WO2017059659A1 - 一种新型长径比均匀的有节点银纳米线的制备方法 - Google Patents

一种新型长径比均匀的有节点银纳米线的制备方法 Download PDF

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WO2017059659A1
WO2017059659A1 PCT/CN2016/076381 CN2016076381W WO2017059659A1 WO 2017059659 A1 WO2017059659 A1 WO 2017059659A1 CN 2016076381 W CN2016076381 W CN 2016076381W WO 2017059659 A1 WO2017059659 A1 WO 2017059659A1
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silver
triol
silver nanowires
silver nanowire
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刘碧桃
李璐
金容�
陈善勇
黎军军
闫恒庆
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Chongqing University of Arts and Sciences
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Priority to JP2018516809A priority patent/JP6735342B2/ja
Priority to EP16852970.9A priority patent/EP3360629B1/en
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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

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  • the invention relates to a method for preparing silver nanowires, in particular to a novel method for preparing silver nanowires with nodes.
  • the nanowires have a one-dimensional structure that is limited to 100 nm or less in the lateral direction, and typical metal nanowires have an aspect ratio of 1000 or more.
  • Silver nanowires have good electrical conductivity, light transmission and flexural resistance, making it possible to realize flexible transparent conductive films.
  • the preparation methods of silver nanowires have accumulated a lot, such as template method, hydrothermal method, self-assembly method, polyol method and so on.
  • the application of silver nanowires to flexible transparent conductive films has been reported in many patents and literatures. In 2011, Liu Cai-Hong et al.
  • a novel silver nanowire with uniform aspect ratio is prepared, and a silver nanowire transparent conductive film is prepared, so that the nodes exist at the intersection of the silver nanowires, and no subsequent processing is needed. Therefore, a method for controlling silver nanowires with low control factors, simple and rapid, and high-purity and high-purity, new-type nodes with uniform aspect ratio is also invented.
  • the object of the present invention is to provide a novel method for preparing a node-free silver nanowire with a simple aspect ratio and a uniform cost ratio.
  • the mother liquid containing the above silver-containing nanowires is obtained by diluting and centrifuging with absolute ethanol.
  • the silver nanowires produced by the method have high purity.
  • the dispersing agent in the above preparation method is polyvinylpyrrolidone (M w ⁇ 1300000), and the triol is a pure solution of glycerol analysis.
  • step (3) In order to make the obtained silver nanowire nodes more uniformly distributed, higher in purity, and uniform in aspect ratio, it is further preferred that in the above step (3), 40 ml, 0.05 M silver nitrate/triol solution is added to 60 ml, 0.67. The mixture of M polyvinylpyrrolidone/triol was stirred and mixed uniformly.
  • the number of times of centrifugation described above is two.
  • the silver nanowire prepared by the invention is a high quality ITO substitute material, and the silver nanowire of the invention has a uniform distribution of nodes, which significantly reduces the subsequent processing cost; the aspect ratio is uniform, and the silver nanowire slurry is uniformly coated on the transparent film.
  • the transparent conductive film prepared thereon has a light transmittance of more than 85%, and the long diameter of the silver nanowires is distributed in a diameter of 30 to 60 nm and a length of 10 to 20 ⁇ m, which is advantageous for the subsequent improvement of the conductivity; no particles exist and the purity is high.
  • the preparation method of the invention is simple, easy to control, low in cost, and suitable for industrial scale production.
  • Example 1 is a scanning electron microscope (SEM) image of a silver nanowire synthesized in Example 1 of the present invention
  • Example 2 is a transmission electron microscope (TEM) image of a silver nanowire synthesized in Example 1 of the present invention
  • Example 3 is a scanning electron microscope (SEM) image of a silver nanowire synthesized in Example 2 of the present invention
  • FIG. 1 is a scanning electron microscope (SEM) photograph of the silver nanowire obtained in the present example
  • FIG. 2 is a transmission microscope (TEM) photograph of the silver nanowire obtained in the present example.
  • FIG. 2 is a scanning electron microscope (SEM) photograph of the silver nanowire obtained in the present example.

