CN113265635A - 一种过渡金属硫化物材料图案化的制备方法和产品 - Google Patents
一种过渡金属硫化物材料图案化的制备方法和产品 Download PDFInfo
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Abstract
本发明涉及一种过渡金属硫化物材料图案化的制备方法和产品,利用简单可控的磁控溅射镀膜法在衬底材料上直接制备出厚度均匀的过渡金属薄膜,再进行RIE反应离子刻蚀,利用具有化学反应性的气体与过渡金属薄反应,形成图案化的过渡金属薄膜,最后将图案化的过渡金属薄膜放入管式炉,利用硫粉升华与过渡金属发生反应进行硫化,最后生成图案化的硫化物,为二维材料在电子学与光电子学器件领域提供前瞻性工作。
Description
技术领域
本发明属于新型半导体材料制备技术和应用领域,涉及过渡金属硫化物材料图案化的制备,尤其涉及一种制备简单、快速、图案化尺寸可控,不会造成样品表面污染及边界钝化的过渡金属硫化物材料图案化的制备方法和产品。
背景技术
随着全球人口的迅速膨胀,经济的快速增长,人们对高端电子产品的需求也日益提高。高端电子产品,其内部电路终究是离不开半导体集成技术。集成电路(integratedcircuit,IC)是通过形成于基底或不同膜层中的图案化特征(feature)构成的元件装置以及内连线结构所建构。目前来说,图案化设计(例如光刻)是整个半导体制作过程中很重要的一个关键制程,其主要是将所设计的图案,例如电路布局形成于一个或多个光掩模上,然后再通过曝光(exposure)与显影(development)步骤将光掩模上的图案转移至一膜层上的光致抗蚀剂层内,以将此复杂的布局图案精确地转移至半导体芯片上。半导体集成电路工业处于快速发展的阶段,而集成电路材料以及设计在技术上的进步使得每一代生产的集成电路变得比先前生产的集成电路更小且其电路也变得更复杂。在集成电路发展过程中,功能性密度(例如:每一个芯片区域中内连接单元的数目)已经普遍增加,而几何尺寸(例如:工艺中所能创造出最小的元件或线路)则是普遍下降。
二维材料(如过渡金属硫化物)是由单层或少层原子或分子层组成的超薄材料体系,具有极大的比表面积和超高的载流子迁移速率,被认为是替代硅的下一代半导体材料。在基板上将二维材料结构成所需的图案化设计是其实现功能器件的关键和最重要的步骤。然而,在现有技术持续发展下,随着二维材料元器件的关键尺寸日渐缩小,对图案化技术的解析度和成本要求也越来越高。
二维材料有望成为下一代小型化电子器件的核心材料。为实现此类应用,需要对材料进行裁剪。通过常规的微纳加工技术,包括光刻和反应离子干法刻蚀(RIE)或者化学溶液湿法腐蚀,可对其进行加工裁剪。然而,在这些加工步骤中,二维材料需要接触光刻胶、溶液以及高能离子等,带来样品的表面污染及边界钝化等问题。在电子器件工作过程中,污染物作为电子散射中心,降低了材料的导电性,从而影响器件性能的提升。
湿法刻蚀是一个纯粹的化学反应过程,是指利用溶液与预刻蚀材料之间的化学反应来除去未被掩蔽膜材料掩蔽的部分而达到刻蚀目的。缺点是:对图形的控制性较差;不能用于小的特征尺寸;会产生大量的化学废液,造成环境污染。
电子束曝光(EBL,electron beam lithography)技术是一种扫描电子聚焦束以在被称为抗蚀剂(曝光)的电子敏感膜覆盖的表面上绘制自定义形状的实践。缺点:技术繁琐,产率低,生产成本极高;高能粒子轰击会造成母相材料晶格缺陷。
发明内容
本发明的目的是实现大面积过渡金属硫化物(如MoS2)二维材料的无污染图案化剪裁,提供了一种过渡金属硫化物材料图案化的制备方法。利用简单可控的磁控溅射镀膜法在衬底材料上直接制备出厚度均匀的过渡金属薄膜,再进行RIE反应离子刻蚀,利用具有化学反应性的气体与过渡金属薄反应,形成图案化的过渡金属薄膜,最后将图案化的过渡金属薄膜放入管式炉,利用硫粉升华与过渡金属发生反应进行硫化,最后生成图案化的硫化物,为二维材料在电子学与光电子学器件领域提供前瞻性工作。
本发明另一个目的是为了提供该制备方法得到的过渡金属硫化物材料。
