CN114773686B - HEC/BNNS/AgNWs composite film and preparation method thereof - Google Patents
HEC/BNNS/AgNWs composite film and preparation method thereof Download PDFInfo
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- 239000002042 Silver nanowire Substances 0.000 title claims abstract description 111
- 239000002131 composite material Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000000243 solution Substances 0.000 claims abstract description 56
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 53
- 238000000498 ball milling Methods 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000011259 mixed solution Substances 0.000 claims abstract description 24
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 229910052582 BN Inorganic materials 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 33
- 239000007788 liquid Substances 0.000 claims description 26
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 15
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 14
- 239000006185 dispersion Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 239000011324 bead Substances 0.000 claims description 8
- 238000007865 diluting Methods 0.000 claims description 8
- 239000012895 dilution Substances 0.000 claims description 8
- 238000010790 dilution Methods 0.000 claims description 8
- -1 polytetrafluoroethylene Polymers 0.000 claims description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 8
- 238000005266 casting Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 19
- 238000010345 tape casting Methods 0.000 abstract description 7
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 230000035945 sensitivity Effects 0.000 abstract description 3
- 238000010382 chemical cross-linking Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 118
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 118
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 118
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- 239000000138 intercalating agent Substances 0.000 description 5
- 238000011056 performance test Methods 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 4
- 238000011895 specific detection Methods 0.000 description 4
- 239000002270 dispersing agent Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920003086 cellulose ether Polymers 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000004020 conductor Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000006266 etherification reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
- C08J2301/26—Cellulose ethers
- C08J2301/28—Alkyl ethers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
Abstract
The invention discloses a HEC/BNNS/AgNWs composite film and a preparation method thereof, comprising the following steps: mixing boron nitride with HEC solution, and ball milling to obtain HEC/BNNS solution; mixing the layered silver nanowire with the HEC/BNNS solution, and standing to obtain a HEC/BNNS/AgNWs mixed solution; forming a film from the HEC/BNNS/AgNWs mixed solution by using a tape casting method to obtain a HEC/BNNS/AgNWs composite film; the invention brings excellent mechanical properties for the composite material through the physical and chemical crosslinking effect between HEC and the nano materials BNNS and AgNWs; fully utilizes the heat-conducting property of BNNS and the electric conductivity of AgNWs; the composite film is ensured to have a flexible material with high heat conduction and high electric conduction, and the requirements of high strength, high flexibility and high sensitivity of the sensor material are met.
Description
Technical Field
The invention belongs to the technical field of composite film materials, and particularly relates to a HEC/BNNS/AgNWs composite film and a preparation method thereof.
Background
With the rapid development of intelligent wearable devices, the demand for flexible, biodegradable sensors is increasingly urgent; the traditional semiconductor material, ceramic material and the like can be used for preparing the sensor, but the traditional semiconductor material and ceramic material have poor mechanical properties and high preparation cost, and the requirements of flexibility and high sensitivity required by the preparation of the flexible sensor cannot be met.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides a HEC/BNNS/AgNWs composite film and a preparation method thereof, which are used for solving the technical problems of poor mechanical properties and high preparation cost of the existing sensor manufacturing material.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of HEC/BNNS/AgNWs composite film, comprising the following steps:
mixing boron nitride with HEC solution, and ball milling to obtain HEC/BNNS solution;
drying the silver nanowire dispersion liquid to obtain layered silver nanowires;
mixing the layered silver nanowire with the HEC/BNNS solution, and standing to obtain a HEC/BNNS/AgNWs mixed solution;
and forming a film on the HEC/BNNS/AgNWs mixed solution by using a casting method to obtain the HEC/BNNS/AgNWs composite film.
Further, the preparation process of the HEC solution specifically comprises the following steps:
adding HEC into deionized water, and stirring and dispersing under the water bath condition to obtain HEC solution; wherein the water bath temperature is 30-60 ℃, and the stirring and dispersing time is 4-8h.
Further, mixing boron nitride with HEC solution, ball milling to obtain HEC/BNNS solution, which comprises the following steps:
adding boron nitride into the HEC solution, adding grinding beads, and performing ball milling to obtain a HEC/BNNS solution;
wherein the ball milling rotating speed is 300-700rpm, and the ball milling time is 6-12h; the mass ratio of the boron nitride to the HEC solution is (0.1-1): (20-40) the concentration of the HEC solution is 1% -5%.