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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)

Abstract

一种银纳米线制备方法，将分散剂溶解于三元醇中配置成黏稠透明溶液，然后将硝酸银溶解于三元醇中配置成透明溶液，再将硝酸银溶液转入分散剂溶液中混合均匀，最后将混合溶液转移至反应釜中，再放入设定温度（170～200℃）的烘箱保温一段时间结束反应。将银纳米线的母液用酒精稀释后离心分离有机物，得到长径比均匀、有节点的银纳米线。上述银纳米线制备方法简单易操作，可提高银纳米线的产量和均匀度。

Description

一种新型长径比均匀的有节点银纳米线的制备方法 技术领域
本发明涉及银纳米线的制备方法，特别是一种新型有节点的银纳米线制备方法。
背景技术
纳米线具有在横向上被限制在100nm以下的一维结构，典型的金属纳米线的长径比在1000以上。银纳米线具有良好的导电性，透光性和耐屈挠性等特点，实现柔性透明导电薄膜成为可能。通过研究学者的努力，银纳米线的制备方法已经累积了很多，如模板法，水热法，自组装法，多元醇法等。将银纳米线应用于柔性透明导电薄膜，已有许多专利和文献报道。2011年，Liu Cai-Hong等人报道银纳米线在柔性PET上制备透明导电薄膜，导电率达175Ω/sq，透射率75％，并研究了柔性薄膜的特性，经过100次弯曲后，电阻变化小于2％。(Nanoscale Re-search Letters,2011,6(75):1-8)2015年，中国专利201510034152.8公开了乙二醇还原法制备Ag纳米线，并制备透明导电电极，电阻0.97～95Ω/sq。Haifei Lu等人制备了银纳米线后制备成透明导电薄膜，再将薄膜浸在含有硝酸银和柠檬酸钠的水溶液中，光照，让银颗粒在银纳米线交叉处 选择性生长，这样大大提高透明导电薄膜的导电性能和稳定性。(Haifei Lu,Di Zhang,Xingang Ren,Selective Growth and Integration of Silver Nanoparticles on Silver Nanowires at Room Conditions for Transparent Nano-Network Electrode，ACS Nano,2014,8(10),pp 10980–10987)上述方法较为复杂。制备出新型有节点的长径比均匀的银纳米线，再制备银纳米线透明导电薄膜，这样银纳米线交叉处就已经存在节点，不需要后续加工。因此发明一种控制因素少，简单快速、大量制备高纯度无颗粒、新型有节点、长径比均匀的银纳米线的方法及其重要。
发明内容
本发明的目的在于提供一种简单易控制、成本经济的新型长径比均匀的有节点银纳米线制备方法。
本发明目的通过如下技术方案实现：
一种银纳米线制备方法，其特征在于，按如下步骤进行：
(1)将分散剂溶解于三元醇中配置成黏稠透明溶液；
(2)将硝酸银溶解于三元醇中配置成透明溶液；
(3)将上述硝酸银/三元醇溶液转入分散剂/三元醇溶液中混合均匀得到混合溶液，最后将所述混合溶液转移至反应釜中，在170-200℃下反应7-8小时，放入冷水中冷却得到含银纳米线的母液；
(4)将上述含银纳米线的母液用无水乙醇稀释离心分离制得。该方法制得的银纳米线纯度高。
为了使银纳米线存在节点，上述制备方法中分散剂为聚乙烯吡咯烷酮(Mw≈1300000)，三元醇为丙三醇分析纯溶液。
为了使制得的银纳米线节点更均匀分布、纯度更高、长径比均匀，进一步优选地，上述步骤(3)中，是将40ml，0.05M硝酸银/三元醇溶液加入60ml，0.67M聚乙烯吡咯烷酮/三元醇溶液中搅拌混合均匀。
更优选地，上述离心次数为2次。
本发明具有如下有益效果：
采用本发明制备银纳米线是一种优质的ITO替代材料，本发明银纳米线均匀分布有节点、显著减少了后续加工成本；长径比均匀、该银纳米线浆料均匀涂布在透明薄膜上制备成的透明导电薄膜透光率达85％以上，银纳米线的长径分布在直径30～60nm、长10～20μm，大大利于后续导电性能的提升；无颗粒存在、纯度高。本发明制备方法简单易控制、成本低、适于工业化规模生产。
附图说明
图1是本发明实施例1合成的银纳米线扫描电子显微镜(SEM)图；
图2是本发明实施例1合成的银纳米线透射电子显微镜(TEM)图；
图3是本发明实施例2合成的银纳米线扫描电子显微镜(SEM)图；
具体实施方式
下面结合具体实施例对本发明技术作进一步说明。
实施例1：
将40ml，0.05M硝酸银/三元醇溶液加入60ml，0.67M聚乙烯吡咯烷酮/三元醇溶液中，搅拌混合均匀，然后将混合溶液转移至反应釜中，最后将反应釜放入温度已升至170℃的烘箱中，保温8h后取出结束实验；
将反应釜中Ag纳米线母液用无水乙醇稀释离心分离，重复2次，得到直径30～60nm，长10～20μm的新型长径比均匀的有节点银纳米线分散在异丙醇或无水乙醇中；图1是本实施例得到的银纳米线的扫描电子显微镜(SEM)照片，图2是本实施例得到的银纳米线的透射显微镜(TEM)照片。
实施例2：
将40ml，0.05M硝酸银/三元醇溶液加入60ml，0.67M聚乙烯吡咯烷酮/三元醇溶液中，搅拌混合均匀，然后将混合溶液转移至反应釜中，最后将反应釜放入温度已升至200℃的烘箱中，保温8h后取出结束实验；
将反应釜中Ag纳米线母液用无水乙醇稀释离心分离，重复2次，得到直径30～60nm，长10～20μm的新型长径比均匀的有节点银纳米线分散在异丙醇或无水乙醇中；图2是本实施例得到的银纳米线的扫描电子显微镜(SEM)照片。

