CN112608506A - Preparation method of metal nanowire coating/polymer composite material with low contact resistance - Google Patents
Preparation method of metal nanowire coating/polymer composite material with low contact resistance Download PDFInfo
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- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/044—Forming conductive coatings; Forming coatings having anti-static properties
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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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
- C23C14/025—Metallic sublayers
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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
- C23C14/14—Metallic material, boron or silicon
- C23C14/20—Metallic material, boron or silicon on organic substrates
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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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- C—CHEMISTRY; METALLURGY
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- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2307/00—Characterised by the use of natural rubber
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/20—Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups
Abstract
The invention discloses a preparation method of a metal nanowire coating/polymer composite material with low contact resistance, which is characterized in that metal nanowires are dispersed in aqueous solution by utilizing ultrasound or stirring, then the metal nanowires are coated on the surface of a polymer substrate, the metal nanowire coating/polymer composite material is obtained after drying, and finally a metal nanowire film is sputtered on the surface of the metal nanowire coating/polymer composite material by a magnetron sputtering process, so that the metal nanowire coating/polymer composite material with low contact resistance, which can be used in the fields of electric conduction and electromagnetic shielding, is obtained.
Description
Technical Field
The invention relates to a preparation method of a metal nanowire coating with low contact resistance.
Background
With the rapid development of modern electronic industry, wireless communication and digitization technology, the problem of electromagnetic radiation generated by high frequency devices is more serious. The elimination of electromagnetic radiation is a major approach to safeguard national defense safety and human health. Compared with metallic materials mainly reflecting electromagnetic waves, polymer-based electromagnetic shielding materials have been a research hotspot due to their advantages of high absorption, low reflection, low density and easy processing, and have received extensive attention from both academic and industrial fields. The conductive filler commonly used in the field of polymer-based electromagnetic shielding materials comprises metal nanowires, carbon black, carbon nanotubes, graphene, MXene and the like. Among them, the metal nanowires have the advantages of high conductivity and large length-diameter ratio, and thus become a hot research point in the field of polymer-based electromagnetic shielding materials. However, in order to improve the dispersibility of the metal nanowires in the aqueous solution, a large amount of surfactant is coated on the surfaces of the metal nanowires, which prevents the metal nanowires from directly contacting with each other, so that the metal nanowires have high contact resistance, and the metal nanowires are not favorable for obtaining efficient electromagnetic shielding materials. At present, scientists propose to solve the problem by using hot pressing, nano welding, sintering and other methods. Although the methods can reduce the resistance of the metal nanowire coating by 15-50%, the methods usually involve higher temperature or strong acid solution, and cannot meet the development requirements of energy-saving and environment-friendly green industry. Therefore, it is still a great problem to develop an energy-saving and environment-friendly method to reduce the contact resistance of the metal nanowire coating.
Disclosure of Invention
The invention aims to provide a preparation method of a metal nanowire coating/polymer composite material with low contact resistance aiming at the defects of the prior art, which is characterized in that metal nanowires are dispersed in aqueous solution by utilizing ultrasound or stirring, then the metal nanowires are coated on the surface of a polymer substrate, the metal nanowire coating/polymer composite material is obtained after drying, and finally a metal nanowire film is sputtered on the surface of the metal nanowire coating/polymer composite material by a magnetron sputtering process, so that the metal nanowire coating/polymer composite material with low contact resistance which can be used in the fields of electric conduction and electromagnetic shielding is obtained.
The purpose of the invention is realized by the following technical measures:
a method for preparing a metal nanowire coating/polymer composite material with low contact resistance, comprising the following steps:
(1) under the action of a surfactant, dispersing metal nanowires in water by utilizing ultrasound or stirring, wherein the mass ratio of the metal nanowires to the surfactant is 100-0.01;
(2) coating the metal nanowire dispersion liquid on the surface of a polymer base material, drying, and obtaining a metal nanowire coating/polymer composite material through a plurality of coating-drying cycle times;
(3) and sputtering a layer of metal nano film capable of reducing the contact resistance of the metal nanowire on the surface of the metal nanowire coating/polymer composite material by utilizing a magnetron sputtering process to obtain the metal nanowire coating/polymer composite material with low contact resistance.
