CN104810160B - A kind of ambrose alloy subcarbonate nano-wire array, preparation method and the usage - Google Patents
A kind of ambrose alloy subcarbonate nano-wire array, preparation method and the usage Download PDFInfo
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- 239000002070 nanowire Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000956 alloy Substances 0.000 title abstract 5
- 229910045601 alloy Inorganic materials 0.000 title abstract 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910052802 copper Inorganic materials 0.000 claims abstract description 33
- 239000010949 copper Substances 0.000 claims abstract description 33
- 239000006260 foam Substances 0.000 claims abstract description 26
- 239000007772 electrode material Substances 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 56
- YOCUPQPZWBBYIX-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Cu] YOCUPQPZWBBYIX-UHFFFAOYSA-N 0.000 claims description 56
- 239000012154 double-distilled water Substances 0.000 claims description 18
- 238000004140 cleaning Methods 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 12
- 239000004202 carbamide Substances 0.000 claims description 12
- SXTLQDJHRPXDSB-UHFFFAOYSA-N copper;dinitrate;trihydrate Chemical compound O.O.O.[Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O SXTLQDJHRPXDSB-UHFFFAOYSA-N 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 4
- 150000001879 copper Chemical class 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 150000002815 nickel Chemical class 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000003990 capacitor Substances 0.000 abstract 1
- 239000000376 reactant Substances 0.000 abstract 1
- 230000035484 reaction time Effects 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- 238000001878 scanning electron micrograph Methods 0.000 description 12
- 238000000034 method Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 4
- 238000002484 cyclic voltammetry Methods 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 238000003491 array Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000011218 binary composite Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
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- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
Description
技术领域technical field
本发明涉及纳米材料合成领域，具体涉及一种镍铜碱式碳酸盐纳米线阵列、其制备方法及应用。The invention relates to the field of nanomaterial synthesis, in particular to a nickel-copper basic carbonate nanowire array, a preparation method and application thereof.
背景技术Background technique
超级电容器具有功率密度高、充电时间短、温度特性好、使用寿命长等优点。随着科学技术突飞猛进的发展以及电子储能产品的更新换代，超级电容器电极材料的研究已经引起了研究者们的极大兴趣。目前，传统的超级电容器电极材料主要有以下几类：碳材料类电极材料、导电聚合物类电极材料、贵金属氧化物类电极材料。高性能的超级电容器电极材料需满足以下两点要求：电极材料的导电性好和比表面积大。然而，在实际应用中，人们发现，这些传统的电极材料或多或少都存在各自的缺陷，如：活性面积小，导电性差、电容量低，循环时间短，能量密度和功率密度小，由于这些缺陷的存在，很难满足现实中更高的应用需求。Supercapacitors have the advantages of high power density, short charging time, good temperature characteristics, and long service life. With the rapid development of science and technology and the upgrading of electronic energy storage products, the research on electrode materials for supercapacitors has aroused great interest of researchers. At present, the traditional supercapacitor electrode materials mainly include the following categories: carbon material electrode materials, conductive polymer electrode materials, and noble metal oxide electrode materials. A high-performance supercapacitor electrode material needs to meet the following two requirements: the electrode material has good conductivity and a large specific surface area. However, in practical applications, it is found that these traditional electrode materials have more or less their own defects, such as: small active area, poor conductivity, low capacitance, short cycle time, low energy density and power density, due to The existence of these defects makes it difficult to meet the higher application requirements in reality.
