CN110491682B - MOF衍生的双金属氢氧化物Ni/Co-MDH的合成及应用 - Google Patents
MOF衍生的双金属氢氧化物Ni/Co-MDH的合成及应用 Download PDFInfo
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- 229910000000 metal hydroxide Inorganic materials 0.000 title claims abstract description 14
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- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 16
- 239000012921 cobalt-based metal-organic framework Substances 0.000 claims abstract description 16
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- OYFRNYNHAZOYNF-UHFFFAOYSA-N 2,5-dihydroxyterephthalic acid Chemical compound OC(=O)C1=CC(O)=C(C(O)=O)C=C1O OYFRNYNHAZOYNF-UHFFFAOYSA-N 0.000 claims description 22
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 20
- 239000011259 mixed solution Substances 0.000 claims description 9
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 9
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- 239000000463 material Substances 0.000 abstract description 37
- 238000001308 synthesis method Methods 0.000 abstract description 3
- XTAARPJDFFXHGH-GRPBBMKTSA-N [(5s,8r,9s,10s,13s,14s,17s)-10,13-dimethyl-3-oxo-1,2,4,5,6,7,8,9,11,12,14,15,16,17-tetradecahydrocyclopenta[a]phenanthren-17-yl] propanoate Chemical compound C([C@@H]1CC2)C(=O)CC[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@H](OC(=O)CC)[C@@]2(C)CC1 XTAARPJDFFXHGH-GRPBBMKTSA-N 0.000 abstract 2
- 239000003990 capacitor Substances 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 37
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- 238000000634 powder X-ray diffraction Methods 0.000 description 4
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- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
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- ZBYYWKJVSFHYJL-UHFFFAOYSA-L cobalt(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Co+2].CC([O-])=O.CC([O-])=O ZBYYWKJVSFHYJL-UHFFFAOYSA-L 0.000 description 1
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- 229940078487 nickel acetate tetrahydrate Drugs 0.000 description 1
- OINIXPNQKAZCRL-UHFFFAOYSA-L nickel(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Ni+2].CC([O-])=O.CC([O-])=O OINIXPNQKAZCRL-UHFFFAOYSA-L 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
