CN110508292A - 用于电催化全解水的金属掺杂二硫化铼纳米片阵列的制备方法 - Google Patents
用于电催化全解水的金属掺杂二硫化铼纳米片阵列的制备方法 Download PDFInfo
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Abstract
本发明涉及一种用于电催化全解水的金属掺杂二硫化铼纳米片阵列的制备方法，包括下列步骤：将六水合硝酸盐、高铼酸铵、盐酸羟胺和硫脲，溶入去离子水，形成混合溶液；将上述混合溶液转移到高压釜中，将一片酸处理过的碳布浸入混合溶液中，置于200‑230℃的烘箱中，保温一段时间。将高压釜自然冷却至室温，取出载满样品的碳布，清洗干净后干燥处理，得到产物金属掺杂二硫化铼纳米片阵列M‑ReS2/CC。所述的方法制备的M‑ReS2/CC应用于HER电催化剂。
Description
技术领域
本发明属于电催化技术领域，具体涉及一种金属掺杂改性二硫化铼纳米片阵列的制备方法。
背景技术
氢是理想的清洁能源载体，电催化分解水是一种低成本且清洁的获取氢能源的方式。电催化分解水包括阴极析氢反应(HER)和阳极析氧反应(OER)两个半反应，然而析氢和析氧反应的过电位较高，因此必须要有高效、稳定的电催化剂才能实现。目前用于电催化剂仍存在价格昂贵、功能单一、催化活性低、稳定性差等缺点，严重制约了电解水法制氢技术的发展，故急需开发低成本、双功能、高活性、高稳定性的材料来解决这一问题。
二维层状过渡金属二硫化物(TMDs)纳米材料的发现，具有成本低廉、边缘位点催化活性高的特点，高度不对称的1T’相TMDs材料—ReS2已被研究者证明具有优于1T相和2H相导电性和稳定性的特点。ReS2独特的弱耦合作用不仅能够促进电解质离子在层间的扩散，而且能够暴露出更多的边缘位置和基准面，作为活性中心来达到最佳的电催化性能。现阶段对ReS2电催化剂的研究集中于HER反应，没有研究OER反应相关的工作，这是因为过渡金属二硫化物对OER反应的中间产物吸附能力太低。通过查阅文献发现，Ni、Fe基OER催化剂是现阶段有望替代贵金属催化剂的潜在候选者之一，掺杂过渡金属元素所引起固有缺陷可以促进中间产物在催化剂表面的吸附。因此我们提出利用过渡金属元素掺杂的方法引入缺陷，调控ReS2的电子结构以及中间产物在催化剂表面的吸附作用，使其在碱性条件下具有良好的电催化OER性能，制备出性能优异的电催化双功能全解水催化剂。
发明内容
本发明的目的是提供一种用于电催化全解水的金属掺杂二硫化铼纳米片阵列的制备方法，在碳布表面直接生长出金属掺杂二硫化铼的纳米片阵列，并将其用于电催化全解水反应。该材料为金属(M＝Fe、Co、Ni、Mn、Cu、Zn)掺杂ReS2纳米片阵列生长在碳布上，制备过程简单，作为双功能全解水电催化剂，具有良好的电化学性能。本发明采用的方法具有良好的普适性，适用于大多数过渡金属，制备工艺简单，耗时短，并可提高二硫化铼的电催化性能。本发明的技术方案如下：
一种用于电催化全解水的金属掺杂二硫化铼纳米片阵列的制备方法，包括下列步骤：
(1).将六水合硝酸盐、高铼酸铵、盐酸羟胺和硫脲，按照摩尔比为(1～5):10:30:45的配比溶入去离子水，形成混合溶液。
(2).将上述混合溶液转移到高压釜中，将一片酸处理过的碳布浸入混合溶液中，置于200-230℃的烘箱中，保温一段时间。
(3).将高压釜自然冷却至室温，取出载满样品的碳布，清洗干净后干燥处理，得到产物金属掺杂二硫化铼纳米片阵列M-ReS2/CC。
所述的六水合硝酸盐为六水合硝酸镍、六水合硝酸钴、六水合硝酸铁、六水合硝酸锰、六水合硝酸铜或硝酸锌中的一种或混合物。
所述的方法制备的M-ReS2/CC可应用于HER电催化剂。
与现有的技术相比，本发明的优点在于：
(1).本发明利用一步水热的方法在碳布表面直接生长出金属元素掺杂二硫化铼纳米片阵列。该方法具有良好的普适性，适用于大多数过渡金属，制备工艺简单，耗时短。
(2).本发明利用金属元素掺杂的方法改性过渡金属二硫化物，同时提高二硫化铼析氢、析氧反应活性，使其成为高效的双功能全解水电催化剂。
(3).产物原位生长在碳布表面，制备出的自支撑结构可直接作为电极进行电催化反应，无需添加价格高昂的粘结剂涂覆在玻碳电极表面，制备工艺简单，降低成本，暴露出更多的活性位点，提高电催化活性。
附图说明
