CN115161737A - Method for preparing electromagnetic shielding material for copper electrodeposition on surface of flexible substrate - Google Patents
Method for preparing electromagnetic shielding material for copper electrodeposition on surface of flexible substrate Download PDFInfo
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- CN115161737A CN115161737A CN202210512760.5A CN202210512760A CN115161737A CN 115161737 A CN115161737 A CN 115161737A CN 202210512760 A CN202210512760 A CN 202210512760A CN 115161737 A CN115161737 A CN 115161737A
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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
- C25D7/00—Electroplating characterised by the article coated
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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
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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
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/36—Pretreatment of metallic surfaces to be electroplated of iron or steel
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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
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/38—Pretreatment of metallic surfaces to be electroplated of refractory metals or nickel
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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
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/38—Pretreatment of metallic surfaces to be electroplated of refractory metals or nickel
- C25D5/40—Nickel; Chromium
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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
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
- H05K9/0088—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising a plurality of shielding layers; combining different shielding material structure
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
- H05K9/009—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive fibres, e.g. metal fibres, carbon fibres, metallised textile fibres, electro-conductive mesh, woven, non-woven mat, fleece, cross-linked
Abstract
The invention discloses a method for preparing an electromagnetic shielding material by copper electrodeposition on the surface of a flexible substrate, belonging to the technical field of material science and engineering. The method can endow the flexible material with electromagnetic shielding performance and further improve the performance of the flexible material. The flexible electromagnetic shielding material with high electromagnetic shielding efficiency is prepared by an electrodeposition process of copper and is obtained by further anchoring treatment. The flexible substrate includes a stainless steel mesh, a nickel mesh, a tungsten mesh, and a carbon cloth. The invention has the advantages of high efficiency, strong applicability and the like.
Description
Technical Field
The invention relates to a method for preparing an electromagnetic shielding material by copper electrodeposition on the surface of a flexible substrate, belonging to the technical field of material science and engineering.
Background
The integrated circuit is an important component of the scientific and technological development of China, and is the basis for realizing intellectualization and digitization in various industries of China. According to the statistical data of the Chinese semiconductor industry association, the following data are displayed: in 2020, the import quantity of Chinese integrated circuits is 5435 hundred million, the year-by-year increase is 22.1%, the total import amount is 24207 hundred million yuan, and the year-by-year increase is 14.8%. 4.34 trillion yuan is sold in the industry all year round in 2021, and the year-on-year growth is 20.1%; wherein the sales of the design industry is 1.65 trillion yuan, and the comparably increase is 24.1 percent; the sales of the manufacturing industry is 1.1 trillion yuan, and the year by year increases by 25.1%; the sales of the seal industry is 1.56 trillion yuan, and the sales of the seal industry is increased by 13 percent on a par. Under the economic mode of high-speed development in China, the integrated circuit technology has become one of the indispensable basic conditions in modern industry and scientific and technological development. The downstream of electromagnetic shielding (EMI) materials is a demand end, and the fields of communication equipment, computers, mobile phone terminals, automobile electronics, household appliances, national defense and military industry and the like are mainly provided. The downstream application of electromagnetic shielding is wide, and the global material market demand is rapidly increased under the drive of the rapid development of the downstream market.
As electronic products increasingly use low power, high speed, high integration circuits, these devices are more vulnerable to electromagnetic interference than ever before. Meanwhile, the increase of high-power household appliances and office automation equipment, the wide application of mobile communication and wireless networks and the like greatly increase electromagnetic interference sources. Generally, the electromagnetic wave band of common electronic products is in the range of several megahertz to 300 gigahertz, which indicates that the electromagnetic compatibility property is required by all electronic products. Therefore, it is necessary to adopt a certain technical means to enable various electronic and electrical devices in the same electromagnetic environment to work normally without interfering with the normal work of other devices. The elimination of electromagnetic interference and the protection of electromagnetic radiation can be achieved by two means, reflection and absorption of electromagnetic waves. The reflection loss process achieves the purpose of shielding mainly through reflection of electromagnetic waves, and effective reflection shielding requires materials capable of reflecting most incident electromagnetic waves. For a medium with high conductivity, such as silver, copper and other materials, a continuous conductive path formed on the surface of the medium can form effective reflection loss on electromagnetic waves, and the reflection shielding plays a main role; for media with high magnetic permeability, such as iron, magnetic steel and other materials, the absorption shield plays a main role. When electromagnetic shielding is performed through reflection loss, a series of practical application problems can be caused, for example, reflected electromagnetic waves influence normal operation of external electronic devices and the interior of the devices, and secondary electromagnetic wave radiation interference is generated. According to the electromagnetic wave theory and the interaction principle of the material and the electromagnetic wave, the more effective method is to enhance the absorption efficiency of the shielding material to the electromagnetic wave, so that the electromagnetic radiation energy is lost in the material as much as possible, and the interference to surrounding devices is reduced.
