CN107324407B - 一种NiCo2O4六方柱晶体及其制备方法 - Google Patents
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- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 claims abstract description 6
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 15
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- 229910017052 cobalt Inorganic materials 0.000 description 1
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Abstract
一种NiCo2O4六方柱晶体及其制备方法,首先,按照摩尔比称取Ni(NO3)2·6H2O和Co(NO3)2·6H2O,溶于去离子水中配制成溶液A,称取强碱,溶于去离子水中配置成溶液B,其次,将溶液B迅速转移进入溶液A中,强力搅拌得到混合溶液,将混合溶液在抽真空条件下在下进行旋蒸,得到前驱体,再次,将前驱体取出,离心固液分离,水洗,醇洗,干燥,最后,将干燥后的前驱体取出研磨,煅烧,即得到六方柱状NiCo2O4晶体,采用旋蒸法制备NiCo2O4六方柱晶体,制备出的NiCo2O4六方柱晶体具有微米级尺寸,且形貌均一、尺寸规整、结晶度较高,具有原料廉价易得、制备工艺简单、重复性强、成本较低、对环境危害小的特点。
Description
技术领域
本发明属于无机晶体材料制备技术领域,特别涉及一种NiCo2O4六方柱晶体及其制备方法。
背景技术
双金属氧化物NiCo2O4具有尖晶石晶体结构,由于其独特的结构特征,在磁性材料、传感器、电化学储能、光电催化等领域具有广泛的应用。NiCo2O4的形貌结构与其性能有着直接紧密的联系,如具有分级多孔结构的NiCo2O4作为超级电容器电极材料时,可使电子和离子传输路径变短,接触位点更多,从而可有效提高电化学活性。因此,对NiCo2O4实现特定形貌的可控制备具有非常重要的应用价值。
目前,已报道的NiCo2O4的形貌非常丰富,有纳米线、纳米花、纳米棒、纳米管、纳米片和纳米针等形貌。制备方法也层出不穷,如共沉淀法、喷雾热解法、溶胶凝胶法、电沉积法、静电纺丝法、模板法等。福州大学郑玉婴等人(中国专利,公开号CN 106315695 A) 发明了一种杨梅状钴酸镍纳米材料及其制备方法,该方法是利用水热法制备得到了杨梅状钴酸镍纳米微球,表面生长整齐排列的纳米棒,具有较大比表面积,可应用于超级电容器电极材料。但水热法对设备材质要求高,反应温度相对较高,反应时间长(9-15h),且需进行真空干燥,在实际生产中有一定的局限性。中国专利CN 106315695 A 公开了一种多孔钴酸镍材料的溶胶凝胶制备方法,该专利利用溶胶凝胶法结合后续煅烧工艺制备得到多孔钴酸镍,孔径分布均匀且尺寸小于200nm。但该法同样存在反应时间过长(12-16h),反应温度高的问题,而且需要粉碎过筛,工艺繁琐。徐开兵(中国专利,公开号 CN 106067388 A)发明了钴酸镍纳米材料及其复合电极材料的制备方法,该方法采用高压静电纺丝技术实现了钴酸镍纳米线和纳米管的可控制备,但也存在设备昂贵复杂,能耗较高,且需额外引入高分子聚合物等不足。Chen等人(Chen J,Ru Q,Mo Y,et al.Design and synthesis of hollow NiCo2O4nanoboxes as anodes for lithium-ion and sodium-ion batteries.[J].PhysicalChemistry Chemical Physics,2016,18(28):18949.) 以ZIF-67作为模板剂结合随后的退火处理制备得到中空多孔 NiCo2O4纳米箱,当其被用作锂离子电池负极材料时,表现出较高的储锂性能。但上述研究中NiCo2O4前躯体的合成有两个阶段,即 ZIF-67晶体的合成与NiCo2O4纳米箱的制备,工艺复杂,且原料中甲醇毒性较大,在实际应用中局限很大。
现有技术中所制备的NiCo2O4绝大多数具有纳米级尺寸,并未发现微米级NiCo2O4规则六方柱晶体的相关报道,且制备方法也没有涉及旋蒸技术。
发明内容
为了克服上述现有技术的缺点,本发明的目的在于提供一种 NiCo2O4六方柱晶体及其制备方法,采用旋蒸法制备NiCo2O4六方柱晶体,制备出的NiCo2O4六方柱晶体具有微米级尺寸,且形貌均一、尺寸规整、结晶度较高,具有原料廉价易得、制备工艺简单、重复性强、成本较低、对环境危害小的特点。
为了达到上述目的,本发明采取的技术方案为:
一种NiCo2O4六方柱晶体,所述NiCo2O4为六方柱状规则晶体,晶体尺寸为0.5-2μm。
一种NiCo2O4六方柱晶体的制备方法,步骤如下:
步骤1:按照摩尔比1:(1.6-2.4)称取Ni(NO3)2·6H2O和 Co(NO3)2·6H2O,将Ni(NO3)2·6H2O溶于去离子水中配制成溶液,再将Co(NO3)2·6H2O溶于溶液中,得到溶液A;
步骤2:按照强碱与Ni(NO3)2·6H2O摩尔比为(100-300):1称取强碱,溶于去离子水中配置成溶液B;
步骤3:将溶液B迅速转移进入溶液A中,在600-1500r/min转速下搅拌2-20min,得 到混合溶液;
步骤4:将混合溶液转移进入旋蒸容器中并固定于旋转蒸发仪上,抽真空条件下在50-90℃下进行旋蒸,旋蒸时间0.5-3h,得到前驱体;
步骤5:将前驱体取出,离心固液分离,水洗至洗出液pH为7,再醇洗;
步骤6;将醇洗后的前驱体放入恒温干燥箱中进行干燥;
步骤7:将干燥后的前驱体取出研磨至粒度为100-300目, 200-400℃下煅烧2-6h,即得到六方柱状NiCo2O4晶体。
所述步骤2强碱采用NaOH。
所述步骤4的旋蒸容器采用茄形烧瓶。
所述步骤5醇洗采用无水乙醇,醇洗次数为2-5次。
所述步骤6干燥温度为40-120℃,干燥时间为10-24h。
本发明与现有技术相比的有益效果为:
所制备的NiCo2O4晶体为六方柱状,形貌均一、尺寸规整,晶体尺寸在0.5-2μm之间,结晶度较高。
本发明采用廉价易得的常规原料Ni(NO3)2·6H2O和 Co(NO3)2·6H2O,对环境危害小;所采用的旋蒸法工艺简单,抽真空条件下在50-90℃下进行旋蒸,旋蒸时间0.5-3h,反应温度低、时间短、制备周期短,成本较低,并可通过旋蒸参数的调整对NiCo2O4六方柱晶体进行不同尺寸的可控制备,如:控制抽真空条件下,温度 80℃,旋蒸时间0.5h,可制备出粒径约为0.75-0.9μm规则尺寸的 NiCo2O4六方柱晶体。本发明可重复操作性强,所制备的产品稳定性好,在催化、能源等领域具有良好的应用前景,如将NiCo2O4六方柱晶体制成超级电容器电极材料,比电容可达568F/g,具有较高的比电容和良好的电化学稳定性,是一种理想的超级电容器电极材料。
附图说明
图1为本发明中旋蒸法制备产物的XRD图谱。
图2为旋蒸法制备产物NiCo2O4的SEM照片。
图3为旋蒸法制备产物NiCo2O4的TEM照片。
图4(a)为NiCo2O4六方柱的SEM照片;(b)为NiCo2O4六方柱的EDS图谱。
图5为NiCo2O4六方柱晶体在不同扫速下的循环伏安曲线。
图6(a)为NiCo2O4六方柱晶体在不同电流密度下的充放电曲线(a);图6(b)为NiCo2O4六方柱晶体在不同电流密度下的比电容值。
具体实施方式
下面结合实施例对本发明做进一步详细说明。
实施例一:
步骤1:按照摩尔比1:2称取Ni(NO3)2·6H2O和Co(NO3)2·6H2O,将Ni(NO3)2·6H2O溶于去离子水中配制成溶液,再将Co(NO3)2·6H2O 溶于溶液中,得到溶液A。
步骤2:按照NaOH与Ni(NO3)2·6H2O摩尔比为200:1称取NaOH,溶于去离子水中配置成溶液B。
步骤3:将溶液B迅速转移进入溶液A中,1200r/min转速下搅拌5min,得到混合溶 液。
步骤4:将混合溶液转移进入茄形烧瓶中并固定于旋转蒸发仪上,抽真空条件下在80℃下进行旋蒸,旋蒸时间0.5h,得到前驱体。
步骤5:将前驱体取出,离心分离,水洗至洗出液pH为7,再采用无水乙醇进行醇洗3次。
步骤6;将醇洗后的前驱体放入恒温干燥箱中,60℃干燥24h;
步骤7:将干燥后的前驱体取出研磨至粒度为100目,300℃下煅烧5h,即得到六方柱状NiCo2O4晶体。
参见图1,可以看出所有衍射峰均与纯相NiCo2O4的标准谱 (JCPDS No.20-0781)相吻合,无其他杂相生成,证明所得产物为结晶良好的NiCo2O4。
参见图2,可以明显观察到,所得NiCo2O4为六方柱状规则晶体,尺寸约为0.85μm,发育良好。
参见图3,可以明显观察到,所得NiCo2O4为规则六方柱晶体,发育良好,与图2所示形貌完全一致。
参见图4,本发明采用旋蒸法制备产物的EDS图谱,Ni、Co、O 的原子比近似等于1:2:4,符合NiCo2O4的化学组成。
本发明所制备的NiCo2O4六方柱晶体在催化、能源等领域具有良好的应用前景。如将NiCo2O4六方柱晶体制成超级电容器电极材料,进行循环伏安及恒流充放电测试,1A/g电流密度下比电容可达 568F/g,具有较大的比电容值。且大扫速下循环伏安曲线未出现明显的扭曲,产品表现出良好的倍率性能及电化学稳定性,是一种理想的超级电容器电极材料。
参见图5,可以看出,当扫描速率从5mV/s依次增大至100mV/s,循环伏安曲线形状保持完好,未出现明显的扭曲,证明该发明产物具有良好的倍率性能及电化学稳定性。
参见图6,充放电曲线表现为典型的赝电容超级电容器电极材料的形状特征,具有明显的充放电平台,且充放电曲线对称,表明本发明中旋蒸法制备产物具有出色的电化学可逆性。同时可观察到,1A/g 电流密度下比电容可达568F/g,具有较大的比电容值,16A/g大电流密度下比电容依然高达403F/g,具有优异的倍率性能。
实施例二:
步骤1:按照摩尔比1:1.6称取Ni(NO3)2·6H2O和Co(NO3)2·6H2O,将Ni(NO3)2·6H2O溶于去离子水中配制成溶液,再将Co(NO3)2·6H2O 溶于溶液中,得到溶液A。
步骤2:按照NaOH与Ni(NO3)2·6H2O摩尔比为300:1称取NaOH,溶于去离子水中配置成溶液B。
步骤3:将溶液B迅速转移进入溶液A中,600r/min转速下搅拌20min,得到混合溶 液。
步骤4:将混合溶液转移进入茄形烧瓶中并固定于旋转蒸发仪上,抽真空条件下在50℃下进行旋蒸,旋蒸时间3h,得到前驱体。
步骤5:将前驱体取出,离心分离,水洗至洗出液pH为7,再采用无水乙醇进行醇洗2次。
步骤6;将醇洗后的前驱体放入恒温干燥箱中,120℃干燥18h;
步骤7:将干燥后的前驱体取出研磨至粒度为300目,200℃下煅烧6h,即得到六方柱状NiCo2O4晶体。
实施例三:
步骤1:按照摩尔比1:2.4称取Ni(NO3)2·6H2O和Co(NO3)2·6H2O,将Ni(NO3)2·6H2O溶于去离子水中配制成溶液,再将Co(NO3)2·6H2O 溶于溶液中,得到溶液A。
步骤2:按照NaOH与Ni(NO3)2·6H2O摩尔比为100:1称取NaOH,溶于去离子水中配置成溶液B。
步骤3:将溶液B迅速转移进入溶液A中,1500r/min转速下搅拌2min,得到混合溶 液。
步骤4:将混合溶液转移进入茄形烧瓶中并固定于旋转蒸发仪上,抽真空条件下在90℃下进行旋蒸,旋蒸时间1.5h,得到前驱体。
步骤5:将前驱体取出,离心分离,水洗至洗出液pH为7,再采用无水乙醇进行醇洗5次。
步骤6;将醇洗后的前驱体放入恒温干燥箱中,40℃干燥10h;
步骤7:将干燥后的前驱体取出研磨至粒度为200目,400℃下煅烧2h,即得到六方柱状NiCo2O4晶体。
Claims (5)
1.一种NiCo2O4六方柱晶体,其特征在于,所述NiCo2O4为六方柱状规则晶体,晶体尺寸为0.5-2μm,其制备方法步骤如下:
步骤1:按照摩尔比1:(1.6-2.4)称取Ni(NO3)2·6H2O和Co(NO3)2·6H2O,将Ni(NO3)2·6H2O溶于去离子水中配制成溶液,再将Co(NO3)2·6H2O溶于溶液中,得到溶液A;
步骤2:按照强碱与Ni(NO3)2·6H2O摩尔比为(100-300):1称取强碱,溶于去离子水中配置成溶液B;
步骤3:将溶液B迅速转移进入溶液A中,在600-1500r/min转速下搅拌2-20min,得到混合溶液;
步骤4:将混合溶液转移进入旋蒸容器中并固定于旋转蒸发仪上,抽真空条件下在50-90℃下进行旋蒸,旋蒸时间0.5-3h,得到前驱体;
步骤5:将前驱体取出,离心固液分离,水洗至洗出液pH为7,再醇洗;
步骤6:将醇洗后的前驱体放入恒温干燥箱中进行干燥;
步骤7:将干燥后的前驱体取出研磨至粒度为100-300目,200-400℃下煅烧2-6h,即得到六方柱状NiCo2O4晶体。
2.根据权利要求1所述的一种NiCo2O4六方柱晶体的制备方法,其特征在于,所述步骤2强碱采用Na OH。
3.根据权利要求1所述的一种NiCo2O4六方柱晶体的制备方法,其特征在于,所述步骤4的旋蒸容器采用茄形烧瓶。
4.根据权利要求1所述的一种NiCo2O4六方柱晶体的制备方法,其特征在于,所述步骤5醇洗采用无水乙醇,醇洗次数为2-5次。
5.根据权利要求1所述的一种NiCo2O4六方柱晶体的制备方法,其特征在于,所述步骤6干燥温度为40-120℃,干燥时间为10-24h。
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