CN112237928B - 一种析氢电催化剂铁硫及其制备方法 - Google Patents
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- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 19
- 239000001257 hydrogen Substances 0.000 title claims abstract description 19
- 239000010411 electrocatalyst Substances 0.000 title claims abstract description 18
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 title claims abstract description 15
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
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- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
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- 239000002243 precursor Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
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- 238000007789 sealing Methods 0.000 claims description 4
- 229940048181 sodium sulfide nonahydrate Drugs 0.000 claims description 4
- WMDLZMCDBSJMTM-UHFFFAOYSA-M sodium;sulfanide;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Na+].[SH-] WMDLZMCDBSJMTM-UHFFFAOYSA-M 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
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- 238000005464 sample preparation method Methods 0.000 description 1
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- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001075 voltammogram Methods 0.000 description 1
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Abstract
本发明公开了一种析氢电催化剂铁硫的制备方法，该方法为：称取原料和配置悬浊液；水热反应；微波水热法处理。本发明还公开一种析氢电催化剂铁硫，其采用如上所述的方法制备而成。
Description
技术领域
本发明涉及一种制备析氢电催化剂铁硫的方法及该方法制备的化合物。
背景技术
近年来，随着环境污染的加剧和石油资源的枯竭，绿色可持续能源的开发成为当今世界的一个热门话题。通过电催化的方法获得氢气是一种高效的方式。其中贵金属的催化剂由于成本昂贵，严重影响其发展。而价格便宜且地球储量丰富的电催化剂备受关注。因此，开发不含贵金属、地球储量丰富、廉价的、铁和硫的化学配比为1：1铁硫析氢电催化剂是一个有效的解决途径。
评价电催化制氢性能的一个重要指标就是过电位。过电位越低，在电催化制氢过程中所需要消耗的电能就越少，制氢的性能越好。因此，如何降低析氢电催化剂的过电位也是一个关键问题。
发明内容
本发明的目的在于提供一种析氢电催化剂铁硫的制备方法，该制备方法能使析氢电催化剂铁硫获得较小的过电位。
本发明的实现包括以下步骤：将九水硫化钠和铁粉按摩尔比1：1的比例称取，原料的总量为0.1摩尔，将称量好的原料放置在烧杯中，将35毫升的去离子水加入烧杯内，用玻璃棒搅拌10分钟后，在超声清洗器中超声20分钟；将烧杯中混合物转移到反应釜的内衬中，并将反应釜密封，在140摄氏度反应6天；将所得到的样品离心清洗三次，在冷冻干燥机中干燥后得到前驱体；将200毫克的前驱体置于100毫升的烧杯中，加入35毫升的二甲基亚砜，12毫升的乙二胺和12毫升的乙醇，混合均匀，将混合溶液转移至微波水热反应仪中，微波频率设置为2450兆赫兹，调节微波水热反应仪在120摄氏度反应10分钟，离心清洗后得到析氢电催化剂铁硫。
与现有技术相比，本发明所述的样品制备方法具有以下的优点：能够获得具有更低过电位的铁硫电催化剂。
附图说明
图1为按照对比例和实施例的方法制备的铁硫的XRD图谱。
图2为按照对比例和实施例的方法制备的铁硫的过电位曲线图。
具体实施方式
下面通过具体实施例对本发明做出进一步的具体说明，但本发明并不局限于下述实例。
实施例：将九水硫化钠和铁粉按摩尔比1：1的比例称取，原料的总量为0.1摩尔，将称量好的原料放置在烧杯中，将35毫升的去离子水加入烧杯内，用玻璃棒搅拌10分钟后，在超声清洗器中超声20分钟；将烧杯中混合物转移到反应釜的内衬中，并将反应釜密封，在140摄氏度反应6天；将所得到的样品离心清洗三次，在冷冻干燥机中干燥后得到前驱体；将200毫克的前驱体置于100毫升的烧杯中，加入35毫升的二甲基亚砜，12毫升的乙二胺和12毫升的乙醇，混合均匀，将混合溶液转移至微波水热反应仪中，微波频率设置为2450兆赫兹，调节微波水热反应仪在120摄氏度反应10分钟，离心清洗后得到铁硫电催化剂。
为了说明本实施例的技术效果，按照以下步骤制备样品作为本实施例的对比例：将九水硫化钠和铁粉按摩尔比1：1的比例称取，原料的总量为0.1摩尔，将称量好的原料放置在烧杯中；将35毫升的去离子水加入烧杯内，用玻璃棒搅拌10分钟后，在超声清洗器中超声20分钟；将烧杯中混合物转移到反应釜的内衬中，并将反应釜密封，在140摄氏度反应6天；将所得到的样品离心清洗三次，在冷冻干燥机中干燥后得到样品。
通过X射线衍射的方法对按照实施例和对比例的方法制备的样品进行结构的表征，如图1所示。图1中的实线表示按照对比例的方法制备的样品的X射线图谱，虚线表示按照实施例的方法制备的样品的X射线图谱，竖线表示的是标准的FeS样品X射线衍射峰的位置。标准FeS样品的空间群为P4/nmm，晶格常数为a = 3.6802(5) Å，c = 5.0307(7) Å，α=90°，β= 90°，γ= 90°。通过与标准的FeS样品X射线衍射峰的对比，可以看到，按照对比例的方法制备的样品不含其他物相，是纯净的FeS样品。通过与标准的FeS样品X射线衍射峰的对比，按照实施例的方法制备的样品的衍射峰与标准的FeS衍射峰一一对应起来，表明按照实施例的方法制备的样品是FeS纯相。
采用样品的线性扫描伏安曲线对样品的电催化性能进行对比，如图2所示。图2中方形数据点表示对比例样品的数据，圆形数据点表示实施例样品的数据。按照对比例的方法制备的样品的在-10 mA/cm2的电流密度下的过电位是561 mV,明显高于按照实施例的方法制备的样品的过电位313 mV。
本发明还公开了一种析氢电催化剂铁硫，其采用如实施例所述的方法制备而成。
需要声明的是，以上所述的仅是本发明的优选实施方式，本发明不限于以上实施例。可以理解，本领域技术人员在不脱离本发明的基本构思的前提下直接导出或联想到的其他改进和变化，均应认为包含在本发明的保护范围之内。
Claims (3)
1.一种制备析氢电催化剂铁硫的方法，包括如下步骤：将九水硫化钠和铁粉按摩尔比1：1的比例称取，原料的总量为0.1摩尔，将称量好的原料放置在烧杯中，将35毫升的去离子水加入烧杯内，用玻璃棒搅拌10分钟后，在超声清洗器中超声20分钟；将烧杯中混合物转移到反应釜的内衬中，并将反应釜密封，在140摄氏度反应6天；将所得到的样品离心清洗三次，在冷冻干燥机中干燥后得到前驱体；将200毫克的前驱体置于100毫升的烧杯中，加入35毫升的二甲基亚砜，12毫升的乙二胺和12毫升的乙醇，混合均匀，将混合溶液转移至微波水热反应仪中，微波频率设置为2450兆赫兹，调节微波水热反应仪在120摄氏度反应10分钟，离心清洗后得到析氢电催化剂铁硫。
2.一种析氢电催化剂FeS，其特征在于，所述电催化剂采用如权利要求1中的方法制备而成。
3.如权利要求2所述的电催化剂FeS用于电催化析氢领域。
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