CN111364283A - Silver-plated conductive aramid paper and preparation method thereof - Google Patents
Silver-plated conductive aramid paper and preparation method thereof Download PDFInfo
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- CN111364283A CN111364283A CN202010242357.6A CN202010242357A CN111364283A CN 111364283 A CN111364283 A CN 111364283A CN 202010242357 A CN202010242357 A CN 202010242357A CN 111364283 A CN111364283 A CN 111364283A
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H19/00—Coated paper; Coating material
- D21H19/02—Metal coatings
- D21H19/06—Metal coatings applied as liquid or powder
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H23/00—Processes or apparatus for adding material to the pulp or to the paper
- D21H23/02—Processes or apparatus for adding material to the pulp or to the paper characterised by the manner in which substances are added
- D21H23/22—Addition to the formed paper
- D21H23/50—Spraying or projecting
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H25/00—After-treatment of paper not provided for in groups D21H17/00 - D21H23/00
- D21H25/04—Physical treatment, e.g. heating, irradiating
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Abstract
The invention discloses silver-plated conductive aramid paper and a preparation method thereof, wherein the preparation method comprises the following steps: a. cleaning the aramid paper substrate by using a cleaning agent, removing surface impurities and drying; b. carrying out plasma treatment on the cleaned aramid paper substrate to obtain a surface-activated aramid paper substrate; c. and (3) putting the aramid paper substrate subjected to plasma treatment into a silver-ammonia solution, activating for a certain time, slowly dropwise adding a reducing agent into the solution, reacting for a certain time, taking out the aramid paper substrate, fully cleaning with deionized water, and drying to finally obtain the conductive aramid paper with the silver-plated surface. The prepared conductive aramid paper has the silver content of 3-12% by mass, good conductive performance and electromagnetic shielding performance, simple preparation process and convenient operation.
Description
Technical Field
The invention relates to the technical field of conductive polymer composite materials, in particular to silver-plated conductive aramid fiber paper and a preparation method thereof.
Background
Conductive materials are widely used in many fields such as electrostatic protection, electromagnetic shielding, electrical heating and sensors. Although the traditional metal conductive material has higher conductivity, the traditional metal conductive material has heavy mass and large brittleness, and cannot meet the requirements of the modern society on light weight and flexibility of the material. The conductive polymer composite material has the advantages of light weight, good flexibility, simple preparation process and the like, and is widely concerned in recent years.
The aramid fiber has the advantages of small specific gravity, high specific strength, good impact resistance, chemical corrosion resistance, high temperature resistance and the like, is a good base material for preparing the conductive composite material, and the metal silver has the advantages of light weight and strong conductivity, and the conductive aramid fiber composite material with excellent performance can be obtained by compounding the metal silver and the metal silver. However, due to the surface inertia and the lower hydrophilicity of the aramid fiber, the silver and the aramid fiber are difficult to combine in the preparation process of the conductive composite material, the firmness of the silver particles after combination is lower, and the size of the silver particles in the silver coating and the distribution and arrangement of the silver particles are difficult to control, so that the conductivity of the conductive aramid paper and the electromagnetic shielding effect are directly reduced.
The traditional pretreatment of aramid fiber materials mostly adopts chemical reagents for immersion, coarsening and activation. Patent CN 103668944B discloses an aramid silver-plated conductive fiber and a preparation method thereof, and the aramid silver-plated conductive fiber is finally obtained through coarsening and activation of a large amount of chemical reagents and a chemical silver plating method. The pretreatment of aramid fiber by the method needs to be soaked by a large amount of chemical reagents, the overall requirements on the concentration of the chemical reagents, the reaction time, the reaction temperature and other factors are high, the aramid fiber is endowed with certain conductivity, uncontrollable factors such as the concentration of the chemical reagents after soaking and use are increased, large-scale fine production is not facilitated, meanwhile, the treatment time is long, a large amount of chemical reagents cause certain environmental pollution, and the prepared conductive aramid fiber is low in conductivity.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a silver-plated conductive aramid paper and a method for preparing the same, in which a silver nanoparticle layer is tightly combined with an aramid matrix, and silver nanoparticles are densely arranged, so that the paper has high conductivity and electromagnetic shielding effectiveness, and the method for preparing the same is simple.
In order to solve the problems, the invention adopts the technical scheme that:
a silver-plated conductive aramid paper comprises an aramid paper substrate and a silver nanoparticle layer tightly attached to the surface of the aramid paper substrate;
the mass ratio of the silver content in the conductive aramid paper is 3-12%; the silver nanoparticle layer has smooth surface and is arranged among the silver nanoparticles in a close packing manner.
