Method for preparing silver nanowires

A technology of silver nanowires and silver salts, which is applied in the field of nanomaterials to achieve the effects of high reproducibility, strong controllability, and uniform size and shape

Active Publication Date: 2015-03-25
苏州恒拓服饰有限公司
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0005] Abandoning traditional surfactants, adopting a combination of polyol method and solvothermal method, using the unique protective function of mic

Method used

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  • Method for preparing silver nanowires
  • Method for preparing silver nanowires
  • Method for preparing silver nanowires

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 取油酰氯4.4mL溶于20mL甲苯中,2g超支化聚缩水甘油醚溶于20mL吡啶中,所得油酰氯甲苯溶液逐滴滴至超支化聚缩水甘油醚的吡啶溶液中,冰浴搅拌48h后,80℃条件下旋转蒸发除去多余溶剂,经氯仿洗涤去除多余的油酰氯,得到两亲性超支化聚缩水甘油醚。

[0027] 取21mg两亲性超支化聚缩水甘油醚溶于50ml乙二醇中,得混合溶液A。1.6mg 无水氯化铁和0.212g硝酸银依次加入混合溶液A中,搅拌至金属盐完全溶解,得混合溶液C。将混合溶液C转移至水热反应釜中,180℃反应90min,自然冷却后取出粗产物,经丙酮和无水乙醇反复洗涤,6000r / min离心分离产物,得到直径约为120nm的银纳米线。

[0028] See attached figure 1 ,是本实施例提供的银纳米线的扫描电镜(SEM)图(放大40K倍)。由图可见,银纳米线的直径在120nm左右,且非常均匀。

[0029] See attached figure 2 ,是本实施例提供的银纳米线的透射电镜(TEM)图。图中银纳米线的直径也在120nm左右,分布均匀,与 figure 1 中SEM显示结果基本一致。

[0030] See attached image 3 ,是本实施例获得的纳米银线的XRD谱图。其 XRD衍射峰与纳米银XRD的标准谱图(JCPDS No.4-0781)完全对应,5个衍射峰分别对应为纳米银的(111), (200)、(220)、(311) 和(222)晶面衍射峰,且银纳米线的 (111) 晶面与 (200)晶面的强度比较高,这意味着银纳米线是沿着 (111) 晶面生长的,表明本方法制备得到的产品确为银纳米线。

Embodiment 2

[0032] 取油酰氯1.0mL溶于60mL甲苯中,1g端氨基超支化聚合物溶于80mL吡啶中,所得油酰氯甲苯溶液逐滴滴至端氨基超支化聚合物的吡啶溶液中,25℃搅拌40h后,80℃条件下旋转蒸发除去多余溶剂,经丙酮洗涤去除多余的油酰氯,得到两亲性端氨基超支化聚合物。

[0033] 取84mg两亲性端氨基超支化聚合物溶于50ml乙二醇中,得混合溶液A。0.8mg 无水氯化铁和0.212g硝酸银依次加入混合溶液A中,搅拌至金属盐完全溶解,得混合溶液C。将混合溶液C转移至水热反应釜中,200℃反应80min,自然冷却后取出粗产物,经氯仿和无水乙醇反复洗涤,6000r / min离心分离产物,得到直径约为200nm的银纳米线。

Embodiment 3

[0035]Dissolve 6.0 mL of oleoyl chloride in 40 mL of ether, 2 g of hyperbranched polyglycidyl ether in 40 mL of methanol, and drop the obtained oleoyl chloride ether solution dropwise into the methanol solution of hyperbranched polyglycidyl ether, and stir for 56 hours under ice bath , rotary evaporation at 50°C to remove excess solvent, and wash with ethyl acetate to remove excess oleoyl chloride to obtain amphiphilic hyperbranched polyglycidyl ether.

[0036] Take 108 mg of amphiphilic hyperbranched polyglycidyl ether and dissolve it in 50 ml of ethylene glycol to obtain mixed solution A. Add 5.6mg of anhydrous ferric chloride and 0.45g of silver nitrate to the mixed solution A in sequence, and stir until the metal salt is completely dissolved to obtain the mixed solution C. The mixed solution C was transferred to a hydrothermal reaction kettle, and reacted at 170°C for 100 min. After natural cooling, the crude product was taken out, washed repeatedly with chloroform and abs...

