CN108735980B - 制造核壳纳米颗粒的方法 - Google Patents
制造核壳纳米颗粒的方法 Download PDFInfo
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Abstract
本发明涉及一种可用在电化学电池中的电极材料,该电化学电池用于将二氧化碳转化为有用的产品,例如合成燃料。该电极材料可以包含具有被一个或多个外壳包围的催化性核组分的纳米尺寸的核壳催化剂(即,核壳纳米颗粒或CSN),其中所述外壳中的至少一个具有介孔结构。本发明还提供了电化学电池、电化学电池电极以及制造CSN的方法。
Description
技术领域
本公开总体上涉及核壳纳米颗粒、其制造方法及其作为催化剂的用途。
背景技术
在通电时还原二氧化碳的电化学体系提供了有吸引力的电源选择,因为它们不仅能够抵消二氧化碳(主要温室气体)的排放,而且还能将二氧化碳转化成燃料和其它有用的产品。然而,这种类型的电化学电池带来了重大的技术挑战,例如低的催化活性、产物选择性以及在这种类型的体系中所使用的电极的稳定性等等。
发明内容
本发明的各个方案总体上涉及电极材料,所述电极材料可例如用在用于将二氧化碳转化为有用产品(例如合成燃料)的电化学电池中。该电极材料可以包含纳米尺寸的核壳催化剂(即,核壳纳米颗粒或CSN),其具有被一个或多个外壳包围的催化性核组分。所述外壳中的至少一个可以具有介孔结构。
本公开的各个方案总体上还涉及制造本文所述的CSN的方法。该方法可包括用临时壳组分涂覆催化性核,加热经涂覆的催化性核以将临时壳组分转化成介孔结构,将壳材料沉积到临时壳组分上,并且除去临时壳组分以提供被包含壳材料的介孔壳包围的催化性核组分。
本公开的各个方案总体上还涉及电化学电池电极和电化学电池,其将二氧化碳电化学地转化为例如有用燃料(例如合成燃料)或其它产品,并且其包含本文所述的电极材料。
附图说明
图1a是描绘根据本公开的各个方案的CSN的示例性的实心催化性核组分的剖面示意图。
图1b是描绘根据本公开的各个方案的具有涂层的CSN的示例性的实心催化性核组分的剖面示意图。
图1c是描绘根据本公开的各个方案的CSN的示例性的中空催化性核组分的剖面示意图。
图2是描绘根据本公开的各个方案的CSN的剖面示意图。
图3是描绘根据本公开的各个方案的电化学电池的剖面示意图。
具体实施方式
本公开的各个方案总体上涉及可例如用在电化学电池中的电极材料,所述电化学电池用于将二氧化碳转化为有用产品,例如合成燃料。电极材料可包含具有被一个或多个外壳包围的催化性核组分的纳米尺寸的核壳催化剂(即,核壳纳米颗粒或CSN)。所述外壳中的至少一个可以具有介孔结构。
如本文中所用的,术语“CSN”是指具有被一个或多个壳包围的催化性核组分的纳米尺寸颗粒。根据一些方案,本公开的CSN可以有利地在改善电催化电池中二氧化碳的电催化还原的有效性和/或效率方面具有多功能作用。例如,本公开的CSN可以通过提供具有高水平的催化活性、产物选择性和/或稳定性的含催化剂的电极来提高二氧化碳的电催化还原的有效性和/或效率。
根据本公开的各个方案的CSN包含被一个或多个外壳包围的催化性核组分,其中所述催化性核组分包含一种或多种催化材料。如本文中所用的,“催化材料”是指可用于引起或加速(即“催化”)化学反应的材料。例如,所述催化材料可以是至少部分地对将二氧化碳转化为例如有用燃料或其它产品进行催化的材料。
根据本公开的各个方案可使用的催化材料的实例包括,但不限于,金属(例如,铜、钴、铁、镍、铅和锡)和/或它们的合金和/或它们的氧化物。
