JP6085424B2 - Substrate processing method, substrate processing apparatus, and storage medium - Google Patents
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- Cleaning Or Drying Semiconductors (AREA)
Description
本発明は、超臨界状態または亜臨界状態の流体を用いて基板の表面に付着した液体を除去する技術に関する。 The present invention relates to a technique for removing a liquid adhering to a surface of a substrate using a fluid in a supercritical state or a subcritical state.
基板である半導体ウエハ（以下、ウエハという）などの表面に集積回路の積層構造を形成する半導体装置の製造工程などにおいては、薬液などの洗浄液によりウエハ表面の微小なごみや自然酸化膜を除去するなど、液体を利用してウエハ表面を処理する液処理工程が設けられている。 In the manufacturing process of a semiconductor device in which a laminated structure of an integrated circuit is formed on the surface of a semiconductor wafer (hereinafter referred to as a wafer), which is a substrate, fine dust or a natural oxide film on the wafer surface is removed by a cleaning liquid such as a chemical liquid. A liquid processing step is provided for processing the wafer surface using a liquid.
ところが半導体装置の高集積化に伴い、こうした液処理工程にてウエハの表面に付着した液体などを除去する際に、いわゆるパターン倒れと呼ばれる現象が問題となっている。パターン倒れは、例えばウエハ表面に残った液体を乾燥させる際に、パターンを形成する凹凸の例えば凸部の左右（言い替えると凹部内）に残っている液体が不均一に乾燥することにより、この凸部を左右に引っ張る表面張力のバランスが崩れて液体の多く残っている方向に凸部が倒れる現象である。 However, with the high integration of semiconductor devices, a phenomenon called so-called pattern collapse has become a problem when removing liquid adhering to the wafer surface in such a liquid processing step. Pattern collapse is caused by, for example, drying the liquid remaining on the wafer surface by unevenly drying the liquid remaining on the left and right sides (in other words, in the recesses) of the unevenness that forms the pattern. This is a phenomenon in which the balance of the surface tension that pulls the part to the left and right is broken and the convex part falls down in the direction in which a large amount of liquid remains.
こうしたパターン倒れの発生を抑えつつウエハ表面に付着した液体を除去する手法として超臨界状態や亜臨界状態（以下、これらをまとめて高圧状態という）の流体を用いる方法が知られている。高圧状態の流体（高圧流体）は、液体と比べて粘度が小さく、また液体を抽出する能力も高いことに加え、高圧流体と平衡状態にある液体や気体との間で界面が存在しない。そこで、ウエハ表面に付着した液体を高圧流体と置換し、しかる後、高圧流体を気体に状態変化させると、表面張力の影響を受けることなく液体を乾燥させることができる。 As a technique for removing the liquid adhering to the wafer surface while suppressing the occurrence of such pattern collapse, a method using a fluid in a supercritical state or a subcritical state (hereinafter collectively referred to as a high pressure state) is known. A high-pressure fluid (high-pressure fluid) has a lower viscosity than a liquid and has a high ability to extract the liquid, and there is no interface between the high-pressure fluid and the liquid or gas in an equilibrium state. Therefore, when the liquid adhering to the wafer surface is replaced with a high-pressure fluid and then the state of the high-pressure fluid is changed to a gas, the liquid can be dried without being affected by the surface tension.
発明者は、このような高圧流体を利用してウエハ表面の液体を除去する技術の実用化開発を行っているが、パターンのアスペクト比が大きくなるにつれてパターンの凹部内に入り込んだ液体の除去が困難になる場合があることを把握している。このため、パターンの凹部内の液体を高圧流体で抽出し、当該凹部内を高圧流体で置換することが十分にできず、高圧流体を用いた液体除去技術を実用化する上での大きな課題となっている。 The inventor has been developing a technology for removing the liquid on the wafer surface using such a high-pressure fluid. However, as the pattern aspect ratio increases, the liquid that has entered the recesses of the pattern can be removed. Know that it can be difficult. For this reason, it is not possible to sufficiently extract the liquid in the concave portion of the pattern with the high-pressure fluid and replace the inside of the concave portion with the high-pressure fluid, which is a major problem in putting the liquid removal technology using the high-pressure fluid into practical use. It has become.
ここで特許文献１には、リンス液が付着した基板を所定の条件で超臨界状態となる超臨界物質に浸漬し、これらリンス液と超臨界物質との混合物が共に超臨界状態となる共臨界状態とすることによりリンス液を除去する技術が記載されている。しかしながら本技術は、リンス液と超臨界物質とを混合してから共臨界状態にすることが前提となっているが、我々の実験から、リンス液の臨界温度以下となる共臨界温度付近ではパターン倒れが発生することがわかった。つまり、ウエハ表面にあるリンス液を超臨界状態としてリンス液を除去させるためには、リンス液の臨界温度以上で処理することが必要であることが我々の実験からわかった。また、図１８はウエハ上のリンス液に液体ＣＯ２、超臨界ＣＯ２、気体ＣＯ２をそれぞれ混合した場合のウエハ上のパーティクル数を示しているが、またリンス液と超臨界物質を混合した場合、例えばＣＯ２の超臨界流体を使用した場合、気体状態のＣＯ２と比して、ウエハ上に付着するパーティクルが多いことが我々の実験からわかった。これは高密度である超臨界物質によってパーティクルが輸送されるためであり、この点からリンス液と混合する物質は気体状態であることが好ましく、リンス液が超臨界状態となる圧力以上であればパターン倒壊を抑制し、かつパーティクル低減が可能である。また本技術では、アスペクト比の高いパターンの凹部に入り込んでいるリンス液を短時間で超臨界状態として除去することは困難であり、生産性を確保するためには、より短時間でパターンの凹部内に入り込んだリンス液を除去する必要がある。 Here, in Patent Document 1, a substrate to which a rinsing liquid is attached is immersed in a supercritical material that becomes a supercritical state under a predetermined condition, and a cocriticality in which a mixture of the rinsing liquid and the supercritical material both becomes a supercritical state. A technique for removing the rinsing liquid by setting the state is described. However, this technology is based on the premise that the rinse solution and the supercritical material are mixed before being brought into the cocritical state. From our experiments, however, the pattern near the cocritical temperature, which is lower than the critical temperature of the rinse solution. It turns out that a fall occurs. In other words, it was found from our experiments that in order to remove the rinsing liquid from the rinsing liquid on the wafer surface in a supercritical state, it is necessary to perform treatment at a temperature higher than the critical temperature of the rinsing liquid. FIG. 18 shows the number of particles on the wafer when liquid CO 2 , supercritical CO 2 , and gas CO 2 are mixed with the rinse liquid on the wafer, respectively, and the rinse liquid and the supercritical material are mixed. In some cases, for example, when using a CO 2 supercritical fluid, our experiments have shown that there are more particles adhering to the wafer as compared to gaseous CO 2 . This is because particles are transported by a supercritical substance having a high density. From this point, the substance to be mixed with the rinsing liquid is preferably in a gaseous state, so long as it is equal to or higher than the pressure at which the rinsing liquid becomes a supercritical state. Pattern collapse can be suppressed and particle reduction is possible. Also, with this technology, it is difficult to remove the rinsing liquid entering the concave portion of the pattern having a high aspect ratio as a supercritical state in a short time, and in order to secure productivity, the concave portion of the pattern is shortened in a shorter time. It is necessary to remove the rinse liquid that has entered the inside.
本発明はこのような背景の下になされたものであり、基板のパターン内に入り込んだ乾燥防止用の液体を除去することが可能な基板処理方法、基板処理装置及び、前記方法を記憶した記憶媒体を提供することを目的とする。 The present invention has been made under such a background, and a substrate processing method, a substrate processing apparatus, and a memory storing the method capable of removing a liquid for preventing drying that has entered the pattern of the substrate. The purpose is to provide a medium.
