CN111647881A - Method for growing one-dimensional nano rod-shaped structure material on substrate by using water molten salt method - Google Patents

Method for growing one-dimensional nano rod-shaped structure material on substrate by using water molten salt method Download PDF

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CN111647881A
CN111647881A CN202010314280.9A CN202010314280A CN111647881A CN 111647881 A CN111647881 A CN 111647881A CN 202010314280 A CN202010314280 A CN 202010314280A CN 111647881 A CN111647881 A CN 111647881A
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conical flask
round
putting
bottom conical
deionized water
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雷鸣
黄凯
毕科
郭帅
吴宇峰
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Zibo Zhongci New Material Co ltd
Beijing University of Posts and Telecommunications
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Zibo Zhongci New Material Co ltd
Beijing University of Posts and Telecommunications
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    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/02—Hydrogen or oxygen
    • C25B1/04—Hydrogen or oxygen by electrolysis of water
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

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  • Nanotechnology (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
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  • Inorganic Chemistry (AREA)
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  • Inorganic Compounds Of Heavy Metals (AREA)
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Abstract

The invention relates to a method for growing a one-dimensional nano rod-shaped structure material on a substrate (such as foamed nickel, a steel mesh, a titanium mesh, a molybdenum mesh, carbon fiber cloth and the like) by using a water molten salt method, belonging to the field of material science, engineering technology and chemistry. The metal related to the one-dimensional nano rod-shaped structure material prepared by the invention comprises elements such as Ni, Co, Fe, Mn, Cu, Mo, W, Nb, Ru, Rh, Pd and the like. Firstly, dissolving a certain amount of chemical reagents A and B into a certain amount of deionized water to prepare a reactant solution C with a certain concentration, then soaking a substrate cleaned in advance into the reactant solution C, and then heating for a plurality of hours at a certain temperature to obtain a final product. The method has the advantages of simple operation, high efficiency, wide application range and the like.

