JPS637620A - Apparatus for vaporizing volatile material - Google Patents

Apparatus for vaporizing volatile material

Info

Publication number
JPS637620A
JPS637620A JP61152462A JP15246286A JPS637620A JP S637620 A JPS637620 A JP S637620A JP 61152462 A JP61152462 A JP 61152462A JP 15246286 A JP15246286 A JP 15246286A JP S637620 A JPS637620 A JP S637620A
Authority
JP
Japan
Prior art keywords
volatile substance
carrier gas
container
volatile
substance
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.)
Pending
Application number
JP61152462A
Other languages
Japanese (ja)
Inventor
Toshiya Yokogawa
俊哉 横川
Mototsugu Ogura
基次 小倉
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Panasonic Holdings Corp
Original Assignee
Matsushita Electric Industrial Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Matsushita Electric Industrial Co Ltd filed Critical Matsushita Electric Industrial Co Ltd
Priority to JP61152462A priority Critical patent/JPS637620A/en
Publication of JPS637620A publication Critical patent/JPS637620A/en
Pending legal-status Critical Current

Links

Abstract

(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。
(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

【発明の詳細な説明】 産業上の利用分野 本発明は、蒸気圧の高い液体状の揮発性物質の気化装置
に関するものである。
DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to an apparatus for vaporizing liquid volatile substances having high vapor pressure.

従来の技術 化合物半導体の気相成長(たとえば・・ライド気相エピ
タキシャル成長法や有1機金属気相成長法)。
Conventional techniques: Vapor phase growth of compound semiconductors (e.g. Ride vapor phase epitaxial growth method and organometallic vapor phase growth method).

CVD法による電極形成(たとえばモリブデン電極の形
成)等、半導体装置の結晶成長やプロセスにおいて、揮
発性物質を気化させて、それを原料として用いることが
多い。
BACKGROUND ART In crystal growth and processes for semiconductor devices, such as electrode formation by CVD (for example, formation of molybdenum electrodes), volatile substances are often vaporized and used as raw materials.

その1例として、揮発性物質である有機金属(アルキル
化物)を原料として用いる有機金属気相成長法(Met
al Organic Vapor PhaseEpi
taxy、略してMOVPE)がある。この場合−般に
、高い蒸気圧の液体である有機金属にキャリアガスを流
し込み、その蒸気を含ませて炉へ供給している。このと
きの有機金属の気化装置は、第6図に示すような構造を
している。キャリアガスはマスフローコントローラー6
 tjim シテカス流入管1に導入され、有機金属で
ある揮発性物質2の入った容器3に流入する。ガス流入
管1の先端部4は揮発性物質2の中に挿入されているの
で、流入したキャリアガスは気泡となって揮発性物質2
内を液面まで上ってくる。これをバブリングと呼んでい
る。バブリングしたキャリアガスは気化した揮発性物質
2の蒸気を含み、ガス流出管5を通って容器3がら流出
する。揮発性物質2の気化装置は、通常恒温槽等で容器
3内をある一定の温度に保つことで、揮発性物質2の蒸
気圧を設定して、キャリアガスの流量によって揮発性物
質2の気相成長に用いる供給量を制御する。そして、ガ
ス流出管5は、気相成長装置の成長反応部側のガス管に
接続されており、気化した揮発性物質はキャリアガスに
含まれて気相成長反応部に導入され、結晶が育成される
One example is metal-organic vapor phase epitaxy (Met), which uses volatile organic metals (alkylated substances) as raw materials.
al Organic Vapor PhaseEpi
There is a taxi (MOVPE for short). In this case, a carrier gas is generally poured into the organic metal, which is a liquid with a high vapor pressure, and the organic metal is supplied to the furnace with the vapor contained therein. The organometallic vaporization apparatus at this time has a structure as shown in FIG. Carrier gas is mass flow controller 6
tjim is introduced into the inflow pipe 1 and flows into a container 3 containing a volatile substance 2 which is an organometallic substance. Since the tip 4 of the gas inflow pipe 1 is inserted into the volatile substance 2, the carrier gas that has flowed in becomes bubbles and flows into the volatile substance 2.
The inside rises to the liquid level. This is called bubbling. The bubbled carrier gas contains the vapor of the vaporized volatile substance 2 and exits the container 3 through the gas outlet pipe 5. The vaporization device for the volatile substance 2 sets the vapor pressure of the volatile substance 2 by keeping the inside of the container 3 at a certain temperature in a constant temperature bath, etc., and the vaporization of the volatile substance 2 is controlled by the flow rate of the carrier gas. Control the supply amount used for phase growth. The gas outflow pipe 5 is connected to a gas pipe on the side of the growth reaction section of the vapor growth apparatus, and the vaporized volatile substances are introduced into the vapor growth reaction section while being contained in the carrier gas, and crystals are grown. be done.

