JPH0557205B2 - - Google Patents
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- Publication number
- JPH0557205B2 JPH0557205B2 JP23180984A JP23180984A JPH0557205B2 JP H0557205 B2 JPH0557205 B2 JP H0557205B2 JP 23180984 A JP23180984 A JP 23180984A JP 23180984 A JP23180984 A JP 23180984A JP H0557205 B2 JPH0557205 B2 JP H0557205B2
- Authority
- JP
- Japan
- Prior art keywords
- zns
- film
- substrate
- zns film
- deposited
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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Classifications
-
- 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
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0623—Sulfides, selenides or tellurides
- C23C14/0629—Sulfides, selenides or tellurides of zinc, cadmium or mercury
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Physical Vapour Deposition (AREA)
- Surface Treatment Of Glass (AREA)
Description
【発明の詳細な説明】
＜産業上の利用分野＞
本発明は、大面積基板上に結晶性の良いZnS膜
を低価格で容易に形成しうるZnS膜の作製方法に
関する。DETAILED DESCRIPTION OF THE INVENTION <Industrial Application Field> The present invention relates to a method for manufacturing a ZnS film that can easily form a ZnS film with good crystallinity on a large-area substrate at low cost.
＜従来の技術＞
最近、ZnSは青色発光ダイオードの材料として
注目を集めているが、ZnSは発光特性が特に結晶
性に敏感に影響する。<Prior Art> Recently, ZnS has been attracting attention as a material for blue light emitting diodes, but the light emitting properties of ZnS are particularly sensitive to crystallinity.
従来のZnS膜の作製方法として、真空蒸着法、
スパツタ蒸着法、気相成長法などの方法が行われ
ていたが、導電性の制御が極めて困難であつた。
最近になり、有機金属成長法（Organic Metal
Chemical Vapor Deposition、以下、単に
「MOCVD法」と言う）や分子線エピタキシヤル
法（Molecular Beam Epitaxial Method、以
下、単に「MBE法」という）がZnS膜の導電性
の制御が可能であるとして注目を集めている。例
えば、米国物理学協会発行の学術雑誌、「アブラ
イド フイジツクス レターズ誌（Applied
Physics Letters）」第38巻第５号（1981年）352
頁に、ダブリユ・ステユテイアス氏（W.
STUTIUS）による速報「プリパレイシヨン・オ
ブ・ロー・レジステイビテイ・Ｎ−タイプ・ジン
ク・サルフアイド・バイ・OMVTE
（Preparation of Low Resistivity Ｎ−type
Zinc Selen by OMVTE）」において、有機金属
成長法によりGaAs基板上に直接ZnSe膜の低抵抗
膜を成長、つまり導電性制御できる可能性につい
て報告した。 Conventional methods for producing ZnS films include vacuum evaporation,
Methods such as sputter deposition and vapor phase growth have been used, but it has been extremely difficult to control conductivity.
Recently, organic metal growth
Chemical Vapor Deposition (hereinafter simply referred to as "MOCVD method") and Molecular Beam Epitaxial Method (hereinafter simply referred to as "MBE method") are attracting attention as they are capable of controlling the conductivity of ZnS films. are collecting. For example, Applied Physics Letters is an academic journal published by the American Institute of Physics.
Physics Letters, Vol. 38, No. 5 (1981) 352
On the page, Mr. Davril Steutias (W.
BREAKING NEWS: ``Preparation of Raw Resistance N-Type Zinc Sulfide by OMVTE'' by STUTIUS
(Preparation of Low Resistivity N-type
Zinc Selen by OMVTE), we reported on the possibility of growing a low-resistance ZnSe film directly on a GaAs substrate using an organometallic growth method, that is, controlling the conductivity.
