CN116425199A - 一种二硫化钼纳米卷电催化剂的制备方法 - Google Patents
一种二硫化钼纳米卷电催化剂的制备方法 Download PDFInfo
- Publication number
- CN116425199A CN116425199A CN202310483470.7A CN202310483470A CN116425199A CN 116425199 A CN116425199 A CN 116425199A CN 202310483470 A CN202310483470 A CN 202310483470A CN 116425199 A CN116425199 A CN 116425199A
- Authority
- CN
- China
- Prior art keywords
- molybdenum disulfide
- electrocatalyst
- molybdenum
- disulfide nano
- nano
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 68
- 239000010411 electrocatalyst Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000002135 nanosheet Substances 0.000 claims abstract description 37
- 239000006185 dispersion Substances 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 13
- 239000001257 hydrogen Substances 0.000 claims abstract description 13
- 238000004108 freeze drying Methods 0.000 claims abstract description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 238000009835 boiling Methods 0.000 claims abstract description 6
- 239000003960 organic solvent Substances 0.000 claims abstract description 6
- 238000010791 quenching Methods 0.000 claims abstract description 6
- 230000000171 quenching effect Effects 0.000 claims abstract description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 18
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 9
- 230000007547 defect Effects 0.000 claims description 7
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical group [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 4
- GAEKPEKOJKCEMS-UHFFFAOYSA-N gamma-valerolactone Chemical compound CC1CCC(=O)O1 GAEKPEKOJKCEMS-UHFFFAOYSA-N 0.000 claims description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 3
- 229940087305 limonene Drugs 0.000 claims description 3
- 235000001510 limonene Nutrition 0.000 claims description 3
- 229910052723 transition metal Inorganic materials 0.000 claims description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical group [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 239000011651 chromium Substances 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 235000011187 glycerol Nutrition 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 16
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 13
- 239000000843 powder Substances 0.000 description 9
- 238000005406 washing Methods 0.000 description 9
- MZRVEZGGRBJDDB-UHFFFAOYSA-N N-Butyllithium Chemical compound [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 description 8
