JP4419526B2 - Evaluation method of vaporizer performance - Google Patents

Evaluation method of vaporizer performance Download PDF

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JP4419526B2
JP4419526B2 JP2003378822A JP2003378822A JP4419526B2 JP 4419526 B2 JP4419526 B2 JP 4419526B2 JP 2003378822 A JP2003378822 A JP 2003378822A JP 2003378822 A JP2003378822 A JP 2003378822A JP 4419526 B2 JP4419526 B2 JP 4419526B2
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vaporization
liquid
vaporizer
temperature
liquid material
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尚規 吉岡
達司 川本
満志 川尾
繁 松野
朗 山田
章二 宮下
英興 内川
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Shimadzu Corp
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本発明は、液体有機金属や有機金属溶液等の液体材料を気化する気化器の気化性能評価方法に関する。 The present invention relates to a method for evaluating the vaporization performance of a vaporizer that vaporizes a liquid material such as a liquid organic metal or an organic metal solution .

半導体デバイス製造工程における薄膜形成方法の一つとしてＭＯＣＶＤ（Metal Organic Chemical Vapor Deposition）法があるが、スパッタ等に比べて膜質，成膜速度，ステップカバレッジなどが優れていることから近年盛んに利用されている。ＭＯＣＶＤ装置に用いられているＣＶＤガス供給法としてはバブリング法や昇華法などがあるが、液体有機金属若しくは有機金属を有機溶剤に溶かした液体材料をＣＶＤリアクタ直前で気化して供給する方法が、制御性および安定性の面でより優れた方法として注目されている。この気化方法では、高温に保たれた気化チャンバ内にノズルから液体材料を噴霧して、液体材料を気化させている（例えば、特許文献１参照）。   MOCVD (Metal Organic Chemical Vapor Deposition) method is one of the thin film forming methods in the semiconductor device manufacturing process, but it has been actively used in recent years because of its superior film quality, deposition rate, step coverage, etc. compared to sputtering. ing. The CVD gas supply method used in the MOCVD apparatus includes a bubbling method and a sublimation method, but a method of vaporizing and supplying a liquid material in which a liquid organic metal or an organic metal is dissolved in an organic solvent is supplied immediately before the CVD reactor. It attracts attention as a better method in terms of controllability and stability. In this vaporization method, a liquid material is sprayed from a nozzle into a vaporization chamber maintained at a high temperature to vaporize the liquid material (see, for example, Patent Document 1).

特開平１０−２５１８５３号公報Japanese Patent Laid-Open No. 10-251853

しかしながら、気化の際に液体材料に充分な熱エネルギーを与えることができないと、未気化残渣が発生して配管に詰まりが発生したり、残渣がパーティクルとなってＣＶＤリアクタまで達して成膜不良の原因となるおそれがあった。さらに、複数の成分を混合してから気化する場合、成分によって気化温度や熱分解温度特性が異なり、一部の成分が未気化または熱分解することによる残渣が発生しやすかった。そして、未気化残渣の発生を抑えた効率的な気化を実現するためには、種々の気化条件に対して気化性能を評価する必要があるが、材料特性などから評価が非常に難しく、確立された評価方法が無いというのが現状であった。 However, if sufficient thermal energy cannot be given to the liquid material during vaporization, unvaporized residue is generated and the piping is clogged, or the residue becomes particles and reaches the CVD reactor, resulting in poor film formation. There was a risk of this. Furthermore, when vaporizing after mixing a plurality of components, the vaporization temperature and thermal decomposition temperature characteristics differ depending on the components, and a residue is likely to be generated due to unvaporization or thermal decomposition of some components. In order to achieve efficient vaporization with reduced generation of unvaporized residues, it is necessary to evaluate the vaporization performance under various vaporization conditions. The current situation is that there is no evaluation method.

本発明は、高温に保持された気化チャンバ内に液体有機金属若しくは有機金属溶液から成る液体材料を噴霧して気化する気化器の気化性能評価方法であって、所定量の液体材料を気化チャンバ内に噴霧して気化させた後に、気化チャンバ内の未気化付着物を有機溶剤で除去し、その除去に用いた有機溶剤中の液体材料の含有量を計測し、計測された含有量に基づいて気化性能を評価することを特徴とする。 The present invention relates to a method for evaluating the vaporization performance of a vaporizer in which a liquid material composed of a liquid organic metal or an organic metal solution is sprayed into a vaporization chamber held at a high temperature. After being vaporized by spraying, the unvaporized deposits in the vaporization chamber are removed with an organic solvent, and the content of the liquid material in the organic solvent used for the removal is measured. Based on the measured content It is characterized by evaluating the vaporization performance .

