超級電容器新型電極材料的制備及其性能研究
發(fā)布時間：2019-03-23 16:57
【摘要】：作為新型能量存儲與轉(zhuǎn)換裝置,超級電容器所具有的優(yōu)點包括較高的能量密度功率密度、較長的使用次數(shù)和綠色環(huán)保等。電極材料的改進和優(yōu)化一直是超級電容器研究的重點。如何改善現(xiàn)有電極材料電化學(xué)性能、制備新型高性能的電極材料以及簡化制備工藝和降低制備成本成為目前的研究重點。基于以上背景,本論文做了如下的研究工作:首先,本文以實驗室自制的碳纖維作為前體材料,浸潤PAN/DMF溶液后進行預(yù)氧化熱處理,制備表面改性的碳纖維。利用XRD、Raman、FTIR和SEM對結(jié)構(gòu)組成和表觀形貌進行了表征。采用PAN/DMF濃度10wt%、煅燒溫度290℃和鍛燒時間1h條件下表面改性的碳纖維,在電流密度為0.5 A·g-1時比電容為127.9 F·g-1,比碳纖維前體提高約17.1%,1.0 A·g-1下循環(huán)充放電5000次后比電容保持率為98.5%。其次,以三水合硝酸銅(Cu(NO_3)_2·3H_2O)為銅源,硫脲(NH_2CSNH_2)為硫源,D-葡萄糖酸鈉為絡(luò)合劑,去離子水為反應(yīng)溶劑,通過水熱方法"一鍋"制備了硫化銅/碳(CuS/C)復(fù)合材料。采用XRD、Raman、FTIR、EDS分析產(chǎn)物化學(xué)組成和微觀形貌進行了表征。產(chǎn)物中CuS主要呈球花狀,球的直徑約在1～2μm,表面分布有大量平均寬度在50 nm左右的花瓣狀褶皺。復(fù)合材料中的碳組分主要呈光滑球狀,含量約6 wt%。當水熱溫度為150℃和水熱反應(yīng)時間為24 h時,所制備的CuS/C復(fù)合材料在1 A·g-1的比電容達719.6 F·g1,1000圈后比電容僅衰減20%,綜合電化學(xué)性能良好。接著,以泡沫鎳作為基體材料,先通過水熱法在泡沫鎳孔道內(nèi)填塞了亞微米級碳球,提高整個基體的比表面積,隨后以六水合氯化鎳(NiCl_2·6H_2O)為鎳源,硫脲為硫源,通過水熱法在碳球表面生長Ni_3S_2,制備泡沫鎳@碳球@硫化鎳(NF@CMSs@Ni_3S_2)復(fù)合材料。采用XRD、Raman、SEM、EDS和TEM對元素組成和表面形貌進行表征。當電流密度為0.008 A·cm-2時,復(fù)合材料的面積比電容達7.10 F·cm-2,電流密度增大到0.056 A·cm-2時,面積比電容保持率為54%,2500次循環(huán)充放電后比電容僅衰減19%。最后,通過超聲在泡沫鎳孔隙填塞銅粉,然后浸泡反應(yīng)轉(zhuǎn)化為CuS,制備泡沫鎳填塞CuS(NF@CuS)復(fù)合材料。CuS為六方晶系在泡沫鎳孔隙中呈交聯(lián)片狀,厚度約為0.2μm。該復(fù)合材料具有很高的面積比電容和良好的循環(huán)穩(wěn)定性,在0.090A·cm-2下復(fù)合材料面積比容達11.4 F·cm-2,循環(huán)充放電3000圈后比電容保持在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，
本文編號：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，
本文編號：2446044
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