CN107227480A - A kind of utilization weak acid dye is the method that magnesium material differential arc oxidation film layer is coloured - Google Patents
A kind of utilization weak acid dye is the method that magnesium material differential arc oxidation film layer is coloured Download PDFInfo
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- CN107227480A CN107227480A CN201710392538.5A CN201710392538A CN107227480A CN 107227480 A CN107227480 A CN 107227480A CN 201710392538 A CN201710392538 A CN 201710392538A CN 107227480 A CN107227480 A CN 107227480A
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- Prior art keywords
- film layer
- differential arc
- arc oxidation
- oxidation film
- magnesium material
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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
-
- 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
Abstract
It is the method that magnesium material differential arc oxidation film layer is coloured the invention discloses a kind of utilization weak acid dye, including：Carrying out surface treatment to magnesium material using differential arc oxidization technique makes magnesium material surface in situ grow differential arc oxidation film layer；Immersion coloring is carried out to magnesium material surface in situ growth differential arc oxidation film layer using staining solution；Staining solution is mixed by weak acid dye, dye leveller, pH value regulator and deionized water, and weak acid dye content is 1~10g/L in staining solution, dye leveller is that glauber salt and neopelex, every kind of levelling agent content are 1~5g/L, and the consumption of pH value regulator makes pH value=4.5~5.0 of staining solution.The present invention can not only make magnesium material differential arc oxidation film layer that the beautiful color of various bright-coloured light is presented, magnesium material differential arc oxidation film layer itself is kept to have compared with high-bond and wearability, and simple production process, easily realize volume production, human body and equipment will not be caused corrosion, do not result in environmental pollution.
Description
Technical field
The present invention relates to magnesium material, (the magnesium material refers to magnesium or magnesium alloy, for example：The typical magnesium alloys such as AZ31, AZ61B) surface
Dye technology field, more particularly to a kind of utilization weak acid dye are the method that magnesium material differential arc oxidation film layer is coloured.
Background technology
Magnesium material is the class important meals material that consumption is only second to steel, in Aero-Space, communications and transportation, printing, building
It is widely used Deng field.But magnesium material color is single, corrosion resistance is poor, it is difficult to which it is ornamental to magnesium material and anti-corrosion to meet various industries
The requirement of property.In order to improve magnesium material decorative effect, enhancing corrosion resistance, increase the service life, magnesium material will typically carry out table
Face is handled.
In the last few years, ripe magnesium material surface coloring process mainly had anode oxide film dyestuff colouring, anode oxide film
Electrocolor process, the direct colouring of anodic oxidation etc., but these coloring process can all bring problem of environmental pollution, therefore it is a kind of new
Type process for treating surface --- differential arc oxidization technique just arises at the historic moment.Differential arc oxidization technique breaches conventional anodization technology pair
The limitation of operating voltage, high voltage discharge field is incorporated into by working region, using the instantaneous high-temperature agglomeration of differential of the arc area directly in magnesium
Or the surface in situ growth ceramic layer of magnesium alloy, it is a kind of up-and-coming metal watch so as to improve the surface property of magnesium material
Face treatment technology.
At present, magnesium material is surface-treated using differential arc oxidization technique, white, black etc. can only be formed on magnesium material surface
The differential arc oxidation film layer being faint in color, is hardly formed the beautiful differential arc oxidation film layer of bright-colored light.In the prior art, it can pass through
Cu is added in acidic electrolysis bath2+、Co+Blue differential arc oxidation film layer, but acid electricity are formed on magnesium material surface Deng metal cation
Solution liquid can cause larger corrosion to microarc oxidation equipment provided using stainless steel as reactive tank, and environment can be produced certain
Pollution；The method that a kind of coloring of magnesium alloy micro-arc oxidation composite membrane is disclosed in patent CN103556205A, this method be by containing
There is Cu2+SiO2-ZrO2Colloid solidifies on magnesium alloy surface micro-arc oxidation film, its complex operation, to temperature and hardening time
Control requires higher, is not easy to carry out magnesium alloy surface micro-arc oxidation film layer low-cost, high-volume coloring treatment.
The content of the invention
For above-mentioned weak point of the prior art, weak acid dye is utilized to be the magnesium material differential of the arc the invention provides one kind
The method of oxidation film layer coloring, can not only make magnesium material differential arc oxidation film layer that the beautiful color of various bright-coloured light is presented, keep magnesium material
Differential arc oxidation film layer itself has the corrosion resistance that magnesium material differential arc oxidation film layer is improved compared with high-bond and wearability, Er Qiesheng
Production. art is simple, easily realize volume production, corrosion will not be caused to human body and equipment, does not result in environmental pollution.