The surfactant is at least one of stearic acid, polyvinylpyrrolidone, sodium dodecyl benzene sulfonate, disodium lauryl sulfosuccinate monoester, cetyl trimethyl ammonium bromide and alkylphenol polyoxyethylene ether-10; the metal nanowire is at least one of silver nanowire, copper nanowire and nickel nanowire; the diameter of the metal nanowire is 1-50 nm, and the length of the metal nanowire is 100 nm-100 mu m; the ultrasonic or stirring time is 5 minutes to 10 hours; the concentration of the metal nanowire dispersion liquid is 0.1-50 mg/ml.
The polymer base material is at least one of a polyester film, a polyethylene film, a natural rubber film, a polypropylene film, polyester fiber cloth, cotton fiber cloth, polypropylene non-woven fabric and a cellulose film; the coating process is one of dip coating, spray coating, drop coating and blade coating.
The drying temperature is 10-100 ℃; the drying time is 0.1 to 50 hours, and the number of coating-drying cycles is 1 to 100.
The target material of the magnetron sputtering process is at least one of an iron target, a nickel target, a silver target, a copper target and a cobalt target.
The sputtering power of the magnetron sputtering process is 1-200W, the sputtering pressure is 0.1-2.0 Pa, the sputtering time is 1 minute-10 hours, and the temperature is 10-100 ℃.
The metal nanowire coating/polymer composite material with the conductivity of 0.001-10000S/cm and the electromagnetic shielding effectiveness of 10-100 dB and low contact resistance can be prepared.
The metal coating/polymer composite having low contact resistance can be used in the fields of conductive materials and electromagnetic shielding materials.
The invention has the advantages that:
(1) the temperature required in the process of preparing the metal coating/polymer composite material with low contact resistance is lower, and the method has the advantage of saving energy;
(2) the preparation process only uses water as a solvent, and meets the requirements of environmental protection.
Drawings
Fig. 1 is a photograph of a metal coating/polymer composite (left) and a metal coating/polymer composite with low contact resistance (right).
Detailed Description
The present invention will be specifically described below by way of examples. It should be noted that the following examples are given solely for the purpose of illustration and are not to be construed as limitations on the scope of the invention, as many insubstantial modifications and variations of the invention may be made by those skilled in the art in light of the above teachings.
Example 1 silver nanowires with a diameter of 10 nm and a length of 10 μm are dispersed in water by using ultrasound under the action of polyvinylpyrrolidone, the mass ratio of the silver nanowires to the polyvinylpyrrolidone is 2, a silver nanowire solution with a concentration of 1 mg/ml is obtained after 20 minutes of ultrasound, the silver nanowire solution is coated on a polyester film by using a dip coating process, the polyester film is dried for 0.1 hour at a temperature of 20 ℃, and after 10 times of coating-drying cycle, a silver nanowire coating/polyester film composite material is obtained, finally, an iron target is adopted as a magnetron sputtering target, the sputtering power is 10W, the sputtering pressure is 0.1 Pa, the sputtering time is 30 minutes, and the sputtering temperature is 20 ℃, a layer of iron nanofilm capable of reducing the contact resistance of the silver nanowires is sputtered on the surface of the silver nanowire coating/polyester film composite material, the silver nanowire coating/polyester film composite material with low contact resistance is obtained, the conductivity of the material is 100S/cm, and the electromagnetic shielding efficiency is 60 dB.
Example 2 under the action of sodium dodecylbenzene sulfonate, a nickel nanowire with a diameter of 20 nm and a length of 15 μm is dispersed in water by stirring, the mass ratio of the nickel nanowire to the sodium dodecylbenzene sulfonate is 10, after stirring for 30 minutes, a nickel nanowire solution with a concentration of 5 mg/ml is obtained, the nickel nanowire solution is coated on a cellulose film by a drop coating process, drying is carried out at a temperature of 60 ℃ for 0.2 hour, and after 5 coating-drying cycles, a nickel nanowire coating/cellulose film composite material is obtained, finally, a nickel target is adopted as a magnetron sputtering target material, the sputtering power is 20W, the sputtering pressure is 0.5 Pa, the sputtering time is 40 minutes, and the sputtering temperature is 30 ℃, a layer of nickel nanowire film capable of reducing the contact resistance of the nickel nanowire is sputtered on the surface of the nickel nanowire coating/cellulose film composite material, the nickel nanowire coating/cellulose thin film composite material with low contact resistance is obtained, the conductivity of the material is 1600S/cm, and the electromagnetic shielding efficiency is 100 dB.
