CN112023944A - 一种原位合成铼与二硫化铼异质结构复合材料的制备方法 - Google Patents
一种原位合成铼与二硫化铼异质结构复合材料的制备方法 Download PDFInfo
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Abstract
本发明涉及一种原位合成铼与二硫化铼异质结构复合材料的制备方法,包括下列步骤:将高铼酸铵、盐酸羟胺和硫脲溶入水中,形成混合溶液;将混合溶液转移至高压釜中,并浸入酸处理过的碳布,置于200‑240℃的温度下,保温一段时间;取出载满样品的碳布,清洗后干燥,得到产物二硫化铼纳米片阵列ReS2/CC;将ReS2/CC在加入了保护气的氢气氛围里,升温至550‑650℃,高温处理一段时间后取出,得到产物Re‑ReS2/CC复合材料。所制备的Re‑ReS2/CC应用于HER电催化剂。
Description
技术领域
本发明属于纳米电催化分解水材料的制备技术领域,具体涉及一种原位合成Re-ReS2复合材料的制备方法。
背景技术
随着人类社会的不断发展,能源的需求量也越来越大,随之带来的是日益严重的环境污染和能源危机问题,因此寻求一种清洁可再生的高效能源成为人类社会发展所面临的一大挑战。氢气作为一种新型能源,因其能量密度高,燃烧产物无污染且可循环利用等优点,一直被认为是传统化石燃料的潜在替代品。在所有的制氢过程中,电催化分解水是一种安全、可持续和环保的策略。在电化学分解水装置中,Pt基催化剂被证明是促进析氢反应(HER)最有效的电催化剂,但金属铂的全球储量非常低、价格昂贵、碱性条件下催化活性低、稳定性差等缺点,严重制约了电解水法制氢技术的发展。因此急需开发低成本、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)纳米材料具有成本低廉、边缘位点催化活性高的特点。其中ReS2具有独特的1T’相已被证明具有优于2H相的导电性与1T相的稳定性,在HER中具有良好的发展前景。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。ReS2虽有较高的析氢活性,但与金属铂相比仍有很大差距,而且在全pH范围实现高效稳定的析氢活性仍是一项挑战。大量文献表明,科研工作者对提高电催化活性的手段主要集中在:(1)提高催化材料的比表面积,使单位面积的活性位点数量增大。(2)金属、非金属元素掺杂对主催化材料进行表面改性,来提高活性位点的本征活性与数量。(3)通过材料复合化,进行界面调控,以实现组分之间的协同效应,提高材料的本征催化活性。其中多相材料复合是一种极有效地提高电催化产氢的手段,通过异质界面调控,加速水分解与吸附氢的活性,从而实现全pH范围高效稳定的电解水反应。
所以,本发明拟用水热加高温还原的方法原位合成Re-ReS2复合材料用于全pH范围电解水制氢。这里我们采用碳布(CC)作为导电集流体,在表面垂直生长出二硫化铼纳米片阵列(ReS2/CC),再用高温还原法原位合成铼与二硫化铼异质结构复合材料(Re-ReS2/CC)。经电化学测试,Re-ReS2/CC在酸性和碱性条件下都具有良好的HER活性,当电流密度为10mA cm-2时,在1M KOH电解液中HER过电势仅为66mV,在0.5M H2SO4电解液中HER过电势为63mV。
发明内容
本发明的目的是在碳布表面原位合成Re-ReS2复合材料用于全pH电催化析氢反应。以高铼酸铵为Re源,碳布为导电集流体,先通过水热反应在碳布上生长出ReS2纳米片阵列,再用高温还原的方法原位合成出Re-ReS2/CC复合材料。此方法制备过程简单,作为电解水产氢催化剂,在全pH范围内具有良好的电化学性能。本发明的技术方案通过以下步骤实现:
一种原位合成铼与二硫化铼异质结构复合材料的制备方法,包括下列步骤:
(1)将高铼酸铵、盐酸羟胺和硫脲按照摩尔比为NH4ReO4:HONH3Cl:CH4N2S=1:(2.5-3.5):(4-5)溶入水中,形成混合溶液。
(2)将混合溶液转移至高压釜中,并浸入酸处理过的碳布,置于200-240℃的温度下,保温一段时间。
(3)取出载满样品的碳布,清洗后干燥,得到产物二硫化铼纳米片阵列ReS2/CC。
(4)将ReS2/CC在加入了保护气的氢气氛围里,升温至550-650℃,高温处理一段时间后取出,得到产物Re-ReS2/CC复合材料。
2.根据权利要求1所述的制备方法,其特征在于,步骤(4)里,高温处理的条件为:通入的混合气体的体积比H2/Ar=20/180,600℃升温速率为5℃/min高温处理2h。
