JPH09148257A - Raw material supply device - Google Patents
Raw material supply deviceInfo
- Publication number
- JPH09148257A JPH09148257A JP31075095A JP31075095A JPH09148257A JP H09148257 A JPH09148257 A JP H09148257A JP 31075095 A JP31075095 A JP 31075095A JP 31075095 A JP31075095 A JP 31075095A JP H09148257 A JPH09148257 A JP H09148257A
- Authority
- JP
- Japan
- Prior art keywords
- raw material
- heat
- heating
- temperature
- valve
- 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
Links
- 239000002994 raw material Substances 0.000 title claims abstract description 100
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 239000012159 carrier gas Substances 0.000 claims abstract description 17
- 239000007787 solid Substances 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 11
- 238000001947 vapour-phase growth Methods 0.000 abstract description 10
- 101100023111 Schizosaccharomyces pombe (strain 972 / ATCC 24843) mfc1 gene Proteins 0.000 abstract description 2
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 description 14
- 239000007789 gas Substances 0.000 description 13
- 239000000758 substrate Substances 0.000 description 6
- 230000005587 bubbling Effects 0.000 description 5
- 229920006395 saturated elastomer Polymers 0.000 description 5
- 238000011144 upstream manufacturing Methods 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000000927 vapour-phase epitaxy Methods 0.000 description 3
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052987 metal hydride Inorganic materials 0.000 description 2
- 150000004681 metal hydrides Chemical class 0.000 description 2
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 description 1
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- RBFQJDQYXXHULB-UHFFFAOYSA-N arsane Chemical compound [AsH3] RBFQJDQYXXHULB-UHFFFAOYSA-N 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- VOITXYVAKOUIBA-UHFFFAOYSA-N triethylaluminium Chemical compound CC[Al](CC)CC VOITXYVAKOUIBA-UHFFFAOYSA-N 0.000 description 1
- RGGPNXQUMRMPRA-UHFFFAOYSA-N triethylgallium Chemical compound CC[Ga](CC)CC RGGPNXQUMRMPRA-UHFFFAOYSA-N 0.000 description 1
- IBEFSUTVZWZJEL-UHFFFAOYSA-N trimethylindium Chemical compound C[In](C)C IBEFSUTVZWZJEL-UHFFFAOYSA-N 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Landscapes
- Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
- Chemical Vapour Deposition (AREA)
- Electrodes Of Semiconductors (AREA)
Abstract
(57)【要約】
【課題】 原料が９０℃以上の加熱を必要とする場合で
あっても使用可能とする。
【解決手段】 キャリアガスの流量を制御する流量制御
装置（ＭＦＣ）１１は、恒温槽１２外にある。ＭＦＣ１
１から送られるキャリアガスを予熱する熱交換器１３
と、液体または固体原料を充填する原料容器１４と、熱
交換器１３で予熱されたキャリアガスを直接または原料
容器１４内の原料を通して間接に成長室３０またはベン
トライン２７まで送る管路１５と、管路１５に介装した
複数のバルブ１６〜２２とは、加熱・保温手段２３で９
０℃以上に加熱および保温する。ＭＦＣ１１が恒温槽１
２外にあるので、高温加熱が必要な原料を用いる気相成
長法でもこの装置を用いることができる。
(57) [Abstract] An object of the present invention is to enable use even when a raw material requires heating at 90 ° C. or higher. A flow rate control device (MFC) 11 for controlling a flow rate of a carrier gas is provided outside a constant temperature bath 12. MFC1
Heat exchanger 13 for preheating carrier gas sent from
A raw material container 14 for filling a liquid or solid raw material, and a pipe line 15 for directly feeding the carrier gas preheated by the heat exchanger 13 or indirectly through the raw material in the raw material container 14 to the growth chamber 30 or the vent line 27, The plurality of valves 16 to 22 provided in the conduit 15 are connected to each other by the heating / heat retaining means 23.
Heat and keep warm above 0 ° C. MFC11 is a constant temperature bath 1
Since this is outside the range of 2, the apparatus can also be used in a vapor phase growth method using a raw material that requires high temperature heating.
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、原料供給装置に係
り、特に気相成長装置に用いる原料供給装置に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a raw material supply apparatus, and more particularly to a raw material supply apparatus used in a vapor phase growth apparatus.
【０００２】[0002]
【従来の技術】一般に、半導体素子の製造には、種々の
気相成長法が用いられている。その中で、例えば、砒化
ガリウム（ＧａＡｓ）や燐化インジウム（ＩｎＰ）など
の化合物半導体の製造方法である有機金属気相成長法
（ＯＭーＶＰＥ法）は、有機金属原料と水素化金属原料
とを熱分解させて基板上に薄膜結晶を成長する気相成長
法である。このような気相成長法では、原料をガスの状
態で成長室へ導入している。2. Description of the Related Art In general, various vapor phase growth methods are used for manufacturing semiconductor devices. Among them, for example, an organic metal vapor phase epitaxy method (OM-VPE method), which is a method for manufacturing a compound semiconductor such as gallium arsenide (GaAs) or indium phosphide (InP), is used as an organic metal raw material and a metal hydride raw material. Is a vapor-phase growth method in which a thin film crystal is grown on a substrate by thermal decomposition. In such a vapor phase growth method, the raw material is introduced into the growth chamber in a gas state.
