CN106521602A - Preparing method of magnesium alloy surface composite ceramic film layer - Google Patents
Preparing method of magnesium alloy surface composite ceramic film layer Download PDFInfo
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- CN106521602A CN106521602A CN201610941010.4A CN201610941010A CN106521602A CN 106521602 A CN106521602 A CN 106521602A CN 201610941010 A CN201610941010 A CN 201610941010A CN 106521602 A CN106521602 A CN 106521602A
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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
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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
- C25D11/024—Anodisation under pulsed or modulated current or potential
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Abstract
The invention discloses a preparing method of a magnesium alloy surface composite ceramic film layer. The method is characterized by comprising the following steps: firstly, preparing of oxidation electrolytes; secondly, preparing of leaching solutions; thirdly, oxidizing, wherein a magnesium alloy workpiece serves as an anode, a stainless steel plate serves as a cathode, the oxidation electrolytes in the first step serve as electrolytes, the pulse current is adopted to carry out oxidation, and compression air is adopted for stirring; fourthly, vacuum leaching, wherein the oxidized magnesium alloy is subject to vacuum leaching through the leaching solutions in the second step. Compared with the prior art, the method has the beneficial effects that due to adding of graphene, conducting treatment of the magnesium alloy surface ceramic coating is achieved, the problems that a magnesium alloy oxidization ceramic film layer is loose, porous, poor in corrosion resistance and free of conducting are solved, the conducting performance of the ceramic film layer is improved to a certain degree, and meanwhile the ceramic texture of the oxidization film layer is not affected.
Description
Technical field
A kind of a kind of the present invention relates to metal surface treating method, more particularly to processing method of Mg alloy surface.
Background technology
Magnesium alloy be the minimum structural metallic materials of engineer applied Midst density (its density is the 1/4 of iron and steel, the 2/ of aluminium alloy
3), there is specific strength height, good thermal conductivity, damping shock absorption, be electromagnetically shielded, be easy to machining and easily reclaim,
" green engineering material of 21 century " and " most promising lightweighting materials " is described as, in traffic, electronic communication, space flight and aviation
Wide application prospect is respectively provided with the industrial circle such as defence and military.
But due to the chemical property of magnesium it is more active, although layer oxide film can be formed in natural environment lower surface, but
Due to the oxide-film of self-assembling formation it is not fine and close, it is impossible to play a part of protect the substrate, therefore, magnesium alloy is anti-corrosion in natural environment
Property is poor, this greatly limits popularization and application of the magnesium alloy in all trades and professions.The corrosion resisting property of magnesium alloy to be improved, can be with
Realize by way of alloying and surfacecti proteon are processed, it is most economical, most effective method that wherein surfacecti proteon is processed.
Conventional magnesium alloy surface protective processing method has chemical oxidation, chemical plating, plating, jet deposition, japanning and differential arc oxidation etc.,
Wherein differential arc oxidization technique is due to simple to operate, being affected less, oxide layer corrosion resistance high by component structural and size
One of feature, therefore become the most promising surface treatment method of solution Research on Corrosion of Magnesium Alloys.
As the oxide layer obtained using differential arc oxidization technique has porous, Shandong is rushed et al. once using the method being co-deposited
By MoS2Particle is introduced in oxide layer hole, substantially increases the anti-wear performance of oxide layer.(see《Arms Material scientific and engineering》
MoS2Impact to the oxidation of aluminium alloy shadow matter oxidizing anode, author：Lu Chuan, Zhu Liping, He Yong etc., 2012 years second time of disclosure
Phase)
But when being surface-treated to magnesium alloy using differential arc oxidization technique due to formed be ceramic film, magnesium can be made
Alloy surface becomes non-conductive.But with the increase of magnesium alloy application amount in terms of electronic housings, exploitation can improve magnesium alloy
The corrosion resisting property of housing can guarantee that the surface protection technique of the electric conductivity for significantly reducing magnesium alloy shell becomes urgent need to resolve again
Problem.
The content of the invention
The technical problem to be solved be for the above-mentioned state of the art and provide it is a kind of have ceramic texture and
The preparation method of the Mg alloy surface composite ceramicses film layer with conducting function.
The present invention solve the technical scheme that adopted of above-mentioned technical problem for：A kind of Mg alloy surface composite ceramicses film layer
Preparation method, it is characterised in that comprise the steps：
1. the preparation of oxidation electrolyte：
First dodecylbenzene sodium sulfonate is added in deionized water and is dissolved, graphene powder is added into above-mentioned solution then
In, then ultrasonic disperse sequentially adds phosphoric acid, ammonia and triethanolamine；
2. the preparation of infiltration liquid：
The graphene powder of 3～10g/L is added in inorganic silicon infiltration liquid, Graphene is realized by churned mechanically mode
Dispersion of the powder in inorganic silicon infiltration liquid；
3. be electrolysed, with magnesium alloy workpiece as anode, corrosion resistant plate is negative electrode, using step 1. in oxidation electrolyte as electricity
Solution liquid, is aoxidized using pulse current, is stirred using compressed air；
4. vacuum infiltration；To the magnesium alloy workpiece after oxidation using step 2. in the liquid that is impregnated with carry out vacuum infiltration.
