CN111039332A - 一种多功能双层纳米线层状复合材料的制备方法及其应用 - Google Patents
一种多功能双层纳米线层状复合材料的制备方法及其应用 Download PDFInfo
- Publication number
- CN111039332A CN111039332A CN201911219414.2A CN201911219414A CN111039332A CN 111039332 A CN111039332 A CN 111039332A CN 201911219414 A CN201911219414 A CN 201911219414A CN 111039332 A CN111039332 A CN 111039332A
- Authority
- CN
- China
- Prior art keywords
- preparation
- composite material
- temperature
- mixed solution
- nanowire
- 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.)
- Granted
Links
- 239000002070 nanowire Substances 0.000 title claims abstract description 46
- 239000002131 composite material Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 23
- 239000011259 mixed solution Substances 0.000 claims abstract description 21
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000004202 carbamide Substances 0.000 claims abstract description 20
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 13
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 10
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000137 annealing Methods 0.000 claims abstract description 7
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 239000003990 capacitor Substances 0.000 claims description 12
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 7
- 230000007062 hydrolysis Effects 0.000 claims description 6
- 238000006460 hydrolysis reaction Methods 0.000 claims description 6
- 229960005070 ascorbic acid Drugs 0.000 claims description 5
- 235000010323 ascorbic acid Nutrition 0.000 claims description 5
- 239000011668 ascorbic acid Substances 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 239000006260 foam Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000000151 deposition Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 238000004321 preservation Methods 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 abstract 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 abstract 2
- 239000001257 hydrogen Substances 0.000 description 10
- 229910052739 hydrogen Inorganic materials 0.000 description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 7
- -1 polytetrafluoroethylene Polymers 0.000 description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 description 6
- 238000002156 mixing Methods 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 238000004146 energy storage Methods 0.000 description 4
