CN106011959A - Electrolytic preparation method for nano reticular nickel-copper alloy through eutectic ionic liquid - Google Patents
Electrolytic preparation method for nano reticular nickel-copper alloy through eutectic ionic liquid Download PDFInfo
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- CN106011959A CN106011959A CN201610490451.7A CN201610490451A CN106011959A CN 106011959 A CN106011959 A CN 106011959A CN 201610490451 A CN201610490451 A CN 201610490451A CN 106011959 A CN106011959 A CN 106011959A
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- 230000005496 eutectics Effects 0.000 title claims abstract description 57
- 239000002608 ionic liquid Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 229910000881 Cu alloy Inorganic materials 0.000 title abstract description 5
- YOCUPQPZWBBYIX-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Cu] YOCUPQPZWBBYIX-UHFFFAOYSA-N 0.000 title abstract 4
- 238000000034 method Methods 0.000 claims abstract description 52
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 44
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910052802 copper Inorganic materials 0.000 claims abstract description 42
- 239000010949 copper Substances 0.000 claims abstract description 42
- 239000003792 electrolyte Substances 0.000 claims abstract description 40
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 22
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 22
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000011159 matrix material Substances 0.000 claims abstract description 20
- 230000008021 deposition Effects 0.000 claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 12
- 239000010439 graphite Substances 0.000 claims abstract description 12
- 150000002815 nickel Chemical class 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 32
- 229910000792 Monel Inorganic materials 0.000 claims description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 20
- 239000010409 thin film Substances 0.000 claims description 20
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- 239000002131 composite material Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 229910000831 Steel Inorganic materials 0.000 claims description 13
- 239000010959 steel Substances 0.000 claims description 13
- 238000011010 flushing procedure Methods 0.000 claims description 10
- 229910052759 nickel Inorganic materials 0.000 claims description 10
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 claims description 9
- 235000019743 Choline chloride Nutrition 0.000 claims description 9
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 claims description 9
- 229960003178 choline chloride Drugs 0.000 claims description 9
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 8
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 5
- 150000001298 alcohols Chemical class 0.000 claims description 4
- 150000001408 amides Chemical class 0.000 claims description 4
- 235000013877 carbamide Nutrition 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 4
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 4
- OKIZCWYLBDKLSU-UHFFFAOYSA-M N,N,N-Trimethylmethanaminium chloride Chemical compound [Cl-].C[N+](C)(C)C OKIZCWYLBDKLSU-UHFFFAOYSA-M 0.000 claims description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims 1
- MPTQRFCYZCXJFQ-UHFFFAOYSA-L copper(II) chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Cu+2] MPTQRFCYZCXJFQ-UHFFFAOYSA-L 0.000 abstract description 11
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 8
- 239000010935 stainless steel Substances 0.000 abstract description 5
- 229910001220 stainless steel Inorganic materials 0.000 abstract description 5
- 239000000956 alloy Substances 0.000 abstract description 3
- 239000002243 precursor Substances 0.000 abstract 3
- 150000001879 copper Chemical class 0.000 abstract 1
- 238000000151 deposition Methods 0.000 description 12
- 238000004062 sedimentation Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000004070 electrodeposition Methods 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000002738 chelating agent Substances 0.000 description 2
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 229910000570 Cupronickel Inorganic materials 0.000 description 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-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
- 238000003723 Smelting Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- BNBLBRISEAQIHU-UHFFFAOYSA-N disodium dioxido(dioxo)manganese Chemical compound [Na+].[Na+].[O-][Mn]([O-])(=O)=O BNBLBRISEAQIHU-UHFFFAOYSA-N 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000005363 electrowinning Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000374 eutectic mixture Substances 0.000 description 1
- 239000001257 hydrogen Chemical group 0.000 description 1
- 229910052739 hydrogen Chemical group 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 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
- C25D3/00—Electroplating: Baths therefor
- C25D3/66—Electroplating: Baths therefor from melts
- C25D3/665—Electroplating: Baths therefor from melts from ionic liquids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention relates to an electrolytic preparation method for a nano reticular nickel-copper alloy through an eutectic ionic liquid, and belongs to the technical field of material preparation. The method comprises the steps of firstly, adding a nickel salt precursor and a copper salt precursor into the eutectic ionic liquid, and adopting the mixture as an electrolyte; and carrying out electrolysis at the temperature of 100 DEG C or below to prepare a nano reticular nickel-copper alloy film on a working electrode through adopting a three-electrode system, with a platinum electrode or graphite adopted as an electrolytic anode, a silver wire electrode adopted as a reference electrode, and copper or stainless steel adopted as the working electrode. According to the method, nickel chloride hexahydrate and copper chloride dihydrate are adopted as precursors, flakelike pure copper is adopted as a deposition matrix, a nano reticular nickel-copper alloy material is prepared through an electrolytic method, and the method has the advantages of being controllable and moderate to implement, low in cost, and the like.
