CN109056023A - Sulfuric acid+oxalic acid nitration mixture anode oxidation process - Google Patents

Sulfuric acid+oxalic acid nitration mixture anode oxidation process Download PDF

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Publication number
CN109056023A
CN109056023A CN201810972524.5A CN201810972524A CN109056023A CN 109056023 A CN109056023 A CN 109056023A CN 201810972524 A CN201810972524 A CN 201810972524A CN 109056023 A CN109056023 A CN 109056023A
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China
Prior art keywords
anode
sulfuric acid
oxalic acid
acid
oxidation process
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CN201810972524.5A
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Chinese (zh)
Inventor
张少杰
邵颖
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Shenyang Fortune Precision Equipment Co Ltd
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Shenyang Fortune Precision Equipment Co Ltd
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Priority to CN201810972524.5A priority Critical patent/CN109056023A/en
Publication of CN109056023A publication Critical patent/CN109056023A/en
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/06Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C25D11/08Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/06Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C25D11/10Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing organic acids

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)

Abstract

The invention belongs to a kind of corrosion resistance Hard Anodic Oxidation Process technical fields.Specifically a kind of sulfuric acid+oxalic acid nitration mixture anode oxidation process, (1) use sulfuric acid+oxalic acid mixing tank liquor, and mesoxalic acid concentration as the main component is 50g/L, and sulfuric acid is that auxiliary ingredients concentration is 2g/L;(2) anodization is carried out to aluminum alloy materials workpiece, controlled at 4-6 DEG C, adjustment current density is 1-3A/dm2, the up-flow time is 5-10min, reaction time 3-4h, it is desirable that film thickness 50-100um;(3) after anode reaches film thickness, using 92-100 DEG C pure water sealing of hole 3-4 hours, obtain have higher rotproofness oxidation film.Sulfuric acid+oxalic acid mixing tank liquor anodized is carried out to aluminum alloy materials workpiece, so that anode surface has sulfuric acid hard anode appearance characteristic, there is oxalic acid anode high corrosion resistance energy again, nitration mixture Hard Anodic Oxidation Process anode has obvious hard anode property, higher thicknesses of layers is obtained, there is higher hardness and corrosion resistance.

Description

Sulfuric acid+oxalic acid nitration mixture anode oxidation process
Technical field
The invention belongs to corrosion resistance Hard Anodic Oxidation Process technical fields, more particularly to a kind of corrosion resistance hard Anode oxidation process is suitable for IC and assembles crucial corrosion resistance reaction cavity hard anodic process.
Background technique
Corrosion resistance Hard Anodic Oxidation Process has its special importance.Hard anodic process is due to its property Have a wide range of applications in the industrial production, in the field IC to hard anodic process performance will gas it is higher and higher, especially anode film Corrosion resistance, be widely applied with key reaction cavity and other key components and parts, exploitation have compared with highly corrosion resistant hard Anode, improves equipment performance and service life is significant.
Summary of the invention
For the above technical problems, the present invention provides a kind of sulfuric acid+oxalic acid nitration mixture Hard Anodic Oxidation Process, right Aluminum alloy materials workpiece carries out anodized in sulfuric acid+oxalic acid mix acid liquor, passes through two kinds of acid in control anodic process Ratio, reaction temperature and current density etc..To obtain fine and close oxidation film, there is sulfuric acid hard anode appearance characteristic, again With oxalic acid anode high corrosion resistance energy.
The purpose of the present invention is achieved through the following technical solutions:
A kind of sulfuric acid+oxalic acid nitration mixture anode oxidation process,
(1) sulfuric acid+oxalic acid mixing tank liquor is used, mesoxalic acid concentration as the main component is 50g/L, and sulfuric acid is auxiliary ingredients Concentration is 2g/L;
(2) anodization is carried out to aluminum alloy materials workpiece, controlled at 4-6 DEG C, adjustment current density is 1-3A/dm2, The up-flow time is 5-10min, reaction time 3-4h, it is desirable that film thickness 50-100um;
(3) after anode reaches film thickness, using 92-100 DEG C pure water sealing of hole 3-4 hours, obtain have higher rotproofness oxidation Film.With sulfuric acid hard anode appearance characteristic, and there is oxalic acid anode high corrosion resistance energy.
The invention has the advantages that
The present invention carries out sulfuric acid+oxalic acid mixing tank liquor anodized to aluminum alloy materials workpiece, passes through two kinds of control The ratio of acid so that anode surface has sulfuric acid hard anode appearance characteristic, and has oxalic acid anode high corrosion resistance energy, leads to It crosses and continuously attempts to, nitration mixture Hard Anodic Oxidation Process anode has obvious hard anode property, obtains higher thicknesses of layers, has There are higher hardness and corrosion resistance.
Specific embodiment
Below with reference to embodiment, the present invention will be described in detail.
A kind of sulfuric acid+oxalic acid nitration mixture anode oxidation process,
(1) sulfuric acid+oxalic acid mixing tank liquor is used, mesoxalic acid concentration as the main component is 50g/L, and sulfuric acid is auxiliary ingredients Concentration is 2g/L;
(2) anodization is carried out to aluminum alloy materials workpiece, controlled at 4-6 DEG C, adjustment current density is 1-3A/dm2, The up-flow time is 5-10min, reaction time 3-4h, it is desirable that film thickness 50-100um;
(3) after anode reaches film thickness, using 92-100 DEG C pure water sealing of hole 3-4 hours, obtain have higher rotproofness oxidation Film.With sulfuric acid hard anode appearance characteristic, and there is oxalic acid anode high corrosion resistance energy.
The present invention can effectively improve the anode film of the corrosion resistance of workpiece, using the hydrochloric acid solution of 5%wt through row Bubble Test, i.e., be adhered to strip using sealing water is hidden for glass tube, and test 5%wt salt is added in glass tube Acid solution liquid level high 2-3cm continuously emits three or more bubbles at test zone solution same o'clock in one second, represents test knot Beam, record end time.The corrosion resistance sulfuric acid Hard Anodic Oxidation Process test piece corrosion resistance testing time reaches 8h or more.
Film hardness can reach 400HV, and color difference range is in 40 >=L >=25;1≥a≥-1;6 >=b >=0, it is hard with common sulfuric acid Matter anodic oxidation is identical.
Embodiment
The present invention includes the following steps: that aluminum alloy materials workpiece is carried out anode pre-treatment, first polishing grinding workpiece by (1) Surface, it is desirable that Ra < 16uin after cleaning up, carries out anode pre-treatment and removes surface impurity.
(2) hard anodizing processing is carried out to workpiece, is 50g/L by workpiece oxalic acid concentration as the main component, sulfuric acid is Auxiliary ingredients concentration is 2g/L mixed solution, and controlled at 4-6 DEG C, adjustment current density is 1-3A/dm2, up-flow the time be 5-10min, it is desirable that film thickness 80-100um.
(3) workpiece is subjected to sealing pores, the good workpiece of anode is put into 92-100 DEG C of pure water through row sealing of hole, when sealing of hole Between be 3-4 hours.It is dried up using compressed air, static 24 hours.Obtain that there is higher rotproofness oxidation film.

