CN114000348A - Silver-plated conductive fabric and preparation method and application thereof - Google Patents
Silver-plated conductive fabric and preparation method and application thereof Download PDFInfo
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- CN114000348A CN114000348A CN202111431664.XA CN202111431664A CN114000348A CN 114000348 A CN114000348 A CN 114000348A CN 202111431664 A CN202111431664 A CN 202111431664A CN 114000348 A CN114000348 A CN 114000348A
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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
- 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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- 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
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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
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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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
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
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Abstract
The invention provides a silver-plated conductive fabric and a preparation method and application thereof, belonging to the technical field of conductive fabric materials. The silver-plated conductive fabric comprises a sulfydryl modified fabric and a composite conductive silver layer positioned on the surface of the sulfydryl modified fabric; the composite conductive silver layer comprises a plurality of silver layers and mercapto compound adsorption layers which are alternately laminated; the bottom layer and the surface layer of the composite conductive silver layer are silver layers; the mercapto compound adsorption layer is formed from a mercapto group-containing co-reducing agent. According to the invention, the sulfhydryl modified fabric is combined with the silver layer through a chemical bond, so that the combination strength of the sulfhydryl modified fabric and the silver layer is high; the silver layer is connected with the silver layer through the mercapto compound adsorption layer, and the mercapto group in the mercapto compound adsorption layer can form a stable silver-mercapto complex with the silver, so that the binding force between the silver layer and the silver layer is strong, and the washing resistance of the conductive fabric is further remarkably improved; the silver layer endows the silver-plated conductive fabric with excellent conductivity.
Description
Technical Field
The invention relates to the technical field of conductive fabric materials, in particular to a silver-plated conductive fabric and a preparation method and application thereof.
Background
The intelligent wearable garment mainly adopts the conductive fabric as an electrode material, can be used for collecting and transmitting electric signals such as electrocardio and the like, converts the motion of a human body and the like into the electric signals to sense the motion of the human body, and is used for energy collection and the like as an electrode of a friction generator. Therefore, textile electrode materials have important uses in smart wear garments. Conductive fabrics as electrode materials generally have a conductive property by compounding with a conductive material such as metal, using a textile as a substrate. However, in the using process of the intelligent wearable garment, the conductivity of the conductive fabric is seriously reduced by water washing and the like, so that the effectiveness of the intelligent wearable garment is influenced.
Meanwhile, electronic products and equipment generate electromagnetic wave radiation to different degrees, and the electromagnetic wave radiation not only causes mutual interference among the electronic products, but also harms human health. The metallized fabric has the performances of electromagnetic radiation resistance, static resistance, bacteria resistance and the like, so the metallized fabric becomes a new functional textile material and has wide application in the fields of electromagnetic shielding, medical treatment, military, clothes and the like.
Compared with copper plated and nickel plated fabrics, the silver plated fabric has higher electromagnetic shielding efficiency and conductivity, is soft, breathable and antibacterial, and can be widely applied to the fields of fabric electrodes of intelligent wearable clothes, electromagnetic shielding and special protection. For example, the prior art "research on chemical silver plating and silver plating layer protection of von willi dacron [ D ]. university of shanghai, 2014" discloses a double-layer chemical silver-plated dacron fabric, in which a silver plating layer is uniformly and densely covered on the surface of the dacron fabric. However, the double-layer chemical silver-plated polyester fabric has poor bonding force between the silver plating layer and the polyester fabric, so that the washing resistance of the double-layer chemical silver-plated polyester fabric is poor.
Disclosure of Invention
In view of the above, the present invention provides a silver-plated conductive fabric, and a preparation method and an application thereof.
In order to realize the invention, the invention provides a silver-plated conductive fabric, which comprises a mercapto-modified fabric and a composite conductive silver layer positioned on the surface of the mercapto-modified fabric; the composite conductive silver layer comprises a plurality of silver layers and mercapto compound adsorption layers which are alternately laminated; the bottom layer and the surface layer of the composite conductive silver layer are silver layers; the mercapto compound adsorption layer is formed from a mercapto group-containing co-reducing agent.
Preferably, the number of silver layers in the silver-plated conductive fabric is more than or equal to 2.
Preferably, the thiol-containing co-reducing agent includes one or more of cysteine, acetylcysteine, thiomalic acid, dimercaptosuccinic acid, and thiol.
Preferably, the silver plating amount of the silver-plated conductive fabric is 50-500%.
Preferably, the material of the fabric in the sulfhydryl modified fabric comprises one or more of cotton, viscose fiber, tencel, terylene, spandex and chitosan.
The invention provides a preparation method of the silver-plated conductive fabric in the technical scheme, which comprises the following steps:
(1) mixing the mercapto-modified fabric, silver ammonia solution and composite reducing agent, and carrying out reduction-complexation reaction to form a silver layer on the surface of the mercapto-modified fabric, thereby obtaining a silver-containing fabric; the composite reducing agent comprises a main reducing agent and a sulfydryl-containing auxiliary reducing agent;
(2) placing the silver-containing fabric in a mercapto-containing auxiliary reducing agent solution for adsorption, and forming a mercapto compound adsorption layer on the silver layer surface of the silver-containing fabric;
(3) and (3) repeating the operations of the steps (1) to (2) for a plurality of times on the surface of the sulfhydryl compound adsorption layer, and then repeating the operation of the step (1) for 1 time to obtain the silver-plated conductive fabric.