Claims (7)

  1. 一种银纳米线制备方法，其特征在于，按如下步骤进行：
    (1)将分散剂溶解于三元醇中配置成黏稠透明溶液；
    (2)将硝酸银溶解于三元醇中配置成透明溶液；
    (3)将上述硝酸银/三元醇溶液转入分散剂/三元醇溶液中混合均匀得到混合溶液，最后将所述混合溶液转移至反应釜中，在170-200℃下反应7-8小时，放入冷水中冷却得到含银纳米线的母液；
    (4)将上述含银纳米线的母液用无水乙醇稀释离心分离制得。
  2. 如权利要求1所述银纳米线的制备方法，其特征在于：所述步骤(1)中分散剂为聚乙烯吡咯烷酮。
  3. 如权利要求1或2所述银纳米线的制备方法，其特征在于：所述三元醇为丙三醇分析纯溶液。
  4. 如权利要求2所述银纳米线的制备方法，其特征在于：所述步骤(3)中，是将40ml，0.05M硝酸银/三元醇溶液加入60ml，0.67M聚乙烯吡咯烷酮/三元醇溶液中搅拌混合均匀。
  5. 如权利要求3所述银纳米线的制备方法，其特征在于：所述步骤(3)中，是将40ml，0.05M硝酸银/三元醇溶液加入60ml，0.67M聚乙烯吡咯烷酮/三元醇溶液中搅拌混合均匀。
  6. 如权利要求3所述银纳米线的制备方法，其特征在于：所述离心次数为2次。
  7. 如权利要求5所述银纳米线的制备方法，其特征在于：所述离心次数为2次。
PCT/CN2016/076381 2015-10-09 2016-03-15 一种新型长径比均匀的有节点银纳米线的制备方法 Ceased WO2017059659A1 (zh)

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US15/763,118 US10773312B2 (en) 2015-10-09 2016-03-15 Preparation method for silver nanowires with uniform aspect ratio and nodes
KR1020187009451A KR102070529B1 (ko) 2015-10-09 2016-03-15 균일한 종횡비를 갖는 노드가 있는 은 나노와이어의 신규한 제조방법
JP2018516809A JP6735342B2 (ja) 2015-10-09 2016-03-15 新規のアスペクト比が均一でノードを有する銀ナノワイヤの製造方法
EP16852970.9A EP3360629B1 (en) 2015-10-09 2016-03-15 Method for preparing new silver nanowires with uniform aspect ratio and nodes

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CN105081350B (zh) 2015-10-09 2017-08-29 重庆文理学院 一种新型长径比均匀的有节点银纳米线的制备方法
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US20190054539A1 (en) 2019-02-21
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