CN108405878A - 一种可控结构的纳米银线负载硫化银材料的制备方法 - Google Patents
一种可控结构的纳米银线负载硫化银材料的制备方法 Download PDFInfo
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Abstract
本发明涉及一种可控结构的纳米银线负载硫化银材料的制备方法。所述材料包括双层结构，内层为光滑、均匀的纳米银线，外层为紧密包裹在纳米银线表面的硫化银，且可以通过改变合成条件控制硫化银的负载形态，可以包括层状和纳米颗粒。所述材料的制备方法包括以下步骤：(1)采用改进的多元醇还原法制备合成纳米银线；(2)在硫化钠溶液中可控制备纳米银线负载硫化银材料。本发明所提供的纳米银线负载硫化银材料具有核壳结构，且可以调控硫化银的负载形态，具有制备工艺简单、容易实施且材料形貌可控等优点。本发明所制备的银纳米银线负载硫化银材料可用于光电子材料和光催化等领域。
Description
技术领域
本发明属于功能纳米材料制备技术领域，具体涉及一种硫化银-银复合结构纳米线的制备方法，并且通过改变合成条件能够制备多级结构的纳米材料。
背景技术
纳米线是在横向尺寸在100纳米以下的一维结构。纳米银线(AgNWs)是一类典型的一维纳米材料，除了具备银优良的导电性能外，还具有优异的透光性和抗弯折性，因此被视为是最有可能替代传统氧化铟锡透明电极的材料。纳米银线具有电阻低、价格便宜等优势，因此能够广泛应用于各种透明导电材料，如柔性太阳能电池、电容屏导电材料等，从而为实现柔性、可弯折LED显示、触摸屏等提供了可能性。
硫化银(Ag2S)是一种化学稳定性良好的无机半导体材料，而且具有较好的光电、热电、光吸收和光催化性能，在光催化、光伏电池、光电导元件、荧光成像、红外检测等领域具有重要的应用前景。硫化银还是典型的电子-离子混合导电型半导体材料，在室温下，它不仅能传导电子，还能传导银离子，使其在光学和电子等领域具有重要的应用价值。
金属-半导体复合材料能够有效地提高光电子利用效率，疏散半导体材料表面的电荷并且有效的阻碍电子与空穴的重组。硫化银纳米颗粒负载在纳米银线材料上能够制备高效太阳能电池光，毒性低，所制备的硫化银-纳米银线复合材料是一种绿色且环境友好的电子器件，同时由于硫化银具有合适的禁带宽度，获得了优异的电池光电性能，制备的电池具有优异的光伏性能，因此金属-半导体复合材料硫化银/银这类纳米材料得到广泛的关注。
目前，国内外文献已经报道了球壳结构Ag2S/Ag纳米颗粒的制备、性质和应用(“Synthesis，Morphological Control，and Antibacterial Properties of Hollow/Solid Ag2S/Ag Heterodimers”，J.Am.Chem.Soc.，2010，132，10771-10785)。但是硫化银的溶解度非常低(Ksp＝6.31×10-50)，所以硫化银的形成速率通常过快，这会导致其形貌比较难控制，特别是负载在纳米银线上形成纳米结构的硫化银。因此有必要开发一些温和而又方便的通用方法来制备纳米银线负载硫化银材料。
发明内容
本发明的目的就是为了克服上述现有技术存在的缺陷而提供一种简单制备纳米银线负载硫化银材料的方法，并且可以调控硫化银在纳米银线表面的形貌。
一种纳米银线负载硫化银材料，包括两层结构，内层为光滑、均匀的纳米银线，外层为紧密包裹在纳米银线表面的硫化银纳米颗粒或者薄层。
本发明的目的可以通过以下技术方案来实现：
(1)合成纳米银线，采用改进的多元醇还原法制备：
(1-1)氯化钠(NaCl)和聚乙烯吡咯烷酮(PVP)充分溶解于乙二醇(EG)中，得到PVP/NaCl/EG混合溶液；
(1-2)硝酸银(AgNO3)充分溶解于乙二醇(EG)，得到AgNO3/EG混合溶液；
(1-3)将PVP/NaCl/EG溶液逐滴加入AgNO3/EG混合溶液中，并放在油浴锅里继续加热搅拌；
(1-4)产物分别用丙酮、去离子水分别清洗。
(2)制备纳米银线负载硫化银材料：