Description

Method for growing one-dimensional nano rod-shaped structure material on substrate by using water molten salt method
(2) Field of the invention
The invention relates to a method for growing a one-dimensional nano rod-shaped structure material on a substrate by using a water molten salt method, belonging to the field of material science, engineering technology and chemistry.
(3) Background of the invention
Hydrogen energy is considered one of the cleanest, most promising sustainable energy sources, and electrochemical water splitting is an effective method for large-scale hydrogen production in the prior art. The whole water splitting process comprises two half reactions: a Hydrogen Evolution Reaction (HER) at the cathode and an Oxygen Evolution Reaction (OER) at the anode. Noble metals Pt and IrO2(or RuO)2) Have been identified as the most active electrocatalysts for HER and OER, respectively. However, their high cost, scarcity and poor stability have hindered their large-scale use. Therefore, current research is mainly focused on developing electrocatalysts having high catalytic activity and low cost. To date, the HER properties of phosphides, sulphides, carbides and nitrides of some transition metal compounds, and the OER properties of oxides, nitrides and hydroxides have been reported. However, the catalytic activity of these electrocatalysts needs to be further improved, since most of the above mentioned electrocatalysts cannot be used for bifunctional electrocatalysis of HER and OER in the same electrolyte.
For the preparation of electrodes, most people use binders such as polyvinylidene fluoride (PVDF) and Nafion to attach and fix an electrocatalyst to a current collector for electrochemical performance testing. However, the adhesive hinders the contact of the active site with the electrolyte, resulting in a decrease in electrical conductivity, thereby inhibiting the catalytic performance of the electrocatalyst. In addition, at high current densities, the catalyst on the electrode may be susceptible to delamination, resulting in poor catalytic stability. One key and effective strategy to address these problems is to grow electrocatalysts directly on conductive substrates, such as Carbon Fiber Cloth (CFC) and Nickel Foam (NF) substrates.
Basic salts such as metal carbonate hydroxides and metal nitrate hydroxides have attracted much attention because of their excellent electrocatalytic properties, especially nitrate compounds. Metal nitrate hydroxides have shown great potential in OER performance, but their performance in HER is not very good. From the thermodynamic and kinetic perspectives, the problem of insufficient performance of the nitrate solution in the aspect of HER can be effectively solved by adding a small amount of elements such as high-valence Mo, W, Nb, Ru, Rh, Pd and the like into the nitrate solution, and the OER performance of the nitrate solution is also improved greatly. In addition, metal nitrates generally possess a relatively low melting point and can be converted to nitrate hydroxide by a mild self-decomposition process.
(4) Summary of the invention
1. Objects of the invention
The invention aims to provide a method for growing a one-dimensional nanorod structure material on a substrate by using a water molten salt method. A small amount of high-valence ammonium salt such as Mo, W, Nb, Ru, Rh, Pd and the like is added into nitrate solution of elements such as Ni, Co, Fe, Mn, Cu and the like, and a one-dimensional nano rod-shaped structure material is grown on a substrate such as foamed nickel and the like by a water molten salt method. The material shows excellent electrochemical performance in terms of OER and HER. In addition, the material is found to have stable electrochemical catalytic performance by measuring the time-current and CV curve of the material.
2. The invention of the technology
The key points of the invention are as follows:
(1) preparing a reactant solution A with the mass-volume concentration of 0.1-0.2 g/ml by using a metal nitrate solution and a solvent, pouring the solution into a round-bottom conical flask, wherein the metal nitrate elements are Ni, Co, Fe, Mn and Cu, and the solvent is deionized water.
(2) Adding 0.2-0.3 g of high-valence metal ammonium salt into the solution A, and carrying out ultrasonic treatment on the solution by using an ultrasonic water tank until the solution is in a non-precipitation state, wherein the high-valence metal ammonium salt is Mo, W, Nb, Ru, Rh or Pd.
(3) Putting the round-bottom conical flask into a forced air drier, and heating for 20min at a certain temperature; then putting the cleaned substrate into the round-bottom conical flask, and heating for a certain time at the same temperature, wherein the reaction temperature is 65-125 ℃, and the reaction time is 0.3-10 h.
The method for growing the one-dimensional nano rod-shaped structure material on the substrate by using the water molten salt method has the advantages that: the method has wide application range, can synthesize multi-metal materials such as Ni, Co, Fe, Mn, Cu and the like, is also suitable for various substrates such as foamed nickel, titanium mesh, steel mesh, nickel mesh, carbon fiber cloth and the like, and the synthesized material has firm structure, good heat conductivity and electric conductivity, stable chemical property and simple synthesis process and can be applied to large-scale production.
(5) Attached drawings of the invention
In FIG. 1 a and b are respectively scanning and transmission electron microscope images of the material prepared by the method of the present invention.
(6) Examples of the invention
The following describes embodiments of the method of the invention:
example 1
Preparation of Ni-Mo/NF
