CN105350049B - A kind of preparation method of Mg alloy surface graphene oxide composite coating - Google Patents
A kind of preparation method of Mg alloy surface graphene oxide composite coating Download PDFInfo
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- CN105350049B CN105350049B CN201510817357.3A CN201510817357A CN105350049B CN 105350049 B CN105350049 B CN 105350049B CN 201510817357 A CN201510817357 A CN 201510817357A CN 105350049 B CN105350049 B CN 105350049B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 45
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 32
- 239000011248 coating agent Substances 0.000 title claims abstract description 23
- 238000000576 coating method Methods 0.000 title claims abstract description 23
- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000004070 electrodeposition Methods 0.000 claims abstract description 9
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 6
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims abstract description 5
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 5
- 239000007864 aqueous solution Substances 0.000 claims abstract description 4
- 238000000970 chrono-amperometry Methods 0.000 claims abstract description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 16
- 239000010439 graphite Substances 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000005238 degreasing Methods 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 6
- 239000001488 sodium phosphate Substances 0.000 claims description 6
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 6
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 239000003921 oil Substances 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- 238000005868 electrolysis reaction Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 230000007797 corrosion Effects 0.000 abstract description 10
- 238000005260 corrosion Methods 0.000 abstract description 10
- 239000003792 electrolyte Substances 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical class S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- OQVYMXCRDHDTTH-UHFFFAOYSA-N 4-(diethoxyphosphorylmethyl)-2-[4-(diethoxyphosphorylmethyl)pyridin-2-yl]pyridine Chemical compound CCOP(=O)(OCC)CC1=CC=NC(C=2N=CC=C(CP(=O)(OCC)OCC)C=2)=C1 OQVYMXCRDHDTTH-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 241000238370 Sepia Species 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
- C25D9/08—Electrolytic coating other than with metals with inorganic materials by cathodic processes
- C25D9/12—Electrolytic coating other than with metals with inorganic materials by cathodic processes on light metals
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/18—Electroplating using modulated, pulsed or reversing current
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Treatment Of Metals (AREA)
- Carbon And Carbon Compounds (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
Abstract
The invention discloses a kind of preparation method of Mg alloy surface graphene oxide composite coating.First, magnesium alloy substrate is pre-processed；Then, graphene oxide is prepared, is dissolved in 1 ~ 5 ml/L triethanolamine aqueous solution, carries out electrolyte of the ultrasonic disperse after 2 hours as electro-deposition；Afterwards, using CHI860D type electrochemical workstations, three-electrode system is assembled, pretreated magnesium alloy is Electrode, and platinum electrode is auxiliary electrode, and saturated calomel electrode is reference electrode, selects chronoamperometry to carry out electrochemical deposition to magnesium alloy；Finally, take out magnesium alloy to dry 1 ~ 2 hour at 60 ~ 70 DEG C, obtain Mg alloy surface graphene oxide composite coating.Method of the invention composite coating surface uniform ground simple to operate, prepared, there are the typical pleated structure of graphene oxide, and have relatively low corrosion electric current density and higher electrochemical impedance, can be good at improving the corrosion resistance of magnesium alloy.
Description
Technical field
The invention belongs to metal material surface electrochemical corrosion and protection field, more particularly to a kind of Mg alloy surface oxidation
The preparation method of graphene composite coating.
Background technology
Magnesium alloy is described as " 21 century green engineering metal structure as a kind of very important light metal structure material
Material ".Magnesium alloy has the irreplaceable property of many other materials, such as in light weight, has good castability and chi
Very little stability, very strong reproducibility etc., these performances make magnesium alloy be widely used in metallurgy, aviation, military affairs, electronics, automobile
The fields such as industry, electrode material.But the reason for restricting magnesium alloy practical application development most critical is that magnesium alloy has relatively negative electricity
Electrode potential, easily it is corroded in different complex environments.Graphene oxide possesses the physics of many protrusions, chemical property, tool
There are more prominent aspect ratio and extremely strong barrier property, path of the corrosive medium by matrix can be greatly prolonged, these property
Graphene oxide can be enabled preferably to improve the decay resistance of substrate.Therefore, graphene oxide is a kind of anticorrosion
The new material of excellent performance, application prospect are extensive.But graphene oxide membrane be used for some common metals such as copper, steel and
Alloy, it is less to apply to magnesium alloy.Graphene oxide is innovatively applied to magnesium alloy by the present invention, and combines the side of electro-deposition
Method, triethanolamine/graphene oxide composite coating is prepared in Mg alloy surface, the decay resistance of magnesium alloy is improved, widens magnesium
The practical application area of alloy.
The content of the invention
It is an object of the invention to provide a kind of preparation method of Mg alloy surface graphene oxide composite coating.
