CN102995089B - Oxidation capsule forming method - Google Patents
Oxidation capsule forming method Download PDFInfo
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- CN102995089B CN102995089B CN201210345479.3A CN201210345479A CN102995089B CN 102995089 B CN102995089 B CN 102995089B CN 201210345479 A CN201210345479 A CN 201210345479A CN 102995089 B CN102995089 B CN 102995089B
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- oxide film
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- treated object
- current density
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/12—Anodising more than once, e.g. in different baths
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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)
- Other Surface Treatments For Metallic Materials (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
The invention relates to an oxidation capsule forming method, wherein an oxidation capsule is effectively formed on the large-area surface of an object to be processed. One part of the object to be processed and made of aluminum or aluminum alloy is soaked in the electrolyte for micro-arc oxidation treatment, so as to form an oxidation capsule. Then the boundary of the part of the object formed with the oxidation capsule and the other part of the object is again soaked in the electrolyte for micro-arc oxidation treatment. Therefore, the other part of the object is formed with the oxidation capsule.
Description
Technical field
The present invention relates to the method for forming oxide film thereon on the treated object surface being made up of aluminum or aluminum alloy.
Background technology
The applicant proposed in the past is split on large-area treated object surface, and fraction carries out micro-arc oxidation
Process, thus, oxide film thereon is formed in the whole surface of treated object (with reference to patent document 1).
Method disclosed in the document, using masking material by the position for first processing of treated object with post processing position
Separate, by the position for first processing dipping in the electrolytic solution until the position of masking material, oxide film thereon is formed, by treated object
Lift from electrolyte, remove masking material, the position of post processing is impregnated once again and is aoxidized in the electrolytic solution, by should
Operation is repeated, in 1m2Oxide film thereon is formed in the whole surface of the treated object of above size.
But, in method disclosed in patent document 1, because with treated object is lifted from electrolyte, removing is sheltered
The operation of material, therefore there are problems that inefficient.Further, since masking material can not uniformly adhere on treated object surface,
There is electrolyte into below masking material, the position for first processing becomes uneven and asks with the border at the position of post processing
Topic.In addition, when the removal of masking material is not thorough, there is a problem of impurities left near border.Further, exist and located
The area of reason thing is bigger, produces the bigger problem of the possibility of these problems.
Thus, for example, patent document 2 is proposed, while transporting the flexible substrate drawn from coiled material, shake liquid level on one side
Carry out determining current electroanalysis process etc. dynamicly.But, in the publication, to carrying out being electrolysed the position and untreated position of process
Between border oxide film thereon film quality it is not specifically mentioned, in addition, for the aluminium for being difficult to bend for more than thickness 1mm or
Aluminium alloy, and as process object area maximize occasion above-mentioned citation 1 problem points do not propose yet it is any
Solution.
Though in addition, propose in citation 3 using micro- arc process, while horizontal electric current is maintained like, while in pliability
The method of film forming on substrate, but there is a problem of same with citation 2.
Prior art literature
Patent document
The JP 2009-102721 publication of patent document 1
The JP 2007-332409 publication of patent document 2
The JP 2010-156040 publication of patent document 3
The content of the invention
Invent problem to be solved
Therefore, it is of the invention in order to solve the above problems, to be effectively formed oxidation quilt on large-area treated object surface
For the purpose of film.
Means for solving the problems
In order to solve above-mentioned problem, result that the present inventor is carefully studied finds, with if do not adopted masking material,
Anodized is carried out to large-scale treated object fraction, then treated object occurs to recognize in the past as corrosion near liquid level
When being tested based on knowledge, it has unexpectedly been found that near liquid level, near the corrosion of the treated object that electrolyte is produced and liquid level
Hardly staining metal, but also can solve using masking material when weakness, so as to complete invention below.
That is, the present invention is as described in Section 1, it is characterised in that by more than the thickness 1mm for constituting aluminum or aluminum alloy
The part dipping of treated object carries out in the electrolytic solution micro-arc oxidation process, after being consequently formed oxide film thereon, is defining
The position of above-mentioned oxide film thereon and the border at other positions are not provided with masking material, by define above-mentioned oxide film thereon position and
Other positions are immersed in above-mentioned electrolyte carries out micro-arc oxidation process, thus, at above-mentioned other positions oxide film thereon is formed.
