CN111992735A - Silver nanowire and preparation method thereof - Google Patents
Silver nanowire and preparation method thereof Download PDFInfo
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- CN111992735A CN111992735A CN202010856119.4A CN202010856119A CN111992735A CN 111992735 A CN111992735 A CN 111992735A CN 202010856119 A CN202010856119 A CN 202010856119A CN 111992735 A CN111992735 A CN 111992735A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 127
- 239000002042 Silver nanowire Substances 0.000 title claims abstract description 90
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910052709 silver Inorganic materials 0.000 claims abstract description 43
- 239000004332 silver Substances 0.000 claims abstract description 43
- 239000006185 dispersion Substances 0.000 claims abstract description 25
- 239000000203 mixture Substances 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 150000004820 halides Chemical class 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000007787 solid Substances 0.000 claims abstract description 7
- 239000011248 coating agent Substances 0.000 claims abstract description 4
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 21
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 21
- 239000001509 sodium citrate Substances 0.000 claims description 11
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 11
- 229940038773 trisodium citrate Drugs 0.000 claims description 11
- 229920000642 polymer Polymers 0.000 claims description 9
- JKFYKCYQEWQPTM-UHFFFAOYSA-N 2-azaniumyl-2-(4-fluorophenyl)acetate Chemical compound OC(=O)C(N)C1=CC=C(F)C=C1 JKFYKCYQEWQPTM-UHFFFAOYSA-N 0.000 claims description 5
- 229910021612 Silver iodide Inorganic materials 0.000 claims description 5
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 claims description 5
- 229940045105 silver iodide Drugs 0.000 claims description 5
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 3
- 239000008103 glucose Substances 0.000 claims description 3
- 229960005070 ascorbic acid Drugs 0.000 claims description 2
- 235000010323 ascorbic acid Nutrition 0.000 claims description 2
- 239000011668 ascorbic acid Substances 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 229960001031 glucose Drugs 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 5
- 239000003795 chemical substances by application Substances 0.000 abstract description 5
- -1 silver halide Chemical class 0.000 description 11
- 238000003917 TEM image Methods 0.000 description 9
- 239000007864 aqueous solution Substances 0.000 description 9
- 238000009210 therapy by ultrasound Methods 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 7
- 238000001514 detection method Methods 0.000 description 7
- 238000001000 micrograph Methods 0.000 description 7
- 239000002073 nanorod Substances 0.000 description 5
- 239000002243 precursor Substances 0.000 description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000002070 nanowire Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- TYQCGQRIZGCHNB-JLAZNSOCSA-N l-ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(O)=C(O)C1=O TYQCGQRIZGCHNB-JLAZNSOCSA-N 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 229920006316 polyvinylpyrrolidine Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0547—Nanofibres or nanotubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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Abstract
The invention discloses a preparation method of silver nanowires. Specifically disclosed is a preparation method of a silver nanowire, which comprises the following steps: 1) adding the halide solid of the silver into a reducing agent solution, and uniformly dispersing to obtain a halide dispersion liquid of the silver; 2) adding the halide dispersion liquid of silver into the inner liner of the reaction kettle, and reacting at 60-220 ℃ for 40-360 min to obtain a mixture; 3) centrifugally separating the mixture to obtain silver nanowires; wherein the halide dispersion of silver does not contain a polymeric coating agent. The method does not need to introduce an additional silver nanowire growth control agent, is simple, green and environment-friendly, and has low cost, and the surface of the obtained silver nanowire is clean and has no residues.
Description
Technical Field
The invention relates to the technical field of preparation of nano materials, in particular to a preparation method of silver nanowires.
Technical Field
The one-dimensional metal silver nanowire has unique physical and chemical properties due to the special structure of high axial-to-radial ratio, and is widely applied to the fields of electric conduction, heat conduction, sterilization, catalysis, biological and chemical sensors and the like. Based on the outstanding conductivity, light transmittance and mechanical flexibility of the electrode, the silver nanowire transparent electrode has wide market prospect in the application of flexible wearable electronic devices such as flexible touch screens, flexible displays, flexible solar cells and flexible OLEDs.
