CN101614929B - 一种银、金纳米颗粒分散四氧化三钴光学薄膜及制备方法 - Google Patents

一种银、金纳米颗粒分散四氧化三钴光学薄膜及制备方法 Download PDF

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CN101614929B
CN101614929B CN2009100896831A CN200910089683A CN101614929B CN 101614929 B CN101614929 B CN 101614929B CN 2009100896831 A CN2009100896831 A CN 2009100896831A CN 200910089683 A CN200910089683 A CN 200910089683A CN 101614929 B CN101614929 B CN 101614929B
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CN101614929A (zh
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张波萍
王士京
赵翠华
张美霞
李顺
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University of Science and Technology Beijing USTB
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Abstract

一种银、金纳米颗粒分散四氧化三钴光学薄膜及制备方法,属于金属纳米颗粒与氧化物复合材料领域。本发明提供一种银、金单质金属纳米颗粒分散氧化物非线性光学薄膜,其特征是化学成分组成通式为AgxAuy/(Co3O4)1-x-y,其中x、y分别表示Ag、Au组成元素的摩尔分数,x的取值范围为0.01~0.6,y的取值范围为0.01~0.6,x+y的取值范围为0.02~0.8。纳米银、金颗粒以金属单质的形式分散于四氧化三钴基体中,银、金颗粒直径均为1~100nm,薄膜在350~450nm和550~650nm两个波段观察到吸收峰,增加了光吸收范围,具有优良的非线性光学特性。

