WO2021124810A1 - パッシベーション膜の製造方法 - Google Patents

パッシベーション膜の製造方法 Download PDF

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WO2021124810A1
WO2021124810A1 PCT/JP2020/043674 JP2020043674W WO2021124810A1 WO 2021124810 A1 WO2021124810 A1 WO 2021124810A1 JP 2020043674 W JP2020043674 W JP 2020043674W WO 2021124810 A1 WO2021124810 A1 WO 2021124810A1
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Prior art keywords
passivation
gas
oxygen
substrate
film
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PCT/JP2020/043674
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English (en)
French (fr)
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陽祐 谷本
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昭和電工株式会社
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Priority to JP2021565407A priority Critical patent/JPWO2021124810A1/ja
Priority to EP20902992.5A priority patent/EP4080549A4/en
Priority to US17/612,783 priority patent/US20220246447A1/en
Priority to CN202080036949.0A priority patent/CN113840941A/zh
Priority to KR1020227009094A priority patent/KR20220046675A/ko
Publication of WO2021124810A1 publication Critical patent/WO2021124810A1/ja
Priority to IL290573A priority patent/IL290573A/en

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Definitions

  • the present invention relates to a method for producing a passivation film.
  • semiconductor materials containing elements other than silicon have been attracting attention.
  • the semiconductor material containing an element other than silicon include a semiconductor material containing a group III-V element such as germanium (Ge) and indium gallium arsenide (InGaAs), and molybdenum sulfide (IV) (MoS 2 ).
  • Examples thereof include semiconductor materials containing metal chalcogenides.
  • Patent literature method for forming a passivation film is proposed using a hydrogen sulfide (H 2 S) gas on a substrate such as molybdenum 1).
  • a method for forming a metal chalcogenide a method of treating a molybdenum oxide layer and a tungsten oxide layer with hydrogen sulfide gas to form a molybdenum sulfide layer and a tungsten sulfide layer has been proposed (see, for example, Patent Document 2). ).
  • An object of the present invention is to provide a method for producing a passivation film capable of producing a passivation film having a low concentration of oxygen atoms with good reproducibility.
  • one aspect of the present invention is as follows [1] to [5].
  • a substrate having at least one of germanium and molybdenum on the surface is treated with a passion gas containing an oxygen-containing compound which is a compound having an oxygen atom in the molecule and hydrogen sulfide, and a passion film containing a sulfur atom.
  • a passivation step of forming on the surface of the substrate is provided with a passivation step of forming on the surface of the substrate.
  • a method for producing a passivation film in which the concentration of the oxygen-containing compound in the passivation gas is 0.001 molppm or more and less than 75 molppm.
  • [2] The method for producing a passivation film according to [1], wherein the concentration of the oxygen-containing compound in the passivation gas is 0.5 mol ppm or more and 65 mol ppm or less.
  • [3] The method for producing a passivation film according to [1] or [2], wherein the oxygen-containing compound is at least one of oxygen gas and water.
  • [4] The method for producing a passivation film according to any one of [1] to [3], wherein the substrate has a film containing at least one of germanium and molybdenum on its surface.
  • a substrate having at least one of germanium and molybdenum on the surface is treated with a passivation gas containing an oxygen-containing compound which is a compound having an oxygen atom in the molecule and hydrogen sulfide. Therefore, a passivation step of forming a passivation film containing a sulfur atom on the surface of the substrate is provided.
  • the concentration of the oxygen-containing compound in the passivation gas is 0.001 molppm or more and less than 75 molppm.
  • a stable sulfide film can be produced while suppressing the formation of an unintended oxide film, so that a passivation film having a low oxygen atom concentration can be produced with good reproducibility. It is possible.
  • the concentration of the oxygen-containing compound in the passivation gas is 0.001 molppm or more and 75 molppm or more.
  • the upper limit is preferably 65 mol ppm or less, more preferably 40 mol ppm or less, further preferably 5 mol ppm or less, and the lower limit is 0.5 mol ppm. It may be the above.
  • oxygen-containing compound is not particularly limited, but for example, oxygen gas (O 2 ), water (H 2 O), carbon monoxide (CO), carbon dioxide (CO 2 ), carbonyl sulfide (COS). , And sulfur dioxide (SO 2 ).