本発明に係る基板処理方法は、表面に凹凸パターンが形成され、その凹部内に入り込むように前記パターンを覆う乾燥防止用の液体が付着した基板を処理容器内に搬入する工程と、
次いで、前記基板上の乾燥防止用の液体の温度−圧力状態が、前記乾燥防止用の液体の蒸気圧曲線よりも液相側の領域を通って変化し、超臨界状態または亜臨界状態である高圧状態に達するように、当該処理容器内を外部から加圧しながら基板を加熱し、且つ、前記処理容器内を外部から加圧する圧力と、基板を加熱するために供給する熱との少なくとも一方を変化させ、前記パターンの凹部内に入り込んだ状態のまま前記乾燥防止用の液体を高圧状態とする工程と、
その後、前記処理容器内の流体を高圧状態または気体の状態で排出する工程と、を含むことを特徴とする。
The substrate processing method according to the present invention includes a step of bringing a substrate having a concavo-convex pattern formed on the surface thereof and having a liquid for preventing drying covering the pattern so as to enter the concave portion into the processing container,
Then, the temperature of the liquid for preventing drying on the substrate - the pressure state than said vapor pressure curve of the liquid anti-drying varied through the region of the liquid-phase side is in a supercritical state or subcritical state The substrate is heated while pressurizing the inside of the processing container from the outside so as to reach a high pressure state, and at least one of the pressure for pressurizing the inside of the processing container from the outside and the heat supplied to heat the substrate Changing the liquid for preventing drying to be in a high-pressure state while remaining in the recessed portion of the pattern; and
And a step of discharging the fluid in the processing container in a high-pressure state or a gas state.
前記基板処理方法は以下の特徴を備えていてもよい。
（ａ）前記処理容器内の加圧は、当該処理容器に加圧用の気体または高圧状態の流体を供給することにより行われること。
（ｂ）（ａ）において前記処理容器内の加圧は、加圧用の気体を供給することにより行われ、前記乾燥防止用の液体が臨界圧力以上に加圧され、前記乾燥防止用の液体が超臨界状態になったときに、前記加圧用の気体が気体状態であること。
（ｃ）（ａ）において前記乾燥防止用の液体が臨界圧力以上に加圧され、前記乾燥防止用の液体が超臨界状態になったときに、前記加圧用の気体または高圧状態の流体が高圧状態(超臨界状態または亜臨界状態)であること。
（ｄ）前記処理容器内にて、基板は乾燥防止用の液体に浸漬された状態で加熱されること。
（ｅ）基板は、乾燥防止用の液体が液盛りされた状態で前記処理容器に搬入されること。
（ｆ）前記乾燥防止用の液体が可燃性もしくは不燃性であり、当該液体が付着した基板を搬入する前に、前記処理容器内に不活性ガスを供給する工程を含むこと。
The substrate processing method may include the following features.
(A) Pressurization in the processing container is performed by supplying a gas for pressurization or a fluid in a high pressure state to the processing container.
(B) In (a), pressurization in the processing container is performed by supplying a gas for pressurization, the drying preventing liquid is pressurized to a critical pressure or more, and the drying preventing liquid is when it becomes a supercritical state, it air of the pressurizing is a gas state.
(C) When the anti-drying liquid is pressurized to a critical pressure or higher in (a) and the anti-drying liquid is in a supercritical state, the pressurizing gas or high -pressure fluid is high pressure. State (supercritical state or subcritical state).
(D) The substrate is heated while being immersed in a liquid for preventing drying in the processing container.
(E) The substrate is carried into the processing container in a state where a liquid for preventing drying is accumulated.
(F) The drying prevention liquid is flammable or nonflammable, and includes a step of supplying an inert gas into the processing container before carrying in the substrate to which the liquid adheres.
本発明は、処理容器内の温度−圧力状態が、基板に付着した乾燥防止用の液体の蒸気圧曲線よりも液相側の領域を通って変化し、超臨界状態または亜臨界状態である高圧状態に達するように、処理容器内を加圧しながら基板を加熱する。これにより、当該液体の沸騰を避けつつ、前記パターンの凹部内に入り込んだ状態のまま、この液体を高圧状態の流体に変化させることができるので、パターン倒れの発生を抑えつつ基板に付着した液体を除去することができる。 The present invention relates to a high pressure in which a temperature-pressure state in a processing container changes through a region on a liquid phase side of a vapor pressure curve of a liquid for preventing drying attached to a substrate, and is in a supercritical state or a subcritical state. The substrate is heated while pressurizing the inside of the processing container so as to reach the state. Thereby, while avoiding the boiling of the liquid, the liquid can be changed into a high-pressure fluid while entering the concave portion of the pattern, so that the liquid adhered to the substrate while suppressing the occurrence of pattern collapse. Can be removed.
本発明の基板処理装置を備えた基板処理システムの一例として、被処理基板であるウエハＷに洗浄液を供給して洗浄処理を行う洗浄装置２と、洗浄処理後のウエハＷに付着している乾燥防止用の液体を超臨界状態（高圧状態）にして除去する超臨界処理装置３とを備えた洗浄処理システム１について説明する。 As an example of a substrate processing system including the substrate processing apparatus of the present invention, a cleaning apparatus 2 that supplies a cleaning liquid to a wafer W that is a substrate to be processed and performs a cleaning process, and a drying that adheres to the wafer W after the cleaning process A cleaning processing system 1 including a supercritical processing apparatus 3 that removes a prevention liquid in a supercritical state (high pressure state) will be described.
図１は洗浄処理システム１の全体構成を示す横断平面図、図２はその外観斜視図であり、これらの図に向かって左側を前方とする。洗浄処理システム１では、載置部１１にＦＯＵＰ１００が載置され、このＦＯＵＰ１００に格納された例えば直径３００ｍｍの複数枚のウエハＷが、搬入出部１２及び受け渡し部１３を介して後段の洗浄処理部１４、超臨界処理部１５との間で受け渡され、洗浄装置２、超臨界処理装置３内に順番に搬入されて洗浄処理や乾燥防止用の液体を除去する処理が行われる。図中、１２１はＦＯＵＰ１００と受け渡し部１３との間でウエハＷを搬送する第１の搬送機構、１３１は搬入出部１２と洗浄処理部１４、超臨界処理部１５との間を搬送されるウエハＷが一時的に載置されるバッファとしての役割を果たす受け渡し棚である。 FIG. 1 is a cross-sectional plan view showing the overall configuration of the cleaning processing system 1, and FIG. 2 is an external perspective view thereof. In the cleaning system 1, the FOUP 100 is mounted on the mounting unit 11, and a plurality of wafers W having a diameter of, for example, 300 mm stored in the FOUP 100 are transferred to the subsequent cleaning processing unit via the loading / unloading unit 12 and the transfer unit 13. 14 is transferred to and from the supercritical processing unit 15 and is sequentially carried into the cleaning device 2 and the supercritical processing device 3 to perform a cleaning process and a process for removing the liquid for preventing drying. In the figure, reference numeral 121 denotes a first transfer mechanism for transferring a wafer W between the FOUP 100 and the transfer unit 13, and 131 denotes a wafer transferred between the loading / unloading unit 12, the cleaning processing unit 14, and the supercritical processing unit 15. W is a delivery shelf that serves as a buffer on which W is temporarily placed.
洗浄処理部１４及び超臨界処理部１５は、受け渡し部１３との間の開口部から前後方向に向かって伸びるウエハ搬送路１６２に沿って前方からこの順番に設けられている。洗浄処理部１４には、当該ウエハ搬送路１６２を挟んで洗浄装置２が１台ずつ配置されている。一方、超臨界処理部１５には、本実施の形態の基板処理装置である超臨界処理装置３が、ウエハ搬送路１６２を挟んで３台ずつ、合計６台配置されている。 The cleaning processing unit 14 and the supercritical processing unit 15 are provided in this order from the front along the wafer transfer path 162 extending in the front-rear direction from the opening between the transfer processing unit 13 and the transfer processing unit 13. In the cleaning processing unit 14, one cleaning device 2 is disposed across the wafer transfer path 162. On the other hand, in the supercritical processing section 15, six supercritical processing apparatuses 3, which are substrate processing apparatuses according to the present embodiment, are arranged in three units with the wafer transfer path 162 interposed therebetween.
ウエハＷは、ウエハ搬送路１６２に配置された第２の搬送機構１６１によってこれら各洗浄装置２、超臨界処理装置３及び受け渡し部１３の間を搬送される。ここで洗浄処理部１４や超臨界処理部１５に配置される洗浄装置２や超臨界処理装置３の個数は、単位時間当たりのウエハＷの処理枚数や、洗浄装置２、超臨界処理装置３での処理時間の違いなどにより適宜選択され、これら洗浄装置２や超臨界処理装置３の配置数などに応じて最適なレイアウトが選択される。 The wafer W is transferred between the cleaning device 2, the supercritical processing device 3, and the delivery unit 13 by the second transfer mechanism 161 arranged in the wafer transfer path 162. Here, the number of cleaning apparatuses 2 and supercritical processing apparatuses 3 arranged in the cleaning processing section 14 and the supercritical processing section 15 is the same as the number of wafers W processed per unit time, the cleaning apparatus 2 and the supercritical processing apparatus 3. The optimum layout is selected according to the number of the cleaning apparatuses 2 and supercritical processing apparatuses 3 arranged.
