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22 Proc.of SPIE Vol.8691 纳米银 PVP+硝酸银 86910Q-1

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Particle based conductive silver ink customized for ink jet printing on cellulose electro-active paper

Mohammad Abu Hasan Khondokera, Seong Cheonl Muna, Jaehwan Kim*a

aDepartment of Mechanical Engineering, Inha University, 253 Yonghyun-Dong, Nam-Ku

Incheon 402-751, Korea

ABSTRACT

A previously synthesized silver nanoparticle based conductive silver ink was used in this work to print conductive

electrodes on cellulose electro-active paper (EAPap) by using an inkjet printer. Then, Inkjet printed cellulose EAPap

experienced a post-deposition heat treatment-sintering process to enhance electrical conductivity of printed electrodes by

converting those printed patterns into continuous metallic state. The dependences of electrical bulk resistivity of printed

electrodes on both sintering temperature and sintering time were checked. It was found that, higher sintering

temperatures and longer sintering process result lower resistivity. In addition, the uniformity of the thicknesses of printed

electrodes through transverse direction and the relationship between thickness and the number of printing also had been

analyzed. Those printed electrodes also showed very good adhesion on cellulose EAPap.

Keywords: Conductive silver ink, inkjet printing, cellulose EAPap, printed electrodes, electrical resistivity, sintering

process

1. INTRODUCTION

As a natural biodegradable polymer, cellulose is everywhere. Huge biomass production of cellulose made it as

inexhaustible raw material for environmentally friendly and biocompatible products [1]. The discovery of cellulose as a

smart material dates back to 2006 when Kim et. al. reported the actuation effect of cellulose electro-active paper

(EAPap) [2]. Cellulose EAPap with printed electrode has potentiality in microelectromechanical system (MEMS)

application. Electrodes can be inkjet printed by microscale patterning of lines or dots by ejecting tiny droplets of 10–100

µm diameter [3]. Moreover, promising technologies, such as inkjet printing/electrohydrodynamic jet printing

(EHDP)/drop-on-demand patterning, have been paid attention to print conductive patterns for fabricating flexible,

lightweight, disposable devices and polymer based flexible microelectronics [4–7]. They are one-step processes and do

not need coating and etching.

In this work, an inkjet printer was used to find best printing quality by changing several printing conditions (no. of

nozzle, position of nozzle, firing voltage etc.) and silver ink content. Finally, around 40 µm wide electrodes were

successfully printed on cellulose EAPap with synthesized silver ink. Cellulose EAPap’s were prepared from regenerated

cellulose films by the procedure described elsewhere [8-10].

2. EXPERIMENTAL

2.1 Synthesis process of silver ink

Firstly, silver nanoparticles were synthesized through modified polyol process [11]. In brief, 1.02 g of silver nitrate and

10.2 g of polyvinylpyrrolidone (PVP) were completely dissolved in separate ethylene glycol (EG). PVP solution was

heated up to an appropriate temperature (100–160 °C) in an oil bath. Then the temperature was kept fixed. When it

turned out to be light yellow, silver nitrate solution was then injected slowly into this solution while stirring vigorously.

Then this solution was allowed to be gently stirred for 4 h at fixed temperature. This step results in the formation of

PVP-capped silver nanoparticles. The resulting solution was then dispersed in ethanol. Finally, the dispersed solution

was centrifuged at 9000 rpm for 60 min.

*jaehwan@inha.ac.kr; phone 82-32-874-7325; fax 82-32-832-7325; eapap.com

Nanosensors, Biosensors, and Info-Tech Sensors and Systems 2013, edited by Vijay K. Varadan, Proc. of SPIE Vol. 8691, 86910Q · © 2013 SPIE CCC code: 0277-786X/13/$18 · doi: 10.1117/12.2010095

Proc. of SPIE Vol. 8691 86910Q-1

Downloaded From: http://proceedings.spiedigitallibrary.org/ on 07/21/2013 Terms of Use: http://spiedl.org/terms纤维素活性纸

