CN114029505A - 一种激光烧蚀制备金属单原子的方法 - Google Patents
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- 239000002184 metal Substances 0.000 title claims abstract description 42
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- 238000000034 method Methods 0.000 title claims abstract description 18
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
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Abstract
一种激光烧蚀制备金属单原子的方法,1)将金属前驱体盐与配体溶解在溶剂中,然后滴涂至基底上干燥;2)将步骤1)中的基底转移至容器中,在液相环境下激光处理;所涉及的激光处理参数为功率密度为105~109W/cm2,激光波长范围涵盖紫外、可见和红外光;在步骤1)中所涉及的金属单原子包括铂、金、钯、铱、钌、铑、铯、铜、铬、锡、铁、钴、镍、锌、锰、钒、钽、钨、铼、锇、铪、铟、铷、锶;各元素的前驱体盐包括氯化盐、硫酸盐、磷酸盐、硝酸盐。本发明反应条件温和,快速高效且环保无污染。本发明技术可以实现单一金属单原子以及多元金属单原子在任何材质基底上的担载。
Description
技术领域
本发明涉及单原子的制备技术,尤其是一种基于激光烧蚀技术制备单一或多元金属单原子的方法。
背景技术
金属单原子是指以单原子的形式均匀分布在载体上,原子利用率达到100%的新型催化材料。因其独特的几何结构和电子构型,金属单原作为催化活性中心,可以实现催化反应的高活性和高选择性。然而,与普通催化剂相比,单原子催化的发展仍然处在刚起步萌芽阶段,尤其是目前的制备方法仍旧存在单原子负载量低、稳定性差等缺陷,极大限制了金属单原子催化剂在催化反应方面的应用。基于上述问题,本发明开发了一种简单的激光烧蚀技术,在常温常压条件下可以实现金属单原子在基底上的高载量担载。目前未见有激光烧蚀制备金属单原子的方法的公开。
发明内容
本发明所要解决的技术问题是,提供一种激光烧蚀制备金属单原子的方法。该方法操作简单,成本低廉,反应条件温和,快速高效且环保无污染。
为了实现上述目的,本发明通过如下技术方案实现,一种激光烧蚀制备金属单原子的方法,包括以下步骤:(1)将金属前驱体盐与配体溶解在溶剂中,然后滴涂至基底上干燥;(2)将步骤(1)中的基底转移至容器(烧杯)中,在液相环境下激光处理;所涉及的激光处理参数为功率密度为105~109W/cm2,激光波长范围涵盖紫外、可见和红外光;
在步骤(1)中所涉及的金属单原子包括铂、金、钯、铱、钌、铑、铯、铜、铬、锡、铁、钴、镍、锌、锰、钒、钽、钨、铼、锇、铪、铟、铷、锶;各元素的前驱体盐包括氯化盐、硫酸盐、磷酸盐、硝酸盐溶剂包括但不限于乙醇、甲醇、水、丙酮、异丙醇、二硫化碳等。
配体包括但不限于乙二胺四乙酸,乙二胺四乙酸钠,邻菲罗啉,二硫代氨基甲酸盐,壳聚糖等。
基底包括但不限于碳基底、金属基底、有机材料基底以及无机材料基底等。
更进一步地,在步骤(2)中所涉及的液相环境包括但不限于各类烷烃、乙醇、水、甲醇等。
激光包括但不限于纳秒激光以及飞秒激光。
激光处理参数为功率密度105~109W/cm2,脉冲激光更好,脉冲频率1Hz-80kHz。激光波长涵盖紫外、可见和近红外光。
有益效果:本发明方法包括负载前驱体的基底及激光器。将基底转移至烧杯中,在液相环境下激光烧蚀并超声,从而实现前驱体盐转变为单原子。本发明操作简单,成本低廉,反应条件温和,快速高效且环保无污染。本发明技术可以实现单一金属单原子以及多元金属单原子在任何材质基底上的担载。本发明大幅度简化了目前合成金属单原子的繁琐步骤,实现了简单温和环境下高载量单原子的合成。本发明技术可以实现单一金属单原子以及多元金属单原子在任何材质基底上的担载。
附图说明
图1A为本发明涉及的由具体实施例1中所合成Pt单原子在BP2000载体上的球差电镜图(比例尺:40nm);图1B,1C分别为C元素以及Pt元素在图1A中BP2000载体上的分布图(比例尺:40nm)。
图2A,2B为本发明涉及的由具体实施例2中所合成的Cu单原子在XC-72R载体上的球差电镜图(比例尺:5nm);