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Abstract
本发明提供了一种MOF衍生的双金属氢氧化物Ni/Co‑MDH的合成方法,先以DHTP、Co(Ac)2·4H2O、CTAB为原料,通过水热反应制得Co‑MOF;再将Co‑MOF、Ni(Ac)2·4H2O和CTAB分散在去离子水中,在搅拌下加入DHTP,继续通过水热反应得到前驱体Ni‑MOF@Co‑MOF;然后将Ni‑MOF@Co‑MOF充分分散于KOH溶液中,在115~125℃水热反应1.5~2h,洗涤,干燥,得到Ni/Co‑MDH纳米片。Ni/Co‑MDH材料表现出较大的比表面积和良好的热稳定性,相较于前驱体展现出较优异的电化学性能,作为超级电容器电极材料具有很好的应用前景。
Description
技术领域
本发明涉及一种双金属氢氧化物材料的制备,尤其涉及一种MOF衍生的双金属氢氧化物Ni/Co-MDH纳米片的制备方法,可作为超级电容器电极材料的应用。
背景技术
金属有机框架材料(metal organic frameworks,MOFs)是由有机桥连配体通过配位键的方式将无机金属离子簇中心连接起来形成无限延伸的网络状结构的晶体材料,是近年来发展迅速的一种新型多孔材料,由于其有序的孔道结构和较大的比表面积广泛应用于气体分离,吸附,催化,荧光,传感,载药,储能等领域。MOFs材料是由金属节点和有机配体支撑构成的二维或三维晶体结构,作为电极材料,MOFs材料独特的孔道结构为电解液的渗透和离子传输提供了通道,金属离子或离子簇中心为法拉第氧化还原反应提供了有效的活性位点,表现出赝电容行为,具有较高的比电容,因而可作为一种良好的储能材料。
发明内容
本发明的目的是提供一种MOF衍生的双金属氢氧化物Ni/Co-MDH纳米片的合成方法;
本发明的另一目的是对上述合成的双金属氢氧化物Ni/Co-MDH纳米片的电化学性能进行研究。
一、Ni/Co-MDH纳米片的合成
本发明MOF衍生的双金属氢氧化物Ni/Co-MDH材料的合成方法,包括以下步骤:
(1)Co-MOF的制备:以2,5-二羟基对苯二甲酸(DHTP)和Co(Ac)2·4H2O,十六烷基三甲基溴化胺(CTAB)为原料,以THF和水混合溶液为溶剂,在110~120℃回流2~3h,洗涤,干燥,得到Co-MOF。
2,5-二羟基对苯二甲酸(DHTP)和Co(Ac)2·4H2O的摩尔比为1:1~1:2;2,5-二羟基对苯二甲酸(DHTP)和十六烷基三甲基溴化胺的摩尔比为1:3~1:4。
THF和水的混合溶液中,THF和水的体积比为1:1~1:1.5。
(2)前驱体Ni-MOF @ Co-MOF的制备:将 Co-MOF,Ni(Ac)2·4H2O和十六烷基三甲基溴化胺(CTAB)分散在去离子水中,在搅拌下加入DHTP(2,5-二羟基对苯二甲酸)的THF溶液,搅拌0.5~1h,然后在70~80℃下回流8~9小时,洗涤,干燥,得到前驱体Ni-MOF @ Co-MOF;
Co-MOF与Ni(Ac)2·4H2O的质量比为1:1~1:2;Co-MOF与十六烷基三甲基溴化胺(CTAB)质量比为1:2~1:3;Co-MOF与2,5-二羟基对苯二甲酸的质量比为1:1~1:2。
(3)双金属氢氧化物材料(Ni/Co-MDH)的制备:将前驱体Ni-MOF @ Co-MOF充分分散于2~2.5M的KOH水溶液中搅拌2~3h后转移至反应釜中,在115~125℃水热反应1.5~2h,洗涤,干燥,得到Ni/Co-MDH纳米片。
上述各步骤中,所述干燥均是在60~70℃的真空烘箱干燥10~12小时。
二、Ni/Co-MDH的表征
1、FT-IR分析
图1为本发明合成的Ni/Co-MDH材料的FT-IR图。3440cm-1处的峰是未参与配位的-COOH中-OH伸缩振动峰,1630cm-1的吸收峰是C=O键的伸缩振动峰,3646cm-1的吸收峰是Ni/Co-MDH材料中的-OH伸缩振动峰,说明材料成功合成。
2、扫描电镜分析
图2、图3分别为前驱体Ni-MOF @ Co-MOF材料和Ni/Co-MDH材料的扫描电镜图。扫描电子显微镜照片表明,前驱体Ni-MOF @ Co-MOF呈纳米棒状,Ni/Co-MDH呈现出纳米片堆叠的疏松多孔状纳米花形态。表明通过碱处理剥离方法,将纳米棒状前驱体剥离为纳米片。
3、热重分析
图3为本发明合成的Ni/Co-MDH材料的热分析图。热分析图表明,本发明合成的Ni/Co-MDH材料热稳定性非常好,从25℃~800℃的测试条件下,最终重量保持率在52%。200℃~380℃的失重归结为材料中小分子聚合物的分解,380℃左右的失重归结为结构的坍塌。
4、X射线粉末衍射分析
图4为本发明合成的Ni/Co-MDH材料的X射线粉末衍射图。X射线粉末衍射图表明,Ni/Co-MDH材料具有较好的结晶度。
5、循环伏安测试分析
图5为本发明合成的Ni/Co-MDH材料的循环伏安图。电位窗口为0 ~0.7 V,扫速由5mV s-1增加到80 mV s-1。从图5可以清楚观察到CV曲线呈现出氧化还原峰,表明Ni/Co-MDH电极的主要行为是赝电容控制的。氧化还原峰归因于M(OH)2-MOOH(M对应于Ni或Co)之间的可逆反应。随着扫描速率的增加,氧化峰和还原峰逐渐向更正和更负方向移动,这主要归因于活性材料的电化学极化。