This washing step was repeated three times and the final residue of silver nanoparticles with size less than 50 nm was

obtained. Then previous research work [12] was followed to synthesize silver ink from silver particles. A very small

amount of viscous hydroxyethyl-cellulose (HEC) solution and diethylene glycol (DEG) were added to the residue of

silver nanoparticles. Here, HEC acts as a viscosifier to increase the viscosity [13] and DEG acts as a surfactant to lower

the surface tension of the solution. Then the solid content ranging of about 45 % was adjusted by adding 50-50%

solution of deionized water and DEG. Finally, the conductive silver ink was achieved by sonicating for 1 h and

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纳米银粒子的制备

纳米银粒子的制备

纳米银粒子的制备

摘要：本文采用液相还原法以硼氢化钠作为还原剂，在十二烷基硫酸钠保护下合成了采用一次还原、二次还原制备不同粒径的纳米银，用傅立叶红外光谱（FTIR）、紫外-可见分光光

度计(UV-vis)、荧光分光度计等对纳米银的进行了表征。结果表明：纳米粒子稳定，且二次

还原粒径明显长大。

关键词：纳米银 化学还原法 二次还原

0 引言 纳米粒子一般指尺寸在1nm至100nm之间的粒子，是处在原子簇和宏观体交界的过渡区域。

从一般的微观和宏观的观点看，这样的系统既非典型的微观系统，亦非典型的宏观系统，是

一种典型的介观系统。它具有一系列新异的物理化学特性，涉及到纳米材料中所忽略或根本

不具有的基本物理化学问题。金属纳米材料是纳米材料的一个重要分支，它以贵金属金、银、

铜为代表，其中因为纳米银具有很高的表面活性、表面能催化性能和电导热性能，以及优良的抗菌杀菌活性，在无机抗菌剂、催化剂材料、电子陶瓷材料、低温导热材料、电导涂料等

领域有广阔的应用前景而得到最多的关注，如在化纤中加入少量纳米银，可以改善化纤制品

的某些性能，并使其具有很强的杀菌能力；在氧化硅薄膜中加加少量的纳米银，可以使得镀

这种薄膜的玻璃有一定的光致发性，用纳米银敷衍料涂烧伤创面及久治不愈的痔疮，可以收

到良好的效果。由于纳米银的诸多应用使它的制备变得尤为重要。目前纳米银的制备方法主要有化学还原法、沉积法、电极法、蒸度法、机械研磨法、辐射化学还原法、激光气相法、

激光烧蚀法、微乳液法等。其中化学还原法因其设备简单、操作方便，节能而成为制备的主

要方法。本研究采用聚乙烯吡咯烷酮(PVP)作保护剂，以抗坏血酸和硼氢化钠为还原剂, 采

用连续还原法制备银纳米粒子。

1 实验部分 1.1 化学试剂及仪器 试剂：硝酸银、抗坏血酸、硼氢化钠、聚乙烯吡咯烷酮（PVP）、无水

乙醇、胶棉液。仪器：88-1型磁力搅拌器、DZG-6020型真空干燥箱、玻璃仪器气流干燥

器、SHB-IIIT型循环水式多用真空泵、WB-200型旋转蒸发仪、DDSJ-308A型电导率仪、

制备含有纳米银粒子的聚乙烯醇水凝胶及纳米银加量对抗菌性能的影响

制备含有纳米银粒子的聚乙烯醇水凝胶及纳米银加量对抗菌性能的影响

制备含有纳米银粒子的聚乙烯醇水凝胶及纳米银加量对抗菌性能的影响

Preparation and Antibacterial Effects of PVA-PVP Hydrogels

Containing Silver Nanoparticles

Haijun Yu,1,2Xiaoyi Xu,1,2Xuesi Chen,1Tiancheng

Lu,1,2Peibiao Zhang,1Xiabin Jing1 1State Key Laboratory of

Polymer Physics and Chemistry,Changchun Institute of Applied

Chemistry, Chinese Academy of

Sciences,Changchun130022,People’s Republic of China

2Graduate School of Chinese Academy of

Sciences,Beijing100039,People’s Republic of China

Received20April2006;accepted14May2006

DOI10.1002/app.24835

Published online in Wiley

InterScience().