Preferably, the molar ratio of the main reducing agent to the auxiliary reducing agent containing sulfydryl in the composite reducing agent is 7: 3-9: 1;
the main reducing agent comprises one or more of glucose, galactose, maltose and tartaric acid.
The molar ratio of the composite reducing agent to the silver ions in the silver ammonia solution is 1: 1-2: 1.
Preferably, in the step (1), the concentration of the silver ammonia solution is 0.1-0.3 mol/L;
the dosage ratio of the silver ammonia solution to the mercapto-modified fabric is 1-5 mL/cm2；
The temperature of the reduction-complexation reaction is 30-60 ℃, and the time is 0.5-2 h.
Preferably, in the step (2), the concentration of the solution of the auxiliary reducing agent is 0.05-0.5 mol/L;
the dosage ratio of the auxiliary reducing agent solution to the silver-containing fabric is 1-5 mL/cm2；
The adsorption temperature is 30-80 ℃, and the time is 0.5-2 h.
The invention provides application of the silver-plated conductive fabric in the technical scheme or the silver-plated conductive fabric obtained by the preparation method in the technical scheme in an electrode material or an electromagnetic shielding material.
The invention provides a silver-plated conductive fabric, which comprises a sulfydryl modified fabric and a composite conductive silver layer positioned on the surface of the sulfydryl modified fabric; the composite conductive silver layer comprises a plurality of silver layers and mercapto compound adsorption layers which are alternately laminated; the bottom layer and the surface layer of the composite conductive silver layer are silver layers; the mercapto compound adsorption layer is formed from a mercapto group-containing co-reducing agent. In the invention, the sulfhydryl modified fabric is combined with the silver layer through a chemical bond (Ag-S bond), so that the combination strength of the sulfhydryl modified fabric and the silver layer is high; the silver layer is connected with the silver layer through the mercapto compound adsorption layer, and the mercapto group in the mercapto compound adsorption layer can form a stable silver-mercapto complex with the silver, so that the bonding force between the silver layer and the silver layer is strong, and the water washing resistance of the fabric is further remarkably improved; meanwhile, the silver has excellent conductive performance, so that the silver-plated conductive fabric is endowed with excellent conductive performance. As shown in the embodiment results, the initial resistance of the silver-plated conductive fabric provided by the invention is 0.01-0.077 omega/sq, and the resistance after 200-500 times of washing is 0.57-3.20 omega/sq.
The invention provides a preparation method of the silver-plated conductive fabric in the technical scheme. The invention adopts a stepwise multi-stage in-situ reduction silver deposition mode to prepare the high-stability silver-plated conductive fabric with multiple aggregated conductive silver layers, specifically, the surface of the sulfydryl modified fabric is provided with sulfydryl, a main reducing agent in a composite reducing agent reduces silver ions in a silver ammonia solution into silver simple substance nano particles, and an auxiliary reducing agent containing sulfydryl can play a role in weak reduction and can also increase the sulfydryl content in a system, so that the silver simple substance and the sulfydryl fully undergo a complex reaction to form a stable silver-sulfydryl complex. The sulfhydryl modified fabric is used as a raw material, so that the binding force between the fabric and the silver layer is strong; meanwhile, the auxiliary reducing agent in the composite reducing agent is a sulfydryl compound, and the existence of sulfydryl also improves the binding force among silver simple substance nanoparticles in the silver layer; the mercapto compound adsorption layer enhances the binding force between two adjacent silver layers, so the method can effectively improve the washing resistance of the silver-plated conductive fabric, and can solve the problem that the silver layer of the silver-plated conductive fabric with a single thick silver layer is easy to fall off in the washing process.
Drawings
FIG. 1 is an SEM image of a mercapto-modified polyester fabric;
fig. 2 is an SEM image of the silver-plated conductive fabric prepared in example 1;
fig. 3 is an SEM image of the silver-plated conductive fabric prepared in comparative example 1;
FIG. 4 shows the results of the water washing resistance and conductivity tests of the silver-plated conductive fabrics prepared in examples 1 to 3.
Detailed Description
The invention provides a silver-plated conductive fabric, which comprises a sulfydryl modified fabric and a composite conductive silver layer positioned on the surface of the sulfydryl modified fabric; the composite conductive silver layer comprises a plurality of silver layers and mercapto compound adsorption layers which are alternately laminated; the bottom layer and the surface layer of the composite conductive silver layer are silver layers; the mercapto compound adsorption layer is formed from a mercapto group-containing co-reducing agent.
In the present invention, all the raw material components are commercially available products well known to those skilled in the art unless otherwise specified.
In the invention, the material of the fabric in the sulfhydryl modified fabric preferably comprises one or more of cotton, viscose fiber, tencel, terylene, spandex and chitosan, and more preferably comprises cotton, viscose fiber, tencel, terylene, spandex, chitosan, cotton and terylene blended fabric and cotton and spandex blended fabric. In the present invention, the mercapto group in the mercapto-modified fabric is preferably derived from a mercapto compound, which preferably includes a mercapto group-containing silane coupling agent and/or a mercapto group-containing organic acid; the mercapto silane coupling agent preferably comprises one or more of 3-mercaptopropyltrimethoxysilane, 3-mercaptopropyltriethoxysilane and mercaptopropylmethyldimethoxysilane; the sulfhydryl-containing organic acid preferably comprises one or more of cysteine, acetylcysteine, thioglycolic acid, mercaptopropionic acid, dimercaptosuccinic acid and thiomalic acid.
