CN113445075A - Method for preparing metal single crystal by electrochemical deposition of solid precursor - Google Patents

Method for preparing metal single crystal by electrochemical deposition of solid precursor Download PDF

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CN113445075A
CN113445075A CN202110633724.XA CN202110633724A CN113445075A CN 113445075 A CN113445075 A CN 113445075A CN 202110633724 A CN202110633724 A CN 202110633724A CN 113445075 A CN113445075 A CN 113445075A
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metal
precursor
electrolyte
single crystal
solid
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高海峡
林翌阳
刘敏
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Hunan University of Science and Engineering
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Hunan University of Science and Engineering
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    • 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
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
    • 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
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
    • C25B11/089—Alloys
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/52—Alloys
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • C30B7/12—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by electrolysis

Abstract

The invention belongs to the technical field of chemical synthesis, and particularly relates to a method for preparing metal single crystals by electrochemical deposition of a solid precursor. The method comprises the following steps: (1) selecting a solid precursor or a salt solution of a corresponding metal and an electrolyte solute, wherein the ratio of the molar weight of the corresponding metal solid precursor or the salt solution to the molar weight of the electrolyte solute is 0.0001-0.001, and the electrolyte solute is dissolved by ultrapure water; (2) and adding the metal solid precursor or the salt solution into the electrolyte, and uniformly stirring. The invention can prepare the nano metal single crystal on the electrode in situ by electrochemically depositing metal solid precursor existing in the electrolyte on the electrode in a weak dissolved ion manner.