Further, the preparation process of the silver nanowire dispersion liquid comprises the following specific steps:
mixing and diluting the nano silver wire dispersion liquid with deionized water, and performing ultrasonic dispersion to obtain silver nano dispersion liquid; wherein the dilution factor is 5-50 times; dispersing for 2-10min with ultrasonic power of 200-600W.
Further, the process of drying the silver nanowire dispersion to obtain the layered silver nanowire is specifically as follows:
and (3) placing the silver nanowire dispersion liquid into a polytetrafluoroethylene mould, and drying for 12-48 hours at the temperature of 30-60 ℃ to obtain the layered silver nanowire.
Further, the process of mixing the layered silver nanowire with the HEC/BNNS solution and standing to obtain the HEC/BNNS/AgNWs mixed solution comprises the following steps:
and mixing the layered silver nanowire with the HEC/BNNS solution, and standing for 24-48 hours at the temperature of 25-40 ℃ to obtain the HEC/BNNS/AgNWs mixed solution.
Further, in the process of forming the film of the HEC/BNNS/AgNWs mixed solution, the film forming time is 8-16h, and the film forming temperature is 40-80 ℃.
The invention also provides a HEC/BNNS/AgNWs composite film, which is prepared according to the preparation method of the HEC/BNNS/AgNWs composite film.
Further, the breaking strength of the HEC/BNNS/AgNWs composite film is 40-80MPa, and the conductivity is 2900-6400 S.m -1 The heat conductivity is 2-10 W.m -1 ·K -1 The method comprises the steps of carrying out a first treatment on the surface of the The current change rate is 80% -95% after 1500 times of circulation.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a HEC/BNNS/AgNWs composite film and a preparation method thereof, wherein AgNWs with excellent electrochemical performance and heat conduction performance are selected as a sensor conductive material, BNNS is added into a system as a heat conduction material through HEC as a flexible matrix, a dispersing agent and an intercalating agent, and AgNWs are used as heat conduction and electric conduction materials; the HEC material has excellent film forming property and flexibility, can form a stable network structure through hydrogen bonds, can be used as a dispersing agent and an intercalating agent in the preparation of BNNS, and simultaneously brings excellent heat conductivity through the combined action of the BNNS and AgNWs; wherein HEC is used as an intercalator of BNNS and promotes dispersion of the intercalator, so that excellent mechanical properties are brought to the composite material, simultaneously AgNWs are attached to the surface of HEC/BNNS in a mode of combined action of intercalation and hydrogen bond crosslinking, and the mechanical properties are further enhanced, and meanwhile, sufficient stable conductive properties are brought; the high-strength and high-conductivity HEC/BNNS/AgNWs flexible sensor is prepared by utilizing the excellent conductivity of AgNWs to endow the composite film with conductivity; in the preparation process of the composite film, silver nanowires are paved on the surface of the HEC/BNNS film in an embedded mode, better conductivity and lower material loss are brought compared with a mixed preparation mode, and the surface of the silver nanowires is provided with a plurality of hydroxyl groups, so that hydrogen bond combination can be formed with the HEC/BNNS, and the mechanical property of the material is enhanced.
Drawings
FIG. 1 is a cross-sectional SEM image of HEC/BNNS/AgNWs composite film in example 3.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects solved by the invention more clear, the following specific embodiments are used for further describing the invention in detail. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The invention provides a preparation method of HEC/BNNS/AgNWs composite film, which comprises the following steps:
step 1, adding HEC into deionized water, and mechanically stirring and dispersing for 4-8 hours under the water bath condition to obtain HEC solution; wherein the water bath temperature is 30-60 ℃; the concentration of HEC solution is 1% -5%.
Step 2, adding 0.1-1g of Boron Nitride (BN) into 20-40g of HEC solution, adding 50-150g of agate ball milling beads, and performing ball milling in a planetary ball mill to obtain HEC/BNNS solution; wherein the ball milling rotating speed is 300-700rpm, and the ball milling time is 6-12h.
Step 3, diluting 20mg/L of nano silver wire dispersion liquid with deionized water, and performing ultrasonic dispersion to obtain silver nano wire dispersion liquid; wherein the dilution factor is 5-50 times, the ultrasonic dispersion time is 2-10min, and the ultrasonic power is 200-600W.
And 4, placing 2-10mL of the silver nanowire dispersion liquid into a polytetrafluoroethylene die with the diameter of 8-15cm, and drying for 12-48h at the temperature of 30-60 ℃ to obtain the layered silver nanowire.