At present, the mainstream transparent electrode material indium-doped tin oxide (ITO) has the defects of brittle quality, complex process, limited indium storage capacity, high energy consumption, high cost and the like, and the requirements of the currently popular flexible wearable electronic products are increasingly difficult to meet. The silver nanowire transparent electrode has the advantages of simple process, low cost, excellent photoelectric property, mechanical flexibility and the like, and becomes the most potential alternative material of ITO. The synthesis of silver nanowires has a crucial influence on the final performance of the transparent electrode, and in the traditional preparation of silver nanowires, high molecular polymers are usually added, such as: polyvinylpyrrolidone and the like are used as a control agent for the growth of the silver nanowires to regulate the oriented growth of the silver nanowires, but the polymers are usually insulating, and can remain on the surfaces of the silver nanowires after reaction to form insulating coating layers which are difficult to remove, so that the conductivity of the silver nanowire transparent electrode is seriously reduced, and the application of the silver nanowire transparent electrode in the photoelectric field is influenced. In addition, most of reducing agents used for preparing the silver nanowires are liquid polyhydroxy alcohol, so the cost is high, and ketone organic matters generated after reaction are easy to cause harm to the environment.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of silver nanowires, which has the advantages of low cost, simple process, environmental protection, clean surface and no residue.
One aspect of the present invention provides a method for preparing a silver nanowire, comprising the steps of:
1) adding the halide solid of the silver into a reducing agent solution, and uniformly dispersing to obtain a halide dispersion liquid of the silver;
2) adding the halide dispersion liquid of silver into the inner liner of the reaction kettle, and reacting at 60-220 ℃ for 40-360 min to obtain a mixture;
3) centrifugally separating the mixture to obtain silver nanowires;
wherein the halide dispersion of silver does not contain a polymeric coating agent.
In one embodiment, in the method for preparing silver nanowires, the halide of silver is selected from at least one of silver chloride, silver bromide and silver iodide, and is preferably silver chloride.
In one embodiment, the reducing agent is at least one selected from trisodium citrate, glucose or ascorbic acid, preferably trisodium citrate.
In one embodiment, in the preparation method of the silver nanowire, in the step 1), the molar ratio of the halide of silver to the reducing agent is 1:1 to 1:20, preferably 1:1 to 1: 18.
In one embodiment, in the preparation method of the silver nanowire, the reaction temperature in the step 2) is 120-160 ℃, and preferably 140 ℃.
In one embodiment, in the preparation method of the silver nanowire, the reaction time of the step 2) is 180-220min, preferably 200 min.
In one embodiment, the concentration of the reducing agent solution is 0.05-0.5 g/mL.
In another aspect, the invention provides silver nanowires prepared by the method of the invention.
In the invention, the diameter of the obtained silver nanowire is 30-70nm, and the length is 15-25 μm; preferably, the diameter of the silver nanowires obtained is 45-55 nm.
The silver nanowire prepared by the method does not contain any high molecular polymer on the surface.
In the present invention, the polymer coating refers to a polymer, such as polyvinylpyrrolidone, which is used as a control agent for the growth of the silver nanowires and regulates the oriented growth of the silver nanowires.
Advantageous effects
According to the invention, silver halide is used as a precursor of silver, and is directly added into an aqueous solution of a reducing agent in a form of silver halide solid, silver ions in silver halide release halide ions in the reduction process, and the halide ions can be adsorbed on the side surface of a silver nanorod, so that the growth of the side surface is limited, and the silver halide ions grow into nanowires along the axial direction; in addition, the citrate in the reducer trisodium citrate can also act with the side surface of the silver nanorod to limit the growth of the side surface and promote the growth of the silver nanorod to form a nanowire along the axial direction; the chloride ions and the citrate are used as a synergistic control agent to passivate the side surface of the silver nanorod, so that silver atoms generated by reduction are accumulated on the end surface of the silver nanorod as much as possible, and a silver wire with uniform diameter and long length is obtained (the average length of the silver nanowire is only 3 mu m in the non-prior art). The method overcomes the technical prejudice, takes the silver halide solid as the precursor to react, avoids the synthesis step of the silver halide, simplifies the experiment and ensures the parallelism of different batches of experiments. Meanwhile, the invention also overcomes the defects that in the prior art, the high molecular polymer is required to be added as a control agent to regulate the oriented growth of the silver nanowires, the addition of the high molecular polymer is omitted, and the problem of ensuring the oriented growth of the silver nanowires is solved by taking the halide form of solid silver as a silver precursor.
Meanwhile, because silver halide is insoluble in water, the silver halide solid is adopted to directly react, and the reaction rate is also controlled, although reports about the reduction of silver precursors to obtain nano-silver materials exist in the prior art. However, it is well known that different reaction rates and nanomaterials are obtained by the preparation of the reaction raw materials. The silver nanowires obtained by the method have uniform size and length of more than 20 mu m.