Disclosure of Invention
1. Objects of the invention
The invention aims to provide a method for preparing a novel electromagnetic shielding material, which is characterized in that copper ions are simply and efficiently deposited on a metal mesh substrate by utilizing an electroplating mode, deposited copper simple substances are more tightly combined by Joule heat treatment, a good conductive path is constructed, and the functions of electromagnetic shielding reflection and absorption are realized. The copper deposition amount is changed by adjusting the current density and time during copper deposition, and the influence of the current on the electromagnetic shielding performance during joule heat treatment is studied. Meanwhile, the applicant can obtain the electromagnetic shielding performance of the metal mesh material with low cost equivalent to or more advantageous than the metal mesh material with high cost by the technical method of the patent. The metal mesh substrate has certain flexibility, so that the material can meet the requirements of various electromagnetic shielding materials, and has high universality.
2. The invention of the technology
The key points of the invention are as follows:
a method for preparing an electromagnetic shielding material by copper electrodeposition on the surface of a flexible substrate is characterized by comprising the following steps:
(1) Mixing sodium carbonate (Na) 2 CO 3 ) 28g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 8g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 23g of the purified product was sufficiently dissolved in 1L of ultrapure water to obtain a deoiling liquid (solution A);
(2) Placing a plurality of flexible substrate materials (material A) with the size of 3cm multiplied by 6cm into the solution A, soaking for 5min to remove oil stains and other impurities on the surface of the flexible substrate materials, taking out the flexible substrate materials, and cleaning the flexible substrate materials by using ultrapure water, wherein the flexible substrate materials comprise: stainless steel mesh, nickel mesh, tungsten mesh and carbon cloth;
(3) Sulfuric acid (H) 2 SO 4 ) 100g of blue vitriod (CuSO) 4 ·5H 2 O) 50g, boric acid (H) 3 BO 3 ) 25g of copper electrodeposition solution (solution B) was prepared by sufficiently dissolving the copper electrodeposition solution in 1L of ultrapure water;
(3) Fixing the flexible substrate in the solution B through a metal clip to serve as an electrodeposition cathode for copper ion deposition, electroplating by taking a carbon rod as an electrodeposition anode, and selecting current density as 3A/dm by adopting constant current electroplating during deposition 2 、4A/dm 2 、5A/dm 2 And 6A/dm 2 Times of 100s, 200s and 300s;
(4) After deposition is finished, placing the flexible substrate (material B) with the surface completely covered by copper into an acid copper sulfate solution for storage to avoid oxidation;
(5) And (3) carrying out copper anchoring treatment on the material B in an inert gas environment glove box, wherein the treatment voltage is 6V, the current is 15A, 20A and 25A, and the treatment time is 15s, so that the material C is obtained and is used for testing the electromagnetic shielding performance.
(5) Attached drawings of the invention
FIG. 1 is a photograph of copper electrodeposition.
Fig. 2 is a photograph of a real object of copper electrodeposition on a stainless steel mesh.
FIG. 3 is a photograph of the anchor treated stainless steel mesh after electro-coppering.
FIG. 4 is the electromagnetic absorption performance of the stainless steel mesh after copper electrodeposition for 100s compared with that of the red copper mesh.
Examples of the invention
The following describes embodiments of the method of the invention:
example 1
The joule heat treatment assists the stainless steel net to electroplate the electromagnetic shielding material of copper.
