CN113293351A - Method for plating carbon on surface of copper nanowire - Google Patents
Method for plating carbon on surface of copper nanowire Download PDFInfo
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- CN113293351A CN113293351A CN202110608412.3A CN202110608412A CN113293351A CN 113293351 A CN113293351 A CN 113293351A CN 202110608412 A CN202110608412 A CN 202110608412A CN 113293351 A CN113293351 A CN 113293351A
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- carbon
- copper nanowire
- cunws
- plating
- arc discharge
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0605—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- 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
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
- C23C14/325—Electric arc evaporation
Abstract
The invention provides a method for plating carbon on the surface of a copper nanowire, which adopts a multi-component codeposition device integrating magnetic filtration, arc discharge and plasma into a whole to deposit on a copper nanowire substrate to prepare a CuNWs/C anti-corrosion coating. The magnetic filtration sample has high purity, and sp is generated by combining arc discharge with plasma technology2The carbon is firmly deposited on the surface of the copper nanowire, so that a high-quality corrosion-resistant coating material can be prepared, the performance of the battery is improved, the service life of the battery is prolonged, and the copper-based high-energy-density coating material is applied to high-energy-density full batteries such as lithium-sulfur batteries and lithium-air batteries. The method is simple to operate, convenient in process and high in practical application value.
Description
Technical Field
The invention relates to a method for plating carbon on the surface of a copper nanowire, in particular to a multi-element integrated carbon plating technology and a preparation method of a CuNWs/C anti-corrosion coating, and belongs to the technical field of preparation of surface anti-corrosion coatings.
Background
Lithium ion batteries have been widely used in various portable electronic devices as a high-efficiency secondary battery. With the development of new energy electric automobiles, aerospace and energy storage devices, the energy density and safety performance of lithium batteries are concerned. The corrosion of the negative current collector of the lithium ion battery can cause the influence on the electronic conductivity between the current collector and the electrode active material, and the contact resistance between the current collector and the electrode active material is obviously increased, so that the cycle efficiency, the specific capacity and the service life of the battery are reduced, and the storage performance and the safety performance of the battery are influenced.
At present, the preparation technologies of corrosion-resistant coatings are many, which are mainly classified into wet chemical coating, chemical vapor deposition and physical vapor deposition, but these technologies have the problems of poor material binding force, difficult thickness control, weak mechanical strength and the like, and the development of a preparation technology of a uniform and smooth surface coating with good binding force, adjustable thickness, high mechanical strength is urgently needed.
Through search, the patent with publication number CN111540535A discloses a preparation method of carbon-coated copper nanowires, which comprises adding organic carbon glucose into a copper nanowire dispersion, reacting for 24 hours under a closed condition, and performing washing, drying and other processes, wherein the steps are complicated and the time consumption is long.
Disclosure of Invention
The invention aims to solve the technical problem of providing a diversified carbon plating technology and a preparation method of a CuNWs/C corrosion-resistant coating to overcome the defects of the prior art.
The invention provides a method for plating carbon on the surface of a copper nanowire, which is characterized in that a multielement codeposition device integrating magnetic filtration, arc discharge and plasma is adopted to deposit on a copper nanowire substrate to prepare a CuNWs/C anti-corrosion coating; the method comprises the following steps:
s1, preparing a copper nanowire film;
s2, designing a multi-element integrated codeposition device, wherein the designed multi-element integrated device comprises a magnetic filter, an arc discharge device and a plasma carbon plating device;
s3, the multi-element integrated codeposition device designed in the step 2 adopts a multi-element integrated technology to prepare a CuNWs/C corrosion-resistant coating, a copper nanowire film is used as a substrate, and a carbon arc source is used for deposition.
The invention provides a multi-element integrated carbon plating technology and a preparation method of a CuNWs/C corrosion-resistant coating. In a vacuum environment, plasma is generated by arc discharge, large particles are screened out by magnetic filtration and deposited on the surface of a substrate, and the surface of the copper nanowire is plated with carbon to prepare the CuNWs/C anti-corrosion coating.
The further technical scheme of the invention is as follows:
in the step 3, the multivariate integration technology is a multivariate deposition technology combining a magnetic filtration technology, an arc discharge technology and a plasma technology.
In the step 3, the specific method for preparing the CuNWs/C corrosion-resistant coating is as follows: the solid carbon source generates plasma under the action of arc discharge, large-particle impurities are screened out after magnetic filtration, and sp with high purity is obtained2And enabling the hybrid C plasma to enter a film deposition cavity, and depositing on the copper nanowire substrate to form a CuNWs/C coating.
