JP2599456B2 - Ampoule vacuum sealing - Google Patents
Ampoule vacuum sealingInfo
- Publication number
- JP2599456B2 JP2599456B2 JP1048199A JP4819989A JP2599456B2 JP 2599456 B2 JP2599456 B2 JP 2599456B2 JP 1048199 A JP1048199 A JP 1048199A JP 4819989 A JP4819989 A JP 4819989A JP 2599456 B2 JP2599456 B2 JP 2599456B2
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- JP
- Japan
- Prior art keywords
- ampule
- sealing
- ampoule
- heating
- vacuum
- 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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Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、化合物半導体の結晶成長に用いる石英アン
プルなどのように内部を真空にして封じるアンプルの真
空封じ方法に関し、特に、大口径のアンプルの封じに適
したアンプルの真空封じ方法に関するものである。Description: FIELD OF THE INVENTION The present invention relates to a method for vacuum-sealing ampules, such as quartz ampules used for crystal growth of compound semiconductors, in which the inside is vacuum-sealed, and in particular, large-diameter ampules. The present invention relates to a method for vacuum sealing an ampoule suitable for sealing an ampoule.
石英封管（アンプル）を用いて、化合物半導体の結晶
を成長させる方法として、ブリッジマン法、温度勾配凝
固法、SSD法、温度差法等が知られている。As a method of growing a compound semiconductor crystal using a quartz sealed tube (ampule), a Bridgman method, a temperature gradient solidification method, an SSD method, a temperature difference method, and the like are known.
従来、これらの方法に用いられる石英アンプルのうち
で、特に、大口径（250mmφ以上）の石英アンプルを真
空封じする場合に、封じ箇所に片閉じの中子（スペー
サ）を入れて、熱融着して封じるようにしていた。Conventionally, of the quartz ampules used in these methods, especially when vacuum-sealing a quartz ampule with a large diameter (250 mmφ or more), a one-sided core (spacer) is inserted into the sealed area and heat-sealed. And sealed it.
上述した従来の真空封じ方法では、大口径の石英アン
プルを融着する際に、石英アンプル内に挿入した中子と
の融着部に熱歪が生じやすく、その石英アンプルにクラ
ックが入り、真空封じができなくなるという問題があっ
た。In the conventional vacuum sealing method described above, when a large-diameter quartz ampule is fused, thermal distortion is likely to occur at a fusion portion with a core inserted into the quartz ampule, and the quartz ampule is cracked, and a vacuum is formed. There was a problem that sealing was impossible.
また、従来は、人手により経験にたよって封じ作業を
行っていたので、封じ品質にバラツキが生ずるという問
題があった。Conventionally, the sealing operation has been manually performed based on experience, and thus there has been a problem that the sealing quality varies.
本発明の目的は、真空封じする際に、アンプルの融着
部に熱歪が発生することなく、融着品質が均一なアンプ
ルの真空封じ方法を提供することである。An object of the present invention is to provide a method for vacuum sealing an ampule having a uniform fusion quality without generating heat distortion at the fusion portion of the ampule when vacuum sealing.
第１図は、本発明によるアンプルの真空封じ方法の要
旨を説明するための図である。FIG. 1 is a view for explaining the gist of the method for vacuum sealing an ampule according to the present invention.
本発明は、アンプルの開口側にそのアンプルと同一材
料の片閉じの中子を挿入し、前記アンプルの内部を真空
にして、前記アンプルの外周に配置した複数のバーナを
正逆方向に回転させながら加熱して、前記アンプルに前
記中子を融着して封じるアンプルの真空封じ方法に適用
されるものである。According to the present invention, a single-closed core made of the same material as the ampoule is inserted into the opening side of the ampoule, the inside of the ampoule is evacuated, and a plurality of burners arranged on the outer periphery of the ampoule are rotated in forward and reverse directions. The method is applied to a method of vacuum sealing an ampule in which the core is fused to the ampule and sealed by heating.
この場合に、前記中子の肉厚は、前記アンプルの肉厚
よりも厚くすることが好ましい。中子の肉厚を厚くする
理由は、後述する各工程で加熱のしすぎ等により、アン
プルの封じ部に変形が起こることを防止するためであ
る。In this case, it is preferable that the thickness of the core is larger than the thickness of the ampoule. The reason for increasing the thickness of the core is to prevent the sealing portion of the ampule from being deformed due to excessive heating in each step described later.
本発明は、真空封じする際に、前加熱工程（101）
と、融着工程（102,103）と、後加熱工程（104）を施す
ことを特徴とするものである。The present invention provides a preheating step (101) for vacuum sealing.