According to the preparation method of the silver-plated conductive aramid paper, the diameter of the silver nanoparticles is 80-600nm, and small-size silver nanoparticles are filled in gaps among the large-size silver nanoparticles.
According to the preparation method of the silver-plated conductive aramid paper, the aramid paper substrate is composed of meta-aramid pulp fibers and meta-aramid short fibers, and the thickness of the aramid paper substrate is 0.18-0.3 mm.
According to the preparation method of the silver-plated conductive aramid paper, the surface resistance of the conductive aramid paper is 0.05-0.5 omega/sq.
According to the preparation method of the silver-plated conductive aramid paper, the electromagnetic shielding effectiveness of the conductive aramid paper in an X-wave band (8.2-12.4 GHz) is 70-100 dB, and the electromagnetic shielding effectiveness of the conductive aramid paper in unit thickness is 450-485 dB mm～1。
A preparation method of silver-plated conductive aramid paper is characterized by comprising the following steps: the preparation process is as follows,
(1) cleaning the aramid paper substrate by using a cleaning agent, removing surface impurities and drying;
(2) carrying out plasma treatment on the cleaned aramid paper substrate to obtain a surface-activated aramid paper substrate;
(3) and (3) putting the aramid paper substrate subjected to plasma treatment into a silver-ammonia solution, activating for a certain time, slowly dropwise adding a reducing agent into the solution, reacting for a certain time, taking out the aramid paper substrate, fully cleaning with deionized water, and drying to finally obtain the conductive aramid paper with the silver-plated surface.
According to the preparation method of the silver-plated conductive aramid paper, the plasma treatment method is normal-pressure plasma treatment, the height of a spray head is 2-10 cm, the speed of a spray nozzle is 1-8 m/min, and the duty ratio is 30-90%.
According to the preparation method of the silver-plated conductive aramid paper, the concentration of the silver ammonia solution is 5-40 g/L, and the reducing agent is glucose solution with the concentration range of 10-50 g/L.
According to the preparation method of the silver-plated conductive aramid paper, the cleaning agent used in the step (1) is an ethanol solution, the concentration of the ethanol solution is 50%, and the cleaning time is 30-60 min.
According to the preparation method of the silver-plated conductive aramid paper, the activation time in the step (3) is 15-60 min, and the reaction time is 24-36 h.
The silver-plated conductive aramid paper and the preparation method thereof have the following beneficial effects:
1. the silver-plated conductive aramid paper is prepared by a simple chemical reaction method, has a simple preparation process and low cost, and can be used for large-scale production.
2. The aramid fiber paper substrate is pretreated in a plasma treatment mode, so that the surface of the treated aramid fiber paper substrate generates an etching effect, and meanwhile, the hydrophilicity of the aramid fiber paper substrate is obviously improved by introducing polar groups. By controlling various process parameters in the plasma treatment process, the surface roughness and the specific surface area of the aramid paper substrate are controlled, the amount of introduced polar groups is controlled, and meanwhile, according to the amount of active sites on the surface of the aramid paper substrate after plasma treatment, the concentration of a silver-ammonia solution and the concentration and the dropping speed of glucose are combined, so that the size, distribution and close arrangement conditions of silver nanoparticles are controlled, and the density of the silver nanoparticles is improved.
3. The silver-plated conductive aramid paper prepared by the invention has the advantages that the silver nanoparticles on the surface are firmly attached, the particle size is about 80-600nm, and the silver nanoparticles are closely stacked and arranged, so that the silver nanoparticles with smaller sizes can be filled in gaps among the silver nanoparticles with larger sizes, no obvious gaps and gaps exist among the particles, the conductivity of the conductive aramid paper is further improved, and meanwhile, the more densely the silver nanoparticles are stacked, the higher the electromagnetic shielding efficiency is.
4. The conductive aramid paper prepared by the invention has excellent water washing resistance and bending firmness, after the conductive aramid paper is washed in deionized water for 20 cycles (water temperature is 40 ℃ and each cycle is 30 minutes), the resistance of the conductive aramid paper is increased by 8-14%, the resistance is increased by 1-2% after the conductive aramid paper is bent for 1000 times, after the surface is subjected to plasma treatment, the firmness among silver nanoparticles and between the silver nanoparticles and the surface of the aramid paper base is increased, after the conductive aramid paper is washed and bent for multiple times, the silver nanoparticles drop less, and the influence on the conductivity is less.
5. The silver-plated conductive aramid paper prepared by the invention has stronger high and low temperature resistance and acid and alkali resistance, after high and low temperature treatment, the resistance change is smaller, and meanwhile, under the long-time soaking of strong acid, strong base and organic solvent, the resistance change is kept smaller, and the electromagnetic shielding efficiency is kept above 60dB and far higher than the requirement (30dB) of commercial electromagnetic shielding materials.
