CN113481552B - Preparation method of copper dendrite - Google Patents
Preparation method of copper dendrite Download PDFInfo
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- CN113481552B CN113481552B CN202110796849.4A CN202110796849A CN113481552B CN 113481552 B CN113481552 B CN 113481552B CN 202110796849 A CN202110796849 A CN 202110796849A CN 113481552 B CN113481552 B CN 113481552B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/60—Electroplating characterised by the structure or texture of the layers
- C25D5/605—Surface topography of the layers, e.g. rough, dendritic or nodular layers
Abstract
The invention discloses a preparation method of copper dendrite, which comprises the following steps: step S1: selecting a straightened metal wire as an anode metal wire, and bending the metal wire into closed rings with different shapes as a cathode ring; step S2: preparing an electrolytic reaction tank, preparing an acid electrolyte by using copper salt, and pouring the acid electrolyte into the reaction tank; step S3: placing the cathode ring at the bottom of the reaction tank, vertically inserting the anode metal wire into the reaction tank opposite to the geometric center of the cathode ring, and keeping a spacing distance between the bottom of the reaction tank and the cathode ring; step S4: and applying voltage, heating in a water bath to maintain the temperature of the electrolyte at 50-60 ℃, reacting for 5-10 min, and preparing a layer of copper dendrite on the surface of the cathode ring. The invention provides a controllable synthesis technical means for obtaining copper dendrites with different shapes and composition units (including square blocks, scaly blocks, long strips and nodular blocks) by designing closed cathode rings with different shapes (including circles, squares, regular triangles and rhombuses).
Description
Technical Field
The invention relates to the technical field of metal nano materials, in particular to a preparation method of copper dendrite.
Background
The anti-wetting property, namely the hydrophobicity, is an important property of a solid surface, the surface has super-hydrophobicity, namely the contact angle of the surface and water is large by 150 degrees, and the super-hydrophobic material has the advantages of self-cleaning, oil-water separation, corrosion resistance and the like. In recent years, research on superhydrophobic materials has entered a new stage, and people begin to modify low surface energy substances or construct rough structures on the surfaces to prepare biomimetic micro-nano materials with superhydrophobic properties. The copper material is low in price and has good flexibility and thermoelectric characteristics, but the surface of copper is easy to corrode, and the copper dendrite has high-density corners and edges and a large specific surface area, so that the construction of the copper dendrite is of great significance and is paid attention to in the field of super-hydrophobicity.
At present, related researches on copper dendrites are few, reported preparation methods mainly include electrochemical deposition, chemical vapor deposition, plasma etching, a template method and the like, electrodeposition is a popular method, but in electrodeposition preparation, only one common dendrite with a single composition unit morphology can be obtained usually, and meanwhile, due to violent reaction of aqueous electrolyte, the copper dendrites with uniform and good synthetic morphology are difficult to control. Therefore, a simple preparation method of copper dendrites is urgently needed, different regular composition units can be synthesized, the copper dendrites with various morphologies can be obtained, and the copper dendrites have the advantages of uniformity and good morphology.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of copper dendrites, which synthesizes the copper dendrites with regular composition units (including square blocks, scaly shapes, long strips and nodular shapes) with different shapes by designing closed cathode rings (including circles, squares, triangles and diamonds) with different shapes and adopting a metal wire as an anode for electrodeposition.
In order to solve the technical problem, the invention provides a preparation method of copper dendrite, which is characterized by comprising the following steps: the method comprises the following steps:
s1: selecting a metal wire as an electrode material, polishing, cleaning and drying, selecting a straightened metal wire as an anode metal wire, and bending the metal wire into closed rings with different shapes as a cathode ring;
s2: preparing an electrolytic reaction tank, preparing an acid electrolyte by using copper salt, and pouring the acid electrolyte into the reaction tank;
s3: placing a cathode ring at the bottom of a reaction tank, vertically inserting an anode metal wire into the reaction tank opposite to the geometric center of the cathode ring, keeping a spacing distance between the bottom of the reaction tank and the cathode ring, and respectively connecting the cathode ring and the anode metal wire with the negative electrode and the positive electrode of a low-voltage direct-current power supply;
s4: and applying voltage, heating in a water bath to maintain the temperature of the electrolyte at 50-60 ℃, reacting for 5-10 min, and preparing a layer of copper dendrite on the surface of the cathode ring.