The magnetic filtration sample has high purity, and sp is generated by combining arc discharge with plasma technology2The carbon is firmly deposited on the surface of the copper nanowire, so that a high-quality corrosion-resistant coating material can be prepared, the performance of the battery is improved, the service life of the battery is prolonged, and the copper-based high-energy-density coating material is applied to high-energy-density full batteries such as lithium-sulfur batteries and lithium-air batteries.
Further, the solid carbon source is jointly connected with an arc discharge and plasma device through magnetic filtration screening so as to improve the purity of the sample; the arc source of arc discharge is different metals and non-metals.
Further, the arc source is carbon metal.
Furthermore, the common device adopts a plurality of 1+1 and 1+ N, and the device comprises a reaction chamber, a deposition substrate, a rotatable base, a gas source, a gas inlet and a gas outlet.
Further, the gas source is carbon dioxide (CO)2）。
Further, the thickness of C in the CuNWs/C corrosion-resistant coating is 100 nm.
In the step 1, the preparation method of the copper nanowire film comprises the following steps: adding ethylenediamine to Cu (NO)3)2·3H2And (2) uniformly mixing the solution with the aqueous solution of O, adding the mixed solution into the aqueous solution of NaOH, uniformly stirring, adding a proper amount of hydrazine hydrate, standing in a water bath at 75 ℃ for 1h to obtain CuNWs, and performing suction filtration and cross-filtration cleaning by using ultrapure water and absolute ethyl alcohol to obtain the CuNWs film.
Compared with the prior art, the invention adopting the technical scheme has the following technical effects: the multielement integrated codeposition carbon plating technology combines the magnetic filtration screening technology, the arc discharge technology and the plasma technology, the magnetic filtration screening plasma can obtain a coating with higher purity, and the prepared CuNWs/C has good binding force with a substrate, adjustable thickness and high mechanical strength, and is suitable for being applied to the fields of lithium ion battery current collectors and the like. The method is simple to operate, convenient in process and high in practical application value.
Drawings
FIG. 1 is a schematic structural diagram of a multi-component integrated carbon plating device according to the present invention.
FIG. 2 is an SEM image of a CuNWs/C corrosion-resistant coating in accordance with the present invention.
Detailed Description
The technical scheme of the invention is further explained in detail by combining the attached drawings: the present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the protection authority of the present invention is not limited to the following embodiments.
The invention relates to a multi-element integrated carbon plating device, which consists of a plurality of arc discharge electromagnetic filtering bent pipes. As shown in fig. 1, taking two arc discharge magnetic filtering bent tubes as an example, the binary integrated carbon plating device comprises two magnetic filtering bent tubes 1, a first arc discharge source 2, a second arc discharge source 4, a first solid target 3, a second solid target 5, a chemical vapor reaction chamber 6, an air inlet 7, a deposition substrate 8, a rotatable base 9 and an air outlet 10. Chemical gasThe phase reaction chamber 6 has a rectangular parallelepiped shape and a vacuum atmosphere inside. The lower ends of the two magnetic filtering bent pipes 1 are respectively arranged on the upper part of a chemical vapor reaction chamber 6, the upper ends of the two magnetic filtering bent pipes are respectively connected with a first solid target 3 (or a second solid target 5) through a first arc discharge source 2 (or a second arc discharge source 4), an air inlet 7 is arranged on one side of the chemical vapor reaction chamber 6, an air outlet 10 is arranged on the opposite side, the air inlet 7 is connected with a gas source, and the gas source is CO2 A deposition substrate 8 and a rotatable susceptor 9 are provided inside the chemical vapor reaction chamber 6, the deposition substrate 8 is provided on the rotatable susceptor 9, and the susceptor 9 is installed at the bottom of the chemical vapor reaction chamber 6 and is rotatable 360 deg..
When the binary integrated carbon plating device works, as shown in fig. 2, a solid carbon source is introduced under the vacuum condition to generate plasma under the action of arc discharge, then the plasma is magnetically filtered by a magnetic filtering device to screen out large-particle impurities, and the structure with high purity, namely sp, is obtained2And (3) enabling the hybrid C plasma to enter a thin film deposition cavity, and depositing on the copper nanowire substrate to form a CuNWs/C coating, wherein the thickness of C in the coating is 100 nm. The invention adopts a multivariate integration technology which is a multivariate deposition technology combining a magnetic filtration technology, an arc discharge technology and a plasma technology, improves the purity of a sample by combining a magnetic filtration screening device, an arc discharge device and a plasma device, and the arc source of the multivariate integration technology is different metals and non-metals, particularly carbon metal.
