CN113529047A - 一种MXene/C复合材料的制备方法 - Google Patents
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- 229910052799 carbon Inorganic materials 0.000 claims abstract description 33
- 238000005516 engineering process Methods 0.000 claims abstract description 29
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- 229910002804 graphite Inorganic materials 0.000 description 1
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- 238000010438 heat treatment Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
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Abstract
本发明揭示了一种MXene/C复合材料的制备方法,该方法包括以下步骤:S1:制备MXene片层;S2:用多元一体化镀碳装置对MXene片层进行镀碳,得到MXene/C复合材料。在所述S2步骤中,以MXene材料为基底,碳弧源进行沉积,制得MXene/C复合材料。本发明提供的多元一体化共沉积技术结合了磁过滤筛选技术、弧光放电技术和等离子体技术,制备的MXene/C复合材料厚度可调、简单方便、可大规模生产,适合应用于锂离子电池集流体等领域。
Description
技术领域
本发明涉及一种MXene/C复合材料的制备方法,可用于锂电池电极材料技术领域。
背景技术
新一代锂离子电池储能器件具有高能量密度、高循环稳定性、轻薄、低成本化以及环境友好等特点。锂离子电池的容量可以通过电池设计和电极材料的开发来进一步提高,其中负极材料是影响锂离子电池性能的关键因素。目前商业化的锂离子电池主要是以石墨为负极材料,但它的能量密度较低。因此,迫切需要开发高容量、循环稳定的新一代负极材料。
MXene作为一种新型的二维层状材料,因其超高的导电率以及体积比容量,在锂离子电池中表现出优越的电化学性能。但是由于MXene易堆叠,导致其活性位点数目和可用表面积减小。通过MXene与碳材料进行复合,克服了容量衰减的同时还具备高能量密度的特点,是一种具有巨大的发展潜力的锂离子电池电极材料。经检索发现,公开号为CN201610733990.9的专利公开了一种锂电池电极材料碳柱撑MXene复合材料的制备方法,该方法将MXene材料浸泡在阳离子型碳前驱体中,经离心、洗涤、干燥等过程得到预柱撑MXene,再经高温煅烧(300~800℃),制备碳柱撑MXene材料,该方法过程繁琐,比较耗时,不能大规模生产。
发明内容
本发明的目的就是为了解决现有技术中存在的上述问题,提出一种MXene/C复合材料的制备方法。
本发明的目的将通过以下技术方案得以实现:一种MXene/C复合材料的制备方法,该方法包括以下步骤:
S1:制备MXene片层;
S2:用多元一体化镀碳装置对MXene片层进行镀碳,得到MXene/C复合材料。
优选地,在所述S2步骤中,以MXene材料为基底,碳弧源进行沉积,制得MXene/C复合材料。
优选地,在所述S2步骤中,MXene表面碳层的厚度为200nm。
优选地,所述多元一体化镀碳装置采用多元一体化共沉积技术制备MXene/C复合材料。
优选地,所述多元一体化共沉技术为磁过滤技术、弧光放电技术和等离子体技术相结合。
优选地,在所述S2步骤中,多元一体化镀碳装置包括弧光放电源、固态弧源、磁过滤管、磁过滤干线管和化学气相反应室,其中,化学气相反应室位于所述多元一体化镀碳装置的中心位置,化学气相反应室上设置有基座和沉积基底,化学气相反应室的上端通过磁过滤管和磁过滤干线管连接弧光放电源和等离子体固态弧源,化学气相反应室的两侧分别设有等离子体气体源进口和气体源出口,最后得到复合材料。
本发明采用以上技术方案与现有技术相比,具有以下技术效果:该多元一体化装置包括磁过滤器、弧光放电和等离子体镀碳装置,制备MXene/C复合材料过程如下:在真空条件下,引入固体碳源在弧光放电作用下产生等离子体,通过磁过滤装置筛选去除大颗粒,得到结构为sp2杂化的C等离子体,制备MXene/C复合材料。
本发明提供的多元一体化共沉积技术结合了磁过滤筛选技术、弧光放电技术和等离子体技术,制备的MXene/C复合材料厚度可调、简单方便、可大规模生产,适合应用于锂离子电池集流体等领域。
附图说明
图1为本发明多元一体化镀碳装置的结构示意图。
图2为本发明的MXene材料的SEM图。
具体实施方式
本发明的目的、优点和特点,将通过下面优选实施例的非限制性说明进行图示和解释。这些实施例仅是应用本发明技术方案的典型范例,凡采取等同替换或者等效变换而形成的技术方案,均落在本发明要求保护的范围之内。
本发明揭示了一种MXene/C复合材料的制备方法,该方法包括以下步骤:
S1:制备MXene片层;
S2:用多元一体化镀碳装置对MXene片层进行镀碳,得到MXene/C复合材料。
在所述S2步骤中,以MXene材料为基底,碳弧源进行沉积,制得MXene/C复合材料。在所述S2步骤中,MXene表面碳层的厚度为200nm。