Preferably, the wire size is selected from: the diameter is 1-2 mm, and the material is selected from red copper and brass.
Further, the anode wire size is selected as: the length of the glass is 1-3 cm.
Furthermore, the shape of the cathode ring is selected from a circle, a square, a regular triangle and a rhombus, and the sizes are correspondingly as follows: the diameter is 1-2 cm, the side length is 1-2 cm, and the side length is 1-2 cm.
Further, the copper salt in the copper salt electrolyte is CuCl2、CuSO4Or Cu (NO)3)2One or more of, Cu2+The concentration is selected to be 0.2-0.4 mol/L.
Furthermore, the distance between the bottom of the anode metal wire and the cathode ring is 3-6 mm; the applied voltage is 15-20V.
The invention has the following advantages and beneficial effects:
the invention provides a technical means for obtaining copper dendrites with different morphologies and composition units by adopting a metal wire as an electrode material in electrodeposition preparation and further changing the shape of a closed ring of the metal wire to serve as a cathode. The invention designs the method for processing the metal wire to obtain the closed cathode rings (including circles, squares, regular triangles and rhombuses) with various shapes, and then correspondingly obtains copper dendrites (including scales, squares, long strips and bone nodes) with different shapes on the surface of the cathode ring, thereby obtaining unexpected effects. Compared with other common preparation methods of common copper dendrites with the most strip-shaped form particles, the method has the controllable synthesis effect of the form units with various regular forms, and the obtained copper dendrites are composed of uniform units, have large specific surface area and good form, and can be applied to the fields of super-hydrophobic materials, superconducting materials and the like.
Drawings
FIG. 1 is a scanning electron micrograph of a copper dendrite having a scaly constituent unit prepared in example 1 of the present invention;
FIG. 2 is a scanning electron micrograph of a copper dendrite having a square-shaped constituent unit prepared in example 2 of the present invention;
FIG. 3 is a scanning electron micrograph of copper dendrites having elongated constituent elements prepared according to example 3 of the present invention;
FIG. 4 is a scanning electron micrograph of a copper dendrite having nodular elements prepared according to example 4 of the present invention;
FIG. 5 is a scanning electron micrograph of copper dendrites having spheroidal constituent units prepared according to comparative example 1 of the present invention;
FIG. 6 is a scanning electron micrograph of copper dendrites having spheroidal constituent units prepared according to comparative example 2 of the present invention;
fig. 7 is a scanning electron micrograph of a general copper particle prepared in comparative example 3 of the present invention.
Detailed Description
Example 1
The invention discloses a preparation method of copper dendrite, which comprises the following steps:
step S1: selecting a metal wire as an electrode material, polishing, cleaning and drying, selecting a straightened metal wire as an anode metal wire, and bending the metal wire into closed rings with different shapes as a cathode ring;
step S2: preparing an electrolytic reaction tank, preparing an acid electrolyte by using copper salt, and pouring the acid electrolyte into the reaction tank;
step S3: placing a cathode ring at the bottom of a reaction tank, vertically inserting an anode metal wire into the reaction tank opposite to the geometric center of the cathode ring, keeping a spacing distance between the bottom of the reaction tank and the cathode ring, and respectively connecting the cathode ring and the anode metal wire with the negative electrode and the positive electrode of a low-voltage direct-current power supply;
step S4: applying voltage, heating in water bath to maintain the electrolyte at 55 deg.c, and reacting for 7min to prepare one layer of copper dendrite on the surface of the cathode ring.
