CN107447208B - Method for preparing Pd-Ni-Fe-P alloy film by chemical plating-displacement - Google Patents
Method for preparing Pd-Ni-Fe-P alloy film by chemical plating-displacement Download PDFInfo
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- CN107447208B CN107447208B CN201710486054.7A CN201710486054A CN107447208B CN 107447208 B CN107447208 B CN 107447208B CN 201710486054 A CN201710486054 A CN 201710486054A CN 107447208 B CN107447208 B CN 107447208B
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- 229910001096 P alloy Inorganic materials 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000000126 substance Substances 0.000 title claims abstract description 15
- 238000006073 displacement reaction Methods 0.000 title claims abstract description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 27
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 24
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000007747 plating Methods 0.000 claims abstract description 16
- 239000002608 ionic liquid Substances 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 10
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 10
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 10
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 10
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims abstract description 10
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims abstract description 10
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000004310 lactic acid Substances 0.000 claims abstract description 9
- 235000014655 lactic acid Nutrition 0.000 claims abstract description 9
- 239000001509 sodium citrate Substances 0.000 claims abstract description 9
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims abstract description 9
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 8
- IQQRAVYLUAZUGX-UHFFFAOYSA-N 1-butyl-3-methylimidazolium Chemical compound CCCCN1C=C[N+](C)=C1 IQQRAVYLUAZUGX-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000012046 mixed solvent Substances 0.000 claims abstract description 7
- 239000000758 substrate Substances 0.000 claims abstract description 7
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims abstract description 7
- 229940038773 trisodium citrate Drugs 0.000 claims abstract description 7
- SFILQUUOZXCFLL-UHFFFAOYSA-N Cl.CCCCC1=NC=C(C)N1 Chemical compound Cl.CCCCC1=NC=C(C)N1 SFILQUUOZXCFLL-UHFFFAOYSA-N 0.000 claims abstract description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000004202 carbamide Substances 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract 2
- 238000003756 stirring Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 13
- 239000001257 hydrogen Substances 0.000 abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 13
- 239000000956 alloy Substances 0.000 abstract description 9
- 230000003197 catalytic effect Effects 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 5
- 229910000808 amorphous metal alloy Inorganic materials 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 239000010949 copper Substances 0.000 description 8
- 229910045601 alloy Inorganic materials 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
- 241000080590 Niso Species 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 229910001868 water Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 244000137852 Petrea volubilis Species 0.000 description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 2
- 235000011130 ammonium sulphate Nutrition 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000004070 electrodeposition Methods 0.000 description 2
- 238000007772 electroless plating Methods 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- -1 28% Substances 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 208000021251 Methanol poisoning Diseases 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229910002669 PdNi Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005323 electroforming Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical compound [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/48—Coating with alloys
- C23C18/50—Coating with alloys with alloys based on iron, cobalt or nickel
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/185—Phosphorus; Compounds thereof with iron group metals or platinum group metals
- B01J27/1856—Phosphorus; Compounds thereof with iron group metals or platinum group metals with platinum group metals
-
- B01J35/33—
Abstract
The patent discloses a method for preparing a Pd-Ni-Fe-P alloy film by utilizing chemical plating-replacement, which comprises the following steps: taking nickel sulfate, ferrous sulfate, sodium hypophosphite, lactic acid and trisodium citrate as chemical plating raw materials, and carrying out chemical plating on a Cu sheet substrate to obtain a Ni-Fe-P alloy plated part; adding anhydrous low-melting-point mixed solvent of ionic liquid methylbutyl imidazole chloride (with the molecular formula of BMIMCl), Ethylene Glycol (EG) and urea (with the molar ratio of 1:1:1) and ionic liquid [ BMIM ] containing palladium into a displacement reaction vessel]2PdCl4As a replacement liquid, the Ni-Fe-P alloy plating piece is put into the replacement liquid to be soaked for a period of time, and the Pd-Ni-Fe-P alloy film prepared by the replacement reaction belongs to an amorphous alloy material, has high surface energy, shows high catalytic activity to the hydrogen evolution reaction, and has the advantages of simple process, easy preparation and low price.
Description
Technical Field
The invention belongs to the field of preparation of alloy catalysts, and particularly relates to a method for preparing a Pd-Ni-Fe-P alloy film by utilizing chemical plating-replacement.