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
-
- 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
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- 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
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- 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
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Nanotechnology (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
一种多功能双层纳米线层状复合材料的制备方法及其应用,属于化工材料技术领域,本发明的目的在于提供一种具有低过电位,高面电容和良好倍率性能且具有良好稳定性的多功能双层纳米线层状复合材料的制备方法及其应用。将负载有氧化还原石墨烯的泡沫镍置于硝酸钴和尿素的混合溶液,经过120℃保温10h反应形成CoO纳米线前驱体;将前驱体放入含有硝酸钴、硝酸镍、尿素和氟化铵的混合溶液,置于120‑160℃箱式炉,保温6h,取出样品,得到双层纳米线前驱体,经300‑500℃退火得到多功能双层纳米线层状复合材料。本发明的原料储量丰富易得,价格低廉,而且性能优异,过电位小,面电容大,倍率性能高,循环稳定性较好。
Description
技术领域
本发明属于化工材料技术领域,具体涉及一种多功能双层纳米线层状复合材料的制备方法及其应用。
背景技术
在现有世界能源格局中,煤炭、石油、天然气等传统能源仍占有相当大比例,化石燃料的过度消耗造成了严重的能源短缺和环境污染,这促使研究人员探索能量转换和储存装置。环境友好的电化学能量系统,包括电化学全水解和超级电容器,被认为是未来能量转换和储存技术的核心。
氢作为一种环境友好的可再生能源,可以通过水的分解得到。水的分解被广泛认为是大规模氢能生产的一条有希望和有吸引力的途径,在氢能量供应中起着重要的作用。水的电解过程包括两个重要的反应:阴极上的析氢反应(HER)和阳极上的析氧反应(OER)。电催化析氢反应被认为是高效制氢的重要途径之一。
然而,在实际应用中,由于动力学能垒和材料本身稳定性差造成的高过电位(η),电解效率受到严重阻碍,较大程度地限制了大规模水电解的发展。HER和OER的过电位不可避免,但尽可能的降低过电位对于电催化剂来说非常重要。Pt基材料是目前公认最有效的HER电催化剂,而Ru/Ir氧化物是一种高活性的OER电催化剂,但高成本和稀缺性几乎限制了它们的大规模实际应用。
在储能材料方面,超级电容器具有功率密度高、充放电快、循环寿命长等优点,被称为最有前途的实用电容器器件。随着新能源的研发日趋成熟,高容量电源系统的得以发展,将新能源成功应用在汽车上,成为新能源利用的研究焦点。超级电容器的出现解决了这一领域的瓶颈,它是一种介于传统静电电容器和二次电池之间的一种新型储能装置,综合保留了蓄电池与传统电容器的优势,并弥补了不足之处。超级电容器的充放电过程可以在极短的时间内完成,其电化学稳定性强,具有超长的寿命,放置时间长且性能基本不变,工作的温度范围广,可达70至-40℃。它在国民经济、科学技术和日常生活中得到了广泛的应用,对缓解能源与环境危机、提高人类生活水平有着重要影响,已成为全球经济发展的一个新热点。超级电容器根据储能机理的不同分为双电层电容器和法拉第准电容器(赝电容器)。在相同的电极面积的情况下,后者的容量是前者的10-100倍。过渡金属Mn、Ni、Co、V等的氧化物是研发赝电容器的有效选择,而因其稳定的电压窗口小,能量密度较低等因素,制备高面电容性能的复合双金属氧化物,使其具有两者及其以上元素的共有性质是目前的研究热点。
将能量转换和能量储存整合为一种材料将是未来研究的重点。因此,实现这些绿色能源系统的一个重要挑战是开发能有效转换和储存能量的电极材料。
发明内容
本发明的目的在于提供一种具有低过电位,高面电容和良好倍率性能且具有良好稳定性的多功能双层纳米线层状复合材料的制备方法及其应用。
本发明采用如下技术方案:
一种多功能双层纳米线层状复合材料的制备方法,包括如下步骤:
第一步,将氧化石墨烯置于蒸馏水中超声1h形成均匀的棕色溶液,加入抗坏血酸,超声搅拌均匀后,得到分散液,将清洗干净的泡沫镍置于分散液中,并在水浴锅90℃条件下,沉积6h,取出后,用去离子水冲洗,置于60℃条件下干燥12h,得到负载还原氧化石墨烯的泡沫镍rGO/NF;
第二步,将Co(NO3)2·6H2O和尿素溶于水形成混合溶液A,将rGO/NF置于混合溶液A中,经过箱式炉120℃保温10h,得到CoO纳米线前驱体;
第三步,将Co(NO3)2·6H2O、Ni(NO3)2·6H2O、尿素和氟化铵溶于水形成均匀的混合溶液B,将CoO纳米线前驱体置于混合溶液B中,转移至120-160℃箱式炉中反应,保温6h后,取出样品,得到双层纳米线前驱体,经300-500℃退火,得到层状CoNiO2/CoO材料,记为CoNiO2/CoO-X-Y,其中,X是水热温度,Y是退火温度。
第一步中所述氧化石墨烯和蒸馏水的比例为1mg:3mL,氧化石墨烯和抗坏血酸的质量比为1:3。
第二步中所述Co(NO3)2·6H2O和尿素的摩尔比为1:5,混合溶液A的体积为35mL。