  • oxygen gas O 2
  • water H 2 O
  • CO carbon monoxide
  • CO 2 carbon dioxide
  • COS carbonyl sulfide
  • SO 2 sulfur dioxide
  • the substrate treated with the passivation gas is a substrate having at least one of germanium and molybdenum on the surface, but the form in which the surface of the substrate has at least one of germanium and molybdenum is not particularly limited.
  • the substrate may have a film on its surface containing at least one of germanium and molybdenum.
  • the substrate having a film containing at least one of germanium and molybdenum on the surface may be any substrate as long as the film contains at least one of germanium and molybdenum.
  • the substrate used for formation is suitable.
  • a single crystal silicon substrate in which a film containing at least one of germanium and molybdenum is deposited on the surface by physical vapor deposition (PVD) or chemical vapor deposition (CVD) is preferable.
  • the concentration of hydrogen sulfide in the passivation gas is not particularly limited as long as it is an amount sufficient for forming the passivation film, but it is preferably 1% by volume or more, and more preferably 2% by volume or more. It is preferably 10% by volume or more, more preferably 100% by volume or more.
  • the components other than the hydrogen sulfide and oxygen-containing compounds among the components contained in the passivation gas are not particularly limited, and examples thereof include inert gases such as nitrogen gas and argon gas.
  • the pressure when the substrate is treated with the passivation gas in the passivation step is not particularly limited, but is preferably 1 Pa or more and 101 kPa or less, and is preferably 10 Pa. It is more preferably 90 kPa or more, and further preferably 100 Pa or more and 80 kPa or less.
  • the temperature at which the substrate is treated with the passivation gas in the passivation step is not particularly limited, but the surface of the substrate surface treated with the passivation gas is highly in-plane. In order to obtain uniformity, it is preferably 20 ° C. or higher and 1500 ° C. or lower, more preferably 50 ° C. or higher and 1200 ° C. or lower, and further preferably 100 ° C. or higher and 1000 ° C. or lower.
  • the length of time for treating the substrate with the passivation gas in the passivation step is not particularly limited, but is preferably 120 minutes or less in consideration of the efficiency of the semiconductor device manufacturing process.
  • the time for treating the substrate with the passivation gas is the time required to supply the passivation gas to the chamber containing the substrate and then to finish the treatment of the surface of the substrate with the passivation gas by using a vacuum pump or the like. Refers to the time until exhaust.
  • the method for producing a passivation film according to the present embodiment can be suitably applied to a semiconductor film forming apparatus for forming a passivation film on the surface of a substrate.
  • the structure of this film forming apparatus is not particularly limited, and the positional relationship between the substrate housed in the chamber, which is the reaction vessel, and the piping connected to the chamber is not particularly limited.
  • Example 1 A passivation film was formed on the surface of the substrate using the film forming apparatus 1 shown in FIG.
  • the film forming apparatus 1 includes a chamber 10 for performing a passivation step and a temperature adjusting device (not shown) for adjusting the temperature inside the chamber 10. Inside the chamber 10, a stage 11 for supporting the sample 20 is provided.
  • a silicon oxide film having a thickness of 150 nm was formed on a silicon substrate, and a germanium film having a thickness of 80 nm was further formed on the silicon oxide film.
  • a passage gas air supply pipe 12 for supplying a passage gas containing an oxygen-containing compound and hydrogen sulfide to the chamber 10 and an inert gas supply pipe 12 for supplying an inert gas to the chamber 10 are provided.
  • the air pipe 13 is connected via valves 32 and 33, respectively.
  • an exhaust pipe 15 for discharging the gas in the chamber 10 to the outside is connected to the downstream side of the chamber 10, and a vacuum pump 38 is connected to the downstream side of the exhaust pipe 15 via a valve 35. It is connected.
  • the pressure inside the chamber 10 is controlled by the pressure controller 37 that controls the valve 35.
  • the passivation process was performed using such a film forming apparatus 1.