発明が解決しようとする問題点 通常、揮発性物質はある一定温度に保たれ、その温度に
相当する飽和蒸気量だけバブリング時にH2等のキャリ
アガスに溶けこむ。しかしながら揮発性物質の保温は、
揮発性物質の入った容器を保温し、その熱伝導により外
部より間接的になされるだめ、揮発性物質は充分均一な
保温状態が保てない。また、キャリアガスは通常室温状
態で容器内に導入されるため、その熱により揮発性物質
は充分均一に所望の温度に保てなくなる。従って気相成
長に用いられる原料の供給量の制御が非常に困難となる
Problems to be Solved by the Invention Usually, a volatile substance is kept at a certain temperature, and during bubbling, a volatile substance dissolves into a carrier gas such as H2 by an amount of saturated vapor corresponding to that temperature. However, keeping volatile substances warm is
Unless a container containing a volatile substance is kept warm, and heat is conducted indirectly from the outside, the volatile substance cannot be kept sufficiently uniformly warm. Furthermore, since the carrier gas is normally introduced into the container at room temperature, the heat from the carrier gas makes it difficult to maintain the volatile substance at the desired temperature sufficiently uniformly. Therefore, it becomes very difficult to control the supply amount of raw materials used for vapor phase growth.

問題点を解決するだめの手段 前記問題点を解決する本発明の技術的手段は、気相成長
装置に用いられる揮発性物質を気化させる気化装置にお
いて、その液体原料を収容する容器と液体原料との接触
面積を大きくし、バブリング時にキャリアガスの気泡が
液体原料中を通過する経路を長くするため、その容器内
にその気泡に対して障害物を備えるものである。
Means for Solving the Problems The technical means of the present invention for solving the above problems is that in a vaporization device for vaporizing a volatile substance used in a vapor phase growth device, a container for accommodating the liquid raw material and a container for storing the liquid raw material, In order to increase the contact area of the carrier gas and lengthen the path through which the carrier gas bubbles pass through the liquid raw material during bubbling, the container is provided with obstacles for the bubbles.

作  用 この技術的手段による作用は次のようになる。For production The effect of this technical means is as follows.

揮発性物質をある一定温度に保つ場合、揮発性物質とそ
れを収容する容器との接触面積が大きいだめ、容器がら
揮発性物質への熱伝導も容易で、揮発性物質は非常に均
一な保温状態が保てるっまた、バブリング時にキャリア
ガスの気泡が揮発性物質中を通過する経路が長く、気泡
の揮発物質中の滞在時間が長いため、揮発性物質の温度
変動も極めて小さくなる。
When keeping a volatile substance at a certain temperature, since the contact area between the volatile substance and the container containing it is large, heat conduction from the container to the volatile substance is easy, and the volatile substance is kept at a very uniform temperature. In addition, the carrier gas bubbles have a long path through the volatile substance during bubbling, and the bubbles stay in the volatile substance for a long time, so temperature fluctuations in the volatile substance are extremely small.

実施例 以下、本発明の実施例を添付図面に基づいて説明する。Example Embodiments of the present invention will be described below with reference to the accompanying drawings.

なお本実施例では、揮発性物質としては有機金属(アル
キル化物)であり、有機金属気相成長法(MOVPE)
の原料として用いる場合について示すが、揮発性物質は
有機金属に限るものではなく、また揮発性物質を気化さ
せて用いる装置であれば、いかなる装置にこの気化装置
を接続しても良い。
In this example, the volatile substance is an organic metal (alkylated substance), and the volatile substance is an organic metal (alkylated substance), and the volatile substance is an organic metal (alkylated substance), and the volatile substance is
However, the volatile substance is not limited to organic metals, and this vaporization device may be connected to any device as long as it is a device that vaporizes and uses a volatile substance.

本発明の1実施例を第1図に示す。1はキャリアガスの
流入管である。2は揮発性物質であり、容器3に収容さ
れている。ガス流入管1の先端部4は揮発性物質2の中
に挿入されている。−方5は気化した揮発性物質を含ん
だキャリアガスが流出するガス流出管である。容器3内
はそれと同じ材質(SUS31e)の数枚の平板7が突
出しており、教室に分かれている。隣どうしの室は平板
7の端部でつながっている。そのつながり部分は、キャ
リアガスの気泡が蛇行状に揮発性物質中を通過するよう
に交互に配置されている。これにより揮発性物質2と容
器3との接触面積が大きくなり、またキャリアガスの気
泡が揮発性物質2中を蛇行しながら液面まで上っていく
ため、バブリングのパスが長くなり、気泡の揮発性物質
2中の滞在時間が長くなるので、揮発性物質2は極めて
均一で正確な保温状態が保たれる。
One embodiment of the invention is shown in FIG. 1 is a carrier gas inflow pipe. 2 is a volatile substance, which is contained in a container 3. The tip 4 of the gas inlet tube 1 is inserted into the volatile substance 2. - side 5 is a gas outflow pipe through which carrier gas containing vaporized volatile substances flows out. Inside the container 3, several flat plates 7 made of the same material (SUS31e) protrude and are divided into classrooms. Adjacent chambers are connected at the end of the flat plate 7. The connecting portions are arranged alternately so that carrier gas bubbles pass through the volatile substance in a meandering manner. This increases the contact area between the volatile substance 2 and the container 3, and since the carrier gas bubbles meander through the volatile substance 2 and rise to the liquid level, the bubbling path becomes longer and the bubbles Since the residence time in the volatile substance 2 is increased, the volatile substance 2 is maintained in an extremely uniform and accurate heat-retaining state.

以上のような構造をもつ揮発性物質の気化装置の使用例
を第2図に示す。揮発性物質は有機金属のトリエチルイ
ンジウム41 (TEI 、 (C2H5)3In )
およびトリエチルガリウム42 (TEG、 (02H
5)3Ga )であり、InGaAsPのMOVPE成
長の原料として用いられる場合を示す。第1図に示した
本発明の一実施例の揮発性物質の気化装置は、43およ
び44の部分に接続されている。キャリアガスである水
素(H2)はマスフロー46および46でそれぞれ35
0CC/ mi nおよび80CC/minに制仰され
てそれぞれの気化装置のガス流入管1を通じてTE I
 41およびTEG42へ流れ込み、バブリングして気
化させる。気化したTEIおよびTEGを含んだ水素は
それぞれのガス流出管5を通じてMOVPE成長炉47
へ供給される。−方、PおよびAsの原料としては水素
で5チに希釈したホスフィン48(PH3)およびアル
シン49 (AsH3)が用いられ、それぞれマスフロ
ー5oおよび61で170ル/ m i nおよび10
0ル/ m i nに流量制御されたのち、成長炉47
へ供給される。成長炉47では基板52を670℃に加
熱し、供給された原料の熱分解反応によって基板52上
にInGaAsP四元混晶がエピタキシャル成長する。
FIG. 2 shows an example of the use of a volatile substance vaporization device having the above-described structure. The volatile substance is the organometallic triethylindium-41 (TEI, (C2H5)3In).
and triethyl gallium 42 (TEG, (02H
5) 3Ga) and is used as a raw material for MOVPE growth of InGaAsP. A volatile substance vaporization device according to an embodiment of the present invention shown in FIG. 1 is connected to sections 43 and 44. Hydrogen (H2), which is a carrier gas, has mass flows of 35 and 46, respectively.
TE I through the gas inlet pipe 1 of each vaporizer, controlled at 0 CC/min and 80 CC/min.
41 and TEG 42, and is bubbled and vaporized. Hydrogen containing vaporized TEI and TEG is passed through each gas outlet pipe 5 to the MOVPE growth reactor 47.
supplied to - On the other hand, as raw materials for P and As, phosphine 48 (PH3) and arsine 49 (AsH3) diluted to 50% with hydrogen were used, with mass flows of 50 and 61, respectively, of 170 l/min and 10
After the flow rate was controlled to 0 l/min, the growth furnace 47
supplied to In the growth furnace 47, the substrate 52 is heated to 670° C., and an InGaAsP quaternary mixed crystal is epitaxially grown on the substrate 52 by a thermal decomposition reaction of the supplied raw material.

この手段により成長を連続して多数回行なっても、組成
の変動および膜厚の変動は極めて少なかった。
Even if the growth was performed many times in succession by this method, the fluctuations in composition and film thickness were extremely small.

成長毎にサセプターを交換し40回のrunの組成のバ
ラツキおよび膜厚のバラツキ(成長時間1時間)はそれ
ぞれ、x=0.27±0.03 、7=O,チ0.■お
よび1μm±0.02と極めて制御性良く良好な四元混
晶が得られた。
The compositional variations and film thickness variations (growth time: 1 hour) of 40 runs in which the susceptor was replaced after each growth were x=0.27±0.03, 7=O, and chi0. A good quaternary mixed crystal with extremely good controllability of (1) and 1 μm±0.02 was obtained.

尚、本発明の平板7はバブリングの気泡が揮発性物質2
の液面まで上がりやすいように上方にある程度の傾きを
有するものであってもよい。本実施例を第3図に示す。
In addition, in the flat plate 7 of the present invention, the bubbling air bubbles are volatile substances 2.
It may have a certain degree of inclination upward so that it can easily rise to the liquid level. This embodiment is shown in FIG.

第1図と同一構成部には第1図と同じ番号を記す。Components that are the same as those in FIG. 1 are given the same numbers as in FIG. 1.

また、揮発性物質2のバブリングのパスが、ら線状とな
るよう、気泡に対する障害物として容器内部が、ら線状
となっていてもよい。本実施例は第4図に示す。
Further, the inside of the container may be formed in a linear shape as an obstacle to the bubbles so that the bubbling path of the volatile substance 2 is linear. This embodiment is shown in FIG.

さらに、気泡に対する障害物としてメツシュを用いても
よい。本実施例は第5図に示す。図中9はメツシュであ
る。
Furthermore, a mesh may be used as an obstacle to air bubbles. This embodiment is shown in FIG. 9 in the figure is a mesh.

発明の効果 以上のように本発明によれば、気化装置内に収容される
揮発性物質が極めて均一な保温状態に保たれ、温度変動
もないため、揮発性物質の気化量の制御が非常に正確と
なり、極めて有用である。
Effects of the Invention As described above, according to the present invention, the volatile substances contained in the vaporizer are kept in an extremely uniform temperature state, and there is no temperature fluctuation, so the amount of vaporized volatile substances can be controlled very easily. It is accurate and extremely useful.

【図面の簡単な説明】[Brief explanation of drawings]

第1図は本発明の一実施例の揮発性物質の気化装置の概
略構成図、第2図は本実施例装置の一使用例としての気
相成長装置の概略ガス系統図、第3図、第4図および第
6図は本発明の他の実施例の揮発性物質の気化装置の概
略構成図、第6図は従来の揮発性物質の気化装置の概略
構成図である。 1・・・・・・ガス流入管、2・・・・・・揮発性物質
、3・・・・・・容器、4・・・・・・先端部、5・・
・・・・ガス流出管、7・・・・・・平板。 代理人の氏名 弁理士 中 尾 敏 男 ほか1名”−
Tl儀入゛菅 2−°1赴+1物′W 5“゛1スフ0−]ンLll−ラー 7−°乎社 第3図 第4図 計−°5線イ脣阜g7り 第5図 9−−−メ1.ンエ
FIG. 1 is a schematic configuration diagram of a volatile substance vaporization apparatus according to an embodiment of the present invention, FIG. 2 is a schematic gas system diagram of a vapor phase growth apparatus as an example of the use of this embodiment apparatus, and FIG. 4 and 6 are schematic diagrams of a volatile substance vaporization apparatus according to other embodiments of the present invention, and FIG. 6 is a schematic diagram of a conventional volatile substance vaporization apparatus. 1... Gas inflow pipe, 2... Volatile substance, 3... Container, 4... Tip, 5...
...Gas outflow pipe, 7...Flat plate. Name of agent: Patent attorney Toshio Nakao and one other person”−
Tl entry゛kan 2-°1 go + 1 thing'W 5"゛1 suf 0-]nLll-ra 7-°乎sha Fig. 3 Fig. 4 Total -° 5 line Ig 脣 阜 g7 Fig. 5 9---Me 1.