And 5, adding 20-60g of HEC/BNNS solution into the layered silver nanowire in the step 4, and standing for 24-48h at the temperature of 25-40 ℃ to obtain a HEC/BNNS/AgNWs mixed solution.
Step 6, placing the HEC/BNNS/AgNWs mixed solution obtained in the step 5 in an oven for film formation by a tape casting method to obtain the HEC/BNNS/AgNWs composite film; wherein the film forming time is 8-16h, and the film forming temperature is 40-80 ℃.
The HEC/BNNS/AgNWs composite film prepared by the preparation method provided by the invention has good mechanical properties and higher electric conductivity and heat conductivity; wherein the breaking strength of the HEC/BNNS/AgNWs composite film is 40-80MPa, and the conductivity is 2900-6400 S.m -1 The heat conductivity is 2-10 W.m -1 ·K -1 The method comprises the steps of carrying out a first treatment on the surface of the The current change rate is 80% -95% after 1500 times of circulation.
The preparation principle is as follows:
according to the preparation method of the HEC/BNNS/AgNWs composite film, the HEC material which is high in yield, renewable and environment-friendly is used as a matrix, and the HEC material and the nano materials BNNS and AgNWs mutually generate physical and chemical crosslinking effects, the heat conduction performance of BNNS and the electric conduction performance of AgNWs are fully utilized, the flexible sensor material with high heat conduction and high electric conduction is prepared in a relatively simple mode, and meanwhile the requirements on high strength, high flexibility and high sensitivity of the sensor material are met; cellulose is a natural organic polymer with the most abundant content in nature, and cellulose ether prepared by etherification modification is improved, so that the problems of indissolvable conventional solvents, poor physical and chemical properties and the like are solved, and the cellulose is widely focused in the field of flexible sensors; hydroxyethyl cellulose (HEC) is used as a cellulose ether which has good water solubility and strong film forming property and has realized large-scale production, can be used as a matrix for preparing a flexible sensor, and has no heat conduction and electric conduction properties. Boron nitride nano-sheets (BNNS) are two-dimensional sheet nano-materials with extremely high thermal conductivity and thermal stability but no electric conduction performance, so silver nano-wires (AgNWs) with excellent electric conduction, thermal conductivity, high specific surface area and certain antibacterial performance are added into a HEC/BNNS system to improve the performance of the material. HEC is used as a matrix, a dispersing agent and an intercalator for preparing BNNS, BNNS and AgNWs are used as heat conduction materials, and AgNWs are used as electric conduction materials to prepare the high-heat-conductivity and high-electric-conductivity flexible sensor material with antibacterial performance
Example 1
The embodiment 1 provides a preparation method of the HEC/BNNS/AgNWs composite film, which comprises the following steps:
step 1, adding HEC into deionized water, and mechanically stirring and dispersing for 4 hours under the water bath condition to obtain HEC solution; wherein the water bath temperature is 30 ℃; the concentration of HEC solution was 1%.
Step 2, adding 0.1g of Boron Nitride (BN) into 20g of HEC solution, adding 50g of agate ball milling beads, and performing ball milling in a planetary ball mill to obtain HEC/BNNS solution; wherein the ball milling rotating speed is 300rpm, and the ball milling time is 6 hours.
Step 3, diluting 20mg/L of nano silver wire dispersion liquid with deionized water, and performing ultrasonic dispersion to obtain silver nano wire dispersion liquid; wherein the dilution factor is 50 times, the ultrasonic dispersion time is 2min, and the ultrasonic power is 200W.
And 4, placing 2mL of the silver nanowire dispersion liquid into a polytetrafluoroethylene die with the diameter of 8cm, and drying for 12 hours under the drying condition of 30 ℃ to obtain the layered silver nanowire.
And 5, adding 20g of HEC/BNNS solution into the layered silver nanowire in the step 4, and standing for 24 hours at the temperature of 25 ℃ to obtain a HEC/BNNS/AgNWs mixed solution.
Step 6, placing the HEC/BNNS/AgNWs mixed solution obtained in the step 5 in an oven for film formation by a tape casting method to obtain the HEC/BNNS/AgNWs composite film; wherein the film forming time is 8h, and the film forming temperature is 40 ℃.
