CN111575708A - 一种镍钼聚离子化合物混合相纳米棒阵列的制备方法 - Google Patents
一种镍钼聚离子化合物混合相纳米棒阵列的制备方法 Download PDFInfo
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- 239000002073 nanorod Substances 0.000 title claims abstract description 19
- 150000001875 compounds Chemical class 0.000 title claims abstract description 12
- 229920000831 ionic polymer Polymers 0.000 title claims abstract description 12
- DDTIGTPWGISMKL-UHFFFAOYSA-N molybdenum nickel Chemical compound [Ni].[Mo] DDTIGTPWGISMKL-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 52
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 25
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims abstract description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 4
- 239000011521 glass Substances 0.000 claims description 20
- 238000009210 therapy by ultrasound Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 9
- 239000001257 hydrogen Substances 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 9
- 239000010411 electrocatalyst Substances 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000001075 voltammogram Methods 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 229910003296 Ni-Mo Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- YSMVUKIAKNPOLA-UHFFFAOYSA-M nickel(2+);hydroxide;nitrate Chemical compound [OH-].[Ni+2].[O-][N+]([O-])=O YSMVUKIAKNPOLA-UHFFFAOYSA-M 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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Abstract
本发明公开一种镍钼聚离子化合物混合相纳米棒阵列的制备方法，所述方法采用六水硝酸镍和仲钼酸铵作为原料，在镍片表面加热生长纳米棒阵列；所述纳米棒阵列的电催化析氢过电位为191.2mV，塔菲尔斜率为78.8mV/dec。
Description
技术领域
本发明涉及一种镍钼聚离子化合物混合相纳米棒阵列的制备方法。
技术背景
能源需求的持续增长和矿物燃料的快速消费有力地促进了清洁和可持续能源的发展。氢能被认为是最清洁、最有前途的可持续能源之一，是克服能源短缺挑战的关键解决方案。在现有技术中，电催化分解水制氢是大规模氢气生产中的一种有效的方法。
电解水需要用到电催化剂。从电催化剂的角度来看，贵金属Pt是电解水制氢效率最高的电催化剂。然而它的成本高、稀缺性和稳定性差，使它不能大规模地应用。因此目前的研究主要集中在开发高催化活性、稳定性好、低成本的电催化剂。
发明内容
本发明的目的在于提供一种高催化活性、低成本的镍钼聚离子化合物混合相纳米棒阵列电催化剂。
所述电催化剂的制备方法包括如下步骤：裁剪一块2cm×2cm×1.6mm的镍片，在6M的盐酸中超声处理3分钟，随后在丙酮中超声处理3分钟，再在去离子水中超声处理3分钟；将3克六水硝酸镍和0.2克仲钼酸铵置于20mL的玻璃瓶中，将玻璃瓶在125℃加热20分钟使得玻璃瓶中的盐熔化；再将前述处理过的镍片浸于玻璃瓶内的熔盐中，将玻璃瓶在125℃加热10小时；将镍片取出，用去离子水清洗镍片表面2次，再用酒精清洗镍片表面2次；获得的镍片表面附着有所需的镍钼聚离子化合物混合相纳米棒阵列。
与现有技术相比，本发明所述的样品具有以下的优点：制备的电催化剂呈长条形的纳米棒阵列结构，暴露的活性位点多，电催化析氢过电位和塔菲尔斜率较低。
附图说明
图1是实施例样品的XRD图谱。
图2是实施例样品和对比例样品的SEM图谱。
图3是实施例样品和对比例样品的线性伏安曲线和塔菲尔曲线。
图4是实施例样品和对比例样品的电化学双层电容拟合曲线。
具体实施方式
以下结合具体实施例对本发明的实现进行详细的描述。