本発明によれば、気化チャンバに実際に付着した未気化付着物を有機溶剤で除去して、その有機溶剤中に含まれる液体材料を計測して定量分析しているので、気化器の気化性能を確実に評価することができる。 According to the present invention, the non-vaporized deposit actually attached to the vaporization chamber is removed with an organic solvent, and the liquid material contained in the organic solvent is measured and quantitatively analyzed. Can be reliably evaluated.

以下、図を参照して本発明を実施するための最良の形態を説明する。
図１は気化装置全体の概略構成を示す図である。１は気化器２に液体有機金属や有機金属溶液等（以下では、これらを液体材料と呼ぶ）を供給する液体材料供給装置であり、供給された液体材料は気化器２で気化されてＣＶＤ装置に設けられたＣＶＤリアクタに供給される。例えば、液体有機金属としてはＣｕやＴａなどの有機金属があり、有機金属溶液としてはＢａ，Ｓｒ，Ｔｉ，Ｐｂ，Ｚｒなどの有機金属を有機溶剤に溶かしたもがある。 Hereinafter, the best mode for carrying out the present invention will be described with reference to the drawings .
FIG. 1 is a diagram showing a schematic configuration of the entire vaporizer. Reference numeral 1 denotes a liquid material supply device for supplying a liquid organic metal, an organic metal solution or the like (hereinafter referred to as a liquid material) to the vaporizer 2, and the supplied liquid material is vaporized by the vaporizer 2 to be a CVD apparatus. Is supplied to a CVD reactor provided in For example, liquid organic metals include organic metals such as Cu and Ta, and organic metal solutions include organic metals such as Ba, Sr, Ti, Pb, and Zr dissolved in an organic solvent.

液体材料供給装置１に設けられた材料容器３Ａ，３Ｂ，３Ｃには、ＭＯＣＶＤに用いられる液体材料４Ａ，４Ｂ，４Ｃが充填されている。例えば、ＢＳＴ膜（BaSrTi酸化膜）を成膜する場合には、原料であるＢａ、Ｓｒ、Ｔｉを有機溶剤ＴＨＦ（tetrahydrofuran）で溶解したものが液体材料４Ａ，４Ｂ，４Ｃとして用いられる。また、溶剤容器３ＤにはＴＨＦが溶剤４Ｄとして充填されている。なお、容器３Ａ〜３Ｄは原料の数に応じて設けられ、必ずしも４個とは限らない。   The material containers 3A, 3B, 3C provided in the liquid material supply apparatus 1 are filled with liquid materials 4A, 4B, 4C used for MOCVD. For example, in the case of forming a BST film (BaSrTi oxide film), the raw materials Ba, Sr, and Ti dissolved in an organic solvent THF (tetrahydrofuran) are used as the liquid materials 4A, 4B, and 4C. The solvent container 3D is filled with THF as the solvent 4D. The containers 3A to 3D are provided according to the number of raw materials, and are not necessarily four.

各容器３Ａ〜３Ｄには、チャージガスライン５と移送ライン６Ａ〜６Ｄとが接続されている。各容器３Ａ〜３Ｄ内にチャージガスライン５を介してチャージガスが供給されると、各容器３Ａ〜３Ｄに充填されている液体材料４Ａ〜４Ｃおよび溶剤４Ｄの液面にガス圧が加わり、液体材料４Ａ〜４Ｃおよび溶剤４Ｄが各移送ライン６Ａ〜６Ｄへとそれぞれ押し出される。移送ライン６Ａ〜６Ｄに押し出された各液体材料４Ａ〜４Ｃおよび溶剤４Ｄは、ガス圧によってさらに移送ライン６Ｅへと移送され、この移送ライン６Ｅ内で混合状態となる。   A charge gas line 5 and transfer lines 6A to 6D are connected to the containers 3A to 3D. When charge gas is supplied into the containers 3A to 3D via the charge gas line 5, gas pressure is applied to the liquid surfaces of the liquid materials 4A to 4C and the solvent 4D filled in the containers 3A to 3D, and the liquids Materials 4A-4C and solvent 4D are extruded into transfer lines 6A-6D, respectively. The liquid materials 4A to 4C and the solvent 4D pushed out to the transfer lines 6A to 6D are further transferred to the transfer line 6E by the gas pressure, and are mixed in the transfer line 6E.

