JPH0550479B2 - - Google Patents
Info
- Publication number
- JPH0550479B2 JPH0550479B2 JP27800687A JP27800687A JPH0550479B2 JP H0550479 B2 JPH0550479 B2 JP H0550479B2 JP 27800687 A JP27800687 A JP 27800687A JP 27800687 A JP27800687 A JP 27800687A JP H0550479 B2 JPH0550479 B2 JP H0550479B2
- Authority
- JP
- Japan
- Prior art keywords
- molecular beam
- raw material
- chamber
- beam source
- growth
- 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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- 239000002994 raw material Substances 0.000 claims description 32
- 238000000859 sublimation Methods 0.000 claims description 18
- 230000008022 sublimation Effects 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 description 8
- 239000007789 gas Substances 0.000 description 6
- RBFQJDQYXXHULB-UHFFFAOYSA-N arsane Chemical compound [AsH3] RBFQJDQYXXHULB-UHFFFAOYSA-N 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 229910000980 Aluminium gallium arsenide Inorganic materials 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002341 toxic gas Substances 0.000 description 2
- 229910052787 antimony Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明は、薄膜結晶をエピタキシヤル成長させ
る分子線エピタキシヤル成長装置に使用するAs
分子線源に関するものである。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to an As
It concerns molecular beam sources.
［従来の技術］ 従来のAs分子線源の構成を第２図に示す。[Conventional technology] Figure 2 shows the configuration of a conventional As molecular beam source.
図示のように、ルツボ２を囲んで容器１８内に
熱シールド板１１と抵抗による原料加熱用ヒータ
３が配置され、ルツボ２の底部には熱電対１３が
取付けられ、そのリード線は容器１８の下部に設
けた熱シールド板１１の通孔を通して外側に引出
される。１４はルツボ２の開口部前方に設置され
るシヤツターで、シヤツター１４は回転軸１４′
によつて、ルツボ２の開口部を覆い、あるいは開
口部を開放するように回転することができる。 As shown in the figure, a heat shield plate 11 and a resistance heater 3 for heating the raw material are arranged in a container 18 surrounding the crucible 2. A thermocouple 13 is attached to the bottom of the crucible 2, and its lead wire is connected to the container 18. It is pulled out to the outside through a through hole in the heat shield plate 11 provided at the bottom. 14 is a shutter installed in front of the opening of the crucible 2, and the shutter 14 is connected to the rotating shaft 14'.
can be rotated to cover or open the opening of the crucible 2.
固体As原料１を入れたルツボ２は原料加熱用
ヒータ３で加熱され、ルツボ２の温度は熱電対１
３によつて測定され、As分子線のオン・オフ制
御はシヤツター１４で行われ、分子線強度はAs
原料の温度によつて制御される。 A crucible 2 containing a solid As raw material 1 is heated by a heater 3 for heating the raw material, and the temperature of the crucible 2 is controlled by a thermocouple 1.
3, the on/off control of the As molecular beam is performed by the shutter 14, and the molecular beam intensity is measured by the As molecular beam.
Controlled by the temperature of the raw material.
なお、このようなAs分子線源は従来成長室に
設置されている。 Note that such an As molecular beam source is conventionally installed in a growth chamber.
［発明が解決しようとする問題点］
ところで、上述のような構成を有するAs分子
線源には次のような問題があつた。[Problems to be Solved by the Invention] By the way, the As molecular beam source having the above-mentioned configuration has the following problems.
(1) 分子線強度を調整する際に、固体As原料の
温度が安定してAs分子線強度が一定になるま
でに長時間を要するので、As原料の温度によ
る分子線強度の調整がむつかしい。(1) When adjusting the molecular beam intensity, it takes a long time for the temperature of the solid As raw material to stabilize and the As molecular beam intensity to become constant, so it is difficult to adjust the molecular beam intensity by adjusting the temperature of the As raw material.
(2) As原料の温度を一定に保つていてもAs原料
の消費にともない分子線強度が次第に減少する
という経時変化がある。(2) Even if the temperature of the As raw material is kept constant, there is a change over time in which the molecular beam intensity gradually decreases as the As raw material is consumed.
(3) As分子線源が成長室に取り付けられている
ため、分子線源の大型化には制限があり、一度
に充填できるAs原料の量を増やすことにも限
界がある。As原料の再充填時には成長室内を
大気にさらさねばならないため、再充填後に再
び成長室内を超高真空にまで排気するのに非常
に長い時間を必要とする。(3) Since the As molecular beam source is attached to the growth chamber, there are limits to increasing the size of the molecular beam source, and there are also limits to increasing the amount of As raw material that can be filled at one time. When refilling the As raw material, the growth chamber must be exposed to the atmosphere, so it takes a very long time to evacuate the growth chamber to ultra-high vacuum again after refilling.
