CN107829124A - A kind of colored epithelium manufacturing process for metal surface - Google Patents
A kind of colored epithelium manufacturing process for metal surface Download PDFInfo
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- CN107829124A CN107829124A CN201711084133.1A CN201711084133A CN107829124A CN 107829124 A CN107829124 A CN 107829124A CN 201711084133 A CN201711084133 A CN 201711084133A CN 107829124 A CN107829124 A CN 107829124A
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- epithelium
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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
- C25D11/026—Anodisation with spark discharge
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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
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
-
- 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
- C25D11/14—Producing integrally coloured layers
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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
- C25D11/18—After-treatment, e.g. pore-sealing
- C25D11/24—Chemical after-treatment
- C25D11/246—Chemical after-treatment for sealing layers
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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
- C25D11/26—Anodisation of refractory metals 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
- C25D11/30—Anodisation of magnesium 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
- C25D11/34—Anodisation of metals or alloys not provided for in groups C25D11/04 - C25D11/32
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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)
- General Chemical & Material Sciences (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The invention discloses a kind of colored epithelium manufacturing process for metal surface, it is mainly comprised the following steps：Plasma micro-arc oxidation processing is carried out to metal surface using the pulse power.The electrolyte used includes：6 10g/L basal liquids, 1 5g/L hole sealing agents, 1 5g/L stabilizers, 0.4 0.8g/L dispersants and 0.3 2g/L rare earth salt additives.Present invention process can carry out sealing of hole directly during plasma micro-arc oxidation, without extra post processing sealing of hole step.Manufacturing process cost of the present invention is low, and step is simple, without extra cumbersome technique, requires low to production equipment, the chromatic metallic epithelium wearability being prepared is high, good corrosion resistance.
Description
Technical field
The present invention relates to materials processing technology field, and in particular to a kind of colored epithelium for metal surface manufactures work
Skill.
Background technology
For electronics such as mobile phones, the shell of metal fuselage compared with plastic shell, have it is more attractive in appearance, hold
More texture, at the same it is more resistant and more resistant to scratch etc. superior performance characteristics, requirement of the people to the performance and outward appearance of mobile phone
More and more higher, therefore either spent for the angle that Consumer's Experience or manufacturer are sold, turned into using the shell of metal fuselage
Nowadays the main trend of mobile phone industry development.According to authoritative statistical organization IDC report, the shipment amount year of global smart mobile phone increases
Long rate has exceeded 10.1%, has exceeded 14.3 hundred million.The handling process that the metal surface of handset is initial is anodic oxidation, and
The technological trend that following mobile phone metal fuselage is surface-treated is differential arc oxidization technique, differential arc oxidation (Microarc
Oxidation, MAO) micro-plasma oxidation (Microplasma oxidation, MPO) is also known as, it is in phase by electrolyte
Under conditions of answering electrical parameter, TRANSIENT HIGH TEMPERATURE high pressure caused by arc discharge is relied on to act in aluminium, magnesium, titanium and its alloy surface, it is raw
Grow the ceramic film based on substrate metal oxide.The colored epithelium for metal surface that the present invention is researched and developed manufactures work
Skill, the film layer using plasma discharge phenomenon in electrolyte in non-ferrous metal surface growth in situ into one layer of even compact, is carried
The metallicity of high alumina and aluminium alloy.Closing, oxidation synchronously complete with coloring, without dyeing, (have with traditional chemical dyeing
Engine dyeing material, inorganic dyestuff) to compare, this technology has simple to operate and the characteristics of be easily achieved film layer function point analysis, and technique
Simply, environmental pollution is not caused, is the ep-type material process for treating surface of a novel green.In addition, the present invention can be right
Metal material or other materials are covered, and its epithelium feel is finer and smoother, and metal-like is stronger.In addition, plasma can be simultaneously
High temperature hole sealing, surface do not produce pin hole, spot, silking, effectively shorten manufacturing time without colour fading.
The content of the invention
The problem of existing for prior art, it is an object of the invention to provide a kind of colored epithelium system for metal surface
Make technique.
