CN112458430A - 一种改善硫化钨连续膜均匀性的方法 - Google Patents

一种改善硫化钨连续膜均匀性的方法 Download PDF

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CN112458430A
CN112458430A CN202011426047.6A CN202011426047A CN112458430A CN 112458430 A CN112458430 A CN 112458430A CN 202011426047 A CN202011426047 A CN 202011426047A CN 112458430 A CN112458430 A CN 112458430A
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continuous film
tungsten sulfide
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CN112458430B (zh
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兰飞飞
张嵩
董增印
王再恩
王健
李佳起
杨丹丹
张颖
李强
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CETC 46 Research Institute
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/305—Sulfides, selenides, or tellurides
    • C—CHEMISTRY; METALLURGY
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/02—Pretreatment of the material to be coated
    • C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
    • C23C16/0236—Pretreatment of the material to be coated by cleaning or etching by etching with a reactive gas
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/54—Apparatus specially adapted for continuous coating
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Abstract

本发明公开了一种改善硫化钨连续膜均匀性的方法。该方法的步骤是：首先采用CVD法在特定衬底表面进行连续硫化钨薄膜的生长。生长结束后将获得的连续膜放入石英舟中，然后将装有连续膜的石英舟放入石英系统中，向系统中通入100‑150sccm的Ar，保持系统压力在5‑10mbar，将系统温度升高至950℃‑1000℃，当系统温度达到设定温度后，向系统内通入5sccm‑10sccm的H2，在氢气气氛下对连续膜进行表面热处理。H2对硫化物的单晶终端能够起到一定的刻蚀作用，能够有效去除连续膜表面存在的小尺寸二次成核单晶，提高连续膜均匀性。

Description

一种改善硫化钨连续膜均匀性的方法
技术领域
本发明涉及采用对CVD法制备WS2连续膜进行表面处理工艺，尤其是涉及一种改善硫化钨连续膜均匀性的方法。
背景技术
二维WS2是过渡金属硫化物中的典型代表，是典型的二维层状材料，单层的WS2为直接带隙半导体材料，迁移率超过1000cm2/V·s，远高于同等厚度下硅材料的迁移率；WS2表面无悬挂键，能够在复杂的环境中保持良好的稳定性；WS2基场效应晶体管具有超低的晶态功耗，它的运用将能够显著降低系统功耗。此外，WS2具有优异的光学性能，良好的机械柔韧性。为此，WS2在微电子以及柔性光电子等领域有着潜在的应用前景。
目前CVD法进行WS2单晶生长过程中主要采用三氧化钨作为W源，高纯硫粉作为硫源，在一定生长条件下加热的硫蒸汽随着载气的输运到达三氧化钨源区，与三氧化钨进行反应获得降解的含钨氧化物，这种降解的钨的氧化物沉积在衬底的表面，随着硫蒸汽的持续供应，钨的氧化物被完全硫化，获得WS2薄膜材料。目前研究人员采用CVD法已经能够获得晶圆级的WS2单层连续薄膜，但是由于连续膜生长过程中钨源的持续供应，导致连续膜表面存在大量的二次成核小尺寸单晶，这些小尺寸单晶的存在严重破坏了连续的均匀性，导致连续膜性能的下降。由于连续膜生长过程中成核过程贯穿整个生长过程，所以这些二次成核的小尺寸单晶难以避免，为此，目前采用CVD法获得高均匀性的连续二硫化钨薄膜仍然是硫化钨研究与应用进程中急需解决的难题。
发明内容
本发明的目的是解决现有CVD法生长WS2连续膜中均匀性较差的问题，特别提供一种改善硫化钨连续膜均匀性的方法，以提高连续膜均匀性。
为实现上述目的，本发明所采取的技术方案是：一种改善硫化钨连续膜均匀性的方法，其特征在于，利用H2对硫化钨单晶终端的刻蚀作用，在一定气氛与温度下对获得的连续硫化钨薄膜进行表面热退火处理，处理过程按照以下步骤完成：
第一步，将CVD法获得的连续硫化钨薄膜放置在石英舟表面。
第二步，将石英管放入CVD生长系统中；对CVD生长系统进行抽真空处理，当系统内压力为0mbar时，通入Ar气进行吹扫，Ar气流量为500sccm。
第三步，将Ar气流量降至100sccm-150sccm，系统内压力保持在5mbar-10mbar。
第四步，对系统进行升温，将系统温度升至950℃-1000℃，通入5sccm-10sccm的H2，并保温30min-50min。
第五步，热处理过程结束后，降温，取样。
本发明改善硫化钨连续膜均匀性机理：利用H2对硫化钨单晶终端的刻蚀作用，在一定温度与气氛下，对硫化钨表面进行热处理，利用H2的刻蚀性，对连续膜表现存在的二次成核三角形进行刻蚀处理，去除表面的二次成核三角形，提高连续膜均匀性。
本发明的有益效果是：利用H2对硫化钨表面的刻蚀作用，在一定温度下，利用H2对硫化钨表面二次成核三角形进行表面热处理，能够有效去除表面二次成核三角形，显著提高连续膜均匀性，采用这种方法，能够获得表面均匀性良好的2英寸连续硫化钨薄膜。
附图说明
图1为本发明采用的改善硫化钨连续膜均匀性装置示意图。
具体实施方式
以下结合附图和实施例对本发明作进一步说明。
首先采用CVD法在特定衬底表面进行连续硫化钨薄膜的生长。生长结束后将获得的连续膜放入石英舟中，然后将装有连续膜的石英舟放入石英系统中，向系统中通入100-150sccm的Ar，保持系统压力在5-10mbar，将系统温度升高至950℃-1000℃，当系统温度达到设定温度后，向系统内通入5sccm-10sccm的H2，在氢气气氛下对连续膜进行表面热处理。H2对硫化物的单晶终端能够起到一定的刻蚀作用，能够有效去除连续膜表面存在的小尺寸二次成核单晶，提高连续膜均匀性。
实施例：
第一步，如图1所示，将CVD法获得的硫化钨连续膜1放置在结晶的石英舟2表面，将石英舟置于生长系统内部。
第二步，对系统实施抽真空处理，当系统内压力为0mbar时，通入Ar气进行吹扫，Ar气流量为500sccm。
第三步，将Ar气流量将至100sccm，系统内压力保持在5mbar，对系统升温，系统温度为950℃。
第四步，系统内温度达到设定温度后向系统内通入5sccm的H2，保温40min。
第五步，保温，自然降至室温，取出样品进行测试。通过微分干涉显微镜测试发现，连续膜表面二次成核三角形密度显著降低，连续膜均匀性显著提高。

