CN111172522A - Method for preparing flexible conductive super-hydrophobic composite material on surface of non-woven cotton fiber fabric - Google Patents
Method for preparing flexible conductive super-hydrophobic composite material on surface of non-woven cotton fiber fabric Download PDFInfo
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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
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
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- C23C18/42—Coating with noble metals
- C23C18/44—Coating with noble metals using reducing agents
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- 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
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/28—Sensitising or activating
- C23C18/285—Sensitising or activating with tin based compound or composition
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- 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
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- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
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- 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
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- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
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Abstract
The invention belongs to the technical field of material surface engineering and super-hydrophobic materials, and discloses a method for preparing a flexible conductive super-hydrophobic composite material on the surface of a non-woven cotton fiber fabric. The method mainly comprises the following steps: (1) cleaning a non-woven cotton fiber fabric; (2) sensitizing the non-woven cotton fiber fabric; (3) chemically spraying an Ag conductive coating on the surface of the non-woven cotton fiber fabric; (4) and (3) electrodepositing a super-hydrophobic coating on the surface of the non-woven cotton fiber fabric. The method for preparing the flexible conductive super-hydrophobic composite material on the surface of the non-woven cotton fiber fabric has the advantages of simple preparation process, low cost, uniform plating, flexibility, bending resistance and excellent conductivity, and simultaneously solves the problems of long time consumption, high toxicity of the used reducing agent and high pollution of the traditional chemical plating.
Description
Technical Field
The invention belongs to the technical field of material surface engineering and super-hydrophobic materials, and particularly relates to a method for preparing a flexible conductive super-hydrophobic composite material on the surface of a non-woven cotton fiber fabric.
Background
The super-hydrophobic material has attracted extensive attention and research because of its good performances of corrosion resistance, self-cleaning, ice resistance, fog resistance, etc. In recent years, flexible electronics is rapidly developed to bring convenience to human life, and by combining excellent surface wettability and mechanical flexibility, the application fields of the flexible electronics, such as self-cleaning wearable fabrics, waterproof stress sensors and the like, can be greatly expanded, and the limitation of the environment on the use of flexible electronic products is reduced.
The conventional preparation methods of the super-hydrophobic coating comprise a sol-gel method, a chemical vapor deposition method, a template method, an electrodeposition method and the like, and the methods have complex processes and high equipment cost. Moreover, the methods all need to use surface modifiers to reduce the surface energy, most of the surface modifiers are long-chain silanes or fluorine substances, are expensive and can cause damage to the environment, so that the method for preparing the super-hydrophobic surface of the flexible material, which is simple in process, low in cost, green and environment-friendly, has wide development prospect and research significance.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a method for preparing a flexible conductive super-hydrophobic composite material on the surface of a non-woven cotton fiber fabric, which has the advantages of simple preparation process, low cost, uniform plating, flexibility, bending resistance and excellent conductivity, and simultaneously solves the problems of long time consumption, high toxicity of a used reducing agent and high pollution of the traditional chemical plating.
The purpose of the invention is realized by the following technical scheme:
a method for preparing a flexible conductive super-hydrophobic composite material on the surface of a non-woven cotton fiber fabric comprises the following steps:
(1) nonwoven cotton fabric cleaning
Placing the non-woven cotton fiber fabric in absolute ethyl alcohol for ultrasonic cleaning;
(2) sensitization treatment of non-woven cotton fiber fabric
Soaking the non-woven cotton fiber fabric cleaned in the step (1) in a sensitizing solution, taking out, cleaning and drying; the sensitizing solution is prepared from stannous chloride, hydrochloric acid and water;
(3) ag conductive coating chemically sprayed on surface of non-woven cotton fiber fabric
Putting the silver ammonia solution into a spraying pot A, putting a reducing agent into a spraying pot B, spraying the solutions in the two spraying pots together to the non-woven cotton fiber fabric sensitized in the step (2), cleaning and drying the sprayed non-woven cotton fiber fabric to obtain an Ag conductive coating; the silver-ammonia solution is prepared from silver nitrate, ammonia water and water, and the reducing agent is prepared from glyoxal, triethanolamine and water;
(4) electro-deposition super-hydrophobic coating on surface of non-woven cotton fiber fabric
Putting the Ag conductive coating in the step (3) into a deposition solution for electrodeposition, wherein the Ag conductive coating is a cathode, and a platinum plate is an anode; after electrodeposition, taking out the sample, cleaning, drying by blowing, and vacuum drying; the deposition solution is prepared from myristic acid, cerium nitrate and absolute ethyl alcohol.