Claims (4)

【特許請求の範囲】[Claims] (1)揮発性物質を収容する容器内に、前記揮発性物質
中を通過するキャリアガスの気泡に対する障害物を設け
てなる揮発性物質の気化装置。
(1) A device for vaporizing a volatile substance, in which a container containing the volatile substance is provided with an obstacle for carrier gas bubbles passing through the volatile substance.
(2)バブリング時、キャリアガスの気泡が蛇行状に揮
発性物質中を通過するように、障害物が平板状であり、
交互に複数枚、容器内壁より突出して櫛状に配置されて
いる特許請求の範囲第1項記載の揮発性物質の気化装置
(2) During bubbling, the obstruction is flat so that carrier gas bubbles pass through the volatile substance in a meandering manner;
2. The device for vaporizing a volatile substance according to claim 1, wherein a plurality of the vaporizers are arranged in a comb shape so as to protrude from the inner wall of the container.
(3)バブリング時、キャリアガスの気泡がら線状に揮
発性物質中を通過するように、障害物として容器内が、
ら線状である特許請求の範囲第1項記載の揮発性物質の
気化装置。
(3) During bubbling, the inside of the container acts as an obstacle so that carrier gas bubbles pass linearly through the volatile substance.
The device for vaporizing a volatile substance according to claim 1, which has a spiral shape.
(4)障害物がメッシュである特許請求の範囲第1項記
載の揮発性物質の気化装置。
(4) The volatile substance vaporization device according to claim 1, wherein the obstruction is a mesh.
JP61152462A 1986-06-27 1986-06-27 Apparatus for vaporizing volatile material Pending JPS637620A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP61152462A JPS637620A (en) 1986-06-27 1986-06-27 Apparatus for vaporizing volatile material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP61152462A JPS637620A (en) 1986-06-27 1986-06-27 Apparatus for vaporizing volatile material

Publications (1)

Publication Number Publication Date
JPS637620A true JPS637620A (en) 1988-01-13

Family

ID=15541042

Family Applications (1)

Application Number Title Priority Date Filing Date
JP61152462A Pending JPS637620A (en) 1986-06-27 1986-06-27 Apparatus for vaporizing volatile material

Country Status (1)

Country Link
JP (1) JPS637620A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007134247A (en) * 2005-11-11 2007-05-31 Sanyo Electric Co Ltd Fuel cell device
JP2011509351A (en) * 2008-01-10 2011-03-24 レール・リキード−ソシエテ・アノニム・プール・レテュード・エ・レクスプロワタシオン・デ・プロセデ・ジョルジュ・クロード Solid precursor sublimator
JP2013095663A (en) * 2011-11-03 2013-05-20 Young Green Energy Co Hydrogen generation apparatus
US20140041590A1 (en) * 2012-08-10 2014-02-13 Samsung Display Co., Ltd. Canister

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007134247A (en) * 2005-11-11 2007-05-31 Sanyo Electric Co Ltd Fuel cell device
JP2011509351A (en) * 2008-01-10 2011-03-24 レール・リキード−ソシエテ・アノニム・プール・レテュード・エ・レクスプロワタシオン・デ・プロセデ・ジョルジュ・クロード Solid precursor sublimator
JP2013095663A (en) * 2011-11-03 2013-05-20 Young Green Energy Co Hydrogen generation apparatus
US9061908B2 (en) 2011-11-03 2015-06-23 Young Green Energy Co. Hydrogen-generating device
US20140041590A1 (en) * 2012-08-10 2014-02-13 Samsung Display Co., Ltd. Canister
KR20140020678A (en) * 2012-08-10 2014-02-19 삼성디스플레이 주식회사 Canister, vapor deposition apparatus having the same, method for forming thin film using the same and method for manufacturing organic light emitting display apparatus
US9057125B2 (en) * 2012-08-10 2015-06-16 Samsung Display Co., Ltd. Canister

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