Description
Technical field
A kind of method that the present invention relates to eutectic type ionic liquid electrolytic preparation mesh nanometer monel, belongs to technical field of material.
Background technology
Alloy synthetic technology increasingly arouses people's interest, especially corronil has many excellent performances such as: the alluvial of anti-corrosive properties, antibiont, electrocatalysis, wearability, magnetic, optical, be used for prepare the performances such as nano material, to corronil Study of synthesis method more and more deep.Owing to quickly increasing the demand of material, the new method of corronil is prepared in research and development, it will have more far-reaching practical significance and wider array of using value.
In recent years, the polyol reduction method of corronil, copper sulfate method are prepared, impulse method, electrodeposition process, physics smelting technology, prepared by Mechanical Method, ultrasonic method etc., it is high often to there is temperature in these methods in preparation process, consumes height, the shortcomings such as controlled difficulty is big, big to environmental disruption, equipment and technology is required height, the problems such as Properties Control difficulty is big.Owing to the price of nickel is high, limit the extensive application of corronil, the advantages such as the preparation method probing into new corronil is extremely important, and eutectic type ionic liquid prepares corronil need not add buffer agent, has simple to operate, it is easy to control, good product quality.
Eutectic type ionic liquid has degradable, environmental friendliness, it is easy to synthesis, and utilization rate is high, and cheap, fusing point is low, conducts electricity very well, and steam forces down, electrochemical window width, is the advantages such as liquid object Physicochemical stable in properties under room temperature.Eutectic type ionic liquid is the eutectic mixture under a kind of room temperature synthesized by a certain percentage by quaternary ammonium salt and hydrogen bond for liquid.There is temperature technically due to traditional method high, consume height, controlled difficulty is big, a series of problems such as efficiency is low, and toxicity is big, and eutectic type ionic liquid is prepared corronil material aspect and then demonstrated its superiority, and operation can reach material, and to prepare degree controlled.
Apply for a patent CN104178784A and disclose a kind of method depositing corronil in aqueous；With saturated calomel electrode as reference electrode, platinum electrode is to electrode, copper electrode is negative electrode, using nickel sulfate, copper sulfate, surfactant sodium dodecyl base sodium sulfonate, your sodium manganate of complexing of metal ion agent mixed solution as electrolyte, adjust pH value of solution to 2-6, prepare corronil film with galvanostatic deposition, and under 500 DEG C of high temperature, process 0.5h, obtain the corronil film of densification.This application patent uses aqueous solution as electrolyte, there is solution preparation complexity, and to add expensive surfactant and chelating agent, improves cost；And at high temperature to process, cause energy resource consumption to increase.
Document Wang S, Guo X, Yang H, et al. Electrodeposition mechanism and characterization of Ni Cu
alloy coatings from a eutectic-based ionic liquid[J]. Applied Surface Science,
2014, the method that another kind prepares corronil is described in 288:530-536., wherein solution preparation choline chloride is that 1:2 mixes with carbamide according to mol ratio, form eutectic type ionic liquid, then in eutectic ionic liquid, Nickel dichloride hexahydrate and Copper dichloride dihydrate are added as presoma, the mixed solution formed is as electrolyte solution, using saturated calomel electrode as reference electrode, platinum electrode is as to electrode, copper microelectrode is as working electrode, carry out electro-deposition and produce corronil, obtain the nano-copper-nickel alloy pattern of shuttle shape；The present invention is in a kind of eutectic type ionic liquid, and Electrowinning corronil under constant potential obtains mesh nano corronil material.Its process, without buffer agent, the interpolation of chelating agent, does not carry out the process of high temperature, reduces cost, save energy resource consumption.