First, sodium carbonate (Na) 2 CO 3 ) 28g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 8g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 23g of the mixed solution is fully dissolved in 1L of ultrapure water to prepare degreasing liquid; soaking a plurality of stainless steel nets with the size of 3cm multiplied by 6cm in the solution for 5min to remove oil stains and other impurities on the surfaces of the stainless steel nets, and taking out the stainless steel nets and cleaning the stainless steel nets with ultrapure water; then sulfuric acid (H) 2 SO 4 ) 100g of blue vitriod (CuSO) 4 ·5H 2 O) 50g, boric acid (H) 3 BO 3 ) 25g of the copper electroplating solution is fully dissolved in 1L of ultrapure water to prepare the copper electroplating solution; fixing the stainless steel mesh by using a clamp, putting the stainless steel mesh into an electroplating solution for copper ion deposition, electroplating by taking a carbon rod as an electroplating anode, and selecting current density as 6A/dm 2 The electroplating time is 300s, and after electroplating, the copper deposition metal net is placed into an acid copper sulfate solution for storage to avoid oxidation; and then, carrying out anchoring treatment on the stainless steel mesh in a glove box in an inert gas environment, wherein the treatment voltage is 6V, the current is 25A, and the treatment time is 15s, and finally, taking out the stainless steel mesh from the glove box to carry out an electromagnetic shielding performance test.
Example 2
The joule heat treatment assists the stainless steel net to electroplate the electromagnetic shielding material of copper.
First, sodium carbonate (Na) 2 CO 3 ) 28g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 8g, sodium phosphate dodecahydrate (Na) 3 PO 4 12H 2O) 23g of the purified water was sufficiently dissolved in 1L of ultrapure water to prepare a degreasing liquid; soaking a plurality of stainless steel nets with the size of 3cm multiplied by 6cm in the solution for 5min to remove oil stains and other impurities on the surfaces of the stainless steel nets, and taking out the stainless steel nets and cleaning the stainless steel nets with ultrapure water; then sulfuric acid (H) 2 SO 4 ) 100g of blue vitriod (CuSO) 4 ·5H 2 O) 50g, boric acid (H) 3 BO 3 ) 25g of the copper electroplating solution is fully dissolved in 1L of ultrapure water to prepare the copper electroplating solution; fixing the stainless steel mesh with a fixture, placing into an electroplating solution for copper ion deposition, electroplating with a carbon rod as an electroplating anode, and selecting current density of 6A/dm 2 The electroplating time is 300s, and after electroplating, the copper deposition metal net is placed into an acid copper sulfate solution for storage to avoid oxidation; then the stainless steel net is put in inert gasAnd (4) carrying out anchoring treatment in an environmental glove box, wherein the treatment voltage is 6V, the current is 20A, the treatment time is 15s, and finally taking out the glove box for carrying out an electromagnetic shielding performance test.
Example 3
The joule heat treatment assists the stainless steel net to electroplate the electromagnetic shielding material of copper.
First, sodium carbonate (Na) 2 CO 3 ) 28g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 8g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 23g of the pure mineral oil is fully dissolved in 1L of ultrapure water to prepare degreasing liquid; soaking several stainless steel nets of 3cm × 6cm size in the above solution for 5min to remove oil stain and other impurities on the surface, taking out, and cleaning with ultrapure water; then sulfuric acid (H) 2 SO 4 ) 100g of blue vitriod (CuSO) 4 ·5H 2 O) 50g, boric acid (H) 3 BO 3 ) 25g of the copper electroplating solution is fully dissolved in 1L of ultrapure water to prepare the copper electroplating solution; fixing the stainless steel mesh with a fixture, placing into an electroplating solution for copper ion deposition, electroplating with a carbon rod as an electroplating anode, and selecting current density of 6A/dm 2 The electroplating time is 300s, and after electroplating, the copper deposition metal net is placed into an acid copper sulfate solution for storage to avoid oxidation; and then, carrying out anchoring treatment on the stainless steel mesh in a glove box in an inert gas environment, wherein the treatment voltage is 6V, the current is 15A, and the treatment time is 15s, and finally taking out the stainless steel mesh from the glove box for carrying out an electromagnetic shielding performance test.
Example 4
The joule heat treatment assists the stainless steel net to electroplate the electromagnetic shielding material of copper.