Example 3 under the action of disodium lauryl sulfosuccinate, copper nanowires with a diameter of 50 nm and a length of 50 μm are dispersed in water by using ultrasound, the mass ratio of the copper nanowires to the disodium lauryl sulfosuccinate is 20, a copper nanowire solution with a concentration of 20 mg/ml is obtained after ultrasound is performed for 40 minutes, then the copper nanowire solution is coated on a natural rubber film by using a blade coating process, the natural rubber film is dried at a temperature of 80 ℃ for 0.5 hour, and after 20 times of coating-drying cycles, a copper nanowire coating/natural rubber film composite material is obtained, finally a nickel target is adopted as a magnetron sputtering target, the sputtering power is 10W, the sputtering pressure is 1 Pa, the sputtering time is 60 minutes, and the sputtering temperature is 50 ℃, a layer of nickel nano film capable of reducing the contact resistance of the copper nanowires is sputtered on the surface of the copper nanowire coating/natural rubber film composite material, the copper nanowire coating/natural rubber thin film composite material with low contact resistance is obtained, the conductivity of the material is 10000S/cm, and the electromagnetic shielding efficiency is 99 dB.
Example 4 under the action of alkylphenol ethoxylate-10, silver nanowires with a diameter of 20 nm and a length of 100 μm are dispersed in water by stirring, the mass ratio of the silver nanowires to the alkylphenol ethoxylate-10 is 30, after stirring for 40 minutes, a copper nanowire solution with a concentration of 10 mg/ml is obtained, the silver nanowire solution is coated on a cellulose film by a blade coating process, the cellulose film is dried at a temperature of 60 ℃ for 0.1 hour, and after 10 coating-drying cycles, a silver nanowire coating/cellulose film composite material is obtained, finally, a silver target is adopted as a magnetron sputtering target, a layer of silver nanofilm with a sputtering power of 150W, a sputtering pressure of 1 Pa, a sputtering time of 60 minutes and a sputtering temperature of 30 ℃ is sputtered on the surface of the silver nanowire coating/cellulose film composite material, so as to reduce the contact resistance of the silver nanowires, the silver nanowire coating/cellulose film composite material with low contact resistance is obtained, the conductivity of the material is 9000S/cm, and the electromagnetic shielding efficiency is 98 dB.
Example 5 under the action of alkylphenol ethoxylate-10, a silver nanowire with a diameter of 20 nm and a length of 100 μm is dispersed in water by using ultrasound, the mass ratio of the silver nanowire to the alkylphenol ethoxylate-10 is 30, a copper nanowire solution with a concentration of 5 mg/ml is obtained after 30 minutes of ultrasound, the silver nanowire solution is coated on a polypropylene non-woven fabric by using a blade coating process, the polypropylene non-woven fabric is dried for 0.1 hour at a temperature of 60 ℃, and after 7 times of coating-drying cycles, a silver nanowire coating/polypropylene non-woven fabric composite material is obtained, finally, a silver nano film capable of reducing the contact resistance of the silver nanowire is sputtered on the surface of the silver nanowire coating/polypropylene non-woven fabric composite material by using a silver target as a magnetron sputtering target under the process conditions of a sputtering power of 100W, a sputtering pressure of 0.6 Pa, a sputtering time of 60 minutes and a sputtering temperature of 30 ℃, the silver nanowire coating/polypropylene non-woven fabric composite material with low contact resistance is obtained, the conductivity of the material is 9900S/cm, and the electromagnetic shielding efficiency is 97 dB.
FIG. 1 is a photograph of a metal coating/polymer composite (left) and a metal coating/polymer composite with low contact resistance (right); it can be seen from fig. 1 that the surface of the metal coating/polymer composite material with low contact resistance is darker, indicating that the surface has been sputtered with a metal nano-film.