Summary of the invention
The problem existed for above-mentioned prior art and deficiency, the present invention provides a kind of method of eutectic type ionic liquid electrolytic preparation mesh nanometer monel.The present invention is to be solvent based on eutectic type ionic liquid, prepares mesh nanometer corronil material by the method for electrolysis.The method is that lamellar fine copper is depositing base using Nickel dichloride hexahydrate and Copper dichloride dihydrate as presoma, with electrolysis method prepare the corronil material of mesh nanometer, can reach controlled by the method, gentle, the advantage such as cheap.The present invention is achieved through the following technical solutions.
A kind of method of eutectic type ionic liquid electrolytic preparation mesh nanometer monel, first nickel salt presoma and mantoquita presoma are joined in eutectic type ionic liquid as electrolyte, use three-electrode system, with platinum electrode or graphite as electrolytic anode, silver wire electrode is reference electrode, with copper or rustless steel as working electrode, it is less than 100 degrees Celsius in temperature and carries out being electrolysed and prepare mesh nanometer corronil thin film on the working electrode (s.
It specifically comprises the following steps that
(1) electrolyte configuration: be 1:(1～4 according to mol ratio by quaternary ammonium salt and alcohols or amide) mix homogeneously and obtain eutectic type ionic liquid, then nickel presoma and copper presoma are joined in eutectic type ionic liquid, after being thoroughly mixed uniformly, obtain ionic liquid-mantoquita-nickel salt composite electrolyte；
(2) working electrode surface processes: with copper or rustless steel as working electrode, copper or rustless steel through dilute hydrochloric acid immersions, soaked in absolute ethyl alcohol, dilute hydrochloric acid soaks, working electrode surface is processed by ionized water flushing；
(3) constant-potential electrolysis: use three-electrode system, with platinum electrode or graphite as electrolytic anode, silver wire electrode is reference electrode, will be through the electrode of step (2) surface preparation as working electrode, in ionic liquid-mantoquita-nickel salt composite electrolyte that step (1) is prepared, temperature be 333 ~ 373K, current potential for-0.6 ~-1.0Vvs.Ag carry out potentiostatic deposition deposition 0.5 ~ 2h, by the working electrode matrix after electrolysis through dehydrated alcohol, distilled water flushing, mesh nanometer corronil thin film can be obtained at working electrode matrix surface after drying.
Quaternary ammonium salt in described step (1) is choline chloride or tetramethyl ammonium chloride.
Alcohols in described step (1) is ethylene glycol.
Amide in described step (1) is carbamide or acetamide.
In described step (1), mantoquita presoma is copper chloride or copper sulfate.
In described step (1), nickel salt presoma is Nickel dichloride. or nickel sulfate.
The invention has the beneficial effects as follows: (1), can electrolytic preparation corronil nano material without adding any additive；(2) corronil is dispersed in matrix surface, is evenly distributed, fine and close and bright；(3) reaction condition is gentle, and energy consumption is low, and condition is controlled, does not has the adjustment of acidity-basicity ph；(4) simple to operate, green non-pollution, constant product quality, inexpensive.
Accompanying drawing explanation
Fig. 1 is the mesh nanometer monel SEM figure that the embodiment of the present invention 1 prepares；
Fig. 2 is the mesh nanometer monel XRD figure that the embodiment of the present invention 1 prepares；
Fig. 3 is the mesh nanometer monel dynamic potential polarization curve figure that the embodiment of the present invention 1 prepares；
Fig. 4 is the mesh nanometer monel SEM figure that the embodiment of the present invention 2 prepares；
Fig. 5 is the mesh nanometer monel SEM figure that the embodiment of the present invention 3 prepares；
Fig. 6 is the mesh nanometer monel SEM figure that the embodiment of the present invention 4 prepares；
Fig. 7 is the mesh nanometer monel SEM figure that the embodiment of the present invention 5 prepares.
Detailed description of the invention
Below in conjunction with the accompanying drawings and detailed description of the invention, the invention will be further described.
Embodiment 1
The method of this eutectic type ionic liquid electrolytic preparation mesh nanometer monel, first nickel salt presoma and mantoquita presoma are joined in eutectic type ionic liquid as electrolyte, use three-electrode system, with platinum electrode or graphite as electrolytic anode, silver wire electrode is reference electrode, with copper or rustless steel as working electrode, it is less than 100 degrees Celsius in temperature and carries out being electrolysed and prepare mesh nanometer corronil thin film on the working electrode (s.