洗浄装置２は例えばスピン洗浄によりウエハＷを１枚ずつ洗浄する枚葉式の洗浄装置２として構成され、例えば図３の縦断側面図に示すように、処理空間を形成するアウターチャンバー２１内に配置されたウエハ保持機構２３にてウエハＷをほぼ水平に保持し、このウエハ保持機構２３を鉛直軸周りに回転させることによりウエハＷを回転させる。そして回転するウエハＷの上方にノズルアーム２４を進入させ、その先端部に設けられた薬液ノズル２４１から薬液及びリンス液を予め定められた順に供給することによりウエハの面の洗浄処理が行われる。また、ウエハ保持機構２３の内部にも薬液供給路２３１が形成されており、ここから供給された薬液及びリンス液によってウエハＷの裏面洗浄が行われる。 The cleaning apparatus 2 is configured as a single wafer cleaning apparatus 2 that cleans wafers W one by one by spin cleaning, for example, and is disposed in an outer chamber 21 that forms a processing space, as shown in a vertical side view of FIG. The wafer holding mechanism 23 holds the wafer W substantially horizontally, and the wafer W is rotated by rotating the wafer holding mechanism 23 around the vertical axis. Then, the nozzle arm 24 is advanced above the rotating wafer W, and the chemical liquid and the rinsing liquid are supplied in a predetermined order from the chemical liquid nozzle 241 provided at the tip of the wafer arm 24, whereby the wafer surface is cleaned. Further, a chemical solution supply path 231 is also formed inside the wafer holding mechanism 23, and the back surface of the wafer W is cleaned by the chemical solution and the rinsing solution supplied therefrom.
洗浄処理は、例えばアルカリ性の薬液であるＳＣ１液（アンモニアと過酸化水素水の混合液）によるパーティクルや有機性の汚染物質の除去→リンス液である脱イオン水（DeIonized Water：ＤＩＷ）によるリンス洗浄→酸性薬液である希フッ酸水溶液（以下、ＤＨＦ（Diluted HydroFluoric acid））による自然酸化膜の除去→ＤＩＷによるリンス洗浄が行われる。これらの薬液はアウターチャンバー２１内に配置されたインナーカップ２２やアウターチャンバー２１に受け止められて排液口２２１、２１１より排出される。またアウターチャンバー２１内の雰囲気は排気口２１２より排気されている。 The cleaning process is, for example, removal of particles and organic pollutants with an SC1 solution (a mixture of ammonia and hydrogen peroxide solution), which is an alkaline chemical solution, and a rinse with deionized water (DIW), which is a rinse solution. → Removal of natural oxide film by dilute hydrofluoric acid aqueous solution (hereinafter referred to as DHF (Diluted HydroFluoric acid)) which is an acidic chemical solution → Rinse cleaning by DIW is performed. These chemical solutions are received by the inner cup 22 or the outer chamber 21 disposed in the outer chamber 21 and discharged from the drain ports 221 and 211. The atmosphere in the outer chamber 21 is exhausted from the exhaust port 212.
薬液による洗浄処理を終えたら、ウエハ保持機構２３の回転を停止してから当該表面にＩＰＡ（IsoPropyl Alcohol）を供給し、ウエハＷの表面及び裏面に残存しているＤＩＷと置換する。こうして洗浄処理を終えたそしてウエハＷは、その表面にＩＰＡが液盛りされた状態（ウエハＷ表面にＩＰＡの液膜が形成された状態）のまま例えばウエハ保持機構２３に設けられた不図示の受け渡し機構により第２の搬送機構１６１に受け渡され、洗浄装置２より搬出される。 When the cleaning process using the chemical solution is completed, the rotation of the wafer holding mechanism 23 is stopped, and then IPA (IsoPropyl Alcohol) is supplied to the front surface to replace the DIW remaining on the front and back surfaces of the wafer W. After the cleaning process is completed in this way, the wafer W is not provided in the wafer holding mechanism 23, for example, in a state where IPA is accumulated on the surface (a state where an IPA liquid film is formed on the surface of the wafer W). It is delivered to the second transport mechanism 161 by the delivery mechanism and is carried out from the cleaning device 2.
洗浄装置２にてウエハＷ表面に液盛りされたＩＰＡは、洗浄装置２から超臨界処理装置３へのウエハＷの搬送中や、超臨界処理装置３への搬入動作中に当該ＩＰＡが蒸発（気化）することによってパターン倒れが発生することを防ぐ乾燥防止用の液体としての役割を果たしている。 The IPA accumulated on the surface of the wafer W by the cleaning apparatus 2 evaporates during the transfer of the wafer W from the cleaning apparatus 2 to the supercritical processing apparatus 3 or during the loading operation to the supercritical processing apparatus 3 ( It plays a role as an anti-drying liquid that prevents pattern collapse from occurring due to vaporization.
洗浄装置２での洗浄処理を終え、表面に乾燥防止用のＩＰＡの液盛りがされたウエハＷは、超臨界処理装置３に搬送され、当該ＩＰＡを高圧状態にして除去し、ウエハＷを乾燥する処理が行われる。以下、本実施の形態に係る超臨界処理装置３の構成について図４、図５を参照しながら説明する。超臨界処理装置３は、ウエハＷ表面に付着した乾燥防止用の液体であるＩＰＡを除去する処理が行われる処理容器３１と、この処理容器３１内を加圧するためのガスを供給する加圧流体供給部３６とを備えている。 After the cleaning process in the cleaning apparatus 2 is finished, the wafer W on which the surface of the IPA for preventing drying is deposited is transferred to the supercritical processing apparatus 3 to remove the IPA in a high pressure state, and the wafer W is dried. Processing is performed. Hereinafter, the configuration of the supercritical processing apparatus 3 according to the present embodiment will be described with reference to FIGS. 4 and 5. The supercritical processing apparatus 3 includes a processing container 31 that performs a process for removing IPA that is a liquid for preventing drying attached to the surface of the wafer W, and a pressurized fluid that supplies a gas for pressurizing the inside of the processing container 31. And a supply unit 36.
図５に示すように処理容器３１は、ウエハＷの搬入出用の開口部３１２が形成された筐体状の容器本体３１１と、処理対象のウエハＷを液体ＩＰＡに浸漬した状態で横向きに保持することが可能なウエハトレイ３３１と、このウエハトレイ３３１を支持すると共に、ウエハＷを容器本体３１１内に搬入したとき前記開口部３１２を密閉する蓋部材３３２とを備えている。 As shown in FIG. 5, the processing container 31 is held sideways in a state in which the casing-shaped container body 311 in which an opening 312 for carrying in / out the wafer W is formed and the wafer W to be processed are immersed in the liquid IPA. And a lid member 332 that supports the wafer tray 331 and seals the opening 312 when the wafer W is loaded into the container main body 311.
容器本体１１は、例えば直径３００ｍｍのウエハＷを収容可能な、２００〜１００００ｃｍ３程度の処理空間が形成された容器であり、その上面には、処理容器３１内に加圧流体を供給するための加圧流体供給ライン３５１と、処理容器３１内の流体を排出するための排出ライン３４１とが接続されている。また、処理容器１には処理空間内に供給された高圧状態の処理流体から受ける内圧に抗して、容器本体３１１に向けて蓋部材３３２を押し付け、処理空間を密閉するための不図示の押圧機構が設けられている。 The container body 11 is a container in which a processing space of about 200 to 10000 cm 3 is formed, which can accommodate, for example, a wafer W having a diameter of 300 mm, and a pressurized fluid is supplied into the processing container 31 on the upper surface thereof. A pressurized fluid supply line 351 and a discharge line 341 for discharging the fluid in the processing container 31 are connected. Further, the processing container 1 is pressed against the internal pressure received from the high-pressure processing fluid supplied into the processing space, and the lid member 332 is pressed toward the container body 311 to seal the processing space (not shown). A mechanism is provided.
容器本体３１１には、例えば抵抗発熱体などからなる加熱部であるヒーター３２２と、処理容器３１内の温度を検出するための熱電対などを備えた温度検出部３２３とが設けられており、容器本体３１１を加熱することにより、処理容器３１内の温度を予め設定された温度に加熱し、これにより内部のウエハＷを加熱することができる。ヒーター３２２は、給電部３２１から供給される電力により、発熱量を変化させることが可能であり、温度検出部３２３から取得した温度検出結果に基づき、処理容器３１内の温度を予め定められた昇温スケジュールに基づいて昇温していく。 The container main body 311 is provided with a heater 322 which is a heating unit made of, for example, a resistance heating element, and a temperature detection unit 323 including a thermocouple for detecting the temperature in the processing container 31. By heating the main body 311, the temperature in the processing container 31 can be heated to a preset temperature, thereby heating the wafer W inside. The heater 322 can change the amount of heat generated by the electric power supplied from the power supply unit 321, and the temperature inside the processing container 31 is increased in advance based on the temperature detection result acquired from the temperature detection unit 323. The temperature rises based on the temperature schedule.
加圧流体供給部３６には、処理容器３１内の圧力を大気圧よりも高い０．１〜６ＭＰａ程度に加圧するための高圧ガス（本例では窒素ガス）が保持されている。図４中、３５１は加圧流体供給部３６から処理容器３１に加圧流体を供給するための加圧流体供給ライン、３５２は処理容器３１に設けられた圧力検出部３１３の検出結果に基づき、処理容器３１内が前記圧力に調整されるように加圧流体の供給量を調節する減圧弁である。 The pressurized fluid supply unit 36 holds a high-pressure gas (nitrogen gas in this example) for pressurizing the pressure in the processing container 31 to about 0.1 to 6 MPa, which is higher than the atmospheric pressure. In FIG. 4, 351 is a pressurized fluid supply line for supplying pressurized fluid from the pressurized fluid supply unit 36 to the processing container 31, and 352 is based on the detection result of the pressure detection unit 313 provided in the processing container 31. It is a pressure reducing valve that adjusts the supply amount of the pressurized fluid so that the inside of the processing container 31 is adjusted to the pressure.
以上に説明した構成を備えた洗浄処理システム１や洗浄装置２、超臨界処理装置３は図１、図４に示すように制御部４に接続されている。制御部４は図示しないＣＰＵと記憶部とを備えたコンピュータからなり、記憶部にはこれら洗浄処理システム１や洗浄装置２、超臨界処理装置３の作用、即ちＦＯＵＰ１００からウエハＷを取り出して洗浄装置２にて洗浄処理を行い、次いで超臨界処理装置３にてウエハＷを乾燥する処理を行ってからＦＯＵＰ１００内にウエハＷを搬入するまでの動作に係わる制御についてのステップ（命令）群が組まれたプログラムが記録されている。このプログラムは、例えばハードディスク、コンパクトディスク、マグネットオプティカルディスク、メモリーカード等の記憶媒体に格納され、そこからコンピュータにインストールされる。 The cleaning processing system 1, the cleaning apparatus 2, and the supercritical processing apparatus 3 having the configuration described above are connected to the control unit 4 as shown in FIGS. 1 and 4. The control unit 4 includes a computer including a CPU and a storage unit (not shown). The storage unit is operated by the cleaning processing system 1, the cleaning apparatus 2, and the supercritical processing apparatus 3, that is, the wafer W is taken out from the FOUP 100 and cleaned. Steps (commands) for control related to operations from the cleaning process at 2 and the drying process of the wafer W by the supercritical processing apparatus 3 to the loading of the wafer W into the FOUP 100 are assembled. Recorded programs. This program is stored in a storage medium such as a hard disk, a compact disk, a magnetic optical disk, or a memory card, and installed in the computer therefrom.
特に超臨界処理装置３について制御部４は、ウエハＷを浸漬した状態となっている処理容器３１（ウエハトレイ３３１）内の液体ＩＰＡを加圧された雰囲気下で加熱し、当該ＩＰＡを沸騰させないようにしながら超臨界状態（高圧状態）に変化させることにより、パターン倒れを発生させずに当該液体を除去するように制御信号を出力する。 Particularly, in the supercritical processing apparatus 3, the control unit 4 heats the liquid IPA in the processing container 31 (wafer tray 331) in which the wafer W is immersed in a pressurized atmosphere so as not to boil the IPA. By changing to a supercritical state (high pressure state), the control signal is output so as to remove the liquid without causing pattern collapse.
以上に説明した構成を備えた超臨界処理装置３の作用について図６〜図９の作用図、及びウエハＷを処理している期間中の処理容器３１内の温度-圧力状態を示した図１０を参照しながら説明する。ここで処理容器３１内のＩＰＡの気液平衡が保たれる速度でＩＰＡの加熱を行う場合や、ウエハＷ表面のＩＰＡの液膜が十分に薄く、当該ＩＰＡを昇温する際の応答速度が十分に速い場合などでは、ＩＰＡの温度−圧力状態は処理容器３１内の温度−圧力にほぼ等しいとみなしてよい。従って以下の説明では、特に言及がない限り、処理容器３１内の温度−圧力の説明をもってウエハＷ表面のＩＰＡの温度−圧力状態を示している。図６〜図９において各バルブに付された「Ｓ」の符号は、その開閉バルブが閉状態となっていることを示し、「Ｏ」の符号は開状態となっていることを示している。 The action of the supercritical processing apparatus 3 having the above-described configuration is shown in FIGS. 6 to 9 and the temperature-pressure state in the processing container 31 during the processing of the wafer W is shown in FIG. Will be described with reference to FIG. Here, when the IPA is heated at a speed at which the vapor-liquid equilibrium of the IPA in the processing container 31 is maintained, or when the IPA liquid film on the surface of the wafer W is sufficiently thin, the response speed when raising the temperature of the IPA is high. In a case where the speed is sufficiently fast, the temperature-pressure state of the IPA may be regarded as being approximately equal to the temperature-pressure in the processing container 31. Therefore, in the following description, unless otherwise specified, the temperature-pressure state of the IPA on the surface of the wafer W is shown with the description of the temperature-pressure in the processing chamber 31. 6 to 9, the symbol “S” attached to each valve indicates that the open / close valve is closed, and the symbol “O” indicates that the valve is open. .
既述のように洗浄装置２における洗浄処理を終え、乾燥防止用のＩＰＡを液盛りしたウエハＷが第２の搬送機構１６１に受け渡されると、第２の搬送機構１６１は、ウエハＷを受け入れ可能な超臨界処理装置３の配置されている筐体内に進入する。このときウエハＷの搬入が行われる前の超臨界処理装置３は、ヒーター３２２の給電部３２１をオフにしてＩＰＡの臨界温度（２３５℃）以下の温度、大気圧の状態で待機している。このとき、Ｎ２ガスなどの不活性ガスでパージして処理容器３１内を低酸素雰囲気としておき、ヒーター３２２で処理容器３１内の加熱を開始した後、可燃性のＩＰＡが高温雰囲気下で比較的高い濃度の酸素と接触しないようにするとよい。 As described above, after the cleaning process in the cleaning apparatus 2 is completed and the wafer W on which the IPA for preventing drying is accumulated is transferred to the second transfer mechanism 161, the second transfer mechanism 161 receives the wafer W. It enters into a case where a possible supercritical processing device 3 is arranged. At this time, the supercritical processing apparatus 3 before carrying in the wafer W turns off the power supply part 321 of the heater 322 and stands by at a temperature equal to or lower than the critical temperature (235 ° C.) of IPA and atmospheric pressure. At this time, after purging with an inert gas such as N 2 gas to set the inside of the processing vessel 31 to a low oxygen atmosphere, heating of the processing vessel 31 with the heater 322 is started, and then combustible IPA is compared in a high temperature atmosphere. Avoid contact with high concentrations of oxygen.
処理を実行可能な超臨界処理装置３にウエハＷが搬入されてきたら、図５に示すように容器本体３１１の外にウエハトレイ３３１を移動させ、不図示の支持ピンを介して第２の搬送機構１６１の搬送アームからウエハトレイ３３１にウエハＷを受け渡す。そして、図示しないＩＰＡ供給ノズルからウエハトレイ３３１内に液体ＩＰＡを供給して、ウエハＷが液体ＩＰＡに浸漬された状態とする。次いで、ウエハトレイ３３１を移動させて開口部３１２を介してウエハＷを容器本体３１１の内部に搬入し、蓋部材３３２にて開口部３１２を閉じ処理容器３１内を密閉する（図６）。 When the wafer W is loaded into the supercritical processing apparatus 3 capable of performing processing, the wafer tray 331 is moved out of the container body 311 as shown in FIG. 5, and the second transfer mechanism is connected via a support pin (not shown). The wafer W is transferred from the transfer arm 161 to the wafer tray 331. Then, the liquid IPA is supplied into the wafer tray 331 from an IPA supply nozzle (not shown) so that the wafer W is immersed in the liquid IPA. Next, the wafer tray 331 is moved to carry the wafer W into the container main body 311 through the opening 312, the opening 312 is closed by the lid member 332, and the inside of the processing container 31 is sealed (FIG. 6).
ウエハＷの搬入を終えると、ＩＰＡは狭い処理容器３１内で揮発するので、処理容器３１内の温度-圧力は図１０に一点鎖線で示したＩＰＡの蒸気圧曲線の左端に白丸で記したＡ点付近の状態となる。この状態で処理容器３１内のウエハＷを急激に加熱すると、ウエハＷ表面のＩＰＡが沸騰してパターン内で気泡を発生し、パターン倒れを引き起こす要因となる。一方、ＩＰＡが沸騰しないように処理容器３１内の温度-圧力状態がＩＰＡの蒸気圧曲線上を移動するようにゆっくりと加熱を行い、液体ＩＰＡを超臨界状態に変化させれば、パターン倒れを引き起こすことなく、ウエハＷ表面から液体ＩＰＡを除去することができるが、ウエハＷの処理に長時間を要する。
When the loading of the wafer W is completed, the IPA volatilizes in the narrow processing container 31, and therefore the temperature-pressure in the processing container 31 is indicated by a white circle at the left end of the vapor pressure curve of IPA shown by a one-dot chain line in FIG. It becomes a state near the point. If the wafer W in the processing container 31 is heated rapidly in this state, the IPA on the surface of the wafer W boils and bubbles are generated in the pattern, causing a pattern collapse. On the other hand, the temperature in the processing chamber 31 so as IPA does not boil - performs slowly heated so that the pressure state is moved on the vapor pressure curve of the IPA, it is changed to liquid IPA to the supercritical state, the pattern collapse The liquid IPA can be removed from the surface of the wafer W without causing it, but it takes a long time to process the wafer W.
そこで本例の超臨界処理装置３は、処理容器３１内に加圧流体を供給して加圧し、図１０に黒丸のＢ点で示すように、処理容器３１内の温度-圧力をＩＰＡの蒸気圧曲線から離れた状態とすることにより、急速な加熱を行ってもＩＰＡが沸騰しにくい状態を作り出す。具体的には、図７に示すように加圧流体供給ライン３５１の減圧弁３５２を開き、その開度を調節して処理容器３１内の圧力が０．１〜６ＭＰａの範囲内の例えば０．５ＭＰａとなるように調整する。 Therefore, the supercritical processing apparatus 3 of the present example supplies and pressurizes the pressurized fluid into the processing container 31, and the temperature-pressure in the processing container 31 is changed to the vapor of IPA as indicated by a black circle B in FIG. By making the state away from the pressure curve, the state where IPA is not easily boiled is created even if rapid heating is performed. Specifically, as shown in FIG. 7, the pressure reducing valve 352 of the pressurized fluid supply line 351 is opened, the opening degree is adjusted, and the pressure in the processing container 31 is in the range of 0.1 to 6 MPa, for example, 0. Adjust to 5 MPa.
しかる後、給電部３２１からヒーター３２２への電力供給を開始し、処理容器３１内のＩＰＡを加熱する。このとき、処理容器３１内は加圧されているのでＩＰＡは図１０中に矢印付きの実線で示すように液体の状態維持したまま、蒸気圧曲線よりも液相側の温度-圧力領域を通って加熱される。また、ＩＰＡの一部は蒸発して処理容器３１内の圧力が上昇する。こうして、処理容器３１内の温度-圧力状態がＩＰＡの蒸気圧曲線に近づいたら（図１０のＣ点）、加熱スピードを下げ、ＩＰＡを沸騰させないように加熱を継続する。 Thereafter, power supply from the power supply unit 321 to the heater 322 is started, and the IPA in the processing container 31 is heated. At this time, since the inside of the processing container 31 is pressurized, the IPA passes through the temperature-pressure region on the liquid phase side of the vapor pressure curve while maintaining the liquid state as indicated by the solid line with an arrow in FIG. Heated. Moreover, a part of IPA evaporates and the pressure in the processing container 31 rises. Thus, when the temperature-pressure state in the processing container 31 approaches the vapor pressure curve of IPA (point C in FIG. 10), the heating speed is reduced and heating is continued so as not to boil the IPA.
そして、処理容器３１の温度-圧力状態がＩＰＡの臨界点（超臨界温度２３５℃、臨界圧力４．８ＭＰａ（絶対圧））を超えると、図８に示すように処理容器３１内全体が超臨界流体となる。この結果、ウエハＷのパターンの凹部内に入り込んでいる液体ＩＰＡも周囲のＩＰＡと共に、当該凹部内で超臨界流体となり、パターン倒れを発生させずにウエハＷの表面から液体ＩＰＡを除去することができる。なお、実際には処理容器３１内の雰囲気は、ＩＰＡや加圧流体である窒素、ウエハＷの搬入出時に外部から進入した酸素などの流体が混合された状態であるが、ＩＰＡが超臨界状態のときには、窒素や酸素は気体または超臨界流体の状態となっており、他に液体は存在しない。従ってＩＰＡを超臨界状態とすれば、パターン倒れを発生させずにウエハＷ表面の液体を除去できる。 When the temperature-pressure state of the processing container 31 exceeds the critical point of IPA (supercritical temperature 235 ° C., critical pressure 4.8 MPa (absolute pressure)), the entire processing container 31 is supercritical as shown in FIG. Become fluid. As a result, the liquid IPA entering the concave portion of the pattern of the wafer W also becomes a supercritical fluid in the concave portion together with the surrounding IPA, and the liquid IPA can be removed from the surface of the wafer W without causing pattern collapse. it can. Actually, the atmosphere in the processing vessel 31 is a state in which fluid such as IPA, nitrogen as a pressurized fluid, oxygen entered from the outside when the wafer W is loaded / unloaded is mixed, but the IPA is in a supercritical state. In this case, nitrogen and oxygen are in a gas or supercritical fluid state, and no other liquid exists. Therefore, if the IPA is in a supercritical state, the liquid on the surface of the wafer W can be removed without causing pattern collapse.
こうして処理容器３１内の液体ＩＰＡが全て超臨界状態となるのに十分な時間が経過したら、図９に示すように加圧流体供給ライン３５１の減圧弁３５２を閉じる一方、排出ライン３４１の減圧弁３４２を開いて処理容器３１内の流体を排出する。このとき、処理容器３１はＩＰＡの沸点（８２．４℃）よりも高温（例えば２５０℃）に調整されており、処理容器３１からはＣＯ２及びＩＰＡが超臨界状態、または気体の状態で排出されることになる。この結果、大気圧まで降圧された処理容器３１の内部では、パターン５１内から液体ＩＰＡ６１が除去され、乾燥した状態となったウエハＷを得ることができる。このように、パターン内に進入した液体ＩＰＡを、直接、超臨界ＩＰＡに変化させて除去する手法は、パターンのアスペクト比が１０以上程度と、高アスペクト比になったとき、及びデザインルールが２０ｎｍ以下と、ＩＰＡとＣＯ２が接する開口面積が小さくなったときに特に有効である。 When a sufficient time has passed for all of the liquid IPA in the processing container 31 to be in the supercritical state, the pressure reducing valve 352 of the pressurized fluid supply line 351 is closed as shown in FIG. 342 is opened and the fluid in the processing container 31 is discharged. At this time, the processing vessel 31 is adjusted to a temperature (for example, 250 ° C.) higher than the boiling point of IPA (82.4 ° C.), and CO 2 and IPA are discharged from the processing vessel 31 in a supercritical state or in a gaseous state. Will be. As a result, the liquid IPA 61 is removed from the pattern 51 inside the processing vessel 31 that has been depressurized to atmospheric pressure, and the wafer W that has been dried can be obtained. As described above, the method of removing the liquid IPA that has entered the pattern by directly changing it to the supercritical IPA is when the aspect ratio of the pattern is about 10 or higher and the design rule is 20 nm. This is particularly effective when the opening area where the IPA and CO 2 are in contact with each other becomes smaller.