Example 1
The preparation method of the copper nanowire film comprises the following steps:
s1, weighing 0.964g Cu (NO)3)2·3H2O was added to 40 mL of ultrapure water, 8mL of ethylenediamine was aspirated through a syringe, and the solution was added to the above Cu (NO)3)2·3H2Mixing the O solution and the water solution uniformly, wherein the solution is dark blue and is marked as solution A; weighing 480g of NaOH, dissolving in 800 mL of ultrapure water, and placing a beaker in an ice-water bath to obtain a solution B; adding the mixed solution A into the cooled solution B, and stirring uniformly (about 10 min), wherein the solution is uniform and clear dark blue and is marked as mixed solution C; using a pipette to pipette 800. mu.L of hydrazine hydrate, adding into the mixed solution CStirring until the solution becomes light blue (about 10 min), and recording as solution D; putting the solution D into a water bath kettle at 75 ℃, and standing for 1h to obtain crude CuNWs; and carrying out suction filtration on the obtained crude CuNWs, and carrying out cross suction filtration and cleaning by using ultrapure water and absolute ethyl alcohol to obtain the CuNWs film.
Example 2
The multi-element integrated carbon plating device comprises the following accessories:
s2, a multi-component integrated carbon plating device, which is a multi-component device integrating magnetic filtration, arc discharge and plasma.
As shown in FIG. 1, the apparatus comprises a magnetic filter bend 1, a first arc discharge source 2, a second arc discharge source 4, a first solid target 3, a second solid target 5, a chemical vapor reaction chamber 6, a gas inlet 7, a deposition substrate 8, a rotatable susceptor 9, and a gas outlet 10. The magnetic filtering screening arc discharge plasma device shown in figure 1 comprises two or more magnetic filtering bent pipes and a magnetic filtering main pipe, and can be assembled with more than two arc sources for working. The chemical vapor reaction chamber 6, i.e. the film deposition chamber, is also provided with a deposition substrate 8. The deposition substrate 8 is placed on a rotatable susceptor 9, and the deposition substrate 8 is rotated by a rotation device of the rotatable susceptor 9.
Example 3
The embodiment of the invention relates to a preparation method of a CuNWs/C corrosion-resistant coating, which comprises the following steps:
s3, cleaning the deposition substrate 8 and fixing the substrate on a rotatable base 9 in the film deposition cavity; two arc discharge sources, two magnetic filtering bent pipes 1 and a film deposition cavity are vacuumized, and the vacuum degree reaches 1 multiplied by 10-4Pa; cleaning the coating surface of the deposition substrate 8 by using plasma to remove oil stains and impurities on the coating surface of the deposition substrate 8;
s4, introducing an arc discharge carbon source into the magnetic filtering bent pipe 1 for screening, wherein the deposited arc flow is 100-120A, the current of the magnetic filtering bent pipe is 1.6-2.5A, the negative bias is 160-320V, and the deposition time is 10 min;
and S5, closing the arc discharge source and the magnetic filtration power supply, releasing the vacuum degree, opening the film deposition cavity after the vacuum degree is recovered to the normal pressure state, and taking out the sample to obtain the coating with the carbon-plated surface.
And closing the arc discharge, the magnetic filtration and the power supply of the chemical vapor tubular furnace, releasing the vacuum degree, opening the film deposition cavity after the vacuum degree is recovered to the normal pressure state, and taking out a sample to obtain the CuNWs/C coating, as shown in figure 2.
The multielement integrated carbon plating device has the advantages of simple process, convenient operation and easy large-scale production. The prepared CuNWs/C has good binding force with an electrode substrate, adjustable thickness and high mechanical strength, and is suitable for the fields of lithium ion battery current collectors and the like.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can understand that the modifications or substitutions within the technical scope of the present invention are included in the scope of the present invention, and therefore, the scope of the present invention should be subject to the protection scope of the claims.
Claims (9)
1. A method for plating carbon on the surface of a copper nanowire is characterized in that the method is to deposit on a copper nanowire substrate by adopting a multi-component codeposition device integrating magnetic filtration, arc discharge and plasma into a whole to prepare a CuNWs/C anti-corrosion coating; the method comprises the following steps:
s1, preparing a copper nanowire film;
s2, designing a multi-element integrated codeposition device, wherein the designed multi-element integrated device comprises a magnetic filter, an arc discharge device and a plasma carbon plating device;
s3, preparing the CuNWs/C corrosion-resistant coating by the multi-element integrated codeposition device designed in the step 2 by adopting a multi-element integrated technology.
2. The method for carbon plating of the surfaces of the copper nanowires as claimed in claim 1, wherein in the step 3, the multivariate integration technology is a multivariate deposition technology comprising a combination of a magnetic filtration technology, an arc discharge technology and a plasma technology.