发明内容Contents of the invention
本发明的目的在于针对传统电极材料的不足，本发明提供一种镍铜碱式碳酸盐纳米线阵列。本发明还提供了一种镍铜碱式碳酸盐纳米线阵列的制备方法，及其应用，得到的镍铜碱式碳酸盐纳米线阵列，可直接用作超级电容器电极材料。本发明提供的一种镍铜碱式碳酸盐纳米线阵列材料，以泡沫铜为基底，镍铜碱式碳酸盐纳米线均匀生长在泡沫铜上，该结构排列整齐规则。具体技术方案如下：The purpose of the present invention is to address the shortcomings of traditional electrode materials, and the present invention provides a nickel-copper basic carbonate nanowire array. The invention also provides a preparation method of the nickel-copper basic carbonate nanowire array and its application. The obtained nickel-copper basic carbonate nanowire array can be directly used as a supercapacitor electrode material. The nickel-copper basic carbonate nanowire array material provided by the present invention uses foamed copper as a base, and the nickel-copper basic carbonate nanowires grow evenly on the foamed copper, and the structure is arranged in an orderly manner. The specific technical scheme is as follows:
一种镍铜碱式碳酸盐纳米线阵列，由泡沫铜及在其表面生长的镍铜碱式碳酸盐纳米线阵列构成。A nickel-copper basic carbonate nanowire array is composed of foamed copper and nickel-copper basic carbonate nanowire arrays grown on the surface thereof.
一种镍铜碱式碳酸盐纳米线阵列的制备方法，包括以下步骤：A preparation method of a nickel-copper basic carbonate nanowire array, comprising the following steps:
(1)将二次蒸馏水、二价镍盐、二价铜盐和尿素混合；(1) double distilled water, divalent nickel salt, divalent copper salt and urea are mixed;
(2)搅拌使其均匀混合，得到混合液；(2) Stir to make it evenly mix, obtain mixed liquor;
(3)将混合液倒入反应釜中；(3) Pour the mixed solution into the reactor;
(4)将泡沫铜浸入；(4) immerse foam copper;
(5)反应；(5) Reaction;
(6)冷却；(6) cooling;
(7)干燥，即得到镍铜碱式碳酸盐纳米线阵列。(7) drying to obtain the nickel-copper basic carbonate nanowire array.
进一步地，步骤(4)中泡沫铜为清洗后表面洁净的泡沫铜，和/或，步骤(1)之前还包括步骤：将表面有杂质的泡沫铜清洗干净。Further, the copper foam in step (4) is copper foam with a clean surface after cleaning, and/or, before step (1), a step is also included: cleaning the copper foam with impurities on the surface.
进一步地，步骤(6)中冷却至室温，和/或，步骤(7)中室温干燥。Further, cooling to room temperature in step (6), and/or drying at room temperature in step (7).
进一步地，步骤(6)和(7)之间还包括清洗步骤：所述清洗步骤采用二次蒸馏水、无水乙醇清洗。Further, a cleaning step is also included between steps (6) and (7): said cleaning step uses double distilled water and absolute ethanol to clean.
进一步地，步骤(5)中将反应釜密闭反应，和/或，所述反应为在120-180℃下反应2-10h。Further, in the step (5), the reactor is sealed and reacted, and/or, the reaction is performed at 120-180° C. for 2-10 hours.
进一步地，所述清洗步骤为：将表面有杂质的泡沫铜依次用丙酮、乙醇、二次蒸馏水进行超声清洗，超声清洗时间为10-20min。Further, the cleaning step is: ultrasonically cleaning the copper foam with impurities on the surface with acetone, ethanol, and double distilled water in sequence, and the ultrasonic cleaning time is 10-20 minutes.
进一步地，六水合硝酸镍的浓度≥0.1mol L-1，三水合硝酸铜的浓度≥0.1mol L-1，尿素的浓度≥0.4mol L-1，二次蒸馏水的体积≥20mL。Further, the concentration of nickel nitrate hexahydrate ≥ 0.1 mol L -1 , the concentration of copper nitrate trihydrate ≥ 0.1 mol L -1 , the concentration of urea ≥ 0.4 mol L -1 , and the volume of twice distilled water ≥ 20 mL.
上述镍铜碱式碳酸盐纳米线阵列的用途，用作超级电容器的电极材料。The use of the above-mentioned nickel-copper basic carbonate nanowire array is used as an electrode material for a supercapacitor.