- 239000012299 nitrogen atmosphere Substances 0.000 description 7
- 239000002904 solvent Substances 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 238000009830 intercalation Methods 0.000 description 3
- 230000002687 intercalation Effects 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229940011182 cobalt acetate Drugs 0.000 description 1
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- YJVFFLUZDVXJQI-UHFFFAOYSA-L palladium(ii) acetate Chemical compound [Pd+2].CC([O-])=O.CC([O-])=O YJVFFLUZDVXJQI-UHFFFAOYSA-L 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Inorganic Chemistry (AREA)
- Metallurgy (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
本发明公开了一种二硫化钼纳米卷电催化剂的制备方法,属于化工新材料催化领域,该方法是在高缺陷态的二硫化钼纳米片分散液中滴加高沸点有机溶剂,超声分散后,经过液氮冷淬、低温冻干后,获得具有卷曲形貌的二硫化钼纳米卷;本发明的制备工艺简单,所得二硫化钼纳米卷电催化剂结构稳定,电化学活性面积大,具有优异的电催化性能,在电催化析氢等领域具有良好的应用前景。
Description
技术领域
本发明涉及一种制备二硫化钼纳米卷电催化剂的方法,属于化工新材料催化领域。
背景技术
二硫化钼价格便宜,储量丰富,是目前最具前景的电催化析氢反应(HER)催化剂之一。目前,高HER活性的二硫化钼材料多为二维纳米片状结构,将二维纳米片曲卷形成一维纳米卷结构可以暴露更多活性位点,防止材料堆叠团聚,并且可通过纳米卷结构具有的表面卷曲应力提高催化剂的本征活性。然而,常规的原位生长法难以直接生长出具有一维纳米卷结构的二硫化钼,并且制备耗时长、操作繁杂、限制了二硫化钼电催化剂的发展。
发明内容
针对现有二硫化钼纳米卷电催化剂的制备方法存在的问题,本发明提供了一种制备二硫化钼纳米卷电催化剂的方法,本发明以薄层二硫化钼纳米片分散液为前驱体,通过金属掺杂获得高缺陷态的二硫化钼纳米片,随后在二硫化钼纳米片分散液中滴加一定比例的高沸点有机溶剂,经过液氮冷淬,低温冻干处理,得到具有卷曲形貌的二硫化钼纳米卷。
所述高缺陷态的二硫化钼纳米片为金属掺杂二硫化钼纳米片,尺寸为1~16μm,厚度为0.67~10.0nm,硫化钼的相态包括2H相、1T相、2H与1T混合相态,硫化钼的硫空位缺陷浓度为钼原子的5~35%,金属原子掺杂量为硫化钼摩尔量的1~20%;
高缺陷态的二硫化钼纳米片采用常规方法制得,方法包括但不限于下述方法,例如高缺陷态的二硫化钼纳米片分散液是将块状二硫化钼(尺寸为12~16μm)置于正丁基锂溶液中,在10~30℃、氮气气氛、超声频率为80~100Hz下处理3~10h,正己烷洗涤,干燥,加入去离子水自动剥离,离心洗涤得到片层完整的二维纳米片分散液,然后在分散液中加入金属盐,在惰性气氛下搅拌反应后,水洗涤除去多余金属源,获得高缺陷态的二硫化钼纳米片,再加去离子水分散后获得浓度为0.1~2mg/mL分散液;其中所掺杂的金属元素为钯,钴,锌,铂,铬等ⅢB族到VⅢ族,ⅠB和ⅡB族过渡金属元素。
所述高沸点有机溶剂为N-甲基吡咯烷酮、二甲基亚砜、柠檬烯、γ-戊内酯、甘油、N,N-二甲基甲酰胺、二甲基乙酰胺或碳酸丙烯酯等有机溶剂中的一种或几种,高沸点有机溶剂添加量为二硫化钼分散液体积的0.1~5%。
所述液氮冷淬时间10~30min。
所述低温冻干的冷阱温度为-45~-80℃,冻干时间12~36h。
本发明的有益效果如下:
本发明方法的制备工艺简单,耗时短,结构易调控;通过低温冻干法直接制备出的二硫化钼纳米卷,不仅结构稳定,电化学活性面积大,还表现出优异的电催化活性。
附图说明
图1为实施例1制备的二硫化钼纳米片的SEM图;
图2为实施例1制备的金属掺杂的二硫化钼纳米片的球差扫描透射电镜图;
图3为实施例1制备的金属掺杂的二硫化钼纳米卷的SEM图;
图4为实施例1制备的金属掺杂的二硫化钼纳米片和二硫化钼纳米卷的电催化析氢LSV曲线;
图5为实施例2二硫化钼纳米卷的电催化析氢LSV曲线;
图6为实施例3二硫化钼纳米卷的电催化析氢LSV曲线。
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,本发明保护范围不局限于所述内容。实施例中方法如无特殊说明,均为常规方法,试剂如无特殊说明均为常规市售试剂或按常规方法配制的试剂。
实施例1