Concretely comprise the following steps：
(1) pretreatment of magnesium alloy
Magnesium alloy is polished step by step with the resistance to silicon carbide papers of 600# and 1200# successively, polishes, wash, then in alkaline degreasing
Oil removing 0.5 ~ 2 minute at 60 ~ 80 DEG C in liquid, then through washing, then in absolute ethyl alcohol ultrasonic wave clean 5 ~ 15 minutes, go from
Sub- water ultrasonic wave cleans 2 ~ 3 times, and cold wind drying is standby；The alkaline degreasing formula of liquid is：The g/L of sodium phosphate 20 ~ 30, hydroxide
The g/L of sodium 15 ~ 25, the g/L of sodium carbonate 30 ~ 40.
(2) preparation of graphene oxide
Graphite oxide is prepared by improved Hummers methods, by dilute salt that the graphite oxide percent by volume of preparation is 3%
Acid solution fully washs, then it is neutrality to be washed with deionized water to pH value, and graphite oxide is put into ultrasound stripping in deionized water is
Graphene oxide, then gained graphene oxide suspension is carried out at centrifugation in the centrifuge that rotating speed is 1000 revs/min
Reason, the graphite oxide that lower floor is not completely exfoliated is removed, repeats and carries out centrifugal treating once, obtain supernatant liquor, it is freeze-dried
Graphene oxide powder is obtained after processing.
(3) prepared by composite coating
Using CHI860D type electrochemical workstations, three-electrode system is assembled, is through step (1) pretreated magnesium alloy
Electrode, platinum electrode are auxiliary electrode, and saturated calomel electrode is reference electrode, the graphene oxide that will be prepared through step (2)
The mg of powder 10 ~ 30 is dissolved in 20 ml 1 ~ 5 ml/L triethanolamine aqueous solution, carries out ultrasonic disperse conduct after 2 hours
Electrolyte；Chronoamperometry is selected to carry out electrochemical deposition to magnesium alloy, parameter is arranged to：High potential is -0.90 volt, low potential
For -1.70 volts, step number 10 times, pulse width 100 seconds；Magnesium alloy is taken out after electrochemical deposition to dry at 60 ~ 70 DEG C
1 ~ 2 hour, that is, Mg alloy surface graphene oxide composite coating is made.
The sodium phosphate, sodium hydroxide, sodium carbonate, absolute ethyl alcohol, hydrochloric acid, graphite and triethanolamine be chemistry it is pure and with
Upper purity.
Method of the invention composite coating surface uniform ground simple to operate, prepared, there are graphene oxide allusion quotation
The pleated structure of type, and there is relatively low corrosion electric current density and higher electrochemical impedance, it can be good at improving magnesium alloy
Corrosion resistance, can obtain compound protective coating uniform, that corrosion resistance is high for Mg alloy surface processing.
Brief description of the drawings
Fig. 1 is the SEM figures of Mg alloy surface graphene oxide composite coating prepared by the embodiment of the present invention.
Embodiment
Embodiment：
(1) pretreatment of magnesium alloy
AZ91 magnesium alloys are polished step by step with the resistance to silicon carbide papers of 600# and 1200# successively, polishes, wash, then in alkalescence
Oil removing 1 minute at 60 DEG C in degreasing fluid, reusable heat water and cold water are respectively washed specimen surface, then ultrasonic in absolute ethyl alcohol
Ripple cleans 10 minutes, and deionized water ultrasonic wave cleans 3 times, and cold wind drying is standby；The alkaline degreasing formula of liquid is：Sodium phosphate 20
G/L, the g/L of sodium hydroxide 20, the g/L of sodium carbonate 30.
(2) preparation of graphene oxide
Graphite oxide is prepared by improved Hummers methods, first cools down the 120 ml concentrated sulfuric acids with ice-water bath, under stirring condition,
5 g graphite powders are slowly added in batches, and after question response thing is mixed thoroughly, system is black；It is high to be slowly added to 15 g in batches again
Potassium manganate, now solution is blackish green to react 1 hour.Reacted 2 hours in 40 DEG C of tepidarium afterwards, obtain product as palm fibre
Brown batter shape.Product is moved on into 98 DEG C of waters bath with thermostatic control again persistently to stir 10 minutes, and 330 ml deionized waters are slowly added dropwise,
Product is sepia.Hydrogen peroxide to bubble-free is added dropwise in product to emerge, coloured product is changed into glassy yellow.Filter, will prepare while hot
Graphite oxide with percent by volume be 3% dilute hydrochloric acid solution fully wash, then be washed with deionized water to pH value for neutrality, will
It is graphene oxide that graphite oxide, which is put into ultrasound stripping in deionized water,.It is in rotating speed by gained graphene oxide suspension then
Centrifugal treating is carried out in 1000 revs/min of centrifuge, the graphite oxide that lower floor is not completely exfoliated is removed, repeats and centrifuged
Processing once, obtains supernatant liquor, and graphene oxide powder is obtained after freeze-dried processing.