The purpose of the present invention is achieved through the following technical solutions：
A kind of utilization weak acid dye is the method that magnesium material differential arc oxidation film layer is coloured, including：Utilize differential arc oxidization technique
Surface treatment is carried out to magnesium material makes magnesium material surface in situ grow differential arc oxidation film layer, in addition to：Using staining solution to the magnesium
Material surface in situ growth differential arc oxidation film layer carries out immersion coloring；Wherein, the staining solution by weak acid dye, dye leveller,
PH value regulator and deionized water are mixed, and the content of weak acid dye is 1~10g/L in the staining solution,
Stain is that glauber salt and neopelex, the content of every kind of dye leveller are 1~5g/L, and the consumption of pH value regulator makes
The pH value of the staining solution is adjusted at 20 DEG C between 4.5~5.0.
Preferably, the soak time of the immersion coloring is 1~12 hour, and the longer color of soak time is deeper.
Preferably, magnesium material surface in situ growth differential arc oxidation film layer is carried out using staining solution on coloring apparatus
Immersion coloring, and in the immersion coloring process, the agitating device speed of agitator of the coloring apparatus is 500~1000r/
Min, the thermostat temperature of the coloring apparatus is 20~40 DEG C, and the ultrasonic generator power of the coloring apparatus is 100
~200W.
Preferably, the magnesium material surface in situ growth differential arc oxidation film layer, its surface micropore size is 0.5~5.0 μm, its
Thicknesses of layers is more than 5 μm.
Preferably, described weak acid dye is monoazo class dyestuff.
As seen from the above technical solution provided by the invention, the utilization weak acid dye that the present invention is provided is micro- for magnesium material
The method of arc oxidation film layer coloring is soaked using staining solution to many space differential arc oxidation film layers that magnesium material surface in situ grows
Bubble coloring, and the staining solution uses the weak acid dye without heavy metal ion for raw material, with glauber salt and dodecyl
Benzene sulfonic acid sodium salt is dye leveller, and pH value is between 4.5~5.0, therefore the utilization weak acid dye that the present invention is provided is the magnesium material differential of the arc
The method of oxidation film layer coloring can not only make magnesium material differential arc oxidation film layer that the beautiful color of various bright-coloured light is presented, and keep magnesium material micro-
Arc oxidation film layer itself has the corrosion resistance that magnesium material differential arc oxidation film layer is improved compared with high-bond and wearability, and production
Technique is simple, easily realize volume production, corrosion will not be caused to human body and equipment, does not result in environmental pollution.
Brief description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, being used required in being described below to embodiment
Accompanying drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for this
For the those of ordinary skill in field, on the premise of not paying creative work, other can also be obtained according to these accompanying drawings
Accompanying drawing.
Fig. 1 is in situ to AZ31 magnesium alloys disk surfaces in the embodiment of the present invention 1 using SSX-550 SEM
The differential arc oxidation film layer of growth is observed, the electron scanning micrograph obtained from.
Fig. 2 is to the micro-arc oxidation films after immersion coloring in the embodiment of the present invention 1 using SSX-550 SEM
Layer is observed, the electron scanning micrograph obtained from.
Fig. 3 be the embodiment of the present invention 1 in immersion coloring after pink differential arc oxidation film layer photomacrograph schematic diagram.
Fig. 4 be the embodiment of the present invention 1 in immersion coloring after bright yellow differential arc oxidation film layer photomacrograph schematic diagram.
Embodiment
With reference to the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Ground is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based on this
The embodiment of invention, the every other implementation that those of ordinary skill in the art are obtained under the premise of creative work is not made
Example, belongs to protection scope of the present invention.
Below to being retouched in detail using the method that weak acid dye is the coloring of magnesium material differential arc oxidation film layer in the present invention
State.
A kind of utilization weak acid dye is the method that magnesium material differential arc oxidation film layer is coloured, including：Utilize differential arc oxidization technique
Surface treatment is carried out to magnesium material makes magnesium material surface in situ grow differential arc oxidation film layer, and using staining solution to the magnesium material surface
Growth in situ differential arc oxidation film layer carries out immersion coloring.
Wherein, the staining solution is mixed by weak acid dye, dye leveller, pH value regulator and deionized water, and
And the content of weak acid dye is 1~10g/L in the staining solution, dye leveller be glauber salt and neopelex,
The content of every kind of dye leveller is 1~5g/L, and the consumption of pH value regulator makes the pH value of the staining solution be adjusted at 20 DEG C
To between 4.5~5.0.