以上のような問題点を解決するため、これまで
は、固体As原料を用いず、アルシン（AsH3）ガ
スをAs原料として、ガスボンベから、リークバ
ルブまたはマスフローを介してガスの圧力や流量
を調整して成長室内に導入し、成長室でアルシン
ガスを高温で熱分解することによりAs分子線を
得る、ガスソースのAs分子線源が使われている。
しかし、この方法ではアルシンという毒性ガスを
使用するため作業の安全性の面で非常に大きな問
題があつた。 In order to solve the above problems, conventional methods have been to use arsine (AsH 3 ) gas as an As raw material, without using a solid As raw material, and adjust the pressure and flow rate of the gas from a gas cylinder via a leak valve or mass flow. A gas source As molecular beam source is used, which obtains As molecular beams by thermally decomposing arsine gas at high temperatures in the growth chamber.
However, this method used a toxic gas called arsine, which caused a huge problem in terms of work safety.
［発明の構成］
本発明は従来のアルシンガス使用による安全性
の面で問題を避け、固体As原料を分子線源とし
て用いるものであるが、前記(1)，(2)、(3)で示した
ような問題点を解決し、きわめて効率よく薄膜結
晶をエピタキシヤル成長させる、分子線エピタキ
シヤル成長装置に使用するAs分子線源を提供す
るものである。[Structure of the Invention] The present invention avoids the safety problems caused by the conventional use of arsine gas and uses a solid As raw material as a molecular beam source. The present invention provides an As molecular beam source for use in a molecular beam epitaxial growth apparatus that solves the above problems and allows epitaxial growth of thin film crystals with extremely high efficiency.
以下、第１図に示す実施例により本発明を説明
する。図は、本発明が適用された分子線エピタキ
シヤル成長装置を概略的に示している。 The present invention will be explained below with reference to an embodiment shown in FIG. The figure schematically shows a molecular beam epitaxial growth apparatus to which the present invention is applied.
第２図と同一部分は同一符号で示す。ルツボ２
を囲んでAs昇華室４が形成される。As昇華室４
は一方でゲートバルブ１５を介して真空排気装置
８と配管１７によつて連結され、他方で、バリア
ブル・リークバルブ５を介して成長室６と配管１
６で連結される。 The same parts as in FIG. 2 are indicated by the same reference numerals. Crucible 2
An As sublimation chamber 4 is formed surrounding it. As sublimation chamber 4
is connected via a gate valve 15 to a vacuum pump 8 and a pipe 17 on the one hand, and on the other hand is connected to a growth chamber 6 via a variable leak valve 5 to a pipe 1.
Connected by 6.
ルツボ２に対応し、As昇華室４の外側に固体
As原料加熱用ヒータ３が配置される。また、As
昇華室４より成長室６に至る配管１６およびバリ
アブル・リークバルブ５を囲んで加熱用ヒータ７
が配置される。 Corresponding to crucible 2, the solid is placed outside the As sublimation chamber 4.
A heater 3 for heating the As raw material is arranged. Also, As
A heating heater 7 surrounds the pipe 16 leading from the sublimation chamber 4 to the growth chamber 6 and the variable leak valve 5.
is placed.
なお、図において、９はホルダーに保持された
基板を示し、１０は液体窒素シユラウドを示し、
１１は加熱用ヒータ７に対する熱シールド板を示
し、ルツボ２はその底部に熱電対１３を具えてい
る。 In the figure, 9 indicates a substrate held in a holder, 10 indicates a liquid nitrogen shroud,
Reference numeral 11 indicates a heat shield plate for the heater 7, and the crucible 2 is equipped with a thermocouple 13 at its bottom.
［動作］
本As分子線源は、上記のような構造となつて
いるから、As昇華室４内の固体As原料１がAs原
料加熱用ヒータ３によつて加熱され、昇華した
As蒸気がAs昇華室４内に充満する。このAs蒸気
をバリアブル・リークバルブ５の開閉によりその
流量を制御して成長室６内へAs分子線として導
入することができる。[Operation] Since the present As molecular beam source has the above structure, the solid As raw material 1 in the As sublimation chamber 4 is heated by the As raw material heating heater 3 and sublimated.
As vapor fills the As sublimation chamber 4. This As vapor can be introduced into the growth chamber 6 as an As molecular beam by controlling its flow rate by opening and closing the variable leak valve 5.
このとき、配管１６及びバリアブル・リークバ
ルブ５を別の加熱用ヒータ７により固体As原料
１の温度よりも高温に保持することにより、前記
リークバルブ５や配管１６の内壁にAsが蒸着し
て堆積することはない。 At this time, by keeping the pipe 16 and the variable leak valve 5 at a higher temperature than the solid As raw material 1 using another heater 7, As is vapor-deposited and deposited on the inner wall of the leak valve 5 and the pipe 16. There's nothing to do.
As昇華室４に取り付けられた真空排気装置８
は、As原料１の再充填時にAs昇華室４内を超高
真空にまで真空排気するためのものであり、この
時、バリアブル・リークバルブ５は閉じられてお
り、ゲートバルブ１５の開閉により排気を行なつ
たり、やめたりすることができる。 Vacuum exhaust device 8 attached to As sublimation chamber 4
is for evacuating the As sublimation chamber 4 to an ultra-high vacuum when refilling the As raw material 1. At this time, the variable leak valve 5 is closed, and the gate valve 15 is opened and closed to evacuate the As sublimation chamber 4. You can do it or stop it.
［実施例］
本As分子線源を使用し、薄膜結晶を分子線エ
ピタキシヤル成長させた例を示す。[Example] An example will be shown in which a thin film crystal was grown by molecular beam epitaxial growth using the present As molecular beam source.
As昇華室内のPBN製ルツボに約500ｇの固体
As原料を充填し、真空排気装置でAs昇華室内を
超高真空まで排気した。その後、分子線エピタキ
シヤル成長を行なわせるため、配管及びバリアブ
ル・リークバルブを加熱用ヒータで400℃に加熱、
保持しておき、As昇華室内の真空排気をやめて、
As原料加熱用ヒータにより固体As原料の温度を
220℃まで昇温して一定温度に保持し、As昇華室
内をAsの蒸気で充満させた。次に成長室内の基
板の直前の位置に置かれたイオンゲージ（第１図
に図示していない）により測定した分子線強度
が、例えば１×10-5mbarとなるように、バリア
ブル・リークバルブを調整してAsの蒸気を成長
室内に分子線として導入した。 Approximately 500g of solid was placed in a PBN crucible in the As sublimation chamber.
Filled with As raw material, the As sublimation chamber was evacuated to an ultra-high vacuum using a vacuum evacuation device. Then, in order to perform molecular beam epitaxial growth, the piping and variable leak valve were heated to 400℃ using a heater.
Hold it, stop evacuation of the As sublimation chamber,
The temperature of the solid As raw material is controlled by the heater for heating the As raw material.
The temperature was raised to 220°C and maintained at a constant temperature, and the As sublimation chamber was filled with As vapor. Next, a variable leak valve is installed so that the molecular beam intensity measured by an ion gauge (not shown in Figure 1) placed just in front of the substrate in the growth chamber is, for example, 1 x 10 -5 mbar. The As vapor was introduced into the growth chamber as a molecular beam.
この分子線強度の調整はリークバルブの開閉の
みで行なえるため、通常のAs分子線源に比べて
極めて短時間で容易に行なうことができる。 Since the molecular beam intensity can be adjusted simply by opening and closing a leak valve, it can be easily done in an extremely short time compared to a normal As molecular beam source.
本As分子線源と、別途成長室に設置されてお
り、分子線強度の調整を行なつた通常のGa分子
線源１２、Al分子線源を用いて、650℃程度の成
長温度に加熱された（100）GaAs基板上にGaAs
やAlGaAsのエピタキシヤル薄膜結晶を連続して
何回も成長させた。 Using this As molecular beam source, a normal Ga molecular beam source 12 and an Al molecular beam source that are installed separately in the growth chamber and whose molecular beam intensity is adjusted, the growth temperature is heated to about 650℃. GaAs on (100) GaAs substrate
epitaxial thin film crystals of AlGaAs and AlGaAs were successively grown many times.
従来のAs分子線源では、その大型化が困難で
あつたため１回の固体As原料の充填により約
1μmのエピタキシヤル薄膜を100回程度しか成長
できなかつたが、本実施例のAs分子線源では連
続して約400回の成長を行なえた。さらに、固体
As原料の再充填時にも、成長室内を大気にさら
す必要はない。また、本実施例のAs分子線源で
は、固体As原料の消費にともなうAs分子線強度
の経時的変化は殆んど見られなかつた。 With conventional As molecular beam sources, it was difficult to increase the size of the source, so a single charge of solid As raw material produced approximately
Although it was possible to grow an epitaxial thin film of 1 μm only about 100 times, the As molecular beam source of this example allowed continuous growth to be performed about 400 times. Furthermore, solid
There is no need to expose the inside of the growth chamber to the atmosphere when refilling the As raw material. Furthermore, in the As molecular beam source of this example, almost no change over time in the As molecular beam intensity due to consumption of the solid As raw material was observed.
実施例ではAs原料を使用する場合について述
べたが、本発明はAsに限らず他の昇華性原料例
えばＰ、Sb、Ｓ、Se、Te等にも適用して同様の
効果が得られることは言うまでもない。 Although the example describes the case where As raw material is used, the present invention can be applied not only to As but also to other sublimable raw materials such as P, Sb, S, Se, Te, etc., and similar effects can be obtained. Needless to say.
［発明の効果］
以上説明したように、本発明ではアルシンのよ
うな毒性ガスを使用することなく、比較的取り扱
いの安全な固体As原料を用いて、分子線強度の
調整が容易で、分子線強度の経時変化が殆んどな
いAs分子線源が得られる。[Effects of the Invention] As explained above, the present invention uses a solid As raw material that is relatively safe to handle without using a toxic gas such as arsine, and the molecular beam intensity can be easily adjusted. An As molecular beam source with almost no change in intensity over time can be obtained.
また、分子線源の大型化が可能となり、一度に
多量のAs原料を充填でき、As原料の再充填の回
数を減らすことができるので、分子線エピタキシ
ヤル成長装置の稼動率を著しく向上させることが
できる。 In addition, the molecular beam source can be made larger, a large amount of As raw material can be filled at once, and the number of times the As raw material must be refilled can be reduced, so the operating rate of the molecular beam epitaxial growth apparatus can be significantly improved. I can do it.
第１図は、本発明の一実施例を断面図で示す。
第２図は、従来のAs分子線源を断面図で示す。
１……固体As原料、２……ルツボ、３……As
原料加熱用ヒータ、４……As昇華室、５……バ
リアブル・リークバルブ、６……成長室、７……
加熱用ヒータ、８……真空排気装置、９……基
板、１０……液体窒素シユラウド、１１……熱シ
ールド板、１２……従来の分子線源、１３……熱
電対、１４……シヤツター、１５……ゲートバル
ブ。
FIG. 1 shows an embodiment of the invention in cross-section.
FIG. 2 shows a conventional As molecular beam source in cross section. 1... Solid As raw material, 2... Crucible, 3... As
Heater for heating raw material, 4... As sublimation chamber, 5... Variable leak valve, 6... Growth chamber, 7...
Heating heater, 8...Evacuation device, 9...Substrate, 10...Liquid nitrogen shroud, 11...Heat shield plate, 12...Conventional molecular beam source, 13...Thermocouple, 14...Shutter, 15...Gate valve.
Claims (1)
分子線源であつて、固体As原料を収納するAs昇
華室を備え、該As昇華室を配管によりバリアブ
ル・リークバルブを介して前記成長装置の成長室
と連結するとともに、配管によりゲートバルブを
介して真空排気装置と連結し、前記昇華室及び前
記昇華室より前記成長室に至る配管、バリアブ
ル・リークバルブにそれぞれ加熱用ヒータを配置
したことを特徴とするAs分子線源。1 As used in molecular beam epitaxial growth equipment
The molecular beam source is equipped with an As sublimation chamber that stores a solid As raw material, and the As sublimation chamber is connected to the growth chamber of the growth apparatus through a variable leak valve through piping, and through a gate valve through piping. The As molecular beam source is connected to a vacuum evacuation device, and heaters are arranged in the sublimation chamber, the piping from the sublimation chamber to the growth chamber, and a variable leak valve, respectively.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27800687A JPH01119596A (en) | 1987-11-02 | 1987-11-02 | As molecular beam source |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27800687A JPH01119596A (en) | 1987-11-02 | 1987-11-02 | As molecular beam source |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01119596A JPH01119596A (en) | 1989-05-11 |
| JPH0550479B2 true JPH0550479B2 (en) | 1993-07-29 |
Family
ID=17591318
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP27800687A Granted JPH01119596A (en) | 1987-11-02 | 1987-11-02 | As molecular beam source |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01119596A (en) |
-
1987
- 1987-11-02 JP JP27800687A patent/JPH01119596A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01119596A (en) | 1989-05-11 |
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