CN106119926A - A kind of ceramic coating formed by micro-arc oxidation and preparation method thereof - Google Patents
A kind of ceramic coating formed by micro-arc oxidation and preparation method thereof Download PDFInfo
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- CN106119926A CN106119926A CN201610804669.5A CN201610804669A CN106119926A CN 106119926 A CN106119926 A CN 106119926A CN 201610804669 A CN201610804669 A CN 201610804669A CN 106119926 A CN106119926 A CN 106119926A
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- arc oxidation
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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
- C25D11/30—Anodisation of magnesium or alloys based thereon
Abstract
The invention provides a kind of ceramic coating formed by micro-arc oxidation and preparation method thereof, including safeguarding oxidation processes and sealing pores, magnesium alloy processed by differential arc oxidation after at the strong ceramic membrane of Surface Creation corrosion resistance and thermal diffusivity, sealing pores is carried out again by pore-sealing liquid, strengthen the compactness of ceramic membrane, further enhancing the corrosion resistance of ceramic membrane.The present invention possesses advantages below: 1. form the ceramic membrane that one layer of thermal diffusivity is strong after magnesium alloy is processed by differential arc oxidation on surface, improve the radiating efficiency of magnesium alloy；2. in micro-arc oxidation electrolyte, with the addition of the additive comprising glycerol and tungstates, change the composition of ceramic membrane, enhance the corrosion resistance of ceramic membrane, thus add the corrosion resistance of magnesium alloy, extend service life；3. carry out sealing pores by pore-sealing liquid, make the consistency of ceramic membrane improve, improve the corrosion resistance of magnesium alloy further, solve the problem that ceramic coating formed by micro-arc oxidation color is single on the market at present simultaneously.
Description
Technical field
The present invention relates to differential arc oxidation field, particularly to a kind of ceramic coating formed by micro-arc oxidation and preparation method thereof.
Background technology
In recent years, magnesium alloy is due to its superior strength-weight ratio, good electromagnetic wave shielding and castability, the most increasingly
How to apply to the shell of electronic product, such as notebook, mobile phone etc., but this corrosion resistance to magnesium alloy, heat radiation simultaneously
Property, aging resistance, increase the service life etc. and to have higher requirement.
Differential arc oxidation be have at present most prospect and can improve efficiently Magnesium Anti-Corrosion surface treatment method it
One, it forms thick layer at Mg alloy surface by using different environmentally friendly electrolyte and has the pottery of excellent adhesion
Enamel coating, improves corrosion resistance and the service life of magnesium alloy.
The appearance color of ceramic coating formed by micro-arc oxidation is except white at present, only Lycoperdon polymorphum Vitt and black so that differential arc oxidation is business
Limited in the application of industry product, therefore provide a kind of perfect heat-dissipating, corrosion resistance by force and to carry coloured differential arc oxidation
Ceramic membrane is necessary.
Summary of the invention
Magnesium alloy defines one layer of protectiveness ceramic layer with microcellular structure after differential arc oxidation processes, and ceramic layer has
There is higher heat emissivity coefficient such that it is able to improve the efficiency that magnesium alloy carries out dispelling the heat by heat radiation mode.
The present invention provides a kind of ceramic coating formed by micro-arc oxidation and preparation method thereof, by forming one layer of differential of the arc at Mg alloy surface
Oxide ceramic membrane, improves the problem that Mg alloy surface decay resistance, heat dispersion and solution ceramic membrane color are single.
To achieve these goals, the present invention uses techniques below means: the preparation method of a kind of ceramic coating formed by micro-arc oxidation,
Process and sealing pores including differential arc oxidation, specifically include following step:
Silicate, phosphate and hydroxide are put in same container by S1, with deionized water dissolving, add comprise glycerol and
The additive of tungstates, prepares micro-arc oxidation electrolyte；
Sample is immersed in the electrolyte that S1 prepares by S2, carries out differential arc oxidation process, forms ceramic membrane at sample surfaces；
Sample after differential arc oxidation processes is carried out, is dried by S3；
Sample after S3 processes is put into and is carried out sealing pores in pore-sealing liquid by S4；
S5 retells the sample that S4 obtains and is dried, and can form, at sample surfaces, the ceramic coating formed by micro-arc oxidation that performance is good.
As a further improvement on the present invention, in S1, silicate is sodium silicate, and phosphate is sodium phosphate, and hydroxide is hydrogen
Sodium oxide；The concentration of described sodium silicate is 20g/L-30 g/L, and the concentration of described sodium phosphate is 5g/L-30 g/L, described hydrogen-oxygen
The concentration changing sodium is 3 g/L-6 g/L；Additive comprises glycerol and the tungstates of 0.5 g/L-2 g/L of 5 g/L-10 g/L.