Claims (1)

1.一种改善硫化钨连续膜均匀性的方法，其特征在于，利用H2对硫化钨单晶终端的刻蚀作用，在一定气氛与温度下对获得的连续硫化钨薄膜进行表面热退火处理，处理过程按照以下步骤完成：
第一步，将CVD法获得的连续硫化钨薄膜放置在石英舟表面；
第二步，将石英管放入CVD生长系统中；对CVD生长系统进行抽真空处理，当系统内压力为0mbar时，通入Ar气进行吹扫，Ar气流量为500sccm；
第三步，将Ar气流量降至100sccm-150sccm，系统内压力保持在5mbar-10mbar；
第四步，对系统进行升温，将系统温度升至950℃-1000℃，通入5sccm-10sccm的H2，并保温30min-50min；
第五步，热处理过程结束后，降温，取样。
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113106544A (zh) * 2021-04-12 2021-07-13 东北师范大学 制备大尺寸高质量二维TMDs单晶及薄膜的方法
CN114108099A (zh) * 2021-12-02 2022-03-01 中国电子科技集团公司第四十六研究所 一种蓝宝石衬底上二硫化钨晶向调控方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20160308006A1 (en) * 2015-04-16 2016-10-20 Cornell University Monolayer films of semiconducting metal dichalcogenides, methods of making same, and uses of same
US9721963B1 (en) * 2016-04-08 2017-08-01 Sandisk Technologies Llc Three-dimensional memory device having a transition metal dichalcogenide channel
CN111485224A (zh) * 2019-01-29 2020-08-04 北京石墨烯研究院 化学气相沉积装置

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20160308006A1 (en) * 2015-04-16 2016-10-20 Cornell University Monolayer films of semiconducting metal dichalcogenides, methods of making same, and uses of same
US9721963B1 (en) * 2016-04-08 2017-08-01 Sandisk Technologies Llc Three-dimensional memory device having a transition metal dichalcogenide channel
CN111485224A (zh) * 2019-01-29 2020-08-04 北京石墨烯研究院 化学气相沉积装置

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
MARIYAPPPAN SHANMUGM ET.AL: "Two-dimensional layered semiconductor/graphene heterostructures for solar photovoltaic applications", 《NANOSCALE》 *
YU ZHANG ET AL: "Controlled Growth of High-Quality Monolayer WS2 Layers on Sapphire and Imagine Its Grain Boundary", 《ACS NANO》 *
尤运城等: "类石墨烯二硫化钨薄膜的化学气相沉积法制备及其应用", 《化学进展》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113106544A (zh) * 2021-04-12 2021-07-13 东北师范大学 制备大尺寸高质量二维TMDs单晶及薄膜的方法
CN114108099A (zh) * 2021-12-02 2022-03-01 中国电子科技集团公司第四十六研究所 一种蓝宝石衬底上二硫化钨晶向调控方法

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