液体ＩＰＡ６１が除去され、ウエハＷが乾燥した状態となったら、ウエハトレイ３３１を移動させて処理容器３１からウエハＷを搬出し、第２の搬送機構１６１の搬送アームにウエハＷを受け渡す。しかる後、ウエハＷは搬出棚４３を介して第１の搬送機構１２１に受け渡され、搬入時とは逆の経路を通ってＦＯＵＰ１００内に格納され、ウエハＷに対する一連の動作が完了する。
このとき洗浄システム１内に、清浄空気の気流と接触する雰囲気下などでウエハＷを保持して、処理容器３１内で加熱されたウエハＷを冷却する冷却装置を設け、超臨界処理装置３から取り出したウエハＷを一旦、この冷却装置で冷却してからＦＯＵＰ１００に格納するようにしてもよい。
When the liquid IPA 61 is removed and the wafer W is in a dry state, the wafer tray 331 is moved to unload the wafer W from the processing container 31 and deliver the wafer W to the transfer arm of the second transfer mechanism 161. Thereafter, the wafer W is transferred to the first transfer mechanism 121 via the carry-out shelf 43 and stored in the FOUP 100 through a path opposite to that at the time of loading, and a series of operations on the wafer W is completed.
At this time, the cleaning system 1 is provided with a cooling device for holding the wafer W in an atmosphere in contact with the clean air stream and cooling the wafer W heated in the processing container 31. The taken out wafer W may be once cooled by this cooling device and then stored in the FOUP 100.
本実施の形態に係わる超臨界処理装置３によれば以下の効果がある。処理容器３１内の温度−圧力状態が、ウエハＷに付着した乾燥防止用の液体ＩＰＡの蒸気圧曲線よりも液相側の領域を通るか、または当該蒸気圧曲線上を通って変化し、超臨界状態に達するように、処理容器３１内を加圧しながらウエハＷを加熱する。これにより、液体ＩＰＡの沸騰を避けつつ、前記パターン５１の凹部内に入り込んだ状態のまま、この液体ＩＰＡを超臨界状態に変化させることができるので、パターン倒れの発生を抑えつつウエハＷに付着した液体ＩＰＡを除去することができる。 The supercritical processing apparatus 3 according to the present embodiment has the following effects. The temperature-pressure state in the processing container 31 passes through the region on the liquid phase side of the vapor pressure curve of the drying prevention liquid IPA attached to the wafer W or changes over the vapor pressure curve. The wafer W is heated while pressurizing the inside of the processing container 31 so as to reach the critical state. Accordingly, the liquid IPA can be changed to a supercritical state while entering the concave portion of the pattern 51 while avoiding boiling of the liquid IPA, so that the liquid IPA adheres to the wafer W while suppressing occurrence of pattern collapse. Liquid IPA can be removed.
ここで液体ＩＰＡを沸騰させないようにウエハＷ上の液体ＩＰＡの温度-圧力状態（処理容器３１内の温度-圧力状態）を調整しながら液体ＩＰＡを超臨界状態に変化させるという手法は、液体ＩＰＡに浸漬された状態のウエハＷから当該ＩＰＡを除去する例に適用する場合に限定されるものではない。例えば、パターンの形成されたウエハＷ表面に液盛りされた液体ＩＰＡを除去する場合にも本法は適用することができる。 Here, the method of changing the liquid IPA to the supercritical state while adjusting the temperature-pressure state (temperature-pressure state in the processing vessel 31) of the liquid IPA on the wafer W so as not to boil the liquid IPA is the liquid IPA. The present invention is not limited to the case where the present invention is applied to an example in which the IPA is removed from the wafer W immersed in the wafer. For example, the present method can be applied to the case where the liquid IPA accumulated on the surface of the wafer W on which the pattern is formed is removed.
図１１は、ウエハＷ表面に液盛りされた液体ＩＰＡを除去する超臨界処理装置３の構成例を示している。ウエハＷ表面に液盛りされた液体ＩＰＡの量は、ウエハＷ全体を浸漬可能な量だけウエハトレイ３３１に供給された液体ＩＰＡの量よりも少ない場合が多い。このため、加圧流体で処理容器３１内を加圧した後、液体ＩＰＡの全量を蒸発させても、ＩＰＡが超臨界状態となる圧力となるまで処理容器３１内を昇圧できないおそれがある。 FIG. 11 shows a configuration example of the supercritical processing apparatus 3 for removing the liquid IPA accumulated on the surface of the wafer W. In many cases, the amount of liquid IPA accumulated on the surface of the wafer W is smaller than the amount of liquid IPA supplied to the wafer tray 331 by an amount capable of immersing the entire wafer W. For this reason, even if the whole amount of the liquid IPA is evaporated after pressurizing the inside of the processing container 31 with the pressurized fluid, there is a possibility that the inside of the processing container 31 cannot be pressurized until the pressure reaches a supercritical state.
そこで、図１１に示す超臨界処理装置３は、液体ＩＰＡを加熱して蒸発させた蒸気により処理容器３１内を昇圧する手法に変え、外部から処理容器３１内にガスや高圧流体を供給して、処理容器３１内にＩＰＡの臨界圧力よりも高圧の雰囲気を形成することにより、ＩＰＡを沸騰させないようにしながら超臨界状態に変化させる点が第１の実施の形態と異なる。図１１中、図４に示した第１の実施の形態に係わる超臨界処理装置３と同様の構成要素には、図４に示したものと同様の符号を付してある。 Therefore, the supercritical processing apparatus 3 shown in FIG. 11 is changed to a method in which the pressure inside the processing vessel 31 is increased by the vapor obtained by heating and evaporating the liquid IPA, and gas or high-pressure fluid is supplied into the processing vessel 31 from the outside. The point that the IPA is changed to the supercritical state while preventing the boiling of the IPA by forming an atmosphere higher than the critical pressure of IPA in the processing vessel 31 is different from the first embodiment. In FIG. 11, the same reference numerals as those shown in FIG. 4 are given to the same components as those of the supercritical processing apparatus 3 according to the first embodiment shown in FIG.
図１１に示した超臨界処理装置３は、加圧流体供給部３６に例えば、ＣＯ２が液体の状態で溜められており、加圧流体供給ライン３５１と加圧流体供給部３６との間に、当該ＣＯ２の供給圧力を調整するための、例えばシリンジポンプやダイヤフラムポンプなどからなる昇圧ポンプ３６２と、圧力調整された気体ＣＯ２を保持する加圧流体タンク３６３とが設けられている点が第１の実施の形に係わる超臨界処理装置３とは異なる。加圧流体タンク３６３には、処理容器３１内の圧力をＩＰＡの臨界圧より高い圧力まで昇圧することが可能な十分量の気体ＣＯ２が保持されている。図中、３６１は加圧流体タンク３６３にＣＯ２を供給するＣＯ２供給ラインである。 In the supercritical processing apparatus 3 shown in FIG. 11, for example, CO 2 is stored in a liquid state in the pressurized fluid supply unit 36, and between the pressurized fluid supply line 351 and the pressurized fluid supply unit 36. , for adjusting the supply pressure of the CO 2, for example, a booster pump 362 consisting of such as a syringe pump or a diaphragm pump, the point where the pressurized fluid tank 363 for holding the gas CO 2, which is the pressure adjustment are provided This is different from the supercritical processing apparatus 3 according to the first embodiment. The pressurized fluid tank 363 holds a sufficient amount of gas CO 2 capable of increasing the pressure in the processing container 31 to a pressure higher than the critical pressure of IPA. In the figure, 361 is a CO 2 supply line for supplying a CO 2 pressurized fluid tank 363.
また、制御部４には、温度検出部３２３の温度検出値と圧力検出部３１３の圧力検出値の双方が入力され、処理容器３１内の温度、圧力を監視しながら、ヒーター３２２への給電量や、加圧流体供給ライン３５１の減圧弁３５２の開度を調節することができる。 Further, both the temperature detection value of the temperature detection unit 323 and the pressure detection value of the pressure detection unit 313 are input to the control unit 4, and the power supply amount to the heater 322 is monitored while monitoring the temperature and pressure in the processing container 31. Alternatively, the opening degree of the pressure reducing valve 352 of the pressurized fluid supply line 351 can be adjusted.