图2C为Cu元素在图1B中XC-72R载体上的分散(比例尺:5nm,摘要附图)。
图3A为本发明涉及的由具体实施例3中在TiO2面合成的的多种金属单原子担载的球差电镜图;图3B、3C、3D、3E、3F、3G、3H分别为Ti,O,Pt,Ir,Cu,Ni,W金属单原子在TiO2表面的分布图。
具体实施方式
下面将通过结合附图和具体实施例对本发明做进一步的具体描述,但不能理解为是对本发明保护范围的限定。
实施例1
本发明提供了一种激光烧蚀制备金属单原子的方法,包括如下步骤:
(1)将0.01mol/L浓度的氯铂酸溶解在1ml乙醇中,加入0.04mol/L的乙二胺四乙酸钠1ml水溶液,然后以0.1ml/mg的剂量将混合溶液与BP2000碳载体粉末混合,并加热使溶剂蒸干。
(2)将步骤(1)中的BP2000转移至盛有己烷的烧杯中,利用脉宽为5ns的纳秒脉冲激光烧蚀担载前驱体的BP2000载体,激光平均功率密度设置为2×105W/cm2,频率为30kHz,激光波长属于红外波段。
从图1电镜图可知,由实施例1合成的铂金属单原子分散在BP2000表面。
实施例2
实施例2与实施例1的区别在于,包括以下步骤:
(1)将0.01mol/L浓度的氯化铜溶解在1ml乙醇中,加入0.04mol/L的邻非罗琳1ml乙醇溶液,然后以0.1ml/mg的剂量将混合溶液与XC-72R粉末混合,并加热使溶剂蒸干。
(2)将步骤(1)中的XC-72R粉末转移至盛有己烷的烧杯中,利用脉宽为5ns的纳秒脉冲激光烧蚀担载前驱体的XC-72R载体,激光平均功率密度设置为2×105W/cm2,频率为20kHz,激光波长属于红外波段。
从图2电镜图可知,由实施例2合成的铜金属单原子分散在XC-72R表面。
实施例3
实施例3与实施例1、2的区别在于,包括以下步骤:
(1)将氯铂酸、氯铱酸、氯化铜、氯化镍、氯化钨以各金属元素为0.01mol/L的浓度均匀溶解在乙醇中,然后以0.1ml/mg的剂量将混合溶液与TiO2载体粉末混合,并加热使溶剂蒸干。
(2)将步骤(1)中的碳载体转移至盛有己烷的烧杯中,利用脉宽为5ns的纳秒脉冲激光烧蚀TiO2载体粉末,激光平均功率密度设置为2×105W/cm2,频率为20kHz。
从图3电镜图可知,实施例3合成的各金属单原子均匀分布在TiO2表面,铂、铱、铜、镍、钨等元素均匀分散在TiO2表面。
以上显示和描述了本发明的基本原理、主要特征和本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,本发明要求保护范围由所附的权利要求书、说明书及其等效物界定。
Claims (8)
1.一种激光烧蚀制备金属单原子的方法,其特征在于,包括以下步骤:
(1)将金属前驱体盐与配体溶解在溶剂中,然后滴涂至基底上干燥;
(2)将步骤(1)中的基底转移至容器中,在液相环境下激光处理;所涉及的激光处理参数为功率密度为105~109W/cm2,激光波长范围涵盖紫外、可见和红外光;
在步骤(1)中所涉及的金属单原子包括铂、金、钯、铱、钌、铑、铯、铜、铬、锡、铁、钴、镍、锌、锰、钒、钽、钨、铼、锇、铪、铟、铷、锶;各元素的前驱体盐包括氯化盐、硫酸盐、磷酸盐、硝酸盐。
2.根据权利要求1所述的激光烧蚀制备金属单原子的方法,其特征在于:可以实现单一金属单原子或多元金属单原子在基底上的担载。
3.根据权利要求1所述的激光烧蚀制备金属单原子的方法,其特征在于:在步骤(1)中所涉及的溶剂包括但不限于乙醇、甲醇、水、丙酮、异丙醇等。
4.根据权利要求1所述的激光烧蚀制备金属单原子的方法,其特征在于:在步骤(1)中所涉及的配体包括但不限于乙二胺四乙酸,乙二胺四乙酸钠,邻菲罗啉,二硫代氨基甲酸盐,壳聚糖。
5.根据权利要求1所述的激光烧蚀制备金属单原子的方法,其特征在于:在步骤(1)中所涉及的基底包括但不限于碳基底、金属基底、有机材料基底以及无机材料基底等。
6.根据权利要求1所述的激光烧蚀制备金属单原子的方法,其特征在于:在步骤(2)中所涉及的液相环境包括但不限于各类烷烃、乙醇、水、甲醇。
7.根据权利要求1-6之一所述的激光烧蚀制备金属单原子的方法,其特征在于:在液相环境下激光处理时,施加超声。
8.根据权利要求1-6之一所述的激光烧蚀制备金属单原子的方法,其特征在于:采用脉冲激光方式,激光脉冲频率1Hz-80kH。
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