Fully mixing nickel nitrate hexahydrate and deionized water to prepare a mixed solution A of 0.167g/ml, pouring the mixed solution A into a round-bottom conical flask, adding a small amount of ammonium molybdate tetrahydrate into the round-bottom conical flask, and putting the conical flask into an ultrasonic water tank for ultrasonic treatment until the solution has no precipitate; then putting the round-bottom conical flask into a forced air drier, heating to 125 ℃, preserving the heat for 20min, putting the cleaned foam nickel with certain size into the round-bottom conical flask, and finally heating for 10h at 125 ℃. And after the reaction is finished, cleaning chemical reagents which do not react on the surface of the foamed nickel by using deionized water, and drying in a vacuum drying oven.
Example 2
Preparation of Ni-W/NF
Firstly, fully mixing nickel nitrate hexahydrate and deionized water to prepare a mixed solution A of 0.167mg/ml, pouring the mixed solution A into a round-bottom conical flask, then adding a small amount of ammonium tungstate into the round-bottom conical flask, and putting the conical flask into an ultrasonic water tank for ultrasonic treatment until the solution has no precipitate; then putting the round-bottom conical flask into a forced air drier, heating to 125 ℃, preserving the heat for 20min, putting the cleaned foam nickel with certain size into the round-bottom conical flask, and finally heating for 10h at 125 ℃. And after the reaction is finished, cleaning chemical reagents which do not react on the surface of the foamed nickel by using deionized water, and drying in a vacuum drying oven.
Example 3
Preparation of Ni-Nb/NF
Firstly, fully mixing nickel nitrate hexahydrate and deionized water to prepare a mixed solution A of 0.167g/ml, pouring the mixed solution A into a round-bottom conical flask, then adding a small amount of ammonium niobate oxalate hydrate into the round-bottom conical flask, and putting the conical flask into an ultrasonic water tank for ultrasonic treatment until the solution has no precipitate; then putting the round-bottom conical flask into a forced air drier, heating to 125 ℃, preserving the heat for 20min, putting the cleaned foam nickel with certain size into the round-bottom conical flask, and finally heating for 10h at 125 ℃. And after the reaction is finished, cleaning chemical reagents which do not react on the surface of the foamed nickel by using deionized water, and drying in a vacuum drying oven.
Example 4
Preparation of Co-Mo/NF
Fully mixing cobalt nitrate hexahydrate and deionized water to prepare a mixed solution A of 0.167mg/ml, pouring the mixed solution A into a round-bottom conical flask, adding a small amount of ammonium molybdate tetrahydrate into the round-bottom conical flask, and putting the conical flask into an ultrasonic water tank for ultrasonic treatment until the solution has no precipitate; then putting the round-bottom conical flask into a forced air drier, heating to 85 ℃, preserving the heat for 20min, putting the cleaned foam nickel with certain size into the round-bottom conical flask, and finally heating for 4h at 85 ℃. And after the reaction is finished, cleaning chemical reagents which do not react on the surface of the foamed nickel by using deionized water, and drying in a vacuum drying oven.
Example 5
Preparation of Co-W/NF
Fully mixing cobalt nitrate hexahydrate and deionized water to prepare a mixed solution A of 0.167mg/ml, pouring the mixed solution A into a round-bottom conical flask, adding a small amount of ammonium tungstate into the round-bottom conical flask, and putting the conical flask into an ultrasonic water tank for ultrasonic treatment until the solution has no precipitate; then putting the round-bottom conical flask into a forced air drier, heating to 85 ℃, preserving the heat for 20min, putting the cleaned foam nickel with certain size into the round-bottom conical flask, and finally heating for 4h at 85 ℃. And after the reaction is finished, cleaning chemical reagents which do not react on the surface of the foamed nickel by using deionized water, and drying in a vacuum drying oven.
Example 6
Preparation of Co-Nb/NF
Fully mixing cobalt nitrate hexahydrate and deionized water to prepare a mixed solution A of 0.167mg/ml, pouring the mixed solution A into a round-bottom conical flask, adding a small amount of ammonium niobate oxalate hydrate into the round-bottom conical flask, and putting the conical flask into an ultrasonic water tank for ultrasonic treatment until the solution has no precipitate; then putting the round-bottom conical flask into a forced air drier, heating to 85 ℃, preserving the heat for 20min, putting the cleaned foam nickel with certain size into the round-bottom conical flask, and finally heating for 4h at 85 ℃. And after the reaction is finished, cleaning chemical reagents which do not react on the surface of the foamed nickel by using deionized water, and drying in a vacuum drying oven.
Example 7
Preparation of Mn-Mo/NF
Fully mixing manganese nitrate hexahydrate and deionized water to prepare a mixed solution A of 0.167mg/ml, pouring the mixed solution A into a round-bottom conical flask, adding a small amount of ammonium molybdate tetrahydrate into the round-bottom conical flask, and putting the conical flask into an ultrasonic water tank for ultrasonic treatment until the solution has no precipitate; then putting the round-bottom conical flask into a forced air drier, heating to 65 ℃, preserving the heat for 20min, then putting the cleaned foam nickel with certain size into the round-bottom conical flask, and finally heating for 2h at the temperature of 65 ℃. And after the reaction is finished, cleaning chemical reagents which do not react on the surface of the foamed nickel by using deionized water, and drying in a vacuum drying oven.
Example 8
Preparation of Mn-W/NF
Fully mixing manganese nitrate hexahydrate and deionized water to prepare a mixed solution A of 0.167mg/ml, pouring the mixed solution A into a round-bottom conical flask, adding a small amount of ammonium tungstate into the round-bottom conical flask, and putting the conical flask into an ultrasonic water tank for ultrasonic treatment until the solution has no precipitate; then putting the round-bottom conical flask into a forced air drier, heating to 65 ℃, preserving the heat for 20min, then putting the cleaned foam nickel with certain size into the round-bottom conical flask, and finally heating for 2h at the temperature of 65 ℃. And after the reaction is finished, cleaning chemical reagents which do not react on the surface of the foamed nickel by using deionized water, and drying in a vacuum drying oven.
Example 9
Preparation of Mn-Nb/NF
Fully mixing manganese nitrate hexahydrate and deionized water to prepare a mixed solution A of 0.167mg/ml, pouring the mixed solution A into a round-bottom conical flask, adding a small amount of ammonium niobate oxalate hydrate into the round-bottom conical flask, and putting the conical flask into an ultrasonic water tank for ultrasonic treatment until the solution has no precipitate; then putting the round-bottom conical flask into a forced air drier, heating to 65 ℃, preserving the heat for 20min, then putting the cleaned foam nickel with certain size into the round-bottom conical flask, and finally heating for 2h at the temperature of 65 ℃. And after the reaction is finished, cleaning chemical reagents which do not react on the surface of the foamed nickel by using deionized water, and drying in a vacuum drying oven.
Example 10
Preparation of Fe-Mo/NF
Fully mixing ferric nitrate nonahydrate and deionized water to prepare a mixed solution A of 0.167mg/ml, pouring the mixed solution A into a round-bottom conical flask, adding a small amount of ammonium molybdate tetrahydrate into the round-bottom conical flask, and putting the conical flask into an ultrasonic water tank for ultrasonic treatment until the solution has no precipitate; then putting the round-bottom conical flask into a forced air drier, heating to 110 ℃, preserving the heat for 20min, then putting the cleaned foam nickel with certain size into the round-bottom conical flask, and finally heating for 4h at 110 ℃. And after the reaction is finished, cleaning chemical reagents which do not react on the surface of the foamed nickel by using deionized water, and drying in a vacuum drying oven.
Example 11
Preparation of Fe-W/NF
Firstly, fully mixing ferric nitrate and deionized water to prepare a mixed solution A of 0.167mg/ml, pouring the mixed solution A into a round-bottom conical flask, then adding a small amount of ammonium tungstate into the round-bottom conical flask, and putting the conical flask into an ultrasonic water tank for ultrasonic treatment until the solution has no precipitate; then putting the round-bottom conical flask into a forced air drier, heating to 110 ℃, preserving the heat for 20min, then putting the cleaned foam nickel with certain size into the round-bottom conical flask, and finally heating for 4h at 110 ℃. And after the reaction is finished, cleaning chemical reagents which do not react on the surface of the foamed nickel by using deionized water, and drying in a vacuum drying oven.
Example 12
Preparation of Fe-Nb/NF
Firstly, fully mixing ferric nitrate and deionized water to prepare a mixed solution A of 0.167mg/ml, pouring the mixed solution A into a round-bottom conical flask, then adding a small amount of ammonium niobate oxalate hydrate into the round-bottom conical flask, and putting the conical flask into an ultrasonic water tank for ultrasonic treatment until the solution has no precipitate; then putting the round-bottom conical flask into a forced air drier, heating to 110 ℃, preserving the heat for 20min, then putting the cleaned foam nickel with certain size into the round-bottom conical flask, and finally heating for 4h at 110 ℃. And after the reaction is finished, cleaning chemical reagents which do not react on the surface of the foamed nickel by using deionized water, and drying in a vacuum drying oven.
Example 13
Preparation of Cu-Mo/NF
Fully mixing copper nitrate trihydrate and deionized water to prepare a mixed solution A of 0.167mg/ml, pouring the mixed solution A into a round-bottom conical flask, adding a small amount of ammonium molybdate tetrahydrate into the round-bottom conical flask, and putting the conical flask into an ultrasonic water tank for ultrasonic treatment until the solution has no precipitate; then putting the round-bottom conical flask into a forced air drier, heating to 140 ℃, preserving the heat for 20min, putting the cleaned foam nickel with certain size into the round-bottom conical flask, and finally heating for 30min at 140 ℃. And after the reaction is finished, cleaning chemical reagents which do not react on the surface of the foamed nickel by using deionized water, and drying in a vacuum drying oven.
Example 14
Preparation of Cu-W/NF
Fully mixing copper nitrate trihydrate and deionized water to prepare a mixed solution A of 0.167mg/ml, pouring the mixed solution A into a round-bottom conical flask, adding a small amount of ammonium tungstate into the round-bottom conical flask, and putting the conical flask into an ultrasonic water tank for ultrasonic treatment until the solution has no precipitate; then putting the round-bottom conical flask into a forced air drier, heating to 140 ℃, preserving the heat for 20min, putting the cleaned foam nickel with certain size into the round-bottom conical flask, and finally heating for 30min at 140 ℃. And after the reaction is finished, cleaning chemical reagents which do not react on the surface of the foamed nickel by using deionized water, and drying in a vacuum drying oven.
Example 15
Preparation of Cu-Nb/NF
Firstly, fully mixing copper nitrate trihydrate and deionized water to prepare a mixed solution A of 0.167mg/ml, pouring the mixed solution A into a round-bottom conical flask, then adding a small amount of ammonium niobate oxalate hydrate into the round-bottom conical flask, and putting the conical flask into an ultrasonic water tank for ultrasonic treatment until the solution has no precipitate; then putting the round-bottom conical flask into a forced air drier, heating to 140 ℃, preserving the heat for 20min, putting the cleaned foam nickel with certain size into the round-bottom conical flask, and finally heating for 30min at 140 ℃. And after the reaction is finished, cleaning chemical reagents which do not react on the surface of the foamed nickel by using deionized water, and drying in a vacuum drying oven.

