CN107069025A - 一种层状钴酸锰材料及其制备方法 - Google Patents
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- 239000000463 material Substances 0.000 title claims abstract description 65
- 239000011572 manganese Substances 0.000 title claims abstract description 54
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 53
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000010941 cobalt Substances 0.000 title claims abstract description 51
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 27
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 16
- 239000004202 carbamide Substances 0.000 claims description 16
- 229940011182 cobalt acetate Drugs 0.000 claims description 15
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 15
- 239000012046 mixed solvent Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 229940071125 manganese acetate Drugs 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 9
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 229910018669 Mn—Co Inorganic materials 0.000 claims description 8
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 229940045136 urea Drugs 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 9
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 3
- 241000446313 Lamella Species 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract 1
- 238000002474 experimental method Methods 0.000 description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 4
- 229910003168 MnCo2O4 Inorganic materials 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000005979 thermal decomposition reaction Methods 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 229910021380 Manganese Chloride Inorganic materials 0.000 description 2
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 235000002867 manganese chloride Nutrition 0.000 description 2
- 239000011565 manganese chloride Substances 0.000 description 2
- 229940099607 manganese chloride Drugs 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 1
- 229940099596 manganese sulfate Drugs 0.000 description 1
- 235000007079 manganese sulphate Nutrition 0.000 description 1
- 239000011702 manganese sulphate Substances 0.000 description 1
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
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Abstract
一种层状钴酸锰材料及其制备方法,涉及一种钴酸锰材料及其制备方法。本发明是为了解决目前钴酸锰合成过程中易产生杂质、形貌多为球形,特殊形貌较少的技术问题。本发明的层状钴酸锰材料为层状堆叠的立方体结构。本发明的层状钴酸锰材料的制备方法:一、混合原料;二、溶剂热反应;三、离心分离、洗涤,真空条件干燥;四、焙烧。本发明的优点在于:本发明所采用的溶剂热法操作简单,成本低廉,且此制备方法所得产物纯度高,晶型好,且可控,重现性较佳。本发明所制得的钴酸锰材料为片层堆叠起来的立方体结构,其层与层之间的缝隙有效地提高材料的比表面积,从而增加了材料的活性位点,因此有助于提高材料的性能。
Description
技术领域
本发明涉及一种钴酸锰材料及其制备方法。
背景技术
具有尖晶石结构的材料是一种重要的功能材料,由于其具有结构稳定,组成多样性且带隙窄等特点,能够通过阳离子的置换或者替代,易于形成连续固溶体,不仅丰富了固态类化学信息,而且有助于构筑多层结构的复合氧化物,因此被广泛应用于光电功能材料、磁材料以及传感器等诸多领域。钴酸锰(MnCo2O4)作为一种典型的尖晶石结构的材料,目前已经被广泛研究,并且被报道可以应用在光催化、锂离子电池负极材料、超级电容器电极材料等方面。但是,由于锰元素的价态较多,在合成钴酸锰的过程中易产生Mn2O3、MnO2等杂质,纯相的MnCo2O4较难合成。并且其合成方法主要为水热法、溶剂热法以及热分解法等,所制备的结构多为常见的球形,其他特殊形貌较少。因此,探索合成各种形貌的钴酸锰材料成为提高钴酸锰材料的性能的重要方法之一。
Qian等人以氯化锰和氯化钴为前驱体,乙二醇为溶剂,采用溶剂热-热分解法制备了中空球形的钴酸锰材料,并用于超级电容器电极材料(Jingfa Li,Shenglin Xiong,Xiaowei Li and Yitai Qian.Nanoscale,2013,5,2045-2054)。Yuan等人同样以氯化锰和氯化钴为前驱体,次氮基三乙酸为螯合剂,水和异丙醇为溶剂,利用溶剂热-热分解法制备了钴酸锰纳米线(Yanan Xu,Xiaofeng Wang,Cuihua An,Yijing Wang,Lifang Jiao andHuatang Yuan.J.Mater.Chem.A,2014,2,16480-16488)。Wang等也以硫酸锰和硫酸钴为前驱体合成出钴酸锰微米球(Shunchao Ma,Liqun Sun,Lina Cong,Xuguang Gao,Cen Yao,Xin Guo,Linghua Tai,Peng Mei,Yanping Zeng,Haiming Xie,and RongshunWang.J.Phys.Chem.C,2013,117,25890-25897)。可见,合成各种形貌的钴酸锰材料是目前所研究的热点,并且通过改进钴酸锰的形貌,可以大大提高其性能。
发明内容
本发明是为了解决目前钴酸锰合成过程中易产生杂质、形貌多为球形,特殊形貌较少的技术问题,而提供一种层状钴酸锰材料及其制备方法。
本发明的一种层状钴酸锰材料为层状堆叠的立方体结构,边长为4μm~5μm,三个相邻的面为光滑的,另外三个面具有堆叠层状,单层的厚度为10nm~20nm,层与层的间距为100nm~150nm。
本发明的一种层状钴酸锰材料的制备方法是按以下进行的:
一、将醋酸锰、醋酸钴和尿素溶解在混合溶剂中,搅拌均匀形成粉红色的原料混合溶液;所述的醋酸锰和醋酸钴的物质的量的比为1:(1.5~2.5);所述的醋酸钴和尿素的物质的量的比为1:(13~15);所述的混合溶剂是由水和乙二醇的混合组成,水和乙二醇的体积比为1:2;所述的尿素的物质的量和混合溶剂的体积比为1mmol:(3mL~5mL);
二、将步骤一的粉红色的原料混合溶液密封在水热反应釜中,在温度为150℃~210℃的条件下进行溶剂热反应5.5h~7h,自然冷却至室温;
三、将步骤二中冷却后的产物离心分离,然后用乙醇水溶液洗涤三次,在60℃和真空条件下干燥12h~16h,得到粉红色的Mn-Co前驱体;所述的乙醇水溶液中水和乙醇的体积比为1:2;
四、将步骤三中的粉红色的Mn-Co前驱体在温度为500℃~600℃的条件下,在空气中焙烧3h~4h,得到层状钴酸锰材料。
本发明步骤中须严格控制反应物的量,反应物浓度过高,所制得的钴酸锰成球形,反应物浓度过低,所制得的钴酸锰成四周光滑的立方体结构。
本发明步骤中须严格控制反应温度,反应温度过低,所制得的钴酸锰成纳米片结构。
本发明步骤中须严格控制反应时间,反应时间过短,则反应不完全,得到的产物为多种形貌的混合物。
本发明的优点在于:
本发明所采用的溶剂热法操作简单,成本低廉,且此制备方法所得产物纯度高,晶型好,且可控,重现性较佳。
本发明所制得的钴酸锰材料为片层堆叠起来的立方体结构,其层与层之间的缝隙有效地提高了材料的比表面积,从而增加了材料的活性位点,因此有助于提高材料的性能。
附图说明
图1为试验一制备的层状钴酸锰的XRD图谱;
图2为试验一制备的层状钴酸锰的EDS能谱图;
图3为试验一制备的层状钴酸锰的低倍扫描电镜图;
图4为试验一制备的层状钴酸锰的高倍扫描电镜图;
图5为试验一制备的层状钴酸锰的高倍扫描电镜图。
具体实施方式:
具体实施方式一:本实施方式为一种层状钴酸锰材料,所述的层状钴酸锰材料为层状堆叠的立方体结构,边长为4μm~5μm,三个相邻的面为光滑的,另外三个面具有堆叠层状,单层的厚度为10nm~20nm,层与层的间距为100nm~150nm。
具体实施方式二:本实施方式为具体实施方式一中层状钴酸锰材料的制备方法,具体是按以下进行的:
一、将醋酸锰、醋酸钴和尿素溶解在混合溶剂中,搅拌均匀形成粉红色的原料混合溶液;所述的醋酸锰和醋酸钴的物质的量的比为1:(1.5~2.5);所述的醋酸钴和尿素的物质的量的比为1:(13~15);所述的混合溶剂是由水和乙二醇的混合组成,水和乙二醇的体积比为1:2;所述的尿素的物质的量和混合溶剂的体积比为1mmol:(3mL~5mL);
二、将步骤一的粉红色的原料混合溶液密封在水热反应釜中,在温度为150℃~210℃的条件下进行溶剂热反应5.5h~7h,自然冷却至室温;
三、将步骤二中冷却后的产物离心分离、然后用乙醇水溶液洗涤三次,在60℃和真空条件下干燥12h~16h,得到粉红色的Mn-Co前驱体;所述的乙醇水溶液中水和乙醇的体积比为1:2;
四、将步骤三中的粉红色的Mn-Co前驱体在温度为500℃~600℃的条件下,在空气中焙烧3h~4h,得到层状钴酸锰材料。
具体实施方式三:本实施方式与具体实施方式二不同的是:步骤一中所述的醋酸锰和醋酸钴的物质的量的比为1:2。其它与具体实施方式二相同。
具体实施方式四:本实施方式与具体实施方式二不同的是:步骤一中所述的醋酸钴和尿素的物质的量的比为1:15。其它与具体实施方式二相同。
具体实施方式五:本实施方式与具体实施方式二不同的是:步骤一中所述的尿素的物质的量和混合溶剂的体积比为1mmol:4mL。其它与具体实施方式二相同。
通过以下试验验证本发明的效果:
试验一:本试验为一种层状钴酸锰材料的制备方法,具体是按以下进行的:
一、将醋酸锰、醋酸钴和尿素溶解在混合溶剂中,搅拌均匀形成粉红色的原料混合溶液;所述的醋酸锰和醋酸钴的物质的量的比为1:2;所述的醋酸钴和尿素的物质的量的比为1:15;所述的混合溶剂是由水和乙二醇的混合组成,水和乙二醇的体积比为1:2;所述的尿素的物质的量和混合溶剂的体积比为1mmol:4mL;
二、将步骤一的粉红色的原料混合溶液密封在水热反应釜中,在温度为150℃的条件下进行溶剂热反应5.5h,自然冷却至室温;
三、将步骤二中冷却后的产物离心分离,然后用乙醇水溶液洗涤三次,在60℃和真空条件下干燥12h,得到粉红色的Mn-Co前驱体;所述的乙醇水溶液中水和乙醇的体积比为1:2;
四、将步骤三中的粉红色的Mn-Co前驱体在温度为600℃的条件下,在空气中焙烧4h,得到层状钴酸锰材料。
图1为试验一制备的层状钴酸锰的XRD图谱,图中的几个主要衍射峰与MnCo2O4的标准数据库(JCPDS card,No:23-1237)相一致,证明得到的产物为纯净的MnCo2O4单相。
图2为试验一制备的层状钴酸锰的EDS能谱图,表1为相应的数据表格,从图中可以看出所制得的材料含有Mn、Co和O等元素,且Mn、Co和O的比例接近于1:2:4,进一步验证了MnCo2O4材料的形成。
表1
图3为试验一制备的层状钴酸锰的低倍扫描电镜图,从图中可以看出所制得的材料为层状堆叠的立方体结构,大小均一,边长为4μm~5μm。
图4和5为试验一制备的层状钴酸锰的高倍扫描电镜图,从图中可以看出立方体的MnCo2O4材料有三个相邻的面是光滑的(图5),另外三个面是堆叠层状(图4),单层的厚度为10nm~20nm,层与层的间距为100nm~150nm。
Claims (5)
1.一种层状钴酸锰材料,其特征在于所述的层状钴酸锰材料为层状堆叠的立方体结构,边长为4μm~5μm,三个相邻的面为光滑的,另外三个面具有堆叠层状,单层的厚度为10nm~20nm,层与层的间距为100nm~150nm。
2.如权利要求1所述的一种层状钴酸锰材料的制备方法,其特征在于层状钴酸锰材料的制备方法是按以下进行的:
一、将醋酸锰、醋酸钴和尿素溶解在混合溶剂中,搅拌均匀形成粉红色的原料混合溶液;所述的醋酸锰和醋酸钴的物质的量的比为1:(1.5~2.5);所述的醋酸钴和尿素的物质的量的比为1:(13~15);所述的混合溶剂是由水和乙二醇的混合组成,水和乙二醇的体积比为1:2;所述的尿素的物质的量和混合溶剂的体积比为1mmol:(3mL~5mL);
二、将步骤一的粉红色的原料混合溶液密封在水热反应釜中,在温度为150℃~210℃的条件下进行溶剂热反应5.5h~7h,自然冷却至室温;
三、将步骤二中冷却后的产物离心分离,然后用乙醇水溶液洗涤三次,在60℃和真空条件下干燥12h~16h,得到粉红色的Mn-Co前驱体;所述的乙醇水溶液中水和乙醇的体积比为1:2;
四、将步骤三中的粉红色的Mn-Co前驱体在温度为500℃~600℃的条件下,在空气中焙烧3h~4h,得到层状钴酸锰材料。
3.根据权利要求2所述的一种层状钴酸锰材料的制备方法,其特征在于步骤一中所述的醋酸锰和醋酸钴的物质的量的比为1:2。
4.根据权利要求2所述的一种层状钴酸锰材料的制备方法,其特征在于步骤一中所述的醋酸钴和尿素的物质的量的比为1:15。
5.根据权利要求2所述的一种层状钴酸锰材料的制备方法,其特征在于步骤一中所述的尿素的物质的量和混合溶剂的体积比为1mmol:4mL。
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