所述电催化剂的制备方法包括如下步骤：裁剪一块2cm×2cm×1.6mm的镍片，在6M的盐酸中超声处理3分钟，随后在丙酮中超声处理3分钟，再在去离子水中超声处理3分钟；将3克六水硝酸镍和0.2克仲钼酸铵置于20mL的玻璃瓶中，将玻璃瓶在125℃加热20分钟使得玻璃瓶中的盐熔化；再将前述处理过的镍片浸于玻璃瓶内的熔盐中，将玻璃瓶在125℃加热10小时；将镍片取出，用去离子水清洗镍片表面2次，再用酒精清洗镍片表面2次；获得的镍片表面附着有所需的镍钼聚离子化合物混合相纳米棒阵列。
为了说明实施例的技术效果，按以下步骤作了对比例：裁剪一块2cm×2cm×1.6mm的镍片，在6M的盐酸中超声处理3分钟，随后在丙酮中超声处理3分钟，再在去离子水中超声处理3分钟；将3克六水硝酸镍置于20mL的玻璃瓶中，将玻璃瓶在125℃加热20分钟使得玻璃瓶中的盐熔化；再将前述处理过的镍片浸于玻璃瓶内的熔盐中，将玻璃瓶在125℃加热10小时；将镍片取出，用去离子水清洗镍片表面2次，再用酒精清洗镍片表面2次；获得的镍片表面附着有硝酸镍氢氧化物纳米棒阵列。
对实施例和对比例的样品进行了表征。图1是实施例样品的XRD图谱，可以看出样品的衍射峰与(NH4) Ni2Mo2O8(OH) (PDF#52-0168)和Ni2(OH)2(NO3)2 (PDF#27-0939，如图中箭头所示)的标准数据非常匹配，说明样品是上述两物相的混合物，称之为镍钼聚离子化合物混合相。图2a-b是实施例样品不同放大倍数下的SEM图谱，可以看出样品呈明显的纳米棒阵列结构，并且纳米棒的长度较长。而对比例样品（图2c-d）呈较短的纳米棒颗粒结构。这说明实施例的方法有助于纳米棒的生长。图3是实施例样品和对比例样品的线性伏安曲线和塔菲尔斜率曲线（测试溶液采用1M的KOH溶液）。实施例样品的电催化析氢过电位（100mA/cm2时）为191.2mV，塔菲尔斜率为78.8mV/dec。而对比例样品的电催化析氢过电位（100mA/cm2时）为252.6 mV，塔菲尔斜率为192.4mV/dec。这说明实施例样品具有更优异的电催化析氢性能。图4是电化学双层电容（正比于电化学活性面积）拟合曲线，从中可得到实施例样品的电化学双层电容为21.4 mF cm-2，而对比例样品的电化学双层电容为5.0 mF cm-2。这说明实施例样品的电化学活性面积更大，暴露的活性位点更多。
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)
1.一种镍钼聚离子化合物混合相纳米棒阵列的制备方法，其特征在于包括如下步骤：裁剪一块2cm×2cm×1.6mm的镍片，在6M的盐酸中超声处理3分钟，随后在丙酮中超声处理3分钟，再在去离子水中超声处理3分钟；将3克六水硝酸镍和0.2克仲钼酸铵置于20mL的玻璃瓶中，将玻璃瓶在125℃加热20分钟使得玻璃瓶中的盐熔化；再将前述处理过的镍片浸于玻璃瓶内的熔盐中，将玻璃瓶在125℃加热10小时；将镍片取出，用去离子水清洗镍片表面2次，再用酒精清洗镍片表面2次；获得的镍片表面附着有所需的镍钼聚离子化合物混合相纳米棒阵列。
2.如权利要求1所述的方法制备的镍钼聚离子化合物混合相纳米棒阵列。
3.如权利要求2所述的镍钼聚离子化合物混合相纳米棒阵列在电催化领域的应用。
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107199040A (zh) * | 2017-07-06 | 2017-09-26 | 中国科学院福建物质结构研究所 | 钼酸盐纳米阵列及其制备方法和应用 |
| CN107685150A (zh) * | 2017-08-24 | 2018-02-13 | 武汉理工大学 | 一种氮掺杂碳包覆的Ni＆MoO2超细纳米线及其制备方法和应用 |
| CN108671944A (zh) * | 2018-05-29 | 2018-10-19 | 武汉工程大学 | 一种镍钼氧化物@镍钼硫化物@泡沫镍复合纳米材料及其制备方法与应用 |
| CN109628951A (zh) * | 2018-10-31 | 2019-04-16 | 中山大学 | 一种硫化镍析氢电催化剂及其制备方法与应用 |
| CN110586116A (zh) * | 2019-09-25 | 2019-12-20 | 广西师范大学 | 一种析氢电催化剂的MoO2-Ni/CC复合材料及制备方法 |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107199040A (zh) * | 2017-07-06 | 2017-09-26 | 中国科学院福建物质结构研究所 | 钼酸盐纳米阵列及其制备方法和应用 |
| CN107685150A (zh) * | 2017-08-24 | 2018-02-13 | 武汉理工大学 | 一种氮掺杂碳包覆的Ni＆MoO2超细纳米线及其制备方法和应用 |
| CN108671944A (zh) * | 2018-05-29 | 2018-10-19 | 武汉工程大学 | 一种镍钼氧化物@镍钼硫化物@泡沫镍复合纳米材料及其制备方法与应用 |
| CN109628951A (zh) * | 2018-10-31 | 2019-04-16 | 中山大学 | 一种硫化镍析氢电催化剂及其制备方法与应用 |
| CN110586116A (zh) * | 2019-09-25 | 2019-12-20 | 广西师范大学 | 一种析氢电催化剂的MoO2-Ni/CC复合材料及制备方法 |
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