Wherein, the wire size is selected as: the diameter is 1-2 mm, and the material is red copper; the anode wire size is selected as follows: the length is 2 cm; the shape of the cathode ring is selected to be circular, and the sizes are correspondingly as follows: diameter 1.5 cm; the copper salt in the copper salt electrolyte is CuSO4，Cu2+The concentration is selected to be 0.3 mol/L; the distance between the bottom of the anode metal wire and the cathode ring is 4 mm; the applied voltage was 18V.
As shown in fig. 1, which is a scanning electron micrograph of the copper dendrite having a scale-like constituent unit prepared by the circular closed cathode ring of example 1, it can be seen that the copper dendrite is composed of copper particles having a uniform scale shape.
Example 2
The invention discloses a preparation method of copper dendrite, which comprises the following steps:
step S1: selecting a metal wire as an electrode material, polishing, cleaning and drying, selecting a straightened metal wire as an anode metal wire, and bending the metal wire into closed rings with different shapes as a cathode ring;
step S2: preparing an electrolytic reaction tank, preparing an acid electrolyte by using copper salt, and pouring the acid electrolyte into the reaction tank;
step S3: placing a cathode ring at the bottom of a reaction tank, vertically inserting an anode metal wire into the reaction tank opposite to the geometric center of the cathode ring, keeping a spacing distance between the bottom of the reaction tank and the cathode ring, and respectively connecting the cathode ring and the anode metal wire with the negative electrode and the positive electrode of a low-voltage direct-current power supply;
step S4: applying voltage, heating in water bath to maintain the electrolyte at 55 deg.c, and reacting for 7min to prepare one layer of copper dendrite on the surface of the cathode ring.
Wherein, the wire size is selected as: the diameter is 1-2 mm, and the material is red copper; the anode wire size is selected as follows: the length is 2 cm; the shape of the cathode ring is selected to be square, and the corresponding sizes are as follows: the side length is 1.5 cm; the copper salt in the copper salt electrolyte is CuSO4，Cu2+The concentration is selected to be 0.3 mol/L; the distance between the bottom of the anode metal wire and the cathode ring is 4 mm; the applied voltage was 18V.
As shown in fig. 2, which is a scanning electron micrograph of copper dendrites having a square-shaped constituent unit prepared by square closed cathode rings of example 2, it can be seen that the copper dendrites are composed of copper particles having a uniform square shape.
Example 3
The invention discloses a preparation method of copper dendrite, which comprises the following steps:
step S1: selecting a metal wire as an electrode material, polishing, cleaning and drying, selecting a straightened metal wire as an anode metal wire, and bending the metal wire into closed rings with different shapes as a cathode ring;
step S2: preparing an electrolytic reaction tank, preparing an acid electrolyte by using copper salt, and pouring the acid electrolyte into the reaction tank;
step S3: placing a cathode ring at the bottom of a reaction tank, vertically inserting an anode metal wire into the reaction tank opposite to the geometric center of the cathode ring, keeping a spacing distance between the bottom of the reaction tank and the cathode ring, and respectively connecting the cathode ring and the anode metal wire with the negative electrode and the positive electrode of a low-voltage direct-current power supply;
step S4: applying voltage, heating in water bath to maintain the electrolyte at 55 deg.c, and reacting for 7min to prepare one layer of copper dendrite on the surface of the cathode ring.
Wherein, the wire size is selected as: the diameter is 1-2 mm, and the material is red copper; the anode wire size is selected as follows: the length is 2 cm; the shape of the cathode ring is selected to be a regular triangle, and the corresponding sizes are as follows: the side length is 1.5 cm; the copper salt in the copper salt electrolyte is CuSO4，Cu2+The concentration is selected to be 0.3 mol/L; the distance between the bottom of the anode metal wire and the cathode ring is 4 mm; the applied voltage was 18V.
As shown in fig. 3, which is a scanning electron micrograph of copper dendrites having elongated constituent cells prepared by the regular triangular closed cathode ring of example 3, it can be seen that the copper dendrites are composed of uniform elongated copper particles.