And a fusion step (102, 103) and a post-heating step (104).
前加熱工程（101）は、前記アンプルの全周を低温で
加熱する工程である。The preheating step (101) is a step of heating the entire circumference of the ampule at a low temperature.
この場合、前加熱工程は、前記アンプルの封じ部全体
の温度が800℃〜1000℃となるか、または封じ部全体の
色の波長が0.68μｍ〜0.70μｍになるまで加熱すること
が好ましい。In this case, in the preheating step, it is preferable to heat the ampoule until the temperature of the entire sealing portion becomes 800 ° C. to 1000 ° C. or the color wavelength of the entire sealing portion becomes 0.68 μm to 0.70 μm.
融着工程は、前記アンプルの外周の一部を高温で加熱
して融着し外周の他の部分を低温で加熱しながら（10
2）、前記融着部分を順次移動して全周にわたり融着す
る（103）工程である。In the fusing step, a part of the outer periphery of the ampoule is heated and fused at a high temperature, and the other part of the outer periphery is heated at a low temperature (10
2), a step (103) of sequentially moving the fused portion to fuse over the entire circumference;
つまり、大口径のアンプルの外周をｎ分割した場合
に、まず1/nだけ融着し、他の部分はなまし加熱する（1
02）。融着部分をｎ回順番に移動して（103）、アンプ
ルを全周にわたって封じ切る。In other words, when the outer circumference of a large-diameter ampule is divided into n parts, first, 1 / n is fused and the other parts are annealed and heated (1).
02). The fused portion is sequentially moved n times (103), and the ampule is completely sealed.
後加熱工程（104）は、前記融着工程で前記中子が融
着したアンプルの外周を低温で加熱する工程である。The post-heating step (104) is a step of heating the outer circumference of the ampule to which the core has been fused in the fusion step at a low temperature.
本発明は、前述のように構成されているので、融着工
程で、融着部分以外の部分を低温でなまし加熱するとと
もに、融着工程の前後の前加熱工程と後加熱工程で低温
でなまし加熱するので、アンプルの融着部に熱歪を残さ
ない。Since the present invention is configured as described above, in the fusing step, portions other than the fusing part are anneal and heated at a low temperature, and the pre-heating step and the post-heating step before and after the fusing step are performed at a low temperature. Since annealing is performed, no thermal distortion is left in the fused portion of the ampoule.
以下、図面等を参照して、実施例につき、本発明を詳
細に説明する。Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings.
第２図および第３図は、本発明によるアンプルの真空
封じ方法を実施するための装置を示した図、第４図は、
本発明によるアンプルの真空封じ方法の実施例を説明す
るための図である。2 and 3 show an apparatus for carrying out the method for vacuum sealing an ampoule according to the present invention, and FIG.
It is a figure for explaining an example of a vacuum sealing method of an ampule according to the present invention.
石英アンプル１の開口側に、石英アンプル１と同じ石
英で造られた片閉じの中子２を挿入する。中子２の肉厚
は、石英アンプル１の肉厚よりも厚いものを用いて、封
じ作業中に、中子２がつぶれて変形してしまうのを防止
している。A one-sided core 2 made of the same quartz as the quartz ampule 1 is inserted into the opening side of the quartz ampule 1. The core 2 is thicker than the quartz ampule 1 to prevent the core 2 from being crushed and deformed during the sealing operation.
第２図に示すように、石英アンプル１の外周であって
中子２の挿入された部分には、後述する封じ装置３のバ
ーナ31A,31Bを配置する。石英アンプル１の開口側は、
真空装置４に接続して内部を真空にすることができ、電
離真空計５でポートの真空度を検出することができる。As shown in FIG. 2, burners 31A and 31B of a sealing device 3, which will be described later, are arranged on the outer periphery of the quartz ampule 1 where the core 2 is inserted. The opening side of the quartz ampule 1
The inside can be evacuated by connecting to the vacuum device 4, and the degree of vacuum at the port can be detected by the ionization gauge 5.
封じ装置３は、第３図に示すように、２本のバーナ31
A、31Bが対称な位置に配置されており、バーナ31Aには
ホース32A,33Aで水素ガス，酸素ガスがそれぞれ導入さ
れ、バーナ31Bにはホース32B,33Bで水素ガス，酸素ガス
がそれぞれ導入される。The sealing device 3 includes two burners 31 as shown in FIG.
A and 31B are arranged at symmetrical positions. Hydrogen gas and oxygen gas are introduced into burner 31A by hoses 32A and 33A, respectively, and hydrogen gas and oxygen gas are introduced into burner 31B by hoses 32B and 33B. You.