The Section 2 of the present invention, it is characterised in that in the forming method of the oxide film thereon described in Section 1, from above-mentioned quilt
The front of processed material sequentially forms above-mentioned oxide film thereon.
The Section 3 of the present invention, it is characterised in that in the forming method of the oxide film thereon described in Section 1 or Section 2,
Current density when above-mentioned micro-arc oxidation is processed is 1～6A/dm2。
The Section 4 of the present invention, it is characterised in that the shape of the oxide film thereon described in any one in Section 1～Section 3
Into in method, current density when above-mentioned micro-arc oxidation is processed is 1～4A/dm2。
The Section 5 of the present invention, it is characterised in that the shape of the oxide film thereon described in any one in Section 1～Section 4
Into in method, in the forming process of whole above-mentioned oxide film thereon, the temperature of above-mentioned electrolyte is -10 DEG C～65 DEG C of scope.
Invention effect
According to the present invention, to large area treated object, the deformation such as treated object can not be made to bend and be effectively formed
Oxide film thereon.Further, since it is incomplete not there are problems that masking material is removed, free from admixture residual on treated object.In addition, pressing
According to the present invention, electric current when being processed due to micro-arc oxidation with relatively low, therefore can be not required to Large Copacity power supply.Further, due to can
Energetically reduce the heating in the forming process of whole oxide film thereon, for cooling treatment system system it is compared with the past can be with
Reduce.
Description of the drawings
Fig. 1 is the explanatory diagram of an embodiment of the forming method of the oxide film thereon for representing the present invention.
The sample photo of Fig. 2 (a) embodiments 1, (b) the sample photo of embodiment 2.
Fig. 3 is optical microscope photograph ((a) the 1st oxide film thereon, (b) the 2nd oxide film thereon, (c) of the sample of embodiment 1
Oxide film thereon near border).
Fig. 4 is optical microscope photograph ((a) the 1st oxide film thereon, (b) the 2nd oxide film thereon, (c) of the sample of embodiment 2
Oxide film thereon near border).
The explanation of symbol
1 treated object
2 electrolyte
3 the 1st oxide film thereons
4 the 2nd oxide film thereons
Specific embodiment
The forming method of the oxide film thereon of the present invention, as shown in figure 1, by a part for the treated object 1 of more than thickness 1mm
Being immersed in electrolyte 2 carries out micro-arc oxidation process, formed the 1st oxide film thereon 3, by with the portion for defining the 1st oxide film thereon 3
During other different positions (remaining position) of position are immersed in electrolyte 2, the 2nd oxide film thereon 4 is formed, in the entirety of treated object 1
Upper formation oxide film thereon 3,4.When the 2nd oxide film thereon 4 is formed, because the 1st oxide film thereon 3 becomes dielectric film, therefore only the 2nd is being formed
The position of oxide film thereon 4 intensively forms oxide film thereon.
According to the present invention, due to the becoming between the 1st and the 2nd oxide film thereon 3,4 unlike disclosed in patent document 1
The position on border arranges masking material, therefore oxide film thereon 3,4 effectively can be formed on treated object 1.Further, since on border
Masking material is not provided with, therefore, there is no electrolyte 2 and form uneven oxide film thereon into the downside of masking material, or
Produce the problem of the impurity such as white particulate material.
Further, the so-called masking material in this specification, it is intended that comprising such silicone encapsulant disclosed in patent document 1
Or the masking material of silicon sealant etc., for the portion for separating the position for having defined oxide film thereon and form oxide film thereon later
The part of position.
In the above example, oxide film thereon 3,4 has been generally formed in treated object 1, but the present invention may not be defined in
Oxide film thereon is generally formed in treated object 1.
In addition, with regard to oxide film thereon formation process, selected according to the shape or size of treated object 1, when
When oxide film thereon being divided into into more than 3 times on treated object 1, then masking material number becomes more than 2, therefore is preferred.
Further, the 2nd oxide film thereon 4 is formed if do not lifted the position for defining the 1st oxide film thereon 3 from electrolyte 2,
More effectively oxide film thereon can be generally formed in treated object 1.