Performance test results:
after mechanical, electric and heat conduction performance detection is carried out on the HEC/BNNS/AgNWs composite film prepared in the embodiment 1, the detection result is specifically as follows:
the breaking strength of the HEC/BNNS/AgNWs composite film is 40MPa, and the conductivity is 2900 S.m -1 Thermal conductivity of 2 W.m -1 ·K -1 The method comprises the steps of carrying out a first treatment on the surface of the The current change rate after 1500 cycles was 80%.
Example 2
In the embodiment 2, a preparation method of the HEC/BNNS/AgNWs composite film is provided, which comprises the following steps:
step 1, adding HEC into deionized water, and mechanically stirring and dispersing for 8 hours under the water bath condition to obtain HEC solution; wherein the water bath temperature is 60 ℃; the concentration of HEC solution was 5%.
Step 2, adding 1g of Boron Nitride (BN) into 40g of HEC solution, adding 150g of agate ball milling beads, and performing ball milling in a planetary ball mill to obtain HEC/BNNS solution; wherein the ball milling rotating speed is 700rpm, and the ball milling time is 12 hours.
Step 3, diluting 20mg/L of nano silver wire dispersion liquid with deionized water, and performing ultrasonic dispersion to obtain silver nano wire dispersion liquid; wherein the dilution factor is 5 times, the ultrasonic dispersion time is 10min, and the ultrasonic power is 600W.
And 4, placing 10mL of the silver nanowire dispersion liquid into a polytetrafluoroethylene die with the diameter of 15cm, and drying for 48 hours under the drying condition of 60 ℃ to obtain the layered silver nanowire.
And 5, adding 60g of HEC/BNNS solution into the layered silver nanowire in the step 4, and standing for 48 hours at the temperature of 40 ℃ to obtain a HEC/BNNS/AgNWs mixed solution.
Step 6, placing the HEC/BNNS/AgNWs mixed solution obtained in the step 5 in an oven for film formation by a tape casting method to obtain the HEC/BNNS/AgNWs composite film; wherein the film forming time is 16h, and the film forming temperature is 80 ℃.
Performance test results:
after mechanical, electric and heat conducting performance detection, the HEC/BNNS/AgNWs composite film prepared in example 2 has the following specific detection results:
the breaking strength of the HEC/BNNS/AgNWs composite film is 80MPa, and the conductivity is 5850 S.m -1 Thermal conductivity of 10 W.m -1 ·K -1 The method comprises the steps of carrying out a first treatment on the surface of the The current change rate after 1500 cycles was 90%.
Example 3
In this example 3, a preparation method of a HEC/BNNS/AgNWs composite film is provided, comprising the following steps:
step 1, adding HEC into deionized water, and mechanically stirring and dispersing for 5 hours under the water bath condition to obtain HEC solution; wherein the water bath temperature is 40 ℃; the concentration of HEC solution was 2%.
Step 2, adding 0.5g of Boron Nitride (BN) into 30g of HEC solution, adding 80g of agate ball milling beads, and performing ball milling in a planetary ball mill to obtain HEC/BNNS solution; wherein the ball milling rotating speed is 400rpm, and the ball milling time is 12 hours.
Step 3, diluting 20mg/L of nano silver wire dispersion liquid with deionized water, and performing ultrasonic dispersion to obtain silver nano wire dispersion liquid; wherein the dilution factor is 10 times, the ultrasonic dispersion time is 5min, and the ultrasonic power is 400W.
And 4, placing 9mL of the silver nanowire dispersion liquid into a polytetrafluoroethylene die with the diameter of 9cm, and drying for 36h under the drying condition that the temperature is 40 ℃ to obtain the layered silver nanowire.
And 5, adding 40g of HEC/BNNS solution into the layered silver nanowire in the step 4, and standing for 48 hours at the temperature of 30 ℃ to obtain a HEC/BNNS/AgNWs mixed solution.
Step 6, placing the HEC/BNNS/AgNWs mixed solution obtained in the step 5 in an oven for film formation by a tape casting method to obtain the HEC/BNNS/AgNWs composite film; wherein the film forming time is 12h, and the film forming temperature is 50 ℃.
Performance test results:
after mechanical, electric and heat conducting performance detection, the HEC/BNNS/AgNWs composite film prepared in example 3 has the following specific detection results:
the HEC/BNNS/AgThe fracture strength of the NWs composite film is 74MPa, and the conductivity is 6400 S.m -1 A thermal conductivity of 8.5 W.m -1 ·K -1 The method comprises the steps of carrying out a first treatment on the surface of the The current change rate after 1500 cycles was 95%.