Description

Method for preparing metal single crystal by electrochemical deposition of solid precursor
Technical Field
The invention belongs to the technical field of chemical synthesis, and particularly relates to a method for preparing metal single crystals by electrochemical deposition of a solid precursor.
Background
Because of its uniform and definite atomic arrangement structure, metal single crystals have become the subject of extensive research in recent years, facilitating the characterization of various chemical reactions and exploring reaction mechanisms.
However, the conventional metal single crystal preparation method usually requires relatively severe conditions to perform small-scale preparation, such as a high-temperature high-pressure hydrothermal reaction method and a chemical vapor deposition method requiring special equipment, which brings great troubles to production and life, and therefore, there is a need to develop a simple and easy metal single crystal preparation method.
The electrochemical deposition is used for preparing the metal simple substance, and the method has the advantages of simplicity, rapidness, easy adjustment of reaction conditions and the like, so that the method is researched and applied on a large scale. However, because the reaction process in the electrochemical deposition process is complex, the method is difficult to obtain the metal single crystal with the single crystal face exposed, and therefore, the research and research on preparing the single crystal by electrochemical deposition are lacked.
Disclosure of Invention
In view of the technical current situation, the invention aims to provide a method for preparing metal single crystals by electrochemical deposition by using solid precursors, which has simple technical route and universality, and the prepared metal single crystals have wide application prospect and can be applied to a series of reactions such as electrocatalytic oxygen reduction, carbon dioxide reduction, nitrogen reduction and the like.
The technical scheme provided by the invention is as follows:
a method for preparing metal single crystal by electrochemical deposition of solid precursor comprises the following steps:
(1) electrolyte solute is selected and dissolved by 100mL of ultrapure water to obtain electrolyte with the molar concentration of 0.1 mol/L;
(2) selecting a precursor corresponding to metal, adding a precursor solid of the metal or a precursor salt solution into the electrolyte to ensure that the molar weight ratio of the precursor of the metal to the solute of the electrolyte is between 0.0001 and 0.001, uniformly stirring, wherein the metal precursor with the molar weight of 0.000001 to 0.00001mol exists in the electrolyte; then preparing the nano metal single crystal on the electrode in situ by an electrochemical deposition technology.
In the method for preparing the metal single crystal by using the solid precursor for electrochemical deposition, the electrolyte solute is any single salt, including but not limited to: potassium carbonate, sodium carbonate, potassium bicarbonate, sodium bicarbonate, potassium chloride, sodium chloride, potassium sulfate, and sodium sulfate.
In the method for preparing the metal single crystal by using the solid precursor for electrochemical deposition, the precursor of the corresponding metal is a granular solid of any metal, including but not limited to: solid particles in which the simple substance, oxide, or hydroxide is insoluble in the electrolyte; or the precursor salt solution of the corresponding metal is one of metal salt and hydrate thereof which can react with the electrolyte solute to generate solid precipitate.
According to the method for preparing the metal single crystal by utilizing the solid precursor to carry out electrochemical deposition, the molar weight of the metal precursor solid dispersed into the electrolyte is 0.000001-0.00001 mol, and the metal precursor salt is dissolved by ultrapure water to obtain the metal precursor salt solution with the molar concentration of 0.00001-0.0001 mol/L.
The method for preparing the metal single crystal by electrochemical deposition by using the solid precursor is characterized in that the electrochemical deposition technology is cyclic voltammetry or linear scanning.
The method for preparing the metal single crystal by electrochemical deposition by utilizing the solid precursor is characterized in that the electrode is a self-supporting carbon electrode or a metal electrode.
The method for preparing the metal single crystal by utilizing the solid precursor to carry out electrochemical deposition is characterized in that the metal single crystal prepared by the method is applied to electrocatalytic oxygen reduction reaction, carbon dioxide reduction reaction or nitrogen reduction reaction.
The design idea of the invention is as follows: by utilizing the dissolution balance of a metal solid precursor in an electrolyte solution and carrying out recombination deposition on trace metal ions in the electrolyte by a simple electrochemical deposition method, the deposited species can preferentially grow a certain crystal face under a proper potential, so that the metal single crystal with an excellent structure is formed.
Experiments prove that the method for preparing the metal single crystal by electrochemical deposition by using the solid precursor has the following characteristics and advantages:
(1) the metal nano single crystal prepared by the invention has a good single crystal structure.
(2) Compared with the reported nano single crystal material prepared in an ex-situ mode, the content of the precursor required by the method is very small, and the burden of industrial application can be reduced.
(3) The preparation method of the metal nanosheet catalyst reported at present is often only suitable for preparing a certain nano single crystal, and the preparation method provided by the invention has universality and can be used for preparing any nano single crystal, such as: copper nano-single crystal, iron nano-single crystal, cobalt nano-single crystal, nickel nano-single crystal, and the like.
(5) The nano single crystal prepared by the method is dispersed on an electrode material and can be applied to various electrochemical catalytic reactions.
Drawings
Fig. 1 to 7 are scanning electron microscope and transmission electron microscope of the copper nano single crystal supported on carbon paper prepared in example 1 of the present invention and diffraction, fourier transform spectra thereof. Wherein:
fig. 1 is a scanning electron microscope image of copper nanoplates grown onto carbon nanofibers;
FIG. 2 is a transmission electron microscope spectrum of a copper nano-single crystal, and an inset in FIG. 2 is a selected electron diffraction spectrum of a corresponding position;
FIG. 3 is a high resolution spectrum of a transmission electron microscope of copper nano-single crystal, and an inset in FIG. 3 is a Fourier variation spectrum of the corresponding position;
FIG. 4 is a local high resolution spectrum of a transmission electron microscope of copper nano-single crystals;
FIG. 5 is a elemental area scan map of a copper nano-single crystal transmission electron microscope;
FIG. 6 is a copper nano-single crystal transmission electron microscope element area scan map (copper element signal);
FIG. 7 is a elemental area scan pattern (elemental carbon signal) of a copper nano-single crystal transmission electron microscope.
Detailed Description
In the specific implementation process, the method for preparing the metal single crystal by electrochemical deposition of the solid precursor comprises the following steps: (1) selecting a solid precursor or a salt solution of a corresponding metal and an electrolyte solute, wherein the ratio of the molar weight of the corresponding metal solid precursor or the salt solution to the molar weight of the electrolyte solute is 0.0001-0.001, and the electrolyte solute is dissolved by ultrapure water; (2) and adding the metal solid precursor or the salt solution into the electrolyte, and uniformly stirring.
The present invention will be described in further detail with reference to the following examples and drawings, which are intended to facilitate the understanding of the present invention and are not intended to limit the present invention in any way.
Example 1:
in this example, the preparation method of the copper nano single crystal is as follows:
firstly, weighing a copper source precursor and an electrolyte solute so that the molar weight ratio of the copper source precursor to the electrolyte solute is 0.0005; dissolving the copper source precursor by ultrapure water to obtain a copper source precursor solution with the molar concentration of 0.00005 mol/L; dissolving electrolyte solute by ultrapure water to obtain electrolyte with the molar concentration of 0.1 mol/L; wherein the copper source precursor is copper nitrate trihydrate, and the electrolyte solute is sodium bicarbonate. And then, titrating the copper source precursor solution into the electrolyte, generating copper hydroxide floccule at the moment, uniformly stirring, and introducing high-purity carbon dioxide gas (with the volume purity of 99.99%) to saturation. Then, a standard three-electrode system H-shaped electrolytic cell is connected, a working electrode is a carbon paper electrode, a counter electrode is a platinum sheet electrode, a reference electrode is an Ag/AgCl electrode, electrochemical deposition is carried out by cyclic voltammetry (or linear scanning method), and a copper nanosheet catalyst with the specification size of 0.09cm is obtained on the carbon paper electrode2. Wherein, the scanning window of the cyclic voltammetry is as follows: 0 to-5V vs. Ag/AgCl, and the scanning window of the linear scanning method is as follows: 0 to-5V vs. Ag/AgCl, and the rates are all 0.0001V/s.
As shown in fig. 1-7, the morphology and transmission electron microscope of the prepared copper nano single crystal and its diffraction and fourier transform spectra form a catalyst with uniform nano single crystal structure on the carbon paper substrate.
As can be seen from fig. 1, copper nanomaterial is uniformly grown on the carbon nanofiber.
As can be seen from FIG. 2, the edge of the nano material is thin, and the selective area electron diffraction pattern shows that the material is a nano single crystal material, and the main crystal face of the material is a copper (111) face.
As can be seen from FIG. 3, the direction of the lattice fringes of the nano-material is uniform, and the Fourier transform spectrum of the selected area of the nano-material shows that the nano-material is a single crystal, and the main crystal face of the nano-material is a (111) face of copper.
As can be seen from fig. 4, the lattice spacing of the nanomaterial is 0.215nm, indicating the (111) plane of copper.
As can be seen from FIG. 5, the material has small size and the length and width are about 5 μm.
As can be seen from fig. 6, the main constituent element of the nanomaterial is copper.
As can be seen from fig. 7, the main constituent element of the nanomaterial is not carbon.
Example 2:
in this example, the preparation method of the copper nano single crystal is as follows:
firstly, weighing a copper source precursor and an electrolyte solute to enable the molar weight ratio of the copper source precursor to the electrolyte solute to be 0.00025; dissolving the copper source precursor by ultrapure water to obtain a copper source precursor solution with the molar concentration of 0.000025 mol/L; dissolving electrolyte solute by ultrapure water to obtain electrolyte with the molar concentration of 0.1 mol/L; wherein the copper source precursor is anhydrous copper sulfate, and the electrolyte solute is potassium bicarbonate. And then, titrating the copper source precursor solution into the electrolyte, generating copper hydroxide floccule at the moment, uniformly stirring, and introducing high-purity carbon dioxide gas (with the volume purity of 99.99%) to saturation. Then, a standard three-electrode system H-shaped electrolytic cell is connected, a working electrode is a carbon paper electrode, a counter electrode is a platinum sheet electrode, a reference electrode is an Ag/AgCl electrode, electrochemical deposition is carried out by cyclic voltammetry (or linear scanning method), and a copper nano single crystal catalyst with the specification size of 0.09cm is obtained on the carbon paper electrode2. Wherein, the scanning window of the cyclic voltammetry is as follows: 0 to-5V vs. Ag/AgCl, and the scanning window of the linear scanning method is as follows: 0 to-5V vs. Ag/AgCl, and the rates are all 0.0001V/s.
The morphology and structure of the obtained copper nano single crystal are similar to those of the copper nano single crystal in example 1.