バーナ31A,31Bは、回転環34の切欠部にバーナ口が向
くように固定されている。この回転環34は、案内台35に
回転自在に取り付けられている。回転環34には、駆動モ
ータ36の回転が、その出力軸に設けられた歯車36aおよ
び減速歯車37を介して、伝達されており、正方向および
逆方向に180度まで、一定速度で回転できる。The burners 31A and 31B are fixed to the notches of the rotating ring so that the burner ports face. The rotating ring 34 is rotatably attached to the guide base 35. The rotation of the drive motor 36 is transmitted to the rotating ring 34 via a gear 36a and a reduction gear 37 provided on its output shaft, and can rotate at a constant speed in the forward and reverse directions up to 180 degrees. .
案内台35、駆動モータ36などは、移動台38に固定され
ており、その移動台38の車38aにより、固定部39に敷設
されたレール39a上を移動して、バーナ口を石英アンプ
ル１の封じ部に導くことができる。The guide stand 35, the drive motor 36, and the like are fixed to the movable base 38, and are moved on the rail 39a laid on the fixed part 39 by the wheel 38a of the movable base 38, and the burner opening is set to the quartz ampoule 1 It can be guided to the sealing part.
つぎに、主に第４図を参照しながら、本発明による真
空封じ方法の実施例を説明する。Next, an embodiment of the vacuum sealing method according to the present invention will be described mainly with reference to FIG.
この実施例では、石英アンプル１として、肉厚が3mm
で内径が70mmのものを用い、中子２は、石英アンプル１
の肉厚よりも厚い5mmのものを用いた。In this embodiment, the thickness of the quartz ampoule 1 is 3 mm.
The core 2 is made of quartz ampoule 1
5 mm thicker than was used.
第２図に示すように、中子２が挿入された石英アンプ
ル１を、真空装置５に取り付けて、電離真空計５で監視
しながら、石英アンプル１の内部の真空度を略１×10-7
torrにする。As shown in FIG. 2, the quartz ampule 1 into which the core 2 has been inserted is attached to a vacuum device 5 and the degree of vacuum inside the quartz ampule 1 is approximately 1 × 10 − while monitoring with an ionization vacuum gauge 5. 7
torr.
まず、第4A図に示すように、バーナ31A,31Bに水素ガ
スのみを供給して、800℃程度の炎に調節して、10分程
度なまし加熱をする。このとき、目安として、２本のバ
ーナ31A,31Bを交互に回転させ、石英アンプル１の封じ
部全体が均一に薄い赤色（温度800℃〜1000℃または波
長0.68μｍ〜0.70μｍ）を呈するまであぶり続ける。First, as shown in FIG. 4A, only hydrogen gas is supplied to the burners 31A and 31B, the flame is adjusted to about 800 ° C., and the heating is performed for about 10 minutes. At this time, as a guide, the two burners 31A and 31B are alternately rotated, and the whole sealing portion of the quartz ampule 1 is uniformly colored red (temperature 800 ° C. to 1000 ° C. or wavelength 0.68 μm to 0.70 μm). to continue.
つぎに、第4B図に示すように、片方のバーナ31Aに、
酸素ガスと水素ガスを同時に供給して、約1500℃の炎に
なるように調節し、10〜20分加熱して、石英アンプル１
の片側を融着する（図中Ａで示した部分）。このとき、
もう一方のバーナ31Bには、水素ガスのみを供給して、
約800℃の温度でなまし加熱を行う。Next, as shown in FIG. 4B, one burner 31A
Oxygen gas and hydrogen gas are supplied at the same time, adjusted to a flame of about 1500 ° C, and heated for 10 to 20 minutes.
Is fused on one side (portion indicated by A in the figure). At this time,
Only hydrogen gas is supplied to the other burner 31B,
Annealing heating is performed at a temperature of about 800 ° C.
同様に、第4C図に示すように、片方のバーナ31Bに、
酸素ガスと水素ガスを同時に供給して、約1500℃の炎に
なるように調節し、10〜20分加熱して、石英アンプル１
の別の片側を融着する（図中Ｂで示した部分）。このと
き、もう一方のバーナ31Aには、水素ガスのみを提供し
て、約800℃の温度でなまし加熱を行う。Similarly, as shown in FIG.4C, one burner 31B has
Oxygen gas and hydrogen gas are supplied at the same time, adjusted to a flame of about 1500 ° C, and heated for 10 to 20 minutes.
Is fused on another side (part indicated by B in the figure). At this time, only the hydrogen gas is supplied to the other burner 31A, and annealing is performed at a temperature of about 800 ° C.
石英アンプル１の全周にわたり融着して封じたのち、
第4D図に示すように、さらに30分間だけ、バーナ31A,31
Bに水素ガスのみを供給して、800℃程度の炎に調節して
なまし加熱をする。After fusing and sealing over the entire circumference of the quartz ampule 1,
As shown in FIG. 4D, for an additional 30 minutes, burners 31A, 31
Only hydrogen gas is supplied to B, and the temperature is adjusted to a flame of about 800 ° C. for annealing.
このようにして真空封じした石英アンプルは、融着部
に熱歪がないので、この石英アンプルを用いて、高圧下
で化合物半導体の単結晶成長を確実に行うことができ、
結晶成長の歩留りを高めることができる。また、大口径
のアンプルを用いた半導体ウェハの熱処理実験などにも
役立てることができる。Since the quartz ampule sealed in a vacuum in this manner has no thermal distortion at the fused portion, it is possible to reliably perform single crystal growth of a compound semiconductor under high pressure using this quartz ampule.
The yield of crystal growth can be increased. It can also be used for heat treatment experiments on semiconductor wafers using large-diameter ampules.
以上説明した実施例にとらわれることなく、種々の変
形ができる。Various modifications can be made without being limited to the embodiment described above.
この実施例では、回転式バーナの数は、２本設けた例
を示したが、３本以上で加熱することもできる。In this embodiment, an example is shown in which two rotary burners are provided, but heating can be performed with three or more rotary burners.
３本のバーナを用いる場合には、１つのバーナで外周
の1/3である120度だけ融着し、他の部分を２本のバーナ
でなまし加熱する。つぎに、融着する位置を、1/3ずつ
順次ずらすことにより、アンプルの全周にわたり融着し
て封じ切る。つまり、一度に融着できる距離が限られて
いるので、石英アンプルの外径が大きく外周が長くなっ
た場合には、複数のバーナで外周を区切って融着するこ
とになる。この場合には、後加熱工程は、前述の実施例
の30分よりもさらに長くしたほうがよい。In the case of using three burners, one burner is used to fuse only 120 degrees, which is 1/3 of the outer circumference, and the other part is heated with two burners. Next, the position to be fused is sequentially shifted by 1/3, so that the ampule is fused and sealed over the entire circumference of the ampule. That is, since the distance that can be fused at one time is limited, when the outer diameter of the quartz ampule is large and the outer circumference is long, the outer circumference is divided and fused by a plurality of burners. In this case, it is preferable that the post-heating step be longer than 30 minutes in the above-described embodiment.
４本のバーナを用いる場合には、対向する２本のバー
ナで融着し、他の対向する２本のバーナでなまし加熱し
て、他は実施例と同様にして封じ切ればよい。When four burners are used, fusion is performed by two opposing burners, anneal heating is performed by the other two opposing burners, and sealing is performed in the same manner as in the other embodiments.
封じるアンプルは、石英に限らず、軟化点を変化させ
たり、不純物を混入させた他のガラス管や、銅管等の金
属管等の真空封じにも、本発明を適用できる。The ampule to be sealed is not limited to quartz, and the present invention can be applied to vacuum sealing of other glass tubes having a changed softening point or mixed with impurities, or metal tubes such as copper tubes.
パイレックスガラス管の真空封じに適用する場合に
は、熱歪みが残りやすいので、加熱，なまし時間は２倍
程度行ったほうがよい。また、なまし（前加熱，後加
熱）温度は、約600℃、融着温度は800℃〜1000℃程度に
すればよい。When applied to vacuum sealing of a Pyrex glass tube, heat distortion is likely to remain, so it is better to perform heating and annealing twice or so. The annealing temperature (pre-heating, post-heating) may be about 600 ° C., and the fusing temperature may be about 800 ° C. to 1000 ° C.
小口径のアンプルの真空封じに適用する場合には、加
熱時間は大口径の場合よりも短くてよい。When applied to vacuum sealing of small diameter ampules, the heating time may be shorter than for large diameter ampules.
以上詳しく説明したように、本発明によれば、真空封
じ中の融着工程と、その前後の加熱工程を施すことによ
り、大口径のアンプルの封じ部に熱歪を残すことなく、
確実に真空封じすることができる。As described above in detail, according to the present invention, by performing a fusing step during vacuum sealing and a heating step before and after the fusing step, without leaving thermal distortion in the sealing portion of a large-diameter ampule,
Vacuum sealing can be ensured.