移送ライン６Ｅにはキャリアガスライン７からキャリアガスが供給されるようになっており、キャリアガス、液体材料４Ａ〜４Ｃおよび溶剤４Ｄは気液２相流状態となって気化器２へと供給される。気化器２にはキャリアガスライン７を介してキャリアガスが供給されており、気化された材料はキャリアガスによってＣＶＤリアクタへと送られる。   Carrier gas is supplied to the transfer line 6E from the carrier gas line 7, and the carrier gas, the liquid materials 4A to 4C and the solvent 4D are supplied to the vaporizer 2 in a gas-liquid two-phase flow state. The The vaporizer 2 is supplied with a carrier gas via a carrier gas line 7, and the vaporized material is sent to the CVD reactor by the carrier gas.

なお、チャージガスおよびキャリアガスには窒素ガスやアルゴンガス等の不活性ガスが用いられる。また、移送ライン６Ａ〜６Ｅにおける液体材料４Ａ〜４Ｃや溶剤４Ｄの滞留量はできるだけ低減するのが好ましく、本実施の形態では、移送ライン６Ａ〜６Ｃには１／８インチの配管を用いている。   Note that an inert gas such as nitrogen gas or argon gas is used for the charge gas and the carrier gas. Moreover, it is preferable to reduce the retention amount of the liquid materials 4A to 4C and the solvent 4D in the transfer lines 6A to 6E as much as possible. In this embodiment, 1/8 inch piping is used for the transfer lines 6A to 6C. .

各移送ライン６Ａ〜６Ｄには、マスフローメータ８Ａ〜８Ｄおよび遮断機能付き流量制御バルブ９Ａ〜９Ｄが設けられている。マスフローメータ８Ａ〜８Ｄで液体材料４Ａ〜４Ｃおよび溶剤４Ｄの流量を各々監視しつつ流量制御バルブ９Ａ〜９Ｄを制御して、液体材料４Ａ〜４Ｃおよび溶剤４Ｄの流量が適切となるようにしている。なお、移送ライン６Ｅの気化器直前にミキサを設けて、液体材料４Ａ〜４Ｃの混合状態をより向上させるようにしても良い。さらに、各液体材料４Ａ〜４Ｃの流量を制御する流量制御バルブ９Ａ〜９Ｄに代えて、プランジャポンプ等のポンプを用いて流量制御するようにしても良い。   Each transfer line 6A to 6D is provided with mass flow meters 8A to 8D and flow control valves 9A to 9D with a shut-off function. The flow rate control valves 9A to 9D are controlled while monitoring the flow rates of the liquid materials 4A to 4C and the solvent 4D with the mass flow meters 8A to 8D, respectively, so that the flow rates of the liquid materials 4A to 4C and the solvent 4D are appropriate. . Note that a mixer may be provided immediately before the vaporizer in the transfer line 6E to further improve the mixing state of the liquid materials 4A to 4C. Furthermore, instead of the flow rate control valves 9A to 9D for controlling the flow rates of the liquid materials 4A to 4C, the flow rate may be controlled using a pump such as a plunger pump.