与目前现有技术相比，本发明所制备的镍铜碱式碳酸盐纳米线阵列直接生长在泡沫铜上，可直接作为超级电容器的电极材料，不仅增强了导电性，而且实现了长的稳定性，此外二元复合材料提高了材料的能量密度和功率密度，在能量存储方面具有潜在的应用价值。本发明提供的一种镍铜碱式碳酸盐纳米线阵列的制备方法，是在密闭的高温高压反应釜中，采用二次蒸馏水作为反应溶剂，加入六水合硝酸镍、三水合硝酸铜、尿素混合，搅拌得到均匀混合液，通过加热反应体系，产生一个高压环境而制备镍铜碱式碳酸盐纳米线阵列材料的一种有效方法。本发明操作简便，耗能低，合成成本低，重现性高，所得产物纯度高、晶形好且可控制。Compared with the current existing technology, the nickel-copper basic carbonate nanowire array prepared by the present invention is directly grown on the foamed copper, which can be directly used as the electrode material of the supercapacitor, which not only enhances the conductivity, but also realizes long In addition, the binary composite material improves the energy density and power density of the material, and has potential application value in energy storage. The preparation method of a nickel-copper basic carbonate nanowire array provided by the present invention is to use twice distilled water as the reaction solvent in a closed high-temperature and high-pressure reaction kettle, and add nickel nitrate hexahydrate, copper nitrate trihydrate, and urea It is an effective method for preparing nickel-copper basic carbonate nanowire array material by mixing and stirring to obtain uniform mixed liquid, and generating a high-pressure environment by heating the reaction system. The invention has the advantages of simple and convenient operation, low energy consumption, low synthesis cost and high reproducibility, and the obtained product has high purity, good crystal form and controllability.
附图说明Description of drawings
图1为实施例1制备的镍铜碱式碳酸盐纳米线阵列的低放大倍率的扫描电子显微镜照片(SEM)；Fig. 1 is the scanning electron micrograph (SEM) of the low magnification of the nickel-copper basic carbonate nanowire array prepared by embodiment 1;
图2为实施例1制备的镍铜碱式碳酸盐纳米线阵列的高放大倍率的扫描电子显微镜照片(SEM)；Fig. 2 is the high-magnification scanning electron micrograph (SEM) of the nickel-copper basic carbonate nanowire array prepared in embodiment 1;
图3为实施例1制备的镍铜碱式碳酸盐纳米线阵列的粉末X-射线衍射图(XRD)；Fig. 3 is the powder X-ray diffraction figure (XRD) of the nickel-copper basic carbonate nanowire array prepared in embodiment 1;
图4为实施例1制备的镍铜碱式碳酸盐纳米线阵列的透射电子显微镜照片(TEM)Fig. 4 is the transmission electron micrograph (TEM) of the nickel-copper basic carbonate nanowire array prepared in embodiment 1
图5为实施例2制备的镍铜碱式碳酸盐纳米线阵列的扫描电子显微镜照片(SEM)；Fig. 5 is the scanning electron micrograph (SEM) of the nickel-copper basic carbonate nanowire array prepared in embodiment 2;
图6为实施例3制备的镍铜碱式碳酸盐纳米线阵列的扫描电子显微镜照片(SEM)；Fig. 6 is the scanning electron micrograph (SEM) of the nickel-copper basic carbonate nanowire array prepared in embodiment 3;
图7为实施例4制备的镍铜碱式碳酸盐纳米线阵列的扫描电子显微镜照片(SEM)；Fig. 7 is the scanning electron micrograph (SEM) of the nickel-copper basic carbonate nanowire array prepared in embodiment 4;
图8为实施例5制备的镍铜碱式碳酸盐纳米线阵列的扫描电子显微镜照片(SEM)；Fig. 8 is the scanning electron micrograph (SEM) of the nickel-copper basic carbonate nanowire array prepared in embodiment 5;
图9为实施例1制备的镍铜碱式碳酸盐纳米线阵列的循环伏安曲线图(CV)；Fig. 9 is the cyclic voltammetry curve (CV) of the nickel-copper basic carbonate nanowire array prepared in Example 1;
图10为实施例1制备的镍铜碱式碳酸盐纳米线阵列的充放电曲线图；Fig. 10 is the charge-discharge curve diagram of the nickel-copper basic carbonate nanowire array prepared in Example 1;
图11为实施例1制备的镍铜碱式碳酸盐纳米线阵列的具体电容-电流密度对比曲线图。11 is a specific capacitance-current density comparison curve of the nickel-copper basic carbonate nanowire array prepared in Example 1.