In addition, the metal silver nanowires with clean surfaces and no residues are simply and greenly prepared by reduction with an environment-friendly reducing agent. The silver nanowire surface of the invention does not contain organic materials, so the conductivity is high.
Drawings
Fig. 1 is an X-ray diffraction pattern of the silver nanowire prepared in example 1;
FIG. 2 is a transmission electron microscope image of the silver nanowire prepared in example 1;
FIG. 3 is a transmission electron microscope image of silver nanowires prepared in example 2;
FIG. 4 is a transmission electron microscope image of the silver nanowires prepared in example 3;
FIG. 5 is a transmission electron microscope image of the silver nanowire prepared in example 4;
FIG. 6 is a transmission electron microscope image of silver nanowires prepared in example 5;
FIG. 7 is a transmission electron microscope image of silver nanowires prepared in example 6;
FIG. 8 is a transmission electron micrograph of silver nanowires prepared according to example 7;
fig. 9 is a transmission electron microscope image of the silver nanowire prepared in example 8.
Detailed Description
Example 1:
weighing 2g of silver chloride, adding the silver chloride into 200mL (0.123g/mL) of trisodium citrate aqueous solution, and performing ultrasonic treatment to obtain uniform silver chloride dispersion liquid;
adding the dispersion into the inner liner of a reaction kettle, and reacting at 140 ℃ for 200min to obtain a mixture; and centrifugally separating the mixture to obtain the silver nanowires.
Fig. 1 and 2 are an X-ray diffraction pattern and a transmission electron micrograph of the silver nanowire prepared in example 1, and it can be seen from fig. 1 that the product is a metallic silver phase and is completely crystallized, and it can be seen from fig. 2 that the product is a silver nanowire and has a clean surface without residue. After the detection, the diameter of the obtained silver nanowire is 45-55nm, and the length of the silver nanowire is 15-25 mu m.
Example 2:
weighing 2g of silver bromide, adding the silver bromide into 200mL (0.094g/mL) of trisodium citrate aqueous solution, and performing ultrasonic treatment to obtain a uniform silver bromide dispersion liquid;
adding the dispersion into the inner liner of a reaction kettle, and reacting at 140 ℃ for 200min to obtain a mixture; and centrifugally separating the mixture to obtain the silver nanowires.
Fig. 3 is a transmission electron micrograph of the silver nanowires prepared in example 2, and it can be seen from fig. 3 that the surface of the silver wires is clean without residue and there is a few granular silver. After the detection, the diameter of the obtained silver nanowire is 45-55nm, and the length of the silver nanowire is 15-25 mu m.
Example 3:
weighing 1g of silver iodide, adding the silver iodide into 100mL (0.075g/mL) of trisodium citrate aqueous solution, and performing ultrasonic treatment to obtain a uniform silver iodide dispersion liquid;
adding the dispersion into the inner liner of a reaction kettle, and reacting at 140 ℃ for 200min to obtain a mixture; and centrifugally separating the mixture to obtain the silver nanowires.
Fig. 4 is a transmission electron micrograph of the silver nanowires prepared in example 3, and it can be seen from fig. 4 that the surface of the silver wires is clean without residue and there is a few granular silver. After the detection, the diameter of the obtained silver nanowire is 45-55nm, and the length of the silver nanowire is 15-25 mu m.
Example 4:
weighing 2g of silver chloride, adding the silver chloride into 200mL (0.075g/mL) of glucose aqueous solution, and performing ultrasonic treatment to obtain a uniform silver chloride dispersion liquid;
adding the dispersion into the inner liner of a reaction kettle, and reacting at 120 ℃ for 350min to obtain a mixture; and centrifugally separating the mixture to obtain the silver nanowires.
Fig. 5 is a transmission electron micrograph of the silver nanowire prepared in example 4, and it can be seen from fig. 5 that the surface of the silver nanowire is clean without residue. After the detection, the diameter of the obtained silver nanowire is 45-55nm, and the length of the silver nanowire is 15-25 mu m.
Example 5:
weighing 3g of silver chloride, adding the silver chloride into 300mL (0.021g/mL) of trisodium citrate aqueous solution, and performing ultrasonic treatment to obtain uniform silver chloride dispersion liquid;
adding the dispersion into the inner liner of a reaction kettle, and reacting at 160 ℃ for 200min to obtain a mixture; and centrifugally separating the mixture to obtain the silver nanowires.
