CN108479771A - Au/TiO2复合纳米颗粒及异质结的液相合成方法 - Google Patents
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Abstract
本发明公开了一种Au/TiO2复合纳米颗粒及异质结的液相合成方法,利用光幅照,对分散在甲醛溶液中的TiO2纳米颗粒进行表面无序化非晶重构处理,并在非晶化处理过的TiO2纳米颗粒表面利用静电吸附[Au(OH)4]‑基团;在液相水热条件下实现原位的Au还原,得到非晶过渡Au/TiO2复合颗粒;高压水热二次晶化合成Au/TiO2复合纳米颗粒。本发明不仅能实现Au纳米颗粒与TiO2纳米颗粒的界面有效耦合,制备出复合Au/TiO2纳米颗粒,而且能根据实际应用的需要,方便地控制Au颗粒的大小。
Description
本申请是申请号:201610317837.8、申请日:2016-05-16、名称“非物理吸附Au/TiO2复合纳米颗粒及异质结的液相合成方法”的分案申请。
技术领域
本发明涉及一种贵金属Au/TiO2复合纳米颗粒的制备,尤其是涉及Au和TiO2界面形成非物理吸附晶格结构重构过渡区复合纳米颗粒的制备。
背景技术
TiO2纳米粉体和纳米膜材料在太阳能的存储与利用、光电转换、光致变色及光催化降解大气和水中的污染物等方面具有广泛的应用,为了提高其光催化活性和可见光的利用率,在TiO2颗粒表面进行贵金属修饰,比如金(Au)是常见的手段。从理论上分析,有效的贵金属修饰可改变TiO2能带的带尾,将TiO2的光响应从紫外区域扩展到可见光范围;并在Au和TiO2的界面形成异质结构,促进光生电子和空穴的空间分离,增强光催化活性;且在某些频率区域发生表面等离子共振耦合(SPP),使该频率区域的三维光场耦合成准二维的SPP光场,从而进一步提高对自然光的利用率。然而,由于Au和TiO2的晶格并不匹配,溶胶----凝胶(sol-jel)法和共沉淀法等方法合成的Au/TiO2复合颗粒,Au在TiO2的界面大多以物理吸附状态存在,这种复合粒子界面的连接其实是脆弱的,Au和TiO2容易分离而成为二相混合物。更为严重的是,由于Au和TiO2界面之间是松散的物理吸附,光幅照下纳米TiO2颗粒的光生电子受到单质Au纳米颗粒表面的表面势垒的作用,光生电子难以迁移至Au纳米颗粒,不能实现光生电子和空穴的空间分离而增强光催化活性;在这种情况下,尽管SPP光场耦合仍然可以存在,但强的光场密度并不能和光生电子-空穴的空间分离相联系,其对最终的催化活性的影响难以估计。因此,如何改变TiO2的表面晶格结构以实现Au纳米颗粒的有效修饰是拓展纳米TiO2应用的重要技术。
发明内容
本发明的目的在于提供一种能实现Au纳米颗粒与TiO2纳米颗粒的界面有效耦合,制备出复合Au/TiO2纳米颗粒的非物理吸附Au/TiO2复合纳米颗粒及异质结的液相合成方法。
本发明的技术解决方案是:
一种非物理吸附Au/TiO2复合纳米颗粒及异质结的液相合成方法,其特征是:包括下列步骤:
(1)利用光幅照,对分散在甲醛溶液中的TiO2纳米颗粒进行表面无序化非晶重构处理,并在非晶化处理过的TiO2纳米颗粒表面利用静电吸附[Au(OH)4]-基团;
(2)在液相水热条件下实现原位的Au还原,得到非晶过渡Au/TiO2复合颗粒;
(3)高压水热二次晶化合成Au/TiO2复合纳米颗粒。
在步骤(3)后还进行子晶生长调控Au颗粒尺寸。
目前,溶胶---凝胶法和共沉淀法等方法合成的Au/TiO2复合颗粒的工艺,没有对Au和TiO2的晶格失配进行有效的处理,Au和TiO2其实是脆弱的物理吸附,并且Au的尺寸大小难以调控,Au颗粒在Au/TiO2复合体系中随机分布,存在Au颗粒的偏聚等现象,造成复合颗粒的光生电子-空穴难以有效分离而影响光催化活性和光利用效率。本发明利用非晶化预处理及二次重结晶方法,可制备出强耦合的Au/TiO2复合颗粒,Au颗粒与TiO2颗粒紧密关连,且Au颗粒分布均匀无偏聚,粒径可根据需要通过子晶生长进行调控,以达到不同频率SPP耦合(表面等离子共振)及增强催化等要求。
依据本发明制备的复合Au/TiO2纳米粒子,Au颗粒与TiO2颗粒紧密相连,存在晶格之间的过渡关系,在超声处理下不会解体,是一种非物理吸附的连接关系;Au颗粒粒径连续可控,可根据需要调节粒子的大小,实现不同频率的SPP耦合;复合Au/TiO2纳米颗粒无非晶过渡的紧密结合有利于光生电子从TiO2纳米粒子向Au颗粒的有效传输,增大光电流响应、提升光催化和抗腐蚀性能。
附图说明
下面结合附图和实施例对本发明作进一步说明。
图1是富(001)面的TiO2纳米颗粒的XRD衍射图,其中的插图是颗粒的TEM图。