图1为本发明实施例1得到的Ni-ReS2/CC的SEM照片。从该图明显看出Ni-ReS2/CC呈现片层状形貌，Ni-ReS2纳米片定向垂直生长在碳布表面。
图2为本发明实施例1得到的Ni-ReS2/CC的XRD照片。从该图明显看出在掺杂Ni后仍然是ReS2物相。
图3为本发明实施例1得到的Ni-ReS2/CC的OER性能图。从该图明显看出电催化剂良好的电催化性能。
图4为本发明实施例1得到的Ni-ReS2/CC的HER性能图。从该图明显看出电催化剂良好的电催化性能。
本发明未述及之处适用于现有技术。
以下给出本发明制备方法的具体实施例。这些实施例仅用于详细说明本发明制备方法，并不限制本申请权利要求的保护范围。
具体实施方式
本发明用一步水热的方法制备出过渡金属掺杂二硫化铼纳米片高效双功能全解水电催化剂。这里我们采用碳布(CC)作为导电集流体，硝酸盐作为金属源，在表面垂直生长出金属(M)掺杂的二硫化铼纳米片阵列(M-ReS2/CC)，其中M可为Fe、Co、Ni、Mn、Cu、Zn。经电化学测试，Ni-ReS2/CC具极好的HER和OER活性，在1M KOH电解液中电流密度为10mAcm-2时HER过电势为110mV，OER过电势为210mV。
实施例1
分别称取161mg高铼酸铵(NH4ReO4)、54.4mg硫脲(CH4N2S)、35mg六水合硝酸镍(Ni(NO3)2·6H2O)，125mg盐酸羟胺(HONH3Cl)，溶于20mL去离子水中搅拌30min。将上述溶液转移到50ml聚四氟乙烯内衬不锈钢高压釜中，将CC(WOS109型1.5cm*2cm)垂直放入混合溶液中，在200℃下反应24h。反应后高压釜自然冷却至室温，取出载满样品的CC，用去离子水和乙醇反复洗涤，最后在60℃真空干燥箱中干燥12h，制得Ni-ReS2/CC。
实施例2
分别称取161mg高铼酸铵(NH4ReO4)、54.4mg硫脲(CH4N2S)、30mg六水合硝酸钴(Co(NO3)2·6H2O)，125mg盐酸羟胺(HONH3Cl)，溶于20mL去离子水中搅拌30min。将上述溶液转移到50ml聚四氟乙烯内衬不锈钢高压釜中，将CC(WOS109型1.5cm*2cm)垂直放入混合溶液中，在220℃下反应24h。反应后高压釜自然冷却至室温，取出载满样品的CC，用去离子水和乙醇反复洗涤，最后在60℃真空干燥箱中干燥12h，制得Co-ReS2/CC。
实施例3
分别称取161mg高铼酸铵(NH4ReO4)、54.4mg硫脲(CH4N2S)、28mg三水合硝酸铜(Cu(NO3)2·3H2O)，125mg盐酸羟胺(HONH3Cl)，溶于20mL去离子水中搅拌30min。将上述溶液转移到50ml聚四氟乙烯内衬不锈钢高压釜中，将CC(WOS109型1.5cm*2cm)垂直放入混合溶液中，在200℃下反应21h。反应后高压釜自然冷却至室温，取出载满样品的CC，用去离子水和乙醇反复洗涤，最后在60℃真空干燥箱中干燥12h，制得Cu-ReS2/CC。
实施例4
分别称取322mg高铼酸铵(NH4ReO4)、54.4mg硫脲(CH4N2S)、40mg六水合硝酸锌(Zn(NO3)2·6H2O)，125mg盐酸羟胺(HONH3Cl)，溶于20mL去离子水中搅拌30min。将上述溶液转移到50ml聚四氟乙烯内衬不锈钢高压釜中，将CC(WOS109型1.5cm*2cm)垂直放入混合溶液中，在220℃下反应21h。反应后高压釜自然冷却至室温，取出载满样品的CC，用去离子水和乙醇反复洗涤，最后在60℃真空干燥箱中干燥12h，制得Zn-ReS2/CC。
Claims (3)
1.一种用于电催化全解水的金属掺杂二硫化铼纳米片阵列的制备方法，包括下列步骤：
(1).将六水合硝酸盐、高铼酸铵、盐酸羟胺和硫脲，按照摩尔比为(1～5):10:30:45的配比溶入去离子水，形成混合溶液。
(2).将上述混合溶液转移到高压釜中，将一片酸处理过的碳布浸入混合溶液中，置于200-230℃的烘箱中，保温一段时间。
(3).将高压釜自然冷却至室温，取出载满样品的碳布，清洗干净后干燥处理，得到产物金属掺杂二硫化铼纳米片阵列M-ReS2/CC。
2.根据权利要求1所述的方法，其特征在于，所述的六水合硝酸盐为六水合硝酸镍、六水合硝酸钴、六水合硝酸铁、六水合硝酸锰、六水合硝酸铜或硝酸锌中的一种或混合物。
3.权利要求1所述的方法制备的M-ReS2/CC应用于HER电催化剂。
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