Wherein, the ultrasonic cleaning in the step (1) is to put the non-woven cotton fiber fabric into absolute ethyl alcohol for ultrasonic oscillation for 10-30 min.
In the step (2), the concentration of stannous chloride in the sensitizing solution is 20-40 g/L, and the concentration of 37 wt.% hydrochloric acid is 10-20 ml/L.
The soaking time in the step (2) is 10-30 min, and the soaking temperature is 10-30 ℃; the cleaning is water cleaning.
The concentration of silver nitrate in the silver ammonia solution in the step (3) is 10-20 g/L, and the concentration of 25 wt.% ammonia water is 5-10 ml/L; the concentration of 30 wt.% of glyoxal in the reducing agent is 40-60 ml/L, and the concentration of 85 wt.% of triethanolamine is 10-30 ml/L.
The specific steps of the step (3) are as follows: fixing the non-woven cotton fiber fabric treated in the step (2) in a glove box, aligning nozzles of a spraying pot A and a spraying pot B to the non-woven cotton fiber fabric simultaneously, enabling the distance between the non-woven cotton fiber fabric and a pot nozzle to be 10-15 cm, enabling the spraying speed to be 1-3 times per second, enabling the spraying frequency to be 30-50 times, and cleaning and drying after spraying; the cleaning is water cleaning.
In the step (4), the concentration of myristic acid in the deposition solution is 40-60 g/L, and the concentration of cerium nitrate is 10-30 g/L.
The electrodeposition time in the step (4) is 10-30 min, and the electrodeposition voltage is 10-30V; the cleaning is water cleaning.
The preparation method and the obtained product have the following advantages and effects:
(1) the preparation method has the advantages of simple process, low cost, uniform spraying and the like;
(2) the conductive super-hydrophobic composite material prepared by the invention has the characteristics of good conductivity, good flexibility, bending resistance and the like;
(3) the invention applies the super-hydrophobic property to the field of flexible conductive materials, so that the conductive material has the characteristics of super-hydrophobicity, self-cleaning, corrosion resistance and the like.
Drawings
FIG. 1 is a microscopic topography of a silver layer on the surface of the non-woven cotton fiber fabric in example 1;
FIG. 2 is a microscopic appearance of the super-hydrophobic coating on the surface of the non-woven cotton fiber fabric in example 1;
FIG. 3 is a composition characterization of the conductive super-hydrophobic composite coating prepared on the surface of the non-woven cotton fiber fabric in example 1;
fig. 4 is a tape test of the conductive superhydrophobic composite coating prepared on the surface of the non-woven cotton fiber fabric in example 2.
Detailed Description
The present invention will be described in further detail with reference to the following examples and accompanying drawings.