  • the sample 20 was placed on the stage 11, the pressure in the chamber 10 was reduced to less than 10 Pa, and then the temperature in the chamber 10 was raised to 800 ° C. After that, the valve 32 was opened, and the passivation gas was supplied into the chamber 10 from the passivation gas air supply pipe 12 at a pressure of 101 kPa.
  • This passivation gas is a mixed gas of oxygen gas and hydrogen sulfide gas, and the concentration of oxygen gas in the passivation gas is 60 mol ppm.
  • the flow rate of the passivation gas at this time was 100 sccm, and the pressure in the chamber 10 when the passivation film was formed on the surface of the sample 20 was 67 kPa.
  • sccm represents a flow rate (mL / min) at 0 ° C. and 101.3 kPa.
  • the passivation gas was introduced for 30 minutes, and the surface of the sample 20 was sulphurized under the conditions of a temperature of 800 ° C. and a pressure of 67 kPa to form a passivation film, and then the introduction of the passivation gas was stopped. Then, the inside of the chamber 10 was evacuated by the vacuum pump 38, and nitrogen gas, which is an inert gas, was supplied into the chamber 10 from the inert gas air supply pipe 13, and the inside of the chamber 10 was replaced with the nitrogen gas. Then, the temperature in the chamber 10 was lowered to room temperature, and the sample 20 on which the passivation film was formed was taken out from the chamber 10.
  • nitrogen gas which is an inert gas
  • Example 2 A passivation film was formed on the surface of the substrate in the same manner as in Example 1 except that the concentration of oxygen gas in the passivation gas was 30 mol ppm.
  • Example 3 A passivation film was formed on the surface of the substrate in the same manner as in Example 1 except that the concentration of oxygen gas in the passivation gas was 3.8 mol ppm.
  • Example 4 A passivation film was formed on the surface of the substrate in the same manner as in Example 1 except that the concentration of oxygen gas in the passivation gas was 0.75 mol ppm.
  • Example 1 A passivation film was formed on the surface of the substrate in the same manner as in Example 1 except that the concentration of oxygen gas in the passivation gas was 75 mol ppm.
  • Comparative Example 2 A passivation film was formed on the surface of the substrate in the same manner as in Example 1 except that the concentration of oxygen gas in the passivation gas was 150 mol ppm.
  • Example 5 As the sample 20, a substrate having a silicon oxide film having a thickness of 150 nm formed on the silicon substrate and a molybdenum film having a thickness of 80 nm formed on the silicon substrate was used in the same manner as in Example 1. A passivation film was formed on the surface of the silicon. (Example 6) A passivation film was formed on the surface of the substrate in the same manner as in Example 5 except that the concentration of oxygen gas in the passivation gas was 30 mol ppm.
  • Example 7 A passivation film was formed on the surface of the substrate in the same manner as in Example 5 except that the concentration of oxygen gas in the passivation gas was 3.8 mol ppm.
  • Example 8 A passivation film was formed on the surface of the substrate in the same manner as in Example 5 except that the concentration of oxygen gas in the passivation gas was 0.75 mol ppm.
  • Example 3 A passivation film was formed on the surface of the substrate in the same manner as in Example 5 except that the concentration of oxygen gas in the passivation gas was 75 mol ppm.
  • Comparative Example 4 A passivation film was formed on the surface of the substrate in the same manner as in Example 5 except that the concentration of oxygen gas in the passivation gas was 150 mol ppm.

