CN111185157A - 一种用电催化析氢的低含量高分散的Rh纳米纤维的制备 - Google Patents

一种用电催化析氢的低含量高分散的Rh纳米纤维的制备 Download PDF

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CN111185157A
CN111185157A CN202010035467.5A CN202010035467A CN111185157A CN 111185157 A CN111185157 A CN 111185157A CN 202010035467 A CN202010035467 A CN 202010035467A CN 111185157 A CN111185157 A CN 111185157A
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卜云飞
卜加俊
李峰
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Nanjing Erxiang Foil New Material Technology Co Ltd
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Abstract

本发明具体涉及一种用电催化析氢的低含量高分散的Rh纳米纤维的制备,包括:在烧杯中加入摩尔比为1比4的植酸和0.01g摩尔质量为209.26g/mol的RhCl3。当烧杯中的RhCl3与植酸相互完全溶解后,加入10mL的DMF溶液后,50度水浴加热搅拌过程中加入1gPAN.待全部溶解后形成粘稠液体。将粘稠液体吸入针筒,将针筒装入泵推装置,收集器收集由针头喷射出的针筒里的纤维;在针头与收集器之间施加25kV的电压,生成纤维状前驱体。四收集生成的纤维状前驱体,并将纤维状前驱体放入烘箱干燥12小时后,置入马弗炉煅烧,煅烧全过程通入氮气作为保护气体。本制备方法成本低、活性高、稳定性好。

Description

一种用电催化析氢的低含量高分散的Rh纳米纤维的制备
技术领域
本发明涉及氢能制造领域,具体涉及一种用电催化析氢的低含量高分散的Rh纳米纤维的制备。
背景技术
氢气作为一种绿色能源被广泛的应用在一系列的新能源转换装置中,例如,燃料电池、金属空气电池等。为了获得廉价的氢气,电解水成为关注的焦点。电解水的关键是开发出高效稳定的电解水制氢催化剂。其中贵金属及其化合物,例如Pt、Ir、Ru、Rh、因其较高的效率,和商业化潜力,成为开发研究的热点。然而昂贵的价格和不足的稳定性制约了它的进一步发展。因此开发廉价高效的电解水催化剂成为研究的重中之重。对于贵金属而言,通过形貌控制暴露出具有高活性的晶面和制备成复合型电极材料可以降低原料用量以降低成本。
目前的研究大多集中在通过水热法制备出具有较好纳米形貌的结构,通过纳米形貌可以很好的提高反应活性和原料使用量。然而,水热法的合成量大多集中在毫克级,放大至工业级别的产量需要进行一系列的放大实验,该过程较易出现形貌难以维持、产量难以控制等问题。
发明内容
1.所要解决的技术问题:
针对上述问题,本发明提出一种用电催化析氢的低含量高分散的Rh纳米纤维的制备,为基于静电纺丝法开发出一种用于制备低贵金属含量、高分散度的贵金属纳米纤维的普遍适用的方法。
2.技术方案:
一种用电催化析氢的低含量高分散的Rh纳米纤维的制备,其特征在于:包括以下步骤:
步骤一:在烧杯中加入摩尔比为1比4的植酸,将0.01g摩尔质量为209.26g/mol的RhCl3放入烧杯中。
步骤二:当烧杯中的RhCl3与植酸相互完全溶解后,加入10mL的DMF溶液后,50度水浴加热搅拌过程中加入1gPAN. 待全部溶解后形成粘稠液体。
步骤三:将粘稠液体吸入针筒,将针筒装入泵推装置,收集器收集由针头喷射出的针筒里的纤维;在针头与收集器之间施加25kV的电压,生成纤维状前驱体。
步骤四:收集生成的纤维状前驱体,并将纤维状前驱体放入烘箱干燥12小时后,置入马弗炉煅烧,煅烧全过程通入氮气作为保护气体;即可得到Rh金属均匀分散的碳纳米纤维。
进一步地,所述马弗炉煅烧具体过程为全程采用氮气作为保护气,以1.5℃/min的升温速率提高温度至900℃维持3h小时,之后迅速降温至室温。
3.有益效果:
(1)本制备中基于静电纺丝法,开发出一种用于制备低贵金属含量、高分散度的贵金属纳米纤维的普遍适用的方法,具有更高的制备氢气的催化活性、贵金属含量低、分散度高不团聚、其制备方法用来生成Rh纳米纤维其成本低、活性高、稳定性好。
(2)本制备采用的静电纺丝法使生产出的纳米纤维形貌容易维持、产量容易控制。
附图说明
图1为采用本发明生成的 Rh纳米纤维的TEM图,其中尺度为200nm;
图2为采用本发明生成的 Rh纳米纤维的Rh纳米纤维的在酸或碱中的HER性能图。
具体实施方式
下面结合附图对本发明进行具体的说明。
一种用电催化析氢的低含量高分散的Rh纳米纤维的制备,其特征在于:包括以下步骤:
步骤一:在烧杯中加入摩尔比为1比4的植酸,将0.01g摩尔质量为209.26g/mol的RhCl3放入烧杯中。
步骤二:当烧杯中的RhCl3与植酸相互完全溶解后,加入10mL的DMF溶液后,50度水浴加热搅拌过程中加入1gPAN. 待全部溶解后形成粘稠液体。
步骤三:将粘稠液体吸入针筒,将针筒装入泵推装置,收集器收集由针头喷射出的针筒里的纤维;在针头与收集器之间施加25kV的电压,生成纤维状前驱体。
步骤四:收集生成的纤维状前驱体,并将纤维状前驱体放入烘箱干燥12小时后,置入马弗炉煅烧,煅烧全过程通入氮气作为保护气体,即可得到Rh金属均匀分散的碳纳米纤维。
进一步地,所述马弗炉煅烧具体过程为全程采用氮气作为保护气,以1.5℃/min的升温速率提高温度至900℃维持3h小时,之后迅速降温至室温。
如图1,所示的产物的纳米纤维直径在200 nm左右,其中金属颗粒分布均匀且大小在2.5-5.5 nm, 3.0-3.5 nm粒径占大部分。
对该纳米纤维进行电催化性能测试,如图2所示,无论酸性或碱性条件下都表现出优异的析氢性能。远超Pt/C 或非该纤维结构的Rh 纳米颗粒的效果。且经过10000次循环测试后,该催化剂依然保持了活性。
虽然本发明已以较佳实施例公开如上,但它们并不是用来限定本发明的,任何熟习此技艺者,在不脱离本发明之精神和范围内,自当可作各种变化或润饰,因此本发明的保护范围应当以本申请的权利要求保护范围所界定的为准。

