CN114016073B - 一种Fe掺杂Ni0.85Se纳米片阵列电催化剂的制备方法 - Google Patents
一种Fe掺杂Ni0.85Se纳米片阵列电催化剂的制备方法 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000002135 nanosheet Substances 0.000 title claims description 27
- 239000010411 electrocatalyst Substances 0.000 title claims description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 90
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 28
- 239000006260 foam Substances 0.000 claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 9
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 7
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 abstract description 7
- 239000000758 substrate Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 3
- 150000001450 anions Chemical class 0.000 abstract description 2
- 239000007864 aqueous solution Substances 0.000 abstract description 2
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- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
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- 239000000203 mixture Substances 0.000 abstract description 2
- 239000011669 selenium Substances 0.000 description 49
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 14
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 8
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 8
- 239000000126 substance Substances 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 238000003491 array Methods 0.000 description 3
- -1 hydrogen ions Chemical class 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000002064 nanoplatelet Substances 0.000 description 3
- 229910052711 selenium Inorganic materials 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000013112 stability test Methods 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- 238000001075 voltammogram Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- VREFGVBLTWBCJP-UHFFFAOYSA-N alprazolam Chemical compound C12=CC(Cl)=CC=C2N2C(C)=NN=C2CN=C1C1=CC=CC=C1 VREFGVBLTWBCJP-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- LOKCTEFSRHRXRJ-UHFFFAOYSA-I dipotassium trisodium dihydrogen phosphate hydrogen phosphate dichloride Chemical compound P(=O)(O)(O)[O-].