第三步中所述Co(NO3)2·6H2O、Ni(NO3)2·6H2O、尿素和氟化铵的摩尔比为1.5:1.5:15:8,混合溶液B的体积为30mL。
一种多功能双层纳米线层状复合材料应用于全水解或超级电容器。
本发明的有益效果如下:
本发明的多功能双层纳米线层状复合材料具有较低的析氢过电位,较高的面电容特性,其生产原料价格低廉、制备过程简单、生产效率高、对设备要求低的特点,应用广泛。
本发明制备的多功能双层纳米线层状复合材料CoNiO2/Co-140-400在1M KOH环境中进行析氢反应达到阴极电流密度10 mA cm-2时需要70mV,全水解中达到10 mA cm-2的电流密度时需要1.57V,在2M KOH环境下在1 mA cm-2电流密度下可达 5.37 F cm-2,可应用于全水解和超级电容器等领域,用途广泛。
附图说明
图1是由实施例1-2得到的CoNiO2/Co-140-400纳米线层状复合材料的 XRD曲线。
图2是由实施例1-2获得的CoNiO2/CoO-140-400纳米线层状复合材料的典型扫描电镜照片。
图3是由实施例1-4获得的CoNiO2/CoO-X-400纳米线层状复合材料的析氢极化曲线。
图4是由实施例1,2,5,6获得的CoNiO2/CoO-140-Y纳米线层状复合材料的析氢极化曲线。
图5是由实施例1,2,7获得的CoNiO2/CoO-140-400纳米线层状复合材料的全水解曲线。
图6是由实施例1-2获得的CoNiO2/CoO-140-400纳米线层状复合材料的恒流充放电关系曲线。
具体实施方式
实施例1
将10 mg氧化石墨烯超声置于30 mL蒸馏水中,超声1h形成均匀的棕色溶液后,加入30mg抗坏血酸,超声搅拌均匀后,将清洗干净的泡沫镍放置于分散液中,并在水浴锅90 ℃条件下沉积6小时,取出后用去离子水冲洗样品表面,置于60℃条件下干燥12 h得到rGO/NF。
实施例2
将rGO/NF置于1.019g Co(NO3)2·6H2O和1.051g 尿素混合形成的35mL均匀溶液,经过箱式炉120℃保温10h充分反应形成CoO纳米线前驱体;将前驱体放入含有1.5mmol Co(NO3)2·6H2O、1.5mmol Ni(NO3)2·6H2O、15mmol 尿素和8mmol 氟化铵的30mL均匀混合溶液,转移至聚四氟乙烯内衬并置于140℃箱式炉中反应,保温6h,取出样品,得到双层纳米线前驱体,经400℃退火得到层状CoNiO2/CoO-140-400材料。
实施例3
将rGO/NF置于1.019g Co(NO3)2·6H2O和1.051g 尿素混合形成的35mL均匀溶液,经过箱式炉120℃保温10h充分反应形成CoO纳米线前驱体;将前驱体放入含有1.5mmol Co(NO3)2·6H2O、1.5mmol Ni(NO3)2·6H2O、15mmol 尿素和8mmol 氟化铵的30mL均匀混合溶液,转移至聚四氟乙烯内衬并置于120℃箱式炉中反应,保温6h,取出样品,得到双层纳米线前驱体,经400℃退火得到层状CoNiO2/CoO-120-400材料。
实施例4
将rGO/NF置于1.019g Co(NO3)2·6H2O和1.051g 尿素混合形成的35mL均匀溶液,经过箱式炉120℃保温10h充分反应形成CoO纳米线前驱体;将前驱体放入含有1.5mmol Co(NO3)2·6H2O、1.5mmol Ni(NO3)2·6H2O、15mmol 尿素和8mmol 氟化铵的30mL均匀混合溶液,转移至聚四氟乙烯内衬并置于160℃箱式炉中反应,保温6h,取出样品,得到双层纳米线前驱体,经400℃退火得到层状CoNiO2/CoO-160-400材料。
实施例5
将rGO/NF置于1.019g Co(NO3)2·6H2O和1.051g 尿素混合形成的35mL均匀溶液,经过箱式炉120℃保温10h充分反应形成CoO纳米线前驱体;将前驱体放入含有1.5mmol Co(NO3)2·6H2O、1.5mmol Ni(NO3)2·6H2O、15mmol 尿素和8mmol 氟化铵的30mL均匀混合溶液,转移至聚四氟乙烯内衬并置于140℃箱式炉中反应,保温6h,取出样品,得到双层纳米线前驱体,经300℃退火得到层状CoNiO2/CoO-140-300材料。
实施例6
将rGO/NF置于1.019g Co(NO3)2·6H2O和1.051g 尿素混合形成的35mL均匀溶液,经过箱式炉120℃保温10h充分反应形成CoO纳米线前驱体;将前驱体放入含有1.5mmol Co(NO3)2·6H2O、1.5mmol Ni(NO3)2·6H2O、15mmol 尿素和8mmol 氟化铵的30mL均匀混合溶液,转移至聚四氟乙烯内衬并置于140℃箱式炉中反应,保温6h,取出样品,得到双层纳米线前驱体,经500℃退火得到层状CoNiO2/CoO-140-500材料。
实施例7
将CoNiO2/CoO-140-400材料分别作为阴极和阳极组装成两电极全水解装置,进行全水解测试。
从图1可知,CoNiO2/CoO-140-400材料是由CoNiO2和CoO两相共存的复合材料。
从图2可知,CoNiO2/CoO-140-400是由直径不同的两种针状共存的复合材料,其中粗针的直径大约为130-160nm,细针的直径大约为70-75nm。
从图3可知,CoNiO2/CoO-140-400材料在10mA cm-2的电流密度下需要更少的过电位 (70mV),相对于CoNiO2/CoO-120-400 (100mV),CoNiO2/CoO-160-400 (82mV),表现出更优的催化性能。说明140℃是该实验最佳水热温度。