そして例えば、予備実験などにより処理容器３１を加熱したときの処理容器３１の温度と、液体ＩＰＡが液盛りされたウエハＷの温度との対応関係を把握しておけば、図１２に示すように、予め設定されたスケジュールに基づいて処理容器３１の温度を上昇させたときのウエハＷ温度の経時変化を把握することができる。そして、ウエハＷ表面に液盛りされた液体ＩＰＡの温度がウエハＷの温度と同様の経時変化を示すとすると、ある時刻におけるＩＰＡの温度の蒸気圧よりも処理容器３１内の圧力を高圧に保つことにより、液体ＩＰＡの沸騰を防ぎつつ、当該液体ＩＰＡを超臨界状態に変化させることができる。 For example, if the correspondence between the temperature of the processing container 31 when the processing container 31 is heated by a preliminary experiment or the like and the temperature of the wafer W on which the liquid IPA is accumulated is grasped, as shown in FIG. Thus, it is possible to grasp the change with time of the wafer W temperature when the temperature of the processing container 31 is raised based on a preset schedule. If the temperature of the liquid IPA accumulated on the surface of the wafer W shows a change with time similar to the temperature of the wafer W, the pressure in the processing chamber 31 is kept higher than the vapor pressure of the temperature of the IPA at a certain time. Thus, the liquid IPA can be changed to a supercritical state while preventing the liquid IPA from boiling.
そこで、本例の超臨界処理装置３は、図１３に示すように、ウエハＷ表面に液盛りされたＩＰＡが液体の状態を保ちながら昇温されるように、減圧弁３５２の開度やヒーター３２２の出力を調整し、液体ＩＰＡを超臨界状態に変化させる。 Therefore, as shown in FIG. 13, the supercritical processing apparatus 3 of this example is configured such that the opening of the pressure reducing valve 352 and the heater are heated so that the IPA accumulated on the surface of the wafer W is heated while maintaining the liquid state. Adjust the output of 322 to change the liquid IPA to the supercritical state.
具体例を挙げて説明すると、ＩＰＡが液盛りされたウエハＷを処理容器３１内に搬入すると、液体ＩＰＡが気化し、処理容器３１内の温度圧力状態は図１３のＡ’点付近の状態となる。このとき、図１４に模式的に示すように、ウエハＷ表面に液盛りされていた液体ＩＰＡ６１が気化し、更にパターン５１の凹部に入り込んでいる液体ＩＰＡ６１が気化し始めるとパターン倒れが発生するおそれが高くなる。 To explain with a specific example, when the wafer W on which IPA is accumulated is carried into the processing container 31, the liquid IPA is vaporized, and the temperature and pressure state in the processing container 31 is the state near the point A 'in FIG. Become. At this time, as schematically shown in FIG. 14, if the liquid IPA 61 accumulated on the surface of the wafer W evaporates and further the liquid IPA 61 entering the concave portion of the pattern 51 starts to evaporate, pattern collapse may occur. Becomes higher.
そこでこのような状態となる前に、図１１に示す加圧流体供給ライン３５１の減圧弁３５２を徐々に開いて、加圧流体タンク３６３から気体ＣＯ２を供給し処理容器３１内の圧力を上昇させる（図１３中のＢ’点）。しかる後、所定の昇温スケジュールに基づき処理容器３１の昇温を開始し、ウエハＷを加熱すると共に減圧弁３５２を更に開いて、ウエハＷ上のＩＰＡが液体で存在できるように、処理容器３１内の温度-圧力状態を調整する。 Therefore, before this state is reached, the pressure reducing valve 352 of the pressurized fluid supply line 351 shown in FIG. 11 is gradually opened to supply the gas CO 2 from the pressurized fluid tank 363 to increase the pressure in the processing container 31. (B 'point in FIG. 13). Thereafter, the temperature rise of the processing vessel 31 is started based on a predetermined temperature raising schedule, the wafer W is heated, and the pressure reducing valve 352 is further opened, so that the IPA on the wafer W can exist in the liquid state. Adjust the temperature-pressure state inside.
このとき処理容器３１内では、ＣＯ２の導入当初の温度-圧力状態においては、図１５に示すようにウエハＷの周囲は気体ＣＯ２６４の高圧雰囲気となっている一方、液体ＩＰＡ６１はウエハＷのパターン５１の凹部内に入り込んだ状態で存在している。この状態で、図１３に示した矢印付きの実線に沿って処理容器３１の温度、圧力を上げていき、ＩＰＡの臨界圧力以上でＣＯ２の臨界圧力以下である６ＭＰａまで昇圧する。なお、本実施形体においては、ＣＯ２を超臨界状態や亜臨界状態（高圧状態)まで加圧してもよい。 At this time, in the temperature-pressure state at the beginning of the introduction of CO 2 , the periphery of the wafer W is a high-pressure atmosphere of gas CO 2 64 in the processing vessel 31, while the liquid IPA 61 is in the wafer W The pattern 51 exists in a state of entering the recess. In this state, the temperature and pressure of the processing container 31 are increased along the solid line with an arrow shown in FIG. 13, and the pressure is increased to 6 MPa which is higher than the critical pressure of IPA and lower than the critical pressure of CO 2 . In the present embodiment, CO 2 may be pressurized to a supercritical state or a subcritical state (high pressure state).
このように、ＣＯ２の臨界圧力よりも低く、ＩＰＡの臨界圧力よりも高い雰囲気を形成することにより、加熱されている液体ＩＰＡ６１の周囲には、当該温度における液体ＩＰＡ６１の蒸気圧よりも高圧の雰囲気が形成される。この結果、ウエハＷ表面の液体ＩＰＡ６１は液相の状態を保ったまま（沸騰することなく）高圧雰囲気下で加熱される。やがて処理容器３１内の温度がＩＰＡの臨界温度以上になると、液体ＩＰＡ６１が、パターン５１の凹部内に入り込んだ状態のまま超臨界ＩＰＡ６３となる（図１６）。 Thus, by forming an atmosphere lower than the critical pressure of CO 2 and higher than the critical pressure of IPA, the liquid IPA 61 being heated has a higher pressure than the vapor pressure of the liquid IPA 61 at that temperature. An atmosphere is formed. As a result, the liquid IPA 61 on the surface of the wafer W is heated in a high-pressure atmosphere while maintaining the liquid phase state (without boiling). Eventually, when the temperature in the processing vessel 31 becomes equal to or higher than the critical temperature of IPA, the liquid IPA 61 becomes supercritical IPA 63 while entering the recess of the pattern 51 (FIG. 16).
このように液体ＩＰＡ６１を高圧の気体ＣＯ２６４と接触させた状態のまま処理容器３０内を昇温することにより、前記凹部内の液体ＩＰＡ６１を直接、超臨界ＩＰＡ６３にすることができる。また加圧用の流体が気体状態のＣＯ２であるため、超臨界状態のＣＯ２に比べパーティクル低減が可能である。 In this way, by raising the temperature in the processing vessel 30 while the liquid IPA 61 is in contact with the high-pressure gas CO 2 64, the liquid IPA 61 in the recess can be directly changed to the supercritical IPA 63. Further, since the fluid for pressurization is CO 2 in a gaseous state, particles can be reduced as compared with CO 2 in a supercritical state.
こうして処理容器３１内に気体ＣＯ２６４を供給すると共に、ウエハＷを加熱し、ウエハＷのパターン５１内の液体ＩＰＡ６１が超臨界ＩＰＡ６３となるのに十分な時間が経過したら、加圧流体供給ライン３５１の開閉弁３５２を閉じる一方、排出ライン３４１の減圧弁３４２を開いて処理容器３１内の流体を排出して、処理容器３１からＣＯ２ガス及びＩＰＡを超臨界状態、または気体の状態で排出することにより、液体ＩＰＡが除去され乾燥したウエハＷを得ることができる（図１７）。 In this way, the gas CO 2 64 is supplied into the processing container 31 and the wafer W is heated. When a sufficient time has passed for the liquid IPA 61 in the pattern 51 of the wafer W to become the supercritical IPA 63, the pressurized fluid supply line While closing the on-off valve 352 of the 351, the pressure reducing valve 342 of the discharge line 341 is opened to discharge the fluid in the processing container 31, and the CO 2 gas and IPA are discharged from the processing container 31 in a supercritical state or in a gaseous state. As a result, the liquid IPA is removed and a dry wafer W can be obtained (FIG. 17).
