JP2815076B2 - Molecular beam source crucible for molecular beam epitaxy - Google Patents
Molecular beam source crucible for molecular beam epitaxyInfo
- Publication number
- JP2815076B2 JP2815076B2 JP4113014A JP11301492A JP2815076B2 JP 2815076 B2 JP2815076 B2 JP 2815076B2 JP 4113014 A JP4113014 A JP 4113014A JP 11301492 A JP11301492 A JP 11301492A JP 2815076 B2 JP2815076 B2 JP 2815076B2
- Authority
- JP
- Japan
- Prior art keywords
- molecular beam
- crucible
- beam source
- melt
- mirror
- 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
Links
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- Crystals, And After-Treatments Of Crystals (AREA)
- Physical Deposition Of Substances That Are Components Of Semiconductor Devices (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は分子線エピタキシー用分
子線源るつぼ、特には融液のはい上がりが起こり難い分
子線エピタキシー用分子線源るつぼに関するものであ
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a molecular beam source crucible for molecular beam epitaxy, and more particularly to a molecular beam source crucible for molecular beam epitaxy in which a melt is unlikely to rise.
【０００２】[0002]
【従来の技術】分子線エピタキシーは数原子層レベルの
制御が可能な超格子構造を実現する薄膜製造手段として
急速に発展してきており、例えばＡl 、Ｇa 、Ａs の原
子層からなる超格子は、ある条件下で電子の移動度が通
常より数倍大きくなることから、高速トランジスタとし
ての応用が進められている。BACKGROUND OF THE INVENTION Molecular beam epitaxy has been rapidly developed as a thin film manufacturing means for realizing a superlattice structure capable of controlling several atomic layer level, for example Al, G a, superlattice consisting of atomic layer of A s Since the mobility of electrons becomes several times larger than usual under certain conditions, application as a high-speed transistor has been promoted.
【０００３】他方、この分子線エピタキシーにおいては
分子線源が不可欠とされており、これには通常クヌーセ
ンセルと呼ばれている分子線源が用いられるが、このク
ヌーセンセルは分子線源加熱ヒーター、リフレクター、
分子線源るつぼおよび熱電対からなるものとされてお
り、この分子線源るつぼとしては純度、耐熱性、強度な
どの点から通常熱分解窒化ほう素からなるものとされて
いる。On the other hand, in molecular beam epitaxy, a molecular beam source is indispensable. For this, a molecular beam source usually called a Knudsen cell is used. Reflector,
It is composed of a molecular beam source crucible and a thermocouple. The molecular beam source crucible is usually composed of pyrolytic boron nitride in terms of purity, heat resistance, strength and the like.
【０００４】[0004]
【発明が解決しようとする課題】しかし、この分子線源
るつぼとして熱分解窒化ほう素を用いた場合には、熱分
解窒化ほう素との濡れが良い金属、例えばＡl をこのる
つぼの中で溶融すると、融液がるつぼ内壁面をしみ上が
って遂にはるつぼからあふれ出る、いわゆる「融液のは
い上がり」という現象が起こり、これによってクヌーセ
ンセル内のヒーターが短絡し、装置に致命的な損害を与
える。このため、従来はこのはい上がりを防止するため
に、原料の仕込み量を減らしたり、昇温速度を落とす方
法が採られているが、これには成膜回数の減少、工程時
間の増大という不利がある。However, in the case where pyrolytic boron nitride is used as the molecular beam source crucible, a metal, such as Al, which wets well with pyrolytic boron nitride, is melted in this crucible. Then, the phenomenon that the melt soaks up on the inner wall of the crucible and eventually overflows from the crucible, so-called `` melt rising '' occurs, which short-circuits the heater in the Knudsen cell and causes fatal damage to the equipment. Giving
I can . For this reason, conventionally, in order to prevent the rising, a method of reducing the charged amount of the raw material or a method of decreasing the temperature rising rate has been adopted. There is.