[K+].P(=O)(O)([O-])[O-].[Na+].[Na+].[Cl-].[K+].[Cl-].[Na+] LOKCTEFSRHRXRJ-UHFFFAOYSA-I 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000001453 impedance spectrum Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002953 phosphate buffered saline Substances 0.000 description 2
- QHASIAZYSXZCGO-UHFFFAOYSA-N selanylidenenickel Chemical compound [Se]=[Ni] QHASIAZYSXZCGO-UHFFFAOYSA-N 0.000 description 2
- 238000004729 solvothermal method Methods 0.000 description 2
- 238000010183 spectrum analysis Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- NOQGZXFMHARMLW-UHFFFAOYSA-N Daminozide Chemical compound CN(C)NC(=O)CCC(O)=O NOQGZXFMHARMLW-UHFFFAOYSA-N 0.000 description 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- GGVOVPORYPQPCE-UHFFFAOYSA-M chloronickel Chemical compound [Ni]Cl GGVOVPORYPQPCE-UHFFFAOYSA-M 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
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Abstract
本发明涉及一种Fe掺杂Ni0.85Se纳米片阵列的制备方法。该方法采用NiCl2·6H2O、FeCl3·6H2O、Se粉、NaOH、N2H4·H2O和泡沫镍为主要原料,将阳离子溶液(NiCl2·6H2O、FeCl3·6H2O的水溶液)、阴离子溶液(Se的水合肼溶液)利用磁力搅拌将二者混合,加入预处理的泡沫镍,在180℃下烧结12h实现最终目标产物的制备。本发明方法以泡沫镍为基底,显著提高了样品的比表面积,增加了表面活性位点,促进了电子传输,提高电催化性能。本发明不仅操作简单,步骤明确,而且具有绿色环保、经济、便捷、重复性高等优点,易于实现大规模生产。
Description
技术领域
本发明属于一种适用于电催化应用的新型Fe掺杂Ni0.85Se纳米片阵列的制备方法。具体的说,在泡沫镍(NF)基底上生长Fe掺杂Ni0.85Se纳米片阵列,形成具有优异电化学性质的电催化材料。
背景技术
近年来,电解水技术由于其成本较低、效率高、环境友好、安全性较高等优点而引起广泛关注。电解水过程是由阴极的析氢反应(HER)和阳极的析氧反应(OER)两个半反应组成。由于纯水不导电,因此实验室常用的电解液主要是硫酸(H2SO4)、氢氧化钾(KOH)和磷酸缓冲液(PBS)。原理是把析氢反应和析氧反应的催化剂分别涂在阴极和阳极上,之后浸入到电解液溶液中,当电路中有稳定的直流电通过时,氢离子在阴极消耗电子生成氢气,氢氧根离子在阳极失去电子生成氧气。目前使用的贵金属电催化剂如Pt和RuO2/IrO2,由于价格昂贵限制了电解水的大范围推广。因此急需寻找一种廉价、高效的电催化剂来降低析氢析氧反应的过电位,提高电催化的效率。过渡金属具有结构多变的d轨道电子,且具有价格低廉、结构及形貌可调控等优点,使其在电催化领域得到了大量的研究和应用。S和Se元素最外层都有6个电子,Se的原子半径要大于S,电离能小于S,最重要的是Se的金属性强于S,这使过渡金属硒化物具有更强的导电性和更优异的化学性质。由于Ni和Se的电负性相差不大,Ni和Se可以形成多种非化学计量的NiSe、NiSe2、Ni1-xSe、Ni3Se2、Ni0.85Se材料。其中Ni0.85Se由于具有大量的不饱和原子而展现出优异的电催化性质。通过在Ni0.85Se中掺杂过渡金属Fe元素可优化其电子结构,调控其形貌增加比表面积从而提升其电化学性能。
