CN113840941A - 钝化膜的制造方法 - Google Patents

钝化膜的制造方法 Download PDF

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CN113840941A
CN113840941A CN202080036949.0A CN202080036949A CN113840941A CN 113840941 A CN113840941 A CN 113840941A CN 202080036949 A CN202080036949 A CN 202080036949A CN 113840941 A CN113840941 A CN 113840941A
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passivation
oxygen
substrate
passivation film
gas
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谷本阳祐
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Resonac Holdings Corp
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Showa Denko KK
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Abstract

提供一种钝化膜的制造方法，其能够再现性良好地制造氧原子的浓度低的钝化膜。采用具备钝化工序的方法制造钝化膜，在该钝化工序中，利用含有含氧化合物和硫化氢的钝化气体，对表面具有锗和钼中的至少一者的基板进行处理，在基板的表面上形成含有硫原子的钝化膜，该含氧化合物是在分子中具有氧原子的化合物。钝化气体中的含氧化合物的浓度为0.001摩尔ppm以上且小于75摩尔ppm。

Description

钝化膜的制造方法
技术领域
本发明涉及钝化膜的制造方法。
背景技术
近年来，在半导体领域中，含有除硅(Si)以外的元素的半导体材料受到关注。作为含有除硅以外的元素的半导体材料，例如可举出含有锗(Ge)、铟镓砷(InGaAs)等III-V族元素的半导体材料，含有硫化钼(IV)(MoS2)等金属硫属化物的半导体材料。
这些半导体材料，虽然具有与硅材料相比机动性(迁移率)高的优点，但存在难以成膜的情况、或由于材料间的界面的缺陷密度高而导致机动性降低的情况。
因此，为了降低材料间的界面的缺陷密度，提出了在锗、钼等基板上使用硫化氢(H2S)气体形成钝化膜的方法(例如参照专利文献1)。另外，作为金属硫属化物的成膜方法，提出了利用硫化氢气体对钼氧化物层、钨氧化物层进行处理而形成硫化钼层、硫化钨层的方法(例如参照专利文献2)。
在先技术文献
专利文献1：日本特许公开公报2016年第207789号
专利文献2：日本特许公开公报2017年第61743号
发明内容
发明要解决的课题
但是，根据硫化氢气体的品质，有时会出现钝化膜所含有的氧原子的浓度变高、钝化膜的性能降低的情况。
本发明的课题在于提供一种钝化膜的制造方法，其能够再现性良好地制造氧原子的浓度低的钝化膜。
用于解决课题的手段
为解决上述课题，本发明的一个技术方案如以下的[1]～[5]。
[1]一种钝化膜的制造方法，具备钝化工序，
在所述钝化工序中，利用含有含氧化合物和硫化氢的钝化气体，对表面具有锗和钼中的至少一者的基板进行处理，在所述基板的表面上形成含有硫原子的钝化膜，所述含氧化合物是在分子中具有氧原子的化合物，
所述钝化气体中的所述含氧化合物的浓度为0.001摩尔ppm以上且小于75摩尔ppm。
[2]根据[1]记载的钝化膜的制造方法，所述钝化气体中的所述含氧化合物的浓度为0.5摩尔ppm以上且65摩尔ppm以下。
[3]根据[1]或[2]记载的钝化膜的制造方法，所述含氧化合物是氧气和水中的至少一者。
[4]根据[1]～[3]中任一项记载的钝化膜的制造方法，所述基板在表面具有含有锗和钼中的至少一者的膜。
[5]根据[1]～[4]中任一项记载的钝化膜的制造方法，在温度为20℃以上且1500℃以下、压力为1Pa以上且101kPa以下的条件下，利用所述钝化气体对所述基板进行处理。
发明的效果
根据本发明，能够再现性良好地制造氧原子的浓度低的钝化膜。
附图说明
图1是用于说明本发明涉及的钝化膜的制造方法的一个实施方式的成膜装置的概略图。
图2是表示形成有钝化膜的锗膜的表面状态的分析结果的图表。
图3是表示形成有钝化膜的钼膜的表面状态的分析结果的图表。
具体实施方式
以下，对本发明的一个实施方式进行说明。再者，本实施方式仅表示本发明的一个例子，本发明并不限定于本实施方式。另外，可以对本实施方式施加各种变更或改良，施加了各种变更或改良的方案也包含在本发明中。
