of magnesiumalloy.
Magnesiumalloy conversion processing fluid component of the present invention and content are: phytic acid: 5～45g/l, nitrocalcite: 0.1～3g/l, sodium tartrate: 0.1～5g/l and ammonium meta-vanadate: 0.1～3g/l.
Magnesiumalloy conversion treating solution preferred ingredients of the present invention and content are: phytic acid: 15～25g/l, nitrocalcite: 1～2g/l, sodium tartrate: 2～4g/l and ammonium meta-vanadate: 0.5～1.5g/l.
Best component and the content of magnesiumalloy conversion treating solution of the present invention is: phytic acid: 20g/l, nitrocalcite: 2g/l, sodium tartrate: 1g/l and ammonium meta-vanadate: 2g/l.
The surface treatment method of Mg alloy of conversion treating solution of the present invention is:
1. mechanical pretreatment: with 400～1000# sand papering Mg alloy surface;
2. oil removing degreasing: with the NaOH of massfraction 5～10%, 5～10% Na
2SiO
3With the triethanolamine solution of 5g/l, temperature is 45～55 ℃ and handled 1～2 minute;
3. pickling: use H
3PO
415～25g/l and Na
3PO
410～20g/l solution, room temperature treatment 10 seconds～2 minutes;
4. transform: the magnesiumalloy of above-mentioned processing is immersed the conversion treating solution with trolamine adjustment pH value to 1.5～5, room temperature treatment 5～30 minutes;
5. oven dry: dried 2～10 minutes down or dry up at 105 ± 5 ℃.
Do not contain environmental pollution type compositions such as chromium, fluorine in the conversion treating solution of the present invention, belong to environmentally friendly.The phytic acid component is main membrane-forming agent in the conversion treating solution; Concentration is 5～45g/l, under acidic conditions, forms insoluble phytate with magnesiumalloy interface and metal ion-chelant, and phytic acid concentration is adjustable in specialized range; Excessive concentration is prone to complex compound, and the low excessively film forming that is prone to is imperfect.The nitrocalcite component is a promotor, and concentration is 0.1～3g/l, quickens the formation of conversion film; Make conversion film interior film forming of short period of time at room temperature; Nitrocalcite concentration is adjustable in specialized range, but excessive concentration is prone to form inner complex with phytic acid appearance deposition when pH is higher.Ammonium meta-vanadate is the crystallization fining agent, is concentration 0.1～3g/l, makes the conversion film crystallization careful, even; Improve the density and the quality of conversion film; Ammonium meta-vanadate concentration is adjustable in specialized range, but excessive concentration is prone to lost the effect of crystallization fining agent by nitrate ion reacted vanadous oxide.Sodium tartrate is an inhibiter, and concentration is 0.1～5g/l, and the stabilizing solution potential of hydrogen is in the useful range conversion treating solution for a long time, and sodium tartrate concentration is adjustable in specialized range, and excessive concentration is prone to complex compound.Magnesiumalloy conversion treating solution of the present invention can make AZ series and ZK series magnesiumalloy film forming within the several minutes at room temperature, the rete good compactness, solidity to corrosion is good, with the strong adhesion of base material and top coat.Conversion treating solution of the present invention does not contain environmental pollution compositions such as chromium, fluorine, and treatment process is simple, efficient, can be widely used in the external coating pre-treatment of Mg alloy castings, section bar and magnesium alloy product.
Description of drawings
Fig. 1 is the surface microscopic topographic of embodiment 5 conversion films;
Fig. 2 is conversion film and the corrosion weight loss comparison diagram of die casting AZ91D in the 5%NaCl aqueous solution of embodiment;
Fig. 3 is the organic coating sticking power test pattern of embodiment 5 conversion films.
Embodiment
Embodiment 1
Magnesiumalloy conversion processing fluid component and content are phytic acid: 20g/l, nitrocalcite: 2g/l, sodium tartrate: 1g/l and ammonium meta-vanadate: 2g/l.
Magnesiumalloy conversion processing fluid component and content are phytic acid: 5g/l, nitrocalcite: 1g/l, sodium tartrate: 0.5g/l and ammonium meta-vanadate: 0.2g/l.
Embodiment 3
Magnesiumalloy conversion processing fluid component and content are phytic acid: 45g/l, nitrocalcite: 3g/l, sodium tartrate: 0.2g/l and ammonium meta-vanadate: 1g/l.
Magnesiumalloy conversion processing fluid component and content are phytic acid: 15g/l, nitrocalcite: 0.2g/l, sodium tartrate: 4.5g/l and ammonium meta-vanadate: 3g/l.
Embodiment 5
1. mechanical pretreatment: with 400～1000# sand paper die casting AZ91D Mg alloy surface of polishing successively;
2. oil removing degreasing: with the NaOH of massfraction 8%, 8% Na
2SiO
3With the triethanolamine solution of 5g/l, temperature is 45 ℃ and handled 2 minutes;
3. pickling: use H
3PO
420g/l and Na
3PO
415g/l solution, room temperature treatment 30 seconds;
4. transform: with the conversion treating solution pH value to 4 of trolamine adjustment embodiment 1, the magnesiumalloy with above-mentioned processing under the room temperature condition left standstill in conversion treating solution 10 minutes;
5. dry up.