由于粉末样品易团聚,且在电催化裂解水过程中易脱落,导致其稳定性和电催化效率较低。为解决上述问题,将Fe掺杂Ni0.85Se纳米片制备在泡沫镍基底,一方面提高了Fe掺杂Ni0.85Se纳米片的分散性,提高有效的活性面积和化学稳定性,另一方面Fe掺杂Ni0.85Se纳米片与泡沫镍基底的有效接触可保证载流子的快速迁移,提高电催化效率。本发明首次采用简单的一步溶剂热法合成了一种具有优异的电催化性质的Fe掺杂Ni0.85Se纳米片阵列。
发明内容
本发明的目的是提供一种可应用于电催化领域的纳米片阵列的制备方法,其制备的纳米片具有良好的电催化性能,制备过程简单,步骤明确,易实现工业化生产。
本发明采用NiCl2·6H2O、FeCl3·6H2O、Se粉、N2H4·H2O和泡沫镍为主要原料,制备Fe掺杂Ni0.85Se纳米片阵列,本发明将阳离子溶液(NiCl2·6H2O、FeCl3·6H2O的水溶液)、阴离子溶液(Se粉的水合肼溶液)利用磁力搅拌混合,加入处理过的泡沫镍,在180℃下烧结12h实现最终目标产物的制备。
本发明制备方法的具体步骤为泡沫镍的预处理以及Fe掺杂Ni0.85Se纳米片阵列的制备:
(1)泡沫镍的预处理:取20mm×30mm泡沫镍,利用3.0M HCl洗涤10分钟,然后用丙酮和去离子水清洗,去除表面杂质,干燥处理。60℃真空干燥6h。
(2)Fe掺杂Ni0.85Se纳米片电催化剂的制备:
a、在20mL去离子水中加入NiCl2·6H2O、FeCl3·6H2O和8mmol NaOH搅拌1.5h制成溶液A;其中,NiCl2·6H2O和FeCl3·6H2O的总量为4mmol,FeCl3·6H2O的加入量按照总量4mmol的0.8%~2%计算;
b、将8mmol Se粉加入5mL水合肼中搅拌30min制成溶液B;
c、将溶液A倒入溶液B中,快速搅拌30分钟,获得混合溶液;
d、将混合溶液转移到50mL高压釜中,并插入处理好的泡沫镍,在180℃条件下加热12h;
e、自然冷却至室温后,取出泡沫镍,利用去离子水和无水乙醇清洗,干燥处理后获得所述Fe掺杂Ni0.85Se纳米片阵列电催化剂。
本发明的优点:
1.本发明采用简单的一步溶剂热法将Fe掺杂到Ni0.85Se片阵列中,制备了适用于电催化应用的纳米材料。
2.本发明方法以泡沫镍为基底,显著提高了样品的比表面积,增加了表面活性位点,促进了电子传输,提高电催化性能。
3.本发明不仅操作简单,步骤明确,而且具有绿色环保、经济、便捷、重复性高等优点,易于实现大规模生产。
附图说明
图1是本发明目标产物0.8%Fe-Ni0.85Se和2%Fe-Ni0.85Se纳米片阵列的X射线衍射图。
图2中是本发明目标产物0.8%Fe-Ni0.85Se纳米片阵列的扫描图(a)和能谱图(b)。
图3是本发明目标产物2%Fe-Ni0.85Se纳米片阵列的扫描图(a)和能谱图(b)。
图4是本发明目标产物0.8%Fe-Ni0.85Se的线性扫描伏安曲线(a),塔菲尔图(b),电化学阻抗谱(c),稳定性测试图(d)。
图5是本发明目标产物2%Fe-Ni0.85Se的线性扫描伏安曲线(a),塔菲尔图(b),电化学阻抗谱(c),稳定性测试图(d)。
图6是本发明目标产物2%Fe-Ni0.85Se(+)||0.8%Fe-Ni0.85Se(-)全解水的线性扫描伏安曲线(a),稳定性测试图(b)。
具体实施方式
下面以具体实施例的形式对本发明技术方案做进一步解释和说明。
本发明所需的原料如下:
氯化镍(NiCl2·6H2O,阿拉丁试剂)为分析纯;
氯化铁(FeCl3·6H2O,国药集团化学试剂有限公司)为分析纯;
硒粉(Se,国药集团化学试剂有限公司)为分析纯;
氢氧化钠(NaOH,国药集团化学试剂有限公司)为分析纯
水合肼(N2H4·H2O,国药集团化学试剂有限公司)为分析纯;
盐酸(HCl,国药集团化学试剂有限公司)为分析纯;
丙酮(CH3COCH3,国药集团化学试剂有限公司)为分析纯。
(1)泡沫镍的预处理:
取泡沫镍(20mm×30mm),利用3.0M HCl洗涤10分钟,然后用丙酮和去离子水清洗几次,去除表面杂质,60℃真空干燥6h。
(2)0.8%Fe掺杂Ni0.85Se纳米片阵列电阴极的制备:
在20ml去离子水中加入3.968mmol NiCl2·6H2O,0.032mmol FeCl3·6H2O和8mmolNaOH搅拌1.5h(溶液A)。将8mmol Se粉加入5ml水合肼中搅拌30min(溶液B)。将溶液A倒入溶液B中,快速搅拌30分钟。最后将混合溶液转移到50ml高压釜中,并插入处理好的泡沫镍。180℃下加热12h,然后自然冷却至室温,去除泡沫镍,利用去离子水和无水乙醇清洗3次,60℃干燥6h。
(3)2%Fe掺杂Ni0.85Se纳米片阵列电阳极的制备:
在20ml去离子水中加入3.92mmol NiCl2·6H2O,0.08mmol FeCl3·6H2O和8mmolNaOH搅拌1.5h(溶液A),将8mmol Se粉加入5ml水合肼中搅拌30min(溶液B)。将溶液A倒入溶液B中,快速搅拌30分钟。最后将混合溶液转移到50ml高压釜中,并插入处理好的泡沫镍。180℃下加热12h,然后自然冷却至室温,去除泡沫镍,利用去离子水和无水乙醇清洗3次,60℃干燥6h。
附图1是本发明目标产物0.8%Fe-Ni0.85Se和2%Fe-Ni0.85Se纳米材料的X射线衍射图。从图中可以看出,0.8%-Ni0.85Se样品中所有的衍射峰对应Ni0.85Se JCPDS No.18-0888结构。随着Fe掺杂浓度增加到2%,出现了少量NiSe相关的衍射峰,。
对目标产物0.8%Fe-Ni0.85Se进行扫描电镜表征和EDS能谱分析,如图2所示,0.8%Fe掺杂Ni0.85Se的样品为纳米片形貌。EDS能谱表明Fe元素成功掺杂到Ni0.85Se中。
对目标产物2%Fe-Ni0.85Se进行扫描电镜表征和EDS能谱分析,如图3所示,掺杂2%Fe元素仍保持纳米片阵列的形貌。同时EDS能谱表明Fe元素成功掺杂进去,且随着Fe掺杂量的增加,Fe的含量在增加。
附图4是本发明目标产物的电催化析氢反应性质,从图中可以看出,在电流密度为10mAcm-2时,目标产物中的0.8%-Ni0.85Se具有较低的过电势为120mV,塔菲尔斜率仅为34.11mVdec-1,电荷转移电阻仅为7.416Ω,并且连续测试48小时,电流密度保持稳定。
附图5是本发明目标产物纳米材料的电催化析氧反应性质,从图中可以看出,在电流密度为100mAcm-2时,目标产物中的2%-Ni0.85Se具有较低的过电势为1.54V,塔菲尔斜率为73.40mVdec-1,电荷转移电阻仅为1.57Ω,并且连续测试50小时,电流密度保持稳定。
附图6是本发明目标产物2%Fe-Ni0.85Se(+)||0.8%Fe-Ni0.85Se(-)电极全解水性质图,从图中可以看出在电流密度为100mAcm-2时,目标产物的过电势仅为1.52V。
Claims (6)
1.一种Fe掺杂Ni0.85Se纳米片阵列电催化剂的制备方法,其特征在于,该方法具体步骤如下:
a、在20mL去离子水中加入NiCl2·6H2O、FeCl3·6H2O和8mmol NaOH搅拌1.5h制成溶液A;其中,NiCl2·6H2O和FeCl3·6H2O的总量为4mmol,FeCl3·6H2O的加入量按照总量4mmol的0.8%~2%计算;
b、将8mmol Se粉加入5mL水合肼中搅拌30min制成溶液B;
c、将溶液A倒入溶液B中,快速搅拌30分钟,获得混合溶液;
d、将混合溶液转移到50mL高压釜中,并插入处理好的泡沫镍,在180℃条件下加热12h;
e、自然冷却至室温后,取出泡沫镍,利用去离子水和无水乙醇清洗,干燥处理后获得所述Fe掺杂Ni0.85Se纳米片阵列电催化剂。
2.根据权利要求1所述的Fe掺杂Ni0.85Se纳米片阵列电催化剂的制备方法,其特征在于,所述的泡沫镍利用3.0M HCl洗涤10分钟,然后用丙酮和去离子水清洗,去除表面杂质,干燥处理。
3.根据权利要求1所述的Fe掺杂Ni0.85Se纳米片阵列电催化剂的制备方法,其特征在于,泡沫镍的大小为20mm×30mm。
4.根据权利要求1所述的Fe掺杂Ni0.85Se纳米片阵列电催化剂的制备方法,其特征在于,步骤e中干燥处理时的温度为60℃,采用真空干燥方式干燥6h。
5.一种根据权利要求1~4任意一项所述的方法制备得到的Fe掺杂Ni0.85Se纳米片阵列电催化剂,其特征在于,步骤a中FeCl3·6H2O的加入量为总量4mmol的0.8%时得到0.8%Fe掺杂Ni0.85Se纳米片阵列电阴极。
6.一种根据权利要求1~4任意一项所述的方法制备得到的Fe掺杂Ni0.85Se纳米片阵列电催化剂,其特征在于,步骤a中FeCl3·6H2O的加入量为总量4mmol的2%时得到2%Fe掺杂Ni0.85Se纳米片阵列电阳极。
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