【０００３】上記ＯＭーＶＰＥ法の場合、例えば砒素
（Ａｓ）や燐（Ｐ）の原料として用いるアルシン（Ａｓ
Ｈ3 ）やホスフィン（ＰＨ3 ）などの水素化金属原料
は、ガス原料であるので、そのまま輸送している。一
方、ガリウム（Ｇａ）やインジウム（Ｉｎ）の原料とし
て用いるトリエチルガリウム（（Ｃ2 Ｈ5 ）3 Ｇａ；Ｔ
ＥＧａ）やトリメチルインジウム（（ＣＨ3 ）3 Ｉｎ；
ＴＭＩｎ）などの有機金属原料は、液体または固体であ
ることから、水素ガス等のキャリアガスで輸送すること
としている。つまり、ＴＥＧａは液体であるので、水素
ガスを導入してバブリングさせてＴＥＧａを輸送してい
る。また、ＴＭＩｎは固体であるので、昇華したガスを
水素ガス等で輸送している。In the case of the OM-VPE method, for example, arsine (As) used as a raw material for arsenic (As) and phosphorus (P).
Metal hydride raw materials such as H 3 ) and phosphine (PH 3 ) are gas raw materials and are therefore transported as they are. On the other hand, triethylgallium ((C 2 H 5 ) 3 Ga; T used as a raw material for gallium (Ga) and indium (In)
EGa) and trimethylindium ((CH 3 ) 3 In;
Since an organometallic raw material such as TMIn) is liquid or solid, it is supposed to be transported by a carrier gas such as hydrogen gas. That is, since TEGa is a liquid, hydrogen gas is introduced and bubbled to transport TEGa. Since TMIn is a solid, the sublimated gas is transported by hydrogen gas or the like.
【０００４】ここに、原料の輸送量は、原料の温度で決
まる飽和蒸気圧とキャリアガスの流量で制御される。例
えば、ＴＥＧａの場合には２０℃で４．６ｍｍＨｇ、Ｔ
ＭＩｎの場合には２０℃で１．８ｍｍＨｇの飽和蒸気圧
を示し、ＴＥＧａやＴＭＩｎは、この程度の蒸気圧で十
分な量の原料を供給することができる。The transport amount of the raw material is controlled by the saturated vapor pressure determined by the temperature of the raw material and the flow rate of the carrier gas. For example, in the case of TEGa, at 20 ° C., 4.6 mmHg, T
In the case of MIn, a saturated vapor pressure of 1.8 mmHg is shown at 20 ° C., and TEGa and TMIn can supply a sufficient amount of raw material with such a vapor pressure.
【０００５】ところが、例えばＡｌ原料であるトリエチ
ルアルミニウム（（Ｃ2 Ｈ5 ）3 Ａｌ；ＴＥＡｌ）の場
合には、７０℃まで加熱しないと実用的な蒸気圧１．８
ｍｍＨｇが得られない。このように、室温以上に原料を
加熱した場合には、原料容器から成長室までの間を加熱
しないと低温部において原料が凝縮してしまう。そのた
め、従来では、恒温槽の中で原料を直接に加熱し、発生
した原料ガスを同じく恒温槽の中に設けた流量制御装置
で制御し、原料容器から成長室に至るまでの間を加熱す
るようにしている。However, for example, in the case of triethylaluminum ((C 2 H 5 ) 3 Al; TEAl) which is an Al raw material, a practical vapor pressure of 1.8 is required unless it is heated to 70 ° C.
mmHg cannot be obtained. As described above, when the raw material is heated to room temperature or higher, the raw material is condensed in the low temperature part unless the space between the raw material container and the growth chamber is heated. Therefore, conventionally, the raw material is directly heated in the constant temperature bath, and the generated raw material gas is controlled by the flow rate control device also provided in the constant temperature bath to heat the space from the raw material container to the growth chamber. I am trying.