为了实现上述目的,本发明采用以下技术方案:
一种过渡金属硫化物材料图案化的制备方法,所述制备方法包括以下步骤:
1)通过磁控溅射将靶材溅射至衬底上,得到镀有金属薄膜的衬底;
2)在步骤1)得到的镀有金属薄膜的衬底上固定掩膜版,进行刻蚀,得到阵列化金属膜的衬底;
3)将步骤2)得到的刻蚀后的阵列化金属膜的衬底与硫粉置于同一反应容器内,保护气体氛围中,进行硫化反应;退火,得到图案化的过渡金属硫化物材料;
其中,所述靶材为含有过渡金属元素的靶材或者过渡金属单质。
作为本发明的一种优选方案,所述的过渡金属为钼或钨。
作为本发明的一种优选方案,步骤1)中,磁控溅射的参数为压强1.1~1.3Pa直流溅射功率:70~90W,镀膜时间15~20min,膜厚:20~30nm。
作为本发明的一种优选方案,步骤2)中,所述刻蚀为RIE反应离子刻蚀,刻蚀参数为:氧气和六氟化硫占比1∶1,刻蚀功率18~12W,刻蚀时间60~100s。
作为本发明的一种优选方案,步骤3)中,通过比对镀膜刻蚀前后衬底质量确定衬底上金属膜的质量,硫粉的质量为金属膜质量的1/8-1/10。
作为本发明的一种优选方案,步骤3)中,硫化反应的温度为750-1000℃,反应时间55-65min。
作为本发明的一种优选方案,步骤3)中,退火程序为反应结束后,按照8℃/min的降温速率,将温度下降至300-400℃后,将降温速率改为5℃/min,将温度降至100℃以下。
作为本发明的一种优选方案,步骤3)中,所述保护气体为氩气,氩气的流量为100-150sccm。
作为本发明的一种优选方案,步骤3)中,硫粉放置在反应容器的低温区,阵列化金属膜的衬底放置在反应容器的高温区。
一种上述制备方法制得的图案化的过渡金属硫化物材料。
相对于现有技术,本发明至少具有以下明显优点:
1)本发明所需要的原材料储备丰富、价格低廉,并且合成所利用设备简单快速易调节。
2)本发明生长出来的过渡金属硫化物是阵列图案化的,尺寸可控。
3)金属钼的内部结构和化学性质很稳定,不会造成样品表面污染及边界钝化等问题。
附图说明
图1是本发明制备方法流程示意图。
图2是Mo薄膜的AFM(原子力显微镜)厚度图。
图3是图案化Mo膜硫化过程。
图4是阵列化MoS2的光学照片。
具体实施方式
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
参见图1,本发明提供了一种过渡金属硫化物材料图案化的制备方法,所述制备方法包括以下步骤:
1)通过磁控溅射将靶材溅射至衬底上,得到镀有金属薄膜的衬底;
2)在步骤1)得到的镀有金属薄膜的衬底上固定掩膜版,进行刻蚀,得到阵列化金属膜的衬底;
3)将步骤2)得到的刻蚀后的阵列化金属膜的衬底与硫粉置于同一反应容器内,保护气体氛围中,进行硫化反应;退火,得到图案化的过渡金属硫化物材料;
其中,所述靶材为含有过渡金属元素的靶材或者过渡金属单质,优选地,过渡金属元素为钼或钨;更优选地,本发明所用的过渡金属为钼。
以下将通过实施例对本发明进行详细描述。
实施例:
本实施例提供了图案化MoS2二维材料的制备方法,具体为:
1)选用纯度为99.9%的金属钼靶材作为制备二硫化钼薄膜的原材料;
选取靶材的一面,先用砂纸打磨去除表面的氧化钼和杂质;在将整片硅片切割成几小块,用高温耐热胶把切割好的硅片固定在基板上,把钼靶材放入非磁性靶位上,关闭真空室,进行抽真空;当压强控制在1.1~1.3Pa,打开直流电流源,进行预溅射,预溅射时间2~3min;待直流溅射功率稳定在80W,打开挡板,进行直流溅射镀膜,镀膜时间控制在18±1min;
2)将步骤1)制备好的均匀的钼薄膜,在其上面固定好一块预制的掩膜版,将样品放入RIE反应离子刻蚀器里面进行反应离子干法刻蚀;刻蚀的时候,氧气和六氟化硫都设置为20sccm左右,刻蚀功率设置为20W,刻蚀时间设置为50~60s;等刻蚀结束后,可以看得出有明显的圆形形状出现在硅片上,此时就可以将样品进行厚度等表征,如图2所示;
