CN105688941B - Species CuS @ MoS heterogeneous catalytic nano-matrix material and the water electrolysis hydrogen production applications - Google Patents

Species CuS @ MoS heterogeneous catalytic nano-matrix material and the water electrolysis hydrogen production applications Download PDF

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CN105688941B
CN105688941B CN 201610020477 CN201610020477A CN105688941B CN 105688941 B CN105688941 B CN 105688941B CN 201610020477 CN201610020477 CN 201610020477 CN 201610020477 A CN201610020477 A CN 201610020477A CN 105688941 B CN105688941 B CN 105688941B
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mos
nano
cus
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CN105688941A (en )
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汪乐余
郭冲
徐骏
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北京化工大学
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies or technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30Hydrogen technology
    • Y02E60/36Hydrogen production from non-carbon containing sources
    • Y02E60/366Hydrogen production from non-carbon containing sources by electrolysis of water

Abstract

本发明公开了种CuS@MoS异质纳米骨架材料及其催化电解水制氢的应用。 The present invention discloses the use of a heterogeneous species CuS @ MoS nano-matrix catalytic materials and the water electrolysis hydrogen production. 本发明采用热分解前驱体的方法,以CuS为支撑骨架,通过MoS刻蚀得到了表面富含活性边缘位点、具有极高活性和稳定性的超小的环形的CuS@MoS异质纳米框结构,除去其表面配体后和C粉混合,然后涂覆在电极上应用于催化电解水制氢。 The present invention is the method of thermal decomposition of the precursor in order to support the skeleton CuS obtained ultra-small annular edge surface active sites enriched with high activity and stability of the nano-hetero CuS @ MoS frame by etching MoS structure, which after removal of surface ligands and C powder were mixed and then applied to the coating on the catalytic water electrolysis hydrogen electrode. 作为种非贵金属催化剂,由于其具有很好的结晶性且富含MoS活性边缘位点,能降低水中氢气的析出电位,可以替代铂成为有效的电催化析氢材料,当电流密度达到10mA/cm和200mA/cm的时候,过电势仅分别为133mV和206mV,在报道过的MoS纳米催化剂中展现出最高活性和高稳定性。 Non-noble metal catalysts as a seed, because of its good crystallinity and the active edge MoS rich sites, to reduce the hydrogen evolution potential in water, can be an effective alternative to platinum electrical materials for hydrogen evolution, when the current density of 10mA / cm and 200mA / cm when only overpotential of 133mV and 206mV, respectively, exhibit high stability and the highest activity reported in the MoS nano catalyst. 由于溶剂热法可以进行合理的扩展,本发明为大量发展其它的非贵金属硫化物催化剂开辟了新的道路。 Since the solvothermal method can be reasonably extended, the present invention is the development of a large number of other non-noble metal sulphide catalysts opened a new path.

Description

—种Cu7S4@M〇S2异质纳米骨架材料及其催化电解水制氢的应用 - Species Cu7S4 @ M〇S2 heterogeneous catalytic nano-matrix material and the water electrolysis hydrogen production applications

技术领域 FIELD

[0001]本发明属于纳米材料制备技术领域,特别涉及一种具有极高催化析氢活性的Cu7S4@M〇S2纳米异质结构骨架材料,可以应用于催化电解水产氢。 [0001] The present invention belongs to the technical field of the preparation of nanomaterials, in particular, relates to a nano-matrix Cu7S4 @ M〇S2 heterostructure material having a very high catalytic activity for hydrogen evolution, it can be applied to catalyze the electrolytic hydrogen production.