Example 1
A method for preparing a flexible conductive super-hydrophobic composite material on the surface of a non-woven cotton fiber fabric comprises the following specific operation steps:
(1) ultrasonic cleaning
Placing the non-woven cotton fiber fabric with the specification of 30mm multiplied by 40mm into absolute ethyl alcohol for ultrasonic cleaning for 10min, taking out the non-woven cotton fiber fabric, washing the non-woven cotton fiber fabric by using a large amount of deionized water, and drying the non-woven cotton fiber fabric by using a blower after washing;
(2) sensitization treatment of non-woven cotton fiber fabric
Weighing 2g of stannous chloride, dissolving the stannous chloride in 100ml of deionized water, and slowly dropwise adding 10ml of 37 wt% hydrochloric acid into the solution to prepare sensitizing solution; soaking the non-woven cotton fiber fabric cleaned in the step (1) in a sensitizing solution for 10min to perform a sensitization reaction, wherein the reaction temperature is 15 ℃; taking out the non-woven cotton fiber fabric, washing the non-woven cotton fiber fabric with deionized water, washing the redundant sensitizing solution, and drying the non-woven cotton fiber fabric with a blower after washing;
(3) ag conductive coating (namely conductive silver layer) chemically sprayed on surface of non-woven cotton fabric
Weighing 1g of silver nitrate, dissolving the silver nitrate into 100ml of deionized water, dropwise adding ammonia water into the solution, wherein the solution becomes turbid firstly and then becomes clear gradually, and when the solution just becomes clear, the dropwise adding of the ammonia water is stopped, so that the silver-ammonia solution is prepared; measuring 4ml of 30 wt.% glyoxal, 1ml of 85 wt.% triethanolamine and 100ml of deionized water, mixing the glyoxal, the triethanolamine and the deionized water, and performing ultrasonic dispersion to prepare a reducing agent; putting the silver ammonia solution into a spraying pot A, putting a reducing agent into a spraying pot B, fixing the non-woven cotton fiber fabric treated in the step (2) in a glove box, simultaneously aligning the nozzles of the spraying pot A and the spraying pot B with the non-woven cotton fiber fabric, spraying the liquid in the spraying pot to the surface of the non-woven cotton fiber fabric at a spraying speed of 1 time per second, wherein the spraying times are 30 times, taking out the non-woven cotton fiber fabric after the spraying is finished, cleaning the non-woven cotton fiber fabric with a large amount of deionized water, and finally drying the non-woven cotton fiber fabric by blowing, namely preparing the Ag conductive coating on the surface of the non-woven cotton fiber fabric;
(4) electro-deposition super-hydrophobic coating (namely conductive super-hydrophobic composite coating) on surface of non-woven cotton fiber fabric
Weighing 4g of myristic acid and 1g of cerium nitrate, and dissolving the myristic acid and the cerium nitrate in 100ml of absolute ethyl alcohol; putting the Ag conductive coating in the step (3) into a deposition solution for electrodeposition, wherein the Ag conductive coating is a cathode, a platinum plate is an anode, the deposition voltage is 10V, and the deposition time is 10 min; and after electrodeposition, taking out the sample, cleaning, blow-drying and drying in a vacuum drying oven.
The conductive super-hydrophobic composite coating prepared on the surface of the non-woven cotton fabric is detected and characterized as follows:
(1) and (3) morphology analysis: and (3) carrying out microscopic morphology analysis on the conductive silver layer and the conductive super-hydrophobic composite coating by using a scanning electron microscope, wherein the nano silver particles are uniformly distributed on the surface of the non-woven cotton fiber fabric, as shown in figures 1 and 2.
(2) And (3) component analysis: the conductive super-hydrophobic composite coating is subjected to composition analysis by an X-ray diffractometer (XRD), and as shown in figure 3, the XRD of the conductive super-hydrophobic composite coating has 5 silver peaks which respectively correspond to the (111), (200), (220), (311) and (222) crystal faces of the face-centered cubic metallic silver.
(3) Conductivity: the surface resistance of the conductive silver layer is 7.34m omega/square, and the surface resistance of the conductive super-hydrophobic composite coating is 8.64m omega/square.
(4) Super-hydrophobicity: the contact angle of the surface distilled water of the conductive silver layer is 106 degrees, and the contact angle of the surface distilled water of the conductive super-hydrophobic composite coating is 157 degrees.
(5) The coating binding properties were tested using a Baige test, i.e. a standard tape test method: the conductive silver layer partially falls off, and the conductive super-hydrophobic composite coating does not fall off, because the combination of the composite coating and the base material is promoted by the electrodeposition technology.
In the embodiment, the preparation method has the advantages of simple process, low cost, difficult shedding of the coating, and good bending resistance and scraping resistance.