To achieve these goals, the present invention uses following technical scheme：
A kind of colored epithelium manufacturing process for metal surface, comprise the following steps：
(1) oil removing, washing, alkaline etching, washing, pickling, washing process are carried out successively to prefabricated metal unplated piece；
(2) in 30-70 DEG C of drying；
(3) the metal unplated piece after drying is put into the electrolytic cell equipped with electrolyte, the electrolyte includes：6-10g/
L basal liquids, 1-5g/L hole sealing agents, 1-5g/L stabilizers, 0.4-0.8g/L dispersants and 0.3-2g/L rare earth salt additives；
(4) plasma micro-arc oxidation processing is carried out.
Preferably, the material of the metal unplated piece is aluminium alloy, titanium alloy, magnesium alloy or kirsite.
Preferably, the basal liquid be sodium phosphate, sodium polyphosphate, potassium phosphate, potassium polyphosphate, sodium chloride, potassium chloride,
One or more aqueous solution in sodium metasilicate, potassium silicate, sodium molybdate, potassium molybdate.
Preferably, the hole sealing agent is vinyl, phenolic resin, epoxy resin, polyurethane, aluminium vinyl, aluminium
One or more in silicone resin.
Preferably, the stabilizer is ethylene glycol and/or glycerine.
Preferably, the dispersant is polyoxyethylene aliphatic alcohol ether and/or aliphatic acid polyethenoxy ether.
Preferably, the rare earth salt additives are neodymium chloride, Europium chloride, inidum chloride, cerium chloride, praseodymium chloride, lanthanum chloride, nitre
Sour dysprosium, europium nitrate, gallium nitrate, indium nitrate, cerous nitrate, lanthanum nitrate, praseodymium nitrate, neodymium nitrate, lanthanum sulfate, cerous sulfate, Dineodymium trisulfate, sulphur
One or more in sour praseodymium.
Preferably, the plasma micro-arc oxidation treatment conditions are：Power supply used is the pulse power, pulse frequency 300-
4000Hz, dutycycle 10%-50%, whole voltage are 200-1000V, current density 20-100mA/cm2, electrolyte temperature
For 20-50 DEG C, the differential arc oxidation time is 10-30min.
Beneficial effects of the present invention：
(1) present invention process carries out sealing of hole directly in micro-arc oxidation process, it is not necessary to which post processing carries out sealing of hole, and technique is more
Simply；
(2) the micro-arc oxidation films wearability of present invention process preparation, good corrosion resistance；
(3) present invention process working condition is controllable, require low to production equipment, production efficiency is high.
Embodiment
In order to preferably explain the present invention, it is described further in conjunction with specific examples below, but the present invention is unlimited
In specific embodiment.
Embodiment 1
A kind of colored epithelium manufacturing process for metal surface, step are as follows：
(1) oil removing, washing, alkaline etching, washing, pickling, washing process are carried out successively to prefabricated aluminium alloy unplated piece；
(2) in 50 DEG C of drying；
(3) 6g/L sodium molybdate aqueous solutions, 1g/L aluminium vinyl, 1g/L glycerine, 0.4g/L polyethylene glycol oxides fat are prepared
The electrolyte of alcohol ether and 0.3g/L cerium chlorides, the aluminium alloy unplated piece after drying is put into the electrolytic cell equipped with electrolyte；
(4) it is whole using pulse power progress plasma micro-arc oxidation processing, pulse frequency 300Hz, dutycycle 10%
Voltage is 200V, current density 20mA/cm2, electrolyte temperature is 20 DEG C, and the differential arc oxidation time is 10min.