背景技术 Background technique

[0002] 作为电解水的基本步骤的析氢反应在实际运用中需要有效和低成本的催化剂达至IJ快速的动力学过程。 [0002] As the basic steps of the electrolysis of water, hydrogen evolution reaction in practical use and low cost requires effective IJ catalyst to achieve fast kinetics. 一直以来,Pt被认为是活性最好的电解水析氢催化剂,然而它的低含量和昂贵的价格限制了它的大范围应用。 All along, Pt is considered to be the best active hydrogenation catalyst for water electrolysis, but its high price and low content limits its wide range of applications. 作为一个很有前景的低廉的替代Pt的析氢催化剂,纳米结构的MoS2得到了广泛研宄。 As a promising alternative to hydrogen evolution catalyst Pt is low, MoS2 nanostructures widely study based. 迄今为止,很多研宄者通过大量的实验和计算证实了层状的M〇S2的催化活性位于它的边缘位点,而位于边缘的不饱和S原子在催化析氢反应中起到了重要作用。 To date, many are demonstrated by the study based on a large number of experiments and calculations of the catalytically active layer located at its edge M〇S2 site, and at the edge of an unsaturated S atoms play an important role in the hydrogen evolution reaction. 正是基于这个原因,研宄者尝试了各种方法去提高纳米MoS2暴露的活性位点数目。 It is for this reason, research traitor who tried various methods to increase the number of nano MoS2 exposed active sites.

[0003] 近来由于无定形的M〇S2包含很多的活性不饱和S原子,能够有效催化析氢反应,因此吸引了科学家的关注。 [0003] Recently, because of the amorphous active M〇S2 contains many unsaturated S atoms, which can effectively catalyze hydrogen evolution reaction, thus attracting the attention of scientists. 然而,无定形的S原子具有很差的结晶性,导致了它在酸中具有相对高的溶解性和差的电化学稳定性,从而限制了它的实际应用。 However, amorphous S atom having poor crystallinity, which leads to a relatively high solubility and poor electrochemical stability in an acid, thus limiting its practical applications. 因此,为了同时达到高的析氢活性和长时间稳定性,发展一个既有丰富的活性边缘位点又具有很高的结晶性的M〇S2纳米催化剂是一个行之有效的方法。 Accordingly, in order to simultaneously achieve a high long-term stability and activity of hydrogen evolution, a development of both rich active site edge and having a high crystallinity M〇S2 nano catalyst it is an effective method.

发明内容 SUMMARY

[0004]本发明为满足能源工业领域的需求,特别设计一种具有极高催化产氢活性和稳定性的超小的圆环形Cu7S4@M〇S2异质纳米框结构,可以应用于催化电解水制氢。 Ultra small circular [0004] The present invention is to meet the need for energy industry, in particular, to design a high catalytic activity and stability of the hydrogen production Cu7S4 @ M〇S2 nano heterostructure frame structure, may be applied to the catalytic electrolysis hydrogen production from water.

[0005]本发明采用热分解前驱体的方法,以CU7S4为支撑骨架,通过MoS2刻蚀得到了表面富含活性边缘位点、具有极高活性和稳定性的超小的环形的CU7S4@M〇S2异质纳米框结构,除去其表面配体后和C粉混合,然后涂覆在电极上应用于催化电解水制氢。 [0005] The present invention employs the thermal decomposition of the precursor, as the support frame to CU7S4 obtained ultra-small annular edge surface active sites enriched with high activity and stability CU7S4 @ M〇 by etching MoS2 S2 nano-hetero structure frame, which rear surface ligands removal and C powder were mixed and then applied to the coating on the catalytic water electrolysis hydrogen electrode.

[0006]本发明所述的Cu7S4@M〇S2异质纳米骨架材料的制备方法,其具体步骤如下: [0006] The production method according to the present invention Cu7S4 @ M〇S2 heterogeneous nano-matrix material, the specific steps are as follows:

[0007] a •将4_6ml油胺和4-6ml十八稀搅拌混合,然后加入0.1-0.5mmol的Cu的前驱体和2〇-140mg的S的前驱体,在190-21(TC保持10-20min后,继续加热到260-31(TC时加入〇.2-lmmol的Mo的前驱体和0.4-2mmol的S的前驱体,在275-300°C保持5-30min; [0007] a • 4_6ml oleylamine and the lean 4-6ml eighteen stirred and mixed, followed by addition of Cu 0.1-0.5mmol of the precursor and the precursor of the S-140mg 2〇 in 190-21 (TC holding 10- after 20min, the precursor to heating continued 260-31 (added 〇.2-lmmol precursor of Mo and S TC of 0.4-2mmol maintain 5-30min at 275-300 ° C;