如本文中所用的,术语“催化性核组分”是指CSN的内部组分。
催化性核组分可以通过本领域已知的任何方法来合成。例如,可以通过将金属前体溶液与还原剂混合以形成金属纳米颗粒来合成所述催化性核组分。在一些实施方案中,可以在防止或以其它方式抑制催化性核组分在合成期间氧化的稳定剂的存在下合成催化性核组分,并且该稳定剂在其上形成壳之前可容易地从催化性核组分中除去。例如,在合成催化性核组分期间所使用的体积大的聚合物如聚乙烯吡咯烷酮(分子量为55,000g/mol)抑制催化性核组分的氧化。然而,这样的稳定剂在合成后不易从催化性核组分中除去。不受任何特定理论的限制,残余稳定剂可在催化性核组分和壳之间形成额外的层,其降低了所需体系中CSN的性能。
根据一些方案,催化性核组分可以是实心核组分。如本文所使用的,术语“实心”意指,例如,非中空的。如图1a中所示,实心核组分10可以包含一种或多种催化材料11。例如,实心核组分可以包含第一催化材料,例如金属。
如图1b中所示,实心核组分10可另外包含涂覆第一催化材料11的第二催化材料12。例如,涂层可包含金属氧化物。根据一些方案,可以通过在空气中加热第一催化材料、电化学地氧化第一催化材料的外层、和/或在第一催化材料上沉积第二催化材料来形成涂层。涂层可以提供对第一催化材料的完全覆盖(即覆盖第一催化材料的表面积的100%)或可以提供对第一催化材料的部分覆盖(即覆盖第一催化材料的小于100%的表面积)。
根据一些方案,催化性核组分可以是非实心的。例如,催化性核组分可以是中空的,例如空心球。如图1c中所示,例如,中空的核组分14可以包含一种或多种第一催化材料13。例如,中空的核组分可以包含金属氧化物。如上所述,中空球也可以任选地包含涂覆第一催化材料的第二催化材料。
根据一些方案,催化性核组分可以被一个或多个外壳包围。如图2中所示,CSN 20可以包括包围催化性核组分22的外壳21,催化性核组分22可以是如本文中所述的任何催化性核组分。如图2中所示,外壳21可以是介孔壳。如本文中所用的,术语“介孔”意指包含例如直径在2与50nm之间的孔。
例如,外壳可以覆盖催化性核组分的表面积的至少90%,催化性核组分的表面积的至少80%,催化性核组分的表面积的至少70%,催化性核组分的表面积的至少60%,催化性核组分的表面积的至少50%,催化性核组分的表面积的至少40%,催化性核组分的表面积的至少30%,催化性核组分的表面积的至少20%,或催化性核组分的表面积的至少10%。
外壳可以包含例如具有某些期望特性的壳材料,特别是当用在用于将二氧化碳电化学地转化为燃料、聚合物和/或其它产品的电化学电池中时。壳材料的一个期望特征可以是其与二氧化碳和/或碳酸根离子的相互作用。例如,壳材料可以与碳相互作用,使得二氧化碳和/或碳酸根离子通过强化学键被吸附和/或化学吸附到CSN表面上。该相互作用还可以在CSN表面上提供单层类型的二氧化碳和/或碳酸根离子。例如,没有壳材料的纳米颗粒催化剂可以表现出一系列与二氧化碳和/或碳酸根离子的结合模式(例如弯曲地、直线地、氧结合和/或碳结合到催化表面),而根据本公开的CSN可呈现单一的结合模式。相较于没有壳材料的纳米颗粒,该特征至少在部分上可增大CSN表面上的二氧化碳和/或碳酸根离子的局部浓度和/或增大二氧化碳和/或碳酸根离子被吸附和/或被化学吸附在表面上的时间量(并且因此,可提供可被催化性核组分催化的二氧化碳和/或碳酸根离子的浓度)。该特征也可有助于提高反应产物的特异性。因此,所述壳材料可以,例如,有助于克服与二氧化碳在含水电解质中溶解性差相关联的问题,并提高由这种类型的电化学电池产生的反应产物的催化活性和特异性。