Example 4
The invention discloses a preparation method of copper dendrite, which comprises the following steps:
step S1: selecting a metal wire as an electrode material, polishing, cleaning and drying, selecting a straightened metal wire as an anode metal wire, and bending the metal wire into closed rings with different shapes as a cathode ring;
step S2: preparing an electrolytic reaction tank, preparing an acid electrolyte by using copper salt, and pouring the acid electrolyte into the reaction tank;
step S3: placing a cathode ring at the bottom of a reaction tank, vertically inserting an anode metal wire into the reaction tank opposite to the geometric center of the cathode ring, keeping a spacing distance between the bottom of the reaction tank and the cathode ring, and respectively connecting the cathode ring and the anode metal wire with the negative electrode and the positive electrode of a low-voltage direct-current power supply;
step S4: applying voltage, heating in water bath to maintain the electrolyte at 55 deg.c, and reacting for 7min to prepare one layer of copper dendrite on the surface of the cathode ring.
Wherein, the wire size is selected as: the diameter is 1-2 mm, and the material is red copper; the anode wire size is selected as follows: the length is 2 cm; the shape of the cathode ring is selected to be circular, and the sizes are correspondingly as follows: diameter 1.5 cm; the copper salt in the copper salt electrolyte is CuSO4，Cu2+The concentration is selected to be 0.3 mol/L; of the bottom of the anode wire and the cathode ringThe spacing distance is 4 mm; the applied voltage was 18V.
As shown in fig. 4, which is a scanning electron micrograph of the copper dendrite having nodular constituent elements prepared by diamond-shaped closed cathode rings of example 4, it can be seen that the copper dendrite is composed of copper particles having a uniform nodular shape.
Comparative example 1
In the prior art, the preparation method of the copper dendrite comprises the following steps:
step S1: selecting a metal wire as an electrode material, polishing, cleaning and drying, selecting a straightened metal wire as an anode metal wire, and bending the metal wire into unclosed rings with different shapes as a cathode ring;
step S2: preparing an electrolytic reaction tank, preparing an acid electrolyte by using copper salt, and pouring the acid electrolyte into the reaction tank;
step S3: placing a cathode ring at the bottom of a reaction tank, vertically inserting an anode metal wire into the reaction tank opposite to the geometric center of the cathode ring, keeping a spacing distance between the bottom of the reaction tank and the cathode ring, and respectively connecting the cathode ring and the anode metal wire with the negative electrode and the positive electrode of a low-voltage direct-current power supply;
step S4: applying voltage, heating in water bath to maintain the electrolyte at 55 deg.c, and reacting for 7min to prepare one layer of copper dendrite on the surface of the cathode ring.
Wherein, the wire size is selected as: the diameter is 1-2 mm, and the material is red copper; the anode wire size is selected as follows: the length is 2 cm; the shape of the cathode ring is selected to be a semi-arc shape, and the size is correspondingly as follows: diameter 1.5 cm; the copper salt in the copper salt electrolyte is CuSO4，Cu2+The concentration is selected to be 0.3 mol/L; the distance between the bottom of the anode metal wire and the cathode ring is 4 mm; the applied voltage was 18V.
As shown in fig. 5, which is a scanning electron micrograph of copper dendrites having spheroidal constituent units prepared by semi-circular arc-shaped unclosed cathode rings of comparative example 1, it can be seen that the shape of the sparse copper dendrites begins to disappear, but there is a dendrite-like structure.
Comparative example 2
In the prior art, the preparation method of the copper dendrite comprises the following steps:
step S1: selecting a metal wire as an electrode material, polishing, cleaning and drying, selecting a straightened metal wire as an anode metal wire, and bending the metal wire into unclosed rings with different shapes as a cathode ring;
step S2: preparing an electrolytic reaction tank, preparing an acid electrolyte by using copper salt, and pouring the acid electrolyte into the reaction tank;
step S3: placing a cathode ring at the bottom of a reaction tank, vertically inserting an anode metal wire into the reaction tank opposite to the geometric center of the cathode ring, keeping a spacing distance between the bottom of the reaction tank and the cathode ring, and respectively connecting the cathode ring and the anode metal wire with the negative electrode and the positive electrode of a low-voltage direct-current power supply;
step S4: applying voltage, heating in water bath to maintain the electrolyte at 55 deg.c, and reacting for 7min to prepare one layer of copper dendrite on the surface of the cathode ring.