It specifically comprises the following steps that
(1) electrolyte configuration: be that 1:2 is mixed homogeneously and obtained eutectic type ionic liquid according to mol ratio by choline chloride and ethylene glycol, then 6.0g nickel presoma (Nickel dichloride hexahydrate) and 0.80g copper presoma (Copper dichloride dihydrate) is joined in 50ml eutectic type ionic liquid, after being thoroughly mixed uniformly, obtain ionic liquid-mantoquita-nickel salt composite electrolyte；
(2) working electrode surface processes: with copper (1.5cm × 1.5cm × 0.1cm) as working electrode, and copper soaks (concentration is that 1% dilute hydrochloric acid soaks 15min), soaked in absolute ethyl alcohol (concentration is 95% soaked in absolute ethyl alcohol 10min) through dilute hydrochloric acid, dilute hydrochloric acid soaks (concentration is that 1% dilute hydrochloric acid soaks 10min), ionized water rinses and processes working electrode surface；
(3) constant-potential electrolysis: use three-electrode system, with platinum electrode for electrolysis to electrode, silver wire electrode is reference electrode, will be through the electrode of step (2) surface preparation as working electrode, electrode spacing is 1cm, in ionic liquid-mantoquita-nickel salt composite electrolyte that step (1) is prepared, temperature be 333K, sedimentation potential be-0.6V potentiostatic deposition 0.5h, by the working electrode matrix after electrolysis through dehydrated alcohol, deionized water rinsing, mesh nanometer corronil thin film can be obtained at working electrode matrix surface after drying.
Above-mentioned prepare mesh nanometer corronil thin film SEM figure as it is shown in figure 1, XRD figure as shown in Figure 2.Using copper sheet that surface is mesh nanometer corronil thin film as working electrode, platinum electrode is made electrode, silver wire electrode is as reference electrode, 1MKOH solution is electrolyte, in the scanning volt-ampere test of electrochemical workstation enterprising line linearity, its result shows, when-100mV current potential, the electric current density of corronil is 5.108mAcm-2, the electric current density of copper sheet is 0.477mAcm-2；When-200mV current potential, the electric current density of corronil is 29.867mAcm-2, the electric current density of copper sheet is 0.935mAcm-2；When-300mV current potential, the electric current density of corronil is 79.6mAcm-2, the electric current density of copper sheet is 2.224mAcm-2；Demonstrating from data above, compared with copper sheet, the catalytic performance of corronil significantly improves, and dynamic potential polarization curve figure is as shown in Figure 3.
Embodiment 2
The method of this eutectic type ionic liquid electrolytic preparation mesh nanometer monel, first nickel salt presoma and mantoquita presoma are joined in eutectic type ionic liquid as electrolyte, use three-electrode system, with platinum electrode or graphite as electrolytic anode, silver wire electrode is reference electrode, with copper or rustless steel as working electrode, it is less than 100 degrees Celsius in temperature and carries out being electrolysed and prepare mesh nanometer corronil thin film on the working electrode (s.
It specifically comprises the following steps that
(1) electrolyte configuration: be that 1:3 is mixed homogeneously and obtained eutectic type ionic liquid according to mol ratio by choline chloride and carbamide, then 6.0g nickel presoma (Nickel dichloride hexahydrate) and 0.80g copper presoma (Copper dichloride dihydrate) is joined in 50ml eutectic type ionic liquid, after being thoroughly mixed uniformly, obtain ionic liquid-mantoquita-nickel salt composite electrolyte；
(2) working electrode surface processes: with stainless steel substrates (1.5cm × 1.5cm × 0.1cm) as working electrode, and copper soaks (concentration is that 1% dilute hydrochloric acid soaks 15min), soaked in absolute ethyl alcohol (concentration is 95% soaked in absolute ethyl alcohol 10min) through dilute hydrochloric acid, dilute hydrochloric acid soaks (concentration is that 1% dilute hydrochloric acid soaks 10min), ionized water rinses and processes working electrode surface；
(3) constant-potential electrolysis: use three-electrode system, with platinum electrode as electrolytic anode, silver wire electrode is reference electrode, will be through the electrode of step (2) surface preparation as working electrode, electrode spacing is 1cm, in ionic liquid-mantoquita-nickel salt composite electrolyte that step (1) is prepared, it is 333K in temperature, sedimentation potential is-0.7V potentiostatic deposition 0.5h, by the working electrode matrix after electrolysis through dehydrated alcohol, distilled water flushing, mesh nanometer corronil thin film can be obtained after drying at working electrode matrix surface, mesh nanometer monel SEM schemes as shown in Figure 4.