Background
The most abundant oxygen element in the universe is the cleanest ideal fuel. Hydrogen is to be understood as future fuel. Electrolysis of aqueous solutions is a way to produce clean hydrogen energy, which, although not inexpensive, provides high purity hydrogen and avoids the use of fossil fuels, without the greenhouse gases CO: and (4) directly discharging. Therefore, the low cost of hydrogen production is such that this technologyKey element of commercialization. In order to meet the requirements of professional, economic and environmental protection and obtain cheap hydrogen products, the research on obtaining a coating material suitable for electrolysis is necessary. Noble metals such as Pt and Ru have high activity and are expensive for industrial use. The transition metals palladium, nickel, iron, cobalt and the like and alloys thereof have the dual advantages of low hydrogen evolution overpotential and low cost. Doping of nano-sized Pd (nano-particles, nano-wires or nano-pores, etc.) is an effective method. The hot point of research at present is to add non-noble metal elements such as Co, Ni, Cu, Fe and the like. Such as Mustain, etc. by electrodeposition on a gold electrode at room temperature using a two-site coordination method3The oxygen reduction catalytic activity of the Co polycrystalline catalyst is very close to that of polycrystalline Pt under the same condition, and the Co polycrystalline catalyst has better methanol poisoning resistance. PdNi prepared by electrodeposition2The catalytic activity and stability of the catalyst to formic acid are superior to those of pure Pd catalyst. Some non-metallic doping can also promote the catalytic properties of Pd. For example, the addition of P can make surface atoms have high activity, increase the density of hydrogen evolution exchange current, reduce hydrogen evolution overpotential, and show high catalytic activity and stability for hydrogen evolution reaction. However, due to the difficulty in preparation, few reports on ternary or higher complex doping in nano-Pd are reported. The main methods for preparing palladium-based films are conventional roll-to-roll, Physical Vapor Deposition (PVD), Chemical Vapor Deposition (CVD), electroplating or electroforming, Electroless Plating (EP), and spray pyrolysis.
The invention firstly uses nickel sulfate (NiSO)4·7H2O), ferrous sulfate (FeSO)4·7H2O) as metal precursor, sodium hypophosphite (NaH)2PO2·H2O) is used as a reducing agent to reduce metal ions, the obtained alloy Ni-Fe-P is loaded on the surface of a substrate, and Pd is carried out by taking the alloy Ni-Fe-P as the reducing agent2+Reducing the metal Pd particles to form a Pd-Ni-Fe-P alloy film.
Disclosure of Invention
The invention aims to provide a method for preparing a Pd-Ni-Fe-P alloy film by utilizing electroless plating-replacement. The Pd-Ni-Fe-P alloy membrane prepared by the method has excellent catalytic activity, and the preparation method is simple, low in cost and free of professional operation.
The invention provides a method for preparing a Pd-Ni-Fe-P alloy film by utilizing chemical plating-replacement, which is characterized in that nickel sulfate (NiSO) is added into a chemical plating bath4·7H2O), ferrous sulfate (FeSO)4·7H2O), sodium hypophosphite (NaH)2PO2·H2O), lactic acid and trisodium citrate are used as chemical plating solution, fully stirred and chemically plated on a Cu sheet to obtain a Ni-Fe-P alloy plated part; adding anhydrous low-melting-point mixed solvent of ionic liquid methylbutyl imidazole chloride (with the molecular formula of BMIMCl), Ethylene Glycol (EG) and urea (with the molar ratio of 1:1:1) and ionic liquid [ BMIM ] containing palladium into a displacement reaction vessel]2PdCl4And as a replacement solution, putting the Ni-Fe-P alloy plated piece into the replacement solution to be soaked for a period of time to prepare the Pd-Ni-Fe-P alloy film.
Preferably, the plating solution of the Ni-Fe-P alloy has the optimized formula and the process conditions as follows: 35g/L of nickel sulfate, 40g/L of sodium hypophosphite, 12g/L of ferrous sulfate, 30g/L of trisodium citrate, 20g/L of ammonium sulfate and 20mL/L of lactic acid, wherein the temperature of the solution is (90 +/-2) DEG C, and the pH value of the solution is 9.0-10.0.
Preferably, the palladium ion liquid [ BMIM ] in the displacement liquid]2PdCl4The concentration is 5-10g/L, the alloy plating piece is soaked in the replacement liquid for 8-12h, the temperature is kept at 50-70 ℃, and the stirring speed is controlled at 200-300 rm.
A method for preparing a Pd-Ni-Fe-P alloy film by utilizing chemical plating-displacement comprises the following specific steps:
step 2, respectively weighing a certain amount of nickel sulfate (NiSO)4·7H2O), ferrous sulfate (FeSO)4·7H2O), sodium hypophosphite (NaH)2PO2·H2O), lactic acid and trisodium citrate, and respectively dissolving with distilled water to obtain clear solution. Dissolving the dissolved nickel sulfate solution, ferrous sulfate, lactic acid and sodium hypophosphite solution in a solventStirring, adding into sodium citrate solution, adding distilled water to 200mL, stirring to obtain chemical plating solution, and sucking appropriate amount of sodium hydroxide solution with a suction tube to adjust pH value of the plating solution.