本实施方式涉及的钝化膜的制造方法，具备钝化工序，在钝化工序中，利用含有含氧化合物和硫化氢的钝化气体，对表面具有锗和钼中的至少一者的基板进行处理，在基板的表面上形成含有硫原子的钝化膜，该含氧化合物是在分子中具有氧原子的化合物。并且，钝化气体中的含氧化合物的浓度为0.001摩尔ppm以上且小于75摩尔ppm。
通过本实施方式涉及的钝化膜的制造方法，能够抑制不希望的氧化膜的生成，并且生成稳定的硫化膜，因此能够再现性良好地制造氧原子的浓度低的钝化膜。
为了充分抑制不希望的氧化膜的生成，再现性良好地制造氧原子的浓度低的钝化膜，需要使钝化气体中的含氧化合物的浓度为0.001摩尔ppm以上且小于75摩尔ppm，上限优选为65摩尔ppm以下，更优选为40摩尔ppm以下，进一步优选为5摩尔ppm以下，下限可以为0.5摩尔ppm以上。再者，钝化气体中的含氧化合物的浓度越低越好，但低于0.001摩尔ppm的浓度难以测定。
对于含氧化合物的种类没有特别限定，例如可举出氧气(O2)、水(H2O)、一氧化碳(CO)、二氧化碳(CO2)、硫化羰(COS)和二氧化硫(SO2)。这些含氧化合物之中，优选氧气和水中的至少一者。
用钝化气体处理的基板是在表面具有锗和钼中的至少一者的基板，但对于基板的表面以何种形态具有锗和钼中的至少一种并没有特别限定。例如，基板可以在表面具有含有锗和钼中的至少一者的膜。
另外，在表面具有含有锗和钼中的至少一者的膜的基板，只要膜含有锗和钼中的至少一者，则可以是任意的基板，例如优选在半导体元件的形成中所使用的基板。特别优选通过物理蒸镀(PVD)、化学蒸镀(CVD)而在表面形成了含有锗和钼中的至少一者的膜的单晶硅基板。
钝化气体中的硫化氢的浓度只要是足以形成钝化膜的量就没有特别限定，优选为1体积％以上，更优选为2体积％以上，进一步优选为10体积％以上，特别优选为100体积％。对于钝化气体所含有的成分之中除了硫化氢和含氧化合物以外的成分没有特别限定，例如可举出氮气、氩气等惰性气体。
对于钝化工序中利用钝化气体对基板进行处理时的压力(例如利用钝化气体进行处理的腔室内的压力)没有特别限定，优选为1Pa以上且101kPa以下，更优选为10Pa以上且90kPa以下，进一步优选为100Pa以上且80kPa以下。
另外，对于钝化工序中利用钝化气体对基板进行处理时的温度(例如配置在腔室内的基板的温度)没有特别限定，为了得到利用钝化气体进行的基板表面处理的高面内均匀性，优选为20℃以上且1500℃以下，更优选为50℃以上且1200℃以下，进一步优选为100℃以上且1000℃以下。
另外，对于钝化工序中利用钝化气体对基板进行处理的时间长度没有特别限定，考虑到半导体元件制造工艺的效率，优选为120分钟以内。再者，所谓利用钝化气体对基板进行处理的时间，是指从向收纳有基板的腔室供给钝化气体起，直到为了结束利用钝化气体进行的基板表面处理而通过真空泵等将腔室内的钝化气体排出为止的时间。
本实施方式涉及的钝化膜的制造方法，能够很好地应用于在基板的表面形成钝化膜的半导体的成膜装置。对于该成膜装置的结构没有特别限定，对于在作为反应容器的腔室内收纳的基板与连接于腔室的配管之间的位置关系也没有特别限定。
实施例
以下示出实施例和比较例，对本发明进行更详细的说明。
(实施例1)
使用图1所示的成膜装置1，在基板的表面形成了钝化膜。成膜装置1具有进行钝化工序的腔室10、和调整腔室10的内部温度的温度调整装置(未图示)。在腔室10的内部具备支撑试样20的平台11。作为试样20，使用了在硅基板上形成厚度150nm的硅氧化膜、进而在其上形成厚度80nm的锗膜的试样。
腔室10中，在其上游侧分别经由阀32、33连接有将含有含氧化合物和硫化氢的钝化气体供给到腔室10的钝化气体供气用配管12、和将惰性气体供给到腔室10的惰性气体供气用配管13。
另外，腔室10中，在其下游侧连接有将腔室10内的气体排出到外部的排气用配管15，在排气用配管15的下游侧经由阀35连接有真空泵38。腔室10的内部的压力由控制阀35的压力控制器37控制。
使用这样的成膜装置1进行钝化工序。在平台11上设置试样20，将腔室10内的压力减压至小于10Pa之后，将腔室10内的温度升温至800℃。然后，使阀32为打开状态，以101kPa的压力从钝化气体供气用配管12向腔室10内供给钝化气体。该钝化气体是氧气与硫化氢气体的混合气体，钝化气体中的氧气的浓度为60摩尔ppm。此时的钝化气体的流量为100sccm，在试样20的表面形成钝化膜时的腔室10内的压力为67kPa。再者，sccm表示0℃、101.3kPa时的流量(mL/min)。