As a further improvement on the present invention, when carrying out differential arc oxidation process, in electrolyte, the density of electric current is 0.03A/
cm2-0.17 A/cm2, pulse frequency is 500Hz-2600Hz, and the process time is 240 seconds-720 seconds；After treatment, magnesium closes
Gold surface forms one layer and has chemistry and the ceramic layer of mechanical protection performance, it is thus achieved that the thickness of ceramic coating formed by micro-arc oxidation be 5um-
40um。
As a further improvement on the present invention, sample deionized water and 100% ethanol after in S3, differential arc oxidation processes are clear
Wash, clean 5s-10s；S5 is dried process to the sample after sealing pores, and temperature is 60 DEG C-100 DEG C, and the time is
40min-70min。
Particularly, described pore-sealing liquid comprises the Na of 10g/L-20g/L2SiO3‧9H2The Ni of O, 2g/L-6g/L
(CH3COO)2‧4H2The H of O, 0.5g/L-2g/L3BO3, the thiourea of 0.5g/L-2g/L and deionized water, under room temperature, sample is soaked
Entering pore-sealing liquid 10min-60min, obtaining a kind of corrosion resistance is 9 grades, and thermal diffusivity is micro-not less than radiation test coefficient 0.87
Arc oxide ceramic membrane.
Particularly, described pore-sealing liquid comprises the Ce (NO of 10g/L-15 g/L3)3‧6H2The 35% of O, 0.5-1.2 g/L
H2O2, the H of 0.6 g/L-1.2 g/L3BO3, sample to be put in pore-sealing liquid, pore-sealing liquid temperature is 20 DEG C-50 DEG C, during process
Between be 20min-180min, obtaining a kind of corrosion resistance is 9 grades, and thermal diffusivity not less than radiation test coefficient 0.87 and color is
The ceramic coating formed by micro-arc oxidation of PANTONE P 4-15U color.
Beneficial effects of the present invention:
1., by configuring micro-arc oxidation electrolyte, after making magnesium alloy be processed, form one layer of thermal diffusivity by differential arc oxidation on surface
Strong ceramic membrane, improves the radiating efficiency of magnesium alloy；
2. in micro-arc oxidation electrolyte, with the addition of the additive comprising glycerol and tungstates, change the composition of ceramic membrane, increase
The strong corrosion resistance of ceramic membrane, thus add the corrosion resistance of magnesium alloy, extend service life；
3. carry out sealing pores by pore-sealing liquid, make the consistency of ceramic membrane improve, improve the anticorrosive of magnesium alloy further
Property, solve the problem that ceramic coating formed by micro-arc oxidation color is single on the market at present simultaneously；
4. the present invention provides the preparation method of a kind of ceramic coating formed by micro-arc oxidation, relative to common differential arc oxidation compound film technology,
The present invention has the features such as environmental protection, decay resistance is high, heat dispersion is more preferable, can be widely applied to electronic market.
Accompanying drawing explanation
Fig. 1 and Fig. 2 is the SEM image of the Mg alloy surface after differential arc oxidation processes respectively and seals based on cerium hole sealing solution
The SEM image of the magnesium alloy sample surfaces that the differential arc oxidation behind hole processed；
Fig. 3 is the magnesium alloy sample of the yellow differential arc oxidation sealing pores by preparing based on cerium pore-sealing liquid, and the color of sample is
Standard Colors code PANTONE P 4-15U color；
Fig. 4 and Fig. 5 magnesium alloy sample after untreated magnesium alloy sample and Microarc Oxidation Surface Treatment remote when being 90 DEG C respectively
Infrared radiation coefficient.
Detailed description of the invention
The present invention is further described below in conjunction with the accompanying drawings with specific embodiment.Unless stated otherwise, the present invention uses
Reagent, equipment and method be the art conventional commercial reagent, equipment and conventional use of method.
Embodiment one: prepare thermal diffusivity and the strong ceramic coating formed by micro-arc oxidation of decay resistance
Step 1, prepares micro-arc oxidation electrolyte
First, by the sodium silicate of 30g/L, the phosphoric acid of 8g/L is received and the sodium hydroxid of 5g/L, adds rustless steel container, uses deionization
Water dissolution.Then the sodium tungstate of 6g/L glycerol and 1g/L is added as additive.
