EP3360628A1 - Uniform aspect ratio silver nanowires preparation method - Google Patents
Uniform aspect ratio silver nanowires preparation method Download PDFInfo
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- EP3360628A1 EP3360628A1 EP16852969.1A EP16852969A EP3360628A1 EP 3360628 A1 EP3360628 A1 EP 3360628A1 EP 16852969 A EP16852969 A EP 16852969A EP 3360628 A1 EP3360628 A1 EP 3360628A1
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- silver nanowires
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- glycerol
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 239000002042 Silver nanowire Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 51
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 9
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 9
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 9
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 9
- 239000000376 reactant Substances 0.000 claims abstract description 3
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 7
- 239000012498 ultrapure water Substances 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 7
- 238000009776 industrial production Methods 0.000 abstract description 2
- 150000002500 ions Chemical class 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 37
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 8
- 239000010408 film Substances 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000010413 mother solution Substances 0.000 description 3
- 239000002070 nanowire Substances 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000004917 polyol method Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/25—Noble metals, i.e. Ag Au, Ir, Os, Pd, Pt, Rh, Ru
- B22F2301/255—Silver or gold
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2304/00—Physical aspects of the powder
- B22F2304/05—Submicron size particles
- B22F2304/054—Particle size between 1 and 100 nm
Definitions
- the present invention relates to a preparation method for silver nanowires, and more particularly, to a preparation method for silver nanowires with a uniform aspect ratio.
- silver nanowires Based on the properties of high specific surface area, electrical conductivity and thermal conductivity, silver nanowires have a broad application prospect. Especially, the silver nanowires can be used as an alternative material of ITO in fields such as solar energy, OLED, and flexible and large-size touch screen displays, and used in fields such as conductive polymers, composite materials, and electrode printing ink additives. Therefore, the preparation of silver nanowires has become a focus of researchers. At present, there are many documents and patent reports on the preparation methods and applications of silver nanowires.
- Xia Younan the first one who prepares silver nanowires with a polyol method, proposed the preparation of silver nanowires with a high aspect ratio by using Pt as seeds and reducing silver nitrate by ethylene glycol (Advanced Materials (2002) 14,883 ).
- the polyol reduction method was combined with the hydrothermal method, and a small amount of sodium chloride, ferric chloride, copper chloride and other metal halide were introduced to function with Ag ions to form a colloid, which serves as seeds to prepare silver nanowires.
- the silver nanowires can be quickly prepared by the combination of the polyol method and the microwave method.
- the silver nanowires thus obtained have a relatively non-uniform aspect ratio, and have a large amount of impurities.
- Chinese Patent Application No. 200810019828.6 disclosed a batch preparation method for silver nanowires
- Chinese Patent Application No. 201010559335.9 disclosed a method for preparing silver nanowires with controlled diameter by using a cation-controlled microwave method.
- he prepared silver nanowires are less than 30 ⁇ m in length, and have a non-uniform aspect ratio.
- Chinese Patent No. CN 1843670A reported the use of a composite solvent of glycerol and water or ethanol or isopropanol for reduction to prepare silver nanowires.
- the obtained silver nanowires have a length of 5-200 ⁇ m and a diameter of 70-90 nm. Although many preparation methods for silver nanowires have been reported, few of them can obtain silver nanowires with a uniform aspect ratio and no other particles or impurities. Therefore, it is very important to invent a method that has a stable process, has fewer control factors, is simple and quick, can prepare a large quantity of Ag nanowires.
- the present invention is directed to a preparation method of silver nanowires with a uniform aspect ratio, which is simple, easy to control, and cost-effective.
- the present invention is achieved through the following technical solution.
- a preparation method for silver nanowires includes the following steps:
- reaction time in the reaction kettle is 9-10 hours.
- step (1) 0.16 g-0.32 g silver nitrate is dissolved at room temperature in 20 ml of glycerol to get the solution A.
- step (2) 5 g-7 g polyvinylpyrrolidone is dissolved at room temperature in 80 ml of glycerol to get the solution B.
- step (4) 2.5 ml-10 ml of the ultrapure water is added into the solution C and mixed uniformly to form the solution D.
- centrifuging is performed twice.
- the preparation method of the present invention is simple to operate, easy to control, cost-effective, and very suitable for large-scale industrial production.
- the prepared silver nanowires have a uniform aspect ratio, and transparent conductive films based on the silver nanowires have a high transparency of 90-91 %.
- the silver nanowires have a diameter of up to 30-40 nm and a length of 10-20 ⁇ m, and the silver nanowires with the aspect ratio have small resistance, which is beneficial to the improvement of electrical conductivity.
- the silver nanowires have no particles and feature high purity.
