CN111321394A - 一种气相沉积制备纳米片状磷化钴的方法 - Google Patents

一种气相沉积制备纳米片状磷化钴的方法 Download PDF

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CN111321394A
CN111321394A CN202010130123.2A CN202010130123A CN111321394A CN 111321394 A CN111321394 A CN 111321394A CN 202010130123 A CN202010130123 A CN 202010130123A CN 111321394 A CN111321394 A CN 111321394A
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陈道理
杨绪勇
委福祥
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Xuyi Xinyuan Optical Science Technology Co ltd
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Abstract

本发明提供一种气相沉积制备纳米片状磷化钴的方法，包括以下步骤：步骤(1).将钴源与2‑甲基咪唑按照摩尔比1:8称量，将钴源与溶剂按1摩尔钴对应20毫升溶剂进行配比形成溶液A；将称量好的2‑甲基咪唑溶于同样体积的溶剂中形成溶液B；将B倒入A中，在室温下静置12‑24h；步骤(2).离心清洗后，真空干燥不少于12h，即获得前驱体；步骤(3).将上述前驱体同磷源按照摩尔比1:5称量，一起置于通保护气的管式炉中；步骤(4).使管式炉在气氛保护条件下按照升温曲线进行升温过程，再在300℃～500℃下反应2～5h，冷却至室温即得纳米片状磷化钴。本发明其结构稳定，排列有序，有利于后续合成加工；原料为钴的硝酸盐、氯化盐、或乙酸盐，原料价格低廉。