Is being 8% through the die casting AZ91D magnesiumalloy after the above-mentioned processing through the weight loss after 10 days 5%NaCl solution impregnation, and follow-up organic coating is drawn the lattice test, and its sticking power reaches 0 grade.
Embodiment 6
1. mechanical pretreatment: with 400～1000# sand paper die casting AZ91D Mg alloy surface of polishing successively;
2. oil removing degreasing: with the NaOH of massfraction 5%, 10% Na
2SiO
3With the triethanolamine solution of 5g/l, temperature is 50 ℃ and handled 1 minute;
3. pickling: use H
3PO
415g/l and Na
3PO
410g/l solution, room temperature treatment 60 seconds;
4. transform: with the conversion treating solution pH value to 2 of trolamine adjustment embodiment 2, the magnesiumalloy with above-mentioned processing under the room temperature condition left standstill in conversion treating solution 5 minutes;
5. dry up.
Through the weight loss of the die casting AZ91D after the above-mentioned processing after flooding through 10 days 5%NaCl Ji liquid is 70%.
Embodiment 7
1. mechanical pretreatment: with 400～1000# sand paper die casting AZ91D Mg alloy surface of polishing successively;
2. oil removing degreasing: with the NaOH of massfraction 10%, 5% Na
2SiO
3With the triethanolamine solution of 5g/l, temperature is 45 ℃ and handled 1 minute;
3. pickling: use H
3PO
420g/l and Na
3PO
45g/l solution, room temperature treatment 40 seconds;
4. transform: with the conversion treating solution pH value to 3 of trolamine adjustment embodiment 3, the magnesiumalloy with above-mentioned processing under the room temperature condition left standstill in conversion treating solution 15 minutes;
5. dry up.
Is being 50% through the die casting AZ91D after the above-mentioned processing through the weight loss after 10 days 5%NaCl solution impregnation.
Embodiment 8
1. mechanical pretreatment: with 400～1000# sand paper die casting AZ91D Mg alloy surface of polishing successively;
2. oil removing degreasing: with the NaOH of massfraction 10%, 10% Na
2SiO
3With the triethanolamine solution of 5g/l, temperature is 50 ℃ and handled 1 minute;
3. pickling: use H
3PO
4The 20g/ Na that gets along well
3PO
415g/l solution, room temperature treatment 20 seconds;
4. transform: with the conversion treating solution pH value to 2.6 of trolamine adjustment embodiment 2, the magnesiumalloy with above-mentioned processing under the room temperature condition left standstill in conversion treating solution 20 minutes;
5. dry up.
Is being 18% through the die casting AZ91D after the above-mentioned processing through the weight loss after 10 days 5%NaCl solution impregnation.
Claims (4)
1. a Mg alloy surface conversion treating solution is characterized in that component and content are: phytic acid: 5～45g/l, nitrocalcite: 0.1～3g/l, sodium tartrate: 0.1～5g/l and ammonium meta-vanadate: 0.1～3g/l.
2. conversion treating solution according to claim 1 is characterized in that component and content are: phytic acid: 15～25g/l, nitrocalcite: 1～2g/l, sodium tartrate: 2～4g/l and ammonium meta-vanadate: 0.5～1.5g/.
3. conversion treating solution according to claim 1 is characterized in that component and content are: phytic acid: 20g/l, nitrocalcite: 2g/l, sodium tartrate: 1g/l and ammonium meta-vanadate: 2g/l.
4. the surface treatment method of Mg alloy of conversion treating solution according to claim 1 is characterized in that:
1) mechanical pretreatment: with 400～1000# sand papering Mg alloy surface;
2) oil removing degreasing: with the NaOH of massfraction 5～10%, 5～10% Na
2SiO
3With the triethanolamine solution of 5g/l, temperature is 45～55 ℃ and handled 1～2 minute;
3) pickling: use H
3PO
415～25g/l and Na
3PO
410～20g/l solution, room temperature treatment 10 seconds～2 minutes;
4) transform: the magnesiumalloy of above-mentioned processing is immersed the conversion treating solution with trolamine adjustment pH value to 1.5～5, room temperature treatment 5～30 minutes;
5) oven dry: dried 2～10 minutes down or dry up at 105 ± 5 ℃.
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Cited By (10)
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| CN104120421A (en) * | 2014-08-12 | 2014-10-29 | 钱宏彬 | Chromium-free chemical conversion membrane treatment agent of magnesium alloy and preparation method thereof |
| CN107245710A (en) * | 2017-05-11 | 2017-10-13 | 安徽省金寨县新诚机械制造有限公司 | A kind of environmentally friendly surface treatment liquid of magnesium alloy |
| CN111534815A (en) * | 2020-05-22 | 2020-08-14 | 山东大学 | Pretreatment liquid capable of forming washable natural color conversion film on metal surface and preparation method thereof |
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| CN102660736B (en) | 2013-10-30 |
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