図２〜図４は気化器２の詳細を示す図であり、図２は気化器２を正面から見た断面図、図３は図２のＡ−Ａ’断面図、図４は図２のＢ部の拡大図である。図２に示すように、気化器２は液体材料４Ａ〜４Ｃを霧化する霧化部２０と、霧化部２０で霧化された液体材料４Ａ〜４Ｃをさらに気化する気化チャンバ２１とを備えている。気化チャンバ２１のチャンバ本体２１ａには、水平方向（図示左右方向）に延在する円筒空洞２２が形成されている。霧化部２０は、円筒空洞２２に対して鉛直下方向に霧化ガスを吹き出すように取り付けられている。フランジ２１ｂはチャンバ本体２１ａに対して着脱可能であって、例えば、チャンバ内をクリーニングするような場合には、フランジ２１ｂを外して円筒空洞２２を大気開放して洗浄を行う。   2 to 4 are views showing details of the vaporizer 2, FIG. 2 is a cross-sectional view of the vaporizer 2 seen from the front, FIG. 3 is a cross-sectional view taken along line AA 'of FIG. 2, and FIG. It is an enlarged view of the B section. As shown in FIG. 2, the vaporizer 2 includes an atomization unit 20 that atomizes the liquid materials 4A to 4C and a vaporization chamber 21 that further vaporizes the liquid materials 4A to 4C atomized by the atomization unit 20. ing. A cylindrical cavity 22 extending in the horizontal direction (left-right direction in the figure) is formed in the chamber body 21a of the vaporization chamber 21. The atomization unit 20 is attached so as to blow out the atomized gas vertically downward with respect to the cylindrical cavity 22. The flange 21b can be attached to and detached from the chamber main body 21a. For example, when cleaning the inside of the chamber, the flange 21b is removed and the cylindrical cavity 22 is opened to the atmosphere for cleaning.

霧化部２０には、移送ライン６Ｅから液体材料４Ａ〜４Ｃの混合液が供給されるとともに、キャリアガスライン７を介してキャリアガスが供給される。図４のＢ部拡大図に示すように、混合液およびキャリアガスが流れる配管は内側配管２３と外側配管２４とから成る２重管構造を有しており、内側配管２３の内部を混合液が気液２相流状態で流れ、内側配管２３と外側配管２４との間の環状空間をキャリアガスが流れる。気化部２０の先端部分にはオリフィス部材２５が設けられており、キャリアガスは内側配管２３とオリフィス部材２５との隙間をチャンバ内空間に噴出する。その結果、液体材料４Ａ〜４Ｃの混合液は内側配管２３の先端から霧状となって噴出する。   The atomizing unit 20 is supplied with the liquid mixture of the liquid materials 4A to 4C from the transfer line 6E and is also supplied with the carrier gas via the carrier gas line 7. As shown in the enlarged view of part B in FIG. 4, the pipe through which the mixed liquid and the carrier gas flow has a double pipe structure including an inner pipe 23 and an outer pipe 24, and the mixed liquid passes through the inner pipe 23. It flows in a gas-liquid two-phase flow state, and the carrier gas flows through the annular space between the inner pipe 23 and the outer pipe 24. An orifice member 25 is provided at the distal end portion of the vaporizing section 20, and the carrier gas is jetted through the gap between the inner pipe 23 and the orifice member 25 into the chamber space. As a result, the liquid mixture of the liquid materials 4 </ b> A to 4 </ b> C is ejected in the form of a mist from the tip of the inner pipe 23.

図２に示すように、霧化部２０のケーシング２７の下部はチャンバ本体２１ａに固定されており、チャンバ本体２１ａからの熱流入により高温となっている。一方、ケーシング２７の上部端部には水冷ジャケット２８が設けられており、この冷却ジャケット２８から下方に延びる冷却ロッド内に上記２重管が配設されている。上述したオリフィス部材２５は熱伝導率の低い樹脂等で形成され、図４のように外側配管２４の先端部分とケーシング先端部との間に挟持されて、両者の間の断熱部材としても機能している。   As shown in FIG. 2, the lower part of the casing 27 of the atomization part 20 is being fixed to the chamber main body 21a, and becomes high temperature by heat inflow from the chamber main body 21a. On the other hand, a water cooling jacket 28 is provided at the upper end of the casing 27, and the double pipe is disposed in a cooling rod extending downward from the cooling jacket 28. The orifice member 25 described above is formed of a resin having a low thermal conductivity, and is sandwiched between the distal end portion of the outer pipe 24 and the casing distal end portion as shown in FIG. 4 and functions as a heat insulating member between the two. ing.

