CN111203253A - 一种氮掺杂碳包覆的球状Ni/Pd异质结构纳米材料的合成方法 - Google Patents
一种氮掺杂碳包覆的球状Ni/Pd异质结构纳米材料的合成方法 Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 23
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 18
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- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 46
- TWBYWOBDOCUKOW-UHFFFAOYSA-N isonicotinic acid Chemical compound OC(=O)C1=CC=NC=C1 TWBYWOBDOCUKOW-UHFFFAOYSA-N 0.000 claims abstract description 22
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Abstract
一种氮掺杂碳包覆的球状Ni/Pd异质结构纳米材料的合成方法，通过分步法，首先通过水热法合成镍钛与异烟酸配位形成前驱物，原位高温煅烧制备NiO多孔球状材料，经氢气气氛还原得到多孔Ni单质多孔微球，最后原位溶液置换得到氮掺杂碳包覆的球状Ni/Pd异质结构复合材料。本发明的方法简单易行，通过水热合成法、高温煅烧、原位置换反应得到一种氮掺杂碳包覆的球状Ni/Pd异质结构纳米材料；所制备的氮掺杂碳包覆的球状Ni/Pd异质结构材料属于一种具有氮掺杂碳包覆3D构型金属纳米颗粒的催化剂，相对于单纯的金属纳米颗粒催化剂有着更好的活性，稳定性和回收率，可作为新的催化材料，具有较好的应用前景。
Description
技术领域
本发明涉及纳米材料的合成，具体涉及一种氮掺杂碳包覆的球状Ni/Pd异质结构纳米材料的合成方法。
背景技术
金属纳米颗粒的催化剂由于具有高比例的表面活性原子，在多相催化中表现出很高的活性，成为目前研究的关键。对于如何提高金属纳米颗粒基催化剂的活性，目前研究可通过构建双金属复合物来提高单金属纳米颗粒催化活性的能力，该双金属复合物可通过电子结构调整在两种组合物之间提供协同效应.特别是当过渡金属(如Fe，Co和Ni)与贵金属纳米颗粒结合使用，可以降低成本并增强催化活性，使其成为更具吸引力的催化剂，同时氮掺杂碳的存在可以对反应基体的吸附，可进一步促进了催化过程，提高催化活性。
此外，具有特定形貌的纳米材料也可以提高其表面活性位点的裸露比例，例如构建由金属纳米粒子组装并具有特定形貌的三维(3D)介孔结构，此结构既可将大部分表面原子裸露在材料外部，其反应分子可以充分于表面进行接触，同时避免金属纳米粒子的聚集。此外，所构建的3D结构具有较大的尺寸分布，可以轻松地从非均相催化的反应溶液中分离出来。最重要的是，通过构建由金属纳米颗粒组装而成的3D介孔结构作为催化剂，可以很好地平衡活性，稳定性和回收率之间的关系。
因此设计一种具有氮掺杂碳包覆的3D结构金属纳米颗粒的催化剂是一项有意义的工作，但仍然是存在巨大的挑战。
发明内容
本发明的目的是提供一种简单易行的氮掺杂碳包覆的球状Ni/Pd异质结构纳米材料的合成方法，通过分步法，首先通过水热法合成镍钛与异烟酸配位形成前驱物，原位高温煅烧制备NiO多孔球状材料，经氢气气氛还原得到多孔Ni单质多孔微球，最后原位溶液置换得到氮掺杂碳包覆的球状Ni/Pd异质结构复合材料。
具体而言，本发明提供了一种氮掺杂碳包覆的球状Ni/Pd异质结构纳米材料的合成方法，包括以下步骤：
S1：将六水合硝酸镍和异烟酸溶解在N,N-二甲基甲酰胺、无水乙醇和去离子水的混合溶液中，再将混合溶液转移至反应釜中，加热一段时间，离心收集产物，清洗，烘干得Ni与异烟酸配位前驱物；
S2：将步骤S1中值得的前驱物在保护气氛中高温煅烧，合成NiO微球；
S3：将步骤S2制备的NiO微球在H2/Ar气氛中高温煅烧，合成Ni单质微球；
S4：将获得的Ni单质微球颗粒和四氯钯酸钠(II)溶解在去离子水中得分散体，然后将分散体超声处理一段时间后置于烤箱中加热一段时间，离心收集产物，洗涤，干燥，得氮掺杂碳包覆的球状Ni/Pd异质结构纳米材料。
进一步的，所述步骤S1中，N,N-二甲基甲酰胺、无水乙醇和去离子水的体积比为9：5：1。
进一步的，所述步骤S1中，所述反应釜为聚四氟乙烯高压反应釜，加热温度为150℃，加热时间为6h。
进一步的，所述步骤S2中，所述保护气氛为氩气氛围，煅烧温度为450℃，升温速率为2℃·min-1，煅烧时间为2h。
进一步的，所述步骤S3中，H2/Ar气氛中，H2：的浓度为10％，煅烧温度为400℃，升温速率为2℃·min-1。