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Abstract

The invention discloses a method for preparing silver nanowires. The silver nanowires are prepared controllably by the self-assembly characteristic of micelle of amphiphilic hyperbranched polymer. The method comprises the following specific steps of dissolving or dispersing the amphiphilic hyperbranched polymer in polyhydric alcohol; adding halogenous inorganic salt or sulfurated inorganic salt in the mixture; adding silver salt in the mixture after the halogenous inorganic salt or sulfurated inorganic salt is dissolved in the mixture completely; placing obtained mixed solution in a sealed reaction kettle; performing constant-temperature reaction at a certain temperature in a range of 120-240 DEG C; naturally cooling down a reaction product to obtain raw products of silver nanowires; and washing the raw products by using organic solvent and centrifugally separating the raw products to obtain the silver nanowires. A one-kettle solvothermal method is used, the amphiphilic hyperbranched polymer is used for preparation of the silver nanowires, and the silver nanowires with uniform sizes and morphologies can be obtained. The steps of the method are simple and are easy to operate; the controllability and the reproducibility are high; and the silver nanowires are easily produced in batches.

Description

technical field [0001] 本发明涉及一种制备银纳米线的方法,属于纳米材料领域。 Background technique [0002] 近年来,一维贵金属纳米材料因其独特的电、磁、热、光学性能,及其在微电子器件、光电子器件、传感器等领域的巨大应用潜力而备受关注。一维贵金属纳米材料因具备表面等离子体共振吸收性能,可用于荧光、拉曼散射等信号的放大增强;此外,因其最大吸收峰与环境介电常数的关系,使其可用于传感器及电子和光学器件的制备。在众多一维贵金属纳米材料中,银纳米线除具备上述等离子体共振吸收性能外,还具有非常优良的电导和热导性能,且在不同环境下均显示出高稳定性,已广泛应用于偏光器件、分子器件、光电子晶体、催化剂、生物化学传感器、太阳能电池等领域,且在各类导电材料中有着极其重要的作用,其前景广阔。 [0003] 目前,银纳米线的制备方法有多种,主要分为模板法、晶种生长法和湿热化学法。模板法又分为硬模板法和软模板法。硬模板法通常以多孔氧化铝、碳纳米管、气凝胶等为模板,通过电沉积、化学沉积等方式制备银纳米线;软模板法则是以高分子表面活性剂为模板,再以化学还原法制备各类银纳米线。其优点是可严格控制银纳米线的尺寸形貌均匀一致,但是其尺寸、形貌受控于模板本身所具有的形貌、尺寸,因此其对合成模板的要求较高,且后续对银纳米线表面模板的去除过程复杂、成本高,难以高效、简便、大量地合成银纳米线。晶种生长法可在室温下成功制备金属纳米线,但需要事先引入晶种,导致其制备过程繁琐、实用性差。 [0004] 多羟基还原法又叫多元醇法,是目前制备银纳米线的最主要方法。中国发明专利CN103433503A, CN103537710A, CN102689018A, CN102328095A, CN101934378A分别公开了银纳米线的合成方法,各方法主体均为将银盐和聚乙烯吡咯烷酮的多羟基醇溶液缓慢匀速混合,或外加还原性成分,经绝氧加热、搅拌数小时至数十小时不等,得到银纳米线。这些方法需要冷凝回流、惰性气体保护,尤其溶液混合速度、加热温度等因素会直接影响到产品的尺寸大小、形貌均一性、产量等,因此操作难度大,可控性差,不易批量生产。此外,上述方法中均使用到了聚乙烯吡咯烷酮(PVP),在该类体系下,PVP通过优先吸附于多重孪晶晶种的{100}晶面族,使其...

Claims

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Application Information

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IPC IPC(8): B22F9/24B82Y40/00
Inventor 熊佳庆林红陈宇岳修阿男
Owner 苏州恒拓服饰有限公司
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