(2-1)将先前合成出的纳米银线加入到一定浓度的硫化钠溶液中搅拌；
(2-2)光照或者避光进行反应；
(2-3)产物用乙醇、去离子水分别清洗。
步骤(1-1)中，氯化钠的乙二醇溶液质量浓度为0.06-0.2mg/mL；
步骤(1-1)中，聚乙烯吡咯烷酮的乙二醇溶液质量浓度为0.06-0.2g/mL；
步骤(1-2)中，硝酸银的乙二醇溶液质量浓度为6-20mg/mL；
步骤(1-3)中，反应温度为120-180℃；
步骤(1-4)中，先用丙酮清洗3次，再用去离子水清洗3次。
步骤(2-1)中，采用0.02-0.5mM的硫化钠溶液，纳米银线在硫化钠溶液的浓度0.04-1mM；
步骤(2-2)中，反应在室温下进行4-48小时；
步骤(2-3)中，先用乙醇清洗3次，再用去离子水清洗3次。
与目前现有技术相比，本发明利用两步法合成了纳米银线负载硫化银材料的方法，并且可以调控硫化银在纳米银线表面的形貌。制备得到的纳米银线负载硫化银材料尺寸均匀，具有一维纳米结构，构建了一个新颖高效的光电化学传感器平台。纳米银线内层可以快速的转移电子，表面的硫化银纳米结构可以有效的阻碍电子与空穴的重组，拓宽了电极对可见光的吸收范围，提高光电流转化效率。此外，本申请所得的纳米银线负载硫化银还可以用于喷墨打印或喷涂等方式，用于大规模制备对电极。
附图说明
图1为实施例1制备的纳米银线负载硫化银材料的X射线衍射谱图；
图2为实施例1制备的纳米银线负载硫化银材料的透射电子显微镜照片；
图3为实施例2制备的纳米银线负载硫化银材料的X射线衍射谱图；
图4为实施例2制备的纳米银线负载硫化银材料的透射电子显微镜照片；
具体实施方式
以下结合实例对本发明进行进一步的详述。
实施例1
(1)分别称取一定质量的氯化钠和聚乙烯吡咯烷酮，充分溶解于乙二醇中，得到PVP/NaCl/EG混合溶液。氯化钠的乙二醇溶液质量浓度为0.06-0.1mg/mL；聚乙烯吡咯烷酮的乙二醇溶液质量浓度为0.06-0.1g/mL。
(2)称取一定质量硝酸银充分溶解于乙二醇(EG)，得到AgNO3/EG混合溶液。硝酸银的乙二醇溶液质量浓度为6-12mg/mL。
(3)将PVP/NaCl/EG溶液逐滴加入AgNO3/EG混合溶液中，并放在油浴锅里继续加热搅拌，反应温度为120-160℃。
(4)先用丙酮清洗3次，再用去离子水清洗3次。
(5)将一定量的纳米银线加入到10mL一定浓度的硫化钠溶液中在避光条件下搅拌反应24h；
(6)产物先用乙醇清洗3次，再用去离子水清洗3次，最终得到纳米银线负载硫化银材料。
实例1所得的纳米银线负载硫化银材料的X射线衍射谱图如图1。从图中可以看出，所得到的材料含有纳米银线和硫化银，证实了合成反应确实成功制备了纳米银线负载硫化银材料。制备所得材料的透射电子显微镜照片如图2，材料的形貌仍为一维纳米线结构，形貌均匀，直径约为40nm，硫化银以层状形态成功负载在纳米银线表面。
实施例2
(1)分别称取一定质量的氯化钠和聚乙烯吡咯烷酮，充分溶解于乙二醇中，得到PVP/NaCl/EG混合溶液。氯化钠的乙二醇溶液质量浓度为0.1-0.2mg/mL；聚乙烯吡咯烷酮的乙二醇溶液质量浓度为0.1-0.2g/mL。
(2)称取一定质量硝酸银充分溶解于乙二醇(EG)，得到AgNO3/EG混合溶液。硝酸银的乙二醇溶液质量浓度为10-20mg/mL。
(3)将PVP/NaCl/EG溶液逐滴加入AgNO3/EG混合溶液中，并放在油浴锅里继续加热搅拌，反应温度为140-180℃。
(4)先用丙酮清洗3次，再用去离子水清洗3次。
(5)将一定量的纳米银线加入到10mL一定浓度的硫化钠溶液中在500W氙灯照射条件下搅拌反应12h；
(6)产物先用乙醇清洗3次，再用去离子水清洗3次，最终得到纳米银线负载硫化银材料。
实例2所得的纳米银线负载硫化银材料的X射线衍射谱图如图3。从图中可以看出，所得到的材料含有纳米银线和硫化银，证实了合成反应确实成功制备了纳米银线负载硫化银材料。制备所得材料的透射电子显微镜照片如图4，材料的主体形貌仍为一维纳米线结构，形貌均匀，直径约为40nm，但是表面产生了球状颗粒，说明光照条件下硫化银能够以纳米颗粒负载在纳米银线表面。
