CN108554423A - 一种基于液相硫化法制备泡沫镍负载硫化镍的方法 - Google Patents
一种基于液相硫化法制备泡沫镍负载硫化镍的方法 Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 39
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000004073 vulcanization Methods 0.000 title claims abstract description 12
- 239000007791 liquid phase Substances 0.000 title claims abstract description 11
- 239000006260 foam Substances 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethyl mercaptane Natural products CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 claims abstract description 12
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001548 drop coating Methods 0.000 claims abstract description 7
- YGHCWPXPAHSSNA-UHFFFAOYSA-N nickel subsulfide Chemical compound [Ni].[Ni]=S.[Ni]=S YGHCWPXPAHSSNA-UHFFFAOYSA-N 0.000 claims abstract 2
- GHKCSRZBNZQHKW-UHFFFAOYSA-N 1-sulfanylethanol Chemical class CC(O)S GHKCSRZBNZQHKW-UHFFFAOYSA-N 0.000 claims description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 2
- -1 mercaptoethanol nickel Chemical compound 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 8
- 238000013459 approach Methods 0.000 abstract description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 12
- 229910052739 hydrogen Inorganic materials 0.000 description 12
- 239000001257 hydrogen Substances 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 9
- 238000005868 electrolysis reaction Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000011161 development Methods 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 238000002407 reforming Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/049—Sulfides with chromium, molybdenum, tungsten or polonium with iron group metals or platinum group metals
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Abstract
一种基于液相硫化法制备泡沫镍负载硫化镍的方法。该方法包括以下步骤:将巯基乙醇均匀滴涂在泡沫镍(NF)上;然后置于加热板上,在285℃‑315℃下加热50~100s,得到泡沫镍负载硫化镍(Ni3S2/NF)。其中,涂覆量为每平方厘米0.05~0.30mL。本发明采用液相硫化法制备泡沫镍负载硫化镍,极大的简化了制备工艺,大大缩短制备时间。
Description
技术领域
本发明涉及一种液相硫化法制备泡沫镍负载硫化镍(Ni3S2/NF)的方法,属于电催化制氢领域。
背景技术
随着经济的发展,人们对能源的需求也日益增加。20世纪初期及之前,人们获得能源的主要途径是通过传统的化石能源得到,但化石能源是不可在生能源,其储量的逐年减少,使得能源危机发生的可能性与日俱增;并且化石燃料的燃烧引起一系列的环境问题,导致了环境污染和温室效应加剧等。为了解决人类将要面对的能源危机,寻求一种高效、无污染、储量丰富的能源成为重要研究方向。在二十世纪七十年代,氢气作为一种新兴能源越来越受到人们的重视。
目前,工业制氢的方法主要分为三种:重整甲烷蒸汽、煤的气化以及电解水制氢三种方法;其中超过95%的氢气是通过重整甲烷蒸汽和煤的气化方法制备的,只有4%的氢气是通过电解水的方法所制备的。显然,当前的制氢方法仍然依赖化石燃料,但依赖于化石燃料的制氢技术并不能从根源解决环境污染和二氧化碳的排放导致的温室效应等问题。因此前两种制氢方法违背了我们使用清洁能源的初衷,所以发展电解水制氢成为最有潜力且可持续发展的途径。
