CN114807848A - 一种大面积二碲化钼的pld制备方法 - Google Patents
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Abstract
本发明公开了一种大面积二碲化钼的PLD制备方法,方法在脉冲激光沉积系统(PLD)真空腔室内一定的温度与压力条件下,将处理好的氟晶云母基片利用脉冲激光沉积系统进行二碲化钼(MoTe2)薄膜的沉积,随后将沉积好的薄膜及适量Te粉末封装进真空石英管中进行高温退火。根据不同的退火条件可以制备出半导体相(2H‑MoTe2)和金属相(1T’‑MoTe2)两种不同相的薄膜。本发明方法原理简单,所制备的二碲化钼厚度也可以通过改变沉积的时间进行调控从而满足不同的实验要求,与传统方法相比能够稳定制备出厘米级别的大面积二碲化钼薄膜,并且能极大地节省原材料,降低成本,更加符合现代化工业制备二碲化钼的工艺要求。
Description
技术领域
本发明公开了一种大面积二碲化钼的PLD制备方法,属于电子材料技术领域。
背景技术
自2004年通过机械剥离技术得到的石墨烯材料出现以来,其独特的物理性质和电子输运特性引起了研究者们极大的兴趣,先后出现了包括六方氮化硼(h-BN)、黑磷(BP)、过渡金属硫族化合物(TMDs)等二维材料。在这其中,过渡金属硫属化合物种类繁多,其结构、电学、磁学等性质也不尽相同,导电性从绝缘体、半导体、半金属到金属,磁性也从铁磁、反铁磁到顺磁,这些新材料的出现为探索新奇的物理现象和物理机理提供了理想的平台。
TMDs材料是一类具有MX2结构的层状材料,M代表过渡金属元素,主要包括第四副族过渡金属(Ti,Zr,Hf等),第五副族过渡金属(V,Nb,Ta)以及第六副族的过渡金属(Mo,W等);X指硫族元素(S,Se,Te),这类层状材料具有X-M-X的原子层结构,即在两层硫族原子层(X)中间加入一层过渡金属原子层(M),层间以微弱的范德瓦尔斯力相连,层间距在0.65nm左右。根据原子层的堆垛方式以及金属原子的配位形式,块体TMDCs层状材料具有多种晶相结构,总体上可以分为2H型,1T型和3R型,分别属于六方晶系、三方晶系和单斜晶系的TMDCs材料。其中1T型TMDCs材料不能稳定存在,而是以1T'晶相的方式存在。
二维层状二碲化钼(MoTe2)材料属于二维层状过渡金属硫族化合物中的一种,MoTe2以其独特的尺寸特征、电子特性和物理性质,已成为凝聚态物理、材料科学和化学领域重要的研究材料。在TMDs材料中,MoTe2具有较小的能带带隙,对整个光谱都具有很强的光吸收性能,故MoTe2光电器件的工作范围可从可见光区域拓展到近红外区域,且能在隧穿场效应晶体管中实现更高的驱动电流,使其在薄膜晶体管、光催化、传感器等电子器件方面大显身手。
目前二碲化钼薄膜的制备方法主要包括单晶样品机械剥离法、化学气相沉积法制备单晶纳米片等,但上述方法难以实现大面积、低成本的二碲化钼薄膜制备,因此寻找一种兼顾质量和大面积的制备方法显得尤为重要。
发明内容
发明要解决的技术问题
本发明针对现有技术难以制备高质量大面积二碲化钼的问题,提出一种大面积二碲化钼的PLD制备方法。
技术方案
为达到上述目的,本发明提供的技术方案为:
一种大面积二碲化钼的PLD制备方法,其特征在于,包括以下步骤:
步骤1:对氟晶云母基片使用丙酮、酒精、去离子水进行处理;
步骤2:将处理好的氟晶云母基片以及二碲化钼靶材放入脉冲激光沉积系统真空腔室,将腔室抽成真空后加热氟晶云母基片到恒定温度;
步骤3:保持步骤2中真空腔室环境不变,将激光通过透镜照射于二碲化钼靶材上,在基片上进行二碲化钼薄膜沉积;
步骤4:保持真空腔室内温度气压环境不变,将步骤3所得基片进行原位退火,将薄膜自然冷却至室温;
步骤5:关闭脉冲激光沉积系统,从真空腔室内取出基片样品;
步骤6:将步骤5所得样品与适量Te粉末放入单开口石英管中,抽至高真空后封好管口,随后加热至一定温度,在Te气氛下进行退火并以恒定降温速率缓慢降温,制备得到半导体相二碲化钼薄膜;将步骤5所得样品与适量Te粉末放入单开口石英管中,抽至高真空后封好管口,随后加热至一定温度,在Te气氛下退火,随后将样品放入冷水中快速淬火降温,制备得到金属相二碲化钼薄膜。
进一步地,步骤3中的激光源为KrF准分子激光器。
进一步地,步骤3的沉积过程中靶材放置于匀速转动的转动台上。
有益效果
采用本发明的技术方案,能够产生以下有益效果:
本发明方法原理简单易于推广,所制备的二碲化钼厚度也可以通过改变沉积的时间进行调控,满足不同的实验要求;
本发明方法与传统方法相比能够稳定制备出厘米级别的大面积二碲化钼薄膜,并且能极大地节省原材料,降低成本,更加符合现代化工业制备二碲化钼的工艺要求。
附图说明
图1为本发明制备方法的流程图;
图2为本发明所制二碲化钼薄膜的光学照片;