Step 2, differential arc oxidation processes
The sample used in test is business level magnesium alloy AZ31B, and other magnesium alloys (such as AZ91D), content of magnesium is more than 88%
It is also applied for the present invention.Sample size is 30 mm × 1, mm × 30 mm.Sample is immersed above-described solution is carried out micro-
Arc oxidation processes, the electric current density of enforcement is 0.15 A/ cm2, pulse frequency is 1500Hz, 720 seconds persistent period.At Jing Guo
After reason, Mg alloy surface forms one layer of ceramic layer with chemistry and mechanical protection performance, and the thickness of ceramic layer is 30um.
Step 3, cleaning-drying processes
Under room temperature, by the sample that processes through differential arc oxidation at deionized water wash, it is then immersed in 100% ethanol, 8 seconds time,
Last dry in baking box, the temperature being dried is 70 DEG C, time 15min.
Step 4, sealing pores
Described another kind of sealing pores method is that sample immerses 15g/L Na2SiO3‧9H2O, 5g/L Ni (CH3COO)2‧
4H2O, 0.5g/L H3BO3In the solution formulated with 1.0 g/L thiourea and deionized water, by described solution left standstill 2 before using
Hour, described differential arc oxidation sample is at room temperature immersed 50min in above-mentioned pore-sealing liquid, the above-mentioned differential of the arc can be sealed by this method
The micropore of oxidized surface.
Step 5, dried
The described sample through sealing pores is dried process, and temperature is 100 DEG C, and the time is 50min.
Embodiment two: prepare the ceramic coating formed by micro-arc oxidation that color number is PANTONE P 4-15U
Step 1, prepares micro-arc oxidation electrolyte
First, by the sodium silicate of 25g/L, the phosphoric acid of 10g/L is received and the sodium hydroxid of 3g/L, adds rustless steel container, spend from
Sub-water dissolution.Then the sodium tungstate of 5g/L glycerol and 1g/L is added as additive.
Step 2, differential arc oxidation processes
The sample used in test is business level magnesium alloy AZ31B, and other magnesium alloys (such as AZ91D), content of magnesium is more than 88%
It is also applied for the present invention.Sample size is 30 mm × 1, mm × 30 mm.Sample is immersed above-described solution is carried out micro-
Arc oxidation processes, the electric current density of enforcement is 0.1 A/ cm2, pulse frequency is 600Hz, 240 seconds persistent period.Through processing
After, Mg alloy surface forms one layer of ceramic layer with chemistry and mechanical protection performance, and the thickness of ceramic layer is 10um.
Step 3, cleaning-drying processes
Under room temperature, by the sample that processes through differential arc oxidation at deionized water wash, it is then immersed in 100% ethanol, 6 seconds time,
Last dry in baking box, the temperature being dried is 60 DEG C, time 20min.
Step 4, sealing pores
First method be by cleaning-drying after sample immerse 10g/L Ce (NO3)3‧6H2O, 0.6g/L 35%H2O2, 1.0g/
L H3BO3In the solution being made into, keeping described solution temperature in dipping process is 30 DEG C, and the persistent period is 40min.Pass through
This method can seal the micropore of above-mentioned differential arc oxidization surface, and makes color sample become Standard Colors code PANTONE P 4-
15U color.
Step 5, dried
The described sample through sealing pores is dried process, and temperature is 80 DEG C, and the time is 60min.
Fig. 1 and Fig. 2 is the SEM image of the Mg alloy surface after differential arc oxidation processes respectively and seals based on cerium hole sealing solution
The SEM image of the magnesium alloy sample surfaces that the differential arc oxidation behind hole processed；Fig. 3 is the yellow by preparing based on cerium pore-sealing liquid
The magnesium alloy sample of differential arc oxidation sealing pores, the color of sample is Standard Colors code PANTONE P 4-15U color；Fig. 4
The far infrared radiation of magnesium alloy sample after untreated magnesium alloy sample and Microarc Oxidation Surface Treatment when being 90 DEG C respectively with Fig. 5
Coefficient.
The specific implementation method of present invention described above, is not intended that limiting the scope of the present invention.Any basis
Various other that the technology design of the present invention is made change and deformation accordingly, should be included in the guarantor of the claims in the present invention
In the range of protecting.
Claims (10)
1. a preparation method for ceramic coating formed by micro-arc oxidation, processes and sealing pores including differential arc oxidation, it is characterised in that include
Following steps:
Silicate, phosphate and hydroxide are put in same container by S1, with deionized water dissolving, add comprise glycerol and
The additive of tungstates, prepares micro-arc oxidation electrolyte；
Sample is immersed in the electrolyte that S1 prepares by S2, carries out differential arc oxidation process, forms ceramic membrane at sample surfaces；
Sample after differential arc oxidation processes is carried out, is dried by S3；
Sample after S3 processes is put into and is carried out sealing pores in pore-sealing liquid by S4；
S5 retells the sample that S4 obtains and is dried, and can form, at sample surfaces, the ceramic coating formed by micro-arc oxidation that performance is good.