In the above example, during the 1st oxide film thereon 3 is formed, micro- electric arc oxygen is carried out with the current density for specifying
Change is processed, and makes voltage keep certain after the voltage for reaching regulation.The judgement that formation with regard to the 1st oxide film thereon 3 terminates, though in electricity
Pressure reaches certain rear current density slowly to be reduced, but preferably with respect to current density during the certain start to process of voltage, in electricity
Current density terminates the formation of the 1st oxide film thereon 3 and processes when reaching 1/100～1/10, start the formation of the 2nd oxide film thereon 4
Process.
Current density when processing with regard to micro-arc oxidation, preferably 1～6.0A/dm2, more preferably 1～4A/dm2.When being less than
1A/dm2When, electric discharge becomes insufficient, when more than 6.0A/dm2When, the boundary film quality between the 1st and the 2nd oxide film thereon 3,4
Amount becomes uneven.
In addition, in the forming process of whole oxide film thereon 3,4, the temperature for preferably making electrolyte 2 is -10～65 DEG C.This
It is because that large-scale cooling device can not be used, but stable oxide film thereon is formed using the small-sized cooling device such as cooler.
Further, in the present invention, treated object 1 is not limited to tabular, including the treated object of three-dimensional shape.This be because
For, despite the treated object of three-dimensional shape, oxide film thereon is also can partially form, treated object movement, rotation etc. are made, in shape
Position and other positions into oxide film thereon forms oxide film thereon.Further, since by with the portion for being initially formed oxide film thereon
When the adjacent position in position is as other positions, in a certain direction movement carries out continuous processing can to make treated object, thus is preferred
's.
In addition, " flat-shaped part " in this specification, including hole or surface is formed through irregular part is formed.
As the treated object 1 used in the present invention, as long as it is difficult to the aluminum or aluminum alloy of more than thickness 1mm for deforming i.e.
Can, for example, as aluminium alloy, fine aluminium system (JIS alloy models can be adopted：1N30,1050,1070,1080,1085), Al-Mn
System's (JIS alloy models：3005th, 3104), Al-Mg systems (JIS alloy models：5652nd, 5052,5454), Al-Mg-Si systems (JIS
Alloy model：6061st, 6063), Al-Cu systems (JIS alloy models：2011st, 2014,2017,2024), (JIS is closed for Al-Zn-Mg systems
Metal type number：7075 etc.) etc..
The electrolyte used in micro-arc oxidation process as the present invention, can adopt known used in the process
Electrolyte.For example, can be by disodium hydrogen phosphate, sodium tripolyphosphate, sodium dihydrogen phosphate, super polyphosphate sodium
(sodiumultrapolyphosphate), sodium metasilicate, potassium hydroxide, diphosphate sodium, tertiary sodium phosphate, sodium aluminate, sodium metasilicate
And a kind in NaOH etc. or the mixture in them is soluble in water uses.
The oxide film thereon of formation, for example, it is also possible to include using aluminum oxide as principal component, additionally, also containing such as hydrogen-oxygen
Change the material of the aluminium compounds such as aluminium.The thickness of the oxide film thereon, for example, less than more than 5 μm 30 μm, preferably more than 5 μm and 20 μm
Following scope.
In addition, the oxide film thereon formed according to the present invention, due to fine and close structure, for example, using the aluminium containing Si
During alloy, even if Si becomes crystalline state, by the effect of the Si, still can effectively suppress the increasing of the crystal defect of the oxide film thereon
Plus.Thus, the discharging amount for becoming the gas of impurity is suppressed to seldom.Therefore, aluminum or aluminum alloy of the invention, is adapted as height
The surface treatment of the vacuum plant part used under vacuum.
Embodiment
Below, embodiments of the invention are compared with comparative example and are illustrated.
In embodiment 1 and comparative example 1, as treated object, using aluminium alloy (A5052) cutting become into 40 × 80 ×
Sample obtained from the size of 2mm.
In addition, as the electrolyte of micro-arc oxidation process, using respectively by potassium hydroxide, sodium metasilicate and tertiary sodium phosphate
It is dissolved in the alkaline electrolyte that pure water reaches 3g/L.
Above-mentioned electrolyte is put in electrolytic cell of the carbon system of being provided with to electrode, electric current is determined with direct current carries out micro-arc oxidation
Process.