【０００６】図２は、従来のテトラエトキシシラン
（（ＯＣ2 Ｈ5 ）4 Ｓｉ；ＴＥＯＳ）用の原料供給装置
を示す。この装置では、恒温槽１内に、ＴＥＯＳ２を充
填した原料容器３と、キャリアガスの開閉を行うバルブ
４、５と、パージガスの開閉を行うバルブ６と、ガスの
流量の制御を行う流量制御装置（ＭＦＣ）７とが設置さ
れている。そして、ＭＦＣ７から送られるガスは、図示
を省略した成長室へランバルブを介して供給される一
方、排気の場合には、ベントバルブを介して排気経路へ
送られるようになっている。ここで、ランバルブおよび
ベントバルブは、恒温槽１外にあり、成長室近傍に設け
られている。また、原料容器３から成長室に至るまでは
ＭＦＣ７を介して配管され、ランバルブおよびベントバ
ルブとともに恒温槽１外の管路も成長室に至るまで加
熱、保温する構造になっている。FIG. 2 shows a conventional raw material supply device for tetraethoxysilane ((OC 2 H 5 ) 4 Si; TEOS). In this apparatus, a raw material container 3 filled with TEOS 2 in a constant temperature bath 1, valves 4 and 5 for opening and closing a carrier gas, a valve 6 for opening and closing a purge gas, and a flow rate control device for controlling a gas flow rate. (MFC) 7 is installed. The gas sent from the MFC 7 is supplied to a growth chamber (not shown) via a run valve, while in the case of exhaust, it is sent to an exhaust path via a vent valve. Here, the run valve and the vent valve are provided outside the constant temperature bath 1 and near the growth chamber. Further, a pipe from the raw material container 3 to the growth chamber is provided through the MFC 7, and the run valve and the vent valve as well as the pipeline outside the thermostatic chamber 1 are heated and kept warm up to the growth chamber.
【０００７】このような原料供給装置を用いて気相成長
を行う場合、所定の温度で発生した飽和蒸気圧の原料ガ
スは、キャリアガスとともに、その温度を維持するよう
に恒温槽１内で加熱、保温されているＭＦＣ７で流量が
制御され、成長室へ送られる。When vapor phase growth is performed using such a raw material supply device, the raw material gas having a saturated vapor pressure generated at a predetermined temperature is heated in the constant temperature bath 1 together with the carrier gas so as to maintain the temperature. The flow rate is controlled by the MFC 7 which is kept warm and sent to the growth chamber.
【０００８】ＴＥＯＳは、２７℃で３．０ｍｍＨｇの飽
和蒸気圧を示し、８２℃では４３．５ｍｍＨｇの飽和蒸
気圧を示すが、現実には、成長速度を上げる等の関係か
ら、上記装置における原料容器３の温度は８２℃に、恒
温槽１の温度は８５℃に設定している。[0008] TEOS exhibits a saturated vapor pressure of 3.0 mmHg at 27 ° C and a saturated vapor pressure of 43.5 mmHg at 82 ° C. The temperature of the container 3 is set to 82 ° C, and the temperature of the constant temperature bath 1 is set to 85 ° C.
【０００９】[0009]
【発明が解決しようとする課題】上記従来の原料供給装
置においては、ＭＦＣ７は原料容器３よりも成長室側
（下流側）に配置されているので、ガスを所定の温度よ
り低温にさせないため、ＭＦＣ７を原料供給装置の恒温
槽１内に配置している。したがって、９０℃以上に加熱
しないと実用的な蒸気圧が得られず、十分な量の原料を
供給することができない原料を用いる場合にあっては、
ＭＦＣ７の耐熱性の点から使用できないという問題があ
った。In the above-mentioned conventional raw material supply apparatus, since the MFC 7 is arranged on the growth chamber side (downstream side) of the raw material container 3, the gas is kept at a temperature lower than a predetermined temperature. The MFC 7 is placed in the constant temperature bath 1 of the raw material supply device. Therefore, in the case of using a raw material that cannot obtain a practical vapor pressure and cannot supply a sufficient amount of raw material unless it is heated to 90 ° C. or higher,
There is a problem that it cannot be used in terms of heat resistance of MFC7.
【００１０】また、従来のように、ランバルブおよびベ
ントバルブを成長室近傍に配置すると、原料容器３から
成長室までに１０ｍ程度の配管を要する。ここで、１０
ｍの直管を加熱するのであれば、テープヒータを巻き付
ければ比較的容易に加熱することができ、温度制御も１
台の温度センサを管路に設置すればよい。しかし、実際
の装置内には多数の継ぎ手や曲げ部があり、また配管の
固定のために台座を用いる必要がある。さらに、原料供
給装置と成長室とは筐体を分けるため、隔壁を貫通する
バルクヘッドユニオンのような継ぎ手がある。このよう
に、台座や継ぎ手があると、熱容量が大きくなったり、
熱の逃げが発生する。したがって、その部分の温度を計
測してヒータにフィードバックする必要があり、場所毎
に温度センサを設置し、ヒータを分割しなければならな
い。特に、高温になるほど温度制御は困難となる。ま
た、ランバルブおよびベントバルブは、高温タイプでは
特に熱容量が大きいため、単独で加熱すると温度を安定
させることが困難である。When the run valve and the vent valve are arranged near the growth chamber as in the conventional case, a pipe of about 10 m is required from the raw material container 3 to the growth chamber. Where 10
If a straight tube of m is to be heated, it can be heated relatively easily by winding a tape heater, and the temperature control is also 1
The temperature sensor of the table may be installed in the pipeline. However, there are many joints and bends in the actual device, and it is necessary to use a pedestal for fixing the pipe. Further, since the raw material supply device and the growth chamber are separated from each other, there is a joint such as a bulkhead union penetrating the partition wall. In this way, if there is a pedestal or joint, the heat capacity will increase,
Heat escape occurs. Therefore, it is necessary to measure the temperature of that portion and feed it back to the heater, and it is necessary to install a temperature sensor at each location and divide the heater. Especially, the higher the temperature, the more difficult the temperature control becomes. Further, since the run valve and the vent valve have a particularly large heat capacity in the high temperature type, it is difficult to stabilize the temperature when heated alone.
【００１１】本発明は、かかる従来の問題点に鑑みてな
されたもので、原料が９０℃以上の加熱を必要とする場
合であっても使用可能な原料供給装置を提供することを
目的とする。The present invention has been made in view of the above conventional problems, and an object thereof is to provide a raw material supply device which can be used even when the raw material requires heating at 90 ° C. or higher. .
【００１２】特に、請求項４に係る発明は、上記目的に
加え、安定した温度制御を容易に行うことができる原料
供給装置を提供することを目的とする。In particular, in addition to the above object, it is an object of the invention according to claim 4 to provide a raw material supply device capable of easily performing stable temperature control.
【００１３】[0013]
【課題を解決するための手段】上記課題を解決するため
に、請求項１に係る発明は、キャリアガスの流量を制御
する流量制御装置と、前記流量制御装置から送られるキ
ャリアガスを予熱する熱交換器と、液体または固体原料
を充填する原料容器と、前記熱交換器で予熱されたキャ
リアガスを直接または前記原料容器内の原料を通して間
接に成長室または排気経路まで送る管路と、前記管路に
介装した複数のバルブと、前記熱交換器、前記原料容
器、前記管路および前記バルブを９０℃以上に加熱およ
び保温する加熱・保温手段とを具備して原料供給装置を
構成した。In order to solve the above-mentioned problems, the invention according to claim 1 relates to a flow rate control device for controlling the flow rate of carrier gas, and heat for preheating carrier gas sent from the flow rate control device. An exchanger, a raw material container filled with a liquid or solid raw material, a pipeline for directly feeding a carrier gas preheated in the heat exchanger or indirectly through a raw material in the raw material container to a growth chamber or an exhaust passage, and the pipe A raw material supply device was configured by including a plurality of valves provided in the passage, and a heating / warming means for heating and keeping the heat exchanger, the raw material container, the pipe and the valve at 90 ° C. or higher.
【００１４】この原料供給装置は、流量制御装置を原料
容器より上流側に設けるとともに、高温に加熱しない構
成としたので、９０℃以上の加熱を必要とする原料を用
いる気相成長法の場合であっても適用することができ
る。In this raw material supply device, the flow rate control device is provided upstream of the raw material container and is not heated to a high temperature. Therefore, in the case of the vapor phase growth method using a raw material which requires heating at 90 ° C. or higher. It can be applied even if there is.
【００１５】請求項２に係る発明は、請求項１に係る原
料供給装置において、前記加熱・保温手段はヒータ線お
よび保温材からなることを特徴とする。According to a second aspect of the present invention, in the raw material supply apparatus according to the first aspect, the heating / heat retaining means comprises a heater wire and a heat retaining material.
【００１６】ヒータ線は、熱交換器、原料容器、管路お
よびバルブに巻き付けるか、溶接して設けるとよい。The heater wire may be wound around the heat exchanger, the raw material container, the pipe line and the valve or welded.
【００１７】請求項３に係る発明は、請求項１に係る原
料供給装置において、前記加熱・保温手段はランプであ
ることを特徴とする。According to a third aspect of the present invention, in the raw material supply device according to the first aspect, the heating / heat retaining means is a lamp.
【００１８】請求項４に係る発明は、請求項１に係る原
料供給装置において、前記熱交換器、前記原料容器、前
記管路および前記バルブを恒温槽内に設置し、前記恒温
槽内に温度センサを設けるとともに、前記温度センサか
らのデータに基づき保温が一定の温度となるように加熱
・保温手段を制御する温度制御装置を具備したことを特
徴とする。According to a fourth aspect of the present invention, in the raw material supply apparatus according to the first aspect, the heat exchanger, the raw material container, the pipeline and the valve are installed in a constant temperature bath, and a temperature is set in the constant temperature bath. In addition to the provision of the sensor, a temperature control device for controlling the heating / heat-retaining means so that the heat retention is kept at a constant temperature based on the data from the temperature sensor is provided.
【００１９】この原料供給装置では、熱交換器、原料容
器、管路およびランバルブやベントバルブなどのバルブ
全体を恒温槽内に配置し、恒温槽内に温度センサを設け
て温度制御するので、安定した温度制御を容易に行うこ
とができる。In this raw material supply device, the heat exchanger, the raw material container, the pipeline, and the entire valve such as the run valve and the vent valve are arranged in the constant temperature tank, and a temperature sensor is provided in the constant temperature tank to control the temperature, so that the temperature is stable. The temperature control can be easily performed.