Embodiment 3
The method of this eutectic type ionic liquid electrolytic preparation mesh nanometer monel, first nickel salt presoma and mantoquita presoma are joined in eutectic type ionic liquid as electrolyte, use three-electrode system, with platinum electrode or graphite as electrolytic anode, silver wire electrode is reference electrode, with copper or rustless steel as working electrode, it is less than 100 degrees Celsius in temperature and carries out being electrolysed and prepare mesh nanometer corronil thin film on the working electrode (s.
It specifically comprises the following steps that
(1) electrolyte configuration: be that 1:4 is mixed homogeneously and obtained eutectic type ionic liquid according to mol ratio by choline chloride and acetamide, then 6.0g nickel presoma (Nickel dichloride hexahydrate) and 0.80g copper presoma (Copper dichloride dihydrate) is joined in 50ml eutectic type ionic liquid, after being thoroughly mixed uniformly, obtain ionic liquid-mantoquita-nickel salt composite electrolyte；
(2) working electrode surface processes: with copper sheet (1.5cm × 1.5cm × 0.1cm) as working electrode, and copper soaks (concentration is that 1% dilute hydrochloric acid soaks 15min), soaked in absolute ethyl alcohol (concentration is 95% soaked in absolute ethyl alcohol 10min) through dilute hydrochloric acid, dilute hydrochloric acid soaks (concentration is that 1% dilute hydrochloric acid soaks 10min), working electrode surface is processed by deionized water rinsing；
(3) constant-potential electrolysis: use three-electrode system, with platinum electrode as electrolytic anode, silver wire electrode is reference electrode, will be through the electrode of step (2) surface preparation as working electrode, electrode spacing is 1cm, in ionic liquid-mantoquita-nickel salt composite electrolyte that step (1) is prepared, it is 333K in temperature, sedimentation potential carries out potentiostatic deposition 2h for-0.6V, by the working electrode matrix after electrolysis through dehydrated alcohol, distilled water flushing, mesh nanometer corronil thin film can be obtained after drying at working electrode matrix surface, mesh nanometer monel SEM schemes as shown in Figure 5.
Embodiment 4
The method of this eutectic type ionic liquid electrolytic preparation mesh nanometer monel, first nickel salt presoma and mantoquita presoma are joined in eutectic type ionic liquid as electrolyte, use three-electrode system, with platinum electrode or graphite as electrolytic anode, silver wire electrode is reference electrode, with copper or rustless steel as working electrode, it is less than 100 degrees Celsius in temperature and carries out being electrolysed and prepare mesh nanometer corronil thin film on the working electrode (s.
It specifically comprises the following steps that
(1) electrolyte configuration: be that 1:2 is mixed homogeneously and obtained eutectic type ionic liquid according to mol ratio by tetramethyl ammonium chloride and acetamide, then 6.0g nickel presoma (Nickel dichloride hexahydrate) and 0.80g copper presoma (Copper dichloride dihydrate) is joined in 50ml eutectic type ionic liquid, after being thoroughly mixed uniformly, obtain ionic liquid-mantoquita-nickel salt composite electrolyte；
(2) working electrode surface processes: with copper sheet (1.5cm × 1.5cm × 0.1cm) as working electrode, and copper soaks (concentration is that 1% dilute hydrochloric acid soaks 15min), soaked in absolute ethyl alcohol (concentration is 95% soaked in absolute ethyl alcohol 10min) through dilute hydrochloric acid, dilute hydrochloric acid soaks (concentration is that 1% dilute hydrochloric acid soaks 10min), working electrode surface is processed by deionized water rinsing；
(3) constant-potential electrolysis: use three-electrode system, with platinum electrode as electrolytic anode, silver wire electrode is reference electrode, will be through the electrode of step (2) surface preparation as working electrode, electrode spacing is 1cm, in ionic liquid-mantoquita-nickel salt composite electrolyte that step (1) is prepared, it is 333K in temperature, sedimentation potential carries out potentiostatic deposition 0.5h for-0.9V, by the working electrode matrix after electrolysis through dehydrated alcohol, distilled water flushing, mesh nanometer corronil thin film can be obtained after drying at working electrode matrix surface, mesh nanometer monel SEM schemes as shown in Figure 6.