进行30分钟钝化气体的导入，在温度800℃、压力67kPa的条件下将试样20的表面硫化而形成钝化膜后，停止钝化气体的导入。然后，用真空泵38使腔室10的内部成为真空，从惰性气体供气用配管13向腔室10内供给作为惰性气体的氮气，用氮气置换腔室10的内部。然后，将腔室10内的温度降低至室温，将形成有钝化膜的试样20从腔室10取出。
(实施例2)
除了将钝化气体中的氧气的浓度设为30摩尔ppm以外，与实施例1同样地在基板的表面形成了钝化膜。
(实施例3)
除了将钝化气体中的氧气的浓度设为3.8摩尔ppm以外，与实施例1同样地在基板的表面形成了钝化膜。
(实施例4)
除了将钝化气体中的氧气的浓度设为0.75摩尔ppm以外，与实施例1同样地在基板的表面形成了钝化膜。
(比较例1)
除了将钝化气体中的氧气的浓度设为75摩尔ppm以外，与实施例1同样地在基板的表面形成了钝化膜。
(比较例2)
除了将钝化气体中的氧气的浓度设为150摩尔ppm以外，与实施例1同样地在基板的表面形成了钝化膜。
(实施例5)
作为试样20，使用了在硅基板上形成厚度150nm的硅氧化膜、进而在其上形成厚度80nm的钼膜的试样，除此以外与实施例1同样地在基板的表面形成了钝化膜。
(实施例6)
除了将钝化气体中的氧气的浓度设为30摩尔ppm以外，与实施例5同样地在基板的表面形成了钝化膜。
(实施例7)
除了将钝化气体中的氧气的浓度设为3.8摩尔ppm以外，与实施例5同样地在基板的表面形成了钝化膜。
(实施例8)
除了将钝化气体中的氧气的浓度设为0.75摩尔ppm以外，与实施例5同样地在基板的表面形成了钝化膜。
(比较例3)
除了将钝化气体中的氧气的浓度设为75摩尔ppm以外，与实施例5同样地在基板的表面形成了钝化膜。
(比较例4)
除了将钝化气体中的氧气的浓度设为150摩尔ppm以外，与实施例5同样地在基板的表面形成了钝化膜。
对于实施例1～8和比较例1～4的形成有钝化膜的试样20，采用飞行时间型二次离子质谱分析法(TOF-SIMS：Time-of-Flight Secondary Ion Mass Spectrometry)进行分析，分析了形成有钝化膜的锗膜或钼膜的表面状态。将各个钝化膜中的氧化锗(GeOx)、硫化锗(GeSx)、氧化钼(MoOx)、硫化钼(MoSx)的量示于表1、2和图2、3的图表中。
表1
实施例1 实施例2 实施例3 实施例4 比较例1 比较例2
氧气的浓度(摩尔ppm) 60 30 3.8 0.75 75 150
GeOx的量(任意单位) 516 472 385 292 827 1821
GeSx的量(任意单位) 822 936 1408 1507 390 384
GeOx/GeSx比 0.63 0.50 0.27 0.19 2.12 4.74
表2
实施例5 实施例6 实施例7 实施例8 比较例3 比较例4
氧气的浓度(摩尔ppm) 60 30 3.8 0.75 75 150
MoOx的量(任意单位) 501 430 424 272 852 1639
MoSx的量(任意单位) 748 833 1211 1266 382 357
MoOx/MoSx比 0.67 0.52 0.35 0.21 2.23 4.59
由表1、2和图2、3的图表可知，钝化气体中的氧气的浓度为75摩尔ppm以上的比较例1、2、3、4中，试样20的钝化膜中的氧化物的量相对于硫化物的量的比率大。与此相对，钝化气体中的氧气的浓度小于75摩尔ppm的实施例1～8中，试样20的钝化膜中的氧化物的量相对于硫化物的量的比率明显小于比较例，该结果表示在实施例与比较例之间存在临界条件。这样，显示出通过利用氧气浓度低的钝化气体进行处理，能够在抑制氧化膜生成的同时形成硫化膜。
附图标记说明
1···成膜装置
10···腔室
11···平台
12···钝化气体供气用配管
13···惰性气体供气用配管
15···排气用配管
20···试样

Claims (5)

1.一种钝化膜的制造方法，具备钝化工序，
在所述钝化工序中，利用含有含氧化合物和硫化氢的钝化气体，对表面具有锗和钼中的至少一者的基板进行处理，在所述基板的表面上形成含有硫原子的钝化膜，所述含氧化合物是在分子中具有氧原子的化合物，
所述钝化气体中的所述含氧化合物的浓度为0.001摩尔ppm以上且小于75摩尔ppm。
2.根据权利要求1所述的钝化膜的制造方法，
所述钝化气体中的所述含氧化合物的浓度为0.5摩尔ppm以上且65摩尔ppm以下。
3.根据权利要求1或2所述的钝化膜的制造方法，
所述含氧化合物是氧气和水中的至少一者。
4.根据权利要求1～3中任一项所述的钝化膜的制造方法，
所述基板在表面具有含有锗和钼中的至少一者的膜。
5.根据权利要求1～4中任一项所述的钝化膜的制造方法，
在温度为20℃以上且1500℃以下、压力为1Pa以上且101kPa以下的条件下，利用所述钝化气体对所述基板进行处理。
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