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Abstract

酸素原子の濃度が低いパッシベーション膜を再現性良く製造することが可能なパッシベーション膜の製造方法を提供する。ゲルマニウム及びモリブデンの少なくとも一方を表面に有する基板を、分子中に酸素原子を有する化合物である酸素含有化合物と硫化水素とを含有するパッシベーションガスで処理して、硫黄原子を含有するパッシベーション膜を基板の表面上に形成するパッシベーション工程を備える方法により、パッシベーション膜を製造する。パッシベーションガス中の酸素含有化合物の濃度は、０．００１モルｐｐｍ以上７５モルｐｐｍ未満である。

Description

パッシベーション膜の製造方法
　本発明はパッシベーション膜の製造方法に関する。
　近年、半導体分野において、シリコン（Ｓｉ）以外の元素を含有する半導体材料が注目されている。シリコン以外の元素を含有する半導体材料としては、例えば、ゲルマニウム（Ｇｅ）、インジウムガリウム砒素（ＩｎＧａＡｓ）等のＩＩＩ－Ｖ族元素を含有する半導体材料や、硫化モリブデン（ＩＶ）（ＭｏＳ2）等の金属カルコゲナイドを含有する半導体材料が挙げられる。
　これらの半導体材料は、シリコン材料と比較してモビリティ（移動度）が高いというメリットを有しているものの、成膜が困難である場合や、材料間の界面の欠陥密度が高いことによりモビリティが低下する場合があった。
　そこで、材料間の界面の欠陥密度を低くするために、ゲルマニウム、モリブデン等の基板の上に硫化水素（Ｈ2Ｓ）ガスを用いてパッシベーション膜を形成する方法が提案されている（例えば特許文献１を参照）。また、金属カルコゲナイドの成膜方法として、モリブデン酸化物層、タングステン酸化物層を硫化水素ガスで処理して硫化モリブデン層、硫化タングステン層を形成する方法が提案されている（例えば特許文献２を参照）。
日本国特許公開公報　２０１６年第２０７７８９号 日本国特許公開公報　２０１７年第６１７４３号
　しかしながら、硫化水素ガスの品質によって、パッシベーション膜が含有する酸素原子の濃度が高くなり、パッシベーション膜の性能が低下する場合があった。
　本発明は、酸素原子の濃度が低いパッシベーション膜を再現性良く製造することが可能なパッシベーション膜の製造方法を提供することを課題とする。
　前記課題を解決するため、本発明の一態様は以下の［１］～［５］の通りである。
［１］　ゲルマニウム及びモリブデンの少なくとも一方を表面に有する基板を、分子中に酸素原子を有する化合物である酸素含有化合物と硫化水素とを含有するパッシベーションガスで処理して、硫黄原子を含有するパッシベーション膜を前記基板の表面上に形成するパッシベーション工程を備え、
　前記パッシベーションガス中の前記酸素含有化合物の濃度が０．００１モルｐｐｍ以上７５モルｐｐｍ未満であるパッシベーション膜の製造方法。
［２］　前記パッシベーションガス中の前記酸素含有化合物の濃度が０．５モルｐｐｍ以上６５モルｐｐｍ以下である［１］に記載のパッシベーション膜の製造方法。
［３］　前記酸素含有化合物が酸素ガス及び水の少なくとも一方である［１］又は［２］に記載のパッシベーション膜の製造方法。
［４］　前記基板は、ゲルマニウム及びモリブデンの少なくとも一方を含有する膜を表面に有する［１］～［３］のいずれか一項に記載のパッシベーション膜の製造方法。
［５］　温度２０℃以上１５００℃以下、圧力１Ｐａ以上１０１ｋＰａ以下の条件下で、前記基板を前記パッシベーションガスで処理する［１］～［４］のいずれか一項に記載のパッシベーション膜の製造方法。
　本発明によれば、酸素原子の濃度が低いパッシベーション膜を再現性良く製造することが可能である。
本発明に係るパッシベーション膜の製造方法の一実施形態を説明する成膜装置の概略図である。 パッシベーション膜が形成されたゲルマニウム膜の表面状態の分析結果を示すグラフである。 パッシベーション膜が形成されたモリブデン膜の表面状態の分析結果を示すグラフである。
