CN110983426A - Interface rapid and controllable preparation method of cuprous bromide nanocrystal material regulated and controlled by nickel ions and solvent - Google Patents

Interface rapid and controllable preparation method of cuprous bromide nanocrystal material regulated and controlled by nickel ions and solvent Download PDF

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Publication number
CN110983426A
CN110983426A CN201910448314.0A CN201910448314A CN110983426A CN 110983426 A CN110983426 A CN 110983426A CN 201910448314 A CN201910448314 A CN 201910448314A CN 110983426 A CN110983426 A CN 110983426A
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copper
solvent
copper foil
bromide solution
bromide
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苗中正
黄一麒
吴昊
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Yancheng Teachers University
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Yancheng Teachers University
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    • 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
    • C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
    • 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
    • C30B29/12—Halides

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemically Coating (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)

Abstract

The invention provides a method for preparing a cuprous bromide nanocrystal material interface by regulating and controlling nickel ions and a solvent. And (3) adopting the liquid which is easy to volatilize as a solvent of the copper bromide solution, adding nickel chloride into the copper bromide solution as a regulating agent, and uniformly coating the copper bromide solution on the surface of the copper foil for spontaneous reaction to prepare the cuprous bromide crystal material. According to the method disclosed by the invention, the cuprous bromide crystals with amorphous, polyhedral, cake-shaped and sheet-shaped structures are directly prepared on the copper foil substrate by adding nickel ions and adjusting the types of solvents, so that the quick preparation of the cuprous bromide crystal material is realized, the reaction time is greatly reduced, the reaction process is not limited in a solution any more, the field of the cuprous bromide preparation method is expanded, reaction additives are reduced, and the method has the characteristics of simplicity in preparation, low cost and easiness in industrial batch production.