在电解水制氢过程中,电解水成本高的问题一直阻碍其发展。电催化剂的使用成为最有效降低电解水制氢成本的应对策略。然而电催化性能最佳的贵金属催化剂储量有限,其广泛应用受到限制。硫化镍因其具有低成本、良好的稳定性、高导电性等优点而备受人们关注,硫化镍的相关研究也层出不穷。2015年Tewodros Asefa课题组报道了通过5小时水热法制备泡沫镍负载硫化镍,在10mA/cm2时的过电势为-223mV;2016沈培康课题组报道了通过在600℃下3小时化学气相沉积法制备泡沫镍负载硫化镍,在10mA/cm2时的过电势为-199mV。但目前报道中,硫化镍的制备方法存在耗时长、高温、电催化性能不佳等缺点,其制备工艺有待改善。
发明内容
本发明的目的在于针对当前技术中存在的以化学气相沉积法时高温的问题,以及水热法、溶剂热法时耗时长,反应釜高压不安全的缺点,提供一种基于液相硫化法制备泡沫镍负载硫化镍的方法。该方法首次采用液体硫源巯基乙醇进行硫化泡沫镍,只需要经过超短时间加热即可进行硫化,得到泡沫镍负载硫化镍并提高其电催化性能。本发明工艺简易快捷,低成本,并且重复率以及材料利用率都很高。
本发明的技术方案为:
一种基于液相硫化法制备泡沫镍负载硫化镍的方法,包括以下步骤:
(1)泡沫镍上滴涂巯基乙醇
将巯基乙醇涂覆在泡沫镍(NF)上;
其中,每平方厘米泡沫镍涂覆有0.05~0.30mL巯基乙醇;
(2)制备泡沫镍负载硫化镍
将步骤(1)中滴涂好巯基乙醇的泡沫镍(NF)置于加热板上,在285℃-315℃下加热50~100s,得到泡沫镍负载硫化镍(Ni3S2/NF)。
所述的巯基乙醇的纯度为99%。
所述的泡沫镍的纯度为95%,密度为0.45g/cm3,孔隙率为95%,厚度为0.5~2mm。
本发明的有益效果:
(1)本方法采用液相硫化法制备泡沫镍负载硫化镍,极大的简化了制备工艺,大大缩短制备时间。
(2)本方法制备得到的泡沫镍负载硫化镍的电催化性能优于通过水热法、溶剂热法、化学气相沉积法、电沉积法等方法制备的泡沫镍负载硫化镍,同时也节省资源、低成本。
(3)本方法制备得到的硫化镍均匀负载在泡沫镍上,形成超薄薄膜覆盖在泡沫镍表面,有助于提高泡沫镍负载硫化镍的电催化性能。
(4)本方法不仅可以用来制备硫化镍,还可以延伸至制备其他的过渡金属硫化物,其他步骤同实施例1,不同之处为采用了其他泡沫金属(如泡沫铜、泡沫铁镍等其他泡沫过渡金属)进行硫化,具有广泛的实用性、普适性。
附图说明
图1为实施例1的X射线衍射图;
图2为实施例1的SEM扫描图;
图3为实施例1的极化曲线图。
具体实施方式
本发明涉及的泡沫镍的生产厂家为Sigam公司,纯度为95%,密度为0.45g/cm3,尺寸为1cm*1cm,孔隙率为95%,厚度为1mm;巯基乙醇的生产厂家为天津光复精细化工研究所,纯度为99%,密度为1.11g/cm3。
实施例1
(1)泡沫镍上滴涂巯基乙醇
将0.1mL巯基乙醇均匀滴涂在1cm*1cm的泡沫镍的一侧表面上;
(2)制备泡沫镍负载硫化镍
将步骤(1)中滴涂好巯基乙醇的泡沫镍置于加热板上,在300℃下加热50s,最后得到泡沫镍负载硫化镍(Ni3S2/NF)。X射线衍射图(图1)中的(101)、(110)、(003)、(202)、(113)、(211)、(122)、(300)晶面分别与标准卡片JCPDS No.44-1418相对应,证明为纯相的硫化镍,表明所发明的方法可以用来制备纯相的硫化镍(Ni3S2);其中三个最强的衍射峰为泡沫镍基底的衍射峰,图1中的(111)、(200)、(220)晶面分别与标准卡片JCPDSNo.04-0850相对应,证明为纯相的基底镍单质(NF)。SEM扫描图(图2)表明硫化镍(Ni3S2)以薄膜的形式均匀的包覆在泡沫镍(NF)上,并且硫化镍薄膜的厚度约为200nm。极化曲线图(图3)表明泡沫镍负载硫化镍在10mA/cm2时的过电势为-131mV(在1M KOH电解液下进行电催化测试),相较于其他报道其具有优异的电催化性能。
实施例2
其他步骤同实施例1,不同之处为加热温度,由加热温度300℃变化为310℃。得到的产品接近实施例1,得到厚度约为150nm的硫化镍薄膜。
实施例3
其他步骤同实施例1,不同之处为加热时间,由加热时间50s变化为100s。得到的产品接近实施例1,得到厚度约为200nm的硫化镍薄膜。
对比例1
其他步骤同实施例1,不同之处为加热温度,由加热温度300℃变化为200℃。得到的产品不同于实施例1,未得到硫化镍薄膜。
对比例2
其他步骤同实施例1,不同之处为加热时间,由加热时间50s变化为30s。得到的产品不同于实施例1,未得到硫化镍薄膜。
本发明未尽事宜为公知技术。
Claims (3)
1.一种基于液相硫化法制备泡沫镍负载硫化镍的方法,其特征为该方法包括以下步骤:
(1)泡沫镍上滴涂巯基乙醇
将巯基乙醇涂覆在泡沫镍(NF)上;
其中,每平方厘米泡沫镍涂覆有0.05~0.30mL巯基乙醇;
(2)制备泡沫镍负载硫化镍
将步骤(1)中涂覆有巯基乙醇的泡沫镍(NF)置于加热板上,在285℃-315℃下加热50~100s,得到泡沫镍负载硫化镍(Ni3S2/NF)。
2.如权利要求1所述的基于液相硫化法制备泡沫镍负载硫化镍的方法,其特征为所述的巯基乙醇的纯度为99%。
3.如权利要求1所述的基于液相硫化法制备泡沫镍负载硫化镍的方法,其特征为所述的泡沫镍的纯度为95%,密度为0.45g/cm3,孔隙率为95%,厚度为0.5~2mm。
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CN109821554A (zh) * | 2019-01-17 | 2019-05-31 | 河北工业大学 | 一种Ni-Fe-S纳米片花的制备方法 |
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