(embodiment 1)
The 40mm of the front end of the length direction of sample is impregnated in the electrolytic solution, with until 450V current densities are as 6.0A/
dm2After forming the 1st oxide film thereon, carry out determining voltage process with 450V, until current density reaches 0.28A/dm2, then, will try
Sample mass-impregnation in the electrolytic solution, with leading section the 2nd oxide film thereon is identically formed.In the whole operation for forming oxide film thereon
In, the temperature of electrolyte is below 65 DEG C.Terminate used in addition, being formed from the 1st oxide film thereon and starting to the 2nd oxide film thereon to be formed
Time be：1st oxide film thereon formed the time for 1.5 hours, and the 2nd oxide film thereon formed the time for 1.5 hours, added up to 3 hours.
(embodiment 2)
Method to embodiment 1, is 3.6A/dm except current density is made2In addition, enter under conditions of similarly to Example 1
OK.Further, the current density at the end of voltage is processed of determining after the 1st oxide film thereon is formed is 0.25A/dm2.Forming oxidation quilt
In the whole operation of film, the temperature of electrolyte is below 45 DEG C.In addition, formed from the 1st oxide film thereon starting to the 2nd oxide film thereon
Formation terminates the time used similarly to Example 1, adds up to 3 hours.
(comparative example 1)
At the front end 40mm of the length direction away from sample, sheltered with silicone encapsulant, by the 1st oxide film thereon and
2 oxide film thereons separate.After the 1st oxide film thereon is formed, from electrolyte treated object is lifted, after peeling masking material, form the 2nd
Oxide film thereon.With until 450V current densities are as 6.0A/dm2, electrolyte temperature processed for less than 65 DEG C.In addition, from the 1st
Oxide film thereon forms to start to the 2nd oxide film thereon to be formed and terminates the time used and be：Oxide film thereon formed the time be 1.5 hours,
The drying time of masking material is 24 hours, the overburden operation time of masking material is 1 hour, is added up to 26.5 hours, this for
1st and the 2nd oxide film thereon is necessary, therefore is added up to 53 hours.
Any one of embodiment 1 and 2, adopts the border of oxide film thereon of different operations formation all for uniform border.
As shown in the photo of the sample after the process of the embodiment 1 and 2 in Fig. 2, it is known that embodiment 1 and embodiment 2
Compare, the width width on border, the color distinction of the 1st and the 2nd oxide film thereon is big, forms striated apperance.
In addition, as shown in the optical microscope photograph of the embodiment 2 in the embodiment 1, Fig. 4 in Fig. 3, it is known that implement
Compared with Example 2, many in the boundary black splotch of the 1st and the 2nd oxide film thereon, configuration of surface is coarse for example 1.
In addition, in comparative example 1 when masking material is peeled off, due to being simply peeled away, therefore having used close for peeling off
The plastics scraper of envelope agent.Although plastics system, such as peeled off with scraper to neatly peel off, then to examination when peeling off
Sample causes to damage.
In addition, the time necessary to the formation of the oxide film thereon of comparative example 1 is understood, compared with embodiment 1 or embodiment 2,
Nearly 20 times are differed, inefficient.
Claims (4)
1. a kind of forming method of oxide film thereon, it is characterised in that in more than the thickness 1mm by the way that aluminum or aluminum alloy is constituted
Current density in the electrolytic solution, is set to 1～6A/dm by the part dipping of treated object2Carry out micro-arc oxidation process to be formed
Oxide film thereon, makes voltage be certain, carries out determining voltage process, and the current density determined when voltage processes beginning is reached in current density
1/100～1/10 after, the boundary at the position and other positions that define above-mentioned oxide film thereon is not provided with mask material, will
The position and other positions of above-mentioned oxide film thereon is defined while being immersed in above-mentioned electrolyte, current density is set to into 1～6A/
dm2Micro-arc oxidation process is carried out, thus, at above-mentioned other positions oxide film thereon is formed.
2. the forming method of the oxide film thereon described in claim 1, it is characterised in that from the front of above-mentioned treated object successively
Form above-mentioned oxide film thereon.
