CN106430329A - 一种超级电容器电极材料及其制备方法 - Google Patents
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- 239000007772 electrode material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 6
- 239000003990 capacitor Substances 0.000 claims description 18
- 229920000742 Cotton Polymers 0.000 claims description 14
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 claims description 4
- 229910019981 La1-xCaxCoO3 Inorganic materials 0.000 claims description 4
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- 229910052746 lanthanum Inorganic materials 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000005238 degreasing Methods 0.000 claims description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000011575 calcium Substances 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 238000004146 energy storage Methods 0.000 description 4
- LTUDISCZKZHRMJ-UHFFFAOYSA-N potassium;hydrate Chemical compound O.[K] LTUDISCZKZHRMJ-UHFFFAOYSA-N 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- LLSDKQJKOVVTOJ-UHFFFAOYSA-L calcium chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Ca+2] LLSDKQJKOVVTOJ-UHFFFAOYSA-L 0.000 description 3
- 229940052299 calcium chloride dihydrate Drugs 0.000 description 3
- OQUOOEBLAKQCOP-UHFFFAOYSA-N nitric acid;hexahydrate Chemical compound O.O.O.O.O.O.O[N+]([O-])=O OQUOOEBLAKQCOP-UHFFFAOYSA-N 0.000 description 3
- 239000002482 conductive additive Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- GJKFIJKSBFYMQK-UHFFFAOYSA-N lanthanum(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GJKFIJKSBFYMQK-UHFFFAOYSA-N 0.000 description 2
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 description 2
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 2
- ZHJGWYRLJUCMRT-UHFFFAOYSA-N 5-[6-[(4-methylpiperazin-1-yl)methyl]benzimidazol-1-yl]-3-[1-[2-(trifluoromethyl)phenyl]ethoxy]thiophene-2-carboxamide Chemical compound C=1C=CC=C(C(F)(F)F)C=1C(C)OC(=C(S1)C(N)=O)C=C1N(C1=C2)C=NC1=CC=C2CN1CCN(C)CC1 ZHJGWYRLJUCMRT-UHFFFAOYSA-N 0.000 description 1
- -1 Co respectively Substances 0.000 description 1
- 229910002518 CoFe2O4 Inorganic materials 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 229910003264 NiFe2O4 Inorganic materials 0.000 description 1
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- GEYXPJBPASPPLI-UHFFFAOYSA-N manganese(III) oxide Inorganic materials O=[Mn]O[Mn]=O GEYXPJBPASPPLI-UHFFFAOYSA-N 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- NQNBVCBUOCNRFZ-UHFFFAOYSA-N nickel ferrite Chemical compound [Ni]=O.O=[Fe]O[Fe]=O NQNBVCBUOCNRFZ-UHFFFAOYSA-N 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/006—Compounds containing, besides cobalt, two or more other elements, with the exception of oxygen or hydrogen
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- 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
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Abstract
本发明公开了一种超级电容器电极材料及其制备方法,该电极材料的化学式为La1‑ xCaxCoO3,其中,0.05≤x≤0.45。本发明制备得到的电极材料具有优异的导电性能,且制备方法简单,操作便捷,适合一定规模和工业化生产。