Embodiment 5
The method of this eutectic type ionic liquid electrolytic preparation mesh nanometer monel, first nickel salt presoma and mantoquita presoma are joined in eutectic type ionic liquid as electrolyte, use three-electrode system, with platinum electrode or graphite as electrolytic anode, silver wire electrode is reference electrode, with copper or rustless steel as working electrode, it is less than 100 degrees Celsius in temperature and carries out being electrolysed and prepare mesh nanometer corronil thin film on the working electrode (s.
It specifically comprises the following steps that
(1) electrolyte configuration: be that 1:3 is mixed homogeneously and obtained eutectic type ionic liquid according to mol ratio by choline chloride and ethylene glycol amine, then 6.0g nickel presoma (Nickel dichloride hexahydrate) and 0.80g copper presoma (Copper dichloride dihydrate) is joined in 50ml eutectic type ionic liquid, after being thoroughly mixed uniformly, obtain ionic liquid-mantoquita-nickel salt composite electrolyte；
(2) working electrode surface processes: with stainless steel substrates (1.5cm × 1.5cm × 0.1cm) as working electrode, and copper soaks (concentration is that 1% dilute hydrochloric acid soaks 15min), soaked in absolute ethyl alcohol (concentration is 95% soaked in absolute ethyl alcohol 10min) through dilute hydrochloric acid, dilute hydrochloric acid soaks (concentration is that 1% dilute hydrochloric acid soaks 10min), ionized water rinses and processes working electrode surface；
(3) constant-potential electrolysis: use three-electrode system, with platinum electrode as electrolytic anode, silver wire electrode is reference electrode, will be through the electrode of step (2) surface preparation as working electrode, electrode spacing is 1cm, in ionic liquid-mantoquita-nickel salt composite electrolyte that step (1) is prepared, it is 333K in temperature, sedimentation potential is-0.8V potentiostatic deposition 0.5h, by the working electrode matrix after electrolysis through dehydrated alcohol, distilled water flushing, mesh nanometer corronil thin film can be obtained after drying at working electrode matrix surface, mesh nanometer monel SEM schemes as shown in Figure 7.
Embodiment 6
The method of this eutectic type ionic liquid electrolytic preparation mesh nanometer monel, first nickel salt presoma and mantoquita presoma are joined in eutectic type ionic liquid as electrolyte, use three-electrode system, with platinum electrode or graphite as electrolytic anode, silver wire electrode is reference electrode, with copper or rustless steel as working electrode, it is less than 100 degrees Celsius in temperature and carries out being electrolysed and prepare mesh nanometer corronil thin film on the working electrode (s.
It specifically comprises the following steps that
(1) electrolyte configuration: be that 1:1 is mixed homogeneously and obtained eutectic type ionic liquid according to mol ratio by choline chloride and ethylene glycol amine, then 6.0g nickel presoma (Nickel dichloride hexahydrate) and 0.80g copper presoma (Copper dichloride dihydrate) is joined in 50ml eutectic type ionic liquid, after being thoroughly mixed uniformly, obtain ionic liquid-mantoquita-nickel salt composite electrolyte；
(2) working electrode surface processes: with stainless steel substrates (1.5cm × 1.5cm × 0.1cm) as working electrode, and copper soaks (concentration is that 1% dilute hydrochloric acid soaks 15min), soaked in absolute ethyl alcohol (concentration is 95% soaked in absolute ethyl alcohol 10min) through dilute hydrochloric acid, dilute hydrochloric acid soaks (concentration is that 1% dilute hydrochloric acid soaks 10min), ionized water rinses and processes working electrode surface；
(3) constant-potential electrolysis: use three-electrode system, with platinum electrode as electrolytic anode, silver wire electrode is reference electrode, will be through the electrode of step (2) surface preparation as working electrode, electrode spacing is 1cm, in ionic liquid-mantoquita-nickel salt composite electrolyte that step (1) is prepared, temperature be 373K, sedimentation potential be-1.0V potentiostatic deposition 1.5h, by the working electrode matrix after electrolysis through dehydrated alcohol, distilled water flushing, mesh nanometer corronil thin film can be obtained at working electrode matrix surface after drying.