Description

Interface rapid and controllable preparation method of cuprous bromide nanocrystal material regulated and controlled by nickel ions and solvent
Technical Field
The invention relates to the field of preparation of cuprous bromide crystal materials, in particular to a method for quickly and controllably preparing an interface of a cuprous bromide nanocrystal material regulated and controlled by nickel ions and a solvent.
Background
Cuprous bromide is an inorganic halide and is widely used in chemical industry, metallurgical industry, pharmaceutical chemical industry, pesticide engineering and the like. The existing preparation method of the cuprous bromide crystal material mainly reduces divalent copper ions. For example, mixing copper sulfate and potassium bromide solution, introducing sulfur dioxide gas for reaction, controlling the temperature to be 40-60 ℃, and reactingThe substance is washed, filtered and dried to obtain cuprous bromide. Another method for preparing cuprous bromide is to add ketone sulfate, copper powder, sodium bromide, concentrated sulfuric acid and water into a reflux device, and heat and reflux to prepare cuprous bromide crystals. In addition, it has been reported that a hydrothermal reduction method is used to prepare cuprous bromide crystals, a mixed solution is prepared from a water-soluble divalent copper salt and a water-soluble bromide with a certain concentration, the mixed solution is left to stand, insoluble impurities are filtered off, and the H content of the mixed solution is adjusted by using a corresponding acid+And (3) transferring the feed liquid into a pressure-resistant corrosion-resistant reaction kettle, then, metering and adding a reducing agent, and carrying out hydrothermal reaction to obtain cuprous bromide crystals. The reaction process of the preparation method usually needs heating and must be generated in solution, the reaction time is long, the raw material cost is high, the mother liquor contains sulfuric acid with strong corrosiveness, and concentrated water containing substances such as acid, sodium bromide, iron and the like is often left to cause the defects of environmental pollution and the like.
Disclosure of Invention
The method for preparing the cuprous bromide nanocrystal material by controlling the interface of the cuprous bromide nanocrystal material by the nickel ions and the solvent is provided, the cuprous bromide crystal is directly prepared on the copper foil substrate by controlling the type of the solvent, the addition amount of the solution and the concentration of the nickel ions, the reaction time is greatly reduced, the cost is low, the process is simple, and the shape and the size of the crystal are controllable.
The invention adopts the following technical scheme:
a method for preparing a cuprous bromide nanocrystal material interface by nickel ion and solvent regulation and control quickly and controllably comprises the following steps:
(1) adopting a volatile liquid as a solvent of a copper bromide solution to obtain a copper bromide solution with a certain concentration range, and adding nickel chloride as a regulating agent into the copper bromide solution;
(2) coating the copper bromide solution containing nickel ions on the surface of the copper foil, controlling the addition amount of the copper bromide solution, and placing the copper foil at a certain range of temperature to enable the reaction to rapidly occur.
The solvent in step (1) may be water, ethanol, propanol, dichloromethane, gasoline, butanol, acetone, diethyl ether, acetaldehyde, petroleum ether and their mixture solution, preferably ethanol, water or their mixture solution.
The copper bromide solution in a certain concentration range in the step (1) means that the concentration of the copper bromide is controlled within the saturation solubility of the copper bromide in each solvent, liquid which is easy to volatilize is used as the solvent of the copper bromide solution, the preferred temperature is 0-20 ℃, and the preferred concentration range is 0.01-1 mol/L.
The adding amount of the nickel chloride in the step (1) is in the range of 0.01-10% of the molar concentration of the copper bromide solution.
The method for coating the copper foil surface with the copper bromide solution in the step (2) is suitable for various methods such as drop coating, wire bar coating method, spraying and the like, and the preferable method is the wire bar coating method.
The copper foil in the step (2) is suitable for various copper foil materials, and preferably the copper foil is subjected to surface polishing treatment.
The adding amount of the copper bromide solution in the step (2) is determined according to the ambient temperature and the coating area, the preferable temperature is 0-20 ℃, and the adding amount of the copper bromide solution is 0.5L/m2。
And (3) placing the copper foil in a certain range of temperature to enable the reaction to rapidly occur, wherein the preferable temperature is 0-80 ℃, and the preferable time is 0.1-600 s.
The invention has the following advantages:
(1) the invention provides a method for preparing a cuprous bromide nanocrystal material by regulating nickel ions and a solvent, which is characterized in that cuprous bromide crystals are directly prepared on a copper foil substrate by regulating the types of the nickel ions and the solvent, so that the cuprous bromide nanocrystal material is quickly prepared, the reaction time is greatly shortened, the reaction process is not limited in a solution, the field of a cuprous bromide preparation method is expanded, reaction additives are reduced, and the method has the characteristics of simple preparation, low cost and easiness in industrial batch production.
(2) The cuprous bromide crystal material prepared by the method has the advantages of uniform granularity, stable performance, controllable appearance, controllable size and the like, and continuous or dispersed cuprous bromide crystals are directly prepared on the copper foil and have amorphous, polyhedral, cake-shaped and flaky structures.
Drawings
FIG. 1 is a scanning electron micrograph of cuprous bromide crystals prepared in example 1 using water as solvent. The concentration of the copper bromide solution is 0.5mol/L, the size of cuprous bromide crystal is 3-10 mu m, and the copper bromide solution has an amorphous structure.
FIG. 2 is a scanning electron micrograph of cuprous bromide crystals prepared in example 2 using water and ethanol as solvents. The volume ratio of water to ethanol is 1: 1, the concentration of the copper bromide solution is 0.5mol/L, the size of cuprous bromide crystals is 500mm-3 mu m, and the cuprous bromide crystal structure is amorphous and polyhedral.
FIG. 3 is a scanning electron micrograph of cuprous bromide crystalline material prepared by ethanol as solvent in example 3. The concentration of the copper bromide solution is 0.5mol/L, the size of the cuprous bromide crystal is 100nm-1 mu m, and the copper bromide crystal has a polyhedral structure.
FIG. 4 is a scanning electron micrograph of cuprous bromide crystalline material prepared by using water and ethanol as solvents and adding nickel chloride in example 4. The concentration of the copper bromide solution is 0.5mol/L, and Ni is in the solution2+And Cu2+The concentration ratio is 0.01: 1, the size of cuprous bromide crystal is 200nm-2 μm, and the cuprous bromide crystal has a cake-shaped and sheet-shaped structure.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the purpose of facilitating understanding of the present invention and should not be construed as specifically limiting the present invention.
Example 1
(1) Selecting a copper foil with the thickness of 25um, wherein one surface or two surfaces of the copper foil are polished planes, cleaning the surface of the copper foil by deionized water, and then drying the copper foil in an environment at 60 ℃ for later use.
(2) Adding copper bromide dihydrate powder into deionized water, stirring for 2 minutes, and preparing a copper bromide aqueous solution with the concentration of 0.5 mol/L.
(3) The polished surface of the copper foil was coated with an aqueous solution of copper bromide at a concentration of 0.5mol/L to form a uniform continuous liquid film.
(4) And (3) rapidly placing the copper foil bearing the copper bromide aqueous solution in an oven at the temperature of 60 ℃ for drying treatment for 5 min.
(5) And (3) cleaning the cuprous bromide crystal film on the surface of the copper foil by using absolute ethyl alcohol, and drying and storing.
Example 2
(1) Selecting a copper foil with the thickness of 25um, wherein one surface or two surfaces of the copper foil are polished planes, cleaning the surface of the copper foil by deionized water, and then drying the copper foil in an environment at 60 ℃ for later use.
(2) Adding copper bromide dihydrate powder into a mixed solvent of deionized water and ethanol, stirring for 2 minutes, and preparing a copper bromide solution with the concentration of 0.5 mol/L.
(3) The copper bromide solution with the concentration of 0.5mol/L is coated on the polished surface of the copper foil to form a uniform and continuous liquid film.
(4) And quickly placing the copper foil bearing the copper bromide solution in an oven with the temperature of 60 ℃ for drying treatment for 5 min.
(5) And (3) cleaning the cuprous bromide crystal film on the surface of the copper foil by using absolute ethyl alcohol, and drying and storing.
Example 3
(1) Selecting a copper foil with the thickness of 25um, wherein one surface or two surfaces of the copper foil are polished planes, cleaning the surface of the copper foil by deionized water, and then drying the copper foil in an environment at 60 ℃ for later use.
(2) Adding copper bromide dihydrate powder into an ethanol solvent, stirring for 2 minutes, and preparing a copper bromide solution with the concentration of 0.5 mol/L.
(3) The copper bromide solution with the concentration of 0.5mol/L is coated on the polished surface of the copper foil to form a uniform and continuous liquid film.
(4) And quickly placing the copper foil bearing the copper bromide solution in an oven with the temperature of 60 ℃ for drying treatment for 5 min.
(5) And (3) cleaning the cuprous bromide crystal film on the surface of the copper foil by using absolute ethyl alcohol, and drying and storing.
Example 4
(1) Selecting a copper foil with the thickness of 25um, wherein one surface or two surfaces of the copper foil are polished planes, cleaning the surface of the copper foil by deionized water, and then drying the copper foil in an environment at 60 ℃ for later use.
(2) Adding copper bromide dihydrate powder to removeStirring for 2 min to obtain copper bromide solution with concentration of 0.5mol/L, adding nickel chloride powder to obtain Ni2+And Cu2+The concentration ratio is 0.01: 1.
(3) The copper bromide solution with the concentration of 0.5mol/L is coated on the polished surface of the copper foil to form a uniform and continuous liquid film.
(4) And quickly placing the copper foil bearing the copper bromide solution in an oven with the temperature of 60 ℃ for drying treatment for 5 min.
(5) And (3) cleaning the cuprous bromide crystal film on the surface of the copper foil by using absolute ethyl alcohol, and drying and storing.
The applicant states that the present invention is illustrated by the above examples to show the detailed process equipment and process flow of the present invention, but the present invention is not limited to the above detailed process equipment and process flow, i.e. it does not mean that the present invention must rely on the above detailed process equipment and process flow to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.