Description

一种气相沉积制备纳米片状磷化钴的方法
技术领域
本发明涉及纳米片状磷化钴制备技术领域，具体为一种气相沉积制备纳米片状磷化钴的方法。
背景技术
磷化钴具有良好的金属性质和良好的导电性，在许多领域得到了广泛的研究，如作为电催化剂用于水的裂解，作为负极材料用于锂离子电池，作为催化剂用于加氢脱硫反应等。目前国内所合成的磷化钴其形貌大多是纳米球、纳米线及纳米球等。如中国专利CN201910027895.0公开了一种氮掺杂的磷化钴/纳米碳复合材料及其制备方法和应用，其特点是将磷源、钴源、合成凝胶的单体在聚合助剂下聚合,得到双网络水凝胶；双网络水凝胶经冷冻干燥处理,得到干凝胶；干凝胶在保护性气氛、750-1000℃下煅烧；将煅烧产物与纳米碳材料复合得到磷化钴/纳米碳复合材料。中国专利201811655267.9公开了一种磷化钴纳米线电解水产氢催化剂及其制备方法，其特点是在反应釜中加入硫酸钴尿素、水以及乙二醇中充分溶解；将反应釜加热至130-170℃,进行水热反应,得到磷化钴前驱体；待反应釜自然冷却至常温后,加入氨水和乙二醇、三氧化钼；将反应釜加热至110-135℃,直至得到固态磷化钴；将得到的固态磷化钴置于500-600℃的环境内煅烧2-3小时,得到成品。上诉专利均存在反应温度过高，且在电化学应用中，产物磷化钴的形貌不利于电解质进入电极材料内部，离子扩散距离过长等缺点，不利于在实际应用中达到节约产能，增加产率的目的。
发明内容
本发明所解决的技术问题在于提供一种气相沉积制备纳米片状磷化钴的方法，以解决上述背景技术中提出的问题。
本发明所解决的技术问题采用以下技术方案来实现：一种气相沉积制备纳米片状磷化钴的方法，包括以下步骤：
步骤(1).将钴源与2-甲基咪唑按照摩尔比1:8称量，将钴源与溶剂按1摩尔钴对应20毫升溶剂进行配比形成溶液A；
将称量好的2-甲基咪唑溶于同样体积的溶剂中形成溶液B；
将B倒入A中，搅拌后形成均一溶液，在室温下静置12-24h；
步骤(2).离心清洗后，真空干燥不少于12h，即获得前驱体；通过液相沉积在室温下静置制备出了片状前驱体纳米阵列，其结构稳定，排列有序，有利于后续合成加工；
步骤(3).将上述前驱体同磷源按照摩尔比1:5称量一起置于通保护气的管式炉中，磷源置于管式炉上游，前驱体置于下游；
步骤(4).设置升温曲线，使管式炉在气氛保护条件下按照升温曲线进行升温过程，再在300℃～500℃下反应2～5h，蒸发的磷元素在前驱体表面发生气相沉积反应，片状前驱体转化为片状的磷化钴，冷却至室温即得纳米片状磷化钴。
进一步地，所述步骤(1)中钴源为钴的硝酸盐、氯化盐、乙酸盐中至少一种。
进一步地，所述步骤(1)中溶剂为去离子水，甲醇中至少一种。
进一步地，所述步骤(3)中磷源为磷单质。
进一步地，所述步骤(4)中保护气体为氩气，氮气中至少一种。
进一步地，所述步骤(4)中升温速度为(3-6)℃/分钟。
与现有技术相比，本发明的有益效果是：
1、本发明通过液相沉积在室温下静置制备出了片状前驱体纳米阵列，其结构稳定，排列有序，有利于后续合成加工；原料为钴的硝酸盐、氯化盐、或乙酸盐，原料价格低廉。
2、本发明制备出的纳米片状磷化钴形貌结构稳定，有序排列的纳米阵列使得电解液容易进入电极内部，片状结构大大缩短了离子扩散长度，有利于增强法拉第氧化还原反应。
3、本发明的制备方法，工序段，易于操作，反应温度相对较低，适合工业化生产以及新能源储能如超级电容器、燃料电池等领域的应用。
附图说明
图1为本发明的纳米片状磷化钴的扫描电镜图。
具体实施方式
实施例1
一种气相沉积制备纳米片状磷化钴的方法，包括以下步骤：
步骤(1).将钴源与2-甲基咪唑按照摩尔比1:8称量，将钴源与溶剂按1摩尔钴对应20毫升溶剂进行配比形成溶液A；
将称量好的2-甲基咪唑溶于同样体积的溶剂中形成溶液B；
将B倒入A中，搅拌后形成均一溶液，在室温下静置12-24h；钴源为钴的氯化盐；溶剂为去离子水。
步骤(2).离心清洗后，真空干燥不少于12h，即获得前驱体；通过液相沉积在室温下静置制备出了片状前驱体纳米阵列，其结构稳定，排列有序，有利于后续合成加工。
步骤(3).将上述前驱体同磷源按照摩尔比1:5称量一起置于通保护气的管式炉中，磷源置于管式炉上游，前驱体置于下游；磷源为磷单质。
步骤(4).设置升温曲线，使管式炉在气氛保护条件下按照升温曲线进行升温过程，再在400℃下反应4h，蒸发的磷元素在前驱体表面发生气相沉积反应，片状前驱体转化为片状的磷化钴，冷却至室温即得纳米片状磷化钴；保护气体为氮气；升温速度为3℃/分钟。
实施例2
一种气相沉积制备纳米片状磷化钴的方法，包括以下步骤：
步骤(1).将钴源与2-甲基咪唑按照摩尔比1:8称量，将钴源与溶剂按1摩尔钴对应20毫升溶剂进行配比形成溶液A；
将称量好的2-甲基咪唑溶于同样体积的溶剂中形成溶液B；
将B倒入A中，搅拌后形成均一溶液，在室温下静置12-24h；钴源为钴的乙酸盐；溶剂为甲醇。
步骤(2).离心清洗后，真空干燥不少于12h，即获得前驱体；通过液相沉积在室温下静置制备出了片状前驱体纳米阵列，其结构稳定，排列有序，有利于后续合成加工。
步骤(3).将上述前驱体同磷源按照摩尔比1:5称量一起置于通保护气的管式炉中，磷源置于管式炉上游，前驱体置于下游；磷源为磷单质。
步骤(4).设置升温曲线，使管式炉在气氛保护条件下按照升温曲线进行升温过程，再在300℃下反应2h，蒸发的磷元素在前驱体表面发生气相沉积反应，片状前驱体转化为片状的磷化钴，冷却至室温即得纳米片状磷化钴；保护气体为氮气；升温速度为5℃/分钟。
实施例3
一种气相沉积制备纳米片状磷化钴的方法，包括以下步骤：
步骤(1).将钴源与2-甲基咪唑按照摩尔比1:8称量，将钴源与溶剂按1摩尔钴对应20毫升溶剂进行配比形成溶液A；
将称量好的2-甲基咪唑溶于同样体积的溶剂中形成溶液B；
将B倒入A中，搅拌后形成均一溶液，在室温下静置12-24h；钴源为钴的硝酸盐；溶剂为去离子水。
步骤(2).离心清洗后，真空干燥不少于12h，即获得前驱体；通过液相沉积在室温下静置制备出了片状前驱体纳米阵列，其结构稳定，排列有序，有利于后续合成加工。
步骤(3).将上述前驱体同磷源按照摩尔比1:5称量一起置于通保护气的管式炉中，磷源置于管式炉上游，前驱体置于下游；磷源为磷单质。
步骤(4).设置升温曲线，使管式炉在气氛保护条件下按照升温曲线进行升温过程，再在500℃下反应5h，蒸发的磷元素在前驱体表面发生气相沉积反应，片状前驱体转化为片状的磷化钴，冷却至室温即得纳米片状磷化钴；保护气体为氩气，升温速度为6℃/分钟。
以上显示和描述了本发明的基本原理和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，这些变化和改进都落入要求保护的本发明范围内。本发明的要求保护范围由所附的权利要求书及其等效物界定。

Claims (6)

1.一种气相沉积制备纳米片状磷化钴的方法，其特征在于：包括以下步骤：
步骤(1).将钴源与2-甲基咪唑按照摩尔比1:8称量，将钴源与溶剂按1摩尔钴对应20毫升溶剂进行配比形成溶液A；
将称量好的2-甲基咪唑溶于同样体积的溶剂中形成溶液B；
将B倒入A中，搅拌后形成均一溶液，在室温下静置12-24h；
步骤(2).离心清洗后，真空干燥不少于12h，即获得前驱体；通过液相沉积在室温下静置制备出了片状前驱体纳米阵列，其结构稳定，排列有序，有利于后续合成加工；
步骤(3).将上述前驱体同磷源按照摩尔比1:5称量一起置于通保护气的管式炉中，磷源置于管式炉上游，前驱体置于下游；
步骤(4).设置升温曲线，使管式炉在气氛保护条件下按照升温曲线进行升温过程，再在300℃～500℃下反应2～5h，蒸发的磷元素在前驱体表面发生气相沉积反应，片状前驱体转化为片状的磷化钴，冷却至室温即得纳米片状磷化钴。
2.根据权利要求1所述的一种气相沉积制备纳米片状磷化钴的方法，其特征在于：所述步骤(1)中钴源为钴的硝酸盐、氯化盐、乙酸盐中至少一种。
3.根据权利要求1所述的一种气相沉积制备纳米片状磷化钴的方法，其特征在于：所述步骤(1)中溶剂为去离子水，甲醇中至少一种。
4.根据权利要求1所述的一种气相沉积制备纳米片状磷化钴的方法，其特征在于：所述步骤(3)中磷源为磷单质。
5.根据权利要求1所述的一种气相沉积制备纳米片状磷化钴的方法，其特征在于：所述步骤(4)中保护气体为氩气，氮气中至少一种。
6.根据权利要求1所述的一种气相沉积制备纳米片状磷化钴的方法，其特征在于：所述步骤(4)中升温速度为(3-6)℃/分钟。
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