Example 2
A method for preparing a flexible conductive super-hydrophobic composite material on the surface of a non-woven cotton fiber fabric comprises the following specific operation steps:
(1) ultrasonic cleaning
Placing the non-woven cotton fiber fabric with the specification of 30mm multiplied by 40mm into absolute ethyl alcohol for ultrasonic cleaning for 20min, taking out the non-woven cotton fiber fabric, washing the non-woven cotton fiber fabric by using a large amount of deionized water, and drying the non-woven cotton fiber fabric by using a blower after washing;
(2) sensitization treatment of non-woven cotton fiber fabric
Weighing 3g of stannous chloride, dissolving the stannous chloride in 100ml of deionized water, and slowly dropwise adding 15ml of 37 wt% hydrochloric acid into the solution to prepare sensitizing solution; soaking the non-woven cotton fiber fabric cleaned in the step (1) in a sensitizing solution for 20min for carrying out a sensitization reaction at the temperature of 20 ℃; taking out the non-woven cotton fiber fabric, washing the non-woven cotton fiber fabric with deionized water, washing the redundant sensitizing solution, and drying the non-woven cotton fiber fabric with a blower after washing;
(3) ag conductive coating (namely conductive silver layer) chemically sprayed on surface of non-woven cotton fabric
Weighing 1.5g of silver nitrate, dissolving the silver nitrate in 100ml of deionized water, dropwise adding ammonia water into the solution, wherein the solution becomes turbid firstly and then becomes clear gradually, and when the solution just becomes clear, stopping dropwise adding the ammonia water, so that the silver-ammonia solution is prepared; measuring 5ml of 30 wt.% glyoxal, 2ml of 85 wt.% triethanolamine and 100ml of deionized water, mixing the glyoxal, the triethanolamine and the deionized water, and performing ultrasonic dispersion to prepare a reducing agent; putting the silver ammonia solution into a spraying pot A, putting a reducing agent into a spraying pot B, fixing the non-woven cotton fiber fabric treated in the step (2) in a glove box, simultaneously aligning the nozzles of the spraying pot A and the spraying pot B with the non-woven cotton fiber fabric, spraying the liquid in the spraying pot to the surface of the non-woven cotton fiber fabric at a spraying speed of 2 times per second, wherein the spraying times are 40 times, taking out the non-woven cotton fiber fabric after the spraying is finished, cleaning the non-woven cotton fiber fabric with a large amount of deionized water, and finally drying the non-woven cotton fiber fabric by blowing, namely preparing the Ag conductive coating on the surface of the non-woven cotton fiber fabric;
(4) electro-deposition super-hydrophobic coating (namely conductive super-hydrophobic composite coating) on surface of non-woven cotton fiber fabric
Weighing 5g of myristic acid and 2g of cerium nitrate, and dissolving the myristic acid and the cerium nitrate in 100ml of absolute ethyl alcohol; putting the Ag conductive coating in the step (3) into a deposition solution for electrodeposition, wherein the Ag conductive coating is a cathode, a platinum plate is an anode, the deposition voltage is 20V, and the deposition time is 20 min; and after electrodeposition, taking out the sample, cleaning, blow-drying and drying in a vacuum drying oven.
The conductive super-hydrophobic composite coating prepared on the surface of the non-woven cotton fabric is detected and characterized as follows:
(1) and (3) morphology analysis: and (3) carrying out microscopic morphology analysis on the conductive silver layer and the conductive super-hydrophobic composite coating by using a scanning electron microscope, wherein the nano silver particles are uniformly distributed on the surface of the non-woven cotton fiber fabric, and the method is similar to that shown in the figures 1 and 2.
(2) And (3) component analysis: the composition analysis of the conductive super-hydrophobic composite coating is carried out by utilizing an X-ray diffractometer (XRD), 5 silver peaks appear on the XRD of the conductive super-hydrophobic composite coating and respectively correspond to the (111), (200), (220), (311) and (222) crystal faces of the face-centered cubic metal silver.
(3) Conductivity: the surface resistance of the conductive silver layer is 7.25m omega/square, and the surface resistance of the conductive super-hydrophobic composite coating is 8.79m omega/square. (4) The bonding performance of the coating is tested by adopting a Baige experiment, namely a standard adhesive tape test method: the conductive silver layer is partially peeled off through a test of the adhesive tape, and the conductive super-hydrophobic composite coating is not peeled off (as shown in figure 4), because the combination of the composite coating and the substrate is promoted by the electrodeposition technology.
(5) Super-hydrophobicity: the contact angle of the surface distilled water of the conductive silver layer is 105 degrees, and the contact angle of the surface distilled water of the conductive super-hydrophobic composite coating is 155 degrees.
In the embodiment, the preparation method has the advantages of simple process, low cost, difficult shedding of the coating, and good bending resistance and scraping resistance.