In the present invention, the method for preparing the mercapto-modified fabric preferably comprises the steps of: and modifying the fabric by utilizing a sulfhydryl compound to obtain the sulfhydryl modified fabric.
In the present invention, the fabric is preferably post-wash activated prior to use; the washing preferably comprises alcohol washing and water washing, and the alcohol for alcohol washing preferably comprises ethanol and/or methanol; the washing is preferably carried out under ultrasonic conditions, and the conditions of the ultrasonic washing are not particularly limited in the invention, so that dust and grease pollutants on the surface of the fabric can be removed. In the present invention, the activation is preferably acid activation and/or base activation; the acid for acid activation is preferably a hydrochloric acid solution, and the concentration of the hydrochloric acid solution is preferably 0.1-1 mol/L, and more preferably 0.5-0.8 mol/L; the dosage of the acid is not specially limited, and the fabric can be immersed; the temperature of acid activation is preferably 30-50 ℃, and more preferably 30-40 ℃; the acid activation time is preferably 0.5-2 h, and more preferably 0.5-1 h; the alkali activating alkali is preferably NaOH solution, and the concentration of the NaOH solution is preferably 30-300 g/L, and more preferably 30-50 g/L; the dosage of the alkali is not specially limited, and the fabric can be immersed; the temperature of alkali activation is preferably 30-70 ℃, and more preferably 50-70 ℃; the alkali activation time is preferably 0.5-2 h, and more preferably 0.5-1 h; the activation aims to hydrolyze the fiber part in the fabric, increase the hydroxyl on the fiber surface, and facilitate the grafting reaction with mercapto compounds such as silane coupling agent, so that the fabric has mercapto groups, and the mercapto groups can be combined with silver through chemical bonds, thereby greatly improving the bonding force between the fabric and the silver layer. After the activation, the invention preferably further comprises washing the activated fabric to be neutral and then drying the fabric; in the present invention, the drying temperature and time are not particularly limited, and the drying may be carried out to a constant weight.
In the present invention, the mercapto compound is preferably used in the form of a mercapto compound solution, and the concentration of the mercapto compound solution is preferably 0.05 to 0.5mol/L, more preferably 0.1 to 0.4mol/L, and further preferably 0.2 to 0.3 mol/L. In the present invention, the ratio of the amount of the substance of the mercapto compound to the area of the fabric is preferably 0.5 to 25 mol: 1m2More preferably 5 to 20 mol: 1m2More preferably 10 to 15 mol: 1m2. In the invention, the modification temperature is preferably 30-100 ℃, and more preferably 80-100 ℃; the modification time is preferably 0.5-5 h, and more preferably 1-2 h. In the invention, in the modification process, the mercapto compound is grafted to the surface of the fabric, so that the fabric is provided with mercapto; when the mercapto compound is a mercapto silane coupling agent, hydroxyl in the fabric and silanol in the mercapto silane coupling agent are subjected to condensation reaction to form a Si-O-C bond; when the sulfhydryl compound is organic acid containing sulfhydryl, hydroxyl in the fabric and carboxyl in the organic acid containing sulfhydryl are subjected to esterification reaction to form ester bond, so that the binding force between the fabric and a silver layer is improved, and a foundation is laid for obtaining the silver-plated conductive fabric with high stability.
In the invention, the sulfhydryl compound adsorption layer is formed by a sulfhydryl-containing auxiliary reducing agent, and the sulfhydryl-containing auxiliary reducing agent comprises one or more of cysteine, acetylcysteine, thiomalic acid, dimercaptosuccinic acid and thiol. In the invention, the mercapto-containing co-reducing agent contains a plurality of functional groups, wherein cysteine contains mercapto, amino and carboxyl, acetylcysteine, thiomalic acid and dimercaptosuccinic acid contain mercapto and carboxyl, and the mercaptan contains mercapto, and the functional groups can adsorb silver, thereby not only increasing the binding force between a silver layer and a silver layer, but also increasing the binding force between silver single-substance nanoparticles and silver single-substance nanoparticles in the silver layer.
In the invention, the number of silver layers in the silver-plated conductive fabric is preferably not less than 2, more preferably 2-4, and further preferably 2-3. In the invention, the silver plating amount (i.e. the proportion of the mass of silver to the mass of the fabric) of the silver-plated conductive fabric is preferably 50-500%, and more preferably 100-200%.
The invention provides a preparation method of the silver-plated conductive fabric in the technical scheme, which comprises the following steps:
(1) mixing the mercapto-modified fabric, silver ammonia solution and composite reducing agent, and carrying out reduction-complexation reaction to form a silver layer on the surface of the mercapto-modified fabric, thereby obtaining a silver-containing fabric; the composite reducing agent comprises a main reducing agent and a sulfydryl-containing auxiliary reducing agent;
(2) placing the silver-containing fabric in a mercapto-containing auxiliary reducing agent solution for adsorption, and forming a mercapto compound adsorption layer on the silver layer surface of the silver-containing fabric;
(3) and (3) repeating the operations of the steps (1) to (2) for a plurality of times on the surface of the sulfhydryl compound adsorption layer, and then repeating the operation of the step (1) for 1 time to obtain the silver-plated conductive fabric.