实施例3
(1)分别称取一定质量的氯化钠和聚乙烯吡咯烷酮，充分溶解于乙二醇中，得到PVP/NaCl/EG混合溶液。氯化钠的乙二醇溶液质量浓度为0.1-0.2mg/mL；聚乙烯吡咯烷酮的乙二醇溶液质量浓度为0.1-0.2g/mL。
(2)称取一定质量硝酸银充分溶解于乙二醇(EG)，得到AgNO3/EG混合溶液。硝酸银的乙二醇溶液质量浓度为10-20mg/mL。
(3)将PVP/NaCl/EG溶液逐滴加入AgNO3/EG混合溶液中，并放在油浴锅里继续加热搅拌，反应温度为130-160℃。
(4)先用丙酮清洗3次，再用去离子水清洗3次。
(5)将一定量的纳米银线加入到10mL一定浓度的硫化钾溶液中在紫外灯照射条件下搅拌反应8h；
(6)产物先用乙醇清洗3次，再用去离子水清洗3次，最终得到纳米银线负载硫化银材料。
Claims (5)
1.一种可控结构的纳米银线负载硫化银材料的制备方法，其特征在于，所述纳米银线负载硫化银材料包括双层结构，内层为光滑、均匀的纳米银线，外层为紧密包裹在纳米银线表面的硫化银，且可以通过改变合成条件控制硫化银的负载形态，可以包括层状和纳米颗粒；具体包括以下步骤：
(1)采用多元醇还原法制备合成纳米银线，包括：
(1-1)将氯化钠(NaCl)和聚乙烯吡咯烷酮(PVP)充分溶解于乙二醇(EG)中，得到PVP/NaCl/EG混合溶液，
(1-2)硝酸银(AgNO3)充分溶解于乙二醇(EG)，得到AgNO3/EG混合溶液，
(1-3)将PVP/NaCl/EG溶液逐滴加入AgNO3/EG混合溶液中，并放在油浴锅里继续加热搅拌，
(1-4)产物先用丙酮清洗3次，再用去离子水清洗3次；
(2)制备纳米银线负载硫化银材料：
(2-1)将先前合成的纳米银线加入到一定浓度的硫化钠溶液中搅拌，
(2-2)产物先用丙酮清洗3次，再用去离子水清洗3次。
2.如权利要求1所述纳米银线负载硫化银材料的制备方法，其特征在于，步骤(1)中，在合成纳米银线过程中，氯化钠的乙二醇溶液质量浓度为0.06-0.2mg/mL，聚乙烯吡咯烷酮的乙二醇溶液质量浓度为0.06-0.2g/mL，硝酸银的乙二醇溶液质量浓度为6-20mg/mL，反应温度为120-180℃。
3.如权利要求1所述纳米银线负载硫化银材料的制备方法，其特征在于，步骤(2)中，将先前合成的纳米银线加入到硫化钠溶液中，硫化钠浓度为0.02-0.5mM，纳米银线的浓度是0.04-1mM，反应时间是4-48小时。
4.如权利要求1所述纳米银线负载硫化银材料的制备方法，其特征在于，步骤(2)中，将先前合成的纳米银线加入到硫化钠溶液中，硫化钠也可以是硫化钾、硫化铵、硫氢化钠等可溶性硫化物。
5.如权利要求1所述纳米银线负载硫化银材料的制备方法，其特征在于，步骤(2)中，将先前合成的纳米银线加入到硫化钠溶液中，通过光照或者避光条件控制纳米银线上硫化银的负载形态，包括层状和纳米颗粒，光照可以采用氙灯、紫外灯等光源。
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109248693A (zh) * | 2018-10-25 | 2019-01-22 | 中南大学 | 一种改性硫化锌纳米线光催化材料及其制备方法 |
| CN110752066A (zh) * | 2019-11-25 | 2020-02-04 | 四川浩宇华东科技有限公司 | 基于银类纳米线的高透屏蔽薄膜的制备方法 |
| CN114373569A (zh) * | 2022-01-26 | 2022-04-19 | 苏州诺菲纳米科技有限公司 | 一种纳米银线柔性膜黑化处理方法 |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102009172A (zh) * | 2010-09-27 | 2011-04-13 | 山东大学 | 一种Ag/Ag2S核/壳纳米结构电阻开关材料及其制备方法 |
| CN102744417A (zh) * | 2011-06-16 | 2012-10-24 | 浙江科创新材料科技有限公司 | 一种高长径比纳米银线的制备方法 |