1、称取1g二硫化钼粉末(12~16μm)、10 mL以正己烷为溶剂的正丁基锂溶液(2.5M,溶剂为正己烷,市购),于氮气氛围的史莱克管中反应,保持超声频率为80Hz,温度27℃,插层3h后使用正己烷洗涤,氮气吹扫干燥后,加入去离子水剥离,离心洗涤(依次进行3000rmp离心留沉积、加水分散、13000rmp离心留沉积、加水分散、3000rmp离心留悬浮液、13000rmp留沉积,洗至pH约等于8~9,加水分散)得到二硫化钼纳米片分散液,其中二硫化钼纳米片扫描电镜图如图1所示,从图中可以看出,块状二硫化钼被成功剥离成片层完整的二维纳米片结构;随后,在40mL浓度为1mg/mL的分散液中加入5.61mg的乙酸钯粉末,氮气气氛下常温搅拌12 h,水离心洗涤至pH=7,得到片层尺寸为2μm,厚度为0.67-2nm,1T和2H相的相态比例为3:1,缺陷浓度为32%的高缺陷态二硫化钼纳米片,其球差扫描透射电镜图见图2,从图中看出纳米片暴露出大量缺陷,在二硫化钼二维纳米片基面上可以明显看到存在大量缺陷;高缺陷态二硫化钼纳米片用水分散后,在2mL浓度1mg/mL的分散液中滴加6μL的N-甲基吡咯烷酮溶剂超声分散20min,液氮冷淬20min,冷阱温度为-80℃,冻干24h得到二硫化钼纳米卷,二硫化钼纳米卷的扫描电镜图见图3,从图中可以看出本是超薄结构的二硫化钼纳米片,在冻干后结构整体呈纤维状。
2、采用含有阳极、阴极的电解水装置,将本实施例制得二硫化钼纳米卷应用在电催化析氢反应中,以电解液为0.5M的H2SO4,在电压为0.2 ~ -1.2V下进行酸性析氢测试,结果如图4所示,硫化钼纳米卷在酸性条件下表现出优异的析氢性能。
实施例2
称取1g二硫化钼粉末(12~16μm)、10 mL以正己烷为溶剂的正丁基锂溶液(2.5M,溶剂为正己烷,市购),于氮气氛围的史莱克管中反应,保持超声频率为90Hz,温度25℃,插层4h后使用正己烷洗涤,氮气吹扫干燥后,加入去离子水剥离,离心洗涤(同实施例1)得到二硫化钼纳米片分散液,块状二硫化钼被成功剥离成片层完整的二维纳米片结构;随后,在40mL浓度为1mg/mL的分散液中加入6.9mg的乙酸钴粉末,氮气气氛下常温搅拌12 h,水离心洗涤至pH=7,得到片层尺寸为2μm,厚度为0.67~2nm,1T和2H相的相态比例为2:1,缺陷浓度为13%的高缺陷态二硫化钼纳米片;高缺陷态二硫化钼纳米片用水分散后,在2mL浓度0.5mg/mL的分散液中滴加12μL的二甲基亚砜超声分散20min,液氮冷淬30min,冷阱温度为-80℃,冻干24h得到二硫化钼纳米卷,将本实施例制得二硫化钼纳米卷应用在电催化析氢反应中,以电解液为0.5M的H2SO4,在电压为0.2 ~ -1.2V下进行酸性析氢测试,结果见图5。
实施例3
称取1g二硫化钼粉末(12~16μm)、10 mL以正己烷为溶剂的正丁基锂溶液(2.5M,溶剂为正己烷,市购),于氮气氛围的史莱克管中反应,保持超声频率为100Hz,温度20℃,插层5h后使用正己烷洗涤,氮气吹扫干燥后,加入去离子水剥离,离心洗涤(同实施例1)得到二硫化钼纳米片分散液,块状二硫化钼被成功剥离成片层完整的二维纳米片结构;随后,在40mL浓度为1mg/mL的分散液中加入11.3mg的氯化锌粉末,氮气气氛下常温搅拌12 h,水离心洗涤至pH=7,得到片层尺寸为2μm,厚度为0.67~2nm,1T和2H相的相态比例为3:1,缺陷浓度为30%的高缺陷态二硫化钼纳米片;高缺陷态二硫化钼纳米片用水分散后,在2mL浓度1.5mg/mL的分散液中滴加18μL的柠檬烯超声分散20min,液氮冷淬30min,冷阱温度为-80℃,冻干36h得到二硫化钼纳米卷,将本实施例制得二硫化钼纳米卷应用在电催化析氢反应中,以电解液为0.5M的H2SO4,在电压为0.2 ~ -1.2V下进行酸性析氢测试,结果见图6。
Claims (7)
1.一种二硫化钼纳米卷电催化剂的制备方法,其特征在于:在高缺陷态的二硫化钼纳米片分散液中滴加高沸点有机溶剂,超声分散后,经过液氮冷淬、低温冻干后,获得具有卷曲形貌的二硫化钼纳米卷。
2.根据权利要求1所述的二硫化钼纳米卷电催化剂的制备方法,其特征在于:高沸点有机溶剂为N-甲基吡咯烷酮、二甲基亚砜、柠檬烯、γ-戊内酯、甘油、N,N-二甲基甲酰胺、二甲基乙酰胺、碳酸丙烯酯中的一种或几种,高沸点有机溶剂添加量为二硫化钼分散液体积的0.1~5%。
3.根据权利要求1所述的二硫化钼纳米卷电催化剂的制备方法,其特征在于:高缺陷态的二硫化钼纳米片为金属掺杂二硫化钼纳米片,尺寸为1~16μm,厚度为0.67~10.0nm,硫化钼的相态包括2H相、1T相、2H与1T混合相态,硫化钼的硫空位缺陷浓度为钼原子的5~35%,金属原子掺杂量为硫化钼摩尔量的1~20%。
4.根据权利要求3所述的二硫化钼纳米卷电催化剂的制备方法,其特征在于:掺杂的金属元素选自ⅢB族到VⅢ族,ⅠB和ⅡB族过渡金属元素。
5.根据权利要求4所述的二硫化钼纳米卷电催化剂的制备方法,其特征在于:掺杂的金属元素选自钯、钴、锌、铂、铬。
6.根据权利要求1所述的二硫化钼纳米卷电催化剂的制备方法,其特征在于:二硫化钼分散液的浓度为0.1~2mg/mL。
7.权利要求1-6任一项所述的二硫化钼纳米卷电催化剂的制备方法制得的二硫化钼纳米卷电催化剂在析氢反应中的应用。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202310483470.7A CN116425199A (zh) | 2023-05-04 | 2023-05-04 | 一种二硫化钼纳米卷电催化剂的制备方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202310483470.7A CN116425199A (zh) | 2023-05-04 | 2023-05-04 | 一种二硫化钼纳米卷电催化剂的制备方法 |
Publications (1)
Publication Number | Publication Date |
---|---|
CN116425199A true CN116425199A (zh) | 2023-07-14 |
Family
ID=87090771
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202310483470.7A Pending CN116425199A (zh) | 2023-05-04 | 2023-05-04 | 一种二硫化钼纳米卷电催化剂的制备方法 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN116425199A (zh) |