Example 3:
in this example, the preparation method of the copper nano single crystal is as follows:
firstly, weighing a copper source precursor and an electrolyte solute to enable the molar weight ratio of the copper source precursor to the electrolyte solute to be 0.000125; dissolving the copper source precursor by ultrapure water to obtain a copper source precursor solution with the molar concentration of 0.0000125 mol/L; dissolving electrolyte solute by ultrapure water to obtain electrolyte with the molar concentration of 0.1 mol/L; wherein the copper source precursor is copper chloride, and the electrolyte solute is sodium sulfate. And then, titrating the copper source precursor solution into the electrolyte, generating copper hydroxide floccule at the moment, uniformly stirring, and introducing high-purity carbon dioxide gas (with the volume purity of 99.99%) to saturation. Then, a standard three-electrode system H-shaped electrolytic cell is connected, a working electrode is a carbon paper electrode, a counter electrode is a platinum sheet electrode, a reference electrode is an Ag/AgCl electrode, electrochemical deposition is carried out by cyclic voltammetry (or linear scanning method), and a copper nanosheet catalyst with the specification size of 0.09cm is obtained on the carbon paper electrode2. Wherein, the scanning window of the cyclic voltammetry is as follows: 0 to-5V vs. Ag/AgCl, and the scanning window of the linear scanning method is as follows: 0 to-5V vs. Ag/AgCl, and the rates are all 0.0001V/s.
The morphology and structure of the obtained copper nano single crystal are similar to those of the copper nano single crystal in example 1.
Example 4:
in this example, the preparation method of the copper nano single crystal is as follows:
firstly, weighing copper source precursor solid and electrolyte solute to enable the molar weight ratio of the copper source precursor solid to the electrolyte solute to be 0.00075; dissolving electrolyte solute by ultrapure water to obtain electrolyte with the molar concentration of 0.1 mol/L; wherein the copper source precursor solid is copper hydroxide, and the electrolyte solute is sodium chloride. And then, pouring the copper source precursor solid into the electrolyte, uniformly stirring, and introducing high-purity carbon dioxide gas (with the volume purity of 99.99%) to saturation. Then connecting into a standard three-electrode system H-type electrolytic cell, using carbon paper electrode as working electrode, platinum sheet electrode as counter electrode and Ag/AgCl electrode as reference electrode, performing electrochemical deposition by cyclic voltammetry (or linear scanning method), and obtaining copper nano single crystal with specification size of0.09cm2. Wherein, the scanning window of the cyclic voltammetry is as follows: 0 to-5V vs. Ag/AgCl, and the scanning window of the linear scanning method is as follows: 0 to-5V vs. Ag/AgCl, and the rates are all 0.0001V/s.
The morphology and structure of the obtained copper nano single crystal are similar to those of the copper nano single crystal in example 1.
Example 5:
in this example, the preparation method of the iron nano single crystal is as follows:
firstly, weighing iron source precursor solid and electrolyte solute to enable the molar weight ratio of the iron source precursor solid to the electrolyte solute to be 0.00075; dissolving electrolyte solute by ultrapure water to obtain electrolyte with the molar concentration of 0.1 mol/L; wherein the iron source precursor solid is ferric hydroxide, and the electrolyte solute is sodium chloride. And then, pouring the iron source precursor solid into the electrolyte, uniformly stirring, and introducing high-purity carbon dioxide gas (with the volume purity of 99.99%) to saturation. Then, a standard three-electrode system H-shaped electrolytic cell is connected, a working electrode is a carbon paper electrode, a counter electrode is a platinum sheet electrode, a reference electrode is an Ag/AgCl electrode, electrochemical deposition is carried out by cyclic voltammetry (or linear scanning method), and iron nano single crystals with the specification size of 0.09cm are obtained on the carbon paper electrode2. Wherein, the scanning window of the cyclic voltammetry is as follows: 0 to-5V vs. Ag/AgCl, and the scanning window of the linear scanning method is as follows: 0 to-5V vs. Ag/AgCl, and the rates are all 0.0001V/s.
Example 6:
in this example, the preparation method of the nickel nano single crystal is as follows:
firstly, weighing nickel source precursor solid and electrolyte solute to enable the molar weight ratio of the nickel source precursor solid to the electrolyte solute to be 0.00075; dissolving electrolyte solute by ultrapure water to obtain electrolyte with the molar concentration of 0.1 mol/L; wherein the nickel source precursor solid is nickel hydroxide, and the electrolyte solute is sodium chloride. And then, pouring the nickel source precursor solid into the electrolyte, uniformly stirring, and introducing high-purity carbon dioxide gas (with the volume purity of 99.99%) to saturation. Then, a standard three-electrode system H-type electrolytic cell is connected, the working electrode is a carbon paper electrode, the counter electrode is a platinum sheet electrode, the reference electrode is an Ag/AgCl electrode, and cyclic voltammetry (or linear scanning) is carried out to perform electricityChemical deposition to obtain nanometer nickel monocrystal of 0.09cm size on the carbon paper electrode2. Wherein, the scanning window of the cyclic voltammetry is as follows: 0 to-5V vs. Ag/AgCl, and the scanning window of the linear scanning method is as follows: 0 to-5V vs. Ag/AgCl, and the rates are all 0.0001V/s.
The invention can prepare the nano metal single crystal on the electrode in situ by electrochemically depositing metal solid precursor existing in the electrolyte on the electrode in a weak dissolved ion manner.
The embodiments described above are intended to illustrate the technical solutions of the present invention in detail, and it should be understood that the above-mentioned embodiments are only specific embodiments of the present invention, and are not intended to limit the present invention, and any modification, supplement or similar substitution made within the scope of the principles of the present invention should be included in the protection scope of the present invention.