Wherein, the wire size is selected as: the diameter is 1-2 mm, and the material is red copper; the anode wire size is selected as follows: the length is 2 cm; the shape of the cathode ring is selected as two sides of a regular triangle or a rhombus, and the sizes are correspondingly as follows: the side length is 1.5 cm; the copper salt in the copper salt electrolyte is CuSO4，Cu2+The concentration is selected to be 0.3 mol/L; the distance between the bottom of the anode metal wire and the cathode ring is 4 mm; the applied voltage was 18V.
As shown in fig. 6, which is a scanning electron micrograph of copper dendrites having a spheroidal constituent unit prepared by unclosed cathode rings composed of both sides of regular triangles or rhombuses in comparative example 2, it can be seen that the shape of the sparse copper dendrites begins to disappear, but there is a dendrite-like structure.
Comparative example 3
In the prior art, the preparation method of the copper dendrite comprises the following steps:
step S1: selecting metal wires as electrode materials, polishing, cleaning and drying, and selecting straightened metal wires as anode metal wires and cathode metal wires;
step S2: preparing an electrolytic reaction tank, preparing an acid electrolyte by using copper salt, and pouring the acid electrolyte into the reaction tank;
step S3: placing a cathode metal wire at the bottom of the reaction tank, vertically inserting an anode metal wire into the reaction tank opposite to the geometric center of the cathode metal wire, keeping a spacing distance between the bottom of the reaction tank and the cathode metal wire, and respectively connecting the cathode metal wire and the anode metal wire with the negative electrode and the positive electrode of a low-voltage direct-current power supply;
step S4: applying voltage, heating in water bath to maintain the electrolyte at 55 deg.c, and reacting for 7min to prepare one layer of copper dendrite on the surface of the cathode wire.
Wherein, the wire size is selected as: the diameter is 1-2 mm, and the material is red copper; the dimensions of the anode wire and the cathode wire are selected as follows: the length is 2 cm; the copper salt in the copper salt electrolyte is CuSO4，Cu2+The concentration is selected to be 0.3 mol/L; the distance between the bottom of the anode metal wire and the cathode metal wire is 4 mm; the applied voltage was 18V.
As shown in fig. 7, which is a scanning electron micrograph of the general copper particles prepared by straightening the cathode wire of comparative example 3, it can be seen that the dendrite structure has completely disappeared under the reaction conditions.
With the above examples and comparative examples, it can be seen that:
different embodiments of the invention and comparative examples are different only in the shape and closing manner of the cathode wire, examples 1 to 4 of the invention are reactions performed under closed circular, square, regular triangular and rhombic cathode rings specified by the invention, copper dendrites with different specific morphologies disclosed by the invention are obtained, comparative examples 1 and 2 are also prepared by processing the wire into a ring shape, but are not closed (the two sides of the semicircular shape and the regular triangular or rhombic shape are in sequence), only dendrite-like structures can be obtained, comparative example 3 is not prepared by adopting the ring manner, and the straightened wire is directly adopted as the cathode, so that common copper particles are obtained. As can be seen from the above, the processing into rings and the sealing treatment play an important role in the controllable preparation of the copper dendrites with different morphologies.
It should be noted that, according to the implementation requirement, each step described in the present application can be divided into more steps, and two or more steps or partial operations of the steps can be combined into a new step to achieve the purpose of the present invention.