所述多元一体化镀碳装置采用多元一体化共沉积技术制备MXene/C复合材料。所述多元一体化共沉技术为磁过滤技术、弧光放电技术和等离子体技术相结合。
在所述S2步骤中,多元一体化镀碳装置包括弧光放电源1、固态弧源2、磁过滤管3、磁过滤干线管400和化学气相反应室100,其中,化学气相反应室位于所述多元一体化镀碳装置的中心位置,化学气相反应室上设置有基座200和沉积基底300,化学气相反应室的上端通过磁过滤管3和磁过滤干线管400连接弧光放电源1和等离子体固态弧源2,化学气相反应室的两侧分别设有等离子体气体源进口500和气体源出口600,最后得到复合材料700。
通过磁过滤筛选与弧光放电、等离子体装置共联,提高样品纯度,弧源为不同金属及非金属;该气体源为二氧化碳CO2。
MXene材料的制备:将氟化锂溶于盐酸中,搅拌均匀,缓慢加入Ti3AlC2,35-45℃下搅拌24小时,然后用去离子水洗涤、离心6~8次,使溶液的PH大于6,收集沉淀并将其溶于100mL去离子水中,在氩气保护下超声3小时。最后离心并收集上清液。
MXene/C复合材料的制备:在弧光放电作用下,固体碳源产生等离子体,经过磁过滤后筛选掉大颗粒杂志,纯度高的sp2杂化C等离子体进入薄膜沉积腔,在MXene基底上进行沉积形成MXene/C复合材料,如图2所示。
实施例1
本实施例为MXene片层的制备方法,该制备方法包括以下步骤:
将1.5g LiF溶解在30mL,9M HCl中;将1.5g Ti3AlC2散体分散到混合物中,60℃加热72h;用去离子水洗涤多次直到PH值高于6,真空干燥12h;将刻蚀后的多层Mxene产物分散于100mL去离子水中,Ar气下超声1h,以3500rpm离心1h,收集上清液。
实施例2
该多元一体化装置包括以下部件:包括磁过滤、弧光放电、等离子体于一体的多元化装置。在图1中,该装置由弧光放电系统:弧光放电源1和固态弧源2;磁过滤系统:磁过滤管3和磁过滤干线管400;化学气相沉积系统:化学气相反应室100,设置有基座200和沉积基底300等三大部件组成,还连接有等离子体气体源进口500和气体源出口600,最后在复合涂层700可制得MXene/C复合电极材料。
实施例3
本实施例揭示了一种MXene/C电极材料的制备方法,该制备方法包括以下步骤:
S1、将沉积基底300清洗后固定在可旋转的基座200上;将弧光放电源、磁过滤管和沉积腔进行抽取真空,真空度达到1X10-4Pa;采用等离子对沉积基底的镀膜表面进行清洗,去除沉积基底镀膜表面的油污及杂质;
S2、将弧光放电碳源引入磁过滤管中进行筛选,沉积弧流为100~120A,磁过滤弯管电流为1.6~2.5A,负偏压为160~320V,沉积时间为10min;
S3、关闭弧光放电、磁过滤电源,释放真空度,待恢复至常压状态后打开薄膜沉积腔取出样品得到表面镀碳的MXene/C材料。
S4、关闭弧光放电、磁过滤和化学气相管式炉电源,释放真空度,待恢复至常压状态后打开薄膜沉积腔取出样品得到MXene/C电极材料,如图2所示。
本发明的方法为采用磁过滤、弧光放电、等离子体于一体的多元化装置,在MXene表面镀碳,制备MXene/C复合电极材料。磁过滤样品纯度高,弧光放电结合等离子体技术将sp2碳牢固地沉积在MXene表面,能够制备出高质量的电极材料,提高电池的性能和使用寿命。本发明操作简单,工艺方便,具有现实的应用价值。
本发明的多元一体化装置工艺简单、操作方便、易于大规模生产。制备的MXene/C电极材料厚度可调,适合应用于锂离子电池集流体等领域。
本发明介绍一种多元一体化技术与MXene/C复合材料的制备方法,在真空环境下,利用弧光放电产生等离子体,制备了一种MXene/C电极材料。本发明提供的多元一体化共沉积技术结合了磁过滤筛选技术、弧光放电技术和等离子体技术,制备的MXene/C复合材料厚度可调、简单方便、可大规模生产,适合应用于锂离子电池集流体等领域。
本发明尚有多种实施方式,凡采用等同变换或者等效变换而形成的所有技术方案,均落在本发明的保护范围之内。
Claims (6)
1.一种MXene/C复合材料的制备方法,其特征在于:该方法包括以下步骤:
S1:制备MXene片层;
S2:用多元一体化镀碳装置对MXene片层进行镀碳,得到MXene/C复合材料。
2.根据权利要求1所述的一种MXene/C复合材料的制备方法,其特征在于:在所述S2步骤中,以MXene材料为基底,碳弧源进行沉积,制得MXene/C复合材料。
3.根据权利要求1所述的一种MXene/C复合材料的制备方法,其特征在于:在所述S2步骤中,MXene表面碳层的厚度为200nm。
4.根据权利要求1所述的一种MXene/C复合材料的制备方法,其特征在于:所述多元一体化镀碳装置采用多元一体化共沉积技术制备MXene/C复合材料。
5.根据权利要求4所述的一种MXene/C复合材料的制备方法,其特征在于:所述多元一体化共沉技术为磁过滤技术、弧光放电技术和等离子体技术相结合。
6.根据权利要求1所述的一种MXene/C复合材料的制备方法,其特征在于:
在所述S2步骤中,多元一体化镀碳装置包括弧光放电源(1)、固态弧源(2)、磁过滤管(3)、磁过滤干线管(400)和化学气相反应室(100),其中,化学气相反应室位于所述多元一体化镀碳装置的中心位置,化学气相反应室上设置有基座(200)和沉积基底(300),化学气相反应室的上端通过磁过滤管(3)和磁过滤干线管(400)连接弧光放电源(1)和等离子体固态弧源(2),化学气相反应室的两侧分别设有等离子体气体源进口(500)和气体源出口(600),最后得到复合材料(700)。
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