Example 3
A method for preparing a flexible conductive super-hydrophobic composite material on the surface of a non-woven cotton fiber fabric comprises the following specific operation steps:
(1) ultrasonic cleaning
Placing the non-woven cotton fiber fabric with the specification of 30mm multiplied by 40mm into absolute ethyl alcohol for ultrasonic cleaning for 30min, taking out the non-woven cotton fiber fabric, washing the non-woven cotton fiber fabric by using a large amount of deionized water, and drying the non-woven cotton fiber fabric by using a blower after washing;
(2) sensitization treatment of non-woven cotton fiber fabric
Weighing 4g of stannous chloride, dissolving the stannous chloride in 100ml of deionized water, and slowly dropwise adding 20ml of 37 wt% hydrochloric acid into the solution to prepare sensitizing solution; soaking the non-woven cotton fiber fabric cleaned in the step (1) in a sensitizing solution for 30min for carrying out a sensitization reaction at the temperature of 30 ℃; taking out the non-woven cotton fiber fabric, washing the non-woven cotton fiber fabric with deionized water, washing the redundant sensitizing solution, and drying the non-woven cotton fiber fabric with a blower after washing;
(3) ag conductive coating (namely conductive silver layer) chemically sprayed on surface of non-woven cotton fabric
Weighing 2g of silver nitrate, dissolving the silver nitrate into 100ml of deionized water, dropwise adding ammonia water into the solution, wherein the solution becomes turbid firstly and then becomes clear gradually, and when the solution just becomes clear, the dropwise adding of the ammonia water is stopped, so that the silver-ammonia solution is prepared; measuring 6ml of 30 wt.% glyoxal, 3ml of 85 wt.% triethanolamine and 100ml of deionized water, mixing the glyoxal, the triethanolamine and the deionized water, and performing ultrasonic dispersion to prepare a reducing agent; putting the silver ammonia solution into a spraying pot A, putting a reducing agent into a spraying pot B, fixing the non-woven cotton fiber fabric treated in the step (2) in a glove box, simultaneously aligning the nozzles of the spraying pot A and the spraying pot B with the non-woven cotton fiber fabric, spraying the liquid in the spraying pot to the surface of the non-woven cotton fiber fabric at a spraying speed of 3 times per second, wherein the spraying times are 50 times, taking out the non-woven cotton fiber fabric after the spraying is finished, cleaning the non-woven cotton fiber fabric with a large amount of deionized water, and finally drying the non-woven cotton fiber fabric by blowing, namely preparing the Ag conductive coating on the surface of the non-woven cotton fiber fabric;
(4) electro-deposition super-hydrophobic coating (namely conductive super-hydrophobic composite coating) on surface of non-woven cotton fiber fabric
Weighing 6g of myristic acid and 3g of cerium nitrate, and dissolving the myristic acid and the cerium nitrate in 100ml of absolute ethyl alcohol; putting the Ag conductive coating in the step (3) into a deposition solution for electrodeposition, wherein the Ag conductive coating is a cathode, a platinum plate is an anode, the deposition voltage is 30V, and the deposition time is 30 min; and after electrodeposition, taking out the sample, cleaning, blow-drying and drying in a vacuum drying oven.
The conductive super-hydrophobic composite coating prepared on the surface of the non-woven cotton fabric is detected and characterized as follows:
(1) and (3) morphology analysis: and (3) carrying out microscopic morphology analysis on the conductive silver layer and the conductive super-hydrophobic composite coating by using a scanning electron microscope, wherein the nano silver particles are uniformly distributed on the surface of the non-woven cotton fiber fabric.
(2) And (3) component analysis: the composition analysis of the conductive super-hydrophobic composite coating is carried out by utilizing an X-ray diffractometer (XRD), 5 silver peaks appear on the XRD of the conductive super-hydrophobic composite coating and respectively correspond to the (111), (200), (220), (311) and (222) crystal faces of the face-centered cubic metal silver.
(3) Conductivity: the surface resistance of the conductive silver layer is 7.52m omega/square, and the surface resistance of the conductive super-hydrophobic composite coating is 8.81m omega/square.
(4) Super-hydrophobicity: the contact angle of the surface distilled water of the conductive silver layer is 108 degrees, and the contact angle of the surface distilled water of the conductive super-hydrophobic composite coating is 156 degrees.