壳材料的另一个期望的特征可以是其改变CSN表面的pH值。例如,壳材料可以改变CSN表面的碱性。例如,这种pH改性可以,例如,影响CSN表面上的二氧化碳和/或碳酸根离子的吸附和/或化学吸附(并且因此影响可被催化性核组分催化的二氧化碳/碳酸根离子的浓度)。
壳材料的另一个期望的特征可以是其降低了反应中间体与CSN的结合能。例如,由具有反应中间体高结合能的催化剂催化的反应通常需要比由具有较低结合能的催化剂催化的反应更多的能量。因此,通过降低反应中间体的结合能,壳材料可以通过减少反应所需的能量来改善催化性核组分的催化活性。
壳材料的另一个期望的特征可以是其对电子周转(turnover)的影响。例如,壳材料可以包含促进快速电子周转的组分,与没有所述壳材料的催化剂纳米颗粒相比,其可以提高二氧化碳被催化性核组分转化的速率。
壳材料可以具有上述特征中的部分或全部,等等。
壳材料可以包含卤素。卤素可以,例如,能够与碳形成强化学键。根据一些方案,卤素可以包含在卤化物和/或三元化合物的阴离子中。例如,壳材料可以包含氟化物和/或氟氧化物。
壳材料可包含氧。根据一些方案,氧原子可包含在阴离子,例如氧化物、氢氧化物和/或氟氧化物的阴离子中。
壳材料还可以包含金属。所述金属,例如,可能能够提供促进二氧化碳还原期间的快速电子周转的氧化还原对。根据一些方案,金属可以包含在卤化物、氧化物、氢氧化物和/或三元化合物的阳离子中。可用于壳材料的金属的例子包括,但不限于,镧、钙、铈、镁、和锰。
根据本公开可使用的壳材料的实例包括,但不限于,LaF3、CeF3、CaF2、MgF2、LaOF、CeOF、La2O3、CeO2、CaO、MgO、La(OH)3、Ca(OH)2、Ce(OH)3、Ce(OH)3、Mg(OH)2及其组合。
本公开的各个方案总体上还涉及制造本文中所述的CSN的方法。
该方法可以包括,首先提供如本文中所述的催化性核组分,并用临时壳组分涂覆催化性核组分。如本文中所使用的,术语“临时壳组分”是指在制造CSN的过程中使用、但在该过程期间被至少部分地去除的组分。
根据本公开有用的临时壳组分的实例包括,但不限于,SiO2和具有与SiO2相似的化学和物理性质的金属氧化物,例如TiO2、Al2O3和/或ZnO。
可以通过本领域已知的任何方式用临时壳组分涂覆催化性核组分。根据一些方案,临时壳组分可以覆盖,例如,催化性核组分的表面积的至少50%,优选至少60%,更优选至少70%,甚至更优选至少80%,甚至更优选至少90%,并且最优选100%。
该方法可以包括在足以使临时壳组分转变成介孔结构的条件下加热涂覆有临时壳组分的催化性核组分。例如,加热催化性核组分可以包括煅烧。如本文中所用的,术语“煅烧”是指足以促进热分解地加热组合物。根据一些方案,煅烧可以包括在空气和/或氧气和/或惰性气体中加热至高温。然而,煅烧也可以指包含有限的空气和/或氧气和/或惰性气体或者没有空气和/或氧气和/或惰性气体的热工艺。
例如,可以将涂覆有临时壳组分的催化性核组分加热到250℃-400℃,优选275℃-375℃,甚至更优选300℃-350℃的温度。可以将涂覆有临时壳组分的催化性核组分加热达足以将临时壳组分转化成介孔结构的时间。例如,可以将涂覆有临时壳组分的催化性核组分加热约1至10小时,优选约1至8小时,更优选约2至6小时的时间。应该理解,加热时间可能受到一个或多个条件的影响,所述条件包括临时壳组分的厚度、存在的任何稳定剂的属性、以及组分在其中加热的气氛(例如空气和/或氧气和/或惰性气体)。