- 0.16 g silver nitrate was dissolved at room temperature in 20 ml of glycerol to get a solution A; 5 g polyvinylpyrrolidone was dissolved at room temperature in 80 ml of glycerol to get a solution B; the solution A and the solution B were mixed uniformly to form a solution C; then, 5 ml of ultrapure water was added into the solution C and mixed uniformly to form a solution D, finally, the solution D was transferred into a reaction kettle, the reaction kettle was put into an oven with a set temperature of 160°C, and the reaction ended after a certain time of reaction.
- FIG. 1 is a scanning electron microscope (SEM) diagram of a silver nanowire synthesized in Example 1.
- the silver nanowires prepared in Example 1 above were formulated into 1g/L silver nanowire slurry, and 500 ⁇ L of slurry was uniformly coated on an A4-size transparent film to prepare a transparent conductive film.
- the sheet resistance of the transparent conductive film was 42 ohm/sq.
- the transmittance of the transparent conductive film was measured with a UV-Vis spectrophotometer. As shown in FIG. 2 , at the visible light wavelength of 550 nm, the transmittance of the transparent conductive film was 90.8%.
- 0.16 g silver nitrate was dissolved at room temperature in 20 ml of glycerol to get a solution A; 5 g polyvinylpyrrolidone was dissolved at room temperature in 80 ml of glycerol to get a solution B; the solution A and the solution B were mixed uniformly to form a solution C; then, 2.5 ml of ultrapure water was added into the solution C and mixed uniformly to form a solution D, finally, the solution D was transferred into a reaction kettle, the reaction kettle was put into an oven with a set temperature of 160°C, and the reaction ended after a certain time of reaction.
- the Ag nanowire mother solution in the reaction kettle was diluted with alcohol and centrifuged twice to obtain precipitated silver nanowires having a diameter of 30-40 nm and a length of 10-20 ⁇ m, which was dispersed in isopropanol.
- 0.32 g silver nitrate was dissolved at room temperature in 20 ml of glycerol to get a solution A; 7 g polyvinylpyrrolidone was dissolved at room temperature in 80 ml of glycerol to get a solution B; the solution A and the solution B were mixed uniformly to form a solution C; then, 10 ml of ultrapure water was added into the solution C and mixed uniformly to form a solution D, finally, the solution D was transferred into a reaction kettle, the reaction kettle was put into an oven with a set temperature of 160°C, and the reaction ended after a certain time of reaction.
- the Ag nanowire mother solution in the reaction kettle was diluted with alcohol and centrifuged twice to obtain precipitated silver nanowires having a diameter of 30-40 nm and a length of 10-20 ⁇ m, which was dispersed in isopropanol.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Conductive Materials (AREA)
- Non-Insulated Conductors (AREA)
Abstract
Description
- The present invention relates to a preparation method for silver nanowires, and more particularly, to a preparation method for silver nanowires with a uniform aspect ratio.
- Based on the properties of high specific surface area, electrical conductivity and thermal conductivity, silver nanowires have a broad application prospect. Especially, the silver nanowires can be used as an alternative material of ITO in fields such as solar energy, OLED, and flexible and large-size touch screen displays, and used in fields such as conductive polymers, composite materials, and electrode printing ink additives. Therefore, the preparation of silver nanowires has become a focus of researchers. At present, there are many documents and patent reports on the preparation methods and applications of silver nanowires. For example, Xia Younan, the first one who prepares silver nanowires with a polyol method, proposed the preparation of silver nanowires with a high aspect ratio by using Pt as seeds and reducing silver nitrate by ethylene glycol (Advanced Materials (2002) 14,883).The polyol reduction method was combined with the hydrothermal method, and a small amount of sodium chloride, ferric chloride, copper chloride and other metal halide were introduced to function with Ag ions to form a colloid, which serves as seeds to prepare silver nanowires. The silver nanowires can be quickly prepared by the combination of the polyol method and the microwave method. However, the silver nanowires thus obtained have a relatively non-uniform aspect ratio, and have a large amount of impurities. For example, Chinese Patent Application No.
200810019828.6 201010559335.9 CN 1843670A reported the use of a composite solvent of glycerol and water or ethanol or isopropanol for reduction to prepare silver nanowires. The obtained silver nanowires have a length of 5-200 µm and a diameter of 70-90 nm. Although many preparation methods for silver nanowires have been reported, few of them can obtain silver nanowires with a uniform aspect ratio and no other particles or impurities. Therefore, it is very important to invent a method that has a stable process, has fewer control factors, is simple and quick, can prepare a large quantity of Ag nanowires. - The present invention is directed to a preparation method of silver nanowires with a uniform aspect ratio, which is simple, easy to control, and cost-effective.