以上に説明したように、外部から高圧流体を供給することにより処理容器３１内の圧力を調整し、液体ＩＰＡの沸騰を避けつつ当該ＩＰＡを超臨界状態に変化させてウエハＷから除去する技術は、ウエハＷ表面に液盛りされたＩＰＡを除去する例以外にも適用できる。図５に示すように、ウエハトレイ３３１内に載置されたウエハＷを浸漬したＩＰＡを除去する場合にも、本技術を適用してもよい。 As described above, the technique of adjusting the pressure in the processing vessel 31 by supplying a high-pressure fluid from the outside, changing the IPA to a supercritical state while removing the liquid IPA from boiling, and removing it from the wafer W is as follows. Further, the present invention can be applied to an example other than the example in which the IPA accumulated on the surface of the wafer W is removed. As shown in FIG. 5, the present technology may also be applied when removing the IPA in which the wafer W placed in the wafer tray 331 is immersed.
また、処理容器３１内を加圧する手法は、高圧ガスや超臨界流体を供給する場合に限定されるものではない。Ｎ２やＣＯ２の亜臨界流体を供給して加圧してもよい。この他、流体を供給して処理容器３１内を加圧する手法に替えて、例えば処理容器３１をピストン構造とし、ウエハＷを収容した処理容器３１内の空間を圧縮することにより加圧を行ってもよい。 Moreover, the method of pressurizing the inside of the processing container 31 is not limited to the case where high pressure gas or supercritical fluid is supplied. N 2 or CO 2 subcritical fluid may be supplied and pressurized. In addition, instead of the method of supplying a fluid and pressurizing the inside of the processing container 31, for example, the processing container 31 has a piston structure and pressurization is performed by compressing the space in the processing container 31 containing the wafer W. Also good.
更に、乾燥防止用の流体もＩＰＡに限定されるものではなく、メタノールやエタノールなどのアルコール、各種のフッ素系溶媒(フッ化アルコール、ハイドロフルオロエーテルなど)、アセトンなどを用いてもよく、これら乾燥防止用の液体を亜臨界状態としてウエハＷ表面から除去する場合も本発明に含まれる。この他、例えば乾燥防止用の液体が不燃性である場合であっても、乾燥防止用の液体が高圧状態となった後の変質防止などを目的として、不活性ガスによる処理容器３１内のパージを行ってから不燃性の液体で覆われたウエハＷを進入させてもよい。 Further, the drying preventing fluid is not limited to IPA, and alcohols such as methanol and ethanol, various fluorinated solvents (fluorinated alcohols, hydrofluoroethers, etc.), acetone, etc. may be used. The case where the liquid for prevention is removed from the surface of the wafer W in a subcritical state is also included in the present invention. In addition, for example, even if the drying prevention liquid is nonflammable, purging the inside of the processing container 31 with an inert gas for the purpose of preventing deterioration after the drying prevention liquid becomes a high pressure state. After performing the above, the wafer W covered with the nonflammable liquid may be entered.
更にまた、処理容器３１の構造は、図５に示したように耐圧性を備えた容器全体を加熱する場合に限定されない。例えばステンレススチールや炭素鋼、チタン、ハステロイ（登録商標）、インコネル（登録商標）など、耐圧性が高い一方で比較的熱伝導率の低い材料からなる耐圧容器の内側に、アルミニウム、銅、窒化アルミニウム、炭化ケイ素などからなる、耐圧容器よりも熱伝導率の高い材料からなる内部容器を入れ子構造にして設け、この内部容器をヒーター３２２などで加熱してもよい。このとき、これら耐圧容器と内部容器との間に石英やアルミナなどからなる断熱層を設け、内部容器のみを加熱することにより、処理容器３１の熱応答性が向上すると共に、エネルギー消費量も低減できる。 Furthermore, the structure of the processing container 31 is not limited to heating the entire container having pressure resistance as shown in FIG. For example, aluminum, copper, and aluminum nitride are placed inside a pressure vessel made of a material having high pressure resistance but relatively low thermal conductivity, such as stainless steel, carbon steel, titanium, Hastelloy (registered trademark), and Inconel (registered trademark). Alternatively, an inner container made of a material having a higher thermal conductivity than that of the pressure resistant container made of silicon carbide or the like may be provided in a nested structure, and the inner container may be heated by a heater 322 or the like. At this time, by providing a heat insulating layer made of quartz, alumina or the like between the pressure vessel and the inner vessel and heating only the inner vessel, the thermal responsiveness of the processing vessel 31 is improved and the energy consumption is also reduced. it can.
Ｗ ウエハ
１ 洗浄システム
２ 洗浄装置
３ 超臨界処理装置
３１ 処理容器
３２２ ヒーター
３４１ 排出ライン
３５１ 加圧流体供給ライン
４ 制御部
W Wafer 1 Cleaning system 2 Cleaning device 3 Supercritical processing device 31 Processing vessel 322 Heater 341 Discharge line 351 Pressurized fluid supply line 4 Control unit
Claims (15)
次いで、前記基板上の乾燥防止用の液体の温度−圧力状態が、前記乾燥防止用の液体の蒸気圧曲線よりも液相側の領域を通って変化し、超臨界状態または亜臨界状態である高圧状態に達するように、当該処理容器内を外部から加圧しながら基板を加熱し、且つ、前記処理容器内を外部から加圧する圧力と、基板を加熱するために供給する熱との少なくとも一方を変化させ、前記パターンの凹部内に入り込んだ状態のまま前記乾燥防止用の液体を高圧状態とする工程と、
その後、前記処理容器内の流体を高圧状態または気体の状態で排出する工程と、を含むことを特徴とする基板処理方法。 A step of carrying a substrate having a concavo-convex pattern formed on the surface, and an anti-drying liquid covering the pattern so as to enter the concave portion into the processing container;
Then, the temperature of the liquid for preventing drying on the substrate - the pressure state than said vapor pressure curve of the liquid anti-drying varied through the region of the liquid-phase side is in a supercritical state or subcritical state The substrate is heated while pressurizing the inside of the processing container from the outside so as to reach a high pressure state, and at least one of the pressure for pressurizing the inside of the processing container from the outside and the heat supplied to heat the substrate Changing the liquid for preventing drying to be in a high-pressure state while remaining in the recessed portion of the pattern; and
And a step of discharging the fluid in the processing container in a high-pressure state or in a gas state.
この処理容器と外部との間で基板の搬入出を行うための搬入出部と、
前記処理容器の内部を外部から加圧するための加圧部と、
前記処理容器内の基板を加熱するための加熱部と、
前記処理容器内の流体を排出するための排出ラインと、
乾燥防止用の液体が付着した基板を前記処理容器に搬入し、次いで、前記基板上の乾燥防止用の液体の温度−圧力状態が、前記乾燥防止用の液体の蒸気圧曲線よりも液相側の領域を通って変化し、超臨界状態または亜臨界状態である高圧状態に達するように、前記処理容器内を加圧しながら基板を加熱し、且つ、前記処理容器内を外部から加圧する圧力と、基板を加熱するために供給する熱との少なくとも一方を変化させ、前記パターンの凹部内に入り込んだ状態のまま前記乾燥防止用の液体を高圧状態とし、その後、前記処理容器内の流体を高圧状態または気体の状態で排出するように制御信号を出力する制御部と、を備えたことを特徴とする基板処理装置。 A processing container in which a liquid for preventing drying that enters the concave portion from the substrate having a concave and convex pattern formed on the surface and adheres so as to cover the pattern is removed,
A loading / unloading unit for loading / unloading the substrate between the processing container and the outside;
A pressurizing unit for pressurizing the inside of the processing container from the outside;
A heating unit for heating the substrate in the processing container;
A discharge line for discharging the fluid in the processing vessel;
The liquid for preventing drying are attached substrate is carried into the processing vessel, then, the temperature of the liquid anti-drying on the substrate - the pressure conditions, the liquid phase side of the vapor pressure curve of the liquid for the anti-drying The substrate is heated while pressurizing the inside of the processing vessel so as to reach a high pressure state which is a supercritical state or a subcritical state, and the inside of the processing vessel is pressurized from outside. Then, at least one of heat supplied to heat the substrate is changed, the liquid for preventing drying is brought into a high-pressure state while remaining in the concave portion of the pattern, and then the fluid in the processing vessel is pressurized And a control unit that outputs a control signal so as to be discharged in a state or a gas state.
前記プログラムは請求項１ないし７の何れか一つに記載された基板処理方法を実行するためにステップが組まれていることを特徴とする記憶媒体。 A storage medium storing a computer program used in a substrate processing apparatus for removing a liquid for preventing drying that enters a recess from a substrate having a concavo-convex pattern formed on the surface thereof and adheres so as to cover the pattern. ,
A storage medium characterized in that the program has steps for executing the substrate processing method according to any one of claims 1 to 7.
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