一旦已经将临时壳组分转化成介孔结构,就可将壳材料沉积到介孔结构上。壳材料可以包含本文中所述的任何壳材料。
壳材料可通过本领域已知的足以将壳材料沉积到介孔结构的表面积的例如至少50%,优选至少60%,更优选至少70%,甚至更优选至少80%,甚至更优选至少90%,最优选100%上的任何方式沉积到介孔结构上。例如,可以将壳材料的前体与纳米颗粒(即,涂覆有临时壳组分介孔结构的催化性核组分)组合和/或混合,使得壳材料充分沉积到介孔结构上。
一旦壳材料沉积到介孔结构上,该方法就可包括除去临时壳组分,以提供由包含壳材料的介孔壳包围的催化性核组分。
例如,可以通过蚀刻去除临时壳组分。如本文中所使用的,术语“蚀刻”是指例如使用蚀刻剂选择性地化学地溶解、分解和/或以其它方式移除一种组分的工艺。根据本发明有用的蚀刻剂包括,但不限于,强酸和/或强碱,例如NaOH、HF、KOH、LiOH、RbOH、HI、HBr和HCl。如本文中所用的,术语“强碱”和“强酸”分别指在水中完全解离的碱或酸。
该方法可以包括使纳米颗粒(即,包含催化性核组分,所述催化性核组分被涂覆有壳材料沉积在其上的临时壳组分介孔结构)与蚀刻剂接触,使得临时壳组分被部分地或完全地去除。根据一些方案,例如,去除临时壳组分的至少50%,优选至少60%,更优选至少70%,甚至更优选至少80%,甚至更优选至少90%,和最优选100%。
本公开的各个方案总体上还涉及电化学电池电极和电化学电池,其将二氧化碳电化学地转化成例如有用的燃料(例如合成燃料)或其它产品,并且其包含本文中所述的电极材料。术语“电化学电池”是指通过引入电能来促进化学反应的装置和/或装置部件。电化学电池具有两个或更多个电极(例如,正电极和负电极)和电解质。
本公开的各个方案还大体上涉及包含本文中所述的CSN的电化学电池和电化学电池电极。具体地,如图3中所示,本公开的电化学电池30可以包含,例如,至少一个包括CSN32的阴极31、阳极33和液体电解质34,并且当给电池通电时可以将二氧化碳转化成有用的产品(例如,燃料、聚合物等)。例如,电化学电池可将二氧化碳还原成一氧化碳、C2-C3烷烃、C2-C3烯烃、C2-C3醇、C2-C3羧酸、C2-C3醛或其组合。根据一些方案,给电化学电池通电而不产生任何额外的二氧化碳。
所述电化学电池可以包括包含电催化剂、特别是包含如本文中所述的CSN的电催化剂的电极(例如阴极)。相对于现有技术已知的电极,本公开的电极显示出一定的区别性特性。例如,与本领域已知的其它电极相比,根据本公开的电极可以显示出更高的催化活性、稳定性和选择性。这些区别性特性可以至少部分地由CSN的催化性核组分与一个或多个外壳的组合产生。
例如,至少部分地由于CSN的外壳,本公开的各个方案的电极可以显示出比已知电极更高的稳定性。例如,外壳可以保护催化性核组分免受电解质溶液的腐蚀和/或抑制析氢反应。所述外壳还可以减少或抑制杂质在电解质中的碳沉积和/或金属沉积,其可能随时间降低催化性能。如本文所述,至少部分地由于壳材料的期望特征,本公开的电极还可以显示出更高的催化活性和/或选择性。
虽然已经结合上面概述的示例性方案描述了本文中所述的各个方案,但是对于那些具有本领域至少普通技能的人来说,各种替代、修改、变体、改进和/或实质性等同,无论是已知的还是目前未预料到的或目前未能预料到的,均可变得显而易见。因此,如上所述的示例性方案旨在是说明性的,而非限制性的。在不脱离本公开的精神和范围的情况下可以做出各种改变。因此,本公开旨在涵盖所有已知或以后开发的替代、修改、变体、改进和/或实质性等同。