Description
技术领域
本发明涉及一种用于超级电容器的电极材料及其制备方法。
背景技术
随着能源危机的日益加剧,新能源材料的开发和研究受到了广泛关注。其中,超级电容器作为一种新型的储能器件,兼具了电池高能量以及电容器高功率的优点,具备充电快速、电阻小、储能大、寿命长、安全可靠的特点。以金属氧化物作为电极材料的赝电容器是近年来新提出的储能器件,由于其储能密度是双电层电容器的 10~100倍以上,逐步取代双电层电容器成为人们研究的热点。
目前,大多数用于赝电容器的金属氧化物都是过渡金属氧化物,例如NiO,Co2O3,Fe3O4,Mn2O3, RuO2,NiFe2O4,CoFe2O4等等。这类材料具有环境友好、低成本等优点,但是它们的电阻值较高,后期进行器件组装时还需要加入导电添加物,实际应用过程中的比电容值还是远低于理论值。
发明内容
本发明的目的是为了解决现有技术中存在的缺陷,提供一种比电容值高、成本低廉的电极材料。
为了达到上述目的,本发明提供了一种超级电容器电极材料,该电极材料的化学式为La1-xCaxCoO3,其中,0.05≤x≤0.45。其中x优选范围:0.25~0.37。
本发明还提供了上述电极材料的制备方法,包括以下步骤:
(1)分别取金属La、Ca、Co的硝酸盐或氯化盐,以及柠檬酸,加入水中,搅拌均匀得到混合溶液;所述金属La、Ca、Co的摩尔比为1-x:x:1,其中,0.05≤x≤0.45;所述柠檬酸与金属Co的摩尔比为2:1~3:1;
(2)取脱脂棉加入步骤(1)中制备的混合溶液中,吸附5~30min后得到脱脂棉/溶液混合物;所述脱脂棉的加入量为每0.1mol金属Co取10~40g;
(3)将步骤(2)制备得到的混合物放置在烘箱中,100~140℃下干燥2~5h后得到前驱体;
(4)将步骤(3)中制备得到的前驱体置于马弗炉中,以升温速率8~15℃/min加热到800~1000℃,保温1~3 h,即可得到所述La1-xCaxCoO3。
本发明相比现有技术具有以下优点:
1. 本发明制备的La1-x Ca x CoO3,其内部结构中的电子可以在不同价态的离子之间跃迁,具有优异的导电性,在后期器件组装过程中可以极大的减少导电添加物的用量。
2. 本发明制备的超级电容器电极材料具有较高的比电容值,并且循环稳定特性优异。
3. 本发明的超级电容器电极材料制备方法简单,操作便捷,适合一定规模和工业化生产。
附图说明
图1为本发明实施例1制备得到的电极材料的XRD图;
图2为本发明实施例2制备得到的电极材料的SEM图;
图3为本发明实施例3制备得到的电极材料的比电容值随扫描速率的变化关系图。
具体实施方式
下面结合实施例对本发明作进一步说明,但不应以此限制本发明的保护范围。
实施例1
(1)称取41.136g六水合硝酸镧、1.181g四水合硝酸钙、29.103g六水合硝酸钴和46.231g一水合柠檬酸加入到去离子水中(去离子水的加入量以充分溶解为宜),均匀搅拌后制得混合溶液;
(2)称取40g脱脂棉加入到混合溶液中,吸附30min后得到脱脂棉/溶液混合物;
(3)将步骤(2)的混合物放置在烘箱中,140℃干燥2h得到前驱体;
(4)将前驱体置于马弗炉中,以升温速率8℃/min加热到1000℃,保温3 h,即可得到超级电容器用电极材料La0.95Ca0.05CoO3。
经测定,所制备的超级电容器电极材料表现为纯相的钙钛矿结构,其XRD图谱如图1所示。当扫描速度为50mV/s时,比电容值达到817F/g,表现出优异的电化学性能。
实施例2:
(1)称取36.806g六水合硝酸镧、2.205g二水合氯化钙、23.793g六水合氯化钴和55.752g一水合柠檬酸加入到去离子水中,均匀搅拌后制得混合溶液;
(2)称取30g脱脂棉加入到混合溶液中,吸附5min后得到脱脂棉/溶液混合物;
(3)将步骤(2)的混合物放置在烘箱中,100℃干燥5h得到前驱体;
(4)将前驱体置于马弗炉中,以升温速率15℃/min加热到800℃,保温1h,即可得到超级电容器用电极材料La0.85Ca0.15CoO3。
经测定,当扫描速度为50mV/s时,所制备的超级电容器电极材料的比电容值达到875F/g,表现出优异的电化学性能。所制备材料的微观形貌图如图2所示,从图中可以看出,制得的超级电容器电极材料呈现无规则纳米颗粒形貌,颗粒粒径为30~100nm,具备较高的比表面积。。
实施例3:
(1)称取25.996g七水合氯化镧、4.410g二水合氯化钙、29.103g六水合硝酸钴和63.042g一水合柠檬酸加入到去离子水中,均匀搅拌后制得混合溶液;
(2)称取25g脱脂棉加入到混合溶液中,吸附10min后得到脱脂棉/溶液混合物;
(3)将步骤(2)的混合物放置在烘箱中,120℃干燥4h得到前驱体;
(4)将前驱体置于马弗炉中,以升温速率10℃/min加热到900℃,保温2h,即可得到超级电容器用电极材料La0.7Ca0.3CoO3。
图3所示为制备得到的电极材料的比电容值随扫描速率的变化关系图,从图中可以看出当扫描速度为50mV/s时,所制备的超级电容器电极材料的比电容值达到975F/g,表现出优异的电化学性能。
实施例4:
(1)称取20.425g七水合氯化镧、6.615g二水合氯化钙、23.793g六水合硝酸钴和42.028g一水合柠檬酸加入到去离子水中,均匀搅拌后制得混合溶液;
(2)称取10g脱脂棉加入到混合溶液中,吸附20min后得到脱脂棉/溶液混合物;
(3)将步骤(2)的混合物放置在烘箱中,110℃干燥3h得到前驱体;
(4)将前驱体置于马弗炉中,以升温速率12℃/min加热到900℃,保温2 h,即可得到超级电容器用电极材料。
经测定,当扫描速度为50mV/s时,所制备的超级电容器电极材料的比电容值达到930F/g,表现出优异的电化学性能。
Claims (4)
1.一种超级电容器电极材料,其特征在于:所述电极材料的化学式为La1-xCaxCoO3,其中,0.05≤x≤0.45。
2.根据权利要求1所述的电极材料,其特征在于:所述x的取值范围为:0.25~0.37。
3.权利要求1所述电极材料的制备方法,其特征在于:包括以下步骤:
(1)分别取金属La、Ca、Co的硝酸盐或氯化盐,以及柠檬酸,加入水中,搅拌均匀得到混合溶液;所述金属La、Ca、Co的摩尔比为1-x:x:1,其中,0.05≤x≤0.45;所述柠檬酸与金属Co的摩尔比为2:1~3:1;
(2)取脱脂棉加入步骤(1)中制备的混合溶液中,吸附5~30min后得到脱脂棉/溶液混合物;所述脱脂棉的加入量为每0.1mol金属Co取10~40g;
(3)将步骤(2)制备得到的混合物放置在烘箱中,100~140℃下干燥2~5h后得到前驱体;
(4)将步骤(3)中制备得到的前驱体置于马弗炉中,以升温速率8~15℃/min加热到800~1000℃,保温1~3 h,即可得到所述La1-xCaxCoO3。
4.根据权利要求3所述的制备方法,其特征在于:所述x的取值范围为:0.25~0.37。
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