　本発明の一実施形態について以下に説明する。なお、本実施形態は本発明の一例を示したものであって、本発明は本実施形態に限定されるものではない。また、本実施形態には種々の変更又は改良を加えることが可能であり、その様な変更又は改良を加えた形態も本発明に含まれ得る。
　本実施形態に係るパッシベーション膜の製造方法は、ゲルマニウム及びモリブデンの少なくとも一方を表面に有する基板を、分子中に酸素原子を有する化合物である酸素含有化合物と硫化水素とを含有するパッシベーションガスで処理して、硫黄原子を含有するパッシベーション膜を基板の表面上に形成するパッシベーション工程を備える。そして、パッシベーションガス中の酸素含有化合物の濃度は、０．００１モルｐｐｍ以上７５モルｐｐｍ未満である。
　本実施形態に係るパッシベーション膜の製造方法によれば、意図しない酸化膜の生成を抑制しつつ安定な硫化膜を生成することができるので、酸素原子の濃度が低いパッシベーション膜を再現性良く製造することが可能である。
　意図しない酸化膜の生成を十分に抑制して、酸素原子の濃度が低いパッシベーション膜を再現性良く製造するためには、パッシベーションガス中の酸素含有化合物の濃度は０．００１モルｐｐｍ以上７５モルｐｐｍ未満とする必要があるが、上限は、６５モルｐｐｍ以下とすることが好ましく、４０モルｐｐｍ以下とすることがより好ましく、５モルｐｐｍ以下とすることがさらに好ましく、下限は０．５モルｐｐｍ以上であってもよい。なお、パッシベーションガス中の酸素含有化合物の濃度は低いほど好ましいが、０．００１モルｐｐｍよりも低い濃度は測定が困難である。
　酸素含有化合物の種類は特に限定されるものではないが、例えば、酸素ガス（Ｏ2）、水（Ｈ2Ｏ）、一酸化炭素（ＣＯ）、二酸化炭素（ＣＯ2）、硫化カルボニル（ＣＯＳ）、及び二酸化硫黄（ＳＯ2）が挙げられる。これらの酸素含有化合物の中では、酸素ガス及び水の少なくとも一方が好ましい。
　パッシベーションガスで処理される基板は、ゲルマニウム及びモリブデンの少なくとも一方を表面に有する基板であるが、基板の表面がゲルマニウム及びモリブデンの少なくとも一方をどのような形態で有しているかは、特に限定されない。例えば、基板は、ゲルマニウム及びモリブデンの少なくとも一方を含有する膜を表面に有していてもよい。
　また、ゲルマニウム及びモリブデンの少なくとも一方を含有する膜を表面に有する基板は、膜がゲルマニウム及びモリブデンの少なくとも一方を含有するならば、どのような基板であっても差し支えないが、例えば、半導体素子の形成に使用される基板が好適である。特に、ゲルマニウム及びモリブデンの少なくとも一方を含有する膜が物理蒸着（ＰＶＤ）や化学蒸着（ＣＶＤ）で表面に成膜された単結晶シリコン基板が好ましい。
　パッシベーションガス中の硫化水素の濃度は、パッシベーション膜の成膜に十分な量であれば特に限定されるものではないが、１体積％以上であることが好ましく、２体積％以上であることがより好ましく、１０体積％以上であることがさらに好ましく、１００体積％であることが特に好ましい。パッシベーションガスに含有される成分のうち硫化水素及び酸素含有化合物以外の成分は、特に限定されるものではないが、例えば、窒素ガス、アルゴンガス等の不活性ガスを挙げることができる。
　パッシベーション工程において基板をパッシベーションガスで処理する際の圧力（例えば、パッシベーションガスによる処理が行われるチャンバー内の圧力）は、特に限定されるものではないが、１Ｐａ以上１０１ｋＰａ以下であることが好ましく、１０Ｐａ以上９０ｋＰａ以下であることがより好ましく、１００Ｐａ以上８０ｋＰａ以下であることがさらに好ましい。
　また、パッシベーション工程において基板をパッシベーションガスで処理する際の温度（例えば、チャンバー内に配された基板の温度）は、特に限定されるものではないが、パッシベーションガスによる基板表面の処理の高い面内均一性を得るためには、２０℃以上１５００℃以下であることが好ましく、５０℃以上１２００℃以下であることがより好ましく、１００℃以上１０００℃以下であることがさらに好ましい。