(5) The coating binding properties were tested using a Baige test, i.e. a standard tape test method: the conductive silver layer partially falls off, and the conductive super-hydrophobic composite coating does not fall off, because the combination of the composite coating and the base material is promoted by the electrodeposition technology.
In the embodiment, the preparation method has the advantages of simple process, low cost, easy shedding of the coating, and good bending resistance and scraping resistance.
Comparative example 1
A method for chemically plating silver and electrodepositing a composite coating material on the surface of a non-woven cotton fiber fabric comprises the following specific operation steps:
(1) ultrasonic cleaning
Placing the non-woven cotton fiber fabric with the specification of 30mm multiplied by 40mm into absolute ethyl alcohol for ultrasonic cleaning for 20min, taking out the non-woven cotton fiber fabric, washing the non-woven cotton fiber fabric by using a large amount of deionized water, and drying the non-woven cotton fiber fabric by using a blower after washing;
(2) sensitization treatment of non-woven cotton fiber fabric
Weighing 3g of stannous chloride, dissolving the stannous chloride in 100ml of deionized water, and slowly dropwise adding 15ml of 37 wt% hydrochloric acid into the solution to prepare sensitizing solution; soaking the non-woven cotton fiber fabric cleaned in the step (1) in a sensitizing solution for 20min for carrying out a sensitization reaction at the temperature of 20 ℃; taking out the non-woven cotton fiber fabric, washing the non-woven cotton fiber fabric with deionized water, washing the redundant sensitizing solution, and drying the non-woven cotton fiber fabric with a blower after washing;
(3) silver-plated conductive coating on surface of non-woven cotton fiber fabric by chemical immersion
Weighing 1.5g of silver nitrate, dissolving the silver nitrate in 100ml of deionized water, dropwise adding ammonia water into the solution, wherein the solution becomes turbid firstly and then becomes clear gradually, and when the solution just becomes clear, stopping dropwise adding the ammonia water, so that the silver-ammonia solution is prepared; 2g of glucose and 100ml of deionized water are weighed, the glucose and the deionized water are mixed and subjected to ultrasonic dispersion, and a reducing agent is prepared; soaking the non-woven cotton fiber fabric in a silver ammonia solution, pouring a reducing agent into the silver ammonia solution, taking out the non-woven cotton fiber fabric after 5 minutes, cleaning the non-woven cotton fiber fabric by using a large amount of deionized water, and finally drying the non-woven cotton fiber fabric by blowing, namely preparing an Ag conductive coating on the surface of the non-woven cotton fiber fabric;
(4) surface electrodeposition composite coating of non-woven cotton fiber fabric
Weighing 5g of myristic acid and 2g of cerium nitrate, and dissolving the myristic acid and the cerium nitrate in 100ml of absolute ethyl alcohol; putting the Ag conductive coating in the step (3) into a deposition solution for electrodeposition, wherein the Ag conductive coating is a cathode, a platinum plate is an anode, the deposition voltage is 20V, and the deposition time is 20 min; and after electrodeposition, taking out the sample, cleaning, blow-drying and drying in a vacuum drying oven.
The composite coating prepared on the surface of the non-woven cotton fiber fabric is detected and characterized as follows:
(1) super-hydrophobicity: the contact angle of the surface of the distilled water of the silver-plated coating is 102 degrees, and the contact angle of the surface of the distilled water of the composite coating is 136 degrees.