3. the forming method of the oxide film thereon described in claim 1 or 2, it is characterised in that when above-mentioned micro-arc oxidation is processed
Current density is 1～4A/dm2。
4. the forming method of the oxide film thereon described in claim 1 or 2, it is characterised in that in the shape of whole above-mentioned oxide film thereon
Into during, the temperature of above-mentioned electrolyte is -10 DEG C～65 DEG C of scope.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2011-198275 | 2011-09-12 | ||
| JP2011198275A JP5770575B2 (en) | 2011-09-12 | 2011-09-12 | Formation method of oxide film |
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| Publication Number | Publication Date |
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| CN102995089A CN102995089A (en) | 2013-03-27 |
| CN102995089B true CN102995089B (en) | 2017-05-03 |
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| CN201210345479.3A Active CN102995089B (en) | 2011-09-12 | 2012-09-12 | Oxidation capsule forming method |
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| JP (1) | JP5770575B2 (en) |
| KR (1) | KR101610994B1 (en) |
| CN (1) | CN102995089B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101709602B1 (en) * | 2015-12-10 | 2017-02-23 | 영남대학교 산학협력단 | Method of Aluminium Coating Layer with Anti-oxidation Using Micro arc Electrolytic Oxidation |
| CN106929897A (en) * | 2015-12-30 | 2017-07-07 | 比亚迪股份有限公司 | A kind of Al-alloy casing and preparation method thereof |
| JP6558649B2 (en) * | 2017-08-23 | 2019-08-14 | 株式会社アルバック | Surface treatment method and surface treatment apparatus |
| SG11202009058SA (en) * | 2018-07-30 | 2020-10-29 | Ulvac Techno Ltd | Substrate lifting apparatus and substrate transferring method |
| JP7218201B2 (en) * | 2019-02-13 | 2023-02-06 | アルバックテクノ株式会社 | Method for regenerating oxide film on aluminum parts |
| CN113913892A (en) * | 2021-10-29 | 2022-01-11 | 西安庄信新材料科技有限公司 | Micro-arc oxidation device with variable cathode area and surface treatment method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1954100A (en) * | 2004-01-12 | 2007-04-25 | 阿列克谢·亚历山德罗维奇·尼基福罗夫 | Method for producing heavy highly adhesive protective coatings on valve-metal parts by micro-arc oxidation |
| CN101082137A (en) * | 2007-03-12 | 2007-12-05 | 兰州理工大学 | Treatment fluid for improving performance of magnesium alloy differential arc oxidation film layer and pretreatment method |
| CN101210336A (en) * | 2006-12-31 | 2008-07-02 | 比亚迪股份有限公司 | Surface treatment method for light metal material |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE202004010821U1 (en) * | 2003-07-23 | 2004-12-23 | The Boc Group Plc, Windlesham | vacuum component |
| CN101057007B (en) * | 2004-11-05 | 2011-04-27 | 日本帕卡濑精株式会社 | Method of electrolytic ceramic coating for metal, electrolyte for use in electrolytic ceramic coating for metal, and metal material |
| JP4836921B2 (en) * | 2007-10-25 | 2011-12-14 | 株式会社アルバック | Surface treatment method |
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- 2011-09-12 JP JP2011198275A patent/JP5770575B2/en active Active
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- 2012-08-22 KR KR1020120091827A patent/KR101610994B1/en active IP Right Grant
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1954100A (en) * | 2004-01-12 | 2007-04-25 | 阿列克谢·亚历山德罗维奇·尼基福罗夫 | Method for producing heavy highly adhesive protective coatings on valve-metal parts by micro-arc oxidation |
| CN101210336A (en) * | 2006-12-31 | 2008-07-02 | 比亚迪股份有限公司 | Surface treatment method for light metal material |
| CN101082137A (en) * | 2007-03-12 | 2007-12-05 | 兰州理工大学 | Treatment fluid for improving performance of magnesium alloy differential arc oxidation film layer and pretreatment method |
Also Published As
| Publication number | Publication date |
|---|---|
| KR20130028856A (en) | 2013-03-20 |
| KR101610994B1 (en) | 2016-04-08 |
| CN102995089A (en) | 2013-03-27 |
| JP5770575B2 (en) | 2015-08-26 |
| JP2013060613A (en) | 2013-04-04 |
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