Preferably, step 2. described in mechanical agitation it is as follows：Churned mechanically speed be 100～200 turns/
Point, diluent adopts Polyethylene Glycol.
Preferably, step 3. described in electrolytic condition it is as follows：Stirring 50～200Hz of pulse current frequency, dutycycle
10%～80%, oxidate current is 0.5～2A/dm2, oxidization time 10～20 minutes.
Preferably, step 4. described in vacuum infiltration condition it is as follows：Magnesium alloy workpiece is vacantly placed in and fills infiltration
In the Dewar vessel of liquid, to container vacuum-pumping, when the vacuum in container reaches -0.1bar, then by magnesium alloy workpiece submergence
In infiltration liquid, open gas bleeder valve by container return normal barometric pressure, then again repeatedly evacuation, lose heart 3 times, finally open lose heart
Valve, after making the air pressure in Dewar vessel return to normal barometric pressure, takes out magnesium alloy workpiece.
Graphene is due to superpower electric conductivity, the intensity of superelevation, better than the heat conductivility and super large of CNT
The excellent properties such as specific surface area, have broad application prospects the aspects such as conduction, the heat conductivility of material are improved.There is research table
Bright Graphene is added in organic polymer makes composite, can greatly improve the electric conductivity of composite.Therefore,
The present invention considers by Graphene is introduced in oxide layer to improve the electric conductivity of differential arc oxidation layer.
Differential arc oxidation layer is in the presence of high voltage to grow the ceramics to be formed in the light-alloy surface in situ such as aluminum, magnesium, titanium
Film layer, based on metal-oxide, with porous.Using the porous of differential arc oxidation layer, Graphene can be introduced and be aoxidized
In layer.The present invention is introduced into Graphene in oxide layer using two kinds of approach, and one is to add Graphene in microarc oxidation solution, is made
Graphene adsorbs in the hole of oxide layer with the carrying out of oxidizing process；Two is, by graphene dispersion in infiltration liquid, to adopt
Vacuum infiltration technique carries out infiltration process to differential arc oxidation layer, so that Graphene is entered in the hole of differential arc oxidation layer, improves
The content of Graphene in oxide layer.
Compared with prior art, it is an advantage of the current invention that：Being made up of two parts prepared by the present invention, a part are to contain
The differential arc oxidation layer of Graphene, used as bottom, wherein Graphene content reaches more than 20% (at.).Another part is graphitiferous
The inorganic silicon Infiltration layer of alkene, as top layer, due to adding Graphene, realizes at the conducting of Mg alloy surface ceramic coating
Reason, it is loose porous to solve magnesium alloy oxide ceramic film layer, and corrosion resistance is poor and nonconducting problem, improves pottery to a certain extent
The electric conductivity of porcelain film layer, while the ceramic texture of oxidation film layer is not affected, in terms of the surfacecti proteon of magnesium alloy electronic housing
With larger application prospect.The surface conductanceization that can be used for all kinds of magnesium alloy shells is processed.
Description of the drawings
Fig. 1 is the surface topography of the magnesium alloy differential arc oxidation film layer of the graphene-containing prepared using embodiment 1.
Fig. 2 is the microphotograph of the magnesium alloy differential arc oxidation film layer of the graphene-containing prepared using embodiment 1.
Power spectrums of the Fig. 3 for magnesium alloy differential arc oxidation film layer in square frame in Fig. 2.
Fig. 4 is the Raman spectrum of the composite ceramicses film layer of the Mg alloy surface graphene-containing prepared using embodiment 1.
Specific embodiment
The present invention is described in further detail below in conjunction with accompanying drawing embodiment.
Embodiment 1, with reference to shown in Fig. 1～Fig. 4, using phosphoric acid 25g/L, ammonia 120g/L, triethanolamine 65g/L, graphite
Alkene dispersion 10g/L, dodecylbenzene sodium sulfonate 3g/L are aoxidized to AZ80 magnesium alloys, the preparation of oxidation electrolyte：First will
Dodecylbenzene sodium sulfonate is dissolved in adding appropriate amount of deionized water, is then added graphene dispersion body in above-mentioned solution, ultrasound
Dispersion 20 minutes, then sequentially adds phosphoric acid, ammonia and triethanolamine.