(3) prepared by composite coating
Using CHI860D type electrochemical workstations, three-electrode system is assembled, is through step (1) pretreated magnesium alloy
Electrode, platinum electrode are auxiliary electrode, and saturated calomel electrode is reference electrode, the graphene oxide that will be prepared through step (2)
The mg of powder 20 is dissolved in the 20 mL 3 ml/L triethanolamine aqueous solution, carries out ultrasonic disperse after 2 hours as electrolysis
Liquid.Chronoamperometry is selected to carry out electrochemical deposition to magnesium alloy, parameter is arranged to：High potential is -0.90 volt, low potential for -
1.70 volts, step number 10 times, pulse width 100 seconds.Magnesium alloy is taken out after electrochemical deposition to dry 1 hour at 60 DEG C,
Obtain Mg alloy surface graphene oxide composite coating.
The sodium phosphate, sodium hydroxide, sodium carbonate, absolute ethyl alcohol, sulfuric acid, potassium permanganate, hydrogen peroxide, hydrochloric acid, graphite and
Triethanolamine is that chemistry is pure.
Composite coating made from the present embodiment shows that whole coating uniform is smooth by SEM, has pleated structure,
Surface does not have open defect.Show the characteristic peak of graphene oxide in spectrogram be present by XRD.
Electrochemistry corrosion resisting property test is carried out to composite coating made from the present embodiment, using three-electrode system（With multiple
The magnesium alloy sample for closing coating is Electrode, and platinum electrode is auxiliary electrode, and saturated calomel electrode is reference electrode）, corrosion Jie
Matter is the NaCl solution that mass percent concentration is 3.5%.The corrosion electric current density for the composite coating that the present embodiment is obtained is
1.104×10-6 A/cm2, than the corrosion electric current density 1.951 × 10 of blank AZ91 magnesium alloys-5 A/cm2, reduce a quantity
Level, the electrochemical impedance of composite coating reach 1.010 × 104 Ω·cm2, than the electrochemical impedance of blank AZ91 magnesium alloys
5.750×102 Ω·cm2, increase two orders of magnitude, it will be apparent that improve the corrosion resisting property of magnesium alloy.
Claims (1)
1. a kind of preparation method of Mg alloy surface graphene oxide composite coating, it is characterised in that concretely comprise the following steps：
(1) pretreatment of magnesium alloy
Magnesium alloy is polished step by step with the resistance to silicon carbide papers of 600# and 1200# successively, polishes, wash, then in alkaline degreasing liquid
Oil removing 0.5 ~ 2 minute at 60 ~ 80 DEG C, then through washing, then ultrasonic wave cleans 5 ~ 15 minutes in absolute ethyl alcohol, deionized water
Ultrasonic wave cleans 2 ~ 3 times, and cold wind drying is standby；The alkaline degreasing formula of liquid is：The g/L of sodium phosphate 20 ~ 30, sodium hydroxide 15 ~
25 g/L, the g/L of sodium carbonate 30 ~ 40；
(2) preparation of graphene oxide
Graphite oxide is prepared by improved Hummers methods, and the graphite oxide percent by volume of preparation is molten for 3% watery hydrochloric acid
Liquid fully washs, then it is neutrality to be washed with deionized water to pH value, and graphite oxide is put into ultrasound in deionized water peels off as oxidation
Graphene, gained graphene oxide suspension is then subjected to centrifugal treating in the centrifuge that rotating speed is 1000 revs/min,
The graphite oxide that lower floor is not completely exfoliated is removed, repeats and carries out centrifugal treating once, obtain supernatant liquor, freeze-dried processing
Graphene oxide powder is obtained afterwards；
(3) prepared by composite coating
Using CHI860D type electrochemical workstations, three-electrode system is assembled, is research through step (1) pretreated magnesium alloy
Electrode, platinum electrode are auxiliary electrode, and saturated calomel electrode is reference electrode, the graphene oxide powder that will be prepared through step (2)
10 ~ 30 mg are dissolved in 20 mL 1 ~ 5 mL/L triethanolamine aqueous solution, carry out ultrasonic disperse after 2 hours as electrolysis
Liquid；Chronoamperometry is selected to carry out electrochemical deposition to magnesium alloy, parameter is arranged to：High potential is -0.90 volt, low potential for -
1.70 volts, step number 10 times, pulse width 100 seconds；Magnesium alloy is taken out after electrochemical deposition 1 ~ 2 is dried at 60 ~ 70 DEG C
Hour, that is, Mg alloy surface graphene oxide composite coating is made；
The sodium phosphate, sodium hydroxide, sodium carbonate, absolute ethyl alcohol, hydrochloric acid, graphite and triethanolamine are that chemistry is pure and pure above
Degree.
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| CN109355689A (en) * | 2018-12-11 | 2019-02-19 | 山东工商学院 | The method and its application of super-hydrophobic coat are prepared based on electrodeposition process |
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Application publication date: 20160224 Assignee: Guilin Changlong Machinery Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2023980044422 Denomination of invention: A preparation method of graphene oxide composite coating on magnesium alloy surface Granted publication date: 20171212 License type: Common License Record date: 20231026 Application publication date: 20160224 Assignee: Guilin Xinglong Metal Products Processing Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2023980044396 Denomination of invention: A preparation method of graphene oxide composite coating on magnesium alloy surface Granted publication date: 20171212 License type: Common License Record date: 20231027 |
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