Citations (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104445153A (zh) * | 2013-09-13 | 2015-03-25 | 中国科学院兰州化学物理研究所 | 一种由石墨烯宏量制备炭纳米卷的方法 |
WO2017062736A1 (en) * | 2015-10-08 | 2017-04-13 | Board Of Trustees Of The University Of Illinois | Structured molybdenum disulfide materials for electrocatalytic applications |
CN106992319A (zh) * | 2017-02-22 | 2017-07-28 | 东莞市联洲知识产权运营管理有限公司 | 一种高倍率性能的钠离子电池的制备方法 |
CN108217608A (zh) * | 2017-12-27 | 2018-06-29 | 中国科学院化学研究所 | 二维材料纳米卷及其制备方法和应用 |
CN108671942A (zh) * | 2018-04-04 | 2018-10-19 | 山东大学 | 一种催化剂用二硫化钼及其制备方法和应用 |
US20190003064A1 (en) * | 2017-06-29 | 2019-01-03 | National Technology & Engineering Solutions Of Sandia, Llc | Crumpled Transition Metal Dichalcogenide Sheets |
CN113562766A (zh) * | 2020-04-28 | 2021-10-29 | 中国科学院化学研究所 | 改性金属硫属化合物纳米片及其制备方法和应用 |
CN113753955A (zh) * | 2021-10-19 | 2021-12-07 | 天津大学 | 一种具有褶皱的二硫化钼纳米片、其制备方法及用途 |
CN114405521A (zh) * | 2020-10-12 | 2022-04-29 | 武汉理工大学 | 一种缺陷丰富的掺锌二硫化钼纳米片析氢电催化剂的制备方法 |
US20220143585A1 (en) * | 2020-11-10 | 2022-05-12 | National Technology & Engineering Solutions Of Sandia, Llc | Electrocatalyst comprising a crumpled transition metal dichalcogenide support loaded with monodispersed metal nanoparticles |
CN114671404A (zh) * | 2022-03-23 | 2022-06-28 | 昆明理工大学 | 一种MoS2催化剂在H2S原位诱导下催化甲烷重整制氢的方法 |
CN115029724A (zh) * | 2022-06-09 | 2022-09-09 | 武汉科技大学 | 一种金属掺杂2h相二硫化钼电催化剂的制备方法及其应用 |
-
2023
- 2023-05-04 CN CN202310483470.7A patent/CN116425199A/zh active Pending
Patent Citations (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104445153A (zh) * | 2013-09-13 | 2015-03-25 | 中国科学院兰州化学物理研究所 | 一种由石墨烯宏量制备炭纳米卷的方法 |
WO2017062736A1 (en) * | 2015-10-08 | 2017-04-13 | Board Of Trustees Of The University Of Illinois | Structured molybdenum disulfide materials for electrocatalytic applications |
CN106992319A (zh) * | 2017-02-22 | 2017-07-28 | 东莞市联洲知识产权运营管理有限公司 | 一种高倍率性能的钠离子电池的制备方法 |
US20190003064A1 (en) * | 2017-06-29 | 2019-01-03 | National Technology & Engineering Solutions Of Sandia, Llc | Crumpled Transition Metal Dichalcogenide Sheets |
CN108217608A (zh) * | 2017-12-27 | 2018-06-29 | 中国科学院化学研究所 | 二维材料纳米卷及其制备方法和应用 |
CN108671942A (zh) * | 2018-04-04 | 2018-10-19 | 山东大学 | 一种催化剂用二硫化钼及其制备方法和应用 |
CN113562766A (zh) * | 2020-04-28 | 2021-10-29 | 中国科学院化学研究所 | 改性金属硫属化合物纳米片及其制备方法和应用 |
CN114405521A (zh) * | 2020-10-12 | 2022-04-29 | 武汉理工大学 | 一种缺陷丰富的掺锌二硫化钼纳米片析氢电催化剂的制备方法 |