Specimen size is 40mm × 50mm × 4mm, in 10% (W/W) HNO after upper extension3Soak 0.5 minute in solution, take out
Rinsed well with circulating water, then hung over sample dress on the anode rod in oxidation trough, it is ensured that hanger and anode rod contact are good,
And sample is fully immersed in oxidation solution.Aoxidized using pulse current, pulse current frequency 50Hz, dutycycle 50%, oxygen
Galvanic current density is 1A/dm2, oxidization time 20 minutes, oxidation take out workpiece after terminating, are rinsed with circulating water, then hot at 60 DEG C
Soak 5 minutes in water, taking-up is dried；Vacuum infiltration is carried out, infiltration liquid is consisted of：The graphene powder of 3g/L is added into inorganic silicon
In infiltration liquid, stirred 20 minutes using 100 revs/min of speed mechanicals.Vacuum infiltration method is：Workpiece is vacantly placed in and is filled
State in the Dewar vessel of infiltration liquid, using air-extractor to container vacuum-pumping, when the vacuum in container reaches -0.1bar,
Again workpiece is immersed in infiltration liquid, open gas bleeder valve by container return normal barometric pressure, then again repeatedly evacuation, lose heart 3 times,
So that infiltration liquid is entered in the hole of oxide layer, gas bleeder valve is finally opened, makes the air pressure in Dewar vessel return to normal barometric pressure
Afterwards, workpiece is taken out, is placed in after drying in 180 DEG C of baking ovens and toasts 10 minutes, then natural cooling, that is, be obtained the graphitiferous of the present invention
The composite ceramicses film layer of alkene.
With reference to shown in Fig. 1～Fig. 4, about 40 microns of the thickness of the composite film of preparation, the thickness of wherein oxide layer is about
25 microns, about 15 microns of Infiltration layer thickness, in oxide layer, the content of Graphene is more than 20%, and composite ceramicses film layer is conductive.
In Fig. 3, concrete composition ratio is as follows：
Embodiment 2, using phosphoric acid 35g/L, ammonia 135g/L, triethanolamine 75g/L, graphene dispersion body 15g/L, 12
Sodium alkyl benzene sulfonate 4g/L is aoxidized to AZ61 magnesium alloys, the preparation of oxidation electrolyte：First dodecylbenzene sodium sulfonate is added
Enter in appropriate amount of deionized water and dissolve, then add graphene dispersion body in above-mentioned solution, ultrasonic disperse 20 minutes, then again according to
Secondary addition phosphoric acid, ammonia and triethanolamine.
Specimen size is 40mm × 50mm × 4mm, in 10% (W/W) HNO after upper extension3Soak 0.5 minute in solution, take out
Rinsed well with circulating water, then hung over sample dress on the anode rod in oxidation trough, it is ensured that hanger and anode rod contact are good,
And sample is fully immersed in oxidation solution.Aoxidized using pulse current, pulse current frequency 100Hz, dutycycle 60%, oxygen
Galvanic current density is 2A/dm2, oxidization time 15 minutes, oxidation take out workpiece after terminating, are rinsed with circulating water, then hot at 60 DEG C
Soak 5 minutes in water, taking-up is dried；Vacuum infiltration is carried out, infiltration liquid is consisted of：The graphene powder of 8g/L is added into inorganic silicon
In infiltration liquid, stirred 30 minutes using 100 revs/min of speed mechanicals, diluted using the Polyethylene Glycol of 50mL/L.Vacuum infiltration side
Method is：Workpiece is vacantly placed in the Dewar vessel for filling above-mentioned infiltration liquid, using air-extractor to container vacuum-pumping, works as container
In vacuum when reaching -0.1bar, then workpiece is immersed in infiltration liquid, opens gas bleeder valve and return normal barometric pressure by container,
Then again repeatedly evacuation, lose heart 3 times so that infiltration liquid enter oxide layer hole in, finally open gas bleeder valve, hold vacuum
After air pressure in device returns to normal barometric pressure, workpiece is taken out, be placed in after drying in 180 DEG C of baking ovens and toast 10 minutes, it is then natural
Cooling, that is, be obtained the composite ceramicses film layer of the graphene-containing of the present invention.
About 50 microns of the thickness of the composite film of preparation, wherein about 30 microns of the thickness of oxide layer, Infiltration layer thickness
About 20 microns, in oxide layer, the content of Graphene is more than 20%, and composite ceramicses film layer is conductive.
Embodiment 3, using phosphatase 24 5g/L, ammonia 150g/L, triethanolamine 80g/L, graphene dispersion body 20g/L, 12
Sodium alkyl benzene sulfonate 5g/L is aoxidized to AZ31 magnesium alloys, the preparation of oxidation electrolyte：First dodecylbenzene sodium sulfonate is added
Enter in appropriate amount of deionized water and dissolve, then add graphene dispersion body in above-mentioned solution, ultrasonic disperse 20 minutes, then again according to
Secondary addition phosphoric acid, ammonia and triethanolamine.