　さらに、パッシベーション工程において基板をパッシベーションガスで処理する時間の長さは、特に限定されるものではないが、半導体素子製造プロセスの効率を考慮すると、１２０分以内であることが好ましい。なお、基板をパッシベーションガスで処理する時間とは、基板が収容されたチャンバーにパッシベーションガスを供給してから、パッシベーションガスによる基板の表面の処理を終えるためにチャンバー内のパッシベーションガスを真空ポンプ等により排気するまでの時間を指す。
　本実施形態に係るパッシベーション膜の製造方法は、基板の表面にパッシベーション膜を成膜する半導体の成膜装置に対して好適に適用することができる。この成膜装置の構造は特に限定されるものではなく、反応容器であるチャンバー内に収容された基板と、チャンバーに接続された配管との位置関係も特に限定されない。
　以下に実施例及び比較例を示して、本発明をより詳細に説明する。
（実施例１）
　図１に示す成膜装置１を用いて、基板の表面にパッシベーション膜を成膜した。成膜装置１は、パッシベーション工程を行うチャンバー１０と、チャンバー１０の内部の温度を調整する温度調整装置（図示せず）と、を有する。チャンバー１０の内部には、試料２０を支持するステージ１１が備えられている。試料２０としては、シリコン基板上に厚さ１５０ｎｍのシリコン酸化膜が形成され、さらにその上に厚さ８０ｎｍのゲルマニウム膜が形成されたものを使用した。
　チャンバー１０には、その上流側に、酸素含有化合物と硫化水素とを含有するパッシベーションガスをチャンバー１０に供給するパッシベーションガス給気用配管１２と、不活性ガスをチャンバー１０に供給する不活性ガス給気用配管１３とが、それぞれバルブ３２、３３を介して接続されている。
　また、チャンバー１０には、その下流側に、チャンバー１０内のガスを外部に排出する排気用配管１５が接続されており、排気用配管１５の下流側にはバルブ３５を介して真空ポンプ３８が接続されている。チャンバー１０の内部の圧力は、バルブ３５を制御する圧力コントローラ３７により制御される。
　このような成膜装置１を使用して、パッシベーション工程を行った。ステージ１１上に試料２０を設置し、チャンバー１０内の圧力を１０Ｐａ未満まで減圧した後に、チャンバー１０内の温度を８００℃に昇温した。その後、バルブ３２を開状態とし、パッシベーションガス給気用配管１２からチャンバー１０内にパッシベーションガスを１０１ｋＰａの圧力で供給した。このパッシベーションガスは酸素ガスと硫化水素ガスの混合ガスであり、パッシベーションガス中の酸素ガスの濃度は６０モルｐｐｍである。このときのパッシベーションガスの流量は１００ｓｃｃｍとし、試料２０の表面にパッシベーション膜を成膜する際のチャンバー１０内の圧力は６７ｋＰａとした。なお、ｓｃｃｍは、０℃、１０１．３ｋＰａにおける流量（ｍＬ／ｍｉｎ）を表す。
　パッシベーションガスの導入を３０分間行って、温度８００℃、圧力６７ｋＰａの条件下で試料２０の表面を硫化しパッシベーション膜を成膜したら、パッシベーションガスの導入を停止した。そして、チャンバー１０の内部を真空ポンプ３８で真空にし、不活性ガス給気用配管１３からチャンバー１０内に不活性ガスである窒素ガスを供給してチャンバー１０の内部を窒素ガスで置換した。その後、チャンバー１０内の温度を室温に下げて、パッシベーション膜を成膜した試料２０をチャンバー１０から取り出した。
（実施例２）
　パッシベーションガス中の酸素ガスの濃度を３０モルｐｐｍとした点以外は、実施例１と同様にして、基板の表面にパッシベーション膜を成膜した。
（実施例３）
　パッシベーションガス中の酸素ガスの濃度を３．８モルｐｐｍとした点以外は、実施例１と同様にして、基板の表面にパッシベーション膜を成膜した。
（実施例４）
　パッシベーションガス中の酸素ガスの濃度を０．７５モルｐｐｍとした点以外は、実施例１と同様にして、基板の表面にパッシベーション膜を成膜した。
（比較例１）
　パッシベーションガス中の酸素ガスの濃度を７５モルｐｐｍとした点以外は、実施例１と同様にして、基板の表面にパッシベーション膜を成膜した。
（比較例２）
　パッシベーションガス中の酸素ガスの濃度を１５０モルｐｐｍとした点以外は、実施例１と同様にして、基板の表面にパッシベーション膜を成膜した。
（実施例５）