图3为本发明所制二碲化钼的原子力显微镜图;
图4为本发明所制2H-MoTe2薄膜的拉曼光谱;
图5为本发明所制1T’-MoTe2薄膜的拉曼光谱。
具体实施方式
为进一步了解本发明的内容,结合附图和具体实施方式对本发明作详细描述。
本发明首先通过脉冲激光沉积系统在基底上沉积二碲化钼薄膜,随后将沉积好的薄膜及Te粉末封装进真空石英管中,进行高温退火,根据不同的退火条件可以制备出2H-MoTe2和1T’-MoTe2这两种不同相的薄膜,整体制备步骤如图1所示。
步骤1:对氟晶云母基片使用丙酮、酒精、去离子水进行处理,本实施例所采用的方法为:首先将氟晶云母基片分别在丙酮、无水乙醇中超声清洗5分钟,然后将清洗后的基片在去离子水中浸泡20分钟。
步骤2:将装有处理好的氟晶云母基片以及二碲化钼靶材放入真空腔室,将腔室抽成真空后加热氟晶云母基片到恒定温度,在本实施例中腔室内压抽至4.6±1×10-7mbar,加热温度为200±5℃。
步骤3:保持步骤2真空腔室环境不变,将激光通过透镜照射于二碲化钼靶材上,本实施例中采用KrF准分子激光器,激光波长为248nm,靶材与激光束的夹角约为45°,激光束的平均能量密度约为1.5J/cm2,激光重复频率为2Hz,沉积时间根据选择厚度而决定。沉积时靶材放置在转动台上,保持均匀速率进行转动,其目的是使激光均匀的打在靶材上面,从而在增加薄膜生长的稳定性同时延长靶材使用的寿命。
步骤4:制得步骤3薄膜后,将样品基片原位退火约5min,然后将薄膜自然冷却至室温,原位退火过程保持真空腔室内气压不变,目的是使生长完成的薄膜更加平整。
步骤5:关闭脉冲激光沉积系统,从真空腔室内取出基片样品。
步骤6:将基片样品和2.0mg Te粉末放入单开口石英管中,抽至高真空后封好管口,随后加热到700±5℃,在Te气氛下退火12h,以2℃/min降温速率缓慢降温,得到半导体相(2H-MoTe2)二碲化钼薄膜;将样品和2.0mg Te粉末放入单开口石英管中,抽至高真空后封好管口,随后加热到900±5℃,在Te气氛下退火12h,随后将样品放入冷水中快速淬火降温,制备得到金属相(1T’-MoTe2)二碲化钼薄膜。
图2为上述实施例所制二碲化钼薄膜的光学照片,可以看出其样品尺寸可以达到1×1cm2,表面为亮黑色。
图3为本发明所制二碲化钼的原子力显微镜(AFM)图,图中可以观察到制备得到的样品厚度约为10nm,粗糙度约为0.7nm,体现了样品表面形貌的高质量。
图4为本发明所制2H相的二碲化钼的拉曼(Raman)光谱。其中二碲化钼的特征峰A1g、E2g以及B2g分别位于169.82cm-1、233.0cm-1以及289.6cm-1处,这一结果与文献中报道2H相的二碲化钼相符合,表明成功制备了2H相的二碲化钼结晶样品。
图5为本发明所制1T’相的二碲化钼的拉曼(Raman)光谱。其中二碲化钼的特征峰分别为于109.06cm-1(Au)、127.46cm-1(Ag)、162.7cm-1(Bg)以及256.2cm-1(Ag)处,这一结果与文献中报道1T’相的二碲化钼相符合,表明成功制备了1T’相的二碲化钼结晶样品。
以上示意性的对本发明及其实施方式进行了描述,该描述没有限制性,附图中所示的也只是本发明的实施方式之一,实际的结构并不局限于此。所以,如果本领域的普通技术人员受其启示,在不脱离本发明创造宗旨的情况下,不经创造性的设计出与该技术方案相似的结构方式及实施例,均应属于本发明的保护范围。
Claims (3)
1.一种大面积二碲化钼的PLD制备方法,其特征在于,包括以下步骤:
步骤1:对氟晶云母基片使用丙酮、酒精、去离子水进行处理;
步骤2:将处理好的氟晶云母基片以及二碲化钼靶材放入脉冲激光沉积系统真空腔室,将腔室抽成真空后加热氟晶云母基片到恒定温度;
步骤3:保持步骤2中真空腔室环境不变,将激光通过透镜照射于二碲化钼靶材上,在基片上进行二碲化钼薄膜沉积;
步骤4:保持真空腔室内温度气压环境不变,将步骤3所得基片进行原位退火,将薄膜自然冷却至室温;
步骤5:关闭脉冲激光沉积系统,从真空腔室内取出基片样品;
步骤6:将步骤5所得样品与适量Te粉末放入单开口石英管中,抽至高真空后封好管口,随后加热至一定温度,在Te气氛下进行退火并以恒定降温速率缓慢降温,制备得到半导体相二碲化钼薄膜;将步骤5所得样品与适量Te粉末放入单开口石英管中,抽至高真空后封好管口,随后加热至一定温度,在Te气氛下退火,随后将样品放入冷水中快速淬火降温,制备得到金属相二碲化钼薄膜。
2.如权利要求1所述的一种大面积二碲化钼的PLD制备方法,其特征在于,所述步骤3中的激光源为KrF准分子激光器。
3.如权利要求1所述的一种大面积二碲化钼的PLD制备方法,其特征在于,所述步骤3的沉积过程中靶材放置于匀速转动的转动台上。
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