ABSTRACT:The poly(vinyl alcohol)/poly(N-vinyl pyr-rolidone)(PVA–PVP)hydrogels containing silver nanopar-ticles

were prepared by repeated freezing–thawing treat-ment.The

silver content in the solid composition was in the range of0.1–1.0wt%,the silver particle size was from 20to100nm,and the

一种纳米银颗粒的制备方法

一种纳米银颗粒的制备方法

一种纳米银颗粒的制备方法

纳米银颗粒的制备方法有很多种，其中一种常见的方法是化学还原法。以下是一个简单的化学还原法制备纳米银颗粒的步骤：

 材料和仪器:

1. 氧化银（Ag2O）或硝酸银（AgNO3）等银盐。

2. 还原剂，如植物提取物、蔗糖、柠檬酸等。

3. 保护剂，如聚乙烯吡咯烷酮（PVP）等。

4. 搅拌器、恒温槽、离心机等基础实验仪器。

 步骤:

1. 溶液制备： 将一定量的氧化银或硝酸银加入适量的溶剂中，形成含有银离子的溶液。

2. 还原反应： 向银盐溶液中逐滴加入还原剂，同时搅拌。还原剂能够将银离子还原成元素银，形成纳米银颗粒。

3. 保护剂的添加： 为了防止纳米银颗粒聚集和沉淀，添加适量的保护剂。保护剂能够包裹在纳米银颗粒表面，防止它们相互结合。

4. 反应控制： 控制还原反应的速度和温度，以控制纳米银颗粒的大小和分布。

5. 搅拌和分离： 在反应完成后，继续搅拌一段时间，然后使用离心机将纳米银颗粒从溶液中分离出来。

6. 洗涤： 用适量的溶剂多次洗涤纳米银颗粒，去除未反应的物质和剩余的还原剂。

7. 干燥： 将洗涤后的纳米银颗粒在适当的条件下干燥，得到纳米银粉末。

请注意，这只是一种制备纳米银颗粒的基本方法，具体的步骤和条件可能因不同的实验目的而有所变化。在进行实验前，请确保熟悉所使用的化学品的性质和安全注意事项。

纳米银的置换反应制备及其表征

纳米银的置换反应制备及其表征

银是人类最早使用的金属之一[1]。纳米银是氧化银组成的粒径在1～100 nm之间、具有高比表面积的颗粒[2]。纳米银颗粒以其独特的光学、电学、热学、磁学性能而著称[3]。气凝胶是在保持凝胶三维网络结构不变的条件下，将其中的液体溶剂除去而形成的一种高度多孔材料[4]，气凝胶具有孔隙率高、密度低等特点[5]，现已应用于绝热材料[6]、催化剂载体[7]和生物传感器[8]等领域。纤维素基气凝胶具有生物可降解的纤维素材料和多孔气凝胶材料两者的优点，成为继无机气凝胶和合成聚合物气凝胶之后的第3代气凝胶[9]。刘真真等人[10]使用旧报纸为原料，制备出纤维素基气凝胶，再通过热分解制备出碳基气凝胶，用于吸附甲醇和硅油，实现了废旧材料的重新利用。

将纳米银负载于纤维素基气凝胶基体中，可减少纳米银本身的聚集性，同时提高纳米银颗粒的回收效率。纤维素基气凝胶具有吸附性能，可用于吸附染料和其他有机物。银本身具有催化还原对硝基苯酚[11]、催化亚甲基蓝的脱色[12]等功能。因此，纳米银/纳米二醛纤维素气凝胶可作为载银催化剂应用于催化反应。现行方法是将气凝胶浸泡在硝酸银溶液中，经临界干燥或冷冻干燥后制备载银气凝胶。如将乙酸纤维素纤维气凝胶浸泡在硝酸银溶液中，可得到载银量为6.89%的载银气凝胶[13]。但该方法制备的气凝胶载银量低，不利于载银气凝胶在催化、导电等领域的应用。使用纳米纤维素作为基材制备载银气凝胶可以增大纳米银的负载面积。同时，对纤维素基材料进行高碘酸盐氧化改性以增加纳米银颗粒原位生成的反应位点，从而提高纤维素基材料的载银量。

本实验使用高碘酸钠将漂白硫酸盐针叶木浆氧化成二醛纤维素，以硝酸银为前驱体制备出纳米银/二醛纤维素复合物，后经高压均质法得到纳米银/纳米二醛纤维素复合物，最终通过冷冻干燥法得到纳米银/纳米二醛纤维素气凝胶。探究了不同氧化时间对纤维素基原料的影响及对载银气凝胶的微观结构和结构组成进行表征。

1 实 验