Mixing a sulfydryl modified fabric, a silver ammonia solution and a composite reducing agent, and carrying out reduction-complexation reaction to form a silver layer on the surface of the sulfydryl modified fabric to obtain a silver-containing fabric; the composite reducing agent comprises a main reducing agent and a sulfydryl-containing auxiliary reducing agent.
In the invention, the concentration of the silver ammonia solution is preferably 0.1-0.3 mol/L, more preferably 0.15-0.25 mol/L, and even more preferably 0.2 mol/L. In the invention, the dosage ratio of the silver ammonia solution to the sulfydryl modified fabric is preferably 1-5 mL/cm2More preferably 2 to 4mL/cm2More preferably 3mL/cm2。
In the invention, the composite reducing agent comprises a main reducing agent and a sulfydryl-containing auxiliary reducing agent; the main reducing agent preferably comprises one or more of glucose, galactose, maltose and tartaric acid; the type of the sulfydryl-containing auxiliary reducing agent is preferably the same as the selectable type of the sulfydryl-containing auxiliary reducing agent, and the description is omitted; the molar ratio of the main reducing agent to the mercapto-containing auxiliary reducing agent is preferably 7:3 to 9:1, more preferably 4:1 to 9:1, and even more preferably 4:1 to 5: 1. In the invention, the composite reducing agent is preferably used in the form of a composite reducing agent solution, and the concentration of the main reducing agent in the composite reducing agent solution is preferably 0.1-0.2 mol/L, and more preferably 0.1-0.15 mol/L; the solvent in the composite reducing agent solution is preferably water. In the invention, the composite reducing agent solution preferably further comprises a stabilizer, and the stabilizer is preferably ethanol; the volume concentration of the stabilizer in the composite reducing agent solution is preferably 10-25%, and more preferably 15-18%; according to the invention, the storage time of the composite reducing agent solution can be prolonged by adding the stabilizing agent into the composite reducing agent solution.
In the invention, the molar ratio of the composite reducing agent to the silver ions in the silver ammonia solution is preferably 1: 1-2: 1, more preferably 1.2: 1-1.8: 1, and further preferably 1.5: 1-1.6: 1.
In the invention, the temperature of the reduction-complexation reaction is preferably 30-60 ℃, and more preferably 40-50 ℃; the time of the reduction-complexation reaction is preferably 0.5-2 h, and more preferably 1-1.5 h; in the reduction-complexation reaction process, silver ions in the silver-ammonia solution are reduced into silver simple substance nanoparticles, and the silver simple substance nanoparticles and sulfydryl in the sulfydryl modified fabric are subjected to complexation reaction to generate a stable silver-sulfydryl complex; meanwhile, the composite reducing agent can also adjust the speed of reducing and complexing deposition of silver ions on the surface of the mercapto-modified fabric, and a compact silver layer is formed on the surface of the mercapto-modified fabric; moreover, the sulfydryl-containing auxiliary reducing agent in the composite reducing agent can enhance the bonding strength between the silver nanoparticles in the silver layer.
After the silver-containing fabric is obtained, the silver-containing fabric is placed in a mercapto-containing auxiliary reducing agent solution for adsorption, and a mercapto compound adsorption layer is formed on the surface of the silver layer of the silver-containing fabric.
In the present invention, the mercapto group-containing coreductive agent in the mercapto group-containing coreductive agent solution is preferably the same as the mercapto group-containing coreductive agentThe selectable types of the same are the same, and are not described herein again; the concentration of the sulfydryl-containing auxiliary reducing agent solution is preferably 0.05-0.5 mol/L, more preferably 0.1-0.4 mol/L, and further preferably 0.2-0.3 mol/L; the dosage ratio of the auxiliary reducing agent solution to the silver-containing fabric is preferably 1-5 mL/cm2More preferably 2 to 4mL/cm2More preferably 3mL/cm2. In the invention, the adsorption temperature is preferably 30-80 ℃, and more preferably 50-60 ℃; the adsorption time is preferably 0.5-2 h, and more preferably 1-1.5 h. In the invention, during the adsorption process, the mercapto group in the mercapto group-containing auxiliary reducing agent and the silver in the silver layer are subjected to a complex reaction to form a stable silver-mercapto complex, so that the bonding strength between the mercapto compound adsorption layer and the silver layer in the silver-containing fabric is improved.
After the sulfhydryl compound adsorption layer is obtained, the operations of the steps (1) to (2) are repeated for a plurality of times on the surface of the sulfhydryl compound adsorption layer, and then the operation of the step (1) is repeated for 1 time to obtain the silver-plated conductive fabric.
In the present invention, the number of times of repeating the operations of the steps (1) to (2) is preferably not less than 0, more preferably 0 to 2 times, and still more preferably 1 time.