Specimen size is 40mm × 50mm × 4mm, in 10% (W/W) HNO after upper extension3Soak 0.5 minute in solution, take out
Rinsed well with circulating water, then hung over sample dress on the anode rod in oxidation trough, it is ensured that hanger and anode rod contact are good,
And sample is fully immersed in oxidation solution.Aoxidized using pulse current, pulse current frequency 50Hz, dutycycle 70%, oxygen
Galvanic current density is 2A/dm2, oxidization time 15 minutes, oxidation take out workpiece after terminating, are rinsed with circulating water, then hot at 60 DEG C
Soak 5 minutes in water, taking-up is dried；Vacuum infiltration is carried out, infiltration liquid is consisted of：The graphene powder of 10g/L is added inorganic
In silicon infiltration liquid, stirred 30 minutes using 100 revs/min of speed mechanicals, diluted using the Polyethylene Glycol of 60mL/L.Vacuum infiltration
Method is：Workpiece is vacantly placed in the Dewar vessel for filling above-mentioned infiltration liquid, using air-extractor to container vacuum-pumping, works as appearance
When vacuum in device reaches -0.1bar, then workpiece is immersed in infiltration liquid, open gas bleeder valve and normal gas is returned by container
Pressure, then again repeatedly evacuation, lose heart 3 times so that infiltration liquid is entered in the hole of oxide layer, finally open gas bleeder valve, make true
After air pressure in empty returns to normal barometric pressure, workpiece is taken out, be placed in baking 10 minutes in 180 DEG C of baking ovens after drying, then
Natural cooling, that is, be obtained the composite ceramicses film layer of the graphene-containing of the present invention.
About 55 microns of the thickness of the composite film of preparation, wherein about 35 microns of the thickness of oxide layer, Infiltration layer thickness
About 20 microns, in oxide layer, the content of Graphene is more than 20%, and composite ceramicses film layer is conductive.
Claims (5)
1. a kind of preparation method of Mg alloy surface composite ceramicses film layer, it is characterised in that comprise the steps：
1. the preparation of oxidation electrolyte：
First dodecylbenzene sodium sulfonate is added in deionized water and is dissolved, then graphene powder is added in above-mentioned solution,
Ultrasonic disperse 30min, then sequentially adds phosphoric acid, ammonia and triethanolamine；
2. the preparation of infiltration liquid：
The graphene powder of 3～10g/L is added in inorganic silicon infiltration liquid, graphene powder is realized by churned mechanically mode
Dispersion in inorganic silicon infiltration liquid；
3. aoxidize：With magnesium alloy workpiece as anode, corrosion resistant plate is negative electrode, using step 1. in oxidation electrolyte as electrolysis
Liquid, is aoxidized using pulse current, is stirred using compressed air；
4. vacuum infiltration：To the magnesium alloy workpiece after oxidation using step 2. in the liquid that is impregnated with carry out vacuum infiltration.
2. preparation method according to claim 1, it is characterised in that step 2. described in mechanical agitation it is as follows：Machine
The speed of tool stirring is 100～200 revs/min, and diluent adopts Polyethylene Glycol.
3. preparation method according to claim 1, it is characterised in that step 3. described in oxidizing condition it is as follows：Stirring arteries and veins
50～200Hz of power frequency, dutycycle 10%～80% is rushed, oxidate current is 0.5～2A/dm2, oxidization time 10～20
Minute.
4. preparation method according to claim 1, it is characterised in that step 4. described in vacuum infiltration condition it is as follows：Will
Magnesium alloy workpiece is vacantly placed in the Dewar vessel for filling infiltration liquid, to container vacuum-pumping, reach when the vacuum in container-
During 0.1bar, then magnesium alloy workpiece is immersed in infiltration liquid, open gas bleeder valve and normal barometric pressure is returned by container, then again repeatedly
Evacuation, lose heart 3 times, finally open gas bleeder valve, after making the air pressure in Dewar vessel return to normal barometric pressure, take out magnesium alloy work
Part.
5. preparation method according to claim 1, it is characterised in that step 2. described in inorganic silicon infiltration liquid by such as
It is prepared by lower section method：10～100nm Nano-meter SiO_2s2It is obtained in being scattered in ethylene glycol, Nano-meter SiO_22Mass ratio with ethylene glycol is 10%
～30%.
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Cited By (2)
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| CN112064037A (en) * | 2020-10-13 | 2020-12-11 | 贵州电网有限责任公司 | Preparation method of corrosion-resistant magnesium alloy sacrificial anode |
| CN112251790A (en) * | 2020-10-22 | 2021-01-22 | 中国船舶重工集团公司第七二五研究所 | Preparation method of rare earth magnesium alloy structural member surface composite film layer |
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