CN101392397A - Electrochemistry processing method for generating oxide film on surface of aluminium or aluminium alloy material - Google Patents
Electrochemistry processing method for generating oxide film on surface of aluminium or aluminium alloy material Download PDFInfo
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Abstract
The invention relates to an electrochemical treatment method for forming oxide film on the surface of aluminum or aluminums alloy material, pertaining to the surface protection and finishing field of aluminum or aluminum alloys. The aluminum or aluminum alloy is placed in a compound electrolyte solution, with oxidation by alternating current, and then a film with the thickness of 10-30Mum, hardness 200-450HV and excellent finishing performance can be produced. The compound electrolyte solution is composed of aromatic dicarboxylic acid and derivatives of aromatic dicarboxylic acid, aliphatic carboxylic acid and ammonium salt or organic amine compounds. The work pieces to be oxidized are hung at the two ends of AC electrode while being oxidized; therefore, the efficiency of electro-oxidation in alternating current is one time higher than the efficiency of electro-oxidation in direct current and simultaneously the rectifying installation is saved. The electrochemical treatment method solves the problems such as thinness (less than 10Mum), yellowing and low hardness of the oxide film produced by sulfuric acid alternating current.
Description
Technical field
The present invention relates to the electrochemical process for treating that a kind of aluminum or aluminum alloy material surface generates oxide film, be used for the aluminum or aluminum alloy surfacecti proteon and decorate the field.
Background technology
The electrochemical oxidation of aluminium and alloy thereof is an aluminium surface-treated important means, and direct current is adopted in the research of alumilite process mostly, and less to the research of adopting AC Anodizing.AC Anodizing is a kind of without rectifying installation, and directly uses the method for oxidation of the commercially available alternating-current after the step-down.But two electrode workpiece simultaneous oxidation during ac oxide need not can use big electric current to realize high-speed oxidation to utmost point material, therefore compares with the direct current oxidation style, has efficient height, energy-conservation, low cost and other advantages, is paid close attention to by people always.The sulfuric acid AC Anodizing is used early, but because there is the restriction of cathodic process and electrolytic solution self in alternating-current, the rete that is obtained is thinner, porosity and transparency height, hardness is low, wears no resistance, the rete jaundice is difficult to obtain the rete of thickness greater than 10 μ m, thereby has limited its application.The bottom and the less demanding protection of the workpiece-ornamental oxidation film layer that are mainly used in production of aluminium electric wire and aluminium application are at present handled.Find by literature search, " corrosion science and guard technology " 1996:8 (2): published the article that people such as Cheng Yufeng introduce sulfuric acid AC Anodizing technology on the 144-148, " additive is to the influence of LY12 cast aluminium alloy ac oxide film properties ", this article proposes to add special additive in sulphuric acid soln, the employing AC Anodizing can be at ambient temperature, at Al-Cu is that direct current is difficult to form thick oxide film on the alloy of oxidation, but above-mentioned research electrolytic solution compositional system complexity, oxidization time is longer, is unfavorable for suitability for industrialized production.Chinese patent publication number 87103213 has proposed to adopt AC Anodizing in sulfuric acid and Tai-Ace S 150 mixed electrolytic solution, form the technology of porous oxide film on the aluminium surface, but the hardness and the wear resisting property of the oxidation film layer that obtains are bad, can not be used for aluminium and alloy surface protected decoration thereof, limit the AC Anodizing The Application of Technology.
Summary of the invention
Purpose of the present invention has aimed to provide a kind of electrochemical process for treating that adopts alternating-current to form layer oxide film on the aluminum or aluminum alloy surface, and this method energy consumption is low, and the gained oxidation film layer has higher hardness, thickness and decorate properties.
The objective of the invention is to realize in the following manner:
The aluminum or aluminum alloy workpiece is hung over the electrode two ends, place composite electrolytic solution, in 2min, voltage of alternating current is adjusted to set(ting)value from zero, and remains unchanged; Current density raises along with voltage and increases, reach peak current density after, along with the formation of rete, current density reduces gradually, finishes until film forming; Behind ac oxide, generate the oxide film that one deck has higher hardness, thickness and decorate properties on the aluminum or aluminum alloy surface; Described composite electrolytic solution is made up of aromatic carboxylic acid and derivative (containing 6～15 carbon atoms), aliphatic carboxylic acid (containing 2～8 carbon atoms) and ammonium salt or organic amine compound.
