CN102888641B - Hard Anodic Oxidation of Aluminum Alloy electrolytic solution and method - Google Patents
Hard Anodic Oxidation of Aluminum Alloy electrolytic solution and method Download PDFInfo
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Abstract
A kind of Hard Anodic Oxidation of Aluminum Alloy electrolytic solution and method, the method comprises the following steps: → polishing → neutralization → hard anodizing → reanodizing → sealing of hole → baking is stung → neutralized to degreasing → alkali; The hard anodizing electrolytic solution wherein used during hard anodizing, often liter of this electrolytic solution comprises following component: (a) sulfuric acid 50 ~ 100g; (b) propanedioic acid 20 ~ 40g; (c) oxalic acid 10 ~ 30g; (d) glycerine 1 ~ 10g.The hard anodized film with oilness is generated by Hard Anodic Oxidation of Aluminum Alloy electrolytic solution of the present invention and method.
Description
[technical field]
The present invention relates to a kind of Hard Anodic Oxidation of Aluminum Alloy electrolytic solution and method, and in particular to a kind of electrolytic solution and the method for preparing the hard anodized film with oilness.
[background technology]
Hard anodizing electrolysis process is a lot, and now widely used have (1) sulfuric acid hard anodizing method; (2) oxalic acid hard anodizing method; (3) mixed acid type hard anodizing method.
Aluminum alloy materials because surperficial matter is soft, wear no resistance and the defect such as frictional coefficient is high, so need the tribology surface modification treatment of carrying out Al and Alalloy in use, namely first hard anodizing is carried out in aluminum alloy surface, then form slip coating on aluminium alloy film surface and the various lubricating substance of inside deposition, thus aluminum alloy surface frictional coefficient is reduced.
Aluminum or aluminum alloy anodic oxidation rear surface is dispersed with a large amount of nano level hole, there is higher free energy, but solid surface can not reduce the surface free energy of system by the method reducing surface-area as liquid, can only adsorb external agency to reduce the free energy of system.Therefore, in order to obtain the hard anodized film with oilness, traditional method be by anode after aluminum or aluminum alloy be immersed in the aqueous dispersions of nano lubricating particle, but the shortcoming of the method is nano particle easily reunites and grow up, when particle diameter is greater than the diameter of oxidation fenestra, cause lubricated granules cannot enter into the hole of anodic oxidation formation, thus affect the lubricant effect of anode oxide film.
[summary of the invention]
In view of this, the object of this invention is to provide a kind of Hard Anodic Oxidation of Aluminum Alloy electrolytic solution and method, generate the hard anodized film with oilness by this Hard Anodic Oxidation of Aluminum Alloy electrolytic solution and method.
In order to achieve the above object, the invention provides a kind of Hard Anodic Oxidation of Aluminum Alloy electrolytic solution, often liter of this electrolytic solution comprises following component:
(a) sulfuric acid 50 ~ 100g;
(b) propanedioic acid 20 ~ 40g;
(c) oxalic acid 10 ~ 30g;
(d) glycerine 1 ~ 10g.
Especially, above-mentioned Hard Anodic Oxidation of Aluminum Alloy electrolytic solution, often liter of this electrolytic solution comprises following component:
(a) sulfuric acid 100g;
(b) propanedioic acid 20g;
(c) oxalic acid 20g;
(d) glycerine 2g.
Especially, above-mentioned Hard Anodic Oxidation of Aluminum Alloy electrolytic solution, often liter of this electrolytic solution comprises following component:
(a) sulfuric acid 80g;
(b) propanedioic acid 30g;
(c) oxalic acid 30g;
(d) glycerine 5g.
Especially, above-mentioned Hard Anodic Oxidation of Aluminum Alloy electrolytic solution, often liter of this electrolytic solution comprises following component:
(a) sulfuric acid 50g;
(b) propanedioic acid 40g;
(c) oxalic acid 30g;
(d) glycerine 6g.
In addition, the present invention also provides a kind of Hard Anodic Oxidation of Aluminum Alloy method, and it comprises the following steps:
→ polishing → neutralization → hard anodizing → reanodizing → sealing of hole → baking is stung → neutralized to degreasing → alkali; The hard anodizing electrolytic solution wherein used during hard anodizing often rises and comprises following component:
(a) sulfuric acid 50 ~ 100g;
(b) propanedioic acid 20 ~ 40g;
(c) oxalic acid 10 ~ 30g;
(d) glycerine 1 ~ 10g.
Especially, during above-mentioned hard anodizing, voltage is 30 ~ 100V, and current density is 2.5 ~ 3.0A/dm
2, the treatment time is 50 ~ 300min, and treatment temp is 15 ~ 21 DEG C.
Especially, during above-mentioned reanodizing with sulfuric acid and ammonium tetrathiomolybdate for electrolytic solution, temperature is 15 ~ 30 DEG C, and voltage is 12 ~ 18V, and current density is 0.25 ~ 5A/dm
2, the treatment time is 30 ~ 300s.
