EP3360628A1 - Procédé de préparation de nanofils d'argent à rapport d'aspect uniforme - Google Patents

Procédé de préparation de nanofils d'argent à rapport d'aspect uniforme Download PDF

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Publication number
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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European Patent Office
Prior art keywords
solution
silver nanowires
preparation
reaction
glycerol
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EP16852969.1A
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German (de)
English (en)
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EP3360628A4 (fr
EP3360628B1 (fr
Inventor
Lu Li
Bitao LIU
Rong Jin
Shanyong CHEN
Hengqing YAN
Youwei GUAN
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Chongqing University of Arts and Sciences
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Chongqing University of Arts and Sciences
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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.

Landscapes

  • 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)
EP16852969.1A 2015-10-09 2016-03-14 Procédé de préparation de nanofils d'argent à rapport d'aspect uniforme Active EP3360628B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201510645800.3A CN105081351B (zh) 2015-10-09 2015-10-09 一种均匀的高长径比银纳米线的制备方法
PCT/CN2016/076284 WO2017059658A1 (fr) 2015-10-09 2016-03-14 Procédé de préparation de nanofils d'argent à rapport d'aspect uniforme

Publications (3)

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EP3360628A1 true EP3360628A1 (fr) 2018-08-15
EP3360628A4 EP3360628A4 (fr) 2019-07-24
EP3360628B1 EP3360628B1 (fr) 2022-02-09

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US (1) US20190054540A1 (fr)
EP (1) EP3360628B1 (fr)
JP (1) JP6732897B2 (fr)
KR (1) KR102071814B1 (fr)
CN (1) CN105081351B (fr)
WO (1) WO2017059658A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10687269B2 (en) 2015-10-09 2020-06-16 Apple Inc. Architecture for wireless network access

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CN105081351B (zh) * 2015-10-09 2017-09-26 重庆文理学院 一种均匀的高长径比银纳米线的制备方法
CN105537613B (zh) * 2015-12-25 2017-10-31 蚌埠玻璃工业设计研究院 一种微波辅助水热制备长银纳米线的方法
CN105921766A (zh) * 2016-06-14 2016-09-07 吕振瑞 一种宏量制备单分散银纳米线的方法
CN107645829B (zh) * 2017-10-16 2020-07-10 广东天承科技有限公司 一种电路板导电液及其制备方法和应用
CN108687358B (zh) * 2018-05-24 2021-03-19 首都师范大学 一种制备复合型银纳米线的方法
CN108436105B (zh) * 2018-06-07 2023-06-20 乐凯华光印刷科技有限公司 一种超长纳米银线分散液及其制备方法
CN109622984A (zh) * 2018-12-07 2019-04-16 陕西煤业化工技术研究院有限责任公司 一种超纯超细银纳米线的制备方法
CN110280781B (zh) * 2019-08-07 2022-10-25 上海渝芝实业有限公司 一种高性能的大长径比纳米银线，及其制备方法
CN113953524A (zh) * 2021-10-12 2022-01-21 浙江工业大学 一种新型多元醇溶剂热法纳米银胶的合成
CN114433865A (zh) * 2022-01-27 2022-05-06 昆明贵研新材料科技有限公司 一种高纯度银纳米线的合成方法
CN114734049A (zh) * 2022-03-14 2022-07-12 上海大学 一种利用硼氢化钠制备超小尺寸纳米银的方法
CN115870510A (zh) * 2022-11-29 2023-03-31 德清县浙工大莫干山研究院 一种水分辅助制备超细银纳米线的方法

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CN105081348B (zh) * 2015-10-09 2017-08-08 重庆文理学院 一种常压一锅法制备无颗粒高纯度银纳米线的方法
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US10687269B2 (en) 2015-10-09 2020-06-16 Apple Inc. Architecture for wireless network access

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Publication number Publication date
JP6732897B2 (ja) 2020-07-29
KR102071814B1 (ko) 2020-01-30
WO2017059658A1 (fr) 2017-04-13
CN105081351A (zh) 2015-11-25
EP3360628A4 (fr) 2019-07-24
CN105081351B (zh) 2017-09-26
KR20180049011A (ko) 2018-05-10
EP3360628B1 (fr) 2022-02-09
US20190054540A1 (en) 2019-02-21
JP2018532048A (ja) 2018-11-01

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