The method adopts a step-by-step multi-stage in-situ reduction silver deposition mode, silver is plated on the surface of the fabric modified by sulfydryl, the binding force between the silver layer and the fabric can be enhanced, and a good foundation is laid for high washability; when the first silver layer is prepared, the speed of silver ion reduction deposition on the surface of the fabric can be adjusted by using a composite reducing agent, so that a uniform and compact silver layer is obtained; meanwhile, the mercapto group of the auxiliary reducing agent can also enhance the binding force between silver particles in the silver layer, thereby enhancing the washability of the silver-plated fabric; the auxiliary reducing agent containing sulfydryl is used for enhancing the binding force between two silver layers, so that the defect that a single-layer thick silver layer is easy to fall off in the washing process is avoided. Therefore, the preparation method provided by the invention can improve the binding force between the silver layer and the fabric and between the silver layers, thereby greatly improving the washing fastness of the silver-plated conductive fabric.
The invention also provides the application of the silver-plated conductive fabric in the technical scheme or the silver-plated conductive fabric obtained by the preparation method in the technical scheme in an electrode material or an electromagnetic shielding material. In the invention, the electrode material is preferably an electrode material for intelligent wearable clothes; the intelligent wearing clothes preferably comprise intelligent wearing clothes for electrocardiogram monitoring; the electromagnetic shielding material is preferably an electromagnetic shielding material for electromagnetic shielding clothes.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Sequentially carrying out ethanol ultrasonic washing and water ultrasonic washing on a polyester fabric (3cm multiplied by 3cm), treating a NaOH aqueous solution with the concentration of 30g/L for 1h at the temperature of 70 ℃, then washing the polyester fabric to be neutral, and drying the polyester fabric to constant weight to obtain an activated fabric; and (3) placing the activated fabric in 10mL of 3-mercaptopropyl trimethoxy silane solution with the concentration of 0.05mol/L, and modifying for 60min at the temperature of 100 ℃ to obtain the mercapto-modified fabric.
(2)0.0006mol of glucose, 0.0002mol of tartaric acid and 0.0001mol of cysteine are dissolved in 10mL of water, 2mL of stabilizing agent ethanol is added and mixed evenly to obtain the compound reducing agent solution.
(3) Placing the mercapto-modified fabric into 10mL of silver-ammonia solution with the concentration of 0.15mol/L, adding the composite reducing agent solution obtained in the step (2), mixing, and carrying out reduction-complexation reaction at 30 ℃ for 70min to form a silver layer on the surface of the mercapto-modified fabric, so as to obtain a silver-containing fabric;
(4) placing the silver layer-containing fabric in 10mL cysteine solution with the concentration of 0.05mol/L, adsorbing for 50min at 40 ℃, and forming a sulfhydryl compound adsorption layer on the surface of the silver layer; and (3) then placing the silver-plated conductive fabric into 10mL of silver-ammonia solution with the concentration of 0.05mol/L, adding the composite reducing agent solution obtained in the step (2), carrying out reduction-complexation reaction for 70min at 30 ℃, forming a silver layer on the surface of the mercapto compound adsorption layer, washing with water, and drying to constant weight to obtain the silver-plated conductive fabric (two silver layers).
Example 2
(1) Sequentially carrying out ethanol ultrasonic washing and water ultrasonic washing on a polyester fabric (3cm multiplied by 3cm), treating a NaOH aqueous solution with the concentration of 30g/L for 1.5h at the temperature of 60 ℃, then washing the polyester fabric to be neutral, and drying the polyester fabric to constant weight to obtain an activated fabric; and (3) placing the activated fabric into 10mL of 3-mercaptopropyltriethoxysilane solution with the concentration of 0.5mol/L, and modifying for 60min at the temperature of 100 ℃ to obtain the mercapto-modified fabric.
(2)0.002mol of glucose, 0.0004mol of maltose and 0.0004mol of cysteine are dissolved in 20mL of water, and 4mL of stabilizing agent ethanol is added and mixed uniformly to obtain the composite reducing agent solution.
(3) Placing the mercapto-modified fabric into 20mL of silver-ammonia solution with the concentration of 0.2mol/L, adding the composite reducing agent solution obtained in the step (2), mixing, and carrying out reduction-complexation reaction at 35 ℃ for 60min to form a silver layer on the surface of the mercapto-modified fabric, so as to obtain a silver-containing fabric;
(4) placing the silver layer-containing fabric in 20mL of 0.2mol/L thiomalic acid solution, and adsorbing for 60min at the temperature of 30 ℃ to form a sulfhydryl compound adsorption layer on the surface of the silver layer; and (3) then placing the silver-plated conductive fabric into 20mL of silver-ammonia solution with the concentration of 0.2mol/L, adding the composite reducing agent solution obtained in the step (2), carrying out reduction-complexation reaction for 60min at 35 ℃, forming a silver layer on the surface of the mercapto compound adsorption layer, washing with water, and drying to constant weight to obtain the silver-plated conductive fabric (two silver layers).
Example 3
(1) Sequentially carrying out ethanol ultrasonic washing and water ultrasonic washing on a polyester fabric (3cm multiplied by 3cm), treating a NaOH aqueous solution with the concentration of 30g/L for 0.8h at the temperature of 70 ℃, then washing the polyester fabric to be neutral, and drying the polyester fabric to constant weight to obtain an activated fabric; and (3) placing the activated fabric into 10mL of mercaptopropyl methyl dimethoxy silane solution with the concentration of 0.8mol/L, and adsorbing for 60min at the temperature of 100 ℃ to obtain the mercapto-modified fabric.