[0008] b •反应自然冷却后,取出反应液5000-15000转/分离心5-20min,将沉淀分散在正己烷中; After [0008] b • the reaction allowed to cool, the reaction liquid taken out 5000-15000 rev / heart 5-20min separation, the precipitate was dispersed in n-hexane;

[0009] C.将l-10mg的C粉分散到正己烷中,然后加入到步骤b的分散液中,超声30-90min 后,5000-15000转/分离心5-20min,得到负载在C粉上的纳米晶; [0009] C. The C l-10mg of the powder dispersed in n-hexane, and then added to the dispersion of step b, the ultrasonic 30-90min, 5000-15000 rpm / 5-20min centrifuged, the load C to obtain powder the nanocrystals;

[0010] d •将负载在C粉上的纳米晶分散到20-50mL的醋酸中,40-8(TC下搅拌10-20h除去表面配体,5000_15〇00转/分离心5_2〇min,得到Cu7S4@MoS2异质纳米骨架材料,将其分散到水和异丙醇的混合溶剂中。 [0010] d • C will be supported on the powder is dispersed nanocrystals 20-50mL acetate and stirred (at 40-8 TC 10-20h remove surface ligands, 5000_15〇00 rpm / 5_2〇min centrifuged to give Cu7S4 @ MoS2 nano-matrix heterogeneous material, which is dispersed in a mixed solvent of water and isopropanol.

[0011] 所述的Cu的前驱体选自氯化铜、乙酰丙酮铜、硝酸铜。 [0011] The Cu precursor is selected from copper chloride, copper acetylacetonate, copper nitrate.

[0012]所述的Mo的前驱体选自:Mo (CO) 6、Mo (N〇3) 3 • H2〇、M〇C15。 [0012] The Mo precursor is selected from the group: Mo (CO) 6, Mo (N〇3) 3 • H2〇, M〇C15.

[0013]所述的S的前驱体选自:十二硫醇,S粉,N,N-二丁基二硫代甲酸。 Precursor [0013] S is selected according to: dodecyl mercaptan, S powder, N, N- dibutyl dithiocarbamate.

[0014] 将上述制备得到的CmS4@M〇S2异质纳米骨架材料应用于催化电解水制氢。 [0014] The above prepared CmS4 @ M〇S2 obtained nano-matrix material is applied to a heterogeneous catalytic water electrolysis hydrogen production. 具体反应条件:步骤b得到的分散液中加入全氟磺酸溶液,然后涂覆在玻碳电极上,干燥后作为工作电极,在0.5M的H2S〇4溶液中,氮气保护条件下,以玻碳棒作为对电极,饱和甘汞为参比电极,以三电极体系进行催化电解水制氢反应。 Specific reaction conditions: Nafion dispersion solution obtained in step b was added, and then on the glassy carbon electrode as a working electrode, 0.5M solution in H2S〇4, the coating was dried under nitrogen, protected conditions to glass carbon rod as a counter electrode, a saturated calomel electrode as the reference, to the three-electrode system for the catalytic reaction of water electrolysis hydrogen production.

[0015] 本发明的有益效果:本发明公开了一种简单的方法得到具有环状的Cu7S4@M〇S2异质纳米骨架材料。 [0015] Advantageous Effects of Invention: The present invention discloses a simple method to obtain Cu7S4 @ M〇S2 heterogeneous material having a nano-matrix cyclic. 作为一种非贵金属催化剂,由于其具有很好的结晶性且富含M〇S2活性边缘位点,能降低水中氢气的析出电位,可以替代铂成为有效的电催化析氢材料,当电流密度达到1011^/〇112和20011^/〇112的时候,过电势仅分别为13311^和20611^,在报道过的舫32纳米催化剂中展现出最高活性和高稳定性。 As a non-noble metal catalysts, because of its good crystallinity and the active edge M〇S2 rich sites, to reduce the hydrogen evolution potential in water, it can be an effective alternative to platinum electrical materials for hydrogen evolution, when the current density reaches 1011 ^ / ^ 20011 〇112 and / 〇112 when overpotential were only 13311 and 20611 ^ ^, reported in the fang 32 nanocatalyst highest activity and exhibits high stability. 由于溶剂热法可以进行合理的扩展,本发明为大量发展其它的非贵金属硫化物催化剂开辟了新的道路。 Since the solvothermal method can be reasonably extended, the present invention is the development of a large number of other non-noble metal sulphide catalysts opened a new path.