从图4可知,CoNiO2/CoO-140-400材料在10mA cm-2的电流密度下需要更少的过电位 (70mV),相对于CoNiO2/CoO-140-300 (195 mV),CoNiO2/CoO-140-500 (159 mV),表现出更优的催化性能。说明400℃是该实验最佳退火温度。
从图5可知,CoNiO2/CoO-140-400‖CoNiO2/CoO-140-400应用于全水解, 10mA cm-2的电流密度下需要电压1.57 V。
从图6可知,CoNiO2/CoO-140-400在1mAcm-2的电流密度下,其面电容达到5.37Fcm-2。
Claims (5)
1.一种多功能双层纳米线层状复合材料的制备方法,其特征在于:包括如下步骤:
第一步,将氧化石墨烯置于蒸馏水中超声1h形成均匀的棕色溶液,加入抗坏血酸,超声搅拌均匀后,得到分散液,将清洗干净的泡沫镍置于分散液中,并在水浴锅90℃条件下,沉积6h,取出后,用去离子水冲洗,置于60℃条件下干燥12h,得到负载还原氧化石墨烯的泡沫镍rGO/NF;
第二步,将Co(NO3)2·6H2O和尿素溶于水形成混合溶液A,将rGO/NF置于混合溶液A中,经过箱式炉120℃保温10h,得到CoO纳米线前驱体;
第三步,将Co(NO3)2·6H2O、Ni(NO3)2·6H2O、尿素和氟化铵溶于水形成均匀的混合溶液B,将CoO纳米线前驱体置于混合溶液B中,转移至120-160℃箱式炉中反应,保温6h后,取出样品,得到双层纳米线前驱体,经300-500℃退火,得到层状CoNiO2/CoO材料,记为CoNiO2/CoO-X-Y,其中,X是水热温度,Y是退火温度。
2.根据权利要求1所述的一种多功能双层纳米线层状复合材料的制备方法,其特征在于:第一步中所述氧化石墨烯和蒸馏水的比例为1mg:3mL,氧化石墨烯和抗坏血酸的质量比为1:3。
3.根据权利要求1所述的一种多功能双层纳米线层状复合材料的制备方法,其特征在于:第二步中所述Co(NO3)2·6H2O和尿素的摩尔比为1:5,混合溶液A的体积为35mL。
4.根据权利要求1所述的一种多功能双层纳米线层状复合材料的制备方法,其特征在于:第三步中所述Co(NO3)2·6H2O、Ni(NO3)2·6H2O、尿素和氟化铵的摩尔比为1.5:1.5:15:8,混合溶液B的体积为30mL。
5.一种利用权利要求1-4任意一项所述的多功能双层纳米线层状复合材料的制备方法制备的多功能双层纳米线层状复合材料应用于全水解或超级电容器。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201911219414.2A CN111039332B (zh) | 2019-12-03 | 2019-12-03 | 一种多功能双层纳米线层状复合材料的制备方法及其应用 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201911219414.2A CN111039332B (zh) | 2019-12-03 | 2019-12-03 | 一种多功能双层纳米线层状复合材料的制备方法及其应用 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN111039332A true CN111039332A (zh) | 2020-04-21 |
CN111039332B CN111039332B (zh) | 2022-06-07 |
Family
ID=70233383
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201911219414.2A Expired - Fee Related CN111039332B (zh) | 2019-12-03 | 2019-12-03 | 一种多功能双层纳米线层状复合材料的制备方法及其应用 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN111039332B (zh) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111659466A (zh) * | 2020-06-02 | 2020-09-15 | 上海师范大学 | 针球状的ZIF-67@CoO@Co光电催化材料及其制备方法和应用 |
CN114590851A (zh) * | 2022-03-30 | 2022-06-07 | 南京航空航天大学 | 一种具有微纳塔层结构的金属氧化物粉体及其制法 |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109390162A (zh) * | 2018-09-17 | 2019-02-26 | 太原理工大学 | 一种具有优异电化学性能的锰钴硫化物/还原氧化石墨烯复合材料及制备方法 |
-
2019
- 2019-12-03 CN CN201911219414.2A patent/CN111039332B/zh not_active Expired - Fee Related
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109390162A (zh) * | 2018-09-17 | 2019-02-26 | 太原理工大学 | 一种具有优异电化学性能的锰钴硫化物/还原氧化石墨烯复合材料及制备方法 |
Non-Patent Citations (2)