Claims (7)

1. A method for preparing metal single crystal by electrochemical deposition of solid precursor is characterized by comprising the following steps:
(1) electrolyte solute is selected and dissolved by 100mL of ultrapure water to obtain electrolyte with the molar concentration of 0.1 mol/L;
(2) selecting a precursor corresponding to metal, adding a precursor solid of the metal or a precursor salt solution into the electrolyte to ensure that the molar weight ratio of the precursor of the metal to the solute of the electrolyte is between 0.0001 and 0.001, uniformly stirring, wherein the metal precursor with the molar weight of 0.000001 to 0.00001mol exists in the electrolyte; then preparing the nano metal single crystal on the electrode in situ by an electrochemical deposition technology.
2. A method for preparing a single crystal of metal by electrochemical deposition from a solid precursor as claimed in claim 1 wherein the electrolyte solute is any single salt including but not limited to: potassium carbonate, sodium carbonate, potassium bicarbonate, sodium bicarbonate, potassium chloride, sodium chloride, potassium sulfate, and sodium sulfate.
3. The method of claim 1, wherein the precursor of the corresponding metal is a particulate solid of any metal, including but not limited to: solid particles in which the simple substance, oxide, or hydroxide is insoluble in the electrolyte; or the precursor salt solution of the corresponding metal is one of metal salt and hydrate thereof which can react with the electrolyte solute to generate solid precipitate.
4. The method of claim 1, wherein the metal precursor solid is dispersed in the electrolyte in an amount of 0.000001 to 0.00001mol, and the metal precursor salt is dissolved in ultrapure water to obtain a metal precursor salt solution having a molar concentration of 0.00001 to 0.0001 mol/L.
5. A method for preparing a metal single crystal by electrochemical deposition using a solid precursor as claimed in claim 1, wherein the electrochemical deposition technique is cyclic voltammetry or linear sweep.
6. The method for preparing a metal single crystal by electrochemical deposition using a solid precursor as claimed in claim 1, wherein the electrode is a self-supporting carbon electrode or a metal electrode.
7. The method for preparing a metal single crystal by electrochemical deposition using a solid precursor as claimed in one of claims 1 to 6, wherein the metal single crystal prepared according to the method is applied to an electrocatalytic oxygen reduction reaction, a carbon dioxide reduction reaction or a nitrogen reduction reaction.
CN202110633724.XA 2021-06-07 2021-06-07 Method for preparing metal single crystal by electrochemical deposition of solid precursor Pending CN113445075A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102776565A (en) * 2012-08-20 2012-11-14 上海交通大学 Method for preparing nano-structure single crystal silver
US20150128848A1 (en) * 2013-11-12 2015-05-14 Shanghai Switchdiy Digital Technology Co., Ltd. Method of Preparing Nanostructured Single Crystal Silver
CN112481663A (en) * 2020-12-15 2021-03-12 中南大学深圳研究院 Preparation method of copper nanoflower applied to efficient carbon dioxide reduction reaction to generate ethylene
CN112501662A (en) * 2020-12-15 2021-03-16 中南大学深圳研究院 Preparation method of copper nanosheet applied to efficient carbon dioxide reduction reaction for generating methane

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102776565A (en) * 2012-08-20 2012-11-14 上海交通大学 Method for preparing nano-structure single crystal silver
US20150128848A1 (en) * 2013-11-12 2015-05-14 Shanghai Switchdiy Digital Technology Co., Ltd. Method of Preparing Nanostructured Single Crystal Silver
CN112481663A (en) * 2020-12-15 2021-03-12 中南大学深圳研究院 Preparation method of copper nanoflower applied to efficient carbon dioxide reduction reaction to generate ethylene
CN112501662A (en) * 2020-12-15 2021-03-16 中南大学深圳研究院 Preparation method of copper nanosheet applied to efficient carbon dioxide reduction reaction for generating methane

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Application publication date: 20210928