(2) Dissolving 0.0015mol of glucose, 0.0003mol of galactose and 0.0002mol of cysteine in 15mL of water, adding 3mL of stabilizer ethanol, and uniformly mixing to obtain a composite reducing agent solution.
(3) Placing the mercapto-modified fabric into 15mL of silver-ammonia solution with the concentration of 0.2mol/L, adding the composite reducing agent solution obtained in the step (2), mixing, and carrying out reduction-complexation reaction at 40 ℃ for 40min to form a silver layer on the surface of the mercapto-modified fabric, so as to obtain a silver-containing fabric;
(4) placing the silver layer-containing fabric in 15mL of acetylcysteine solution with the concentration of 0.2mol/L, adsorbing for 90min at the temperature of 30 ℃, and forming a sulfhydryl compound adsorption layer on the surface of the silver layer; then placing the silver-ammonia solution into 15mL of silver-ammonia solution with the concentration of 0.2mol/L, adding the composite reducing agent solution obtained in the step (2), carrying out reduction-complexation reaction for 40min at 45 ℃, forming a silver layer on the surface of the mercapto compound adsorption layer, washing with water, and drying to constant weight to obtain a two-silver-layer conductive fabric;
(5) and (4) repeating the operation of the step (4) for 2 times to obtain the silver-plated conductive fabric (four silver layers).
Example 4
(1) Sequentially carrying out ethanol ultrasonic washing and water ultrasonic washing on cotton and polyester blended fabric (3cm multiplied by 3cm), treating NaOH aqueous solution with the concentration of 30g/L for 1h at the temperature of 65 ℃, then washing the fabric to be neutral, and drying the fabric to be constant in weight to obtain activated fabric; and (3) placing the activated fabric in 10mL of acetylcysteine solution with the concentration of 0.5mol/L, and modifying for 30min at the temperature of 100 ℃ to obtain the sulfhydryl modified fabric.
(2) Dissolving 0.0012mol of maltose, 0.00025mol of tartaric acid and 0.0003mol of cysteine in 13mL of water, adding 3mL of stabilizer ethanol, and uniformly mixing to obtain a composite reducing agent solution;
(3) placing the mercapto-modified fabric into 13mL of silver ammonia solution with the concentration of 0.18mol/L, adding the composite reducing agent solution obtained in the step (2), and carrying out reduction-complexation reaction at 35 ℃ for 75min to form a silver layer on the surface of the mercapto-modified fabric, so as to obtain a silver-containing fabric;
(4) placing the silver layer-containing fabric in 10mL of acetylcysteine solution with the concentration of 0.1mol/L, adsorbing for 30min at 35 ℃, and forming a sulfhydryl compound adsorption layer on the surface of the silver layer; and (3) then placing the silver-plated conductive fabric into 10mL of silver-ammonia solution with the concentration of 0.18mol/L, adding the composite reducing agent solution obtained in the step (2), carrying out reduction-complexation reaction for 75min at 35 ℃, and forming a silver layer on the surface of the mercapto compound adsorption layer to obtain the silver-plated conductive fabric (two silver layers).
Example 5
(1) Sequentially carrying out ethanol ultrasonic washing and water ultrasonic washing on a chitosan fabric (3cm multiplied by 3cm), treating a NaOH aqueous solution with the concentration of 30g/L for 1h at the temperature of 70 ℃, then washing the chitosan fabric to be neutral, and drying the chitosan fabric to constant weight to obtain an activated fabric; and (3) placing the activated fabric in 10mL of 0.8mol/L sulfo-malic acid solution, and modifying for 45h at 80 ℃ to obtain the sulfhydryl modified fabric.
(2) Dissolving 0.0013mol of galactose, 0.00028mol of tartaric acid and 0.00018mol of cysteine in 12mL of water, adding 2.5mL of stabilizer ethanol, and uniformly mixing to obtain a composite reducing agent solution;
(3) placing the mercapto-modified fabric into 12mL of silver ammonia solution with the concentration of 0.24mol/L, adding the composite reducing agent solution obtained in the step (2), and carrying out reduction-complexation reaction at 50 ℃ for 75min to form a silver layer on the surface of the mercapto-modified fabric, so as to obtain a silver-containing fabric;
(4) placing the silver layer-containing fabric in 10mL of acetylcysteine solution with the concentration of 0.25mol/L, adsorbing for 40min at 40 ℃, and forming a sulfhydryl compound adsorption layer on the surface of the silver layer; and (3) then placing the silver-plated conductive fabric into 12mL of silver-ammonia solution with the concentration of 0.24mol/L, adding the composite reducing agent solution obtained in the step (2), carrying out reduction-complexation reaction for 75min at 50 ℃, and forming a silver layer on the surface of the mercapto compound adsorption layer to obtain the silver-plated conductive fabric (two silver layers).
Example 6
(1) Sequentially carrying out ethanol ultrasonic washing and water ultrasonic washing on a polyester fabric (3cm multiplied by 3cm), treating a NaOH aqueous solution with the concentration of 30g/L for 1h at the temperature of 70 ℃, then washing the polyester fabric to be neutral, and drying the polyester fabric to constant weight to obtain an activated fabric; and (3) placing the activated fabric in 10mL of 3-mercaptopropyl trimethoxy silane solution with the concentration of 0.8mol/L, and modifying for 60min at the temperature of 100 ℃ to obtain the mercapto-modified fabric.