具体实施方式Detailed ways
下面根据附图对本发明进行详细描述，其为本发明多种实施方式中的一种优选实施例。The present invention will be described in detail below according to the accompanying drawings, which is a preferred embodiment among various implementations of the present invention.
一种镍铜碱式碳酸盐纳米线阵列的制备方法，包括以下步骤：A preparation method of a nickel-copper basic carbonate nanowire array, comprising the following steps:
a、将表面有杂质的泡沫铜清洗干净：将表面有杂质的泡沫铜依次用丙酮、乙醇、二次蒸馏水进行超声清洗，超声清洗时间为10-20min；a. Clean the foamed copper with impurities on the surface: ultrasonically clean the foamed copper with impurities on the surface with acetone, ethanol, and double distilled water in sequence, and the ultrasonic cleaning time is 10-20 minutes;
b、镍铜碱式碳酸盐纳米线阵列制备工序:b, nickel-copper basic carbonate nanowire array preparation process:
将二次蒸馏水、二价镍盐、二价铜盐和尿素混合，不断搅拌使其均匀混合后，得到混合液，倒入反应釜中，将清洗后表面洁净的泡沫铜浸入，将反应釜密闭，反应，冷却至室温，用二次蒸馏水、无水乙醇清洗，室温干燥，即得到镍铜碱式碳酸盐纳米线阵列。所用六水合硝酸镍的浓度≥0.1mol L-1，三水合硝酸铜的浓度≥0.1mol L-1，尿素的浓度≥0.4mol L-1，二次蒸馏水的体积≥20mL。所述反应为在120-180℃下反应2-10h。Mix double-distilled water, divalent nickel salt, divalent copper salt and urea, stir continuously to make it evenly mixed, and get the mixed solution, pour it into the reaction kettle, immerse the cleaned foam copper on the surface, and seal the reaction kettle , react, cool to room temperature, wash with twice distilled water and absolute ethanol, and dry at room temperature to obtain a nickel-copper basic carbonate nanowire array. The concentration of nickel nitrate hexahydrate used is ≥0.1mol L -1 , the concentration of copper nitrate trihydrate is ≥0.1mol L -1 , the concentration of urea is ≥0.4mol L -1 , and the volume of twice distilled water is ≥20mL. The reaction is carried out at 120-180° C. for 2-10 hours.
所制备的镍铜碱式碳酸盐纳米线阵列生长在泡沫铜上，可直接作为超级电容器的电极材料。The as-prepared nickel-copper basic carbonate nanowire arrays are grown on copper foam and can be directly used as electrode materials for supercapacitors.
实施例1Example 1
a、泡沫铜的清洗处理工序:a. Cleaning process of copper foam:
将表面有杂质的泡沫铜依次用丙酮、乙醇、二次蒸馏水进行超声清洗，超声清洗时间为15min；The copper foam with impurities on the surface is ultrasonically cleaned with acetone, ethanol, and double distilled water in sequence, and the ultrasonic cleaning time is 15 minutes;
b、镍铜碱式碳酸盐纳米线阵列制备工序:b, nickel-copper basic carbonate nanowire array preparation process:
在常温下，将2mmol六水合硝酸镍、2mmol三水合硝酸铜和8mmol尿素溶解于20mL二次蒸馏水中，不断搅拌使其均匀混合形成澄清溶液，倒入60mL反应釜中，将处理好的泡沫铜浸入混合液中，拧紧釜盖，在160℃下反应6h，取出反应釜自然冷却至室温，依次用二次蒸馏水、无水乙醇清洗干净，自然晾干，即得到镍铜碱式碳酸盐纳米线阵列。At room temperature, dissolve 2mmol nickel nitrate hexahydrate, 2mmol copper nitrate trihydrate and 8mmol urea in 20mL double-distilled water, stir continuously to make it evenly mixed to form a clear solution, pour it into a 60mL reaction kettle, and put the treated foam copper Immerse in the mixed solution, tighten the lid of the kettle, react at 160°C for 6 hours, take out the reactor and cool it to room temperature naturally, clean it with double distilled water and absolute ethanol in turn, and dry it naturally to obtain nickel-copper basic carbonate nanoparticles line array.