MOCVD法においては、ZnS膜成長用の基板と
してガラス、Si、GaP、GaAsが用いられてお
り、ZnS膜はこれら基板の上面に、それぞれ多結
晶（配向性なし）、配向性を有する多結晶、単結
晶、単結晶として成長させて得られるものであつ
て、結晶性はこの順で良くなると報告されてい
る。 In the MOCVD method, glass, Si, GaP, and GaAs are used as substrates for ZnS film growth. It is obtained by growing a single crystal or a single crystal, and it is reported that crystallinity improves in this order.
＜発明が解決しようとする問題点＞
しかし、ZnS単結晶が成長可能なGaP、GaAs
基板は高価であり、大面積の基板を入手すること
も不可能である。<Problems to be solved by the invention> However, GaP and GaAs, which can grow ZnS single crystals,
Substrates are expensive and large area substrates are not available.
本発明は、従来のZnS膜作製方法におけるこの
ような欠点を解消するためになされたものであつ
て、低価格で大面積の基板を得やすいSi（111）基
板およびガラス基板を使用し、これら基板上面に
それぞれ単結晶および多結晶（配向性あり）の
ZnS膜を成長させうるZnS膜作製方法を提供しよ
うとするものである。 The present invention was made to eliminate these drawbacks in the conventional ZnS film manufacturing method, and uses Si (111) and glass substrates, which are easy to obtain at low cost and have a large area. Single crystal and polycrystalline (with orientation) are formed on the top surface of the substrate.
The present invention aims to provide a method for manufacturing a ZnS film that can grow a ZnS film.
＜問題点を解決するための技術手段＞
本発明者は、上記目的を達成するため、上述し
たSi（111）基板およびガラス基板上に電子ビーム
加熱蒸着したZnS膜がそれぞれ単結晶および
（111）配向の多結晶として形成されるという事実
を基にし、このようなZnS膜をバツフア層として
使用すれば安価で、しかも入手しやすい大面積の
Si（111）基板又はガラス基板を使用してMOCVD
法により、結晶性のよい大面積のZnS膜を作製し
うるとの考の下に実験を重ねた結果、本発明を完
成することができた。<Technical Means for Solving the Problems> In order to achieve the above object, the present inventor has proposed that the ZnS films deposited by electron beam heating on the Si (111) substrate and the glass substrate described above are single crystal and (111), respectively. Based on the fact that ZnS is formed as an oriented polycrystal, it is possible to use such a ZnS film as a buffer layer to create a large-area film that is inexpensive and easily available.
MOCVD using Si (111) substrate or glass substrate
As a result of repeated experiments based on the idea that a large-area ZnS film with good crystallinity could be produced by this method, the present invention was completed.
本発明にかかるZnS膜の作製方法は、基板上面
にZnS膜を蒸着した後、ZnS蒸着膜上に、さらに
有機金属気相成長法によりZnS膜を形成すること
を特徴とするものである。 The method for manufacturing a ZnS film according to the present invention is characterized in that after a ZnS film is deposited on the upper surface of a substrate, a ZnS film is further formed on the ZnS deposited film by metal organic vapor phase epitaxy.
本発明のZnS膜作製方法において、Si（111）基
板又はガラス基板上に蒸着するZnS膜の蒸着方法
は抵抗加熱、電子ビーム加熱、高周波加熱等によ
る真空蒸着、スパツタ蒸着、気相成長法などの方
法が適用できる。また、基板としてSi（111）基板
およびガラス基板が使用できる。 In the ZnS film manufacturing method of the present invention, the ZnS film is deposited on a Si(111) substrate or a glass substrate by vacuum deposition using resistance heating, electron beam heating, high frequency heating, etc., sputter deposition, vapor phase growth, etc. method can be applied. Furthermore, a Si (111) substrate and a glass substrate can be used as the substrate.
有機金属気相成長には、例えばジメチルジンク
（以下、「DMZ」と略称する）とH2Sをソースに
使用する。 For organometallic vapor phase epitaxy, for example, dimethyl zinc (hereinafter abbreviated as "DMZ") and H 2 S are used as sources.