Claims (6)
1. A method for preparing copper dendrites is characterized in that: the method comprises the following steps:
s1: selecting a metal wire as an electrode material, polishing, cleaning and drying, selecting a straightened metal wire as an anode metal wire, and bending the metal wire into closed rings with different shapes as a cathode ring;
s2: preparing an electrolytic reaction tank, preparing an acid electrolyte by using copper salt, and pouring the acid electrolyte into the reaction tank;
s3: placing a cathode ring at the bottom of a reaction tank, vertically inserting an anode metal wire into the reaction tank opposite to the geometric center of the cathode ring, keeping a spacing distance between the bottom of the reaction tank and the cathode ring, and respectively connecting the cathode ring and the anode metal wire with the negative electrode and the positive electrode of a low-voltage direct-current power supply;
s4: and applying voltage, heating in a water bath to maintain the temperature of the electrolyte at 50-60 ℃, reacting for 5-10 min, and preparing a layer of copper dendrite on the surface of the cathode ring.
2. A method of producing copper dendrites according to claim 1 wherein: in step S1, the wire size is selected as: the diameter is 1-2 mm, and the material is red copper or brass; the anode wire is selected from the following sizes: the length of the glass is 1-3 cm.
3. A method of producing copper dendrites according to claim 1 wherein: in step S1, the shape of the cathode ring is selected from any one of a circle, a square, a regular triangle or a rhombus, and the sizes thereof are: the diameter is 1-2 cm, the side length is 1-2 cm or the side length is 1-2 cm.
4. A method of producing copper dendrites according to any one of claims 1 to 3 wherein: in the step S2, the copper salt in the copper salt electrolyte is CuCl2、CuSO4Or Cu (NO)3)2One or a mixture of several of (1), Cu2+The concentration is selected to be 0.2-0.4 mol/L.
5. A method of producing copper dendrites according to claim 4 wherein: in the step S3, the distance between the bottom of the anode wire and the cathode ring is 3-6 mm.
6. A method of producing copper dendrites according to claim 1 or 2 or 3 or 5 wherein: in the step S4, the applied voltage is 15-20V.
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| US4551210A (en) * | 1984-11-13 | 1985-11-05 | Olin Corporation | Dendritic treatment of metallic surfaces for improving adhesive bonding |
| WO2012065083A1 (en) * | 2010-11-14 | 2012-05-18 | Arizona Board Of Regents, A Body Corporate Of The State Of Arizona Acting For And | Dendritic metal structures, methods for making dendritic metal structures, and devices including them |
| CN105568327A (en) * | 2015-12-18 | 2016-05-11 | 西安科技大学 | Electrochemical method for preparing super-hydrophobic surface of copper dendritic crystal |
| CN105908220A (en) * | 2016-05-06 | 2016-08-31 | 上海应用技术学院 | Method for manufacturing micro-nano-silver dendritic crystal through liquid-phase electrodeposition |
| CN106498464A (en) * | 2016-10-24 | 2017-03-15 | 电子科技大学 | A kind of metal receives a micron preparation method for dendrite oldered array |
| CN111647909A (en) * | 2020-07-01 | 2020-09-11 | 中国科学技术大学 | Dendritic copper electrode with hydrophobic surface and preparation method and application thereof |
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2021
- 2021-07-14 CN CN202110796849.4A patent/CN113481552B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4551210A (en) * | 1984-11-13 | 1985-11-05 | Olin Corporation | Dendritic treatment of metallic surfaces for improving adhesive bonding |
| WO2012065083A1 (en) * | 2010-11-14 | 2012-05-18 | Arizona Board Of Regents, A Body Corporate Of The State Of Arizona Acting For And | Dendritic metal structures, methods for making dendritic metal structures, and devices including them |
| CN105568327A (en) * | 2015-12-18 | 2016-05-11 | 西安科技大学 | Electrochemical method for preparing super-hydrophobic surface of copper dendritic crystal |
| CN105908220A (en) * | 2016-05-06 | 2016-08-31 | 上海应用技术学院 | Method for manufacturing micro-nano-silver dendritic crystal through liquid-phase electrodeposition |
| CN106498464A (en) * | 2016-10-24 | 2017-03-15 | 电子科技大学 | A kind of metal receives a micron preparation method for dendrite oldered array |
| CN111647909A (en) * | 2020-07-01 | 2020-09-11 | 中国科学技术大学 | Dendritic copper electrode with hydrophobic surface and preparation method and application thereof |
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