Example 4
In the embodiment 4, a preparation method of the HEC/BNNS/AgNWs composite film is provided, which comprises the following steps:
step 1, adding HEC into deionized water, and mechanically stirring and dispersing for 7 hours under the water bath condition to obtain HEC solution; wherein the water bath temperature is 45 ℃; the concentration of HEC solution was 3%.
Step 2, adding 0.8g of Boron Nitride (BN) into 35g of HEC solution, adding 100g of agate ball milling beads, and performing ball milling in a planetary ball mill to obtain HEC/BNNS solution; wherein the ball milling rotating speed is 600rpm, and the ball milling time is 10 hours.
Step 3, diluting 20mg/L of nano silver wire dispersion liquid with deionized water, and performing ultrasonic dispersion to obtain silver nano wire dispersion liquid; wherein the dilution factor is 30 times, the ultrasonic dispersion time is 3min, and the ultrasonic power is 500W.
And 4, placing 8mL of the silver nanowire dispersion liquid into a polytetrafluoroethylene die with the diameter of 12cm, and drying for 16h under the drying condition of 50 ℃ to obtain the layered silver nanowire.
And 5, adding 50g of HEC/BNNS solution into the layered silver nanowire in the step 4, and standing for 48 hours at the temperature of 35 ℃ to obtain a HEC/BNNS/AgNWs mixed solution.
Step 6, placing the HEC/BNNS/AgNWs mixed solution obtained in the step 5 in an oven for film formation by a tape casting method to obtain the HEC/BNNS/AgNWs composite film; wherein the film forming time is 10h, and the film forming temperature is 60 ℃.
Performance test results:
after mechanical, electric and heat conducting property detection, the HEC/BNNS/AgNWs composite film prepared in example 4 has the following specific detection results:
the breaking strength of the HEC/BNNS/AgNWs composite film is 60MPa, and the conductivity is 4800 S.m -1 Thermal conductivity of 9 W.m -1 ·K -1 The method comprises the steps of carrying out a first treatment on the surface of the The current change rate after 1500 cycles was 85%.
Example 5
In this example 5, a preparation method of a HEC/BNNS/AgNWs composite film is provided, comprising the following steps:
step 1, adding HEC into deionized water, and mechanically stirring and dispersing for 6 hours under the water bath condition to obtain HEC solution; wherein the water bath temperature is 50 ℃; the concentration of HEC solution was 2.5%.
Step 2, adding 0.6g of Boron Nitride (BN) into 25g of HEC solution, adding 120g of agate ball milling beads, and performing ball milling in a planetary ball mill to obtain HEC/BNNS solution; wherein the ball milling rotating speed is 500rpm, and the ball milling time is 8 hours.
Step 3, diluting 20mg/L of nano silver wire dispersion liquid with deionized water, and performing ultrasonic dispersion to obtain silver nano wire dispersion liquid; wherein the dilution factor is 20 times, the ultrasonic dispersion time is 8min, and the ultrasonic power is 300W.
And 4, placing 5mL of the silver nanowire dispersion liquid into a polytetrafluoroethylene die with the diameter of 10cm, and drying for 24 hours under the drying condition of 40 ℃ to obtain the layered silver nanowire.
And 5, adding 30g of HEC/BNNS solution into the layered silver nanowire in the step 4, and standing for 36h at the temperature of 30 ℃ to obtain a HEC/BNNS/AgNWs mixed solution.
Step 6, placing the HEC/BNNS/AgNWs mixed solution obtained in the step 5 in an oven for film formation by a tape casting method to obtain the HEC/BNNS/AgNWs composite film; wherein the film forming time is 14h, and the film forming temperature is 70 ℃.
Performance test results:
after mechanical, electric and heat conducting property detection, the HEC/BNNS/AgNWs composite film prepared in example 5 has the following specific detection results:
the breaking strength of the HEC/BNNS/AgNWs composite film is 55MPa, and the conductivity is 5300 S.m -1 Thermal conductivity of 4.8 W.m -1 ·K -1 The method comprises the steps of carrying out a first treatment on the surface of the The current change rate after 1500 cycles was 90%.