Specifically, this is that the method that magnesium material differential arc oxidation film layer is coloured may include following embodiment party using weak acid dye
Case：
(1) immersion coloring is carried out to magnesium material surface in situ growth differential arc oxidation film layer using staining solution, soaked
The soak time of color is 1~12 hour, and can freely adjust soak time according to the depth of required dyeing, and soak time is got over
Long dyeing is deeper, so as to so that the beautiful color of various bright-coloured light is presented in magnesium material differential arc oxidation film layer.
(2) using staining solution to the magnesium material surface in situ growth differential arc oxidation film layer carry out immersion coloring preferably
Carried out in color equipment；Coloring apparatus can be using in the prior art with agitating device, thermostat and ultrasonic generator
Coloring apparatus, and in described immersion coloring process, the agitating device speed of agitator of the coloring apparatus for 500~
1000r/min, the thermostat temperature of the coloring apparatus is 20~40 DEG C, the ultrasonic generator power of the coloring apparatus
It can be adjusted in 100~200W.
(3) differential arc oxidation film layer of magnesium material surface in situ growth has higher porosity, and its surface micropore size is 0.5
~5.0 μm, its thicknesses of layers is more than 5 μm, so as to so that differential arc oxidation film layer itself is carried with compared with high-bond and wearability
The corrosion resistance of high magnesium material differential arc oxidation film layer, dyeing is more firm, difficult for drop-off.
(4) weak acid dye described in uses the weak acid dye without heavy metal ion, for example：Weak acid dye is main
Monoazo class dyestuff can be used, minority can use di-azo dyes, and dye colour can be using BG- is pink, SE-
4EL is light yellow, RAWV- blue three-colors, will not because these weak acid dyes are without the larger heavy metal ion of environmental pollution
Corrosion is caused to human body and equipment, environmental pollution is not resulted in.
(5) dye leveller described in can use any hydrophilic dispersion auxiliary agent of the prior art, due to detergent alkylate
Sodium sulfonate is anionic surfactant, and, but it has micro- toxicity to weak acid dye dispersion effect preferably；Glauber salt is in acid
Property solution in can also play a part of dispersing aid, it is and non-toxic, therefore the present invention substitutes part 12 using glauber salt
The use of sodium alkyl benzene sulfonate, that is to say, that preferably with glauber salt and the mixed liquor of neopelex in the present invention,
And the content of glauber salt and neopelex is preferably 1~5g/L in the staining solution.
(6) pH value regulator described in can be using any pH value regulator in the prior art, due to the staining solution
PH value between 4.5~5.0, if containing acetic acid or oxalic acid in the dyeing, larger corruption can be produced to differential arc oxidation film layer
Lose, therefore the pH value regulator in the present invention is preferably with sodium dihydrogen phosphate and sodium acid carbonate, to mitigate to differential arc oxidation film layer
Corrosion, and human body and equipment will not be caused corrosion, do not result in environmental pollution yet, disclosure satisfy that every profession and trade to the magnesium material differential of the arc
The requirement of oxidation film layer dyeing.
(7) the magnesium material described in refers to magnesium or magnesium alloy, for example：Magnesium alloy can using magnesium lithium alloy of the prior art,
The typical magnesium alloys such as AZ31, AZ61B.
As fully visible, the present invention can not only make magnesium material differential arc oxidation film layer that the beautiful color of various bright-coloured light is presented, and keep
Magnesium material differential arc oxidation film layer itself has the corrosion resistance that magnesium material differential arc oxidation film layer is improved compared with high-bond and wearability, and
And simple production process, easily realize volume production, human body and equipment will not be caused corrosion, do not result in environmental pollution.
In order to more clearly from show technical scheme provided by the present invention and produced technique effect, below with tool
The utilization weak acid dye that body embodiment is provided the present invention is described in detail for the method that magnesium material differential arc oxidation film layer is coloured.
Embodiment 1
A kind of utilization weak acid dye is the method that magnesium material differential arc oxidation film layer is coloured, and uses the radius to be for 15mm, thickness
3mm AZ31 magnesium alloys disk includes as pending magnesium material matrix, its specific process：
(1) pretreatment process：Successively using 400#, 600#, 800#, 1000#, 1200#, 1500# sand paper to described
The surfaces of AZ31 magnesium alloy disks carries out polishing from coarse to fine, then is polished successively, is cleaned by ultrasonic and (can use absolute ethyl alcohol
Or acetone is cleaned by ultrasonic), dry, so as to obtain pretreated AZ31 magnesium alloys disk.