Embodiment 2
A kind of colored epithelium manufacturing process for metal surface, step are as follows：
(1) oil removing, washing, alkaline etching, washing, pickling, washing process are carried out successively to prefabricated aluminium alloy unplated piece；
(2) in 50 DEG C of drying；
(3) 10g/L sodium molybdate aqueous solutions, 5g/L aluminium vinyl, 5g/L glycerine, 0.8g/L polyethylene glycol oxides fat are prepared
The electrolyte of alcohol ether and 2g/L cerium chlorides, the aluminium alloy unplated piece after drying is put into the electrolytic cell equipped with electrolyte；
(4) using the pulse power carry out plasma micro-arc oxidation processing, pulse frequency 4000Hz, dutycycle 50%,
Whole voltage is 1000V, current density 100mA/cm2, electrolyte temperature is 50 DEG C, and the differential arc oxidation time is 30min.
Embodiment 3
A kind of colored epithelium manufacturing process for metal surface, step are as follows：
(1) oil removing, washing, alkaline etching, washing, pickling, washing process are carried out successively to prefabricated aluminium alloy unplated piece；
(2) in 50 DEG C of drying；
(3) 8g/L sodium molybdate aqueous solutions, 3g/L aluminium vinyl, 3g/L glycerine, 0.6g/L polyethylene glycol oxides fat are prepared
The electrolyte of alcohol ether and 1g/L cerium chlorides, the aluminium alloy unplated piece after drying is put into the electrolytic cell equipped with electrolyte；
(4) using the pulse power carry out plasma micro-arc oxidation processing, pulse frequency 2000Hz, dutycycle 30%,
Whole voltage is 500V, current density 60mA/cm2, electrolyte temperature is 35 DEG C, and the differential arc oxidation time is 20min.
Embodiment 4
A kind of colored epithelium manufacturing process for metal surface, step are as follows：
(1) oil removing, washing, alkaline etching, washing, pickling, washing process are carried out successively to prefabricated aluminium alloy unplated piece；
(2) in 50 DEG C of drying；
(3) 8g/L sodium silicate aqueous solutions, 3g/L aluminium silicone resin, 3g/L ethylene glycol, 0.6g/L aliphatic acid polyoxy second are prepared
The electrolyte of alkene ether and 1g/L cerium chlorides, the aluminium alloy unplated piece after drying is put into the electrolytic cell equipped with electrolyte；
(4) using the pulse power carry out plasma micro-arc oxidation processing, pulse frequency 2000Hz, dutycycle 30%,
Whole voltage is 500V, current density 60mA/cm2, electrolyte temperature is 35 DEG C, and the differential arc oxidation time is 20min.
Embodiment 5
A kind of colored epithelium manufacturing process for metal surface, step are as follows：
(1) oil removing, washing, alkaline etching, washing, pickling, washing process are carried out successively to prefabricated aluminium alloy unplated piece；
(2) in 50 DEG C of drying；
(3) 8g/L sodium molybdate aqueous solutions, 3g/L aluminium vinyl, 3g/L glycerine, 0.6g/L polyethylene glycol oxides fat are prepared
The electrolyte of alcohol ether and 1g/L gallium nitrates, the aluminium alloy unplated piece after drying is put into the electrolytic cell equipped with electrolyte；
(4) using the pulse power carry out plasma micro-arc oxidation processing, pulse frequency 2000Hz, dutycycle 30%,
Whole voltage is 500V, current density 60mA/cm2, electrolyte temperature is 35 DEG C, and the differential arc oxidation time is 20min.
Embodiment 6
A kind of colored epithelium manufacturing process for metal surface, step are as follows：
(1) oil removing, washing, alkaline etching, washing, pickling, washing process are carried out successively to prefabricated magnesium alloy unplated piece；
(2) in 50 DEG C of drying；
(3) 8g/L sodium molybdate aqueous solutions, 3g/L aluminium vinyl, 3g/L glycerine, 0.6g/L polyethylene glycol oxides fat are prepared
The electrolyte of alcohol ether and 1g/L praseodymium sulfates, the magnesium alloy unplated piece after drying is put into the electrolytic cell equipped with electrolyte；
(4) using the pulse power carry out plasma micro-arc oxidation processing, pulse frequency 2000Hz, dutycycle 30%,
Whole voltage is 500V, current density 60mA/cm2, electrolyte temperature is 35 DEG C, and the differential arc oxidation time is 20min.