As shown in fig. 1, a cross-sectional SEM image of the HEC/BNNS/AgNWs composite film of example 3 is shown in fig. 1; as can be seen from fig. 1, silver nanowires are uniformly distributed on the surface of the composite film, and form a bond with the HEC/BNNS film in an embedded manner at the interface, and HEC and BNNS are uniformly distributed inside the film; the flexibility of the composite film is not affected, and meanwhile, the uniform and good mechanical property and the stable and reliable conductive property are brought.
The above embodiment is only one of the implementation manners capable of implementing the technical solution of the present invention, and the scope of the claimed invention is not limited to the embodiment, but also includes any changes, substitutions and other implementation manners easily recognized by those skilled in the art within the technical scope of the present invention.
Claims (6)
1. The preparation method of the HEC/BNNS/AgNWs composite film is characterized by comprising the following steps:
adding boron nitride into the HEC solution, adding grinding beads, and performing ball milling to obtain a HEC/BNNS solution; wherein the ball milling rotating speed is 300-700rpm, and the ball milling time is 6-12h; the mass ratio of the boron nitride to the HEC solution is (0.1-1): (20-40) the concentration of the HEC solution is 1% -5%;
placing the silver nanowire dispersion liquid into a polytetrafluoroethylene mould, and drying for 12-48 hours at the temperature of 30-60 ℃ to obtain layered silver nanowires; mixing and diluting the nano silver wire dispersion liquid with deionized water, and performing ultrasonic dispersion to obtain silver nano wire dispersion liquid; wherein the dilution factor is 5-50 times; dispersing for 2-10min with ultrasonic power of 200-600W;
mixing the layered silver nanowire with the HEC/BNNS solution, and standing to obtain a HEC/BNNS/AgNWs mixed solution;
and forming a film on the HEC/BNNS/AgNWs mixed solution by using a casting method to obtain the HEC/BNNS/AgNWs composite film.
2. The method for preparing the HEC/BNNS/AgNWs composite film according to claim 1, wherein the preparation process of the HEC solution is as follows:
adding HEC into deionized water, and stirring and dispersing under the water bath condition to obtain HEC solution; wherein the water bath temperature is 30-60 ℃, and the stirring and dispersing time is 4-8h.
3. The method for preparing the HEC/BNNS/AgNWs composite film according to claim 1, wherein the process of mixing the layered silver nanowires with the HEC/BNNS solution and standing to obtain the HEC/BNNS/AgNWs mixed solution is specifically as follows:
and mixing the layered silver nanowire with the HEC/BNNS solution, and standing for 24-48 hours at the temperature of 25-40 ℃ to obtain the HEC/BNNS/AgNWs mixed solution.
4. The method for preparing the HEC/BNNS/AgNWs composite film according to claim 1, wherein in the process of forming the film from the HEC/BNNS/AgNWs mixed solution, the film forming time is 8-16h, and the film forming temperature is 40-80 ℃.
5. The HEC/BNNS/AgNWs composite film is characterized in that the HEC/BNNS/AgNWs composite film is prepared by the preparation method of the HEC/BNNS/AgNWs composite film according to any one of claims 1-4.
6. The HEC/BNNS/AgNWs composite film according to claim 5, wherein the breaking strength of the HEC/BNNS/AgNWs composite film is 40-80MPa and the electrical conductivity is 2900-6400 S.m -1 The heat conductivity is 2-10 W.m -1 ·K -1 The method comprises the steps of carrying out a first treatment on the surface of the The current change rate is 80% -95% after 1500 times of circulation.
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| JP2014201687A (en) * | 2013-04-08 | 2014-10-27 | 東洋インキＳｃホールディングス株式会社 | Easily deformable aggregate, heat conductive resin composition, heat conductive member and heat conductive adhesive sheet |
| CN104937044A (en) * | 2012-10-31 | 2015-09-23 | 纳米技术创新公司 | Nanotechnological thermal insulating coating and uses thereof |
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| CN104937044A (en) * | 2012-10-31 | 2015-09-23 | 纳米技术创新公司 | Nanotechnological thermal insulating coating and uses thereof |
| JP2014201687A (en) * | 2013-04-08 | 2014-10-27 | 東洋インキＳｃホールディングス株式会社 | Easily deformable aggregate, heat conductive resin composition, heat conductive member and heat conductive adhesive sheet |
| US10736250B1 (en) * | 2019-03-20 | 2020-08-04 | Korea Institute Of Science And Technology | Transparent flexible silver nanowire-based conducting film and manufacturing method thereof |
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