图2是重构处理过的TiO2纳米颗粒的高分辨TEM图。其中b是方框区域的细节放大图。
图3是Au/TiO2复合纳米颗粒的高分辨TEM图。
图4是Au/TiO2复合纳米颗粒和TiO2纳米颗粒的光电响应比较示意图。
具体实施方式
一种非物理吸附Au/TiO2复合纳米颗粒及异质结的液相合成方法,包括下列步骤:
一、有复合粒子的制备包括如下连续的过程:
1、0.2克富(001)面的TiO2纳米颗粒分散于50ml浓度为37%甲醛溶液中,超声分散30分钟形成稳定的胶体。
2、将超声分散好的TiO2甲醛胶体放置于350W紫外灯的正下方,液面距紫外灯0.5米,紫外辐照2小时,离心分离,并用无水乙醇和去离子水反复清洗。
3、将清洗好的TiO2分散于去离子水中,用硝酸调节PH值至1~1.5,剧烈搅拌并缓慢滴加氯金酸配置混合溶液,(氯金酸水溶液质量浓度为1%,并用NaOH调节PH值至10~11)当混合溶液的PH值至3~3.5时停止加入氯金酸,高速离心分离得到吸附[Au(OH)4]-的TiO2纳米颗粒。
4、将上述处理得到的TiO2纳米再次分散在浓度为37%的HCHO溶液中,70℃水热处理1小时,高速离心分离并用无水乙醇和去离子水洗涤,得到非晶过渡Au/TiO2复合颗粒。
5、将4中的复合粒子装入水热反应釜,180℃水热处理16小时,取出沉淀物并在80℃干燥,得到TiO2二次结晶的Au/ TiO2复合颗粒。
二、子晶生长调控Au颗粒尺寸
Au颗粒尺寸的控制可在上述Au/TiO2复合颗粒的基础上采用二次生长模式进行,典型步骤如下:
1、将0.2克Au/TiO2复合颗粒分散于50ml去离子水中,加入质量浓度为1%用NaOH调节PH值至10~11的氯金酸水溶液10ml混合均匀。
2、向上述溶液中加入37%的HCHO溶液10ml,避光于75℃水热处理1小时,实现在上述Au/TiO2复合颗粒Au位二次生长的Au,高速离心分离并用无水乙醇和去离子水洗涤得到沉淀物。
3、将2中的颗粒装入水热反应釜,150℃水热处理16小时,取出沉淀物并在80℃干燥,得到晶化完整的Au/TiO2复合颗粒,TiO2颗粒上的Au颗粒的典型尺寸会从5nm±2nm增大至10nm±2nm。
4、调节1中的氯金酸水溶液的添加量,可得到不同增大程度的Au/ TiO2复合颗粒。
Claims (1)
1.一种Au/TiO2复合纳米颗粒及异质结的液相合成方法,其特征是:包括下列步骤:
(1)利用光辐照,对分散在甲醛溶液中的TiO2纳米颗粒进行表面无序化非晶重构处理,并在非晶化处理过的TiO2纳米颗粒表面利用静电吸附[Au(OH)4]-;
(2)在液相水热条件下实现原位的Au还原,得到非晶过渡Au/TiO2复合颗粒;
(3)高压水热二次晶化合成Au/TiO2复合纳米颗粒;
步骤(1)的具体方法:
将超声分散好的TiO2甲醛胶体放置于350W紫外灯的正下方,液面距紫外灯0.5米,紫外辐照2小时,离心分离,并用无水乙醇和去离子水反复清洗;
将清洗好的TiO2分散于去离子水中,用硝酸调节pH值至1~1.5,剧烈搅拌并缓慢滴加氯金酸配置混合溶液,氯金酸水溶液质量浓度为1%,并用NaOH调节pH值至10~11;当混合溶液的pH值至3~3.5时停止加入氯金酸,高速离心分离得到吸附[Au(OH)4]-的TiO2纳米颗粒;
步骤(2)的具体方法:将经步骤(1)处理得到的TiO2纳米颗粒再次分散在浓度为37%的HCHO溶液中,70℃水热处理1小时,高速离心分离并用无水乙醇和去离子水洗涤,得到非晶过渡Au/TiO2复合颗粒;
步骤(3)的具体方法:将步骤(2)得到的非晶过渡Au/TiO2复合颗粒装入水热反应釜,180℃水热处理16小时,取出沉淀物并在80℃干燥,得到TiO2二次结晶的Au/ TiO2复合颗粒;
在步骤(3)后还进行子晶生长调控Au颗粒尺寸;步骤如下:
(1)将0.2克Au/TiO2复合颗粒分散于50ml去离子水中,加入质量浓度为1%用NaOH调节PH值至10~11的氯金酸水溶液10ml混合均匀;
(2)向上述溶液中加入37%的HCHO溶液10ml,避光于75℃水热处理1小时,实现在上述Au/TiO2复合颗粒Au位二次生长的Au,高速离心分离并用无水乙醇和去离子水洗涤得到沉淀物;
(3)将2中的颗粒装入水热反应釜,150℃水热处理16小时,取出沉淀物并在80℃干燥,得到晶化完整的Au/TiO2复合颗粒,TiO2颗粒上的Au颗粒的典型尺寸会从5nm±2nm增大至10nm±2nm;
(4)调节1中的氯金酸水溶液的添加量,可得到不同增大程度的Au/ TiO2复合颗粒。
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