CN111696791B - MnO/CNT复合材料的制备方法 - Google Patents
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Abstract
本发明公开了一种MnO/CNT复合材料的制备方法。所述方法按Mn3O4与尿素的质量比为1：5～20，先将Mn3O4粉末材料和尿素混合，并研磨均匀，在保护气氛下，600～800℃下高温煅烧1～5h后得到MnO/CNT复合材料。本发明采用一步高温煅烧法，工艺简单，能耗低。本发明制得的MnO/CNT复合材料，MnO纳米立方体与CNT均匀分布，CNT交错排布在MnO之间，形貌均匀无团聚，在后期的应用中，可增强材料的整体导电性，减少作为各种电子器件的电极过程中，导电剂的使用所造成的电化学性能的降低，提高材料利用率。
Description
技术领域
本发明属于纳米复合材料制备技术领域，涉及一种MnO/CNT复合材料的制备方法。
背景技术
过渡金属氧化物由于其特定结构与性能，在超级电容器、离子电池和光催化等领域受到广泛关注。其中，锰基氧化物应用于国民经济的各个领域，主要包括一氧化锰、二氧化锰、四氧化三锰等。一氧化锰又称氧化亚锰，是锰化合物中重要的一种，主要用作生产铁氧化物的原料、催化剂、冶炼、焊接及电池制造业等。
目前，一氧化锰由于自然资源丰富、合适的电动势、低的电压滞后(<0.8V)，高的理论比容量(756mA h g-1)等特点，被广泛应用于电池材料行业。但其存在导电性差和体积膨胀大等缺点。因此，和高导电性且结构稳定的物质复合是改善一氧化锰电化学性能的有效途径。
目前常见的制备一氧化锰复合材料的方法是两步法。第一步包括水浴法、水热法等，第二步主要为热处理过程(Zhang K et al,Synthesis of nitrogen-doped MnO/grapheme nanosheets hybrid material for lithium ion batteries[J].Acs AppliedMaterials&Interfaces,2012,4(2):658-664.)。上述方法较为复杂，过程中需调控的反应因素较多，包括前驱液的浓度、pH值、锻烧温度等，因此合成的复合材料的分散均匀比较难以控制。MnO也存在自身的问题，如导电性较差，材料利用率较低。通常，MnO/CNT复合材料的制备主要是直接混合锰氧化物前驱体与商用碳纳米管(Xia C et al,Preparation ofpompon-like MnO/carbon nanotube composite microspheres as anodes for lithiumion batteries[J],Electrochimica Acta,2015,180,858-865)，商用碳纳米管的成本较高，且由于锰氧化物前驱体与商用碳纳米管直接混合，制得的复合材料中二者的复合均匀度较差，进而影响其电学性能。
发明内容
本发明的目的在于提供一种MnO/CNT复合材料的制备方法。该方法将锰氧化物前驱体与尿素混合后经过高温煅烧得到均匀复合的MnO/CNT复合材料。
实现本发明目的的技术方案如下：
MnO/CNT复合材料的制备方法，包括以下步骤：
按Mn3O4与尿素的质量比为1：5～20，先将Mn3O4粉末材料和尿素混合，并研磨均匀，在保护气氛下，600～800℃下高温煅烧1～5h，反应结束后，无水乙醇清洗，干燥得到MnO/CNT复合材料。
优选地，所述的Mn3O4与尿素的质量比为1：5～10。
优选地，所述的高温煅烧温度为600～750℃，煅烧时间为2～4h。
优选地，所述的保护气氛可以是氩气或者氮气。
与现有技术相比，本发明具有以下优点：
本发明采用简单的一步高温煅烧法，合成时间短，反应能耗低，工艺简单，过程可控。制得的MnO/CNT复合材料中，MnO纳米立方体与CNT均匀分布，CNT交错排布在MnO之间，形貌均匀无团聚。在后期的应用中，可增强材料的整体导电性，减少作为各种电子器件的电极过程中，导电剂的使用所造成的电化学性能的降低，提高材料利用率。
附图说明
图1是本发明制备的MnO/CNT复合材料的XRD图谱。
图2是本发明制备的MnO/CNT复合材料的高倍SEM图。
图3是本发明制备的MnO/CNT复合材料的低倍SEM图。
图4是本发明制备的MnO/CNT复合材料在25mV/s扫速下的CV曲线。
具体实施方式
下面结合实施例和附图对本发明做进一步详细的描述。
实施例1
按Mn3O4与尿素的质量比为1：5，先将Mn3O4粉末材料和尿素混合，并研磨均匀，在氩气保护气氛的管式炉中高温600℃煅烧2h，反应结束后，无水乙醇清洗，烘干得到MnO/CNT复合材料。
实施例2
按Mn3O4与尿素的质量比为1：10，先将Mn3O4粉末材料和尿素混合，并研磨均匀，在氮气保护气氛的管式炉中高温700℃煅烧2h，反应结束后，无水乙醇清洗，烘干得到MnO/CNT复合材料。
实施例3
按Mn3O4与尿素的质量比为1：10，先将Mn3O4粉末材料和尿素混合，并研磨均匀，在氮气保护气氛的管式炉中高温750℃煅烧4h，反应结束后，无水乙醇清洗，烘干得到MnO/CNT复合材料。
实施例4
按Mn3O4与尿素的质量比为1：10，先将Mn3O4粉末材料和尿素混合，并研磨均匀，在氩气保护气氛的管式炉中高温750℃煅烧4h，反应结束后，无水乙醇清洗，烘干得到MnO/CNT复合材料。
如图1所示，本发明的制备方法制备的MnO/CNT复合材料的XRD图谱，与数据库中的标准卡片No.75-0626完全吻合，说明产物的晶相组成为MnO，此外可见射线衍射峰的峰型尖锐、峰强较高，说明晶型发育良好。
如图2、图3所示，本发明的制备方法制备的MnO/CNT复合材料的SEM图，可见碳纳米管均匀分散在MnO纳米立方体之间，相互交联。
如图4所示，本发明制备的MnO/CNT复合材料电极作为超级电容器正极材料在25mV/s扫速下的CV曲线，存在明显的氧化还原峰，对应MnO中锰的氧化还原过程所提供的容量。
对比例1
按Mn3O4与尿素的质量比为1：10，先将Mn3O4粉末材料和尿素混合，并研磨均匀，在氩气保护气氛的管式炉中高温900℃煅烧4h，反应结束后，无水乙醇清洗，烘干得到MnO/CNT复合材料。与实施例2对比，提高煅烧温度，MnO颗粒的尺寸增大，电极材料性能下降。
Claims (5)
1.MnO/CNT复合材料的制备方法，其特征在于，包括以下步骤：
按Mn3O4与尿素的质量比为1：5～20，先将Mn3O4粉末材料和尿素混合，并研磨均匀，在保护气氛下，600～800℃下高温煅烧1～5h，反应结束后，无水乙醇清洗，干燥得到MnO/CNT复合材料。
2.根据权利要求1所述的制备方法，其特征在于，所述的Mn3O4与尿素的质量比为1：5～10。
3.根据权利要求1所述的制备方法，其特征在于，所述的高温煅烧温度为600～750℃。
4.根据权利要求1所述的制备方法，其特征在于，煅烧时间为2～4h。
5.根据权利要求1所述的制备方法，其特征在于，所述的保护气氛为氩气或者氮气。
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