Embodiment 7
A kind of colored epithelium manufacturing process for metal surface, step are as follows：
(1) oil removing, washing, alkaline etching, washing, pickling, washing process are carried out successively to prefabricated magnesium alloy unplated piece；
(2) in 50 DEG C of drying；
(3) 8g/L sodium molybdate aqueous solutions, 3g/L aluminium vinyl, 3g/L glycerine, 0.6g/L polyethylene glycol oxides fat are prepared
Alcohol ether and 0.5g/L gallium nitrates, the electrolyte of 0.5g/L praseodymium sulfates, the magnesium alloy unplated piece after drying is put into equipped with electrolyte
Electrolytic cell in；
(4) using the pulse power carry out plasma micro-arc oxidation processing, pulse frequency 2000Hz, dutycycle 30%,
Whole voltage is 500V, current density 60mA/cm2, electrolyte temperature is 35 DEG C, and the differential arc oxidation time is 20min.
Comparative example 1
A kind of colored epithelium manufacturing process for metal surface, its step are carried out according to embodiment 1, the difference is that being electrolysed
Rare earth salt additives cerium chloride is not contained in liquid.
The micro-arc oxidation films metal surface that embodiment 1-7 and comparative example 1 are obtained carries out scratch resistance test, pencil hardness is surveyed
Try (ASTMD 3363-74), resistance to soiling test, the test of RCA paper tapes wear-resisting test, surface roughness, neutral salt spray test, test
It the results are shown in Table 1.
Table 1
As can be known from the results of Table 1, the metal surface film layer of differential arc oxidation preparation, resistance to soiling are carried out using the technique of the present invention
Energy, scratch resistance are more preferable, and hardness is very high, and surface roughness is lower, i.e., compactness is more preferable.Particularly embodiment 7 selects 1：1 nitric acid
Gallium and praseodymium sulfate as rare-earth salts additive compound into electrolyte when, the property indices of metal surface are best.
Method of testing：
(1) scratch resistance is tested
Scratch resistance test is carried out with scratching instrument, the gauge head of scratching instrument is the diamond of 0.75 millimeter of diameter, and test angle is
90 °, apply 1N, 2N, 3N ... power respectively in test product surface, if applying the power product surfaces of 3N (containing) below without drawing
Trace, then test product scratch resistance performance is qualified, otherwise to be unqualified.
(2) pencil hardness test
Using the pencil hardometer F130027 methods of inspection, tested according to ASTM D3363 under 750 grams of loads.
(3) resistance to soiling is tested
After picking test solvent isopropanol, artificial perspiration, gasoline with cotton respectively, rubbed 2 minutes in product surface, product table
Face should come off without discoloration, nothing；Test solvent lipstick, hand lotion, vanishing cream, edible oil, insecticide, suntan lotion are being produced respectively again
The coating of product surface is uniform, is rinsed after placing 24 hours with water, product surface should without discoloration, without stains be qualified.
(4) RCA paper tapes wear-resisting test
Use model F350008 RCA paper tape wear resistant instruments, the micro-arc oxidation films for the product surface that rubbed under 175 gram forces
Layer, it is milled to when exposing metal material surface, the number of turns that record rubber wheel rotates.
(5) surface roughness is tested
Use Ra values (arithmetic mean of instantaneous value of roughness value, the method for testing on 3D contourgraph test products surface：Instrument is automatic
Scanning, show result).
(6) neutral salt spray is tested
Outturn sample is placed in salt fog cabinet, it is small with 5 ± 0.5 weight % sodium chloride brine spraying sample 8 at 35 DEG C
Shi Hou, taking-up are observed, and the corroded area of record product sample surfaces accounts for the percentage composition of the coating gross area.
The specific embodiment of the present invention is the foregoing is only, is not intended to limit the scope of the invention, every utilization
The equivalent transformation that the present invention makees, or other related technical fields are directly or indirectly used in, similarly it is included in the present invention's
Among scope of patent protection.