＜作用＞
本発明にかかるZnS膜の作製方法は、導電性の
制御が可能なMOCVD法を採用するに当り、基
板上に一旦、バツフア層としてZnS膜を蒸着させ
てから、ZnS蒸着膜上にMOCVD法でZnS膜を形
成させるため、結晶性がよく、かつ導電性の制御
が可能なZnS膜を作製することができる。<Function> In the method for manufacturing a ZnS film according to the present invention, when adopting the MOCVD method that allows control of conductivity, a ZnS film is first deposited as a buffer layer on a substrate, and then a ZnS film is deposited on the ZnS deposited film. Since the ZnS film is formed using the MOCVD method, it is possible to produce a ZnS film with good crystallinity and controllable conductivity.
＜実施例＞
以下、実施例および比較例を挙げて本発明の内
容を具体的に説明する。<Example> Hereinafter, the content of the present invention will be specifically explained with reference to Examples and Comparative Examples.
実施例 １
Si（111）基板１の表面を希フツ酸でエツチング
して、基板表面のSiO2膜を除いてから、真空槽
２内に入れ、ホルダ３で保持すると共に、ヒータ
４でSi（111）基板１を220℃に加熱する。そして、
10-8Torr程度に排気した真空槽２内に配置した
るつぼ５内のZnSペレツト６をターゲツトとし
て、電子銃７から電子ビームを照射し、基板１の
表面に蒸着速度数Å／secでバツフア層として厚
さ150ÅのZnAs膜８を被着させた。Example 1 The surface of a Si (111) substrate 1 is etched with dilute hydrofluoric acid to remove the SiO 2 film on the surface of the substrate, and then placed in a vacuum chamber 2 and held in a holder 3, while being etched with Si (111) by a heater 4. 111) Heat substrate 1 to 220°C. and,
A ZnS pellet 6 in a crucible 5 placed in a vacuum chamber 2 evacuated to about 10 -8 Torr is irradiated with an electron beam from an electron gun 7 to form a buffer layer on the surface of the substrate 1 at a deposition rate of several Å/sec. Then, a ZnAs film 8 with a thickness of 150 Å was deposited.
次いで、真空槽２内を常圧にもどし、槽内のSi
（111）基板１を取り出し、第２図に示すごとく加
熱炉９内に入れ300℃において約１時間アンニー
ルした。 Next, the inside of the vacuum chamber 2 is returned to normal pressure, and the Si inside the chamber is
(111) The substrate 1 was taken out, placed in a heating furnace 9 as shown in FIG. 2, and annealed at 300° C. for about 1 hour.
その後さらに基板温度を370℃に上げると共に、
図示外のガス供給源から、ジメチルジンク（以
下、「DMZ」で表わす）を流量2.0×10-5mol／
minで、H2Sを流量6.7×10-5mol／minで加熱炉
９内に導入し、60Torrのガス圧の下でDMZと
H2SのMOCVD反応によりZnS蒸着膜８上に、厚
さ4500ÅのZnS膜１０を成長させた。 After that, the substrate temperature was further increased to 370℃,
Dimethyl zinc (hereinafter referred to as "DMZ") was supplied from a gas supply source not shown at a flow rate of 2.0×10 -5 mol/
H 2 S was introduced into the heating furnace 9 at a flow rate of 6.7×10 -5 mol/min, and DMZ and
A ZnS film 10 with a thickness of 4500 Å was grown on the ZnS vapor-deposited film 8 by an H 2 S MOCVD reaction.
得られたZnS膜１０の反射電子線回折像を示す
と第３図に示すごとき干渉回折像Ａ，Ａ，…が得
られ、このZnS膜１０は（111）面に配向した多
結晶であることを示している。 When the reflected electron beam diffraction image of the obtained ZnS film 10 is shown, interference diffraction images A, A, . . . as shown in FIG. It shows.
比較例 １
真空槽内でZnS蒸着膜８を形成せず、基板表面
のSiO2膜を希フツ酸でエツチング除去したSi
（111）基板を、加熱炉内に入れ、実施例１の場合
と同じ条件のMOCVD法で、Si（111）基板上面に
直接ZnS膜１０を厚さ4500Åに成長させた。Comparative Example 1 A Si film in which the ZnS deposited film 8 was not formed in a vacuum chamber, and the SiO 2 film on the substrate surface was removed by etching with dilute hydrofluoric acid.