(2) Dissolving 0.0007mol of galactose, 0.00018mol of tartaric acid and 0.0001mol of cysteine in 10mL of water, adding 1.5mL of stabilizer ethanol, and uniformly mixing to obtain a composite reducing agent solution;
(3) placing the mercapto-modified fabric into 10mL of silver ammonia solution with the concentration of 0.14mol/L, adding the composite reducing agent solution obtained in the step (2), and carrying out reduction-complexation reaction at 40 ℃ for 60min to form a silver layer on the surface of the mercapto-modified fabric, so as to obtain a silver-containing fabric;
(4) spraying 10mL of acetylcysteine solution with the concentration of 0.08mol/L on the fabric containing the silver layer for 5 times, adsorbing for 30min at the temperature of 30 ℃, and forming a sulfhydryl compound adsorption layer on the surface of the silver layer; and (3) then placing the silver-plated conductive fabric into 10mL of silver-ammonia solution with the concentration of 0.14mol/L, adding the composite reducing agent solution obtained in the step (2), carrying out reduction-complexation reaction for 60min at 40 ℃, and forming a silver layer on the surface of the mercapto compound adsorption layer to obtain the silver-plated conductive fabric (two silver layers).
Example 7
(1) Sequentially carrying out ethanol ultrasonic washing and water ultrasonic washing on a cotton fabric (3cm multiplied by 3cm), treating the cotton fabric with NaOH aqueous solution with the concentration of 30g/L for 1h at the temperature of 65 ℃, then washing the cotton fabric with water to be neutral, and drying the cotton fabric to be constant in weight to obtain an activated fabric; and (3) placing the activated fabric in 10mL of 1mol/L acetylcysteine solution, and modifying for 60min at 100 ℃ to obtain the sulfydryl modified fabric.
(2) Dissolving 0.0009mol of maltose, 0.0002mol of galactose and 0.0002mol of cysteine in 9mL of water, adding 2mL of stabilizer ethanol, and uniformly mixing to obtain a composite reducing agent solution;
(3) placing the mercapto-modified fabric into 9mL of silver ammonia solution with the concentration of 0.24mol/L, adding the composite reducing agent solution obtained in the step (2), and carrying out reduction-complexation reaction at 32 ℃ for 70min to form a silver layer on the surface of the mercapto-modified fabric, so as to obtain a silver-containing fabric;
(4) placing the silver layer-containing fabric in 10mL of dimercaptosuccinic acid solution with the concentration of 0.2mol/L, adsorbing for 70min at the temperature of 50 ℃, and forming a mercapto compound adsorption layer on the surface of the silver layer; and (3) then placing the silver-plated conductive fabric into 9mL of silver-ammonia solution with the concentration of 0.24mol/L, adding the composite reducing agent solution obtained in the step (2), and carrying out reduction-complexation reaction for 70min at the temperature of 32 ℃ to obtain the silver-plated conductive fabric (two silver layers).
Comparative example 1
The silver-plated conductive fabric was prepared according to the method of example 1, and the silver-layer-containing fabric obtained in step (3) in example 1 was the silver-plated conductive fabric (a silver layer).
Comparative example 2
A silver-plated conductive fabric was prepared according to the method of example 2, except that the step (4) was replaced with: and (3) placing the fabric containing the silver layer into 20mL of silver ammonia solution with the concentration of 0.2mol/L, adding the composite reducing agent solution obtained in the step (2), carrying out reduction-complexation reaction for 60min at the temperature of 35 ℃, forming a silver layer on the surface of the silver layer, washing with water, and drying to constant weight to obtain the silver-plated conductive fabric (two silver layers).
Comparative example 3
A silver-plated conductive fabric was prepared according to the method of example 3, except that the step (4) was replaced with: and (3) placing the fabric containing the silver layer into 15mL of silver ammonia solution with the concentration of 0.2mol/L, adding the composite reducing agent solution obtained in the step (2), carrying out reduction and complexation reaction for 40min at 45 ℃, forming a silver layer on the surface of the silver layer, washing with water, and drying to constant weight to obtain the conductive fabric with two silver layers.
Comparative example 4
The silver-plated conductive fabric was prepared according to the method of example 4, except that cysteine was not contained in the complex reducing agent solution in step (2).
Comparative example 5
The silver-plated conductive fabric was prepared according to the method of example 5, and the silver-layer-containing fabric obtained in step (3) in example 5 was the silver-plated conductive fabric (a silver layer).
Fig. 1 is an SEM image of a mercapto compound-modified polyester fabric, fig. 2 is an SEM image of a two-silver layer conductive fabric prepared in example 1, and fig. 3 is an SEM image of a one-silver layer conductive fabric prepared in comparative example 1. As shown in the figures 1-3, after the polyester fabric is pretreated and grafted and modified by the mercapto compound, the fiber can still keep the original shape, but a small amount of grooves appear on the surface, and the roughness is increased to some extent; the silver layer on the surface of the silver-plated conductive fabric prepared in the embodiment 1 is compact and uniform, is continuous and is not broken, so that the washability of the conductive fabric is effectively improved; the silver layer on the fiber surface of the silver-plated conductive fabric prepared in comparative example 1 was discontinuous, and there were many fiber surfaces not covered with the silver layer, which seriously affected the washability of the conductive fabric.