【０００５】[0005]
【課題を解決するための手段】本発明はこのような不利
を解決した分子線エピタキシー用分子線源るつぼに関す
るものであり、これはるつぼの内側表面が表面粗さＲ
max ≦2 μm に鏡面仕上げされてなることを特徴とする
ものである。SUMMARY OF THE INVENTION The present invention relates to a molecular beam source crucible for molecular beam epitaxy which solves such disadvantages, and has an inner surface having a surface roughness R.
the max ≦ 2 [mu] m and is characterized in. Doing so is mirror finished.
【０００６】すなわち、本発明者らは分子線エピタキシ
ー用分子線源るつぼにおける融液のはい上がり現象を回
避する方法について種々検討した結果、分子線源るつぼ
の内側表面を鏡面仕上げすると融液のはい上がりが起こ
り難くなることを見出し、これについては例えば熱分解
窒化ほう素製のるつぼの内面表面の表面粗さＲmax を２
μｍ以下に鏡面仕上げすればＡl 融液のはい上がりが起
こり難くなることを確認して本発明を完成させた。以下
にこれをさらに詳述する。That is, the inventors of the present invention have conducted various studies on methods for avoiding the rise of the melt in the molecular beam source crucible for molecular beam epitaxy. As a result, when the inner surface of the molecular beam source crucible is mirror-finished, the melt is cooled. And found that the surface roughness R max of the inner surface of the crucible made of pyrolytic boron nitride was 2 mm.
The present invention was completed by confirming that it was difficult for the Al melt to rise when a mirror finish was applied to a thickness of less than μm. This will be described in more detail below.
【０００７】[0007]
【作用】本発明は、るつぼの内側表面を表面粗さＲ max
≦2 μm に鏡面仕上げすれば、るつぼ材質に濡れ性のよ
い融液であっても、融液がるつぼ内壁面にしみ上がるこ
とがなく、融液のはい上がりが防止できる。According to the present invention, the inner surface of the crucible is made to have a surface roughness Rmax.
If the surface is mirror-finished to ≦ 2 μm, even if the melt has good wettability to the crucible material, the melt does not soak up on the inner wall surface of the crucible, so that the melt can be prevented from rising.
【０００８】本発明による鏡面仕上げはるつぼ中で溶融
される材質にもよるが、通常は表面粗さをRmaxが≦２μ
m とすればよく、この程度に鏡面仕上げされていれば、
融液がるつぼ内壁面をしみ上がって、融液がるつぼから
あふれ出ることが防止される。[0008] by that mirror surface finishing to the present invention will depend on the material to be melted in a crucible, typically the surface roughness Rmax of ≦ 2.mu.
m, and if it is mirror finished to this extent,
The melt is prevented from seeping out of the crucible inner wall surface and overflowing from the crucible.
【０００９】この分子線源るつぼはどのような材質でも
よいが、純度、耐熱性、強度の点から熱分解窒化ほう素
で作られたものがよい。このような熱分解窒化ほう素製
るつぼは公知の方法で、アンモニアと三塩化ほう素との
混合ガスを10Torr以下の圧力下に1,900 ℃で反応させ、
この生成物をグラファイト製の型に析出させ、ついで型
から抜き取り、内面に付着しているグラファイトを空気
酸化で除去し、砥粒による研摩処理によって内側表面鏡
面仕上げすればよい。The molecular beam source crucible may be made of any material , but is preferably made of pyrolytic boron nitride in view of purity, heat resistance and strength. Such a pyrolytic boron nitride crucible is reacted by a known method at 1,900 ° C. under a pressure of 10 Torr or less with a mixed gas of ammonia and boron trichloride.
This product may be precipitated in a graphite mold, then removed from the mold, the graphite adhering to the inner surface may be removed by air oxidation, and the inner surface may be mirror-finished by polishing using abrasive grains.