The (111) substrate was placed in a heating furnace, and by MOCVD under the same conditions as in Example 1, a ZnS film 10 was grown directly on the top surface of the Si (111) substrate to a thickness of 4500 Å.
そして、得られたZnS膜１０の反射電子線回折
像を示すと第４図のごとき同心円状の回折像Ｂ，
Ｂ，…が得られた。この回折像からZnS膜１０の
ZnS結晶は多方向に配向した多結晶であることを
示している。 The reflected electron beam diffraction images of the obtained ZnS film 10 are shown in FIG. 4, with concentric diffraction images B,
B,... were obtained. From this diffraction image, the ZnS film 10
This shows that ZnS crystals are polycrystals oriented in many directions.
実施例 ２
真空槽内のSi（111）基板１の加熱温度を180℃
に調節してZnS膜８を蒸着することと、ZnS膜８
上にMOCVD法により形成するZnS膜の膜厚を
4000Åにすること以外は実施例１と全く同じ製造
方法によつてZnS膜１０を作製した。Example 2 Heating temperature of Si (111) substrate 1 in vacuum chamber was 180°C
The ZnS film 8 is deposited by adjusting the ZnS film 8 to
The thickness of the ZnS film formed on top by MOCVD method is
A ZnS film 10 was manufactured using the same manufacturing method as in Example 1 except that the thickness was 4000 Å.
そして、得られたZnS膜１０のＸ線回折パター
ンＣを第５図に示す。ただし、第５図の横軸は回
折角度（2θ）を度単位で示し、縦軸は回折強度を
示す。 The X-ray diffraction pattern C of the obtained ZnS film 10 is shown in FIG. However, the horizontal axis in FIG. 5 indicates the diffraction angle (2θ) in degrees, and the vertical axis indicates the diffraction intensity.
比較例 ２
Si（111）基板１上面に直接、MOCVD法で被着
するZnS膜１０の膜厚を4000Åにすること以外
は、全く比較例１と同じ方法でZnS膜１０を作製
した。Comparative Example 2 A ZnS film 10 was produced in exactly the same manner as in Comparative Example 1, except that the thickness of the ZnS film 10 was 4000 Å, which was directly deposited on the upper surface of the Si (111) substrate 1 by MOCVD.
かくして得られたZnS膜１０のＸ線回折パター
ンＤを第６図に示す。第６図の結果から、バツフ
ア層８を介して成長させたZnS膜１０の方が、バ
ツフア層８を介さない場合に比べて、（111）ピー
クが強くなり、（111）配向が強くなつていること
がわかる。 FIG. 6 shows the X-ray diffraction pattern D of the ZnS film 10 thus obtained. From the results shown in FIG. 6, the ZnS film 10 grown through the buffer layer 8 has a stronger (111) peak and stronger (111) orientation than when the ZnS film 10 is grown through the buffer layer 8. I know that there is.
以上の結果は、Si（111）基板を用いた場合だけ
でなくガラス基板を使用した場合にも同様の結果
が得られる。 Similar results can be obtained not only when using a Si (111) substrate but also when using a glass substrate.
＜発明の効果＞
以上の説明から明らかなように、Si（111）およ
びガラス基板上へのZnS膜のMOCVD法による成
長において、蒸着したZnS膜をバツフア層として
用いることにより、Si（111）基板上では（111）
配向した多結晶から単結晶へ、またガラス基板上
では、（111）配向性の強い多結晶へ、結晶性の改
善を行うことができる。<Effects of the Invention> As is clear from the above description, in the growth of ZnS films on Si(111) and glass substrates by the MOCVD method, by using the deposited ZnS film as a buffer layer, the Si(111) substrate Above (111)
Crystallinity can be improved from oriented polycrystals to single crystals, and on glass substrates to polycrystals with strong (111) orientation.