Description

一种银、金纳米颗粒分散四氧化三钴光学薄膜及制备方法
技术领域
本发明属于金属纳米颗粒与氧化物复合材料领域,特别是提出了一种银、金纳米颗粒分散四氧化三钴光学薄膜及制备方法,涉及到多种金属纳米颗粒分散氧化物光学薄膜的设计与制备工艺。
背景技术
近几十年来,金属纳米颗粒非线性光学复合薄膜的研究发展迅速,在光电子工业中如光开关、光通讯、光信息处理、光计算机、激光技术等都需要以非线性光学材料为基础材料,金属纳米颗粒非线性光学复合薄膜具有非常广阔的应用前景。现在对此类薄膜的研究已由一元体系金属纳米颗粒非线性光学复合薄膜为主扩展到二元体系金属纳米颗粒非线性光学薄膜。但是所报道的二元体系金属纳米颗粒复合薄膜中,金属颗粒大多数以合金的形式存在,以单质形式存在的报道还比较少见。作为新的非线性材料的候选者,过渡金属氧化物由于电子关联效应,在理论上具有大的光学非线性。与其它制备薄膜的方法相比,溶胶-凝胶法可在不同介质基体中分散多种金属、能够精确控制薄膜的化学计量比,并且还具有制备周期短、操作方便、成本低等优点。采用溶胶-凝胶法制备以单质形式存在的Au、Ag二元金属颗粒分散四氧化三钴光学薄膜还未见报道。
发明内容
一种银、金纳米颗粒分散四氧化三钴光学薄膜及制备方法,其薄膜化学成分组成通式为AgxAuy/(Co3O4)1-x-y,其中x、y分别表示Ag、Au组成元素的摩尔分数,x的取值范围为0.01~0.6,y的取值范围为0.01~0.6,x+y的取值范围为0.02~0.8。本发明采用溶胶-凝胶法制备AgxAuy/(Co3O4)1-x-y复合薄膜,纳米银、金颗粒以金属单质的形式分散于四氧化三钴基体中,银、金颗粒直径均为1~100nm,薄膜在350~450nm和550~650nm两个波段观察到吸收峰。
本发明技术的主要特点是:在所制备的薄膜中,银、金颗粒分别以金属单质的形式分散于氧化物基体中,复合薄膜在光吸收图谱中分别出现了银、金两个较强的等离子共振吸收峰,光吸收图谱如图1所示,增加了光非线性吸收的范围,具有优良的非线性光学性质。
附图说明
图1为本发明设计的一种AgxAuy/(Co3O4)1-x-y复合薄膜的光吸收图谱。
具体实施方式:
实施例1
称取0.8731g的硝酸钴(Co(NO3)2·6H2O),0.1699g的硝酸银(AgNO3)和0.4188g的氯金酸(HAuCl4·4H2O),分别加入到10ml乙二醇独甲醚溶剂中,在磁力搅拌机上搅拌3小时,陈化6小时,得到浓度为0.3mol/L的Co母体溶液、0.1mol/L的Ag母体溶液和0.1mol/L的Au母体溶液;然后量取9.8ml的Co母体溶液和0.2ml的Ag母体溶液,将两种溶液混合,再在磁力搅拌机上搅拌5小时,陈化8小时,制得Ag0.02/(Co3O4)0.98前驱体溶液。用同样的方法,量取9.8ml的Co母体溶液和0.2ml的Au母体溶液,制备Au0.02/(Co3O4)0.98前驱体溶液。匀胶之前,将基片依次在蒸馏水、乙醇、丙酮中超声清洗,然后将其放入干燥箱中烘干,干燥后涂覆一层已配制好的Ag0.02/(Co3O4)0.98前驱体溶液于基片上。匀胶时,先以300rpm的速度运转3秒,再以3000rpm的速度运转10秒,匀胶后进行一次热分解处理,热分解温度为300℃,时间为30秒,涂膜结束后,将样品置于热处理炉中进行退火,退火温度580℃,退火保温时间30分钟。然后按上述步骤再涂覆一层Au0.02/(Co3O4)0.98前驱体溶液于上述基片上,进行相同的匀胶,热分解和退火处理,最后得到Ag0.01Au0.01/(Co3O4)0.98复合光学薄膜。
实施例2
称取0.8731g的硝酸钴(Co(NO3)2·6H2O),0.1699g的硝酸银(AgNO3)和0.4188g的氯金酸(HAuCl4·4H2O),分别加入到10ml乙二醇独甲醚溶剂中,在磁力搅拌机上搅拌3小时,陈化6小时,得到浓度为0.3mol/L的Co母体溶液、0.1mol/L的Ag母体溶液和0.1mol/L的Au母体溶液;然后量取6ml的Co母体溶液和4ml的Ag母体溶液,将两种溶液混合,再在磁力搅拌机上搅拌5小时,陈化8小时,制得Ag0.4/(Co3O4)0.6前驱体溶液。用同样的方法,量取6ml的Co母体溶液和4ml的Au母体溶液,制备Au0.4/(Co3O4)0.6前驱体溶液。匀胶之前,将基片依次在蒸馏水、乙醇、丙酮中超声清洗,然后将其放入干燥箱中烘干,干燥后涂覆一层已配制好的Ag0.4/(Co3O4)0.6前驱体溶液于基片上。匀胶时,先以300rpm的速度运转3秒,再以3000rpm的速度运转10秒,匀胶后进行一次热分解处理,热分解温度为300℃,时间为30秒,涂膜结束后,将样品置于热处理炉中进行退火,退火温度580℃,退火保温时间30分钟。然后按上述步骤再涂覆一层Au0.4/(Co3O4)0.6前驱体溶液于上述基片上,进行相同的匀胶,热分解和退火处理,最后得到Ag0.2Au0.2/(Co3O4)0.6复合光学薄膜。