Claims (2)

1. a kind of sulfuric acid+oxalic acid nitration mixture anode oxidation process, it is characterised in that:
(1) sulfuric acid+oxalic acid mixing tank liquor is used, mesoxalic acid concentration as the main component is 50g/L, and sulfuric acid is auxiliary ingredients concentration For 2g/L;
(2) anodization is carried out to aluminum alloy materials workpiece, controlled at 4-6 DEG C, adjustment current density is 1-3A/dm2, up-flow Time is 5-10min, reaction time 3-4h, it is desirable that film thickness 50-100um;
(3) after anode reaches film thickness, using 92-100 DEG C pure water sealing of hole 3-4 hours, obtain have higher rotproofness oxidation film.
2. sulfuric acid as described in claim 1+oxalic acid nitration mixture Hard Anodic Oxidation Process, it is characterised in that: have sulfuric acid hard sun Pole appearance characteristics, and there is oxalic acid anode high corrosion resistance energy.
CN201810972524.5A 2018-08-24 2018-08-24 Sulfuric acid+oxalic acid nitration mixture anode oxidation process Pending CN109056023A (en)

Priority Applications (1)

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CN201810972524.5A CN109056023A (en) 2018-08-24 2018-08-24 Sulfuric acid+oxalic acid nitration mixture anode oxidation process

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Application Number Priority Date Filing Date Title
CN201810972524.5A CN109056023A (en) 2018-08-24 2018-08-24 Sulfuric acid+oxalic acid nitration mixture anode oxidation process

Publications (1)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110541181A (en) * 2019-09-10 2019-12-06 中国计量大学 Preparation method of aluminum alloy surface thermal control coating
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
CN111893538A (en) * 2020-07-02 2020-11-06 中国航发贵州红林航空动力控制科技有限公司 Hard anodizing process method for 3D printing forming AlSi10Mg aluminum alloy material
CN113106517A (en) * 2021-04-09 2021-07-13 维沃移动通信(重庆)有限公司 Preparation method of decorative ring, decorative ring and electronic equipment
CN114108051A (en) * 2021-12-24 2022-03-01 靖江先锋半导体科技有限公司 Corrosion-resistant mixed acid anodic oxidation process
CN114717628A (en) * 2022-04-14 2022-07-08 广东江丰电子材料有限公司 Preparation method of anodic oxide film

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105887151A (en) * 2016-05-23 2016-08-24 沈阳富创精密设备有限公司 Corrosion resistance sulfuric acid hard anodizing process
CN107641826A (en) * 2016-07-21 2018-01-30 富泰华精密电子(济源)有限公司 Aluminium alloy anode oxide method
CN108193250A (en) * 2018-02-24 2018-06-22 沈阳富创精密设备有限公司 A kind of sulfuric acid+nitration mixture mixing anode oxidation process

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105887151A (en) * 2016-05-23 2016-08-24 沈阳富创精密设备有限公司 Corrosion resistance sulfuric acid hard anodizing process
CN107641826A (en) * 2016-07-21 2018-01-30 富泰华精密电子(济源)有限公司 Aluminium alloy anode oxide method
CN108193250A (en) * 2018-02-24 2018-06-22 沈阳富创精密设备有限公司 A kind of sulfuric acid+nitration mixture mixing anode oxidation process

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN110541181A (en) * 2019-09-10 2019-12-06 中国计量大学 Preparation method of aluminum alloy surface thermal control coating
CN110541181B (en) * 2019-09-10 2021-05-18 中国计量大学 Preparation method of aluminum alloy surface thermal control coating
CN111893538A (en) * 2020-07-02 2020-11-06 中国航发贵州红林航空动力控制科技有限公司 Hard anodizing process method for 3D printing forming AlSi10Mg aluminum alloy material
CN113106517A (en) * 2021-04-09 2021-07-13 维沃移动通信(重庆)有限公司 Preparation method of decorative ring, decorative ring and electronic equipment
CN114108051A (en) * 2021-12-24 2022-03-01 靖江先锋半导体科技有限公司 Corrosion-resistant mixed acid anodic oxidation process
CN114717628A (en) * 2022-04-14 2022-07-08 广东江丰电子材料有限公司 Preparation method of anodic oxide film
CN114717628B (en) * 2022-04-14 2023-11-07 广东江丰电子材料有限公司 Preparation method of anodic oxide film

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Application publication date: 20181221