| KR20140012298A (ko) * | 2012-07-19 | 2014-02-03 | 한국과학기술원 | 핵-껍질 나노구조체의 조성 변화를 통한 표면 플라즈몬 공명의 다양한 색 구현 방법 |
| CN104828773A (zh) * | 2015-03-28 | 2015-08-12 | 安徽师范大学 | 一种聚吡咯/银@硫化银核壳结构纳米线及其用途和制备方法 |
| CN104889388A (zh) * | 2015-05-18 | 2015-09-09 | 华东理工大学 | 一种核壳结构银@硫化银纳米线的制备方法 |
| CN107159881A (zh) * | 2017-06-12 | 2017-09-15 | 青岛科技大学 | 一种银@硫化银核壳结构光热转换纳米材料 |
-
2018
- 2018-03-30 CN CN201810276133.XA patent/CN108405878B/zh active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102009172A (zh) * | 2010-09-27 | 2011-04-13 | 山东大学 | 一种Ag/Ag2S核/壳纳米结构电阻开关材料及其制备方法 |
| CN102744417A (zh) * | 2011-06-16 | 2012-10-24 | 浙江科创新材料科技有限公司 | 一种高长径比纳米银线的制备方法 |
| KR20140012298A (ko) * | 2012-07-19 | 2014-02-03 | 한국과학기술원 | 핵-껍질 나노구조체의 조성 변화를 통한 표면 플라즈몬 공명의 다양한 색 구현 방법 |
| CN104828773A (zh) * | 2015-03-28 | 2015-08-12 | 安徽师范大学 | 一种聚吡咯/银@硫化银核壳结构纳米线及其用途和制备方法 |
| CN104889388A (zh) * | 2015-05-18 | 2015-09-09 | 华东理工大学 | 一种核壳结构银@硫化银纳米线的制备方法 |
| CN107159881A (zh) * | 2017-06-12 | 2017-09-15 | 青岛科技大学 | 一种银@硫化银核壳结构光热转换纳米材料 |
Non-Patent Citations (2)
| Title |
|---|
| ZHANG,YINQING等: "Impacts of Morphology, Natural Organic Matter, Cations, and Ionic Strength on Sulfidation of Silver Nanowires", 《ENVIRONMENTAL SCIENCE & TECHNOLOGY》 * |
| 丁瑞强等: "一种链状多面体银-硫化银复合纳米结构的制备", 《现代化工》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109248693A (zh) * | 2018-10-25 | 2019-01-22 | 中南大学 | 一种改性硫化锌纳米线光催化材料及其制备方法 |
| CN110752066A (zh) * | 2019-11-25 | 2020-02-04 | 四川浩宇华东科技有限公司 | 基于银类纳米线的高透屏蔽薄膜的制备方法 |
| CN110752066B (zh) * | 2019-11-25 | 2020-10-02 | 四川浩宇华东科技有限公司 | 基于银类纳米线的高透屏蔽薄膜的制备方法 |
| CN114373569A (zh) * | 2022-01-26 | 2022-04-19 | 苏州诺菲纳米科技有限公司 | 一种纳米银线柔性膜黑化处理方法 |
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