Claims (2)

1.一种用电催化析氢的低含量高分散的Rh纳米纤维的制备,其特征在于:包括以下步骤:
步骤一:在烧杯中加入摩尔比为1比4的植酸,将0.01g摩尔质量为209.26g/mol的RhCl3放入烧杯中;
步骤二:当烧杯中的RhCl3与植酸相互完全溶解后,加入10mL的DMF溶液后,50度水浴加热搅拌过程中加入1gPAN. 待全部溶解后形成粘稠液体;
步骤三:将粘稠液体吸入针筒,将针筒装入泵推装置,收集器收集由针头喷射出的针筒里的纤维;在针头与收集器之间施加25kV的电压,生成纤维状前驱体;
步骤四:收集生成的纤维状前驱体,并将纤维状前驱体放入烘箱干燥12小时后,置入马弗炉煅烧,煅烧全过程通入氮气作为保护气体;即可得到Rh金属均匀分散的碳纳米纤维。
2.根据权利要求1所述的一种用电催化析氢的低含量高分散的Rh纳米纤维的制备,其特征在于:所述马弗炉煅烧具体过程为全程采用氮气作为保护气,以1.5℃/min的升温速率提高温度至900℃维持3h小时,之后迅速降温至室温。
CN202010035467.5A 2020-01-14 2020-01-14 一种用电催化析氢的低含量高分散的Rh纳米纤维的制备 Pending CN111185157A (zh)

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Citations (1)

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Publication number Priority date Publication date Assignee Title
CN106140162A (zh) * 2016-07-08 2016-11-23 浙江理工大学 一种用于电催化析氢的铜纳米粒子/碳纳米纤维杂化材料的制备方法

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106140162A (zh) * 2016-07-08 2016-11-23 浙江理工大学 一种用于电催化析氢的铜纳米粒子/碳纳米纤维杂化材料的制备方法

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
M. STRECKOVA, ET AL: "Nickel and nickel phosphide nanoparticles embedded in electrospun carbon fibers as favourable electrocatalysts for hydrogen evolution", 《CHEMICAL ENGINEERING JOURNAL》, vol. 303, 1 June 2016 (2016-06-01), pages 167 - 181, XP029708911, DOI: 10.1016/j.cej.2016.05.147 *
M. STRECKOVA, ET AL: "Novel electrocatalysts for hydrogen evolution based on carbon fibers modified by cobalt phosphides", 《APPLIED SURFACE SCIENCE》, vol. 507, 14 December 2019 (2019-12-14), pages 4, XP086094535, DOI: 10.1016/j.apsusc.2019.144927 *
QING QIN,ET AL: "Low Loading of RhxP and RuP on N, P Codoped Carbon as Two Trifunctional Electrocatalysts for the Oxygen and Hydrogen Electrode Reactions", 《ADV. ENERGY MATER.》, vol. 2018, 31 December 2018 (2018-12-31), pages 1 - 3 *

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