3.The method for plating copper on the surface of the copper nanowire as claimed in claim 2, wherein in the step 3, the specific method for preparing the CuNWs/C corrosion-resistant coating is as follows: the solid carbon source generates plasma under the action of arc discharge, large-particle impurities are screened out after magnetic filtration, and sp with high purity is obtained2And enabling the hybrid C plasma to enter a film deposition cavity, and depositing on the copper nanowire substrate to form a CuNWs/C coating.
4. The method for plating carbon on the surface of the copper nanowire as claimed in claim 3, wherein the solid carbon source is combined with an arc discharge and plasma device through magnetic filtration screening to improve the purity of a sample; the arc source of arc discharge is different metals and non-metals.
5. The method for carbon plating of the surfaces of the copper nanowires as claimed in claim 4, wherein the arc source is carbon metal.
6. The method of claim 4, wherein a plurality of 1+1 and 1+ N devices are used, and the device comprises a reaction chamber, a deposition substrate, a rotatable susceptor, a gas source, a gas inlet, and a gas outlet.
7. The method for carbon plating on the surface of the copper nanowire as claimed in claim 6, wherein the gas source is carbon dioxide.
8. The method for carbon plating of the surface of the copper nanowire as recited in claim 3, wherein the thickness of C in the CuNWs/C corrosion-resistant coating is 100 nm.
9. The method for plating carbon on the surface of the copper nanowire according to claim 1, wherein in the step 1, the method for preparing the copper nanowire film comprises the following steps: adding ethylenediamine to Cu (NO)3)2·3H2Mixing with water solution of O, adding the mixed solution into NaOH water solution, and stirringAnd (3) uniformly adding a proper amount of hydrazine hydrate, standing for 1h in a water bath at 75 ℃ to obtain CuNWs, and performing suction filtration, cross-filtration and cleaning by using ultrapure water and absolute ethyl alcohol to obtain the CuNWs film.
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Citations (5)
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| CN1224772A (en) * | 1998-01-24 | 1999-08-04 | 西南交通大学 | Synthesis of carbon-base film |
| CN102560415A (en) * | 2012-01-20 | 2012-07-11 | 中国科学院上海硅酸盐研究所 | Three-dimensional graphene/metal line or metal wire composite structure and preparation method thereof |
| CN105755442A (en) * | 2015-11-06 | 2016-07-13 | 北京师范大学 | Method for preparing DLC (diamond-like carbon) thick films by means of efficient magnetic filter plasma deposition |
| US20160358747A1 (en) * | 2014-01-16 | 2016-12-08 | The University Of Akron | Conductive film and method of making same |
| US20170154701A1 (en) * | 2014-07-09 | 2017-06-01 | Daegu Gyeongbuk Institute Of Science And Technology | Metal nanowire having core-shell structure coated with graphene, and manufacturing method therefor |
-
2021
- 2021-06-01 CN CN202110608412.3A patent/CN113293351A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1224772A (en) * | 1998-01-24 | 1999-08-04 | 西南交通大学 | Synthesis of carbon-base film |
| CN102560415A (en) * | 2012-01-20 | 2012-07-11 | 中国科学院上海硅酸盐研究所 | Three-dimensional graphene/metal line or metal wire composite structure and preparation method thereof |
| US20160358747A1 (en) * | 2014-01-16 | 2016-12-08 | The University Of Akron | Conductive film and method of making same |
| US20170154701A1 (en) * | 2014-07-09 | 2017-06-01 | Daegu Gyeongbuk Institute Of Science And Technology | Metal nanowire having core-shell structure coated with graphene, and manufacturing method therefor |
| CN105755442A (en) * | 2015-11-06 | 2016-07-13 | 北京师范大学 | Method for preparing DLC (diamond-like carbon) thick films by means of efficient magnetic filter plasma deposition |
Non-Patent Citations (4)
| Title |
|---|
| BOHR-RAN HUANG,ET AL: ""Field emission studies of amorphous carbon deposited on copper nanowires grown by cathodic arc plasma deposition"", 《NEW CARBON MATERIALS》, 30 June 2009 (2009-06-30), pages 97 - 101 * |
| BOHR-RAN HUANG: ""Field emission studies of amorphous carbon deposited on copper nanowires grown by cathodic arc plasma deposition"", 《NEW CARBON MATERIALS》, pages 97 - 101 * |
| 沟引宁: ""磁过滤真空弧源沉积C／C 多层复合膜的结构和力学性能研究"", 《真空科学与技术学报》, pages 66 - 69 * |
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