First, sodium carbonate (Na) 2 CO 3 ) 28g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 8g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 23g of the mixed solution is fully dissolved in 1L of ultrapure water to prepare degreasing liquid; soaking several stainless steel nets of 3cm × 6cm size in the above solution for 5min to remove oil stain and other impurities on the surface, taking out, and cleaning with ultrapure water; then sulfuric acid (H) 2 SO 4 ) 100g of blue vitriod (CuSO) 4 ·5H 2 O) 50g, boric acid (H) 3 BO 3 ) 25g, fully dissolving in 1L of ultrapure water to prepare an electrolytic copper plating solution; fixing the stainless steel mesh with a fixture, placing into an electroplating solution for copper ion deposition, electroplating with a carbon rod as an electroplating anode, and constant current electroplating with current density of 3A/dm 2 The electroplating time is 300s, and after electroplating, the copper deposition metal net is placed into an acid copper sulfate solution for storage to avoid oxidation; and then, carrying out anchoring treatment on the stainless steel net in a glove box in an inert gas environment, wherein the treatment voltage is 6V, the current is 25A, the treatment time is 15s, and finally taking out the stainless steel net from the glove box for carrying out electromagnetic shielding performance test.
Example 5
The joule heat treatment assists the stainless steel net to electroplate the electromagnetic shielding material of copper.
First, sodium carbonate (Na) 2 CO 3 ) 28g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 8g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 23g of the mixed solution is fully dissolved in 1L of ultrapure water to prepare degreasing liquid; soaking a plurality of stainless steel nets with the size of 3cm multiplied by 6cm in the solution for 5min to remove oil stains and other impurities on the surfaces of the stainless steel nets, and taking out the stainless steel nets and cleaning the stainless steel nets with ultrapure water; then sulfuric acid (H) 2 SO 4 ) 100g of copper sulfate pentahydrate (CuSO) 4 ·5H 2 O) 50g, boric acid (H) 3 BO 3 ) 25g of the copper electroplating solution is fully dissolved in 1L of ultrapure water to prepare the copper electroplating solution; fixing the stainless steel mesh with a fixture, placing into an electroplating solution for copper ion deposition, electroplating with a carbon rod as an electroplating anode, and constant current electroplating with current density of 3A/dm 2 The electroplating time is 300s, and after electroplating, the copper deposition metal net is placed into an acid copper sulfate solution for storage to avoid oxidation; and then, carrying out anchoring treatment on the stainless steel mesh in a glove box in an inert gas environment, wherein the treatment voltage is 6V, the current is 20A, the treatment time is 15s, and finally taking out the stainless steel mesh from the glove box for carrying out electromagnetic shielding performance test.
Example 6
The joule heat treatment assists the stainless steel net to electroplate the electromagnetic shielding material of copper.
First, sodium carbonate (Na) 2 CO 3 ) 28g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 8g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 23g of the mixed solution is fully dissolved in 1L of ultrapure water to prepare degreasing liquid; soaking several stainless steel nets of 3cm × 6cm size in the above solution for 5min to remove oil stain and other impurities on the surface, taking out, and cleaning with ultrapure water; then sulfuric acid (H) 2 SO 4 ) 100g of copper sulfate pentahydrate (CuSO) 4 ·5H 2 O) 50g, boric acid (H) 3 BO 3 ) 25g of the copper electroplating solution is fully dissolved in 1L of ultrapure water to prepare the copper electroplating solution; fixing the stainless steel mesh by using a clamp, putting the stainless steel mesh into an electroplating solution for copper ion deposition, electroplating by taking a carbon rod as an electroplating anode, and selecting current density as 6A/dm 2 The electroplating time is 300s, and after electroplating, the copper deposition metal net is placed into an acid copper sulfate solution for storage to avoid oxidation; and then, carrying out anchoring treatment on the stainless steel mesh in a glove box in an inert gas environment, wherein the treatment voltage is 6V, the current is 15A, the treatment time is 15s, and finally taking out the stainless steel mesh from the glove box for carrying out an electromagnetic shielding performance test.
Example 7
The joule heat treatment assists the nickel screen to electroplate the electromagnetic shielding material of copper.