Embodiment 7
The method of this eutectic type ionic liquid electrolytic preparation mesh nanometer monel, first nickel salt presoma and mantoquita presoma are joined in eutectic type ionic liquid as electrolyte, use three-electrode system, with platinum electrode or graphite as electrolytic anode, silver wire electrode is reference electrode, with copper or rustless steel as working electrode, it is less than 100 degrees Celsius in temperature and carries out being electrolysed and prepare mesh nanometer corronil thin film on the working electrode (s.
It specifically comprises the following steps that
(1) electrolyte configuration: be that 1:2 is mixed homogeneously and obtained eutectic type ionic liquid according to mol ratio by choline chloride and ethylene glycol amine, then 6.0g nickel presoma (Nickel dichloride hexahydrate) and 0.60g copper presoma (Copper dichloride dihydrate) is joined in 50ml eutectic type ionic liquid, after being thoroughly mixed uniformly, obtain ionic liquid-mantoquita-nickel salt composite electrolyte；
(2) working electrode surface processes: with stainless steel substrates (1.5cm × 1.5cm × 0.1cm) as working electrode, and copper soaks (concentration is that 1% dilute hydrochloric acid soaks 15min), soaked in absolute ethyl alcohol (concentration is 95% soaked in absolute ethyl alcohol 10min) through dilute hydrochloric acid, dilute hydrochloric acid soaks (concentration is that 1% dilute hydrochloric acid soaks 10min), working electrode surface is processed by deionized water rinsing；
(3) constant-potential electrolysis: use three-electrode system, with platinum electrode as electrolytic anode, silver wire electrode is reference electrode, will be through the electrode of step (2) surface preparation as working electrode, electrode spacing is 1cm, in ionic liquid-mantoquita-nickel salt composite electrolyte that step (1) is prepared, temperature be 353K, sedimentation potential be-0.6V, electrolytic deposition 1.8h, by the working electrode matrix after electrolysis through dehydrated alcohol, distilled water flushing, mesh nanometer corronil thin film can be obtained at working electrode matrix surface after drying.
Above in association with accompanying drawing, the detailed description of the invention of the present invention is explained in detail, but the present invention is not limited to above-mentioned embodiment, in the ken that those of ordinary skill in the art are possessed, it is also possible on the premise of without departing from present inventive concept, various changes can be made.
Claims (7)
1. the method for an eutectic type ionic liquid electrolytic preparation mesh nanometer monel, it is characterized in that: first nickel salt presoma and mantoquita presoma are joined in eutectic type ionic liquid as electrolyte, use three-electrode system, with platinum electrode or graphite as electrolytic anode, silver wire electrode is reference electrode, with copper or rustless steel as working electrode, it is less than 100 degrees Celsius in temperature and carries out being electrolysed and prepare mesh nanometer corronil thin film on the working electrode (s.
The method of eutectic type ionic liquid electrolytic preparation mesh nanometer monel the most according to claim 1, it is characterised in that specifically comprise the following steps that
(1) electrolyte configuration: be 1:(1～4 according to mol ratio by quaternary ammonium salt and alcohols or amide) mix homogeneously and obtain eutectic type ionic liquid, then nickel presoma and copper presoma are joined in eutectic type ionic liquid, after being thoroughly mixed uniformly, obtain ionic liquid-mantoquita-nickel salt composite electrolyte；
(2) working electrode surface processes: with copper or rustless steel as working electrode, copper or rustless steel through dilute hydrochloric acid immersions, soaked in absolute ethyl alcohol, dilute hydrochloric acid soaks, working electrode surface is processed by ionized water flushing；
(3) constant-potential electrolysis: use three-electrode system, with platinum electrode or graphite as electrolytic anode, silver wire electrode is reference electrode, will be through the electrode of step (2) surface preparation as working electrode, in ionic liquid-mantoquita-nickel salt composite electrolyte that step (1) is prepared, temperature be 333 ~ 373K, current potential for-0.6 ~-1.0Vvs.Ag carry out potentiostatic deposition deposition 0.5 ~ 2h, by the working electrode matrix after electrolysis through dehydrated alcohol, distilled water flushing, mesh nanometer corronil thin film can be obtained at working electrode matrix surface after drying.