Title |
---|
YIN SUN等: ""The NH4F-induced morphology control of hierarchical CoO@MnO2 core–shell arrays for high performance supercapacitor electrodes"", 《CRYSTENGCOMM》 * |
常玲: ""新颖纳米结构过渡金属(Fe,Co,Ni)氧化物的制备及其电化学储锂/钠性能"", 《中国博士学位论文全文数据库(电子期刊) 工程科技Ⅰ辑》 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111659466A (zh) * | 2020-06-02 | 2020-09-15 | 上海师范大学 | 针球状的ZIF-67@CoO@Co光电催化材料及其制备方法和应用 |
CN114590851A (zh) * | 2022-03-30 | 2022-06-07 | 南京航空航天大学 | 一种具有微纳塔层结构的金属氧化物粉体及其制法 |
CN114590851B (zh) * | 2022-03-30 | 2023-03-31 | 南京航空航天大学 | 一种具有微纳塔层结构的金属氧化物粉体及其制法 |
Also Published As
Publication number | Publication date |
---|---|
CN111039332B (zh) | 2022-06-07 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN103440998B (zh) | 一种钴酸锌纳米片列阵/泡沫镍复合电极、制备方法及其应用 | |
CN107275105B (zh) | 超级电容器电极材料及其制备方法 | |
CN108796551B (zh) | 负载在泡沫镍上的海胆状硫化钴催化剂及其制备方法、作为电解水析氧催化剂的应用 | |
Guan et al. | Facile synthesis of double-layered CoNiO2/CoO nanowire arrays as multifunction electrodes for hydrogen electrocatalysis and supercapacitors | |
CN107342174A (zh) | 一种二维层状CoMoS4纳米片为超级电容器电极材料的制备方法 | |
CN109326456B (zh) | 一种超级电容器及其制备方法 | |
CN110350184B (zh) | 一种用于电池正极材料的高容量NiMoO4储能材料的制备方法 | |
CN106876682A (zh) | 一种具有多孔结构的氧化锰/镍微米球及其制备和应用 | |
CN110993362A (zh) | 一种新型三维电极材料及其制备方法和在超级电容器中的应用 | |
CN112886029B (zh) | 以中空碳纳米管为载体的双功能氧电催化剂的制备及应用 | |
CN111048325A (zh) | 一种作为超级电容器的形貌可控的镍锰硫化物/石墨烯复合材料及其制备方法 | |
CN109390162A (zh) | 一种具有优异电化学性能的锰钴硫化物/还原氧化石墨烯复合材料及制备方法 | |
CN107146711A (zh) | 一种导电基底生长纳米层状金属化合物电极材料及其制备与应用 | |
CN111039332B (zh) | 一种多功能双层纳米线层状复合材料的制备方法及其应用 | |
CN104282445A (zh) | 超级电容器用四氧化三钴氮掺杂碳纳米管复合电极材料及其制备方法 | |
CN106449136A (zh) | α‑氢氧化镍钴电极材料及其制备方法与应用 | |
CN104201008A (zh) | 超级电容器用氧化镍氮掺杂碳纳米管复合电极材料及其制备方法 | |
CN109817475B (zh) | 硫化铋镍正极材料的制备方法及其应用 | |
CN111268745A (zh) | 一种NiMoO4@Co3O4核壳纳米复合材料、制备方法和应用 | |
CN112467077A (zh) | 有效增强多种过渡金属氧化物储电性能的普适性电化学改性制备方法 | |
CN111223683A (zh) | 一种制备碳/纳米二氧化锰复合电极材料的方法 | |
CN113078328A (zh) | 一种用于水系锌-空气电池的Co-FPOH微球材料及其制备方法 | |
CN109081377B (zh) | 一种三维二硫化钼花球阵列及其制备方法和应用 | |
Cui et al. | Facile synthesis of NiCo2S4@ Ni3Se2 nanocomposites for supercapacitor and electrocatalytic H2 production | |
CN111146008A (zh) | 一种作为超级电容器的锰钼硫化物/石墨烯复合电极材料及其制备方法 |
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 | ||
GR01 | Patent grant | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20220607 |
|
CF01 | Termination of patent right due to non-payment of annual fee |