实施例3
称取0.8731g的硝酸钴(Co(NO3)2·6H2O),0.1699g的硝酸银(AgNO3)和0.4188g的氯金酸(HAuCl4·4H2O),分别加入到10ml乙二醇独甲醚溶剂中,在磁力搅拌机上搅拌3小时,陈化6小时,得到浓度为0.3mol/L的Co母体溶液、0.1mol/L的Ag母体溶液和0.1mol/L的Au母体溶液;然后量取1ml的Co母体溶液和9ml的Ag母体溶液,将两种溶液混合,再在磁力搅拌机上搅拌5小时,陈化8小时,制得Ag0.9/(Co3O4)0.1前驱体溶液。用同样的方法,量取4ml的Co母体溶液和6ml的Au母体溶液,制备Au0.6/(Co3O4)0.4前驱体溶液。匀胶之前,将基片依次在蒸馏水、乙醇、丙酮中超声清洗,然后将其放入干燥箱中烘干,干燥后涂覆一层已配制好的Ag0.9/(Co3O4)0.1前驱体溶液于基片上。匀胶时,先以300rpm的速度运转3秒,再以3000rpm的速度运转10秒,匀胶后进行一次热分解处理,热分解温度为300℃,时间为30秒,涂膜结束后,将样品置于热处理炉中进行退火,退火温度580℃,退火保温时间30分钟。一层膜制备完成后按上述步骤再涂覆一层Au0.6/(Co3O4)0.4前驱体溶液于上述基片上,进行相同的匀胶,热分解和退火处理。然后再按相同步骤涂覆一层Ag0.9/(Co3O4)0.1膜,最后得到Ag0.6Au0.2/(Co3O4)0.2复合光学薄膜。
实施例4
称取0.8731g的硝酸钴(Co(NO3)2·6H2O),0.1699g的硝酸银(AgNO3)和0.4188g的氯金酸(HAuCl4·4H2O),分别加入到10ml乙二醇独甲醚溶剂中,在磁力搅拌机上搅拌3小时,陈化6小时,得到浓度为0.3mol/L的Co母体溶液、0.1mol/L的Ag母体溶液和0.1mol/L的Au母体溶液;然后量取1ml的Co母体溶液和9ml的Au母体溶液,将两种溶液混合,再在磁力搅拌机上搅拌5小时,陈化8小时,制得Au0.9/(Co3O4)0.1前驱体溶液。用同样的方法,量取4ml的Co母体溶液和6ml的Ag母体溶液,制备Ag0.6/(Co3O4)0.4前驱体溶液。匀胶之前,将基片依次在蒸馏水、乙醇、丙酮中超声清洗,然后将其放入干燥箱中烘干,干燥后涂覆一层已配制好的Au0.9/(Co3O4)0.1前驱体溶液于基片上。匀胶时,先以300rpm的速度运转3秒,再以3000rpm的速度运转10秒,匀胶后进行一次热分解处理,热分解温度为300℃,时间为30秒,涂膜结束后,将样品置于热处理炉中进行退火,退火温度580℃,退火保温时间30分钟。一层膜制备完成后按上述步骤再涂覆一层Ag0.6/(Co3O4)0.4前驱体溶液于上述基片上,进行相同的匀胶,热分解和退火处理。然后再按相同步骤涂覆一层Au0.9/(Co3O4)0.1膜,最后得到Ag0.2Au0.6/(Co3O4)0.2复合光学薄膜。

Claims (1)

1.一种银、金纳米颗粒分散四氧化三钴光学薄膜的制备方法,其特征是化学成分组成通式为AgxAuy/(Co3O4)1-x-y,其中x、y分别表示Ag、Au组成元素的摩尔分数,x的取值范围为0.01~0.6,y的取值范围为0.01~0.6,x+y的取值范围为0.02~0.8;以硝酸钴,硝酸银、氯金酸和乙二醇独甲醚为原料,采用溶胶-凝胶法合成化学计量比准确、成分均匀的前躯体溶液,然后采用匀胶机在玻璃基片上进行涂膜,经过退火处理最后得到AgxAuy/(Co3O4)1-x-y复合薄膜;复合薄膜中银、金颗粒分别以金属单质的形式分散于四氧化三钴基体中,直径分布均在1~100nm范围内,薄膜在350~450nm和550~650nm两个波段观察到吸收峰。
CN2009100896831A 2009-07-28 2009-07-28 一种银、金纳米颗粒分散四氧化三钴光学薄膜及制备方法 Expired - Fee Related CN101614929B (zh)

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