Claims (8)
1. A method for preparing a metal nanowire coating/polymer composite material with low contact resistance is characterized by comprising the following steps:
(1) under the action of a surfactant, dispersing metal nanowires in water by utilizing ultrasound or stirring, wherein the mass ratio of the metal nanowires to the surfactant is 100-0.01;
(2) coating the metal nanowire dispersion liquid on the surface of a polymer base material, drying, and obtaining a metal nanowire coating/polymer composite material through proper coating-drying cycle times;
(3) and sputtering a layer of metal nano film capable of reducing the contact resistance of the metal nanowire on the surface of the metal nanowire coating/polymer composite material by utilizing a magnetron sputtering process to obtain the metal nanowire coating/polymer composite material with low contact resistance.
2. The method for preparing a metal nanowire coating/polymer composite material with low contact resistance according to claim 1, wherein in the step (1), the surfactant is at least one of stearic acid, polyvinylpyrrolidone, sodium dodecylbenzenesulfonate, disodium laurylsulfosuccinate monoester, cetyltrimethylammonium bromide, and alkylphenol ethoxylate-10; the metal nanowire is at least one of silver nanowire, copper nanowire and nickel nanowire; the diameter of the metal nanowire is 1-50 nm, and the length of the metal nanowire is 100 nm-100 mu m; the ultrasonic or stirring time is 5 minutes to 10 hours; the concentration of the metal nanowire dispersion liquid is 0.1-50 mg/ml.
3. The method for preparing a metal nanowire coating/polymer composite material with low contact resistance as claimed in claim 1, wherein in the step (2), the polymer substrate is at least one of a polyester film, a polyethylene film, a natural rubber film, a polypropylene film, a polyester fiber cloth, a cotton fiber cloth, a polypropylene non-woven fabric and a cellulose film; the coating process is one of dip coating, spray coating, drop coating and blade coating.
4. The method for preparing a metal nanowire coating/polymer composite material with low contact resistance according to claim 1, wherein in the step (2), the drying temperature is 10-100 ℃; the drying time is 0.1 to 50 hours, and the number of coating-drying cycles is 1 to 100.
5. The method for preparing a metal nanowire coating/polymer composite material with low contact resistance as claimed in claim 1, wherein in the step (3), the target material of the magnetron sputtering process is at least one of an iron target, a nickel target, a silver target, a copper target and a cobalt target.
6. The method for preparing a metal nanowire coating/polymer composite material with low contact resistance as claimed in claim 1, wherein in the step (3), the sputtering power of the magnetron sputtering process is 1-200W, the sputtering pressure is 0.1-2.0 Pa, the sputtering time is 1 minute-10 hours, and the temperature is 10-100 ℃.
7. The method for preparing a metal nanowire coating/polymer composite material with low contact resistance as claimed in any one of claims 1 to 6, which can prepare a metal nanowire coating/polymer composite material with low contact resistance having an electrical conductivity of 0.001 to 10000S/cm and an electromagnetic shielding effectiveness of 10 to 100 dB.
8. The metal coating/polymer composite material having low contact resistance prepared according to claim 7 can be used in the fields of conductive materials and electromagnetic shielding materials.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130341074A1 (en) * | 2012-06-22 | 2013-12-26 | Ajay Virkar | Metal nanowire networks and transparent conductive material |
| CN107685154A (en) * | 2017-09-07 | 2018-02-13 | 深圳赢特科技有限公司 | A kind of nano silver wire composite coating and preparation method thereof |
| CN110258106A (en) * | 2019-07-19 | 2019-09-20 | 中南林业科技大学 | A kind of preparation method of the sandwich-type flexible electromagnetic shielding material based on carbon fibre fabric, metallic nickel nano granule and graphene |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130341074A1 (en) * | 2012-06-22 | 2013-12-26 | Ajay Virkar | Metal nanowire networks and transparent conductive material |
| CN107685154A (en) * | 2017-09-07 | 2018-02-13 | 深圳赢特科技有限公司 | A kind of nano silver wire composite coating and preparation method thereof |
| CN110258106A (en) * | 2019-07-19 | 2019-09-20 | 中南林业科技大学 | A kind of preparation method of the sandwich-type flexible electromagnetic shielding material based on carbon fibre fabric, metallic nickel nano granule and graphene |
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| PENGFEI LV: "Metal-based bacterial cellulose of sandwich nanomaterials for anti-oxidation electromagnetic interference shielding", 《MATERIALS AND DESIGN》 * |
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