First, sodium carbonate (Na) 2 CO 3 ) 28g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 8g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 23g of the pure mineral oil is fully dissolved in 1L of ultrapure water to prepare degreasing liquid; soaking several nickel nets of 3cm × 6cm size in the above solution for 5min to remove oil stain and other impurities on the surface, taking out, and cleaning with ultrapure water; then sulfuric acid (H) 2 SO 4 ) 100g of copper sulfate pentahydrate (CuSO) 4 ·5H 2 O) 50g, boric acid (H) 3 BO 3 ) 25g of the copper electroplating solution is fully dissolved in 1L of ultrapure water to prepare the copper electroplating solution; then, the nickel mesh was fixed by a jigPutting the carbon rod into an electroplating solution for copper ion deposition, electroplating by taking the carbon rod as an electroplating anode, and selecting constant current electroplating with the current density of 6A/dm 2 The electroplating time is 300s, and after electroplating, the copper deposition metal net is placed into an acid copper sulfate solution for storage to avoid oxidation; and then, carrying out anchoring treatment on the nickel net in a glove box in an inert gas environment, wherein the treatment voltage is 6V, the current is 25A, the treatment time is 15s, and finally taking out the nickel net from the glove box for carrying out an electromagnetic shielding performance test.
Example 8
And carrying out joule heat treatment to assist the nickel screen in electroplating the electromagnetic shielding material of copper.
First, sodium carbonate (Na) 2 CO 3 ) 28g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 8g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 23g of the mixed solution is fully dissolved in 1L of ultrapure water to prepare degreasing liquid; soaking several nickel nets of 3cm × 6cm size in the above solution for 5min to remove oil stain and other impurities on the surface, taking out, and cleaning with ultrapure water; then sulfuric acid (H) 2 SO 4 ) 100g of copper sulfate pentahydrate (CuSO) 4 ·5H 2 O) 50g, boric acid (H) 3 BO 3 ) 25g of the copper electroplating solution is fully dissolved in 1L of ultrapure water to prepare the copper electroplating solution; fixing the nickel net by using a clamp, putting the nickel net into an electroplating solution for copper ion deposition, electroplating by using a carbon rod as an electroplating anode, and adopting constant current electroplating when electroplating, wherein the current density is selected to be 6A/dm 2 The electroplating time is 300s, and after electroplating, the copper deposition metal net is placed into an acid copper sulfate solution for storage to avoid oxidation; and then, carrying out anchoring treatment on the nickel net in a glove box in an inert gas environment, wherein the treatment voltage is 6V, the current is 20A, the treatment time is 15s, and finally taking out the nickel net from the glove box for carrying out an electromagnetic shielding performance test.
Example 9
The joule heat treatment assists the nickel screen to electroplate the electromagnetic shielding material of copper.
First, sodium carbonate (Na) 2 CO 3 ) 28g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 8g, twelveSodium phosphate hydrate (Na) 3 PO 4 ·12H 2 O) 23g of the pure mineral oil is fully dissolved in 1L of ultrapure water to prepare degreasing liquid; soaking several nickel nets of 3cm × 6cm size in the above solution for 5min to remove oil stain and other impurities on the surface, taking out, and cleaning with ultrapure water; then sulfuric acid (H) 2 SO 4 ) 100g of copper sulfate pentahydrate (CuSO) 4 ·5H 2 O) 50g, boric acid (H) 3 BO 3 ) 25g of the copper electroplating solution is fully dissolved in 1L of ultrapure water to prepare the copper electroplating solution; fixing the nickel net with a clamp, placing the nickel net into an electroplating solution for copper ion deposition, electroplating by taking a carbon rod as an electroplating anode, and adopting constant current electroplating when electroplating, wherein the current density is selected to be 6A/dm 2 The electroplating time is 300s, and after electroplating, the copper deposition metal net is placed into an acid copper sulfate solution for storage to avoid oxidation; and then, carrying out anchoring treatment on the nickel net in a glove box in an inert gas environment, wherein the treatment voltage is 6V, the current is 15A, the treatment time is 15s, and finally taking out the nickel net from the glove box for carrying out an electromagnetic shielding performance test.
Example 10
And the joule heat treatment assists the tungsten mesh in electroplating the electromagnetic shielding material of copper.