(2) differential arc oxidation process：Pretreated AZ31 magnesium alloys disk is carried out at surface using differential arc oxidization technique
Reason makes the surface in situ of AZ31 magnesium alloy disks grow the differential arc oxidation film layer that white is presented.
Specifically, micro-arc oxidation electrolyte is poured into microarc oxidation equipment provided reactive tank of the prior art, and will be pre-
AZ31 magnesium alloy disks after processing are immersed in the micro-arc oxidation electrolyte in the reactive tank, then with pretreated AZ31 magnesium
Alloy disk is as anode, using the reactive tank as negative electrode, is 250~400V, electricity in operating voltage using direct current pulse power source
Source dutycycle is progress differential arc oxidation processing under conditions of 30~60%, and micro-arc oxidation electrolyte temperature is 20~35 DEG C, the differential of the arc
The processing time of oxidation is 5~60min；After differential arc oxidation processing terminates, AZ31 magnesium alloy disks are done with deionized water rinsing
Only, then with hair-dryer dry up, so that obtaining surface in situ grows the AZ31 magnesium alloy disks that white differential arc oxidation film layer is presented.
In actual applications, micro-arc oxidation electrolyte can be made of following methods：It is 10L clean beaker to take a capacity, and
1L water is added in the beaker, 5~20g/L film forming agents, 5~10g/L auxiliary film formers, the work of 1~5g/L surfaces is then sequentially added
Property agent, adds pH value regulator, the micro-arc oxidation electrolyte is obtained pH value and reach 10.0~11.0 at 20 DEG C.
(3) immersion coloring process：It is in situ to AZ31 magnesium alloys disk surfaces using the staining solution of pink or bright yellow
The differential arc oxidation film layer of growth carries out immersion coloring, so as to obtain AZ31 of the micro-arc oxidation films layer surface in pink or bright yellow
Magnesium alloy disk.
Specifically, the staining solution of pink or bright yellow is poured among coloring apparatus, then surface in situ growth is had
The AZ31 magnesium alloy disks of differential arc oxidation film layer are soaked in the staining solution, heat the staining solution make its temperature rise to 20~
40 DEG C, magnetic agitation 500~1000r/min of rotating speed, ultrasonic generator power is 100~200W, and coloration time is 2~12h；
After coloring terminates, the differential arc oxidation film layer padding solution of AZ31 magnesium alloy disks is rinsed well with deionized water, then uses
Hair-dryer is dried up, you can obtain AZ31 magnesium alloy disk of the micro-arc oxidation films layer surface in pink or bright yellow.Actually should
In, the staining solution of pink (or bright yellow) by color be BG- pink (or SE-4EL is light yellow) weak acid dye, member it is bright
Powder, neopelex, pH value regulator and deionized water are mixed, and weak acid dye in the staining solution
Content is 1~10g/L, the content of glauber salt and neopelex is that 1~5g/L, the consumption of pH value regulator make institute
The pH value for stating staining solution is adjusted at 20 DEG C between 4.5~5.0.
Further, the utilization weak acid dye provided in the embodiment of the present invention 1 colours for magnesium material differential arc oxidation film layer
Method implementation process in observed as follows：
(1) the AZ31 magnesium obtained using SSX-550 SEM to differential arc oxidation process in the embodiment of the present invention 1
The differential arc oxidation film layer of the presentation white of alloy disk surfaces growth in situ is observed, so as to obtain scanning as shown in Figure 1
Electron micrograph (FESEM images).Electron scanning micrograph shown in Fig. 1 is carried out with operating supply voltage 350V
The AZ31 magnesium alloy disks that the surface in situ processed after the processing of 20min differential arc oxidations grows white differential arc oxidation film layer exist
Amplification 3000 times when pattern, its surface micropore size is between 0.5~5.0 μm.
(2) differential of the arc oxygen that process is obtained is coloured to immersion in the embodiment of the present invention 1 using SSX-550 SEM
Change film surface to be observed in pink AZ31 magnesium alloy disks, so as to obtain SEM as shown in Figure 2
Photo (FESEM images).As seen from Figure 2：Dye particles are largely adsorbed in micro-arc oxidation films layer surface in granular form, and
Show acicular growth.
(3) it is in pink directly to the micro-arc oxidation films layer surface that immersion coloring process is obtained in the embodiment of the present invention 1
AZ31 magnesium alloy disks are observed, so as to obtain the photomacrograph of the differential arc oxidation film layer after immersion coloring as shown in Figure 3
Schematic diagram.As seen from Figure 3：The embodiment of the present invention 1 is successfully to the white micro- of AZ31 magnesium alloy disk surfaces growth in situ
Arc oxidation film layer is coloured, so that differential arc oxidation film layer shows beautiful pink.