【００２０】[0020]
（実施形態１）図１は、本実施形態の原料供給装置１０
を示すものである。この原料供給装置１０では、キャリ
アガスの流量を制御するＭＦＣ１１は、恒温槽１２外に
配置されている。恒温槽１２内には、ＭＦＣ１１から送
られるキャリアガスを予熱する熱交換器１３と、液体ま
たは固体原料を充填する原料容器１４と、キャリアガス
や原料ガスを輸送する管路１５と、その管路１５に介装
された複数の高温用のバルブ１６、１７、１８、１９、
２０、２１、２２が配設されている。そして、これら熱
交換器１３、原料容器１４、管路１５およびバルブ１６
〜２２には、ヒータ線と保温材からなる加熱・保温部材
２３が巻き付けられている。(Embodiment 1) FIG. 1 shows a raw material supply apparatus 10 of the present embodiment.
It shows. In the raw material supply device 10, the MFC 11 that controls the flow rate of the carrier gas is arranged outside the constant temperature tank 12. In the thermostat 12, a heat exchanger 13 for preheating the carrier gas sent from the MFC 11, a raw material container 14 for filling a liquid or solid raw material, a pipeline 15 for transporting the carrier gas or the raw material gas, and the pipeline 15, a plurality of high temperature valves 16, 17, 18, 19,
20, 21, 22 are provided. Then, these heat exchanger 13, raw material container 14, pipe 15 and valve 16
A heating / heat insulating member 23 including a heater wire and a heat insulating material is wound around 22 to 22.
【００２１】この加熱・保温部材２３は、恒温槽１２外
に設けられた温度制御装置２４に接続されている。ま
た、原料容器１４の周囲の加熱・保温部材２３内には、
温度センサ２５が挿入されている。温度制御装置２４
は、温度センサ２５からのデータに基づき、保温が一定
の温度となるように加熱・保温部材２３を加熱制御する
ことができるようになっている。The heating / heat retaining member 23 is connected to a temperature control device 24 provided outside the constant temperature bath 12. In addition, in the heating / heat insulating member 23 around the raw material container 14,
The temperature sensor 25 is inserted. Temperature control device 24
On the basis of the data from the temperature sensor 25, the heating / heat insulating member 23 can be heated and controlled so that the heat is kept at a constant temperature.
【００２２】恒温槽１２内の部材配置を説明すると、Ｍ
ＦＣ１３側（上流側）に熱交換器１３が配置され、その
下流側の管路１５は分岐されている。分岐した一方の管
路１５は原料容器１４に接続され、他方の管路１５は恒
温槽１２外へ延びている。熱交換器１３と原料容器１４
との間の管路１５には、上流側から順に高温用空気駆動
のバブリングバルブ１６と原料容器１４付属の高温用手
動のバルブ１７が介装されている。一方、前記他方の管
路１５には、高温用空気駆動のバイパスバルブ１８が介
装されている。そして、原料容器１４からバイパスバル
ブ１８の下流の管路１５へ延びる管路１５には、原料容
器１４側から順に原料容器１４付属の高温用手動のバル
ブ１９と高温用空気駆動のバブリングバルブ２０が介装
されている。さらに、バイパスバルブ１８の下流の管路
１５は分岐され、分岐された一方の管路１５は恒温槽１
２外に設けた成長室３０に接続されるランライン２６と
なり、他方の管路１５は成長室３０に接続した排気管３
１に合流されるベントライン（排気経路）２７となる。The arrangement of members in the constant temperature bath 12 will be described.
The heat exchanger 13 is arranged on the FC 13 side (upstream side), and the pipeline 15 on the downstream side is branched. One of the branched pipe lines 15 is connected to the raw material container 14, and the other pipe line 15 extends to the outside of the constant temperature bath 12. Heat exchanger 13 and raw material container 14
A high temperature air-driven bubbling valve 16 and a high temperature manual valve 17 attached to the raw material container 14 are provided in this order from the upstream side in a pipe line 15 between and. On the other hand, a bypass valve 18 driven by high temperature air is provided in the other conduit 15. In the pipe line 15 extending from the raw material container 14 to the pipe line 15 downstream of the bypass valve 18, a high temperature manual valve 19 attached to the raw material container 14 and a high temperature air-driven bubbling valve 20 are sequentially provided from the raw material container 14 side. It is installed. Further, the pipe line 15 downstream of the bypass valve 18 is branched, and the branched pipe line 15 is provided in the constant temperature bath 1.
2 becomes the run line 26 connected to the growth chamber 30 provided outside, and the other conduit 15 is the exhaust pipe 3 connected to the growth chamber 30.
1 to form a vent line (exhaust path) 27.