- The present invention is achieved through the following technical solution.
- A preparation method for silver nanowires includes the following steps:
- (1) dissolving silver nitrate in glycerol to get a solution A;
- (2) dissolving polyvinylpyrrolidone in glycerol to get a solution B;
- (3) mixing uniformly the solution A and the solution B to form a solution C; and
- (4) adding an ultrapure water medium into the solution C and mixing uniformly to form a solution D, finally, transferring the solution D into a reaction kettle for reaction at 150°C±10°C, and centrifuging the reactants to obtain silver nanowires. The obtained silver nanowires have high purity and a uniform aspect ratio.
- Preferably, reaction time in the reaction kettle is 9-10 hours.
- To further improve purity and uniformity of the aspect ratio of the silver nanowires, preferably, in step (1), 0.16 g-0.32 g silver nitrate is dissolved at room temperature in 20 ml of glycerol to get the solution A.
- More preferably, in step (2), 5 g-7 g polyvinylpyrrolidone is dissolved at room temperature in 80 ml of glycerol to get the solution B.
- More preferably, in step (4), 2.5 ml-10 ml of the ultrapure water is added into the solution C and mixed uniformly to form the solution D.
- Further, the centrifuging is performed twice.
- The present invention has the following beneficial effects:
- The preparation method of the present invention is simple to operate, easy to control, cost-effective, and very suitable for large-scale industrial production. The prepared silver nanowires have a uniform aspect ratio, and transparent conductive films based on the silver nanowires have a high transparency of 90-91 %. The silver nanowires have a diameter of up to 30-40 nm and a length of 10-20 µm, and the silver nanowires with the aspect ratio have small resistance, which is beneficial to the improvement of electrical conductivity. In addition, the silver nanowires have no particles and feature high purity.
-
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FIG. 1 is a scanning electron microscope (SEM) diagram of a silver nanowire synthesized in Example 1 of the present invention; and -
FIG. 2 is a diagram showing transmittance of a conductive thin film made of silver nanowires synthesized in Example 1 of the present invention. - The technology of the present invention will be further described below with reference to specific examples.
- 0.16 g silver nitrate was dissolved at room temperature in 20 ml of glycerol to get a solution A; 5 g polyvinylpyrrolidone was dissolved at room temperature in 80 ml of glycerol to get a solution B; the solution A and the solution B were mixed uniformly to form a solution C; then, 5 ml of ultrapure water was added into the solution C and mixed uniformly to form a solution D, finally, the solution D was transferred into a reaction kettle, the reaction kettle was put into an oven with a set temperature of 160°C, and the reaction ended after a certain time of reaction.
- The Ag nanowire mother solution in the reaction kettle was diluted with alcohol and centrifuged twice to obtain precipitated silver nanowires having a diameter of 30-40 nm and a length of 10-20 µm, which were dispersed in isopropanol.
FIG. 1 is a scanning electron microscope (SEM) diagram of a silver nanowire synthesized in Example 1. - The silver nanowires prepared in Example 1 above were formulated into 1g/L silver nanowire slurry, and 500 µL of slurry was uniformly coated on an A4-size transparent film to prepare a transparent conductive film. The sheet resistance of the transparent conductive film was 42 ohm/sq. Then, the transmittance of the transparent conductive film was measured with a UV-Vis spectrophotometer. As shown in
FIG. 2 , at the visible light wavelength of 550 nm, the transmittance of the transparent conductive film was 90.8%. - 0.16 g silver nitrate was dissolved at room temperature in 20 ml of glycerol to get a solution A; 5 g polyvinylpyrrolidone was dissolved at room temperature in 80 ml of glycerol to get a solution B; the solution A and the solution B were mixed uniformly to form a solution C; then, 2.5 ml of ultrapure water was added into the solution C and mixed uniformly to form a solution D, finally, the solution D was transferred into a reaction kettle, the reaction kettle was put into an oven with a set temperature of 160°C, and the reaction ended after a certain time of reaction.
- The Ag nanowire mother solution in the reaction kettle was diluted with alcohol and centrifuged twice to obtain precipitated silver nanowires having a diameter of 30-40 nm and a length of 10-20 µm, which was dispersed in isopropanol.
- 0.32 g silver nitrate was dissolved at room temperature in 20 ml of glycerol to get a solution A; 7 g polyvinylpyrrolidone was dissolved at room temperature in 80 ml of glycerol to get a solution B; the solution A and the solution B were mixed uniformly to form a solution C; then, 10 ml of ultrapure water was added into the solution C and mixed uniformly to form a solution D, finally, the solution D was transferred into a reaction kettle, the reaction kettle was put into an oven with a set temperature of 160°C, and the reaction ended after a certain time of reaction.