US20220143585A1 (en) * | 2020-11-10 | 2022-05-12 | National Technology & Engineering Solutions Of Sandia, Llc | Electrocatalyst comprising a crumpled transition metal dichalcogenide support loaded with monodispersed metal nanoparticles |
CN113753955A (zh) * | 2021-10-19 | 2021-12-07 | 天津大学 | 一种具有褶皱的二硫化钼纳米片、其制备方法及用途 |
CN114671404A (zh) * | 2022-03-23 | 2022-06-28 | 昆明理工大学 | 一种MoS2催化剂在H2S原位诱导下催化甲烷重整制氢的方法 |
CN115029724A (zh) * | 2022-06-09 | 2022-09-09 | 武汉科技大学 | 一种金属掺杂2h相二硫化钼电催化剂的制备方法及其应用 |
Non-Patent Citations (2)
Title |
---|
XIAOPING HUANG ET AL.: "Organic Solvent-Assisted Lyophilization: A Universal Method of Preparing Two-Dimensional Material Nanoscrolls", 《ACS OMEGA》, vol. 4, no. 4, 24 April 2019 (2019-04-24), pages 7426 * |
王娜 等: "二硫化钼基纳米材料在电催化制氢中的研究进展", 《当代化工》, vol. 49, no. 12, 28 December 2020 (2020-12-28) * |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Liu et al. | Methanol electro-oxidation on mesocarbon microbead supported Pt catalysts | |
Du et al. | The effect of Nafion ionomer loading coated on gas diffusion electrodes with in-situ grown Pt nanowires and their durability in proton exchange membrane fuel cells | |
WO2017101132A1 (zh) | 一种有序化膜电极及其制备和应用 | |
CN109841854A (zh) | 一种氮掺杂碳载单原子氧还原催化剂及其制备方法 | |
CN109921041B (zh) | 一种非贵金属氮掺杂空心碳纳米管电催化剂的制备及应用 | |
CN112968185B (zh) | 植物多酚改性的超分子网络框架结构锰基纳米复合电催化剂的制备方法 | |
CN110504456B (zh) | 一种基于氮氧掺杂球/片多孔碳材料的氧还原电极及其制备方法和应用 | |
CN110212204B (zh) | 一种碳纳米片支撑型燃料电池正极材料及其制备方法和应用 | |
CN113036165B (zh) | 一种氮硫掺杂的缺陷化碳纳米管及其制备方法 | |
CN108336292B (zh) | 一种电极及其制备方法和一种碳纳米管及其应用 | |
CN113410473B (zh) | 基于壳聚糖修饰纤维素气凝胶的铁镍多酚网络纳米复合碳材料电催化剂及其制备方法 | |
CN111342063A (zh) | 一种用于氧还原反应的二氧化锰负载氮硫双掺杂石墨烯催化剂、制备方法及应用 | |
CN109585860A (zh) | 一种硫掺杂氧化钴与硫、氮、氧掺杂碳原位复合电极的制备方法 | |
CN116425199A (zh) | 一种二硫化钼纳米卷电催化剂的制备方法 | |
Xiao et al. | CuGeO3 micro-nanomaterial as Electrocatalyst for hydrogen evolution reaction | |
Du et al. | Pulsed electrochemical deposition of Pt NPs on polybenzimidazole-CNT hybrid electrode for high-temperature proton exchange membrane fuel cells | |
CN112023929B (zh) | 一种过渡金属双氢氧化物纳米薄膜与碳纳米管复合材料的制备方法及应用 | |
CN112701307A (zh) | 用于质子膜燃料电池的双mof连接结构纳米复合电催化剂及其制备方法 | |
CN111430729A (zh) | 一种钨酸钴/二硫化钨锌空电池催化剂的制备方法 | |
CN112421060B (zh) | 一种氮掺杂硫化亚铁氧还原催化剂材料及其制备应用 | |
CN113184920B (zh) | NiCo2O4-Ti3C2三维纳米花结构复合材料的制备方法及应用 | |
CN111389431B (zh) | 一种电解水制氢用片状催化剂CoCuPS及其制备方法 | |
CN115000426B (zh) | 一种二维碳化钛负载的双组份高效锌空气电池催化剂及其制备方法和应用 | |
CN113603160B (zh) | 球状Cu-Ni-S复合纳米材料及其制备方法和应用 | |
CN118117105A (zh) | 一种高比表面积多孔碳基铂催化剂及其制备方法和应用 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination |