JPS5948786B2 - Molecular beam crystal growth method - Google Patents
Molecular beam crystal growth methodInfo
- Publication number
- JPS5948786B2 JPS5948786B2 JP20215082A JP20215082A JPS5948786B2 JP S5948786 B2 JPS5948786 B2 JP S5948786B2 JP 20215082 A JP20215082 A JP 20215082A JP 20215082 A JP20215082 A JP 20215082A JP S5948786 B2 JPS5948786 B2 JP S5948786B2
- Authority
- JP
- Japan
- Prior art keywords
- molecular beam
- growth method
- crystal growth
- crystal
- substrate
- 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
Links
- 238000002109 crystal growth method Methods 0.000 title claims description 6
- 239000000758 substrate Substances 0.000 claims description 24
- 239000013078 crystal Substances 0.000 claims description 15
- 239000004065 semiconductor Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000001514 detection method Methods 0.000 claims description 2
- 230000012010 growth Effects 0.000 description 16
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 10
- 230000008020 evaporation Effects 0.000 description 7
- 238000001704 evaporation Methods 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 6
- 238000001451 molecular beam epitaxy Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000005530 etching Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910052594 sapphire Inorganic materials 0.000 description 2
- 239000010980 sapphire Substances 0.000 description 2
- 230000002123 temporal effect Effects 0.000 description 2
- 238000007664 blowing Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 230000003442 weekly effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Physical Deposition Of Substances That Are Components Of Semiconductor Devices (AREA)
Description
【発明の詳細な説明】
本発明は、分子線エビタキシー法（ＭＢＥ法と略称され
る）による化合物半導体の結晶成長に係る。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to crystal growth of compound semiconductors by the molecular beam epitaxy method (abbreviated as MBE method).
特に、基板結晶と組成の異なる成長層の成長に際し、膜
厚を再現性良く制御する方法に関するものである。ＭＢ
Ｅ法による化合物半導体の結晶成長法の利点の一つに、
ウェハ面内の膜厚の均一性と制御性が他の結晶成長法、
例えば液相成長法に対してすぐれていることがあげられ
る。In particular, the present invention relates to a method for controlling the film thickness with good reproducibility when growing a growth layer having a composition different from that of a substrate crystal. M.B.
One of the advantages of the compound semiconductor crystal growth method using the E method is that
The uniformity and controllability of the film thickness within the wafer plane is superior to other crystal growth methods.
For example, it is superior to liquid phase growth.
しかし乍ら、ＭＢＥ法においても、分子ビームの供給速
度が変動したり、蒸発ルツボ内の蒸発物質量が成長回数
と共に減少してくると、成長層の厚みを再現性よく制御
することは困難である。従来、この点については、水晶
振動子や、イオンゲージを分子線ビームの広がりの中に
さし入れて、飛来する分子線強度を一定に保つようなフ
ィードバック制御が行なわれている。しかしこのような
検出器は、基板の直上に設置できない上に、実際に成長
した膜厚を観察しているわけではないので、必ずしも良
好な制御結果が得られなかつた。この他の方法として、
真空容器の外から、ビューインタポートのガラス窓を通
して、レーザ光を成長中の結晶表面に当てて、化合物の
組成差による屈折率差で生ずる干渉パターンの時間変化
を検出する方法が試みられた。しかし、実際には、膜厚
の均一性を確保するために、基板ホルダーごと基板を回
転させることが多いので、レーザ光の方向をうまく検出
器にもどすことは困難であつた。本発明の目的は、上記
の問題点を解決し、基板結晶と組成の異なる成長層の膜
厚を容易に検出しながら成長を行なう方法を提供するこ
とにある。However, even in the MBE method, it is difficult to control the thickness of the grown layer with good reproducibility if the supply rate of the molecular beam fluctuates or if the amount of evaporated material in the evaporation crucible decreases with the number of growths. be. Conventionally, regarding this point, feedback control has been performed in which a crystal oscillator or an ion gauge is inserted into the spread of the molecular beam to keep the intensity of the incoming molecular beam constant. However, such a detector cannot be installed directly above the substrate, and it does not necessarily observe the actual thickness of the grown film, so it has not always been possible to obtain good control results. As another method,
An attempt was made to detect the temporal changes in the interference pattern caused by the difference in refractive index due to the difference in composition of the compounds by shining a laser beam onto the surface of the growing crystal from outside the vacuum container through the glass window of the viewing interface. However, in reality, in order to ensure uniformity of film thickness, the substrate is often rotated together with the substrate holder, so it is difficult to successfully return the direction of the laser beam to the detector. SUMMARY OF THE INVENTION An object of the present invention is to solve the above-mentioned problems and provide a method for growing a growing layer having a composition different from that of a substrate crystal while easily detecting the thickness thereof.
化合物半導体のヘテロ構造の代表例として、ＧａＡｓ基
板結晶の上に、ＧａＡｌＡｓ層を成長する場合を例にと
つて本発明を説明する。第１図は膜厚モニター用赤外検
出器付の分子線エビタキシー成長装置の概略図である。
８は超高真空谷器、４は基板ホールダ一でヒータが設け
られている。The present invention will be described using a case where a GaAlAs layer is grown on a GaAs substrate crystal as a representative example of a compound semiconductor heterostructure. FIG. 1 is a schematic diagram of a molecular beam epitaxy growth apparatus equipped with an infrared detector for monitoring film thickness.
Reference numeral 8 is an ultra-high vacuum valley device, and reference numeral 4 is a substrate holder equipped with a heater.
９はマニユビレータ一である。Reference numeral 9 is a manubilator.
５は試料ののぞき窓、６はこれに接続された赤外検出器
である。5 is a sample viewing window, and 6 is an infrared detector connected to this.
７は蒸発セルである。7 is an evaporation cell.
ＭＢＥ成長法では、ＧａＡｓ結晶１は第１図に示したよ
うに、Ｉｎ２によつて、ＭＯ製の板３にはりつけられた
のち、基板加熱用ヒータ付の基板ホールダ一４にとりつ
けられる。Ｉｎは成長温度の６００〜７００℃では溶け
て、その表面張力によつて、ＧａＡｓを、応力フリーの
状態でＭＯ板にはりつける働きをする。ＭＯ板は、ヒー
トシンクとして、均一加熱に役立つ。この配置で、基板
を成長温度に加熱するとプランク分布に対応したビーク
波長（たとえば１〜２μｍ程度）の赤外線が表面から放
射される。In the MBE growth method, as shown in FIG. 1, a GaAs crystal 1 is attached to an MO plate 3 using In2, and then attached to a substrate holder 14 equipped with a heater for heating the substrate. In melts at the growth temperature of 600 to 700°C, and its surface tension serves to attach GaAs to the MO plate in a stress-free state. The MO plate serves as a heat sink for uniform heating. With this arrangement, when the substrate is heated to the growth temperature, infrared rays with a peak wavelength (for example, about 1 to 2 μm) corresponding to the Planck distribution are emitted from the surface.
この波長域ではＧａＡｓ，ＧａＡｌＡｓはほぼ透明であ
る。ここで、表面基板に、ＧａＡｌＡｓのように、基板
と屈折率の異なる成長層が付着しはじめると、この熱放
射赤外線は、成長中で多重反射して干渉をひきおこす。
従つて、この赤外線の強度を、真空容器のガラス窓を通
して赤外検出器でモニターすると、成長層厚が厚くなる
につれて正弦波的に振動するパターンを示す。干渉パタ
ーンの周期（山と山，谷と谷）に対応する膜厚差をΔｄ
とすると、赤外線の検出波長をλ，ＧａＡｌＡｓの屈折
率をｎとした場合、の関係がなりたつ。In this wavelength range, GaAs and GaAlAs are almost transparent. Here, when a grown layer such as GaAlAs, which has a different refractive index from the substrate, begins to adhere to the surface substrate, this thermal radiation infrared rays undergo multiple reflections during the growth, causing interference.
Therefore, when the intensity of this infrared ray is monitored with an infrared detector through the glass window of the vacuum container, it shows a pattern that oscillates in a sinusoidal manner as the thickness of the grown layer increases. The film thickness difference corresponding to the period of the interference pattern (peak-to-peak, valley-to-trough) is Δd.
Then, when the detection wavelength of infrared rays is λ and the refractive index of GaAlAs is n, the following relationship holds true.
ＧａＡｌＡｓなど多くの化合物半導体の近赤外域での屈
折率は既知であるので、この振動パターンからΔｄがわ
かり、山と谷の数を数えていけば、少くとも（１）式よ
り」（〜２０００１４ｎ〜１０００λの１０分の１精度
で膜厚をモニターすることができる。Since the refractive index of many compound semiconductors such as GaAlAs in the near-infrared region is known, Δd can be found from this vibration pattern, and by counting the number of peaks and valleys, at least from equation (1).'' (~200014n The film thickness can be monitored with an accuracy of 1/10 of ~1000λ.
以下、本発明を実施例に基づいて更に詳細に説明する。Hereinafter, the present invention will be explained in more detail based on examples.
ここでは、半絶縁ＧａＡｓ基板上に、アンドープの高純
度ＧａＡｓ層（ｎ〜１Ｘ１０１４ｃｒｆＬ−３３μｍ）
と、Ｓｉドーブしたキヤリヤ濃度（ｎ〜１×１０１８ｃ
ｍ−３）のｎ−ＧａＯ．７ＡｌＯ．３Ａｓ層（厚さ０．
５μｍ）を順次成長した構造の成長例を示す。Ｈ２ＳＯ
４糸エツナング液で衣面を３μｍエツナング除去したの
ち、純水洗浄、スピンナ一乾燥した半絶縁性ＧａＡｓ結
晶１を、Ｉｎ２を用いてＭＯ板３にはりつける。Here, an undoped high-purity GaAs layer (n~1X1014crfL-33μm) is formed on a semi-insulating GaAs substrate.
and Si-doped carrier concentration (n~1×1018c
m-3) n-GaO. 7AlO. 3As layer (thickness 0.
An example of the growth of a structure in which a thickness of 5 μm) was grown sequentially is shown. H2SO
After etching the surface of the coating by 3 μm using a 4-thread etching solution, the semi-insulating GaAs crystal 1, which had been washed with pure water and dried using a spinner, was attached to the MO plate 3 using In2.
この試料を真空容器８内にセツトし、１×１０−１０Ｔ
０ｒｒの超高真空に排気する。蒸発セル７よりＡｓの分
子線をふきつけながら６５０℃に昇温して、表面の酸化
物を除去する。こののち、Ｇａ，Ａｌ，Ａｓ，Ｓｉの蒸
発セル７のシヤツタ一を適宜開閉して、通常の如く上述
の積層構造を成長した。Ｇａセルは１０００℃，Ａｌセ
ルは１１５０℃，Ａｓセルは３５０℃，Ｓｉセルは１０
００゜Ｃに保つた。成長中の基板温度は６７０℃に保つ
た。蒸発セルと基板との距離は１５ＣｆＬとし、基板ホ
ルダーを毎分３回転で回転させて、ウエハ面内での膜厚
とドーピングレベルの均一性向上をはかつてある。成長
中の基板表面を正面にとらえるのぞき窓５（サファイア
製で、波長４μｍまで透過率９５％以上）を介して、望
遠レンズ付の赤外検出器６で、波長２μｍ前後の赤外線
強度を連続モニターした。This sample was set in a vacuum container 8 and 1×10-10T
Evacuate to ultra-high vacuum of 0rr. The temperature is raised to 650° C. while blowing As molecular beams from the evaporation cell 7 to remove oxides on the surface. Thereafter, the shutters of the Ga, Al, As, and Si evaporation cells 7 were opened and closed as appropriate to grow the above-mentioned laminated structure as usual. Ga cell: 1000℃, Al cell: 1150℃, As cell: 350℃, Si cell: 10℃
It was maintained at 00°C. The substrate temperature during growth was maintained at 670°C. The distance between the evaporation cell and the substrate was 15 CfL, and the substrate holder was rotated at 3 revolutions per minute to improve the uniformity of the film thickness and doping level within the wafer surface. The infrared intensity at a wavelength of around 2 μm is continuously monitored by an infrared detector 6 with a telephoto lens through a viewing window 5 (made of sapphire, transmittance of 95% or more up to a wavelength of 4 μm) that directly captures the surface of the growing substrate. did.
この赤外検出器としては、市販の二色パイロメータを用
いた。これは、３００〜８００℃の温度範囲を、波長２
．３μｍと、１．８μｍの二つの波長での赤外線強度比
から計算で求めるものである。このパイロメータの温度
出力を第２図に示した。成長開始前は６７０℃でほぼ一
定であつたが、ＧａＡｓの成長を開始するとはじめの１
０分位は、基板ヒータ面へのＧａやＧａＡｓ付着で表面
の輻射率が変動するため温度が変動する。その後はほぼ
一定の６７０℃に戻り、ＧａＯ７ＡｌＯ，Ａｓを成長は
じめると、再び１０分程度温度が変動したのち、前述し
た如く表面温度が週期的に変化しはじめた。成長後に、
結晶断面をステイニングしてＳＥＭ観察して厚みを測定
した所、先の（１）式の関係をもとに、第２図の干渉パ
ターンの週期数から求めた厚みと、実測値が目標値５０
００人に対して誤差１５０Ａで一致することがわかる。
同様の方法で、ＧａとＡ２の蒸発セルの温度を１０５０
℃と、１２００℃に変えて成長した所、分子線ビーム強
度の増加により成長速度が増したのに対応して、第２図
に相当する干渉パターンの時間的変動もはやくなつた。
このように、本発明の方法は、簡単な装置で実用上十分
な数１００λの精度で膜厚をリアルタイムで容易にモニ
ターできる点、実用上の価値の大きいものである。従つ
て、あらかじめ成長させる半導体層に対し、屈折率と赤
外線波長との関係で周期と膜厚の関係を換算しておけば
リアルタイムで膜厚モニターできることとなる。A commercially available two-color pyrometer was used as this infrared detector. This covers a temperature range of 300 to 800°C and a wavelength of 2
．． It is calculated from the infrared intensity ratio at two wavelengths, 3 μm and 1.8 μm. The temperature output of this pyrometer is shown in FIG. Before the start of growth, the temperature was almost constant at 670°C, but when the growth of GaAs started, the temperature at 1
At around 0 minutes, the temperature fluctuates because the emissivity of the surface fluctuates due to the adhesion of Ga or GaAs to the substrate heater surface. Thereafter, the temperature returned to a nearly constant level of 670°C, and when GaO7AlO,As started to grow, the temperature again fluctuated for about 10 minutes, and then the surface temperature began to change weekly as described above. After growing up,
The thickness was measured by staining the crystal cross section and observing it with SEM. Based on the relationship in equation (1) above, the thickness calculated from the frequency of the interference pattern in Figure 2 and the actual measured value were the target value. 50
It can be seen that there is a match with an error of 150A for 00 people.
In the same way, the temperature of the Ga and A2 evaporation cells was set to 1050.
When the growth temperature was changed to 1200°C, the growth rate increased due to the increase in the molecular beam intensity, and the temporal fluctuation of the interference pattern corresponding to FIG. 2 also disappeared.
As described above, the method of the present invention has great practical value in that the film thickness can be easily monitored in real time with a practically sufficient precision of several hundred λ using a simple device. Therefore, if the relationship between the period and film thickness of the semiconductor layer to be grown is converted in advance based on the relationship between the refractive index and the infrared wavelength, the film thickness can be monitored in real time.
更にこの赤外検出器の出力の変化分に応じて分子線源の
温度調節或いはシヤツタ一の開閉等を行なわしめること
も可能である。Furthermore, it is also possible to adjust the temperature of the molecular beam source, open and close the shutter, etc. in accordance with changes in the output of the infrared detector.
以上はＧａＡｓ−ＧａＡｌＡｓの場合であつたが、Ｇａ
Ａｓ−ＧａＡｓＰ，ＩｎＰ−１ｎＧａＡｓＰ，ＩｎＰＩ
ｎＧａＡｓなどのほとんどの−Ｖ族化合物半導体のヘテ
ロ構造の組合せについて、基板と成長層は波長１〜２μ
ｍで透明であり、屈折率も知られているので、本発明は
適用できる。The above was the case of GaAs-GaAlAs, but GaAs
As-GaAsP, InP-1nGaAsP, InPI
For most -V group compound semiconductor heterostructure combinations such as nGaAs, the substrate and growth layer have a wavelength of 1-2μ.
Since it is transparent at m and its refractive index is known, the present invention can be applied to it.
また、屈折率を逆に本発明の方法で膜厚から逆算するこ
とに′より、成長層の混晶比組成を求めることも可能で
ある。It is also possible to determine the mixed crystal ratio composition of the grown layer by calculating the refractive index from the film thickness using the method of the present invention.
【図面の簡単な説明】
第１図は本発明の分子線エビタキシ一装置の概要を説明
する図、第２図は成長層の表面温度を二色パイロメータ
で測定した例を示す図である。
１・・・・・・結晶基板、２・・・・・・Ｉｎ、３・・
・・・・ＭＯ板、４・・・・・・基板ホルダー、５・・
・・・・のぞき窓（サファイア）、６・・・・・・赤外
線検出器、７・・・・・・蒸発セル、８・・・・・・超
高真空容器、９・・・・・・マニビユレータ。BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a diagram illustrating the outline of the molecular beam epitaxy apparatus of the present invention, and FIG. 2 is a diagram illustrating an example of measuring the surface temperature of a growing layer with a two-color pyrometer. 1...Crystal substrate, 2...In, 3...
...MO board, 4...Substrate holder, 5...
... Peephole (sapphire), 6 ... Infrared detector, 7 ... Evaporation cell, 8 ... Ultra-high vacuum container, 9 ... manibulator.
Claims (1)
主表面上に分子線エピタキシャル法によつて該半導体基
板結晶と異なる屈折率を有する半導体層を成長させる分
子線結晶成長方法において、該半導体層表面から放射さ
れる赤外光を検出し、該半導体層の層厚の変化に伴なう
当該検出光の干渉パターンの周期を求め、該干渉パター
ンの周期を用いて該半導体層の層厚を観測しながら結晶
成長せしめることを特徴とする分子線結晶成長方法。 ２ 前記赤外光の検出は二色パイロメータに依ることを
特徴とする特許請求の範囲第１項記載の分子線結晶成長
方法。[Scope of Claims] 1. A molecular beam crystal growth method in which a semiconductor layer having a refractive index different from that of the semiconductor substrate crystal is grown by molecular beam epitaxial method on the main surface of the semiconductor substrate crystal while heating the semiconductor substrate crystal. , detects infrared light emitted from the surface of the semiconductor layer, determines the period of the interference pattern of the detected light as the thickness of the semiconductor layer changes, and uses the period of the interference pattern to detect the semiconductor layer. A molecular beam crystal growth method characterized by growing crystals while observing the layer thickness. 2. The molecular beam crystal growth method according to claim 1, wherein the detection of the infrared light is based on a two-color pyrometer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20215082A JPS5948786B2 (en) | 1982-11-19 | 1982-11-19 | Molecular beam crystal growth method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20215082A JPS5948786B2 (en) | 1982-11-19 | 1982-11-19 | Molecular beam crystal growth method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5992998A JPS5992998A (en) | 1984-05-29 |
| JPS5948786B2 true JPS5948786B2 (en) | 1984-11-28 |
Family
ID=16452788
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP20215082A Expired JPS5948786B2 (en) | 1982-11-19 | 1982-11-19 | Molecular beam crystal growth method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5948786B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS649543U (en) * | 1987-07-06 | 1989-01-19 | ||
| WO2018225205A1 (en) | 2017-06-08 | 2018-12-13 | 三井金属アクト株式会社 | Vehicle door lock device and vehicle door lock set |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6142125A (en) * | 1984-08-03 | 1986-02-28 | Rohm Co Ltd | Mbe substrate and method for measuring temperature thereof |
| JPS61122193A (en) * | 1984-11-19 | 1986-06-10 | Anelva Corp | Epitaxial growth with molecular beam |
| JPS61139021A (en) * | 1984-12-10 | 1986-06-26 | Rohm Co Ltd | Temperature measurement of mbe base board |
| JPS63502542A (en) * | 1985-08-07 | 1988-09-22 | オ−ストラリア国 | Controlling the uniformity of growing alloy thin films |
| US5091320A (en) * | 1990-06-15 | 1992-02-25 | Bell Communications Research, Inc. | Ellipsometric control of material growth |
| JP2687742B2 (en) * | 1991-02-04 | 1997-12-08 | 日亜化学工業株式会社 | Method for measuring surface state of semiconductor crystal film |
-
1982
- 1982-11-19 JP JP20215082A patent/JPS5948786B2/en not_active Expired
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS649543U (en) * | 1987-07-06 | 1989-01-19 | ||
| WO2018225205A1 (en) | 2017-06-08 | 2018-12-13 | 三井金属アクト株式会社 | Vehicle door lock device and vehicle door lock set |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5992998A (en) | 1984-05-29 |
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