Claims (1)

1. The invention relates to a method for growing a one-dimensional nano rod-shaped structure material on a substrate (foamed nickel, steel mesh, titanium mesh, molybdenum mesh, carbon fiber cloth and the like) by using a water molten salt method, which is characterized by comprising the following steps of:
(1) respectively cleaning substrates such as foamed nickel and the like by using acetone, alcohol, diluted hydrochloric acid and deionized water, and removing impurities such as grease, oxides and the like on the surfaces of the substrates;
(2) dissolving a certain amount of nitrate chemical reagent A into deionized water, then adding a small amount of chemical reagent B into the solution, uniformly stirring, and finally transferring the solution into a round-bottom conical flask;
(3) putting the substrate such as the foam nickel prepared in advance in the step (1) into the solution (2), then putting the round-bottom conical flask into a blast drying oven, heating for tens of hours under a certain temperature condition, and after the reaction is finished, performing ultrasonic treatment for 1min by using deionized water and cleaning.
CN202010314280.9A 2020-04-20 2020-04-20 Method for growing one-dimensional nano rod-shaped structure material on substrate by using water molten salt method Pending CN111647881A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108385131A (en) * 2018-02-23 2018-08-10 苏州工业职业技术学院 Ferroelectricity composite Cu2O visible light photolysis water hydrogen photocathodes and preparation method thereof
US20190312283A1 (en) * 2018-04-09 2019-10-10 Nanotek Instruments, Inc. Alkali metal-selenium secondary battery containing a graphene foam-protected selenium cathode

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108385131A (en) * 2018-02-23 2018-08-10 苏州工业职业技术学院 Ferroelectricity composite Cu2O visible light photolysis water hydrogen photocathodes and preparation method thereof
US20190312283A1 (en) * 2018-04-09 2019-10-10 Nanotek Instruments, Inc. Alkali metal-selenium secondary battery containing a graphene foam-protected selenium cathode

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
JUNRAN JIA等: "Nickel Molybdenum Nitride Nanorods Grown on Ni Foam as Efficient and Stable Bifunctional Electrocatalysts for Overall Water Splitting", 《ACS APPLIED MATERIALS & INTERFACES》 *

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