(4) it is in bright yellow directly to the micro-arc oxidation films layer surface that immersion coloring process is obtained in the embodiment of the present invention 1
AZ31 magnesium alloy disks are observed, so as to obtain the photomacrograph of the differential arc oxidation film layer after immersion coloring as shown in Figure 4
Schematic diagram.As seen from Figure 4：The embodiment of the present invention 1 is successfully to the white micro- of AZ31 magnesium alloy disk surfaces growth in situ
Arc oxidation film layer is coloured, so that differential arc oxidation film layer shows beautiful bright yellow.
As fully visible, the present invention can not only make magnesium material differential arc oxidation film layer that the beautiful color of various bright-coloured light is presented, and keep
Magnesium material differential arc oxidation film layer itself has the corrosion resistance that magnesium material differential arc oxidation film layer is improved compared with high-bond and wearability, and
And simple production process, easily realize volume production, human body and equipment will not be caused corrosion, do not result in environmental pollution.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art is in the technical scope of present disclosure, the change or replacement that can be readily occurred in,
It should all be included within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Enclose and be defined.
Claims (5)
1. a kind of utilization weak acid dye is the method that magnesium material differential arc oxidation film layer is coloured, including：Utilize differential arc oxidization technique pair
Magnesium material, which carries out surface treatment, makes magnesium material surface in situ grow differential arc oxidation film layer, it is characterised in that also include：Using staining solution
Immersion coloring is carried out to magnesium material surface in situ growth differential arc oxidation film layer；
Wherein, the staining solution is mixed by weak acid dye, dye leveller, pH value regulator and deionized water, and institute
The content for stating weak acid dye in staining solution is 1~10g/L, and dye leveller is glauber salt and neopelex, every kind of
The content of dye leveller is 1~5g/L, and the consumption of pH value regulator makes the pH value of the staining solution be adjusted at 20 DEG C to 4.5
Between~5.0.
2. utilization weak acid dye according to claim 1 is the method that magnesium material differential arc oxidation film layer is coloured, its feature exists
In the soak time of the immersion coloring is 1~12 hour, and the longer color of soak time is deeper.
3. utilization weak acid dye according to claim 1 or 2 is the method that magnesium material differential arc oxidation film layer is coloured, its feature
It is, immersion coloring is carried out to magnesium material surface in situ growth differential arc oxidation film layer using staining solution on coloring apparatus,
And in the immersion coloring process, the agitating device speed of agitator of the coloring apparatus is 500~1000r/min, described
The thermostat temperature of coloring apparatus is 20~40 DEG C, and the ultrasonic generator power of the coloring apparatus is 100~200W.
4. utilization weak acid dye according to claim 1 or 2 is the method that magnesium material differential arc oxidation film layer is coloured, its feature
It is, the magnesium material surface in situ grows differential arc oxidation film layer, its surface micropore size is 0.5~5.0 μm, and its thicknesses of layers is big
In 5 μm.
5. utilization weak acid dye according to claim 1 or 2 is the method that magnesium material differential arc oxidation film layer is coloured, its feature
It is, described weak acid dye is monoazo class dyestuff.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710392538.5A CN107227480A (en) | 2017-05-27 | 2017-05-27 | A kind of utilization weak acid dye is the method that magnesium material differential arc oxidation film layer is coloured |
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| CN201710392538.5A CN107227480A (en) | 2017-05-27 | 2017-05-27 | A kind of utilization weak acid dye is the method that magnesium material differential arc oxidation film layer is coloured |
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| CN101831683A (en) * | 2010-05-28 | 2010-09-15 | 河海大学常州校区 | Coloring method of micro-arc oxidation ceramic layer on surface of magnesium alloy part |
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| CN106086993A (en) * | 2016-07-22 | 2016-11-09 | 中国科学院深圳先进技术研究院 | A kind of magnesium alloy differential arc oxidation electrolyte and magnesium alloy differential arc oxidation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1209151A (en) * | 1996-01-26 | 1999-02-24 | 巴斯福股份公司 | Monoazo dyes contg. fluorosulphonyl group and use thereof |
| EP1793019A2 (en) * | 2005-11-29 | 2007-06-06 | Italfinish S.p.A. | Multivalent electrolytic process for the surface treatment of non ferrous metallic material |
| CN101831683A (en) * | 2010-05-28 | 2010-09-15 | 河海大学常州校区 | Coloring method of micro-arc oxidation ceramic layer on surface of magnesium alloy part |
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