First, sodium carbonate (Na) 2 CO 3 ) 28g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 8g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 23g of the pure mineral oil is fully dissolved in 1L of ultrapure water to prepare degreasing liquid; soaking a plurality of tungsten nets with the size of 3cm multiplied by 6cm in the solution for 5min to remove oil stains and other impurities on the surface of the tungsten nets, and taking out the tungsten nets and cleaning the tungsten nets with ultrapure water; then sulfuric acid (H) 2 SO 4 ) 100g of blue vitriod (CuSO) 4 ·5H 2 O) 50g, boric acid (H) 3 BO 3 ) 25g, fully dissolving in 1L of ultrapure water to prepare an electrolytic copper plating solution; fixing the tungsten net with a fixture, placing the tungsten net into an electroplating solution for copper ion deposition, electroplating by using a carbon rod as an electroplating anode, and adopting constant current electroplating with current density of 6A/dm 2 The electroplating time is 300s, and after electroplating, the copper deposition metal net is placed into an acid copper sulfate solution for storage to avoid oxidation;and then anchoring the tungsten net in a glove box in an inert gas environment, wherein the processing voltage is 6V, the current is 25A, the processing time is 15s, and finally taking out the tungsten net from the glove box for testing the electromagnetic shielding performance.
Example 11
And the joule heat treatment assists the tungsten mesh in electroplating the electromagnetic shielding material of copper.
First, sodium carbonate (Na) 2 CO 3 ) 28g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 8g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 23g of the mixed solution is fully dissolved in 1L of ultrapure water to prepare degreasing liquid; soaking a plurality of tungsten nets with the size of 3cm multiplied by 6cm in the solution for 5min to remove oil stains and other impurities on the surface of the tungsten nets, and taking out the tungsten nets and cleaning the tungsten nets with ultrapure water; then sulfuric acid (H) 2 SO 4 ) 100g of copper sulfate pentahydrate (CuSO) 4 ·5H 2 O) 50g, boric acid (H) 3 BO 3 ) 25g of the copper electroplating solution is fully dissolved in 1L of ultrapure water to prepare the copper electroplating solution; fixing the tungsten net with a fixture, placing the tungsten net into an electroplating solution for copper ion deposition, electroplating by using a carbon rod as an electroplating anode, and adopting constant current electroplating with current density of 6A/dm 2 The electroplating time is 300s, and after electroplating, the copper deposition metal net is placed into an acid copper sulfate solution for storage to avoid oxidation; and then anchoring the tungsten net in a glove box in an inert gas environment, wherein the processing voltage is 6V, the current is 20A, the processing time is 15s, and finally taking out the tungsten net from the glove box for testing the electromagnetic shielding performance.
Example 12
The joule heat treatment assists the tungsten mesh to electroplate the electromagnetic shielding material of copper.
First, sodium carbonate (Na) 2 CO 3 ) 28g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 8g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 23g of the pure mineral oil is fully dissolved in 1L of ultrapure water to prepare degreasing liquid; soaking a plurality of tungsten nets with the size of 3cm multiplied by 6cm in the solution for 5min to remove oil stains and other impurities on the surface of the tungsten nets, and taking out the tungsten nets and cleaning the tungsten nets with ultrapure water; then sulfuric acid (H) 2 SO 4 ) 100g of copper sulfate pentahydrate (CuSO) 4 ·5H 2 O) 50g, boric acid (H) 3 BO 3 ) 25g, fully dissolving in 1L of ultrapure water to prepare an electrolytic copper plating solution; fixing the tungsten net with a fixture, placing the tungsten net into an electroplating solution for copper ion deposition, electroplating by using a carbon rod as an electroplating anode, and adopting constant current electroplating with current density of 6A/dm 2 The electroplating time is 300s, and after electroplating, the copper deposition metal net is placed into an acid copper sulfate solution for storage to avoid oxidation; and then anchoring the tungsten net in a glove box in an inert gas environment, wherein the processing voltage is 6V, the current is 15A, the processing time is 15s, and finally taking out the tungsten net from the glove box for testing the electromagnetic shielding performance.
Example 13
The joule heat treatment assists the stainless steel net to electroplate the electromagnetic shielding material of copper.