Drawings
Fig. 1 is an SEM image of the conductive aramid paper prepared in example 1;
fig. 2 is a graph of temperature versus time for electrical heating made from the conductive aramid paper made in example 2 with different voltages applied.
Detailed Description
Example 1
(1) Commercially available aramid paper substrate with a thickness of 0.18mm is cut into a size of 5cm × 5cm, soaked in 50% ethanol solution, washed for 30min, taken out and dried.
(2) And carrying out normal-temperature plasma treatment on the cleaned aramid paper substrate under the conditions that the height of a nozzle is 4cm, the speed of the nozzle is 1m/min and the duty ratio is 80%.
(3) And (2) putting the aramid paper substrate subjected to plasma treatment into a prepared silver nitrate solution with the concentration of 20g/L, soaking for 30min, slowly dropwise adding a glucose solution with the concentration of 30g/L into the silver nitrate solution, reacting for 24h, taking out the aramid paper substrate, washing for 3 times by using deionized water, and performing vacuum drying at the temperature of 60 ℃ for 24h to obtain the silver-plated conductive aramid paper.
The resistance of the conductive aramid paper prepared in the embodiment is 0.152 omega/sq, and after the conductive aramid paper is placed at the temperature of 80-200 ℃ for 2 hours, the conductive aramid paper is subjected to a conductivity test, wherein the resistance fluctuates between 0.105 omega/sq and 0.183 omega/sq. The conductive aramid paper prepared in this example was tested for S11 and S21 by using a vector network analyzer model ZNB 20 of Rohde & Schwarz, germany, and the total electromagnetic shielding effectiveness was as high as 95.5 dB.
The conductive aramid paper prepared in this example is soaked in an acid solution with a pH of 2, an alkali solution with a pH of 12, and an organic solvent such as ethanol, acetone, n-heptane, xylene, etc. for 7 days, and then subjected to a conductivity test and an electromagnetic shielding effectiveness test, after soaking, the resistance of the conductive aramid paper is still kept below 0.4 Ω/sq, and the electromagnetic shielding effectiveness is kept above 60dB, which is far higher than the requirement for a commercial electromagnetic shielding material (higher than 30 dB).
Example 2
(1) Commercially available aramid paper substrate with a thickness of 0.18mm is cut into a size of 5cm × 5cm, soaked in 50% ethanol solution, washed for 30min, taken out and dried.
(2) And carrying out normal-temperature plasma treatment on the cleaned aramid paper substrate under the conditions that the height of a nozzle is 5cm, the speed of the nozzle is 1m/min and the duty ratio is 80%.
(3) And (2) placing the aramid paper substrate subjected to plasma treatment into a prepared silver nitrate solution with the concentration of 15g/L, soaking for 30min, slowly dripping a glucose solution with the concentration of 30g/L into the silver nitrate solution, reacting for 24h, taking out the aramid paper, cleaning for 3 times by using deionized water, and performing vacuum drying at the temperature of 60 ℃ for 24h to obtain the silver-plated conductive aramid paper.
The resistance of the conductive aramid paper prepared in the embodiment is 0.051 omega/sq, and after the conductive aramid paper is washed in deionized water for 20 cycles (the water temperature is 40 ℃ and each cycle is 30min), the resistance of the conductive aramid paper is increased by 11.9 percent, and the resistance is increased by 1.4 percent after the conductive aramid paper is bent for 1000 times.
The two ends of conductive aramid paper with the size of 10mm × 20mm are coated with copper foil through conductive silver adhesive and are connected with a power supply to form a micro electric heater, the temperature of the electric heater is tested to change along with time when different voltages are applied, as can be seen from figure 2, the temperature of the electric heater is increased from room temperature to 37 ℃ within 20 seconds under the applied voltage of 0.2V, the effect of keeping the human body warm can be achieved, and the temperature of the electric heater is increased to over 200 ℃ within 20 seconds under the applied voltage of 1V, in addition, the temperature of the electric heater can be reduced to the room temperature within 25 seconds after the voltage is removed.
Example 3
(1) Preparing 50% ethanol solution, cutting commercially available aramid paper with the thickness of 0.30mm into pieces with the size of 5cm × 5cm, soaking in the aramid paper, cleaning for 60min, taking out and drying.
(2) And carrying out normal-temperature plasma treatment on the cleaned aramid paper under the conditions that the height of a nozzle is 2cm, the speed of the nozzle is 1m/min and the duty ratio is 30%.