Fig. 6 is a transmission electron micrograph of the silver nanowires prepared in example 5, and it can be seen from fig. 6 that the surface of the silver wires is clean without residue and there is a few granular silver. After the detection, the diameter of the obtained silver nanowire is 45-55nm, and the length of the silver nanowire is 15-25 mu m.
Example 6:
weighing 5g of silver chloride, adding the silver chloride into 500mL (0.308g/mL) of trisodium citrate aqueous solution, and performing ultrasonic treatment to obtain uniform silver chloride dispersion liquid;
adding the dispersion into the inner liner of a reaction kettle, and reacting for 90min at 220 ℃ to obtain a mixture; and centrifugally separating the mixture to obtain the silver nanowires.
Fig. 7 is a transmission electron micrograph of the silver nanowire prepared in example 6, and it can be seen from fig. 7 that the surface of the silver nanowire is clean without residue and there is a few granular silver. After the detection, the diameter of the obtained silver nanowire is 45-55nm, and the length of the silver nanowire is 15-25 mu m.
Example 7:
weighing 1g of silver chloride, adding the silver chloride into 100mL (0.123g/mL) of trisodium citrate aqueous solution, and performing ultrasonic treatment to obtain uniform silver chloride dispersion liquid;
adding the dispersion into the inner liner of a reaction kettle, and reacting at 60 ℃ for 360min to obtain a mixture; and centrifugally separating the mixture to obtain the silver nanowires.
Fig. 8 is a transmission electron micrograph of the silver nanowire prepared in example 7, and it can be seen from fig. 8 that the surface of the silver nanowire is clean without residue and there is a few granular silver. After the detection, the diameter of the obtained silver nanowire is 45-55nm, and the length of the silver nanowire is 15-25 mu m.
Comparative example 8:
respectively weighing 1g of silver chloride and 1.16g of polyvinylpyrrolidone (K30) and adding the silver chloride and the polyvinylpyrrolidone into 100mL (0.123g/mL) of trisodium citrate aqueous solution, and performing ultrasonic treatment to obtain uniform silver chloride dispersion liquid;
adding the dispersion into the inner liner of a reaction kettle, and reacting at 140 ℃ for 200min to obtain a mixture; and centrifugally separating the mixture to obtain the silver nanowires.
Fig. 9 is a transmission electron micrograph of the silver nanowires prepared in comparative example 8, and it can be seen from fig. 9 that a layer of polymer exists on the surface of the silver nanowires. After side examination, the diameter of the obtained silver nanowire is 60-70nm, and the length is 15-25 μm.
Claims (10)
1. A preparation method of silver nanowires comprises the following steps:
1) adding the halide solid of silver into a reducing agent solution to obtain a halide dispersion liquid of silver;
2) adding the halide dispersion liquid of silver into the inner liner of the reaction kettle, and reacting at 60-220 ℃ for 40-360 min to obtain a mixture;
3) centrifugally separating the mixture to obtain silver nanowires;
wherein the halide dispersion of silver does not contain a polymeric coating agent.
2. The production method according to claim 1, wherein the halide of silver is at least one selected from the group consisting of silver chloride, silver bromide and silver iodide.
3. The method of any one of claims 1-2, wherein the reducing agent is selected from at least one of trisodium citrate, glucose, or ascorbic acid.
4. The production method according to any one of claims 1 to 3, wherein in the step 1), the molar ratio of the halide of silver to the reducing agent is 1:1 to 1: 20.
5. The method according to any one of claims 1-4, wherein the reaction temperature in step 2) is 120-160 ℃.
6. The method for preparing silver nanowires as claimed in any one of claims 1-5, wherein the reaction time of step 2) is 180-220 min.
7. The production method according to any one of claims 1 to 6, wherein the concentration of the reducing agent solution is 0.05 to 0.5 g/mL.
8. The production method according to any one of claims 1 to 7, wherein the obtained silver nanowires have a diameter of 30 to 70nm and a length of 15 to 25 μm.
9. Silver nanowires produced by the production method according to any one of claims 1 to 8.
10. The silver nanowires of claim 9, which have a diameter of 30-70nm and a length of 15-25 μm, and the surface of the silver nanowires does not contain any high molecular polymer.
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| CN114082975A (en) * | 2021-11-02 | 2022-02-25 | 深圳先进电子材料国际创新研究院 | Preparation method of silver nanowires |
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| CN114082975B (en) * | 2021-11-02 | 2024-05-24 | 深圳先进电子材料国际创新研究院 | Preparation method of silver nanowire |
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