Aromatic carboxylic acid and derivatives concentration thereof are that 40～100g/L, aliphatic carboxylic acid concentration are that 10～60g/L, ammonium salt or organic amine compound concentration are 20～50g/L in the composite electrolytic solution.
Described aromatic carboxylic acid and derivative thereof are benzene hexacarboxylic acid, sulfophthalic acid or Phenylsulfonic acid; Aliphatic carboxylic acid is citric acid, oxysuccinic acid, oxalic acid, tartrate, propanedioic acid or lactic acid; Ammonium salt or organic amine compound are ammonium phosphate, ammonium citrate, methylamine or trolamine.
The voltage of alternating current set(ting)value is 60～120V.
Power supply adopts the AC power of 50Hz, and voltage is adjusted to 60～120V from 0V, peak current density 5～10A/dm
2, 10～20 ℃ of electrolyte temperatures.
Along with the formation of rete, current density descends gradually, finally reduces to 1～2A/dm
2
Aluminium is commercial-purity aluminium, and aluminium alloy is that Al-Cu is that alloy, Al-Si are that alloy, Al-Mg-Si are that alloy or Al-Zn are alloy.
The oxidation film layer color and luster that forms is canescence or grey black, and film forming speed is more than or equal to 1 μ m/min.
The two ends of ac electrode all hang with treats oxidation workpiece, and workpiece is each other to the utmost point.
Aluminium and alloy thereof are placed composite electrolytic solution, adopt the commercially available alternating-current of 50Hz, in 2min, voltage is adjusted to 60～120V from 0V, and remains unchanged, until off-test.Current density raises with voltage and increases, and reaches peak current density 5～10A/dm
2After, along with the formation of rete, current density descends gradually, finally reduces to 1～2A/dm
2
Processing step is as follows:
(1) preparation electrolytic solution
The electrolytic solution that the present invention adopts is the composite electrolytic solution of being made up of aromatic carboxylic acid and derivative, aliphatic carboxylic acid and ammonium salt or organic amine compound.Commercial-purity aluminium can form complete, xanchromatic oxide film in independent aromatic carboxylic acid and derivative electrolytic solution thereof, but voltage is higher in the oxidising process.The interpolation aliphatic carboxylic acid can improve the thickness and the homogeneity of rete, and the adding of ammonium salt or organic amine compound can reduce oxidation voltage and improve the performance of rete.
The concentration range of aromatic carboxylic acid and derivative thereof is 40～100g/L in the composite electrolytic solution that the present invention adopts, and the aliphatic carboxylic acid concentration range is 10～60g/L, and ammonium salt or organic amine compound concentration range are 20～50g/L.
Described aromatic carboxylic acid and derivative thereof are preferably benzene hexacarboxylic acid, sulfophthalic acid, Phenylsulfonic acid etc.; Aliphatic carboxylic acid is preferably citric acid, oxysuccinic acid, oxalic acid, tartrate, propanedioic acid, lactic acid etc.; Ammonium salt or organic amine compound are preferably ammonium phosphate, ammonium citrate, methylamine, trolamine etc.
(2) Chemical Pretreatment
Degreasing (nitric acid massfraction 5%, room temperature, 5min) → washing → alkali cleaning (sodium hydroxide massfraction 50%, 55～60 ℃, 6min) → washing → neutralization (nitric acid massfraction 10%, room temperature, 5min) → washing
(3) AC Anodizing
In that ((10～60g/L)+ammonium salt or organic amine compound are (in 20～50g/L) composite electrolytic solutions of forming for 40～100g/L)+aliphatic carboxylic acid by aromatic carboxylic acid and derivative thereof, in 2min, voltage is adjusted to the value of setting (60～120V), and remain unchanged from 0V.Current density raises along with voltage and increases, and along with the generation of rete, current density reduces gradually, until off-test.Oxidization time: 10～30min, temperature: 10～20 ℃.
(4) drying
After film forming finished, distilled water cleaned, warm air drying.