図２の霧化部２０により霧化された液体材料４Ａ〜４Ｃは、円筒空洞２２の霧化部先端部と対向する面に向けて噴出され、図３に示すように円筒空洞２２の内周面に沿って矢印Ｒ１のように流れる。気化チャンバ２１にはヒータｈ１〜ｈ９が設けられていて、気化温度以上となるように温度制御されている。そのため、霧状の液体材料４Ａ〜４Ｃは、内周面に沿って流れる間に気化され、キャリアガスと共に排出口２９から排出されてＣＶＤリアクタへと送られる。   The liquid materials 4A to 4C atomized by the atomizing unit 20 in FIG. 2 are ejected toward the surface of the cylindrical cavity 22 facing the tip of the atomizing unit, and the inner periphery of the cylindrical cavity 22 as shown in FIG. It flows along the surface as indicated by an arrow R1. The vaporization chamber 21 is provided with heaters h1 to h9, and the temperature is controlled to be equal to or higher than the vaporization temperature. Therefore, the mist-like liquid materials 4A to 4C are vaporized while flowing along the inner peripheral surface, are discharged from the discharge port 29 together with the carrier gas, and are sent to the CVD reactor.

気化チャンバ本体２１ａおよびフランジ２１ｂに設けられたヒータｈ１〜ｈ９が設けられており、その内のヒータｈ１〜ｈ３は温度センサ３０で検出された温度に基づいて温度調節装置３２により制御される。一方、ヒータｈ４〜ｈ９は温度センサ３１で検出された温度に基づいて温度調節装置３３により制御される。円筒空洞２２の内周面は全面が気化面として機能するが、図２，３に示すように、液体材料４Ａ〜４Ｃは霧化部２０からほぼ鉛直下方向に噴出されるため、図３の面Ｓ１が主な気化面となる。そのため、気化チャンバを均一に加熱した場合でも、気化量（液体材料４Ａ〜４Ｃの流量）が多いと、気化面Ｓ１の温度が気化熱により低下して気化面Ｓ１に未気化成分が残渣として生じやすくなる。   Heaters h1 to h9 provided on the vaporizing chamber main body 21a and the flange 21b are provided, and the heaters h1 to h3 are controlled by the temperature adjusting device 32 based on the temperature detected by the temperature sensor 30. On the other hand, the heaters h4 to h9 are controlled by the temperature adjustment device 33 based on the temperature detected by the temperature sensor 31. The entire inner peripheral surface of the cylindrical cavity 22 functions as a vaporization surface. However, as shown in FIGS. 2 and 3, since the liquid materials 4A to 4C are ejected from the atomizing section 20 substantially vertically downward, The surface S1 is the main vaporization surface. Therefore, even when the vaporization chamber is heated uniformly, if the vaporization amount (flow rate of the liquid materials 4A to 4C) is large, the temperature of the vaporization surface S1 is lowered by the heat of vaporization, and unvaporized components are generated as residues on the vaporization surface S1. It becomes easy.

そこで、本実施の形態では、図２，３に示すように面Ｓ１の近傍に設けられたヒータｈ１〜ｈ３とその他のヒータｈ４〜ｈ９とをそれぞれ別個の温度調節装置３２，３３で制御し、気化の最中にも気化面Ｓ１の温度が最適温度となるように制御するようにした。すなわち、液体材料４Ａ〜４Ｃおよびその流量に応じてヒータｈ１〜ｈ３で発生する熱エネルギーを調節し、気化面Ｓ１の温度を最適温度にする。例えば、熱エネルギーを増やして、気化面Ｓ１の温度を気化チャンバ２１の温度より高めに設定すると、液体材料４Ａ〜４Ｃの熱分解温度が気化温度に近い場合に有効である。その結果、気化面Ｓ１における未気化成分の発生を低減することができる。   Therefore, in the present embodiment, as shown in FIGS. 2 and 3, the heaters h1 to h3 and the other heaters h4 to h9 provided in the vicinity of the surface S1 are controlled by separate temperature control devices 32 and 33, respectively. During the vaporization, the temperature of the vaporization surface S1 is controlled to be the optimum temperature. That is, the thermal energy generated by the heaters h1 to h3 is adjusted according to the liquid materials 4A to 4C and the flow rate thereof, and the temperature of the vaporization surface S1 is set to the optimum temperature. For example, increasing the thermal energy and setting the temperature of the vaporization surface S1 higher than the temperature of the vaporization chamber 21 is effective when the thermal decomposition temperatures of the liquid materials 4A to 4C are close to the vaporization temperature. As a result, it is possible to reduce the generation of unvaporized components on the vaporized surface S1.

ところで、気化チャンバ２１はＳＵＳ材で形成されるのが一般的であるが、気化面として機能する円筒空洞２２の壁面が液体材料４Ａ〜４Ｃと化学反応するという問題があった。本実施の形態では、このような壁面と液体材料４Ａ〜４Ｃとの反応を防止するために、ＣＶＤにより成膜される膜を壁面にコーティングするようにした。例えば、ＢＳＴ膜（BaSrTi酸化膜）を成膜するＣＶＤ装置に使用する気化器であれば、ＢＳＴ膜を壁面にコーティングする。その結果、円筒空洞のＳＵＳ壁面はコーティングされた膜により保護され、気化された金属材料との反応を防止することができる。このような膜としては、ＢＳＴ膜の他に、ＰＺＴ膜（PbZrTi膜）、ＳＴＯ膜（SrTiO２）、TiO２膜、ＳＢＴ膜（SrBiTa酸化膜）等の誘電体膜や、超伝導膜等の酸化物などがある。 Incidentally, the vaporization chamber 21 is generally formed of a SUS material. However, there is a problem that the wall surface of the cylindrical cavity 22 that functions as a vaporization surface chemically reacts with the liquid materials 4A to 4C. In the present embodiment, in order to prevent such a reaction between the wall surface and the liquid materials 4A to 4C, the film formed by CVD is coated on the wall surface. For example, in the case of a vaporizer used in a CVD apparatus for forming a BST film (BaSrTi oxide film), the wall surface is coated with the BST film. As a result, the SUS wall surface of the cylindrical cavity is protected by the coated film, and reaction with the vaporized metal material can be prevented. As such a film, in addition to the BST film, a dielectric film such as a PZT film (PbZrTi film), an STO film (SrTiO 2 ), a TiO 2 film, an SBT film (SrBiTa oxide film), a superconducting film, etc. There are oxides.

次に、気化器の気化性能評価方法について説明する。気化器の気化性能は、気化器に供給された液体材料の内の何パーセントが気化されたかによって評価されるが、これは供給量と気化器内の未気化成分の量との差によって求めることができる。図５は、性能評価の計量の手順を示したものであり、以下では材料としてＢａ，ＳｒおよびＴｉを用いる場合について説明する。   Next, the vaporization performance evaluation method of the vaporizer will be described. The vaporization performance of the vaporizer is evaluated by the percentage of the liquid material supplied to the vaporizer, which is determined by the difference between the feed rate and the amount of unvaporized components in the vaporizer. Can do. FIG. 5 shows a measurement procedure for performance evaluation, and the case where Ba, Sr and Ti are used as materials will be described below.

図５のステップＳ１では、所定量の液体材料を気化器で気化させる。次いで、ステップＳ２のサンプリング工程では、気化面を含めた気化チャンバの全内壁面に付着している未気化成分をエチルアルコール等で除去する。例えば、重さ０．１〜０．３ｇ程度の布にエチルアルコールを含ませ、その布で壁面に付着した未気化成分を拭き取る。ステップＳ３の有機物分解Ａ工程では、拭き取り後の布を塩酸２ｍｌ，過酸化水素０．５ｍｌおよび純水１ｍｌの混合液に浸して、温度１５０℃で１．５時間加熱し、布に付着している有機物を分解する。ステップＳ４の有機物分解Ｂ工程では、ステップＳ３の溶液にさらに塩酸１ｍｌ，過酸化水素０．５ｍｌおよび純水１ｍｌを加えて、温度１５０℃で１．５時間加熱する。 In step S1 of FIG. 5 , a predetermined amount of liquid material is vaporized by a vaporizer. Next, in the sampling process of step S2, unvaporized components adhering to all inner wall surfaces of the vaporization chamber including the vaporized surface are removed with ethyl alcohol or the like. For example, ethyl alcohol is included in a cloth having a weight of about 0.1 to 0.3 g, and the unvaporized components adhering to the wall surface are wiped off with the cloth. In the organic matter decomposition step A of step S3, the cloth after wiping is immersed in a mixed solution of 2 ml of hydrochloric acid, 0.5 ml of hydrogen peroxide and 1 ml of pure water, heated at a temperature of 150 ° C. for 1.5 hours, and adhered to the cloth. Decomposes organic matter. In the organic matter decomposition step B of step S4, 1 ml of hydrochloric acid, 0.5 ml of hydrogen peroxide and 1 ml of pure water are further added to the solution of step S3 and heated at a temperature of 150 ° C. for 1.5 hours.