(2) Bonding performance: the adhesive tape test method is adopted to test the interface bonding performance of the conductive silver coating and the conductive super-hydrophobic composite coating, and the adhesive tape test shows that the conductive silver coating and the conductive super-hydrophobic composite coating are basically completely peeled off, which indicates that the interface bonding performance is poor.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (8)
1. A method for preparing a flexible conductive super-hydrophobic composite material on the surface of a non-woven cotton fiber fabric is characterized by comprising the following steps:
(1) nonwoven cotton fabric cleaning
Placing the non-woven cotton fiber fabric in absolute ethyl alcohol for ultrasonic cleaning;
(2) sensitization treatment of non-woven cotton fiber fabric
Soaking the non-woven cotton fiber fabric cleaned in the step (1) in a sensitizing solution, taking out, cleaning and drying; the sensitizing solution is prepared from stannous chloride, hydrochloric acid and water;
(3) ag conductive coating chemically sprayed on surface of non-woven cotton fiber fabric
Putting the silver ammonia solution into a spraying pot A, putting a reducing agent into a spraying pot B, spraying the solutions in the two spraying pots together to the non-woven cotton fiber fabric sensitized in the step (2), cleaning and drying the sprayed non-woven cotton fiber fabric to obtain an Ag conductive coating; the silver-ammonia solution is prepared from silver nitrate, ammonia water and water, and the reducing agent is prepared from glyoxal, triethanolamine and water;
(4) electro-deposition super-hydrophobic coating on surface of non-woven cotton fiber fabric
Putting the Ag conductive coating in the step (3) into a deposition solution for electrodeposition, wherein the Ag conductive coating is a cathode, and a platinum plate is an anode; after electrodeposition, taking out the sample, cleaning, drying by blowing, and vacuum drying; the deposition solution is prepared from myristic acid, cerium nitrate and absolute ethyl alcohol.
2. The method for preparing the flexible conductive super-hydrophobic composite material on the surface of the non-woven cotton fiber fabric according to claim 1, wherein the concentration of stannous chloride in the sensitizing solution in the step (2) is 20-40 g/L, and the concentration of 37 wt.% hydrochloric acid is 10-20 ml/L.
3. The method for preparing the flexible conductive super-hydrophobic composite material on the surface of the non-woven cotton fiber fabric according to claim 1, wherein the soaking time in the step (2) is 10-30 min, and the soaking temperature is 10-30 ℃; the cleaning is water cleaning.
4. The method for preparing the flexible conductive super-hydrophobic composite material on the surface of the non-woven cotton fiber fabric according to claim 1, wherein the silver nitrate in the silver ammonia solution in the step (3) has a concentration of 10-20 g/L, and the 25 wt.% ammonia water has a concentration of 5-10 ml/L; the concentration of 30 wt.% of glyoxal in the reducing agent is 40-60 ml/L, and the concentration of 85 wt.% of triethanolamine is 10-30 ml/L.
5. The method for preparing the flexible conductive super-hydrophobic composite material on the surface of the non-woven cotton fiber fabric according to claim 1, wherein the specific steps of the step (3) are as follows: fixing the non-woven cotton fiber fabric treated in the step (2) in a glove box, aligning nozzles of a spraying pot A and a spraying pot B to the non-woven cotton fiber fabric simultaneously, enabling the distance between the non-woven cotton fiber fabric and a pot nozzle to be 10-15 cm, enabling the spraying speed to be 1-3 times per second, enabling the spraying frequency to be 30-50 times, and cleaning and drying after spraying; the cleaning is water cleaning.
6. The method for preparing the flexible conductive super-hydrophobic composite material on the surface of the non-woven cotton fiber fabric according to claim 1, wherein the concentration of the myristic acid in the deposition solution in the step (4) is 40-60 g/L, and the concentration of the cerium nitrate in the deposition solution is 10-30 g/L.
7. The method for preparing the flexible conductive super-hydrophobic composite material on the surface of the non-woven cotton fiber fabric according to claim 1, wherein the electrodeposition time in the step (4) is 10-30 min, and the electrodeposition voltage is 10-30V; the cleaning is water cleaning.
8. The method for preparing the flexible conductive superhydrophobic composite material on the surface of the non-woven cotton fiber fabric according to claim 1, wherein the ultrasonic cleaning in the step (1) is to place the non-woven cotton fiber fabric into absolute ethyl alcohol for ultrasonic oscillation for 10-30 min.
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| CN112281472A (en) * | 2020-10-30 | 2021-01-29 | 西北师范大学 | Ag @ Zn (OH)2Preparation process of nanosheet conductive cotton cloth |
| CN114351216A (en) * | 2021-12-28 | 2022-04-15 | 华南理工大学 | Method for preparing super-hydrophobic composite film on surface of flexible matrix conductive metal film |
| CN114351445A (en) * | 2021-12-21 | 2022-04-15 | 华南理工大学 | Method for preparing electromagnetic shielding composite coating on surface of non-woven fabric |
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