附图说明 BRIEF DESCRIPTION

[0016] 图1:Cu7S4〇MoS2异质纳米骨架材料的电镜图、高分辨电镜图和相应的元素面扫面图片。 [0016] FIG. 1: FIG Cu7S4〇MoS2 heterogeneous electron microscopy nano-matrix material, and HREM corresponding elements in FIG scan plane image plane.

具体实施方式 detailed description

[0017] 实施例1 [0017] Example 1

[0018] a•将6ml油胺(0AM)、4ml十八炼(0DE)搅拌混合,加入〇• lmmol的Cu (N〇3) 2 • 3H2〇和20mg N,N-二丁基-二硫代甲酸,在190°C下保持15min,以合成得到的CU7S4纳米颗粒为骨架, 继续加热在300°C时注射0• 2mmo 1的MoCls和0 • 4mmol的S粉,恒温在300°C,保持20min; [0018] a • The 6ml oleylamine (0AM), 4ml eighteen Lian (0DE) stirring and mixing, • lmmol square of Cu (N〇3) 2 • 3H2〇 and 20mg N, N- dibutyl - disulfide generation of formic acid, kept at 190 ° C 15min, to CU7S4 nanoparticle synthesis obtained as a skeleton, and heating was continued injection at 300 ° C 0 • the 2mmo 1 MoCls and S powder 0 • 4mmol and thermostated at 300 ° C, holding 20min;

[0019] b.反应自然冷却后,取出反应液离心(12000转/分)10min,保留沉淀用正己烷溶解收集; . [0019] b After the reaction allowed to cool, the reaction liquid taken out was centrifuged (12,000 rev / min) 10min, to retain the precipitate collected was dissolved with n-hexane;

[0020] C.将4mg的C粉分散到正己烷中,然后加入到步骤b的分散液中,超声80min后,离心(12000转/分)lOmin得负载在C粉上的纳米晶; [0020] C. The C powder 4mg dispersed into n-hexane, and then added to the dispersion of step b, the ultrasonic 80min, centrifuged (12,000 rev / min) to give lOmin supported on nanocrystalline powder C;

[0021] d.将负载在C粉上的纳米晶分散到40mL的醋酸中,7(TC下搅拌15h除去表面配体, 离心(12000转/分)15min,得到Cu7S4@M〇S2异质纳米骨架材料,将其重新分散到1000ul体积比为1:1的水和异丙醇的混合溶剂中。 [0021] d. C powder will be supported on the nanocrystal dispersed in 40mL acetic acid was stirred for 7 (TC 15h under surface ligand was removed, centrifuged (12,000 rev / min) 15min, to give Cu7S4 @ M〇S2 hetero nano reinforcing material, it redispersed to 1000ul volume ratio of 1: a mixed solvent of water and isopropanol 1.

[0022]将上述制备得到的CU7S4麵〇S2异质纳米骨架材料应用于催化电解水制氢。 [0022] The above-prepared surface 〇S2 CU7S4 obtained nano-matrix material is applied to a heterogeneous catalytic water electrolysis hydrogen production. 具体反应条件:步骤b得到的分散液中加入30ul的5wt%全氟磺酸溶液,然后取其中87ul涂覆在玻碳电极(电极直径为3mm)上,干燥后作为工作电极,在0.5M H2S04溶液中,并持续通N2的条件下,以玻碳棒作为对电极,饱和甘汞为参比电极,在〇-_〇• 7v的电位条件下测试其线性伏安曲线(LSV),利用it曲线测试它的稳定性。 Specific reaction conditions: the dispersion obtained in step b was added 30ul of 5wt% Nafion solution, which then take 87ul coated on a glassy carbon electrode (electrode diameter 3mm), and dried as a working electrode in 0.5M H2S04 solution under N2 and continues through to glassy carbon rod as a counter electrode and saturated calomel as reference electrode, linear voltammograms tested (the LSV) in the square-_〇 • 7v potential conditions, the use of it profile test its stability.