The preparation method of ceramic coating formed by micro-arc oxidation the most according to claim 1, it is characterised in that described differential arc oxidation is electrolysed
In liquid, silicate is sodium silicate, and phosphate is sodium phosphate, and hydroxide is sodium hydroxide；Described sodium silicate is in the electrolytic solution
Concentration is 20g/L-30 g/L, and described sodium phosphate concentration in the electrolytic solution is 5g/L-30 g/L, and described sodium hydroxide is in electrolysis
Concentration in liquid is 3 g/L-6 g/L.
The preparation method of ceramic coating formed by micro-arc oxidation the most according to claim 1, it is characterised in that described additive comprises 5
The glycerol of g/L-10 g/L and the tungstates of 0.5g/L-2 g/L.
The preparation method of ceramic coating formed by micro-arc oxidation the most according to claim 1, it is characterised in that carry out differential arc oxidation process
Time, in electrolyte, the density of electric current is 0.03A/cm2-0.17 A/cm2, pulse frequency is 500Hz-2600Hz, and the process time is
240 seconds-720 seconds.
The preparation method of ceramic coating formed by micro-arc oxidation the most according to claim 1, it is characterised in that described pore-sealing liquid comprises
The Na of 10g/L-20g/L2SiO3‧9H2Ni (the CH of O, 2g/L-6g/L3COO)2‧4H2The H of O, 0.5g/L-2g/L3BO3、
The thiourea of 0.5g/L-2g/L and deionized water.
The preparation method of ceramic coating formed by micro-arc oxidation the most according to claim 1, it is characterised in that under room temperature, sample is immersed
10min-60min in pore-sealing liquid.
The preparation method of ceramic coating formed by micro-arc oxidation the most according to claim 1, it is characterised in that described pore-sealing liquid comprises
Ce (the NO of 10g/L-15 g/L3)3‧6H2The 35%H of O, 0.5-1.2 g/L2O2, the H of 0.6 g/L-1.2 g/L3BO3。
The preparation method of ceramic coating formed by micro-arc oxidation the most according to claim 1, it is characterised in that sample is put into 20 DEG C-
In the pore-sealing liquid of 50 DEG C, the process time is 20min-180min.
9. the ceramic coating formed by micro-arc oxidation that the preparation method described in a claim 1 prepares, it is characterised in that described ceramic layer
Corrosion resistance is 9 grades, and thermal diffusivity is not less than radiation test coefficient 0.87, and thickness is 5um-40um.
Ceramic coating formed by micro-arc oxidation the most according to claim 9, it is characterised in that the color of described ceramic membrane is PANTONE
P 4-15U color.
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Cited By (5)
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| CN107937961A (en) * | 2017-11-08 | 2018-04-20 | 天津正天医疗器械有限公司 | The aluminium alloy surface treatment method and pulse electrodeposition hole sealing device of differential arc oxidation combination pulse electrodeposition sealing of hole |
| CN108531955A (en) * | 2018-05-31 | 2018-09-14 | 杭州泛亚卫浴股份有限公司 | One kind being used for bathroom metal works micro-arc oxidization surface processing method |
| CN110904489A (en) * | 2019-12-03 | 2020-03-24 | 天津理工大学 | Micro-arc oxidation electrolyte for preparing high-corrosion-resistance coating on surface of low-carbon steel and preparation method and application thereof |
| CN111172573A (en) * | 2018-11-13 | 2020-05-19 | 北京艾路浦科技发展有限公司 | Preparation method of micro-arc oxidation ceramic membrane |
| CN114425835A (en) * | 2020-10-29 | 2022-05-03 | 比亚迪股份有限公司 | Ceramic matrix, ceramic plastic composite and preparation method thereof |
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| CN110904489A (en) * | 2019-12-03 | 2020-03-24 | 天津理工大学 | Micro-arc oxidation electrolyte for preparing high-corrosion-resistance coating on surface of low-carbon steel and preparation method and application thereof |
| CN114425835A (en) * | 2020-10-29 | 2022-05-03 | 比亚迪股份有限公司 | Ceramic matrix, ceramic plastic composite and preparation method thereof |
| CN114425835B (en) * | 2020-10-29 | 2023-08-08 | 比亚迪股份有限公司 | Ceramic matrix, ceramic plastic composite and preparation method thereof |
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Application publication date: 20161116 |