第１図は、本発明によるアンプルの真空封じ方法の要旨
を説明するための図である。 第２図および第３図は、本発明によるアンプルの真空封
じ方法を実施するための装置を示した図、第４図は、本
発明によるアンプルの真空封じ方法の実施例を説明する
ための図である １……石英アンプル ２……中子 ３……封じ装置 31……バーナ、32,33……ホース 34……回転環、35……案内台 36……駆動モータ、37……減速歯車 38……移動台、39……固定部 ４……真空装置 ５……電離真空計FIG. 1 is a view for explaining the gist of the method for vacuum sealing an ampule according to the present invention. 2 and 3 are views showing an apparatus for carrying out the method for vacuum-sealing an ampule according to the present invention, and FIG. 4 is a view for explaining an embodiment of the method for vacuum-sealing an ampule according to the present invention. 1 ... Quartz ampoule 2 ... Core 3 ... Sealing device 31 ... Burner, 32,33 ... Hose 34 ... Rotating ring, 35 ... Guide table 36 ... Drive motor, 37 ... Reduction gear 38… mobile table, 39… fixed part 4… vacuum device 5… ionization vacuum gauge
───────────────────────────────────────────────────── フロントページの続き (72)発明者 菊田 俊夫 神奈川県横浜市西区岡野２―４―３ 古 河電気工業株式会社横浜研究所内 (56)参考文献 特開 平２−111639（ＪＰ，Ａ) 特開 平２−80336（ＪＰ，Ａ) 特開 昭62−87479（ＪＰ，Ａ) ──────────────────────────────────────────────────続 き Continuation of the front page (72) Inventor Toshio Kikuta 2-4-3 Okano, Nishi-ku, Yokohama-shi, Kanagawa Prefecture Inside the Yokohama Laboratory, Furukawa Electric Co., Ltd. (56) References JP-A-2-111639 (JP, A) JP-A-2-80336 (JP, A) JP-A-62-87479 (JP, A)
Claims (3)
料の片閉じの中子を挿入し、前記アンプルの内部を真空
にして、前記アンプルの外周に配置した複数のバーナを
正逆方向に回転させながら加熱して、前記アンプルに前
記中子を融着して封じるアンプルの真空封じ方法であっ
て、前記アンプルの全周を低温で加熱する前加熱工程
と、前記アンプルの外周の一部を高温で加熱して融着し
外周の他の部分を低温で加熱しながら前記融着部分を順
次移動して全周にわたり融着する融着工程と、前記融着
工程で前記中子が融着したアンプルの外周を低温で加熱
する後加熱工程とから構成したアンプルの真空封じ方
法。1. An ampoule having a one-sided core made of the same material as the ampule is inserted into the opening side of the ampule, the inside of the ampule is evacuated, and a plurality of burners arranged on the outer periphery of the ampule are rotated in forward and reverse directions. A method of vacuum-sealing an ampoule that heats the core while fusing the core to the ampule and sealing the ampule, wherein a pre-heating step of heating the entire circumference of the ampule at a low temperature and a part of the outer circumference of the ampule are performed. A fusion step of heating and melting at a high temperature and sequentially moving the fusion portion while heating the other part of the outer periphery at a low temperature and fusing over the entire circumference; and the core is fused in the fusion step. A method of vacuum-sealing an ampoule, comprising a step of heating the outer periphery of the ampoule at a low temperature and a heating step.
りも厚いことを特徴とする請求項（１）記載のアンプル
の真空封じ方法。2. The method according to claim 1, wherein the thickness of the core is greater than the thickness of the ampoule.
全体の温度が800℃〜1000℃となるか、または封じ部全
体の色の波長が0.68μｍ〜0.70μｍになるまで加熱する
ことを特徴する請求項（１）記載のアンプルの真空封じ
方法。3. The preheating step comprises heating the ampoule until the temperature of the entire sealed portion is 800 ° C. to 1000 ° C. or the color wavelength of the entire sealed portion is 0.68 μm to 0.70 μm. The method for vacuum-sealing an ampule according to claim 1, characterized in that:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1048199A JP2599456B2 (en) | 1989-02-28 | 1989-02-28 | Ampoule vacuum sealing |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1048199A JP2599456B2 (en) | 1989-02-28 | 1989-02-28 | Ampoule vacuum sealing |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02229730A JPH02229730A (en) | 1990-09-12 |
| JP2599456B2 true JP2599456B2 (en) | 1997-04-09 |
Family
ID=12796714
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1048199A Expired - Lifetime JP2599456B2 (en) | 1989-02-28 | 1989-02-28 | Ampoule vacuum sealing |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2599456B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113173695B (en) * | 2020-12-07 | 2022-08-09 | 湖北新华光信息材料有限公司 | Oxyhydrogen torch seals machine |
-
1989
- 1989-02-28 JP JP1048199A patent/JP2599456B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH02229730A (en) | 1990-09-12 |
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