2.权利要求1所制备的Re-ReS2/CC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)本发明利用水热加高温还原的方法原位合成Re-ReS2/CC复合材料,制备工艺简单,耗时短。
(2)本发明利用原位还原的方法,制备出的异质结构改性过渡金属二硫化物同时提高二硫化铼在酸性、碱性条件下的析氢活性,使其成为高效全pH电解水制氢催化剂。
(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Re-ReS2/CC的SEM照片。从该图明显看出Re-ReS2/CC呈现片层状形貌,Re-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Re-ReS2/CC的XRD照片。从该图明显看出物相由Re、ReS2两相组成。
图3为本发明实施例1得到的Re-ReS2/CC在1M KOH条件下的HER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Re-ReS2/CC在0.5M H2SO4条件下的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
实施例1
分别称取161mg高铼酸铵(NH4ReO4)、54.4mg硫脲(CH4N2S)、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,将一片酸处理过的碳布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,在60℃真空干燥箱中干燥12h,制得ReS2/CC。最后,将ReS2/CC置于方舟放入高温管式炉中,用氢气、氩气混合气体(体积比H2/Ar=20/180),600℃升温速率为5℃/min高温处理2h后取出,得到产物Re-ReS2/CC复合材料。
实施例2
分别称取161mg高铼酸铵(NH4ReO4)、54.4mg硫脲(CH4N2S)、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ReS2/CC。最后,将ReS2/CC置于方舟放入高温管式炉中,用氢气、氩气混合气体(体积比H2/Ar=40/160),600℃升温速率为5℃/min高温处理2h后取出,得到产物Re-ReS2/CC复合材料。
实施例3
分别称取161mg高铼酸铵(NH4ReO4)、54.4mg硫脲(CH4N2S)、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ReS2/CC。最后,将ReS2/CC置于方舟放入高温管式炉中,用氢气、氩气混合气体(体积比H2/Ar=20/180),600℃升温速率为3℃/min高温处理2h后取出,得到产物Re-ReS2/CC复合材料。
实施例4
分别称取322mg高铼酸铵(NH4ReO4)、54.4mg硫脲(CH4N2S)、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ReS2/CC。最后,将ReS2/CC置于方舟放入高温管式炉中,用氢气、氩气混合气体(体积比H2/Ar=20/180),500℃升温速率为5℃/min高温处理2h后取出,得到产物Re-ReS2/CC复合材料。
Claims (3)
1.一种原位合成铼与二硫化铼异质结构复合材料的制备方法,包括下列步骤:
(1)将高铼酸铵、盐酸羟胺和硫脲按照摩尔比为NH4ReO4:HONH3Cl:CH4N2S=1:(2.5-3.5):(4-5)溶入水中,形成混合溶液。
(2)将混合溶液转移至高压釜中,并浸入酸处理过的碳布,置于200-240℃的温度下,保温一段时间。
(3)取出载满样品的碳布,清洗后干燥,得到产物二硫化铼纳米片阵列ReS2/CC。
(4)将ReS2/CC在加入了保护气的氢气氛围里,升温至550-650℃,高温处理一段时间后取出,得到产物Re-ReS2/CC复合材料。
2.根据权利要求1所述的制备方法,其特征在于,步骤(4)里,高温处理的条件为:通入的混合气体的体积比H2/Ar=20/180,600℃升温速率为5℃/min高温处理2h。
3.权利要求1所制备的Re-ReS2/CC应用于HER电催化剂。
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