Claims (5)

1. A method for preparing a cuprous bromide nanocrystal material interface by nickel ion and solvent regulation and control quickly and controllably comprises the following steps:
(1) adopting a volatile liquid as a solvent of a copper bromide solution to obtain a copper bromide solution with the concentration range of 0.01-1 mol/L, adding nickel chloride into the copper bromide solution as a regulating agent, wherein the molar concentration of the nickel chloride is 0.01-10% of that of the copper bromide solution;
(2) coating a copper bromide solution containing nickel ions on the surface of the copper foil at the temperature of 0-20 ℃, wherein the addition amount of the copper bromide solution is 0.5L/m2The reaction is fast, the reaction temperature is 0-80 ℃, and the reaction time is 0.1-600 s.
2. The method according to claim 1, wherein the solvent in the step (1) is water, ethanol, propanol, dichloromethane, gasoline, butanol, acetone, diethyl ether, acetaldehyde, petroleum ether or a mixture thereof.
3. The method according to claim 1, wherein the concentration of the copper bromide solution in the step (1) is within a saturation solubility of the copper bromide in the solvent.
4. The method for preparing a copper foil according to claim 1, wherein the method for applying the copper bromide solution to the surface of the copper foil in the step (2) is suitable for a drop coating method, a wire bar coating method, a spray coating method.
5. The production method according to claim 1, wherein the copper foil in the step (2) is applied to a copper foil subjected to surface polishing treatment.
CN201910448314.0A 2019-05-21 2019-05-21 Interface rapid and controllable preparation method of cuprous bromide nanocrystal material regulated and controlled by nickel ions and solvent Withdrawn CN110983426A (en)

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