【００２３】バイパスバルブ１８から成長室３０へ延び
る管路１５のうち、恒温槽１２内の管路１５には高温用
空気駆動のランバルブ２１が介装されている。一方、バ
イパスバルブ１８から排気管３１に合流する管路１５の
うち、恒温槽１２内の管路１５には高温用空気駆動のベ
ントバルブ２２が介装されている。Among the conduits 15 extending from the bypass valve 18 to the growth chamber 30, the high temperature air driven run valve 21 is provided in the conduit 15 in the constant temperature bath 12. On the other hand, of the conduits 15 joining the exhaust pipe 31 from the bypass valve 18, a vent valve 22 driven by high temperature air is provided in the conduit 15 in the constant temperature bath 12.
【００２４】このような構成の原料供給装置１０を用い
て、例えばＩｎＮの結晶成長を行うには、以下のように
する。In order to carry out crystal growth of, for example, InN using the raw material supply device 10 having such a structure, the following steps are performed.
【００２５】まず、成長室３０内に、ＧａＡｓ（１０
０）面基板３２を設置する。次に、固体原料である三塩
化インジウムを充填した原料容器１４付属の手動のバル
ブ１７、１９を開き、温度センサ２５で温度を計測しな
がら、熱交換器１３、原料容器１４、各バルブ１６〜２
２および管路１５、すなわち恒温槽１２内の各部材の温
度が２５０℃になるように温度制御装置２４により加熱
・保温部材２３を加熱制御する。First, in the growth chamber 30, GaAs (10
0) The plane substrate 32 is installed. Next, the manual valves 17 and 19 attached to the raw material container 14 filled with indium trichloride, which is a solid raw material, are opened, and while the temperature is measured by the temperature sensor 25, the heat exchanger 13, the raw material container 14, and each valve 16 to. Two
2 and the pipe line 15, that is, the heating and heat insulating member 23 is controlled by the temperature controller 24 so that the temperature of each member in the constant temperature bath 12 becomes 250 ° C.
【００２６】管路１５にはＭＦＣ１１で流量を制御した
窒素ガスを流す。成長前には、キャリアガスは熱交換器
１３、バイパスバルブ１８、ベントバルブ２２、ヒータ
で加熱されたベントライン２７へ流す。恒温槽１２内の
温度が２５０℃で安定したところで、バブリングバルブ
１６、２０を開き、バイパスバルブ１８を閉じて三塩化
インジウムの輸送を開始する。Nitrogen gas whose flow rate is controlled by the MFC 11 is passed through the pipe 15. Before the growth, the carrier gas is flowed to the heat exchanger 13, the bypass valve 18, the vent valve 22, and the vent line 27 heated by the heater. When the temperature inside the thermostat 12 is stabilized at 250 ° C., the bubbling valves 16 and 20 are opened and the bypass valve 18 is closed to start the transportation of indium trichloride.
【００２７】基板３２を７００℃まで加熱し、成長室３
０に接続した管路３３から２００ｓｃｃｍのアンモニア
（ＮＨ3 ）ガスを導入した後、ベントバルブ２２を閉
じ、ランバルブ２１を開いて三塩化インジウムガスをヒ
ータで２５０℃に加熱されたランライン２６に切り換
え、成長を開始する。ＭＦＣ１１で窒素ガスの流量は１
００ｓｃｃｍに制御する。The substrate 32 is heated to 700 ° C. and the growth chamber 3
After introducing 200 sccm of ammonia (NH 3 ) gas from the conduit 33 connected to 0, the vent valve 22 is closed and the run valve 21 is opened to switch the indium trichloride gas to the run line 26 heated to 250 ° C. by the heater. , Start growing. Nitrogen gas flow rate is 1 with MFC11
Control to 00 sccm.
【００２８】６０分の成長後、ランバルブ２１を閉じ、
ベントバルブ２２を開いて三塩化インジウムガスをベン
トライン２７に切り換えて成長を終了する。成長終了
後、バイパスバルブ１８を開き、バブリングバルブ１
６、２０を閉じて三塩化インジウムの輸送を終了する。
恒温槽１２の温度を室温に戻した後、原料容器１４付属
の手動のバルブ１７、１９を閉じる。After 60 minutes of growth, the run valve 21 was closed,
The vent valve 22 is opened and the indium trichloride gas is switched to the vent line 27 to complete the growth. After the growth is completed, the bypass valve 18 is opened and the bubbling valve 1
Close 6 and 20 to finish the transportation of indium trichloride.
After returning the temperature of the constant temperature bath 12 to room temperature, the manual valves 17 and 19 attached to the raw material container 14 are closed.
【００２９】このような気相成長の結果、基板３２上に
は２μｍのＩｎＮが成長していた。また、Ｘ線回折測定
の結果、立方晶のＩｎＮのピークが観測された。As a result of such vapor phase growth, 2 μm of InN was grown on the substrate 32. As a result of X-ray diffraction measurement, a cubic InN peak was observed.
【００３０】以上のように、本実施形態では、ＭＦＣ１
１を原料容器１４より上流側に設けるとともに、加熱し
ない構成としたので、９０℃以上の加熱が必要な三塩化
インジウムを原料とする気相成長法の場合であっても適
用できる。As described above, in this embodiment, the MFC1
Since No. 1 is provided on the upstream side of the raw material container 14 and is not heated, it can be applied even in the case of the vapor phase growth method using indium trichloride as a raw material, which requires heating at 90 ° C. or higher.
【００３１】特に、熱交換器１３、原料容器１４、管路
１５およびバルブ１６〜２２全体を恒温槽１２内に配置
し、恒温槽１２内に温度センサ２５を設けて温度制御す
ることとしたので、安定した温度制御を容易に行うこと
ができる。また、ランバルブ２１およびベントバルブ２
２を恒温槽１２内に設けたので、両バルブ２１、２２か
ら成長室３０までの配管長を短くすることができ、原料
の切換えを迅速に行うことができ、エピタキシャル界面
の急峻性が向上する。In particular, the heat exchanger 13, the raw material container 14, the pipe 15 and the valves 16 to 22 are all arranged in the constant temperature tank 12, and the temperature sensor 25 is provided in the constant temperature tank 12 to control the temperature. In addition, stable temperature control can be easily performed. In addition, the run valve 21 and the vent valve 2
Since 2 is provided in the constant temperature bath 12, the pipe length from both valves 21 and 22 to the growth chamber 30 can be shortened, the raw materials can be switched quickly, and the sharpness of the epitaxial interface is improved. .
【００３２】（実施形態２）上記実施形態１の原料供給
装置１０の加熱・保温部材２３の代わりに、恒温槽１２
内に赤外線ランプを設置し、温度制御装置２４で恒温槽
１２内の温度が２５０℃になるように制御した後、実施
形態１と同様に三塩化インジウムとアンモニアからＩｎ
Ｎの成長を行う。(Embodiment 2) Instead of the heating / heat-retaining member 23 of the raw material supply apparatus 10 of Embodiment 1, a constant temperature bath 12 is used.
An infrared lamp is installed in the chamber, and the temperature control device 24 controls the temperature in the constant temperature bath 12 to 250 ° C., and then indium trichloride and ammonia are used as In
Grow N.
【００３３】成長の結果、基板３２上には２μｍのＩｎ
Ｎが成長していた。また、Ｘ線回折測定の結果、立方晶
のＩｎＮのピークが観測された。As a result of the growth, 2 μm of In is deposited on the substrate 32.
N was growing. As a result of X-ray diffraction measurement, a cubic InN peak was observed.
【００３４】[0034]
【発明の効果】以上のように、本発明の原料供給装置に
よれば、流量制御装置を原料容器より上流側に設けると
ともに、高温に加熱しない構成としたので、９０℃以上
の加熱を必要とする原料を用いる気相成長法の場合であ
っても適用することができる。As described above, according to the raw material supply device of the present invention, since the flow rate control device is provided upstream of the raw material container and is not heated to a high temperature, heating at 90 ° C. or higher is required. It can be applied even in the case of the vapor phase growth method using the above raw material.
【００３５】さらに、熱交換器、原料容器、管路および
ランバルブやベントバルブなどのバルブ全体を恒温槽内
に配置し、恒温槽内に温度センサを設けて温度制御する
こととすれば、安定した温度制御を容易に行うことがで
きる。Further, if the heat exchanger, the raw material container, the pipe line, and the entire valve such as the run valve and the vent valve are arranged in a constant temperature tank and a temperature sensor is provided in the constant temperature tank to control the temperature, it is stable. The temperature can be easily controlled.
【図１】本発明の実施形態の原料供給装置を示す概略構
成図である。FIG. 1 is a schematic configuration diagram showing a raw material supply device according to an embodiment of the present invention.
【図２】従来の原料供給装置を示す概略構成図である。FIG. 2 is a schematic configuration diagram showing a conventional raw material supply device.
１０…原料供給装置、１１…流量制御装置（ＭＦＣ）、
１２…恒温槽、１３…熱交換器、１４…原料容器、１５
…管路、１６，２０…バブリングバルブ、１７，１９…
バルブ、１８…バイパスバルブ、２１…ランバルブ、２
２…ベントバルブ、２６…ランライン、２７…ベントラ
イン、３０…成長室、３１…排気管、３２…基板10 ... Raw material supply device, 11 ... Flow rate control device (MFC),
12 ... Constant temperature bath, 13 ... Heat exchanger, 14 ... Raw material container, 15
… Pipe lines, 16, 20… Bubbling valves, 17, 19…
Valve, 18 ... Bypass valve, 21 ... Run valve, 2
2 ... Vent valve, 26 ... Run line, 27 ... Vent line, 30 ... Growth chamber, 31 ... Exhaust pipe, 32 ... Substrate
Claims (4)
装置と、前記流量制御装置から送られるキャリアガスを
予熱する熱交換器と、液体または固体原料を充填する原
料容器と、前記熱交換器で予熱されたキャリアガスを直
接または前記原料容器内の原料を通して間接に成長室ま
たは排気経路まで送る管路と、前記管路に介装した複数
のバルブと、前記熱交換器、前記原料容器、前記管路お
よび前記バルブを９０℃以上に加熱および保温する加熱
・保温手段とを具備したことを特徴とする原料供給装
置。1. A flow control device for controlling the flow rate of a carrier gas, a heat exchanger for preheating a carrier gas sent from the flow control device, a raw material container for filling a liquid or solid raw material, and the heat exchanger. A conduit for sending a preheated carrier gas directly or indirectly through a raw material in the raw material container to a growth chamber or an exhaust path, a plurality of valves interposed in the pipeline, the heat exchanger, the raw material container, and the A raw material supply apparatus comprising: a pipe and a heating / heat-retaining means for heating and keeping the valve at 90 ° C. or higher.