Step 3, in an inert gas environment, putting a certain amount of anhydrous low-melting-point mixed solvent of ionic liquid methylbutyl imidazole chloride (with the molecular formula of BMIMCl), Ethylene Glycol (EG) and urea (the molar ratio is 1:1:1) into a replacement reaction vessel, and then respectively adding a certain amount of palladium-containing ionic liquid [ BMIM ] into the low-melting-point mixed solvent]2PdCl4And (3) soaking the alloy plated part obtained in the step (2) in a displacement solution for a period of time, and performing displacement reaction to obtain the Pd-Ni-Fe-P alloy film. The chemical reaction that takes place during the displacement is as follows:
[PdCl4]-2+Fe→Pd+FeCl3 -
[PdCl4]-2+Ni→Pd+NiCl3 -
the invention is characterized in that:
(1) the Pd-Ni-Fe-P alloy film prepared by the invention belongs to an amorphous alloy material, has high surface energy, enables surface atoms to have high activity, increases the density of hydrogen evolution exchange current, reduces hydrogen evolution overpotential, and shows high catalytic activity to hydrogen evolution reaction.
(2) The invention has simple process, mild reaction condition, easy preparation and low price.
Drawings
The attached drawing is a surface topography of the Pd-Ni-Fe-P alloy film in the invention.
Detailed Description
The present invention will be further described with reference to the following embodiments.
step 2, respectively weighing a certain amount of nickel sulfate (NiSO)4·7H2O), ferrous sulfate (FeSO)4·7H2O), HaviaSodium phosphate (NaH)2PO2·H2O), lactic acid and trisodium citrate, and respectively dissolving with distilled water to obtain clear solution. The dissolved nickel sulfate solution, ferrous sulfate, lactic acid and sodium hypophosphite solution are poured into the sodium citrate solution under continuous stirring, distilled water is added into the solution to 200mL and stirred to be used as chemical plating solution, and a proper amount of sodium hydroxide solution is sucked by a suction pipe to adjust the pH value of the plating solution. The plating solution for chemically plating the Ni-Fe-P alloy film has the optimized formula and the process conditions that: 35g/L of nickel sulfate, 40g/L of sodium hypophosphite, 12g/L of ferrous sulfate, 30g/L of trisodium citrate, 20g/L of ammonium sulfate and 20mL/L of lactic acid, wherein the temperature of the solution is (90 +/-2) DEG C, and the pH value of the solution is 10.0.
Step 3, in an inert gas environment, putting 400mL of anhydrous low-melting-point mixed solvent of ionic liquid methylbutyl imidazole chloride (with the molecular formula of BMIMCl), Ethylene Glycol (EG) and urea (in a molar ratio of 1:1:1) into a replacement reaction vessel, and then respectively adding 3g of palladium-containing ionic liquid [ BMIM ] into the low-melting-point mixed solvent]2PdCl4And (3) soaking the alloy plated part obtained in the step (2) in a replacement solution for 10 hours, keeping the temperature at 60 ℃, and controlling the stirring speed at 250rm to obtain the Pd-Ni-Fe-P alloy film. Surface composition analysis was performed using an energy spectrometer (EDX) to obtain its atomic composition: pd, 25.5% (atomic fraction, the same below), Ni, 28%, Fe, 26.5%, P, 20%.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (1)
1. A method for preparing a Pd-Ni-Fe-P alloy film by chemical plating-displacement is characterized by comprising the following steps: taking nickel sulfate, ferrous sulfate, sodium hypophosphite, lactic acid and trisodium citrate as chemical plating raw materials, and carrying out chemical plating on a Cu sheet substrate to obtain a Ni-Fe-P alloy plated part; adding anhydrous low-solubility ionic liquid of methylbutyl imidazole chloride BMIMCl, ethylene glycol EG and urea in a molar ratio of 1:1:1 into a displacement reaction vesselPoint mixed solvent, palladium-containing ionic liquid [ BMIM]2PdCl4As a replacement solution, putting the Ni-Fe-P alloy plated part into the replacement solution to be soaked for a period of time, and preparing a Pd-Ni-Fe-P alloy film through a replacement reaction;
palladium-containing ionic liquid [ BMIM ] in displacement liquid]2PdCl48-15g/L, soaking the Ni-Fe-P alloy plating piece in the replacement liquid for 8-12h, keeping the temperature at 50-70 ℃, and controlling the stirring speed at 200-300 rm.
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| CN108786853A (en) * | 2018-06-13 | 2018-11-13 | 天津大学 | Nano-porous catalyst method, nanoporous PdCuNi-S catalyst and purposes are prepared using crystal alloy |
| CN110292942B (en) * | 2019-06-11 | 2022-09-23 | 广东国鸿氢能科技有限公司 | Sodium borohydride hydrolysis hydrogen production catalyst and preparation method thereof |
| CN110548527B (en) * | 2019-07-26 | 2022-08-09 | 青岛科技大学 | Preparation of load type Ni-Fe-P-MnFeO by chemical plating 3 Method of electrocatalyst |
| CN111013621A (en) * | 2019-11-14 | 2020-04-17 | 河南城建学院 | Method for producing transition metal carbonitrides |
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| TWI522492B (en) * | 2014-01-17 | 2016-02-21 | 國立中央大學 | Metal surface treating method |
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| CN105283582A (en) * | 2013-06-13 | 2016-01-27 | 东洋钢钣株式会社 | Palladium plate coated material and production method therefor |
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