Claims (8)
1. a kind of colored epithelium manufacturing process for metal surface, it is characterised in that comprise the following steps：
(1) oil removing, washing, alkaline etching, washing, pickling, washing process are carried out successively to prefabricated metal unplated piece；
(2) in 30-70 DEG C of drying；
(3) the metal unplated piece after drying is put into the electrolytic cell equipped with electrolyte, the electrolyte includes：6-10g/L bases
Plinth liquid, 1-5g/L hole sealing agents, 1-5g/L stabilizers, 0.4-0.8g/L dispersants and 0.3-2g/L rare earth salt additives；
(4) plasma micro-arc oxidation processing is carried out.
2. the colored epithelium manufacturing process according to claim 1 for metal surface, it is characterised in that the metal is treated
The material of plating piece is aluminium alloy, titanium alloy, magnesium alloy or kirsite.
3. the colored epithelium manufacturing process according to claim 1 for metal surface, it is characterised in that in step (3)
The basal liquid be sodium phosphate, sodium polyphosphate, potassium phosphate, potassium polyphosphate, sodium chloride, potassium chloride, sodium metasilicate, potassium silicate,
One or more aqueous solution in sodium molybdate, potassium molybdate.
4. the colored epithelium manufacturing process according to claim 1 for metal surface, it is characterised in that in step (3)
The hole sealing agent is one kind in vinyl, phenolic resin, epoxy resin, polyurethane, aluminium vinyl, aluminium silicone resin
It is or a variety of.
5. the colored epithelium manufacturing process according to claim 1 for metal surface, it is characterised in that in step (3)
The stabilizer is ethylene glycol and/or glycerine.
6. the colored epithelium manufacturing process for metal surface according to claim, it is characterised in that institute in step (3)
It is polyoxyethylene aliphatic alcohol ether and/or aliphatic acid polyethenoxy ether to state dispersant.
7. the colored epithelium manufacturing process according to claim 1 for metal surface, it is characterised in that in step (3)
The rare earth salt additives are neodymium chloride, Europium chloride, inidum chloride, cerium chloride, praseodymium chloride, lanthanum chloride, dysprosium nitrate, europium nitrate, nitre
One kind in sour gallium, indium nitrate, cerous nitrate, lanthanum nitrate, praseodymium nitrate, neodymium nitrate, lanthanum sulfate, cerous sulfate, Dineodymium trisulfate, praseodymium sulfate or
It is a variety of.
8. the colored epithelium manufacturing process according to claim 1 for metal surface, it is characterised in that in step (4)
The plasma micro-arc oxidation treatment conditions are：Power supply used is the pulse power, pulse frequency 300-4000Hz, and dutycycle is
10%-50%, whole voltage are 200-1000V, current density 20-100mA/cm2, electrolyte temperature is 20-50 DEG C, differential of the arc oxygen
The change time is 10-30min.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711084133.1A CN107829124A (en) | 2017-11-07 | 2017-11-07 | A kind of colored epithelium manufacturing process for metal surface |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711084133.1A CN107829124A (en) | 2017-11-07 | 2017-11-07 | A kind of colored epithelium manufacturing process for metal surface |
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| CN107829124A true CN107829124A (en) | 2018-03-23 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109056028A (en) * | 2018-07-20 | 2018-12-21 | 江苏飞拓界面工程科技有限公司 | A kind of aluminium and aluminium alloy anode oxide aftertreatment fluid and preparation method thereof |
-
2017
- 2017-11-07 CN CN201711084133.1A patent/CN107829124A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109056028A (en) * | 2018-07-20 | 2018-12-21 | 江苏飞拓界面工程科技有限公司 | A kind of aluminium and aluminium alloy anode oxide aftertreatment fluid and preparation method thereof |
| CN109056028B (en) * | 2018-07-20 | 2021-04-06 | 江苏飞拓界面工程科技有限公司 | Aluminum and aluminum alloy anodic oxidation post-treatment fluid and preparation method thereof |
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Application publication date: 20180323 |