Claims (5)

  1. 1.一种CmSWMoS2异质纳米骨架材料的制备方法,其特征在于,其具体步骤如下: a •将4-6ml油胺和4-6ml十八知揽泮混合,然后加入〇. 1—〇. 5mmol的Cu的前驱体和20-140mg的S的前驱体,在190-210°C保持10-20min后,继续加热到260-3KTC时加入〇.2_lmm〇l 的Mo的前驱体和0.4-2mmol的S的前驱体,在275-300°C保持5-30min; b •反应自然冷却后,取出反应液5000-15000转/分离心5-20min,将沉淀分散在正己烷中。 1. A method for preparing nano CmSWMoS2 heterogeneous reinforcing materials, wherein the specific steps are as follows:. A • The 4-6ml 4-6ml eighteen known oleylamine and embrace Pan mixed, followed by addition of 1- billion square. 〇.2_lmm〇l added when the Cu precursor precursor 5mmol and 20-140mg of S after 10-20min maintained at 190-210 ° C, heating was continued to 260-3KTC Mo precursor and 0.4-2mmol S is a precursor, held at 275-300 ° C 5-30min; b • after the reaction was allowed to cool, the reaction liquid taken out 5000-15000 rpm / 5-20min centrifuged, the precipitate was dispersed in n-hexane.
  2. 2. 根据权利要求1所述的制备方法,其特征在于,所述的Cu的前驱体选自氯化铜、乙酰丙酮铜、硝酸铜。 2. The production method according to claim 1, wherein the Cu precursor is selected from copper chloride, copper acetylacetonate, copper nitrate.
  3. 3. 根据权利要求1所述的制备方法,其特征在于,所述的Mo的前驱体选自:Mo (C0) 6、Mo (N〇3) 3 • H2CKM0CI5。 3. The production method according to claim 1, wherein said precursor is selected from Mo: Mo (C0) 6, Mo (N〇3) 3 • H2CKM0CI5. on
  4. 4. 根据权利要求1所述的制备方法,其特征在于,所述的S的前驱体选自:十二硫醇,S 粉,N,N-二丁基二硫代甲酸。 4. The production method according to claim 1, wherein said precursor is selected from S,: dodecyl mercaptan, powder S, N, N- dibutyl dithiocarbamate. 从到促仆由把 From the servant to promote the
  5. 5.根据权利要求1所述的制备方法制备得到的Cu7S4@MoS2异质纳米骨架材料惟化电用牛水制氢的应用。 The heterogeneous Cu7S4 @ MoS2 nano-matrix material prepared according to a preparation obtained by the method of electrical Bovine water but by hydrogen claims.
CN 201610020477 2016-01-13 2016-01-13 Species CuS @ MoS heterogeneous catalytic nano-matrix material and the water electrolysis hydrogen production applications CN105688941B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
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US7125820B2 (en) * 2002-07-31 2006-10-24 Ballard Power Systems Inc. Non-noble metal catalysts for the oxygen reduction reaction
CN101658792A (en) * 2009-09-17 2010-03-03 大连理工大学 Preparation method of transition metal sulfide catalytic material and catalytic application thereof
CN103011292A (en) * 2012-12-04 2013-04-03 北京大学 Nolybdenum disulfide nanometer particle, preparation method and application thereof
CN103060839A (en) * 2011-10-20 2013-04-24 新奥科技发展有限公司 Low temperature preparation method for hydrogen evolution cathode material and application thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7125820B2 (en) * 2002-07-31 2006-10-24 Ballard Power Systems Inc. Non-noble metal catalysts for the oxygen reduction reaction
CN101658792A (en) * 2009-09-17 2010-03-03 大连理工大学 Preparation method of transition metal sulfide catalytic material and catalytic application thereof
CN103060839A (en) * 2011-10-20 2013-04-24 新奥科技发展有限公司 Low temperature preparation method for hydrogen evolution cathode material and application thereof
CN103011292A (en) * 2012-12-04 2013-04-03 北京大学 Nolybdenum disulfide nanometer particle, preparation method and application thereof

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