一种镍铜碱式碳酸盐纳米线阵列的应用，作为超级电容器的电极材料的应用。An application of a nickel-copper basic carbonate nanowire array as an electrode material for a supercapacitor.
所制的镍铜碱式碳酸盐纳米线阵列的形貌如图1所示，镍铜碱式碳酸盐纳米线阵列均匀有序的生长在泡沫铜上。The morphology of the prepared nickel-copper basic carbonate nanowire array is shown in FIG. 1 , and the nickel-copper basic carbonate nanowire array grows uniformly and orderly on the copper foam.
实施例2Example 2
a、泡沫铜的清洗处理工序:与实施例1相同；A, the cleaning process of copper foam: same as embodiment 1;
b、镍铜碱式碳酸盐纳米线阵列制备工序:b, nickel-copper basic carbonate nanowire array preparation process:
在常温下，将2mmol六水合硝酸镍、2mmol三水合硝酸铜和8mmol尿素溶解于20mL二次蒸馏水中，不断搅拌使其均匀混合形成澄清溶液，倒入60mL反应釜中，将处理好的泡沫铜浸入混合液中，拧紧釜盖，在160℃下反应2h，取出反应釜自然冷却至室温，依次用二次蒸馏水、无水乙醇清洗干净，自然晾干，即得到镍铜碱式碳酸盐纳米线阵列。At room temperature, dissolve 2mmol nickel nitrate hexahydrate, 2mmol copper nitrate trihydrate and 8mmol urea in 20mL double-distilled water, stir continuously to make it evenly mixed to form a clear solution, pour it into a 60mL reaction kettle, and put the treated foam copper Immerse in the mixed solution, tighten the lid of the kettle, react at 160°C for 2 hours, take out the reaction kettle and cool it to room temperature naturally, clean it with double distilled water and absolute ethanol in turn, and dry it naturally to obtain nickel-copper basic carbonate nanoparticles line array.
一种镍铜碱式碳酸盐纳米线阵列的应用，作为超级电容器的电极材料的应用。An application of a nickel-copper basic carbonate nanowire array as an electrode material for a supercapacitor.
所制的镍铜碱式碳酸盐纳米线阵列的形貌如图5所示。The morphology of the prepared nickel-copper basic carbonate nanowire array is shown in FIG. 5 .
实施例3Example 3
a、泡沫铜的清洗处理工序:与实施例1相同；A, the cleaning process of copper foam: same as embodiment 1;
b、镍铜碱式碳酸盐纳米线阵列制备工序:b, nickel-copper basic carbonate nanowire array preparation process:
在常温下，将2mmol六水合硝酸镍、2mmol三水合硝酸铜和8mmol尿素溶解于20mL二次蒸馏水中，不断搅拌使其均匀混合形成澄清溶液，倒入60mL反应釜中，将处理好的泡沫铜浸入混合液中，拧紧釜盖，在160℃下反应10h，取出反应釜自然冷却至室温，依次用二次蒸馏水、无水乙醇清洗干净，自然晾干，即得到镍铜碱式碳酸盐纳米线阵列。At room temperature, dissolve 2mmol nickel nitrate hexahydrate, 2mmol copper nitrate trihydrate and 8mmol urea in 20mL double-distilled water, stir continuously to make it evenly mixed to form a clear solution, pour it into a 60mL reaction kettle, and put the treated foam copper Immerse in the mixed solution, tighten the lid of the kettle, react at 160°C for 10 hours, take out the reaction kettle and cool it to room temperature naturally, clean it with double distilled water and absolute ethanol in turn, and dry it naturally to obtain nickel-copper basic carbonate nano line array.