The resistance of the silver-plated conductive fabric prepared in examples 1 to 7 and comparative examples 1 to 5 before and after washing was tested by a KDB-1 type four-probe sheet resistance tester, wherein the washing was performed by a washing machine, laundry detergent was added during the washing, the washing was recorded as 1 washing for 15min, and the test results are shown in fig. 4 and table 1.
TABLE 1 Wash resistance and conductivity test results for silver plated conductive fabrics
| Number of washes | Initial resistance omega/sq | Resistance omega/sq after water washing | |
| Example 1 | 500 | 0.016 | 2.06 |
| Example 2 | 500 | 0.015 | 3.20 |
| Example 3 | 500 | 0.010 | 1.33 |
| Example 4 | 300 | 0.031 | 1.22 |
| Example 5 | 200 | 0.046 | 1.29 |
| Example 6 | 200 | 0.077 | 0.57 |
| Example 7 | 200 | 0.020 | 0.89 |
| Comparative example 1 | 200 | 0.055 | 10.6 |
| Comparative example 2 | 80 | 0.040 | 21.18 |
| Comparative example 3 | 40 | 0.133 | 12.69 |
| Comparative example 4 | 100 | 0.244 | 14.86 |
| Comparative example 5 | 50 | 0.034 | 45.60 |
FIG. 4 shows the results of the water washing resistance and conductivity tests of the silver-plated conductive fabrics prepared in examples 1 to 3.
As can be seen from table 1 and fig. 4, the initial resistance of the silver-plated conductive fabrics prepared in examples 1 to 7 of the present invention is very low, and the resistance of the silver-plated conductive fabrics can be maintained in a low range after 200 to 500 washes. While the silver-plated conductive fabrics prepared in comparative examples 1, 2 and 5 had initial resistances close to those of the examples, but their washfastness was much lower than that of the silver-plated conductive fabrics prepared in the examples of the present invention; the silver-plated conductive fabric prepared in comparative examples 3 to 4 has high initial resistance and poor washability.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The silver-plated conductive fabric is characterized by comprising a sulfydryl modified fabric and a composite conductive silver layer positioned on the surface of the sulfydryl modified fabric; the composite conductive silver layer comprises a plurality of silver layers and mercapto compound adsorption layers which are alternately laminated; the bottom layer and the surface layer of the composite conductive silver layer are silver layers; the mercapto compound adsorption layer is formed from a mercapto group-containing co-reducing agent.
2. The silver-plated conductive fabric according to claim 1, wherein the number of silver layers in the silver-plated conductive fabric is not less than 2.
3. The silver-plated conductive fabric according to claim 1 or 2, wherein the thiol-group-containing co-reducing agent comprises one or more of cysteine, acetylcysteine, thiomalic acid, dimercaptosuccinic acid, and thiol.
4. The silver-plated conductive fabric according to claim 1 or 2, wherein the silver plating amount of the silver-plated conductive fabric is 50 to 500%.
5. The silver-plated conductive fabric according to claim 1, wherein the material of the fabric in the thiol-modified fabric comprises one or more of cotton, viscose, tencel, terylene, spandex and chitosan.
6. The method for preparing silver-plated conductive fabric according to any one of claims 1 to 5, comprising the steps of:
(1) mixing the mercapto-modified fabric, silver ammonia solution and composite reducing agent, and carrying out reduction-complexation reaction to form a silver layer on the surface of the mercapto-modified fabric, thereby obtaining a silver-containing fabric; the composite reducing agent comprises a main reducing agent and a sulfydryl-containing auxiliary reducing agent;
(2) placing the silver-containing fabric in a mercapto-containing auxiliary reducing agent solution for adsorption, and forming a mercapto compound adsorption layer on the silver layer surface of the silver-containing fabric;
(3) and (3) repeating the operations of the steps (1) to (2) for a plurality of times on the surface of the sulfhydryl compound adsorption layer, and then repeating the operation of the step (1) for 1 time to obtain the silver-plated conductive fabric.
7. The preparation method according to claim 6, wherein the molar ratio of the main reducing agent to the mercapto group-containing auxiliary reducing agent in the composite reducing agent is 7:3 to 9: 1;
the main reducing agent comprises one or more of glucose, galactose, maltose and tartaric acid.
The molar ratio of the composite reducing agent to the silver ions in the silver ammonia solution is 1: 1-2: 1.
8. The preparation method according to claim 6, wherein in the step (1), the concentration of the silver ammonia solution is 0.1-0.3 mol/L;
the dosage ratio of the silver ammonia solution to the mercapto-modified fabric is 1-5 mL/cm2；
The temperature of the reduction-complexation reaction is 30-60 ℃, and the time is 0.5-2 h.
9. The preparation method according to claim 6, wherein in the step (2), the concentration of the solution of the coreductant is 0.05 to 0.5 mol/L;
the dosage ratio of the auxiliary reducing agent solution to the silver-containing fabric is 1-5 mL/cm2；
The adsorption temperature is 30-80 ℃, and the time is 0.5-2 h.
10. Use of the silver-plated conductive fabric according to any one of claims 1 to 5 or the silver-plated conductive fabric obtained by the production method according to any one of claims 6 to 9 in an electrode material or an electromagnetic shielding material.
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