(3) And (2) putting the aramid fiber paper after plasma treatment into a prepared silver nitrate solution with the concentration of 5g/L, soaking for 60min, slowly dripping a glucose solution with the concentration of 10g/L into the silver nitrate solution, reacting for 36h, taking out the aramid fiber paper, washing for 3 times by using deionized water, and performing vacuum drying at the temperature of 60 ℃ for 24h to obtain the silver-plated conductive aramid fiber paper.
Example 4
(1) Preparing 50% ethanol solution, cutting commercially available aramid paper with the thickness of 0.30mm into pieces with the size of 5cm × 5cm, soaking in the aramid paper, cleaning for 60min, taking out and drying.
(2) And carrying out normal-temperature plasma treatment on the cleaned aramid paper under the conditions that the height of a nozzle is 10cm, the speed of the nozzle is 8m/min and the duty ratio is 60%.
(3) And (2) putting the aramid fiber paper after plasma treatment into a prepared silver nitrate solution with the concentration of 40g/L, soaking for 15min, slowly dripping a glucose solution with the concentration of 50g/L into the silver nitrate solution, reacting for 24h, taking out the aramid fiber paper, washing for 3 times by using deionized water, and performing vacuum drying at the temperature of 60 ℃ for 24h to obtain the silver-plated conductive aramid fiber paper.
It is to be understood that the above description is not intended to limit the present invention, and the present invention is not limited to the above examples, and that various changes, modifications, additions and substitutions which are within the spirit and scope of the present invention and which can be made by those skilled in the art are also within the scope of the present invention.
Claims (10)
1. The silver-plated conductive aramid paper is characterized in that: comprises an aramid paper substrate and a silver nanoparticle layer tightly attached to the surface of the aramid paper substrate;
the mass ratio of the silver content in the conductive aramid paper is 3-12%; the silver nanoparticle layer has smooth surface and silver nanoparticles are densely packed and arranged.
2. The silver-plated conductive aramid paper as set forth in claim 1, wherein: the diameter of the silver nanoparticles is 80-600nm, and small-size silver nanoparticles are filled in gaps among the large-size silver nanoparticles.
3. The silver-plated conductive aramid paper as set forth in claim 1, wherein: the aramid fiber paper substrate is composed of meta-aramid pulp fibers and meta-aramid short fibers, and the thickness of the aramid fiber paper substrate is 0.18-0.3 mm.
4. The silver-plated conductive aramid paper as set forth in claim 1, wherein: the surface resistance of the conductive aramid paper is 0.05-0.5 omega/sq.
5. The silver-plated conductive aramid paper as set forth in claim 1, wherein: the electromagnetic shielding effectiveness of the conductive aramid paper in an X wave band (8.2-12.4 GHz) is 70-100 dB, and the electromagnetic shielding effectiveness of the conductive aramid paper in unit thickness is 450-485 dB mm～1。
6. A method for preparing silver-plated conductive aramid paper as claimed in any one of claims 1 to 5, characterized in that: the preparation process is as follows,
(1) cleaning the aramid paper substrate by using a cleaning agent, removing surface impurities and drying;
(2) carrying out plasma treatment on the cleaned aramid paper substrate to obtain a surface-activated aramid paper substrate;
(3) and (3) putting the aramid paper substrate subjected to plasma treatment into a silver-ammonia solution, activating for a certain time, slowly dropwise adding a reducing agent into the solution, reacting for a certain time, taking out the aramid paper substrate, fully cleaning with deionized water, and drying to finally obtain the conductive aramid paper with the silver-plated surface.
7. The method for preparing silver-plated conductive aramid paper according to claim 6, characterized by comprising the following steps: the plasma treatment method is normal-pressure plasma treatment, the height of a spray head is 2-10 cm, the speed of a spray nozzle is 1-8 m/min, and the duty ratio is 30-90%.
8. The method for preparing silver-plated conductive aramid paper according to claim 6, characterized by comprising the following steps: the concentration of the silver ammonia solution is 5-40 g/L, and the reducing agent is glucose solution with the concentration of 10-50 g/L.
9. The method for preparing silver-plated conductive aramid paper according to claim 6, characterized by comprising the following steps: the cleaning agent used in the step (1) is an ethanol solution, the concentration of the ethanol solution is 50%, and the cleaning time is 30-60 min.
10. The method for preparing silver-plated conductive aramid paper according to claim 6, characterized by comprising the following steps: the activation time in the step (3) is 15-60 min, and the reaction time is 24-36 h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112663380A (en) * | 2020-12-11 | 2021-04-16 | 华南理工大学 | High-performance electromagnetic shielding composite paper-based material and preparation method and application thereof |
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