- The Ag nanowire mother solution in the reaction kettle was diluted with alcohol and centrifuged twice to obtain precipitated silver nanowires having a diameter of 30-40 nm and a length of 10-20 µm, which was dispersed in isopropanol.
Claims (7)
- A preparation method for silver nanowires, comprising the following steps:(1) dissolving silver nitrate in glycerol to get a solution A;(2) dissolving polyvinylpyrrolidone in glycerol to get a solution B;(3) mixing uniformly the solution A and the solution B to form a solution C; and(4) adding an ultrapure water medium into the solution C and mixing uniformly to form a solution D, finally, transferring the solution D into a reaction kettle for reaction at 150°C±10°C, and centrifuging the reactants to obtain silver nanowires.
- The preparation method according to claim 1, wherein reaction time in the reaction kettle is 9-10 hours.
- The preparation method according to claim 1 or 2, wherein in step (1), 0.16 g-0.32 g silver nitrate is dissolved at room temperature in 20 ml of glycerol to get the solution A.
- The preparation method according to claim 3, wherein in step (2), 5 g-7 g polyvinylpyrrolidone is dissolved at room temperature in 80 ml of glycerol to get the solution B.
- The preparation method according to claim 4, wherein in step (4), 2.5 ml-10 ml of the ultrapure water is added into the solution C and mixed uniformly to form the solution D.
- The preparation method according to claim 1 or 2, wherein the centrifuging is performed twice.
- The preparation method according to claim 5, wherein the centrifuging is performed twice.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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CN201510645800.3A CN105081351B (en) | 2015-10-09 | 2015-10-09 | A kind of preparation method of uniform high length-diameter ratio nano silver wire |
PCT/CN2016/076284 WO2017059658A1 (en) | 2015-10-09 | 2016-03-14 | Uniform aspect ratio silver nanowires preparation method |
Publications (3)
Publication Number | Publication Date |
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EP3360628A1 true EP3360628A1 (en) | 2018-08-15 |
EP3360628A4 EP3360628A4 (en) | 2019-07-24 |
EP3360628B1 EP3360628B1 (en) | 2022-02-09 |
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US (1) | US20190054540A1 (en) |
EP (1) | EP3360628B1 (en) |
JP (1) | JP6732897B2 (en) |
KR (1) | KR102071814B1 (en) |
CN (1) | CN105081351B (en) |
WO (1) | WO2017059658A1 (en) |
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CN105081351B (en) * | 2015-10-09 | 2017-09-26 | 重庆文理学院 | A kind of preparation method of uniform high length-diameter ratio nano silver wire |
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CN113953524A (en) * | 2021-10-12 | 2022-01-21 | 浙江工业大学 | Novel synthesis of nano-silver colloid by polyol solvothermal method |
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CN105081351B (en) * | 2015-10-09 | 2017-09-26 | 重庆文理学院 | A kind of preparation method of uniform high length-diameter ratio nano silver wire |
CN105081348B (en) * | 2015-10-09 | 2017-08-08 | 重庆文理学院 | A kind of normal pressure one kettle way prepares the method without particle high-purity silver nano wire |
CN105081350B (en) * | 2015-10-09 | 2017-08-29 | 重庆文理学院 | A kind of new draw ratio uniformly has the preparation method of node nano silver wire |
-
2015
- 2015-10-09 CN CN201510645800.3A patent/CN105081351B/en not_active Expired - Fee Related
-
2016
- 2016-03-14 KR KR1020187009450A patent/KR102071814B1/en active IP Right Grant
- 2016-03-14 JP JP2018516800A patent/JP6732897B2/en active Active
- 2016-03-14 WO PCT/CN2016/076284 patent/WO2017059658A1/en active Application Filing
- 2016-03-14 US US15/763,119 patent/US20190054540A1/en not_active Abandoned
- 2016-03-14 EP EP16852969.1A patent/EP3360628B1/en active Active
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US10687269B2 (en) | 2015-10-09 | 2020-06-16 | Apple Inc. | Architecture for wireless network access |
Also Published As
Publication number | Publication date |
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JP6732897B2 (en) | 2020-07-29 |
KR102071814B1 (en) | 2020-01-30 |
WO2017059658A1 (en) | 2017-04-13 |
CN105081351A (en) | 2015-11-25 |
EP3360628A4 (en) | 2019-07-24 |
CN105081351B (en) | 2017-09-26 |
KR20180049011A (en) | 2018-05-10 |
EP3360628B1 (en) | 2022-02-09 |
US20190054540A1 (en) | 2019-02-21 |
JP2018532048A (en) | 2018-11-01 |
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