The method of eutectic type ionic liquid electrolytic preparation mesh nanometer monel the most according to claim 2, it is characterised in that: the quaternary ammonium salt in described step (1) is choline chloride or tetramethyl ammonium chloride.
The method of eutectic type ionic liquid electrolytic preparation mesh nanometer monel the most according to claim 2, it is characterised in that: the alcohols in described step (1) is ethylene glycol.
The method of eutectic type ionic liquid electrolytic preparation mesh nanometer monel the most according to claim 2, it is characterised in that: the amide in described step (1) is carbamide or acetamide.
The method of eutectic type ionic liquid electrolytic preparation mesh nanometer monel the most according to claim 2, it is characterised in that: in described step (1), mantoquita presoma is copper chloride or copper sulfate.
The method of eutectic type ionic liquid electrolytic preparation mesh nanometer monel the most according to claim 2, it is characterised in that: in described step (1), nickel salt presoma is Nickel dichloride. or nickel sulfate.
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| CN106623969A (en) * | 2016-11-23 | 2017-05-10 | 昆明理工大学 | Method of preparing nanometer nickel-sulfur alloy through replacement deposition of low eutectic ionic liquid |
| CN107142497A (en) * | 2017-05-31 | 2017-09-08 | 河海大学 | A kind of low temperature melts the anhydrous method for preparing nanometer crystalline Ni W B alloys of salt |
| CN108070887A (en) * | 2016-11-15 | 2018-05-25 | 财团法人工业技术研究院 | Electroplating method and system thereof |
| CN108660483A (en) * | 2018-06-08 | 2018-10-16 | 上海大学 | A kind of preparation method of corronil |
| CN110029370A (en) * | 2019-04-17 | 2019-07-19 | 上海大学 | By the method for low value cupro-nickel composite ore electro-deposition preparation high level ternary alloy three-partalloy |
| CN111041525A (en) * | 2019-12-31 | 2020-04-21 | 谷波技术(常州)有限公司 | Method for enhancing surface of microwave communication device by electroplating Ni-WC composite layer through low-temperature molten salt |
| CN114378300A (en) * | 2022-01-21 | 2022-04-22 | 重庆科技学院 | Method for preparing nano copper powder by using copper oxide as raw material |
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| CN108070887A (en) * | 2016-11-15 | 2018-05-25 | 财团法人工业技术研究院 | Electroplating method and system thereof |
| CN106623969A (en) * | 2016-11-23 | 2017-05-10 | 昆明理工大学 | Method of preparing nanometer nickel-sulfur alloy through replacement deposition of low eutectic ionic liquid |
| CN107142497A (en) * | 2017-05-31 | 2017-09-08 | 河海大学 | A kind of low temperature melts the anhydrous method for preparing nanometer crystalline Ni W B alloys of salt |
| CN107142497B (en) * | 2017-05-31 | 2019-05-28 | 河海大学 | A kind of method that low temperature melts the anhydrous preparation nanometer crystalline Ni-W-B alloy of salt |
| CN108660483A (en) * | 2018-06-08 | 2018-10-16 | 上海大学 | A kind of preparation method of corronil |
| CN110029370A (en) * | 2019-04-17 | 2019-07-19 | 上海大学 | By the method for low value cupro-nickel composite ore electro-deposition preparation high level ternary alloy three-partalloy |
| CN111041525A (en) * | 2019-12-31 | 2020-04-21 | 谷波技术(常州)有限公司 | Method for enhancing surface of microwave communication device by electroplating Ni-WC composite layer through low-temperature molten salt |
| CN111041525B (en) * | 2019-12-31 | 2022-02-08 | 谷波技术(常州)有限公司 | Method for enhancing surface of microwave communication device by electroplating Ni-WC composite layer through low-temperature molten salt |
| CN114378300A (en) * | 2022-01-21 | 2022-04-22 | 重庆科技学院 | Method for preparing nano copper powder by using copper oxide as raw material |
| CN114378300B (en) * | 2022-01-21 | 2023-10-20 | 重庆科技学院 | Method for preparing nanometer copper powder by taking copper oxide as raw material |
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Application publication date: 20161012 |