Especially, during above-mentioned sealing of hole, concentration is that the nickel acetate hole sealing agent of 0.7g/L carries out sealing of hole, and sealing of hole temperature is 80 DEG C, and pH is 5 ~ 6, and the treatment time is 10min.
Especially, washing processing procedure is had in above steps.
Especially, the hard anodized film thickness obtained after two-step anodization is 50 ~ 300 μm.
Compared to prior art, Hard Anodic Oxidation of Aluminum Alloy electrolytic solution of the present invention and method, the hardening oxidation rete of 50 ~ 300 μm can be obtained, slip coating is formed in aluminum alloy surface, and slip coating is combined with base material closely, the aluminium alloy of more abrasion performance, Nai Gaore and anti-extra-high voltage electrical insulativity can also be obtained, make it can be applied in the future technologies such as electronics, computer, space industry, national defence military products, Precision Machinery Elements and solar facilities.
[embodiment]
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
Carry out hard anodize 60min in Al alloy parts dipping acid liquid bath by stinging through degreasing, alkali, neutralize, after polishing and neutralizing treatment, voltage is 30V, and current density is 2.5A/dm
2, treatment temp is 19 ~ 21 DEG C, and the electrolytic solution wherein used during hard anodizing often rises and comprises following component:
(a) sulfuric acid 100g;
(b) propanedioic acid 20g;
(c) oxalic acid 20g;
(d) glycerine 2g;
Then the mixed solution that to put into sulfuric acid and ammonium tetrathiomolybdate by the Al alloy parts after hard anodize be electrolytic solution, be that cathodal closing carries out second time anodic oxidation treatment with aluminium, treatment temp is 22 ~ 24 DEG C, and voltage is 18V, and current density is 0.25A/dm
2, the treatment time is 60s, by second time anodic oxidation, anodic oxidation minute aperture inwall is reacted and generates solid molybdenumdisulphide, thus obtain the anode oxide film with lubricant film; Then carry out sealing of hole with the nickel acetate hole sealing agent that concentration is 0.7g/L, sealing of hole temperature is 80 DEG C, pH=5 ~ 6, sealing pores 10min, can obtain the hard anodic oxidation coating product with fine oilness.
Embodiment 2
Carry out hard anodize 120min in Al alloy parts dipping acid liquid bath by stinging through degreasing, alkali, neutralize, after polishing and neutralizing treatment, voltage is 60V, and current density is 3.0A/dm
2, treatment temp is 17 ~ 19 DEG C, and the electrolytic solution wherein used during hard anodizing often rises and comprises following component:
(a) sulfuric acid 80g;
(b) propanedioic acid 30g;
(c) oxalic acid 30g;
(d) glycerine 5g;
Then the mixed solution that to put into sulfuric acid and ammonium tetrathiomolybdate by the Al alloy parts after hard anodize be electrolytic solution, be that cathodal closing carries out second time anodic oxidation treatment with graphite, treatment temp is 22 ~ 24 DEG C, and voltage is 13V, and current density is 1.5A/dm
2, the treatment time is 150s, by second time anodic oxidation, anodic oxidation minute aperture inwall is reacted and generates solid molybdenumdisulphide, thus obtain the anode oxide film with lubricant film; Then carry out sealing of hole with the nickel acetate hole sealing agent that concentration is 0.7g/L, sealing of hole temperature is 80 DEG C, pH=5 ~ 6, sealing pores 10min, can obtain the hard anodic oxidation coating product with fine oilness.
Embodiment 3
Carry out hard anodize 250min in Al alloy parts dipping acid liquid bath by stinging through degreasing, alkali, neutralize, after polishing and neutralizing treatment, voltage is 90V, and current density is 2.5 ~ 3.0A/dm
2, treatment temp is 15 ~ 17 DEG C, and the electrolytic solution wherein used during hard anodizing often rises and comprises following component:
(a) sulfuric acid 50g;
(b) propanedioic acid 40g;
(c) oxalic acid 30g;
(d) glycerine 6g;
Then the mixed solution that to put into sulfuric acid and ammonium tetrathiomolybdate by the Al alloy parts after hard anodize be electrolytic solution, be that cathodal closing carries out second time anodic oxidation treatment with graphite, treatment temp is 22 ~ 24 DEG C, and voltage is 15V, and current density is 3A/dm
2, the treatment time is 300s, by second time anodic oxidation, anodic oxidation minute aperture inwall is reacted and generates solid molybdenumdisulphide, thus obtain the anode oxide film with lubricant film; Then carry out sealing of hole with the nickel acetate hole sealing agent that concentration is 0.7g/L, sealing of hole temperature is 80 DEG C, pH=5 ~ 6, sealing pores 10min, can obtain the hard anodic oxidation coating product with fine oilness.