ステップＳ５の煮沸・濃縮工程では、さらに純水１ｍｌを加えて１５０℃で０．５時間加熱する。ステップＳ６のろ過・定容工程では、ステップＳ５の溶液をろ過した後、塩酸１ｍｌを添加し、さらに２０〜１００ｍｌに容積をそろえる。ステップＳ７では、ＩＣＰ(誘導結合プラズマ)を用いた分析装置により各元素Ｂａ，Ｓｒ，Ｔｉの定量分析を行い、未気化成分量を算出する。定量分析をする際には、図６に示すような試料をＩＣＰ分析したものを検量線として使用し、検量線との比較から未気化成分量を算出する。ステップＳ８では、気化に使用した液体材料の量と、ステップＳ７で算出された未気化成分量とから気化率を算出する。このように、本実施の形態の評価方法では、気化器内壁面に付着している未気化成分を実際に定量分析しているため、気化器の気化性能を正確に評価することが可能となる。 In the boiling / concentration step of step S5, 1 ml of pure water is further added and heated at 150 ° C. for 0.5 hour. In the filtration / constant volume step of step S6, after filtering the solution of step S5, 1 ml of hydrochloric acid is added, and the volume is further adjusted to 20 to 100 ml. In step S7, each element Ba, Sr, Ti is quantitatively analyzed by an analyzer using ICP (inductively coupled plasma) to calculate the amount of unvaporized components. When quantitative analysis is performed, an ICP analysis of a sample as shown in FIG. 6 is used as a calibration curve, and the amount of unvaporized components is calculated from comparison with the calibration curve. In step S8, the vaporization rate is calculated from the amount of the liquid material used for vaporization and the amount of the unvaporized component calculated in step S7. Thus, in the evaluation method of the present embodiment, since the unvaporized components adhering to the inner wall surface of the vaporizer are actually quantitatively analyzed, it is possible to accurately evaluate the vaporization performance of the vaporizer. .

気化装置全体の概略構成を示す図である。It is a figure which shows schematic structure of the whole vaporization apparatus. 気化器２を詳細に示す図であり、正面から見た断面図である。It is a figure which shows the vaporizer | carburetor 2 in detail, and is sectional drawing seen from the front. 図２のＡ−Ａ’断面図である。It is A-A 'sectional drawing of FIG. 図２のＢ部拡大図である。It is the B section enlarged view of FIG. 本発明による気化性能評価方法の手順を示す図である。It is a figure which shows the procedure of the vaporization performance evaluation method by this invention. 検量線として用いる試料の内容を示す図である。It is a figure which shows the content of the sample used as a calibration curve.

符号の説明Explanation of symbols

１ 液体材料供給装置
２ 気化器
２０ 霧化部
２１ 気化チャンバ
２１ａ チャンバ本体
２２，４５，７７ 円筒空洞
Ｓ１ 気化面 1 Liquid material supply device
2 vaporizers
20 atomization part
21 vaporization chamber
21a chamber body 22, 45, 77 cylindrical cavity
S1 vaporization surface

Claims (1)

高温に保持された気化チャンバ内に液体有機金属若しくは有機金属溶液から成る液体材料を噴霧して気化する気化器の気化性能評価方法であって、
所定量の前記液体材料を前記気化チャンバ内に噴霧して気化させた後に、前記気化チャンバ内の未気化付着物を有機溶剤で除去し、その除去に用いた前記有機溶剤中の前記液体材料の含有量を計測し、計測された含有量に基づいて気化性能を評価することを特徴とする気化性能評価方法。 A method for evaluating the vaporization performance of a vaporizer for vaporizing a liquid material composed of a liquid organic metal or an organic metal solution in a vaporization chamber maintained at a high temperature,
After a predetermined amount of the liquid material is sprayed into the vaporization chamber and vaporized, unvaporized deposits in the vaporization chamber are removed with an organic solvent, and the liquid material in the organic solvent used for the removal is removed. A vaporization performance evaluation method characterized by measuring the content and evaluating the vaporization performance based on the measured content.
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