温材からなることを特徴とする請求項１記載の原料供給
装置。2. The raw material supply apparatus according to claim 1, wherein the heating / heat retaining means comprises a heater wire and a heat retaining material.
を特徴とする請求項１記載の原料供給装置。3. The raw material supply apparatus according to claim 1, wherein the heating / heat retaining means is a lamp.
および前記バルブを恒温槽内に設置し、前記恒温槽内に
温度センサを設けるとともに、前記温度センサからのデ
ータに基づき保温が一定の温度となるように加熱・保温
手段を制御する温度制御装置を具備したことを特徴とす
る請求項１、２または３記載の原料供給装置。4. The heat exchanger, the raw material container, the conduit and the valve are installed in a constant temperature tank, a temperature sensor is provided in the constant temperature tank, and heat retention is constant based on data from the temperature sensor. 4. The raw material supply device according to claim 1, 2 or 3, further comprising a temperature control device for controlling the heating / heat-retaining means so that the temperature of the raw material supply device becomes equal to the above temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31075095A JPH09148257A (en) | 1995-11-29 | 1995-11-29 | Raw material supply device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31075095A JPH09148257A (en) | 1995-11-29 | 1995-11-29 | Raw material supply device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH09148257A true JPH09148257A (en) | 1997-06-06 |
Family
ID=18009038
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP31075095A Pending JPH09148257A (en) | 1995-11-29 | 1995-11-29 | Raw material supply device |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH09148257A (en) |
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| JPH11293465A (en) * | 1998-04-15 | 1999-10-26 | Ebara Corp | Cvd device |
| JP2003031562A (en) * | 2001-07-12 | 2003-01-31 | Tokyo Electron Ltd | Heat treatment equipment |
| JP2004134741A (en) * | 2002-06-17 | 2004-04-30 | Asm Internatl Nv | Control system for sublimation of reactant |
| WO2004066375A1 (en) * | 2003-01-23 | 2004-08-05 | Sony Corporation | Steam oxidization apparatus |
| WO2005024926A1 (en) * | 2003-09-05 | 2005-03-17 | Hitachi Kokusai Electric Inc. | Substrate treating device and method of manufacturing semiconductor device |
| JP2007088166A (en) * | 2005-09-21 | 2007-04-05 | Hitachi Kokusai Electric Inc | Substrate processing equipment |
| JP2008060536A (en) * | 2006-06-09 | 2008-03-13 | Air Products & Chemicals Inc | High flow rate GaCl3 supply |
| JP2009532579A (en) * | 2006-03-30 | 2009-09-10 | アプライド マテリアルズ インコーポレイテッド | Chemical distribution equipment for CVD or ALD |
| JP2012169674A (en) * | 2006-06-09 | 2012-09-06 | Soytec | High volume delivery system for producing gallium trichloride |
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1995
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|---|---|---|---|---|
| JPH11293465A (en) * | 1998-04-15 | 1999-10-26 | Ebara Corp | Cvd device |
| JP2003031562A (en) * | 2001-07-12 | 2003-01-31 | Tokyo Electron Ltd | Heat treatment equipment |
| JP2004134741A (en) * | 2002-06-17 | 2004-04-30 | Asm Internatl Nv | Control system for sublimation of reactant |
| US7438872B2 (en) | 2003-01-23 | 2008-10-21 | Sony Corporation | Steam oxidation apparatus |
| WO2004066375A1 (en) * | 2003-01-23 | 2004-08-05 | Sony Corporation | Steam oxidization apparatus |
| WO2005024926A1 (en) * | 2003-09-05 | 2005-03-17 | Hitachi Kokusai Electric Inc. | Substrate treating device and method of manufacturing semiconductor device |
| JP2007088166A (en) * | 2005-09-21 | 2007-04-05 | Hitachi Kokusai Electric Inc | Substrate processing equipment |
| JP2009532579A (en) * | 2006-03-30 | 2009-09-10 | アプライド マテリアルズ インコーポレイテッド | Chemical distribution equipment for CVD or ALD |
| US8951478B2 (en) | 2006-03-30 | 2015-02-10 | Applied Materials, Inc. | Ampoule with a thermally conductive coating |
| JP2008060536A (en) * | 2006-06-09 | 2008-03-13 | Air Products & Chemicals Inc | High flow rate GaCl3 supply |
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