The present invention also is applicable to the anodic oxidation treatment of various aluminium section bars such as duralumin, cast aluminium and building aluminium alloy except being used for the technical pure anodizing of aluminium.Formed oxidation film layer color and luster difference on different aluminium alloys, rete is on canescence, duralumin and the cast aluminium and is grey black on commercial-purity aluminium and the architectural aluminum section.Oxidizing process parameter oxidation film layer thickness can be 10～30 μ m, hardness is 200～450HV, has good abrasion resistance and decorate properties by adjusting.Electrolytic solution compositional system of the present invention is simple, and environmental pollution is little, meets the development of environmental protection industry, has broken through problems such as sulphuric acid soln AC Anodizing rete thin (less than 10 μ m), jaundice, hardness are low.But two electrode workpiece simultaneous oxidation during ac oxide need not can use big electric current to realize high-speed oxidation to utmost point material, therefore compares with the dc electrolyzing method, has efficient height, energy-conservation, low cost and other advantages.
Embodiment
Following examples are intended to illustrate the present invention rather than limitation of the invention further.The present invention can implement by the described arbitrary mode of summary of the invention.
The present invention utilizes the AC Anodizing technology, in composite electrolytic solution, and control voltage 60～120V, 10～20 ℃ of temperature, oxidization time 10～30min can obtain the oxide film that a layer thickness is 10～30 μ m.
Embodiment 1
Hang on two electrodes through the L3 commercial-purity aluminium after the Chemical Pretreatment, it is of a size of 30mm * 40mm * 1mm.CONTROL PROCESS condition: slowly rise to 120V at 2min inner control voltage, and remain unchanged, until off-test.Current density raises with voltage and increases, and reaches peak current density 8A/dm
2After, along with the generation of rete, current density reduces gradually, finally reduces to 1A/dm
2
Electrolytic solution is formed and processing parameter is:
Benzene hexacarboxylic acid: 40g/L
Citric acid: 60g/L
Ammonium phosphate: 30g/L
Voltage: 120V
Oxidization time: 30min
Temperature: 15 ± 2 ℃
Behind the ac oxide, thicknesses of layers is 28 μ m, and microhardness is 410HV, and rete is canescence.
Embodiment 2
Hang on two electrodes through the L3 commercial-purity aluminium after the Chemical Pretreatment, it is of a size of 30mm * 40mm * 1mm.CONTROL PROCESS condition: slowly rise to 100V at 2min inner control voltage, and remain unchanged, until off-test.Current density raises with voltage and increases, and reaches peak current density 7A/dm
2After, along with the generation of rete, current density reduces gradually.
Electrolytic solution is formed and processing parameter is:
Benzene hexacarboxylic acid: 100g/L
Citric acid: 10g/L
Ammonium phosphate: 20g/L
Voltage: 100V
Oxidization time: 15min
Temperature: 15 ± 2 ℃
Behind the ac oxide, thicknesses of layers is 17 μ m, and microhardness is 380HV, and rete is canescence.
Embodiment 3
Hang on two electrodes through the LY11 aluminium alloy after the Chemical Pretreatment, it is of a size of 30mm * 40mm * 1.5mm.CONTROL PROCESS condition: slowly rise to 60V at 2min inner control voltage, and remain unchanged, until off-test.Current density raises with voltage and increases, and reaches peak current density 6A/dm
2After, current density reduces gradually.
Electrolytic solution is formed and processing parameter is:
Sulfophthalic acid: 80g/L
Oxalic acid: 30g/L
Trolamine: 50g/L
Voltage: 60V
Oxidization time: 10min
Temperature: 20 ± 2 ℃
Behind the ac oxide, thicknesses of layers is 12 μ m, and microhardness is 290HV, and rete is grey black.
Embodiment 4
Test materials adopts 6063 aluminium alloys, and it is of a size of 20mm * 60mm * 1mm.CONTROL PROCESS condition: slowly rise to 80V at 2min inner control voltage, and remain unchanged, until off-test.Current density raises with voltage and increases, and reaches peak current density 7A/dm
2After, current density reduces gradually.
Electrolytic solution is formed and processing parameter is:
Sulfophthalic acid: 60g/L
Tartrate: 20g/L
Ammonium citrate: 40g/L
Voltage: 80V
Oxidization time: 10min
Temperature: 10 ± 2 ℃
Behind the ac oxide, thicknesses of layers is 11 μ m, and microhardness is 330HV, and rete is canescence.