First, sodium carbonate (Na) 2 CO 3 ) 28g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 8g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 23g of the mixed solution is fully dissolved in 1L of ultrapure water to prepare degreasing liquid; soaking several stainless steel nets of 3cm × 6cm size in the above solution for 5min to remove oil stain and other impurities on the surface, taking out, and cleaning with ultrapure water; then sulfuric acid (H) 2 SO 4 ) 100g of blue vitriod (CuSO) 4 ·5H 2 O) 50g, boric acid (H) 3 BO 3 ) 25g of the copper electroplating solution is fully dissolved in 1L of ultrapure water to prepare the copper electroplating solution; fixing the stainless steel mesh with a fixture, placing into an electroplating solution for copper ion deposition, electroplating with a carbon rod as an electroplating anode, and selecting current density of 6A/dm 2 The electroplating time is 200s, and after electroplating, the copper deposition metal net is placed into an acid copper sulfate solution for storage to avoid oxidation; and then, carrying out anchoring treatment on the stainless steel mesh in a glove box in an inert gas environment, wherein the treatment voltage is 6V, and the current is 25A, and finally taking out the stainless steel mesh from the glove box for carrying out an electromagnetic shielding performance test.
Example 14
The joule heat treatment assists the stainless steel net to electroplate the electromagnetic shielding material of copper.
First, sodium carbonate (Na) 2 CO 3 ) 28g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 8g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 23g of the mixed solution is fully dissolved in 1L of ultrapure water to prepare degreasing liquid; soaking a plurality of stainless steel nets with the size of 3cm multiplied by 6cm in the solution for 5min to remove oil stains and other impurities on the surfaces of the stainless steel nets, and taking out the stainless steel nets and cleaning the stainless steel nets with ultrapure water; then sulfuric acid (H) 2 SO 4 ) 100g of copper sulfate pentahydrate (CuSO) 4 ·5H 2 O) 50g, boric acid (H) 3 BO 3 ) 25g of the copper electroplating solution is fully dissolved in 1L of ultrapure water to prepare the copper electroplating solution; fixing the stainless steel mesh with a fixture, placing into an electroplating solution for copper ion deposition, electroplating with a carbon rod as an electroplating anode, and selecting current density of 6A/dm 2 The electroplating time is 100s, and after electroplating, the copper deposition metal net is placed into an acid copper sulfate solution for storage to avoid oxidation; and then, carrying out anchoring treatment on the stainless steel mesh in a glove box in an inert gas environment, wherein the treatment voltage is 6V, the current is 25A, and finally taking out the stainless steel mesh from the glove box to carry out electromagnetic shielding performance test.
Claims (1)
1. A method for preparing an electromagnetic shielding material by copper electrodeposition on the surface of a flexible substrate is characterized by comprising the following steps:
(1) Mixing sodium carbonate (Na) 2 CO 3 ) 28g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 8g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 23g of the purified water was sufficiently dissolved in 1L of ultrapure water to obtain a deoiling liquid (solution A);
(2) Putting a plurality of flexible substrate materials (material A) with the size of 3cm multiplied by 6cm into the solution A, soaking for 5min to remove oil stains and other impurities on the surface of the flexible substrate materials, taking out and cleaning the flexible substrate materials by using ultrapure water, wherein the flexible substrate materials comprise: stainless steel mesh, nickel mesh, tungsten mesh and carbon cloth;
(3) Sulfuric acid (H) 2 SO 4 ) 100g, fiveBlue vitriod (CuSO) 4 ·5H 2 O) 50g, boric acid (H) 3 BO 3 ) 25g of the copper electrodeposition solution was prepared by sufficiently dissolving the copper electrodeposition solution in 1L of ultrapure water (solution B);
(3) Fixing the flexible substrate in the solution B through a metal clamp to serve as an electrodeposition negative electrode for copper ion deposition, electroplating by taking a carbon rod as an electrodeposition positive electrode, and performing constant current electroplating during deposition with the current density of 3A/dm 2 、4A/dm 2 、5A/dm 2 And 6A/dm 2 Times of 100s, 200s and 300s;
(4) After deposition is finished, placing the flexible substrate (material B) with the surface completely covered by copper into an acid copper sulfate solution for storage to avoid oxidation;
(5) And (3) carrying out copper anchoring treatment on the material B in an inert gas environment glove box, wherein the treatment voltage is 6V, the current is 15A, 20A and 25A, and the treatment time is 15s, so that the material C is obtained and is used for testing the electromagnetic shielding performance.
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