6、恒电流充放电测试分析
图6为本发明合成的Ni/Co-MDH材料恒电流充放电曲线图。从图6中可以发现,充放电曲线的平台显示出明显的法拉第反应,与循环伏安曲线结果一直。
7、交流阻抗测试分析
图7为本发明合成的Ni/Co-MDH材料的交流阻抗图。图7显示,在高频区,较小的半圆说明Ni/Co-MDH材料自身内阻较小;在中低频区的Warburg阻抗受制于电极-电解液界面处的离子扩散,较小的Warburg说明材料具有较短的离子扩散路径。
综上所述,本发明以2,5-二羟基对苯二甲酸,四水合乙酸钴,四水合乙酸镍和十六烷基三甲基溴化胺为原料,以THF和水为溶剂,采用水热法先制得纳米棒状前驱体Ni-MOF @Co-MOF材料,再通过碱处理剥离前驱体,制得由纳米片堆叠的疏松多孔状纳米花形态的MOF衍生的双金属氢氧化物材料Ni/Co-MDH材料。电化学性能测试表明,Ni/Co-MDH材料表现出较大的比表面积和良好的热稳定性,相较于前驱体展现出较优异的电化学性能,作为超级电容器电极材料具有很好的应用前景。
附图说明
图1为本发明合成的Ni/Co-MDH材料的红外光谱图。
图2为本发明合成的前驱体Ni-MOF @ Co-MOF材料的扫描电镜图。
图3为本发明合成的Ni/Co-MDH材料的扫描电镜图。
图4为本发明合成的Ni/Co-MDH材料的热分析图。
图5为本发明合成的Ni/Co-MDH材料的X射线粉末衍射图。
图6为本发明合成的Ni/Co-MDH材料煅烧后的循环伏安图。
图7为本发明合成的Ni/Co-MDH材料煅烧后的恒电流充放电的放电曲线图。
图8为本发明合成的Ni/Co-MDH材料煅烧后的交流阻抗图。
具体实施方式
下面通过具体实施例对本发明Ni/Co-MDH材料的合成和性能作进一步说明。
取DHTP(0.793g)和Co(Ac)2·4H2O(0.996g),溶解在100 mL THF和水(1:1/v:v)的混合溶液,并将1gCTAB加入上述混合溶液中,在120℃回流3小时,自然冷却至室温后,用去离子水和乙醇离心洗涤,并在60~70℃的真空烘箱干燥,得到Co-MOF;
取0.02g Co-MOF,0.498g Ni(Ac)2·4H2O和0.5gCTAB分散在40mL去离子水中;再向其中加入40mL含有DHTP(0.396g)的THF溶液,室温下搅拌30分钟,然后在80℃下回流8小时;用去离子水和乙醇离心洗涤,并在60~70℃的真空烘箱干燥中干燥12小时,得到0.2g前驱体Ni-MOF @ Co-MOF。
将前驱体Ni-MOF @ Co-MOF分散于30mL2M的KOH水溶液中搅拌2h后转移至反应釜中,120℃水热反应2h,用去离子水和乙醇离心洗涤,并在60~70℃的真空烘箱干燥中干燥12小时,得到Ni/Co-MDH材料。
电化学性能:上述制备的Ni/Co-MDH材料在1 A g-1,2 A g-1,5 A g-1,8A g-1,10 Ag-1,15 A g-1,20 A g-1,30 A g-1的电流密度下比电容值分别为1816 F g-1,1693 F g-1,1530 F g-1,1474 F g-1,1447 F g-1,1395 F g-1,1350 F g-1,1265 F g-1。
Claims (4)
1.MOF衍生的双金属氢氧化物Ni/Co-MDH的合成方法,包括以下步骤:
(1)Co-MOF的制备:以2,5-二羟基对苯二甲酸和Co(Ac)2·4H2O,十六烷基三甲基溴化胺为原料,以THF和水混合溶液为溶剂,在110~120℃回流2~3h,洗涤,干燥,得到Co-MOF;2,5-二羟基对苯二甲酸和Co(Ac)2·4H2O的摩尔比为1:1~1:2,2,5-二羟基对苯二甲酸和十六烷基三甲基溴化胺的摩尔比为1:3~1:4;
(2)前驱体Ni-MOF @ Co-MOF的制备:将 Co-MOF、Ni(Ac)2·4H2O和十六烷基三甲基溴化胺分散在去离子水中,在搅拌下加入2,5-二羟基对苯二甲酸的THF溶液,搅拌0.5~1h,然后在70~80℃下回流8~9小时,洗涤,干燥,得到前驱体Ni-MOF @ Co-MOF;Co-MOF与Ni(Ac)2·4H2O的质量比为1:1~1:2;Co-MOF与十六烷基三甲基溴化胺质量比为1:2~1:3;Co-MOF与2,5-二羟基对苯二甲酸的质量比为1:1~1:2;
(3)双金属氢氧化物纳米片Ni/Co-MDH的制备:将前驱体Ni-MOF @ Co-MOF充分分散于2~2.5M的KOH水溶液中,搅拌2~3h后转移至反应釜中,在115~125℃水热反应1.5~2h,洗涤,干燥,得到Ni/Co-MDH纳米片。
2.如权利要求1所述MOF衍生的双金属氢氧化物Ni/Co-MDH的合成方法,其特征在于:步骤(1)中THF和水的混合溶液中,THF和水的体积比为1:1~1:1.5。
3.如权利要求1所述MOF衍生的双金属氢氧化物Ni/Co-MDH的合成方法,其特征在于:各步骤中,所述干燥均是在60~70℃的真空烘箱干燥10~12小时。
4.如权利要求1所述方法合成的MOF衍生的双金属氢氧化物Ni/Co-MDH作为超级电容器电极材料的应用。
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