Claims (9)
1, a kind of aluminum or aluminum alloy material surface generates the electrochemical process for treating of oxide film, it is characterized in that, the aluminum or aluminum alloy workpiece is hung over the electrode two ends, places composite electrolytic solution, in 2min voltage of alternating current is adjusted to set(ting)value from zero, and remains unchanged; Current density raises along with voltage and increases, reach peak current density after, along with the formation of rete, current density reduces gradually, finishes until film forming; Behind ac oxide, generate the oxide film that one deck has higher hardness, thickness and decorate properties on the aluminum or aluminum alloy surface; Described composite electrolytic solution is made up of the aromatic carboxylic acid that contains 6～15 carbon atoms and derivative, the aliphatic carboxylic acid that contains 2～8 carbon atoms and ammonium salt or organic amine compound.
2, a kind of aluminum or aluminum alloy material surface according to claim 1 generates the electrochemical process for treating of oxide film, it is characterized in that aromatic carboxylic acid and derivatives concentration thereof are that 40～100g/L, aliphatic carboxylic acid concentration are that 10～60g/L, ammonium salt or organic amine compound concentration are 20～50g/L in the composite electrolytic solution.
3, a kind of aluminum or aluminum alloy material surface according to claim 2 generates the electrochemical process for treating of oxide film, it is characterized in that described aromatic carboxylic acid and derivative thereof are benzene hexacarboxylic acid, sulfophthalic acid or Phenylsulfonic acid; Aliphatic carboxylic acid is citric acid, oxysuccinic acid, oxalic acid, tartrate, propanedioic acid or lactic acid; Ammonium salt or organic amine compound are ammonium phosphate, ammonium citrate, methylamine or trolamine.
4, generate the electrochemical process for treating of oxide film according to the described a kind of aluminum or aluminum alloy material surface of claim 1, it is characterized in that the voltage of alternating current set(ting)value is 60～120V.
5, generate the electrochemical process for treating of oxide film according to each described a kind of aluminum or aluminum alloy material surface of claim 1-4, it is characterized in that power supply adopts the AC power of 50Hz, voltage is adjusted to 60～120V from 0V, peak current density 5～10A/dm
2, 10～20 ℃ of electrolyte temperatures.
6, a kind of aluminum or aluminum alloy material surface according to claim 5 generates the electrochemical process for treating of oxide film, it is characterized in that along with the formation of rete, current density descends gradually, finally reduces to 1～2A/dm
2
7, a kind of aluminum or aluminum alloy material surface according to claim 1 generates the electrochemical process for treating of oxide film, it is characterized in that aluminium is commercial-purity aluminium, and aluminium alloy is that Al-Cu is that alloy, Al-Si are that alloy, Al-Mg-Si are that alloy or Al-Zn are alloy.
8, a kind of aluminum or aluminum alloy material surface according to claim 1 generates the electrochemical process for treating of oxide film, it is characterized in that the oxidation film layer color and luster that forms is canescence or grey black, and film forming speed is more than or equal to 1 μ m/min.
9, a kind of aluminum or aluminum alloy material surface according to claim 1 generates the electrochemical process for treating of oxide film, it is characterized in that the two ends of ac electrode all hang with treats oxidation workpiece, and workpiece is each other to the utmost point.
