CN111701594A - 一种负载型单分散Ni纳米颗粒修饰的三维多孔V2O3微米花的制备方法 - Google Patents
一种负载型单分散Ni纳米颗粒修饰的三维多孔V2O3微米花的制备方法 Download PDFInfo
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Abstract
本发明公开了一种负载型单分散Ni纳米颗粒修饰的三维多孔V2O3微米花的制备方法。所述的材料是将镍盐与钒盐分散于超纯水中，随后放入基底材料，进行水热反应，最后经过热处理制备得到。本发明利用金属离子间还原能力和离子迁移能力的差异，非模板法制备相分离的三维多孔杂化结构。按照本发明所制备的材料结构稳定、纳米孔多、界面丰富、比表面积大、导电性好、物质传输和气体泡脱附快，表现出优异的电催化析氢和析氧活性以及稳定性。同时，本发明方法原料简单、操作性强、条件易控、适用性广，且具有工业应用潜力。
Description
【技术领域】
本发明属于能源转换与存储领域，具体涉及一种单分散Ni纳米颗粒修饰的三维多孔V2O3微米花的制备方法。
【背景技术】
煤、石油和天然气等化石能源的日益匮乏及其使用过程中伴随的污染物和碳排放，迫切需要开发和利用清洁能源，因此，能源转换与存储成为当今一大研究热点。因晶体结构多变，室温下呈金属性，以及具有强电子-电子相互作用，V2O3在锂离子电池、超级电容器、燃料电池等新能源领域引起广泛关注。但受制于电子结构，单组分V2O3的电化学性能并非理想，进而限制了其应用。随着纳米技术的发展，组分调控和微纳米结构调控被认为是进一步提升V2O3电化学活性和稳定性行之有效的方法，特别是其电催化性能。其中，负载型三维多孔杂化结构因其突出的物理化学优势，拥有更广阔的电化学应用前景。一方面，从其物理结构来看，其比表面积大、孔道丰富、结构稳定、结合牢固，可充分暴露反应活性物质、有效缩短物质传输路径、降低反应内阻和减少材料脱落，保障反应的快速平稳进行；另一方面，从其电子结构来看，物质间的相互作用可协同改善单一组分的本征活性和电化学稳定性，甚至催生新的电化学活性，为材料提供无限的应用可能。因此，非模板法制备具有三维多孔结构的V2O3基复合材料对进一步扩宽和提升V2O3电化学性能具有重要意义。
本发明巧妙利用多金属氧化物中离子的迁移和扩散能力不同，制备出未曾报道的单分散Ni纳米颗粒修饰的三维多孔V2O3微米花，且表现出稳定高效的电催化析氢和析氧活性。此外，基于其优异的物理化学性质，在其他电化学领域均有潜在的应用前景。
【发明内容】
本发明的目的在于提供了一种负载型单分散Ni纳米颗粒修饰的多孔V2O3微米花的制备方法。
为此，本发明采用如下技术方案实现上述目的：
负载型单分散Ni纳米颗粒修饰的多孔V2O3微米花的制备：
A.水热制备前驱体
将镍盐与钒盐分散于超纯水中，放入基底材料，转移至反应釜，通过水热反应制备前驱体；
B.热处理反应
将上述步骤所得前驱体进行热处理，即可得到负载型单分散Ni纳米颗粒修饰的多孔V2O3微米花。
可选地，步骤A中镍盐为含结晶水或不含结晶水的镍，浓度为0.001～1mmol/L。
可选地，步骤A中钒盐为偏钒酸盐，浓度为0.001～1mmol/L。
可选地，步骤A中镍盐和钒盐摩尔比为1:10～10:1。
可选地，步骤A中基底材料包括但不仅限于泡沫镍、泡沫铜和碳布。
可选地，步骤A中水热反应温度为60～180℃，反应时间为1～24h，物料填充比为20％～80％。
可选地，步骤B中所述热处理的温度为200～800℃，时间为0.5～6h，升温速率为0.5～20℃/min。
可选地，步骤B中所述热处理在还原性气氛下进行，之前可以经过或不经过惰性氛围下的退火处理，其中，还原性气氛包括但不仅限于氢气和氢氩混合气，惰性气氛包括但不仅限于氮气和氩气。
本发明的有益效果在于：
1.原料简单，合成成本低。
2.涉及使用的设备少，操作性强，材料使用方便，且具有一定柔性，实用价值较高。