一种镍铜碱式碳酸盐纳米线阵列的应用，作为超级电容器的电极材料的应用。An application of a nickel-copper basic carbonate nanowire array as an electrode material for a supercapacitor.
所制的镍铜碱式碳酸盐纳米线阵列的形貌如图6所示。The morphology of the prepared nickel-copper basic carbonate nanowire array is shown in FIG. 6 .
实施例4Example 4
a、泡沫铜的清洗处理工序:与实施例1相同；A, the cleaning process of copper foam: same as embodiment 1;
b、镍铜碱式碳酸盐纳米线阵列制备工序:b, nickel-copper basic carbonate nanowire array preparation process:
在常温下，将2mmol六水合硝酸镍、2mmol三水合硝酸铜和8mmol尿素溶解于20mL二次蒸馏水中，不断搅拌使其均匀混合形成澄清溶液，倒入60mL反应釜中，将处理好的泡沫铜浸入混合液中，拧紧釜盖，在120℃下反应6h，取出反应釜自然冷却至室温，依次用二次蒸馏水、无水乙醇清洗干净，自然晾干，即得到镍铜碱式碳酸盐纳米线阵列。At room temperature, dissolve 2mmol nickel nitrate hexahydrate, 2mmol copper nitrate trihydrate and 8mmol urea in 20mL double-distilled water, stir continuously to make it evenly mixed to form a clear solution, pour it into a 60mL reaction kettle, and put the treated foam copper Immerse in the mixed solution, tighten the lid of the kettle, react at 120°C for 6 hours, take out the reactor and cool it to room temperature naturally, clean it with twice distilled water and absolute ethanol in turn, and dry it naturally to obtain nickel-copper basic carbonate nanoparticles line array.
一种镍铜碱式碳酸盐纳米线阵列的应用，作为超级电容器的电极材料的应用。An application of a nickel-copper basic carbonate nanowire array as an electrode material for a supercapacitor.
所制的镍铜碱式碳酸盐纳米线阵列的形貌如图7所示。The morphology of the prepared nickel-copper basic carbonate nanowire array is shown in FIG. 7 .
实施例5Example 5
a、泡沫铜的清洗处理工序:与实施例1相同；A, the cleaning process of copper foam: same as embodiment 1;
b、镍铜碱式碳酸盐纳米线阵列制备工序:b, nickel-copper basic carbonate nanowire array preparation process:
在常温下，将2mmol六水合硝酸镍、2mmol三水合硝酸铜和8mmol尿素溶解于20mL二次蒸馏水中，不断搅拌使其均匀混合形成澄清溶液，倒入60mL反应釜中，将处理好的泡沫铜浸入混合液中，拧紧釜盖，在180℃下反应6h，取出反应釜自然冷却至室温，依次用二次蒸馏水、无水乙醇清洗干净，自然晾干，即得到镍铜碱式碳酸盐纳米线阵列。At room temperature, dissolve 2mmol nickel nitrate hexahydrate, 2mmol copper nitrate trihydrate and 8mmol urea in 20mL double-distilled water, stir continuously to make it evenly mixed to form a clear solution, pour it into a 60mL reaction kettle, and put the treated foam copper Immerse in the mixed solution, tighten the lid of the kettle, react at 180°C for 6 hours, take out the reactor and cool it to room temperature naturally, clean it with double distilled water and absolute ethanol in turn, and dry it naturally to obtain nickel-copper basic carbonate nanoparticles line array.
一种镍铜碱式碳酸盐纳米线阵列的应用，作为超级电容器的电极材料的应用。An application of a nickel-copper basic carbonate nanowire array as an electrode material for a supercapacitor.
所制的镍铜碱式碳酸盐纳米线阵列的形貌如图8所示。The morphology of the prepared nickel-copper basic carbonate nanowire array is shown in FIG. 8 .
