超级电容器新型电极材料的制备及其性能研究
发布时间：2019-03-23 16:57
【摘要】：作为新型能量存储与转换装置,超级电容器所具有的优点包括较高的能量密度功率密度、较长的使用次数和绿色环保等。电极材料的改进和优化一直是超级电容器研究的重点。如何改善现有电极材料电化学性能、制备新型高性能的电极材料以及简化制备工艺和降低制备成本成为目前的研究重点。基于以上背景,本论文做了如下的研究工作:首先,本文以实验室自制的碳纤维作为前体材料,浸润PAN/DMF溶液后进行预氧化热处理,制备表面改性的碳纤维。利用XRD、Raman、FTIR和SEM对结构组成和表观形貌进行了表征。采用PAN/DMF浓度10wt%、煅烧温度290℃和锻烧时间1h条件下表面改性的碳纤维,在电流密度为0.5 A·g-1时比电容为127.9 F·g-1,比碳纤维前体提高约17.1%,1.0 A·g-1下循环充放电5000次后比电容保持率为98.5%。其次,以三水合硝酸铜(Cu(NO_3)_2·3H_2O)为铜源,硫脲(NH_2CSNH_2)为硫源,D-葡萄糖酸钠为络合剂,去离子水为反应溶剂,通过水热方法"一锅"制备了硫化铜/碳(CuS/C)复合材料。采用XRD、Raman、FTIR、EDS分析产物化学组成和微观形貌进行了表征。产物中CuS主要呈球花状,球的直径约在1～2μm,表面分布有大量平均宽度在50 nm左右的花瓣状褶皱。复合材料中的碳组分主要呈光滑球状,含量约6 wt%。当水热温度为150℃和水热反应时间为24 h时,所制备的CuS/C复合材料在1 A·g-1的比电容达719.6 F·g1,1000圈后比电容仅衰减20%,综合电化学性能良好。接着,以泡沫镍作为基体材料,先通过水热法在泡沫镍孔道内填塞了亚微米级碳球,提高整个基体的比表面积,随后以六水合氯化镍(NiCl_2·6H_2O)为镍源,硫脲为硫源,通过水热法在碳球表面生长Ni_3S_2,制备泡沫镍@碳球@硫化镍(NF@CMSs@Ni_3S_2)复合材料。采用XRD、Raman、SEM、EDS和TEM对元素组成和表面形貌进行表征。当电流密度为0.008 A·cm-2时,复合材料的面积比电容达7.10 F·cm-2,电流密度增大到0.056 A·cm-2时,面积比电容保持率为54%,2500次循环充放电后比电容仅衰减19%。最后,通过超声在泡沫镍孔隙填塞铜粉,然后浸泡反应转化为CuS,制备泡沫镍填塞CuS(NF@CuS)复合材料。CuS为六方晶系在泡沫镍孔隙中呈交联片状,厚度约为0.2μm。该复合材料具有很高的面积比电容和良好的循环稳定性,在0.090A·cm-2下复合材料面积比容达11.4 F·cm-2,循环充放电3000圈后比电容保持在85.0%。
[Abstract]:As a new type of energy storage and conversion device, supercapacitors have the advantages of higher energy density, higher power density, longer usage times and green environment protection. The improvement and optimization of electrode materials have always been the focus of supercapacitor research. How to improve the electrochemical performance of the existing electrode materials, to prepare new high performance electrode materials, to simplify the preparation process and reduce the preparation cost has become the focus of research at present. Based on the above background, this thesis has done the following research work: firstly, using carbon fiber made by ourselves in the laboratory as precursor material, infiltrating PAN/DMF solution and pre-oxidation heat treatment, the surface modified carbon fiber was prepared. The structure composition and apparent morphology were characterized by XRD,Raman,FTIR and SEM. Under the conditions of 10wt% PAN/DMF concentration, 290C calcination temperature and 1h calcination time, the specific capacitance of carbon fiber modified at 0.5A 路g-1 was 127.9 F 路g-1, which was 17.1% higher than that of carbon fiber precursor. After 5000 cycles of charge and discharge at 1.0 A 路g-1, the specific capacitance retention rate was 98.5%. Secondly, copper trihydrate (Cu (NO_3) _ 2 路3H _ 2O was used as copper source, thiourea (NH_2CSNH_2) was used as sulfur source, D-gluconate was used as complexing agent and deionized water was used as reaction solvent. Copper sulfide / carbon (CuS/C) composites were prepared by hydrothermal method. The chemical composition and micromorphology of the products were characterized by XRD,Raman,FTIR,EDS. The CuS was mainly spheroidal, the diameter of the ball was about 1 ~ 2 渭 m, and there were a lot of petal folds with average width of about 50 nm on the surface of the product. The carbon component in the composite is mainly smooth spherical and the content of carbon is about 6 wt%.. When the hydrothermal temperature is 150 鈩，
本文编号：2446044
[Abstract]:As a new type of energy storage and conversion device, supercapacitors have the advantages of higher energy density, higher power density, longer usage times and green environment protection. The improvement and optimization of electrode materials have always been the focus of supercapacitor research. How to improve the electrochemical performance of the existing electrode materials, to prepare new high performance electrode materials, to simplify the preparation process and reduce the preparation cost has become the focus of research at present. Based on the above background, this thesis has done the following research work: firstly, using carbon fiber made by ourselves in the laboratory as precursor material, infiltrating PAN/DMF solution and pre-oxidation heat treatment, the surface modified carbon fiber was prepared. The structure composition and apparent morphology were characterized by XRD,Raman,FTIR and SEM. Under the conditions of 10wt% PAN/DMF concentration, 290C calcination temperature and 1h calcination time, the specific capacitance of carbon fiber modified at 0.5A 路g-1 was 127.9 F 路g-1, which was 17.1% higher than that of carbon fiber precursor. After 5000 cycles of charge and discharge at 1.0 A 路g-1, the specific capacitance retention rate was 98.5%. Secondly, copper trihydrate (Cu (NO_3) _ 2 路3H _ 2O was used as copper source, thiourea (NH_2CSNH_2) was used as sulfur source, D-gluconate was used as complexing agent and deionized water was used as reaction solvent. Copper sulfide / carbon (CuS/C) composites were prepared by hydrothermal method. The chemical composition and micromorphology of the products were characterized by XRD,Raman,FTIR,EDS. The CuS was mainly spheroidal, the diameter of the ball was about 1 ~ 2 渭 m, and there were a lot of petal folds with average width of about 50 nm on the surface of the product. The carbon component in the composite is mainly smooth spherical and the content of carbon is about 6 wt%.. When the hydrothermal temperature is 150 鈩，
本文编号：2446044
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