【００１０】なお、このようにして作られた熱分解窒化
ほう素製るつぼは、これにヒ−タ−、ルフレクタ−、熱
電対を取りつけることで分子線エピタキシ−用分子線源
るつぼとされるが、このるつぼにAlを収納してこれを加
熱溶融しても、このものはその内側表面が鏡面仕上げさ
れているのでAlの融液はこのるつぼ内壁面にしみ上がる
ことが少なく、したがってAl融液がはい上がり、るつぼ
からあふれることはないので、これについては原料の仕
込み量を減少したり、昇温速度をおくらせるなどの手段
をとる必要はなく、したがって成膜可能回数を減少させ
たり、工程時間が増大するということがなくなるという
有利性が与えられる。The crucible made of pyrolytic boron nitride manufactured in this manner is used as a molecular beam source crucible for molecular beam epitaxy by attaching a heater, a reflector and a thermocouple to the crucible. However, even if Al is stored in this crucible and melted by heating, since this is mirror-finished on the inner surface, the Al melt hardly seeps into the inner wall of the crucible, and therefore the Al melt Since it does not rise and does not overflow from the crucible, it is not necessary to take measures such as reducing the amount of raw materials to be charged or increasing the rate of temperature rise. The advantage is provided that time is not increased.
【００１１】[0011]
【実施例】つぎに本発明の実施例をあげる。 実施例 反応炉中に直径12mm、 長さ77mmのグラファイト製の型を
２個置き、炉内を真空ポンプで排気しながら加熱して1,
900 ℃まで昇温させた。ついで、この炉内にNH3 とBCl3
とをそれぞれ４リットル／分、１リットル／分の速さで
供給し、圧力を10Torrに保持しながら20時間反応させて
厚さ0.8mm の熱分解窒化ほう素製るつぼを２個作り、こ
の熱分解窒化ほう素製るつぼをグラファイト製の型から
抜き取り、この際内面に付着していたグラファイトを70
0 ℃で３時間空気酸化処理して除去した。Next, examples of the present invention will be described. Example Two graphite molds each having a diameter of 12 mm and a length of 77 mm were placed in a reaction furnace, and the inside of the furnace was heated while being evacuated with a vacuum pump.
The temperature was raised to 900 ° C. Next, NH 3 and BCl 3
Are supplied at a rate of 4 liters / minute and 1 liter / minute, respectively, and are reacted for 20 hours while maintaining the pressure at 10 Torr to produce two 0.8 mm thick pyrolytic boron nitride crucibles. The crucible made of decomposed boron nitride was removed from the graphite mold, and the graphite adhered to the inner surface was removed at this time.
It was removed by air oxidation at 0 ° C. for 3 hours.
【００１２】また、この２個のるつぼのうちの１個につ
いてはその内側表面を＃1,200 のアルミナ砥粒を用いて
鏡面仕上げしてその表面粗さＲmax を1.3 μm のものと
したが、残りの１個は鏡面仕上げをしなかったのでその
表面粗さは4.8 μm であった。The inner surface of one of the two crucibles is mirror-finished using # 1,200 alumina abrasive grains to have a surface roughness R max of 1.3 μm. One of them did not have a mirror finish, and thus had a surface roughness of 4.8 μm.
【００１３】つぎに、この２個のるつぼにAlを0.34g 仕
込み、これに分子線エピタキシ−装置を装着し、真空ポ
ンプで10-8Torrに減圧しながら10℃／分の速さで1,300
℃まで昇温し、1,300 ℃に保持してAlがるつぼ内壁面を
しみ上って、るつぼの開日部まではい上がる時間を測定
した。Next, 0.34 g of Al was charged into the two crucibles, and a molecular beam epitaxy apparatus was mounted on the two crucibles, and the pressure was reduced to 10 -8 Torr by a vacuum pump at a rate of 10 ° C./min.
The temperature was raised to 1,300 ° C., and the temperature was kept at 1,300 ° C., and the time for Al to soak up the inner wall of the crucible and rise to the opening part of the crucible was measured.
【００１４】その結果、内側表面を鏡面処理したもので
はこの時間が22分であり、鏡面仕上げをしなかったもの
は20分であることから、鏡面仕上げしたもののほうがは
い上がりが起り難いことが確認されたし、このはい上が
りの状況も鏡面仕上げをしなかったものでは場所によっ
てはい上がりの多いところがあったが、鏡面仕上げした
ものについてはAlが水のようにしたたり落ちていくのが
観察された。As a result, this time was 22 minutes for the case where the inner surface was mirror-finished, and 20 minutes for the case where the mirror surface was not finished. Therefore, it was confirmed that the mirror-finished surface was less likely to rise. In the case of this rise, there was a lot of rise depending on the place where mirror finishing was not done, but in the case of mirror finished, it was observed that Al fell like water and dropped. Was.
【００１５】[0015]
【発明の効果】本発明によれば、るつぼ中で溶融された
融液がるつぼ内壁面をしみ上って融液がはい上ることが
抑制され、融液がるつぼからあふれ出ることがなくなる
ので、原料の仕込み量を減少したり、昇温速度を落とす
必要がなく、成膜可能回数を多くし、工程時間を少なく
することができるという有利性が得られる。According to the present invention, Ru melt which has been melted in a pot is suppressed that guests ash melt me on stains the inner wall surface of the crucible, because the melt that there is no overflowing from the crucible In addition, there is no need to reduce the amount of raw materials to be charged or to lower the rate of temperature rise, so that there is an advantage that the number of times a film can be formed is increased and the process time can be reduced.
フロントページの続き (56)参考文献 特開 平３−159989（ＪＰ，Ａ) 岡島芳彦，外３名，”ＭＢＥ用ＰＢＮ ルツボにおけるアルミニウムのはい上が り”，1991年（平成３年）秋季第52回応 用物理学会学術講演会講演予稿集Ｎｏ. ２，平成３年10月，Ｐ．488，12ｐ−Ｐ −13 (58)調査した分野(Int.Cl.6，ＤＢ名) C30B 23/08 H01L 21/203 ＣＡ（ＳＴＮ)Continuation of the front page (56) References JP-A-3-159989 (JP, A) Okajima Yoshihiko, et al., “Introduction of Aluminum in PBN Crucible for MBE”, Autumn 1991 (1991) Proceedings of the 52nd Annual Meeting of the Japan Society of Applied Physics No. 2, October 1991, 488, 12p-P-13 (58) Fields investigated (Int. Cl. 6 , DB name) C30B 23/08 H01L 21/203 CA (STN)
Claims (3)
m に鏡面仕上げされてなることを特徴とする分子線エピ
タキシー用分子線源るつぼ。1. The crucible has an inner surface with a surface roughness R max ≦ 2 μm.
mirror finish has been made this a molecular beam epitaxy for molecular beam source crucible, wherein to m.
の分子線エピタキシー用分子線源るつぼ。2. A molecular beam epitaxy for molecular beam source crucible according to 請 Motomeko 1 made of pyrolytic boron nitride.
項１または２に記載の分子線エピタキシー用分子線源る
つぼ。3. A molecular beam epitaxy for molecular beam source crucible according to claim 1 or 2 is used in the aluminum molecular beam sources.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4113014A JP2815076B2 (en) | 1992-04-06 | 1992-04-06 | Molecular beam source crucible for molecular beam epitaxy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4113014A JP2815076B2 (en) | 1992-04-06 | 1992-04-06 | Molecular beam source crucible for molecular beam epitaxy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH09100195A JPH09100195A (en) | 1997-04-15 |
| JP2815076B2 true JP2815076B2 (en) | 1998-10-27 |
Family
ID=14601278
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4113014A Expired - Lifetime JP2815076B2 (en) | 1992-04-06 | 1992-04-06 | Molecular beam source crucible for molecular beam epitaxy |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2815076B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111893458A (en) * | 2020-07-30 | 2020-11-06 | 山东国晶新材料有限公司 | Demoulding method of narrow-neck crucible |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03159989A (en) * | 1989-11-14 | 1991-07-09 | Fujitsu Ltd | Vacuum deposition apparatus |
-
1992
- 1992-04-06 JP JP4113014A patent/JP2815076B2/en not_active Expired - Lifetime
Non-Patent Citations (1)
| Title |
|---|
| 岡島芳彦，外３名，"ＭＢＥ用ＰＢＮルツボにおけるアルミニウムのはい上がり"，１９９１年（平成３年）秋季第５２回応用物理学会学術講演会講演予稿集Ｎｏ．２，平成３年１０月，Ｐ．４８８，１２ｐ−Ｐ−１３ |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111893458A (en) * | 2020-07-30 | 2020-11-06 | 山东国晶新材料有限公司 | Demoulding method of narrow-neck crucible |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH09100195A (en) | 1997-04-15 |
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