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| CN102312264A (en) * | 2011-08-22 | 2012-01-11 | 吴江市精工铝字制造厂 | Decorative oxidation method for aluminum and aluminum alloy |
| CN102312262A (en) * | 2011-08-22 | 2012-01-11 | 吴江市精工铝字制造厂 | Hard anodization method of mixed acid of copper aluminium alloy |
| CN103834939A (en) * | 2012-11-27 | 2014-06-04 | 汉达精密电子(昆山)有限公司 | Aluminum alloy surface passivation liquid and processing method thereof |
| CN104109782A (en) * | 2013-04-17 | 2014-10-22 | 珠海格力节能环保制冷技术研究中心有限公司 | Aluminium alloy material, aluminium wearing-resistant part and preparation method thereof |
| CN107641827A (en) * | 2017-09-27 | 2018-01-30 | 辽宁忠旺集团有限公司 | A kind of aluminium alloy anode oxide technique |
| CN106757261B (en) * | 2016-11-29 | 2018-11-09 | 中南大学 | A kind of aluminium material surface oxide ceramic membrane and the compound wear-and corrosion-resistant coating and preparation method thereof of zeolite membrane |
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| CN110129853A (en) * | 2018-02-02 | 2019-08-16 | 本田技研工业株式会社 | Anode oxide film forms inorganic agent and anode oxide film forming method |
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2008
- 2008-10-21 CN CN2008101433813A patent/CN101392397B/en not_active Expired - Fee Related
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| CN102312262A (en) * | 2011-08-22 | 2012-01-11 | 吴江市精工铝字制造厂 | Hard anodization method of mixed acid of copper aluminium alloy |
| CN102312262B (en) * | 2011-08-22 | 2013-10-09 | 吴江市精工铝字制造厂 | Hard anodization method of mixed acid of copper aluminium alloy |
| CN102312264B (en) * | 2011-08-22 | 2013-10-09 | 吴江市精工铝字制造厂 | Decorative oxidation method for aluminum and aluminum alloy |
| CN102312264A (en) * | 2011-08-22 | 2012-01-11 | 吴江市精工铝字制造厂 | Decorative oxidation method for aluminum and aluminum alloy |
| CN103834939A (en) * | 2012-11-27 | 2014-06-04 | 汉达精密电子(昆山)有限公司 | Aluminum alloy surface passivation liquid and processing method thereof |
| CN104109782A (en) * | 2013-04-17 | 2014-10-22 | 珠海格力节能环保制冷技术研究中心有限公司 | Aluminium alloy material, aluminium wearing-resistant part and preparation method thereof |
| CN104109782B (en) * | 2013-04-17 | 2016-05-25 | 珠海格力节能环保制冷技术研究中心有限公司 | A kind of aluminum alloy materials, aluminum alloy wear resistant member and preparation method thereof |
| CN109072473A (en) * | 2016-04-27 | 2018-12-21 | 邦及奥卢夫森公司 | The surface Al of the anodization of the high reflection of diffusing reflection and mirror-reflection level with customization |
| CN109072473B (en) * | 2016-04-27 | 2021-03-30 | 邦及奥卢夫森公司 | High reflective anodized Al surfaces with tailored levels of diffuse and specular reflection |
| CN106757261B (en) * | 2016-11-29 | 2018-11-09 | 中南大学 | A kind of aluminium material surface oxide ceramic membrane and the compound wear-and corrosion-resistant coating and preparation method thereof of zeolite membrane |
| CN107641827A (en) * | 2017-09-27 | 2018-01-30 | 辽宁忠旺集团有限公司 | A kind of aluminium alloy anode oxide technique |
| CN110129853A (en) * | 2018-02-02 | 2019-08-16 | 本田技研工业株式会社 | Anode oxide film forms inorganic agent and anode oxide film forming method |
| CN109056022A (en) * | 2018-07-26 | 2018-12-21 | 同曦集团有限公司 | Aluminium and aluminum alloy surface without pole plate oxidation processing technique |
| CN110872721A (en) * | 2018-08-29 | 2020-03-10 | 五十铃自动车株式会社 | Metal molded body having anodic oxide film, method for producing same, piston, and internal combustion engine |
| CN110872721B (en) * | 2018-08-29 | 2022-06-17 | 五十铃自动车株式会社 | Metal molded body having anodic oxide film, method for producing same, piston, and internal combustion engine |
| CN110698683A (en) * | 2019-09-27 | 2020-01-17 | 广西师范大学 | One-dimensional dysprosium polymer and preparation method thereof |
| CN110804189A (en) * | 2019-09-27 | 2020-02-18 | 广西师范大学 | Three-dimensional lutetium polymer and preparation method thereof |
| CN110698683B (en) * | 2019-09-27 | 2021-08-24 | 广西师范大学 | One-dimensional dysprosium polymer and preparation method thereof |
| CN110804189B (en) * | 2019-09-27 | 2021-11-02 | 广西师范大学 | Three-dimensional lutetium polymer and preparation method thereof |
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Assignee: Hunan Ningxiang JiWeiXin Metal Powder Co., Ltd. Assignor: Hunan University Contract record no.: 2011430000280 Denomination of invention: Electrochemistry processing method for generating oxide film on surface of aluminium or aluminium alloy material Granted publication date: 20110420 License type: Exclusive License Open date: 20090325 Record date: 20111103 |
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