实施例6(电化学应用)Embodiment 6 (electrochemical application)
将实施例1制备好的一种镍铜碱式碳酸盐纳米线阵列，直接用来做电极,以KOH溶液作为电解质，做电化学性质测试。A nickel-copper basic carbonate nanowire array prepared in Example 1 was directly used as an electrode, and KOH solution was used as an electrolyte to test its electrochemical properties.
取10mL 6.0M KOH溶液作为电解质溶液放入电解槽中，将实施例1中制备的电极作为工作电极，连接好三电极体系，打开电化学工作站。设定好相关参数，在扫速为5mVs-1时测循环伏安曲线(图9中曲线1)，而后在扫速为10mV s-1时测循环伏安曲线(图9中曲线2)，依次类推得到扫速为20mV s-1(图9中曲线3)、30mV s-1(图9中曲线4)、50mV s-1(图9中曲线5)、70mV s-1(图9中曲线6)、100mV s-1(图9中曲线7)，从得到的CV图可以看出，随着扫速的增加电势呈线性关系。Take 10 mL of 6.0M KOH solution as the electrolyte solution and put it into the electrolytic cell, use the electrode prepared in Example 1 as the working electrode, connect the three-electrode system, and turn on the electrochemical workstation. Set the relevant parameters, measure the cyclic voltammetry curve (curve 1 in Figure 9) when the scan rate is 5mVs -1 , then measure the cyclic voltammetry curve (curve 2 in Figure 9) when the scan rate is 10mV s -1 , By analogy, the scan rates are 20mV s -1 (curve 3 in Figure 9), 30mV s -1 (curve 4 in Figure 9), 50mV s -1 (curve 5 in Figure 9), 70mV s -1 (curve 5 in Figure 9 Curve 6), 100mV s -1 (curve 7 in Figure 9), it can be seen from the obtained CV diagram that the potential has a linear relationship with the increase of the scan rate.
取10mL 6.0M KOH溶液作为电解质溶液放入电解槽中，将实施例1中制备的电极作为工作电极，连接好三电极体系，打开电化学工作站。设定好相关参数，在1A g-1时得到充放电曲线(图10中曲线1)，在2A g-1时得到充放电曲线(图10中曲线2)，在3A g-1时得到充放电曲线(图10中曲线3)，在5A g-1时得到充放电曲线(图10中曲线4)，在10A g-1时得到充放电曲线(图10中曲线5)，从充放电曲线可以得出镍铜碱式碳酸盐纳米线材料作为电极相比其它材料容量大，通过计算在电流密度为1A g-1时，最大的具体电容为971F g-1。Take 10 mL of 6.0M KOH solution as the electrolyte solution and put it into the electrolytic cell, use the electrode prepared in Example 1 as the working electrode, connect the three-electrode system, and turn on the electrochemical workstation. After setting the relevant parameters, the charge-discharge curve (curve 1 in Figure 10) is obtained at 1A g -1 , the charge-discharge curve is obtained at 2A g -1 (curve 2 in Figure 10), and the charge-discharge curve is obtained at 3A g -1 . Discharge curve (curve 3 in Figure 10), the charge-discharge curve (curve 4 in Figure 10) is obtained at 5A g -1 , and the charge-discharge curve (curve 5 in Figure 10) is obtained at 10A g -1 , from the charge-discharge curve It can be concluded that the nickel-copper basic carbonate nanowire material as an electrode has a larger capacity than other materials. By calculation, when the current density is 1A g -1 , the maximum specific capacitance is 971F g -1 .
上面结合附图对本发明进行了示例性描述，显然本发明具体实现并不受上述方式的限制，只要采用了本发明的方法构思和技术方案进行的各种改进，或未经改进直接应用于其它场合的，均在本发明的保护范围之内。The present invention has been exemplarily described above in conjunction with the accompanying drawings. Obviously, the specific implementation of the present invention is not limited by the above methods, as long as the various improvements of the method concept and technical solutions of the present invention are adopted, or directly applied to other Occasions, all within the protection scope of the present invention.
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