Hard Anodic Oxidation of Aluminum Alloy electrolytic solution of the present invention and method, the hardening oxidation rete of 50 ~ 300 μm can be obtained, slip coating is formed in aluminum alloy surface, and slip coating is combined with base material closely, the aluminium alloy of more abrasion performance, Nai Gaore and anti-extra-high voltage electrical insulativity can also be obtained, make it can be applied in the future technologies such as electronics, computer, space industry, national defence military products, Precision Machinery Elements and solar facilities.
It is noted that the invention is not restricted to above-mentioned embodiment, any simple modification that any those skilled in the art do above-described embodiment based on technical solution of the present invention, equivalent variations and modification, all fall within the scope of protection of the present invention.
Claims (5)
1. a Hard Anodic Oxidation of Aluminum Alloy method, is characterized in that, it comprises the following steps:
→ polishing → neutralization → hard anodizing → reanodizing → sealing of hole → baking is stung → neutralized to degreasing → alkali; The hard anodizing electrolytic solution wherein used during hard anodizing often rises and comprises following component:
During above-mentioned reanodizing with sulfuric acid and ammonium tetrathiomolybdate for electrolytic solution, temperature is 15 ~ 30 DEG C, and voltage is 12 ~ 18V, and current density is 0.25 ~ 5A/dm
2, the treatment time is 30 ~ 300s.
2. Hard Anodic Oxidation of Aluminum Alloy method according to claim 1, is characterized in that, during above-mentioned hard anodizing, voltage is 30 ~ 100V, and current density is 2.5 ~ 3.0A/dm
2, the treatment time is 50 ~ 300min, and treatment temp is 15 ~ 21 DEG C.
3. Hard Anodic Oxidation of Aluminum Alloy method according to claim 1, is characterized in that, during above-mentioned sealing of hole, concentration is that the nickel acetate hole sealing agent of 0.7g/L carries out sealing of hole, and sealing of hole temperature is 80 DEG C, and pH is 5 ~ 6, and the treatment time is 10min.
4. Hard Anodic Oxidation of Aluminum Alloy method according to claim 1, is characterized in that, has washing processing procedure in above steps.
5. Hard Anodic Oxidation of Aluminum Alloy method according to claim 1, is characterized in that, the anodic oxidation film thickness obtained after above-mentioned two-step anodization is 50 ~ 300 μm.
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| CN103233259B (en) * | 2013-05-10 | 2016-06-08 | 黄山金瑞泰科技股份有限公司 | The oxidation processing technique of CTP plate |
| CN103451702A (en) * | 2013-08-13 | 2013-12-18 | 河南辉龙铝业股份有限公司 | Aluminum profile anodizing method |
| CN103484916B (en) * | 2013-09-29 | 2016-05-18 | 苏州利达铸造有限公司 | The anodized technique of pack alloy for a kind of digital electronic goods |
| CN103981556B (en) * | 2014-05-19 | 2017-02-22 | 广东美芝制冷设备有限公司 | Electrolyte for hard-anodizing of aluminum alloys and preparation method of aluminum alloy hard self-lubricating coatings |
| CN105200487A (en) * | 2015-09-24 | 2015-12-30 | 马鞍山杰创塑胶科技有限公司 | Salt-fog-resistant aluminum alloy anode oxide film nickel-free hole sealing agent and preparation method thereof |
| CN105401201B (en) * | 2015-12-22 | 2018-11-23 | 上海申和热磁电子有限公司 | A kind of anode oxidation process of the aluminum alloy base material for TFT liquid-crystalline glasses panel |
| CN107090590A (en) * | 2017-04-24 | 2017-08-25 | 南京邮电大学 | A kind of aluminium alloy anode oxide electrolyte and oxidation technology based on corrosion inhibiter |
| CN110607549A (en) * | 2019-08-20 | 2019-12-24 | 帝京半导体科技(苏州)有限公司 | Anti-static hard anodic oxidation process |
| CN110373699B (en) * | 2019-08-22 | 2021-04-02 | 南昌航空大学 | Hard anodic oxidation electrolyte and oxidation method for ZL105 aluminum alloy sand casting |
| CN113755923A (en) * | 2020-09-18 | 2021-12-07 | 英迪那米(徐州)半导体科技有限公司 | Aluminum alloy hard anodic oxidation electrolyte and preparation method thereof |
| CN112899749A (en) * | 2021-01-25 | 2021-06-04 | 广东智目科技有限公司 | Anodic oxidation electrolyte and anodic oxidation method of appearance camera |
| CN114214698B (en) * | 2022-01-12 | 2023-03-21 | 江阴迈科美新能源科技有限公司 | Aluminum profile anodic oxidation process applied to photovoltaic frame |
| CN114540907B (en) * | 2022-02-27 | 2024-09-06 | 山东振挺精工活塞有限公司 | Preparation method of fatigue-resistant aluminum alloy |
| CN114737237B (en) * | 2022-02-27 | 2024-01-05 | 营口赛斯德型材有限公司 | Preparation method of coating material |
| CN117512735B (en) * | 2023-11-20 | 2024-10-18 | 江苏凯威特斯半导体科技有限公司 | Hard anodic oxidation method for aluminum alloy |
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