　試料２０として、シリコン基板上に厚さ１５０ｎｍのシリコン酸化膜が形成され、さらにその上に厚さ８０ｎｍのモリブデン膜が形成されたものを使用した点以外は、実施例１と同様にして、基板の表面にパッシベーション膜を成膜した。
（実施例６）
　パッシベーションガス中の酸素ガスの濃度を３０モルｐｐｍとした点以外は、実施例５と同様にして、基板の表面にパッシベーション膜を成膜した。
（実施例７）
　パッシベーションガス中の酸素ガスの濃度を３．８モルｐｐｍとした点以外は、実施例５と同様にして、基板の表面にパッシベーション膜を成膜した。
（実施例８）
　パッシベーションガス中の酸素ガスの濃度を０．７５モルｐｐｍとした点以外は、実施例５と同様にして、基板の表面にパッシベーション膜を成膜した。
（比較例３）
　パッシベーションガス中の酸素ガスの濃度を７５モルｐｐｍとした点以外は、実施例５と同様にして、基板の表面にパッシベーション膜を成膜した。
（比較例４）
　パッシベーションガス中の酸素ガスの濃度を１５０モルｐｐｍとした点以外は、実施例５と同様にして、基板の表面にパッシベーション膜を成膜した。
　実施例１～８及び比較例１～４のパッシベーション膜を成膜した試料２０に対して、飛行時間型二次イオン質量分析法（ＴＯＦ－ＳＩＭＳ：Time-of-Flight Secondary Ion Mass Spectrometry）による分析を行い、パッシベーション膜が形成されたゲルマニウム膜又はモリブデン膜の表面状態を分析した。それぞれのパッシベーション膜中の酸化ゲルマニウム（ＧｅＯx）、硫化ゲルマニウム（ＧｅＳx）、酸化モリブデン（ＭｏＯx）、硫化モリブデン（ＭｏＳx）の量を表１、２及び図２、３のグラフに示す。
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000002
　表１、２及び図２、３のグラフから分かるように、パッシベーションガス中の酸素ガスの濃度が７５モルｐｐｍ以上である比較例１、２、３、４は、試料２０のパッシベーション膜中の硫化物の量に対する酸化物の量の比率が大きかった。これに対して、パッシベーションガス中の酸素ガスの濃度が７５モルｐｐｍ未満である実施例１～８は、試料２０のパッシベーション膜中の硫化物の量に対する酸化物の量の比率が、比較例に比べて顕著に小さく、実施例と比較例の間に臨界的条件が存在することを示す結果であった。このように、酸素ガスの濃度が低いパッシベーションガスを用いて処理することにより、酸化膜の生成を抑制しつつ硫化膜を成膜できることが示された。
　　　１・・・成膜装置
　　１０・・・チャンバー
　　１１・・・ステージ
　　１２・・・パッシベーションガス給気用配管
　　１３・・・不活性ガス給気用配管
　　１５・・・排気用配管
　　２０・・・試料

Claims (5)

  1. 　ゲルマニウム及びモリブデンの少なくとも一方を表面に有する基板を、分子中に酸素原子を有する化合物である酸素含有化合物と硫化水素とを含有するパッシベーションガスで処理して、硫黄原子を含有するパッシベーション膜を前記基板の表面上に形成するパッシベーション工程を備え、
    　前記パッシベーションガス中の前記酸素含有化合物の濃度が０．００１モルｐｐｍ以上７５モルｐｐｍ未満であるパッシベーション膜の製造方法。
  2. 　前記パッシベーションガス中の前記酸素含有化合物の濃度が０．５モルｐｐｍ以上６５モルｐｐｍ以下である請求項１に記載のパッシベーション膜の製造方法。
  3. 　前記酸素含有化合物が酸素ガス及び水の少なくとも一方である請求項１又は請求項２に記載のパッシベーション膜の製造方法。
  4. 　前記基板は、ゲルマニウム及びモリブデンの少なくとも一方を含有する膜を表面に有する請求項１～３のいずれか一項に記載のパッシベーション膜の製造方法。
  5. 　温度２０℃以上１５００℃以下、圧力１Ｐａ以上１０１ｋＰａ以下の条件下で、前記基板を前記パッシベーションガスで処理する請求項１～４のいずれか一項に記載のパッシベーション膜の製造方法。
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