3)将步骤2)制备好的阵列钼薄膜,取出放入管式炉里面进行硫化操作;通过比对镀膜刻蚀前后硅片质量确定硅片上钼膜的质量,控制钼与硫粉的质量比1:10,分别放入两个石英舟里面;如图3所示,存放硫粉的石英舟,将整个石英舟放置在管式炉前部的低温区;Mo样品放在另一个石英舟中(相距5~7cm),并放在管式炉中间的高温区;
在实验过程中通入氩气作为载气,流量为100sccm(1sccm=1mL/min);在加热前,先通氩气30min,然后30min内将管式炉加温到750~800℃,保持此温度60min来制备MoS2二维材料;等保温结束后,设置管式炉的退火速率,起初设置为8℃/min,等到温度下降到300~400℃,将退火速率改为5℃/min,以此速率进行降温处理,等到炉膛温度变为100℃以下的时候,停止通气,打开炉膛,取出样品,参见图4,生长出来的二硫化钼是阵列图案化的,尺寸可控。
本发明利用简单可控的磁控溅射镀膜法在硅基片上直接制备出厚度均匀的Mo薄膜,再进行RIE反应离子刻蚀,利用具有化学反应性的气体与钼反应,形成图案化的金属钼薄膜,最后将图案化的钼薄膜放入管式炉,利用硫粉升华与金属钼发生反应进行硫化,最后生成图案化的二硫化钼,为二维材料在电子学与光电子学器件领域提供前瞻性工作。
以上所述,仅为本发明的较佳实施例,并非对本发明任何形式上和实质上的限制,应当指出,对于本技术领域的普通技术人员,在不脱离本发明方法的前提下,还将可以做出若干改进和补充,这些改进和补充也应视为本发明的保护范围。凡熟悉本专业的技术人员,在不脱离本发明的精神和范围的情况下,当可利用以上所揭示的技术内容而做出的些许更动、修饰与演变的等同变化,均为本发明的等效实施例;同时,凡依据本发明的实质技术对上述实施例所作的任何等同变化的更动、修饰与演变,均仍属于本发明的技术方案的范围内。
Claims (10)
1.一种过渡金属硫化物材料图案化的制备方法,其特征在于,所述制备方法包括以下步骤:
1)通过磁控溅射将靶材溅射至衬底上,得到镀有金属薄膜的衬底;
2)在步骤1)得到的镀有金属薄膜的衬底上固定掩膜版,进行刻蚀,得到阵列化金属膜的衬底;
3)将步骤2)得到的刻蚀后的阵列化金属膜的衬底与硫粉置于同一反应容器内,保护气体氛围中,进行硫化反应;退火,得到图案化的过渡金属硫化物材料;其中,所述靶材为含有过渡金属元素的靶材或者过渡金属单质。
2.根据权利要求1所述的一种过渡金属硫化物材料图案化的制备方法,其特征在于,所述的过渡金属元素为钼或钨。
3.根据权利要求1或2所述的一种过渡金属硫化物材料图案化的制备方法,其特征在于,步骤1)中,磁控溅射的参数为压强1.1~1.3Pa直流溅射功率:70~90W,镀膜时间15~20min,膜厚:20~30nm。
4.根据权利要求1或2所述的一种过渡金属硫化物材料图案化的制备方法,其特征在于,步骤2)中,所述刻蚀为RIE反应离子刻蚀,刻蚀参数为:氧气和六氟化硫占比1∶1,刻蚀功率18~12W,刻蚀时间60~100s。
5.根据权利要求1或2所述的一种过渡金属硫化物材料图案化的制备方法,其特征在于,步骤3)中,通过比对镀膜刻蚀前后衬底质量确定衬底上金属膜的质量,硫粉的质量为金属膜质量的1/8-1/10。
6.根据权利要求5所述的一种过渡金属硫化物材料图案化的制备方法,其特征在于,步骤3)中,硫化反应的温度为750-1000℃,反应时间55-65min。
7.根据权利要求6所述的一种过渡金属硫化物材料图案化的制备方法,其特征在于,步骤3)中,退火程序为反应结束后,按照8℃/min的降温速率,将温度下降至300-400℃后,将降温速率改为5℃/min,将温度降至100℃以下。
8.根据权利要求7所述的一种过渡金属硫化物材料图案化的制备方法,其特征在于,步骤3)中,所述保护气体为氩气,氩气的流量为100-150sccm。
9.根据权利要求8所述的一种过渡金属硫化物材料图案化的制备方法,其特征在于,步骤3)中,硫粉放置在反应容器的低温区,阵列化金属膜的衬底放置在反应容器的高温区。
10.一种如权利要求1-9任一项所述的过渡金属硫化物材料图案化的制备方法制得的图案化的过渡金属硫化物材料。
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