3.所制备的负载型单分散Ni纳米颗粒修饰的三维多孔V2O3微米花，导电性好、结构稳定、纳米孔多、界面丰富、比表面积大、物质传输和气体脱附快，具有广阔的应用前景。
4.所制备的负载型单分散Ni纳米颗粒修饰的三维多孔V2O3微米花表现出优异的电催化析氢和析氧活性以及稳定性，具有工业应用潜力。
【附图说明】
图1为实施例1所制备的负载型单分散Ni纳米颗粒修饰的三维多孔V2O3微米花的XRD图谱。
图2为实施例1所制备的负载型单分散Ni纳米颗粒修饰的三维多孔V2O3微米花的SEM图。
图3为实施例1所制备的负载型单分散Ni纳米颗粒修饰的三维多孔V2O3微米花的TEM图。
图4为实施例1-2所制备负载型单分散Ni纳米颗粒修饰的三维多孔V2O3微米花以及基底材料的电催化析氢活性测试结果。
图5为以实施例1-2所制备的负载型单分散Ni纳米颗粒修饰的三维多孔V2O3微米花以及基底材料的电催化析氧活性测试结果。
图6为以实施例1所制备的负载型单分散Ni纳米颗粒修饰的三维多孔V2O3微米花的电催化析氢和析氧稳定性测试结果。
【具体实施方式】
下面结合附图和具体的实施例来进一步阐述本发明，但不应以此限制本发明的保护范围。
实施例1：
将1mmol六水合氯化镍、1mmol偏钒酸铵均匀分散于30mL超纯水中，转移至50mL反应釜，放入泡沫镍(2cm*3cm)，将水热釜盖严拧紧，于烘箱中160℃恒温反应6h。待水热釜自然冷却至室温后，取出泡沫镍，用超纯水和无水乙醇冲洗，干燥，于管式炉中，以2℃/min的升温速率，先在高纯氮气中400℃恒温反应2h，管式炉冷却至室温后，再在氢气/氩气混合气中500℃恒温反应2h，即得到泡沫镍负载的单分散Ni纳米颗粒修饰的三维多孔V2O3微米花。
实施例2：
将1mmol六水合氯化镍、1mmol偏钒酸铵均匀分散于30mL超纯水中，转移至50mL反应釜，放入泡沫镍(2cm*3cm)，将水热釜盖严拧紧，于烘箱中160℃恒温反应6h。待水热釜自然冷却至室温后，取出泡沫镍，用超纯水和无水乙醇冲洗，干燥，于管式炉中，以2℃/min的升温速率，在氢气/氩气混合气中500℃恒温反应2h，即得到负载型单分散Ni纳米颗粒修饰的三维多孔V2O3微米花。
以上所述仅为本发明的优选实施例，并不用于限制本发明，凡依本发明申请专利范围所做的等同替换和修改皆属于本发明的保护范围内。
Claims (8)
1.一种负载型单分散Ni纳米颗粒修饰的三维多孔V2O3微米花的制备方法，其特征在于包括如下步骤：
A.水热制备前驱体
将镍盐与钒盐分散于超纯水中，放入基底材料，转移至反应釜，通过水热反应制备前驱体。
B.热处理反应
将上述步骤所得前驱体进行热处理，即可得到负载型单分散Ni纳米颗粒修饰的多孔V2O3微米花。
2.根据权利要求1所述的制备方法，其特征在于，步骤A中镍盐为含结晶水或不含结晶水的镍，浓度为0.001～1mmol/L。
3.根据权利要求1所述的制备方法，其特征在于，步骤A中钒盐为偏钒酸盐，浓度为0.001～1mmol/L。
4.根据权利要求2所述的制备方法，其特征在于，步骤A中镍盐和钒盐摩尔比为1:10～10:1。
5.根据权利要求2所述的制备方法，其特征在于，步骤A中基底材料包括但不仅限于泡沫镍、泡沫铜、碳布。
6.根据权利要求2所述的制备方法，其特征在于，步骤A中水热反应温度为60～180℃，反应时间为1～24h，物料填充比为20％～80％。
7.根据权利要求1所述的制备方法，其特征在于，步骤B中所述热处理的温度为200～800℃，时间为0.5～6h，升温速率为0.5～20℃/min。
8.根据权利要求1所述的制备方法，其特征在于，步骤B中所述热处理在还原性气氛下进行，之前可以经过或不经过惰性氛围下的退火处理，其中，还原性气氛包括但不仅限于氢气和氢氩混合气，惰性气氛包括但不仅限于氮气和氩气。
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