したがつて、このZnS膜を使用して発光効率の
よい大面積の青色発光ダイオードや、電場発光
（EL発光）体を作製することも可能となる。 Therefore, using this ZnS film, it is also possible to produce a large-area blue light emitting diode with good luminous efficiency and an electroluminescent (EL light emitting) body.
第１図は本発明のZnS膜の作製方法における
ZnS蒸着膜作製工程で使用する真空蒸着装置の概
略構造図、第２図はZnS蒸着膜上に形成するZnS
膜の有機金属気相成長法の要領を示す要部断面
図、第３図はSi（111）基板上のバツフア層を介し
てMOCVD法で成長させたZnS膜の反射電子回折
パターン図、第４図はバツフア層を介しないでSi
（111）基板上にMOCVD法で成長させたZnS膜の
反射電子回折パターン図、第５図はSi（111）基板
上のバツフア層を介してMOCVD法で成長させ
たZnS膜のＸ線回折パターン図、第６図はバツフ
ア層を介しないでSi（111）基板上にMOCVD法で
成長させたZnS膜のＸ線回折パターン図である。
Figure 1 shows the ZnS film manufacturing method of the present invention.
A schematic structural diagram of the vacuum evaporation equipment used in the ZnS deposited film production process, Figure 2 shows the ZnS deposited on the ZnS deposited film.
Figure 3 is a cross-sectional view of a main part showing the main points of metal organic vapor phase epitaxy of a film. Figure 3 is a backscattered electron diffraction pattern of a ZnS film grown by MOCVD via a buffer layer on a Si (111) substrate. Figure 4 The figure shows Si without a buffer layer.
A backscattered electron diffraction pattern of a ZnS film grown by MOCVD on a (111) substrate. Figure 5 is an X-ray diffraction pattern of a ZnS film grown by MOCVD through a buffer layer on a Si (111) substrate. Figure 6 shows the X-ray diffraction pattern of a ZnS film grown by MOCVD on a Si (111) substrate without a buffer layer.
Claims (1)
上にさらに有機金属気相成長法によりZnS膜を形
成することを特徴とするZnS膜の作製方法。 ２ 基板にSi（111）基板を使用したことを特徴と
する特許請求の範囲第１項記載のZnS膜の作製方
法。 ３ 基板にガラス基板を使用したことを特徴とす
る特許請求の範囲第１項記載のZnS膜の作製方
法。[Claims] 1. A method for producing a ZnS film, which comprises depositing a ZnS film on the upper surface of a substrate, and then further forming a ZnS film on the ZnS deposited film by metal organic vapor phase epitaxy. 2. The method for manufacturing a ZnS film according to claim 1, characterized in that a Si (111) substrate is used as the substrate. 3. The method for producing a ZnS film according to claim 1, characterized in that a glass substrate is used as the substrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23180984A JPS61111137A (en) | 1984-11-02 | 1984-11-02 | Production of zns film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23180984A JPS61111137A (en) | 1984-11-02 | 1984-11-02 | Production of zns film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61111137A JPS61111137A (en) | 1986-05-29 |
| JPH0557205B2 true JPH0557205B2 (en) | 1993-08-23 |
Family
ID=16929355
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP23180984A Granted JPS61111137A (en) | 1984-11-02 | 1984-11-02 | Production of zns film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61111137A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3867161B2 (en) | 2002-09-20 | 2007-01-10 | 独立行政法人物質・材料研究機構 | Thin film element |
| CN107445488B (en) * | 2017-06-15 | 2020-06-16 | 北京大学 | Method for preparing large-area uniform monolayer transition metal chalcogenide |
| CN110965126B (en) * | 2019-11-19 | 2021-08-10 | 有研国晶辉新材料有限公司 | Normal-pressure annealing method of multispectral ZnS material |
-
1984
- 1984-11-02 JP JP23180984A patent/JPS61111137A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS61111137A (en) | 1986-05-29 |
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