因此,权利要求书并非旨在限于在此示出的方案,而是要符合与权利要求书的语言一致的全部范围,其中以单数形式提及的要素并非意在表示“一个和仅一个”,除非特别如此陈述,而是表示“一个或多个”。本领域普通技术人员已知或将来为本领域普通技术人员所知的贯穿本公开所描述的各个方案的要素的所有结构和功能等同物在此通过引用明确并入本文中,并且旨在包含于权利要求书中。此外,而且,在此公开的任何内容都并非旨在奉献于公众,不管这些公开是否明确记载在权利要求中。除非使用短语“用于......的装置”来明确叙述要素,否则任何权利要求元素都不应被解释为装置加功能。
此外,本文中使用词语“示例”来表示“用作示例、实例或说明”。本文中被描述为“示例”的任何方案并非必然被解释为比其它方案优选或有利。除非特别指出,否则术语“一些”是指一个或多个。诸如“A、B或C中的至少一个”、“A、B和C中的至少一个”和“A、B、C或其任何组合”的组合包括A、B和/或C的任何组合,并且可包括多个/多种A、多个/多种B或多个/多种C。具体地,诸如“A、B或C中的至少一个”、“A、B和C中的至少一个”、和“A、B、C或其任何组合”可以是仅A,仅B,仅C,A和B,A和C,B和C,或A和B和C,其中任何这样的组合可包含A、B或C的一个或多个成员。本文中所公开的均不打算奉献给公众,不管这些公开是否明确记载在权利要求书中。
Claims (7)
1.一种制造核壳纳米颗粒的方法,该方法包括:
提供包含催化材料的催化性核组分,其中所述催化材料包含铜和/或铜的合金和/或铜的氧化物;
用临时壳组分涂覆所述催化性核组分,其中所述临时壳组分包含SiO2;
加热涂覆有所述临时壳组分的所述催化性核组分,以将所述临时壳组分转化为介孔结构;
将壳材料沉积在所述临时壳组分上,其中所述壳材料选自由LaF3、CeF3、CaF2、MgF2、LaOF、CeOF、La2O3、CeO2、CaO、MgO、La(OH)3、Ca(OH)2、Ce(OH)3、Mg(OH)2、及其组合组成的组;
除去所述临时壳组分,以提供由包含所述壳材料的介孔壳包围的催化性核组分,其中除去所述临时壳组分包括蚀刻,所述蚀刻包括使用蚀刻剂选择性地化学地除去所述临时壳组分,所述蚀刻剂包含强酸和/或强碱。
2.根据权利要求1所述的方法,其中,加热涂覆有所述临时壳组分的所述催化性核组分在300℃-350℃的温度下进行。
3.一种用于以电化学方式转化二氧化碳的电化学电池电极,其包括由包含壳材料的介孔壳包围的催化性核组分,
其中,所述催化性核组分包含催化材料,所述催化材料包含铜和/或铜的合金和/或铜的氧化物,并且其中所述壳材料选自由LaF3、CeF3、CaF2、MgF2、LaOF、CeOF、La2O3、CeO2、CaO、MgO、La(OH)3、Ca(OH)2、Ce(OH)3、Mg(OH)2、及其组合组成的组。
4.根据权利要求3所述的电化学电池电极,其中,催化性核组分是中空的。
5.根据权利要求3所述的电化学电池电极,其中,催化性核组分是实心的。
6.一种电化学电池,其包含根据权利要求3所述的电极,其中所述电化学电池被配置用于电化学地转化二氧化碳。
7.根据权利要求6所述的电化学电池,还包括第二电极和电解质。
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