进一步的，所述步骤S4具体包括，将获得的Ni单质微球颗粒和四氯钯酸钠(II)溶解在去离子水中得分散体，然后将分散体超声处理一段时间后置于烤箱中于60℃下反应3小时，离心收集产物，去离子水和乙醇洗涤几次，在60℃下干燥过夜，得氮掺杂碳包覆的球状Ni/Pd异质结构纳米材料。
本发明还提供了由上述合成方法制备的氮掺杂碳包覆的球状Ni/Pd异质结构纳米材料。
与现有技术相比，本发明的有益技术效果：
本发明的方法简单易行，通过水热合成法、高温煅烧、原位置换反应得到一种氮掺杂碳包覆的球状Ni/Pd异质结构纳米材料；所制备的氮掺杂碳包覆的球状Ni/Pd异质结构材料属于一种具有氮掺杂碳包覆3D构型金属纳米颗粒的催化剂，相对于单纯的金属纳米颗粒催化剂有着更好的活性，稳定性和回收率，可作为新的催化材料，具有较好的应用前景。
附图说明
图1是本发明实施例1所制备Ni与异烟酸配位前驱物的扫描电镜图(a)和Ni与异烟酸配位前驱物的X射线粉末衍射图(b)；
图2是本发明实施例1所制备NiO微球的扫描电镜图(a)和NiO微球的X射线粉末衍射图(b)；
图3是本发明实施例1所制备Ni单质的扫描电镜图(a)和Ni单质的X射线粉末衍射图(b)；
图4是本发明实施例1所制备Ni/Pd异质结构的扫描电镜图(a)和Ni/Pd异质结构的X射线粉末衍射图(b)；
图5本发明实施例1所制备的Ni/Pd异质结构的透射图(a-b)；
图6本发明实施例1所制备的Ni/Pd异质结构的元素分布图。
具体实施方式：
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
第一步：合成镍与异烟酸配位前驱物。
取0.0290g六水合硝酸镍和0.0123g的异烟酸溶解在N,N-二甲基甲酰胺(9ml)、无水乙醇(5ml)、去离子水(1mL|)的混合溶液中，将上述混合溶液转移至聚四氟乙烯高压应釜中，加热至150℃，反应时间6h。反应结束后，通过离心收集产物，用无水乙醇清洗产物数次，置于干燥箱中烘干即可得到Ni与异烟酸配位前驱物(图1)。
第二步：合成NiO微球
取球状镍与异烟酸配合物在氩气氛围保护下将其进行高温煅烧，煅烧温度为450℃，2℃·min-1的加热速率下煅烧2h，合成NiO微球(图2)。
第三步：合成Ni单质微球
将第二步合成的NiO微球在2℃·min-1的H2/Ar(H2：10％)气氛中在400℃下煅烧，合成Ni单质微球(图4)。
第四步：合成Ni/Pd异质结构
将获得的Ni单质微球颗粒(0.0150g)和四氯钯酸钠(II)(0.0075g)溶解在去离子水(5ml)中。然后将分散体超声处理10分钟。在烤箱中于60℃下反应3小时后，通过离心收集产物，并用去离子水和乙醇洗涤几次，然后在60℃下干燥过夜，合成氮掺杂碳包覆的球状Ni/Pd异质结构材料(图4-图6)。
Claims (7)
1.一种氮掺杂碳包覆的球状Ni/Pd异质结构纳米材料的合成方法，其特征在于，包括以下步骤：
S1：将六水合硝酸镍和异烟酸溶解在N,N-二甲基甲酰胺、无水乙醇和去离子水的混合溶液中，再将混合溶液转移至反应釜中，加热一段时间，离心收集产物，清洗，烘干得Ni与异烟酸配位前驱物；
S2：将步骤S1中值得的前驱物在保护气氛中高温煅烧，合成NiO微球；
S3：将步骤S2制备的NiO微球在H2/Ar气氛中高温煅烧，合成Ni单质微球；
S4：将获得的Ni单质微球颗粒和四氯钯酸钠(II)溶解在去离子水中得分散体，然后将分散体超声处理一段时间后置于烤箱中加热一段时间，离心收集产物，洗涤，干燥，得氮掺杂碳包覆的球状Ni/Pd异质结构纳米材料。
2.根据权利要求1所述的一种氮掺杂碳包覆的球状Ni/Pd异质结构纳米材料的合成方法，其特征在于，所述步骤S1中，N,N-二甲基甲酰胺、无水乙醇和去离子水的体积比为9：5：1。
3.根据权利要求1所述的一种氮掺杂碳包覆的球状Ni/Pd异质结构纳米材料的合成方法，其特征在于，所述步骤S1中，所述反应釜为聚四氟乙烯高压反应釜，加热温度为150℃，加热时间为6h。
4.根据权利要求1所述的一种氮掺杂碳包覆的球状Ni/Pd异质结构纳米材料的合成方法，其特征在于，所述步骤S2中，所述保护气氛为氩气氛围，煅烧温度为450℃，升温速率为2℃·min-1，煅烧时间为2h。
5.根据权利要求1所述的一种氮掺杂碳包覆的球状Ni/Pd异质结构纳米材料的合成方法，其特征在于，所述步骤S3中，H2/Ar气氛中，H2：的浓度为10％，煅烧温度为400℃，升温速率为2℃·min-1。
6.根据权利要求1所述的一种氮掺杂碳包覆的球状Ni/Pd异质结构纳米材料的合成方法，其特征在于，所述步骤S4具体包括，将获得的Ni单质微球颗粒和四氯钯酸钠(II)溶解在去离子水中得分散体，然后将分散体超声处理一段时间后置于烤箱中于60℃下反应3小时，离心收集产物，去离子水和乙醇洗涤几次，在60℃下干燥过夜，得氮掺杂碳包覆的球状Ni/Pd异质结构纳米材料。
7.由上述任一权利要求所述合成方法制备的氮掺杂碳包覆的球状Ni/Pd异质结构纳米材料。
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