JP2003321217A - Method for cleaning container for high purity chlorosilane - Google Patents
Method for cleaning container for high purity chlorosilaneInfo
- Publication number
- JP2003321217A JP2003321217A JP2002128692A JP2002128692A JP2003321217A JP 2003321217 A JP2003321217 A JP 2003321217A JP 2002128692 A JP2002128692 A JP 2002128692A JP 2002128692 A JP2002128692 A JP 2002128692A JP 2003321217 A JP2003321217 A JP 2003321217A
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- Prior art keywords
- container
- cleaning
- silicon tetrachloride
- purity
- liquid
- 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.)
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、多結晶シリコンの
製造原料等に使用される高純度トリクロロシラン又は高
純度四塩化珪素若しくはこれらの混合物を収容する高純
度クロロシラン容器の内面洗浄方法に関する。TECHNICAL FIELD The present invention relates to a method for cleaning the inner surface of a high-purity chlorosilane container containing high-purity trichlorosilane, high-purity silicon tetrachloride, or a mixture thereof used as a raw material for producing polycrystalline silicon.
【０００２】[0002]
【従来の技術】半導体デバイスの素材であるシリコン単
結晶は、シーメンス法により製造された高純度の多結晶
シリコンを原料として主にＣＺ法により製造される。シ
ーメンス法による多結晶シリコンの製造では、周知のと
おり、反応炉内にセットされた多結晶シリコンの芯材を
通電加熱した状態で、反応炉内に高純度のクロロシラン
ガスを水素ガスと共に供給する。これにより芯材の表面
に多結晶シリコンが析出し、ロッド状の多結晶シリコン
が製造される。2. Description of the Related Art A silicon single crystal, which is a material for a semiconductor device, is mainly manufactured by the CZ method using high-purity polycrystalline silicon manufactured by the Siemens method as a raw material. In the production of polycrystalline silicon by the Siemens method, as is well known, high-purity chlorosilane gas is supplied together with hydrogen gas into the reaction furnace while the core material of the polycrystalline silicon set in the reaction furnace is electrically heated. As a result, polycrystalline silicon is deposited on the surface of the core material, and rod-shaped polycrystalline silicon is manufactured.
【０００３】シーメンス法による多結晶シリコンの製造
に使用されるクロロシラン類としては、トリクロロシラ
ン、四塩化珪素或いはこれらの混合物などがある。トリ
クロロシラン、四塩化珪素は、大気圧における各沸点が
約３２℃、約５７℃であるため、常温下では液体で存在
し、これらの液体は専用の容器に収容されて保管され、
また運搬される。Chlorosilanes used in the production of polycrystalline silicon by the Siemens method include trichlorosilane, silicon tetrachloride, and mixtures thereof. Since trichlorosilane and silicon tetrachloride have respective boiling points at atmospheric pressure of about 32 ° C. and about 57 ° C., they exist as liquids at room temperature, and these liquids are stored and stored in a dedicated container.
Also transported.
【０００４】多結晶シリコンの製造に使用されるクロロ
シランは高純度であることが必要であるため、これを収
容する容器についても内部が清浄なことが要求される。
このため、容器を新しく製造した場合や容器のオーバー
ホールを実施した後には、容器内が洗浄される。そし
て、その洗浄方法としては、容器内面に付着する汚染物
質を純水で洗い流し、容器内を乾燥後、更にその容器内
にクロロシラン液を入れ、容器内面に残留する汚染物質
を洗い流すことが行われている。純水洗浄後にクロロシ
ラン液による再洗浄を行うのは、純水洗浄だけでは初期
汚染が残ることが確認されているからである。Since chlorosilane used for producing polycrystalline silicon needs to have a high purity, the inside of the container for storing it is also required to be clean.
Therefore, the inside of the container is cleaned when the container is newly manufactured or after the container is overhauled. Then, as a cleaning method, the contaminants adhering to the inner surface of the container are washed away with pure water, the inside of the container is dried, and then a chlorosilane solution is further put in the container to wash away the remaining contaminants on the inner surface of the container. ing. The reason why the cleaning with the chlorosilane solution is performed again after the pure water cleaning is that it is confirmed that the initial contamination remains only by the pure water cleaning.
【０００５】ちなみに、高純度とは、そのトリクロロシ
ランを用いて水素還元により析出させた多結晶シリコン
を単結晶化したとき、電気抵抗比でＮ型５００Ω・ｃｍ
以上が得られ、且つ、単結晶中のリン濃度で０．４ｐｐ
ｂｗ以下、ボロン濃度で０．１ｐｐｂｗ以下が得られる
品質をいう。Incidentally, high purity means that when polycrystal silicon deposited by hydrogen reduction using the trichlorosilane is monocrystallized, the electrical resistance ratio is N type 500 Ω · cm.
The above was obtained, and the phosphorus concentration in the single crystal was 0.4 pp.
bw or less, it means the quality that can obtain a boron concentration of 0.1 ppbw or less.
【０００６】[0006]
【発明が解決しようとする課題】従来の高純度クロロシ
ラン容器の内面洗浄方法では、容器内を洗浄液で満杯に
するため、多量の洗浄用クロロシラン液が必要になる。
洗浄に使用された後のクロロシラン液は不純物を多く含
んでいるので、そのままでは多結晶シリコンの製造原料
等に使用することができず、洗浄後に容器から取り出す
必要がある。このため、洗浄に使用するクロロシラン液
が多くなるほどコスト面に悪影響が及ぶことになり、こ
の観点から洗浄に使用する液量を少なくすることが求め
られる。In the conventional method for cleaning the inner surface of a high-purity chlorosilane container, a large amount of cleaning chlorosilane liquid is required to fill the container with the cleaning liquid.
Since the chlorosilane solution used for cleaning contains a large amount of impurities, it cannot be used as it is as a raw material for producing polycrystalline silicon, etc., and must be taken out of the container after cleaning. Therefore, as the amount of chlorosilane liquid used for cleaning increases, the cost is adversely affected, and from this viewpoint, it is required to reduce the amount of liquid used for cleaning.
【０００７】しかしながら、現状の洗浄方法では、クロ
ロシラン液の液量を少なくすると、内面全体の洗浄がで
きなくなる。容器が比較的小さい場合は、液量が少なく
ても容器を揺らすことによって内面全体の洗浄が可能に
なるが、容器が大きい場合は容器を揺らすことが困難で
あり、仮に揺らすことができても設備が大掛かりにな
る。容器の蓋を開放して容器内面に洗浄液を散布するこ
とも考えられるが、クロロシラン類は大気中の水分と容
易に反応し、塩化水素ガスを生じるため、開放での洗浄
は現実的でない。However, in the current cleaning method, if the amount of the chlorosilane liquid is reduced, the entire inner surface cannot be cleaned. If the container is relatively small, it is possible to clean the entire inner surface by shaking the container even if the amount of liquid is small.However, if the container is large, it is difficult to shake the container, and even if it can be shaken. The equipment becomes large-scale. Although it is possible to open the lid of the container and spray the cleaning liquid on the inner surface of the container, chlorosilanes easily react with moisture in the atmosphere to generate hydrogen chloride gas, and therefore, cleaning in an open state is not practical.
【０００８】対象物は異なるが、処理槽内で洗浄用有機
溶剤を蒸発させ、その蒸気を処理槽内の対象物の表面で
凝縮させる蒸気洗浄方法は、例えば特開２０００−１７
８７７６号公報及び特開２００１−１９１０３９号公報
等に開示されている。この蒸気洗浄方法を高純度クロロ
シラン容器の内面洗浄に適用した場合、容器内面に残る
有機溶剤が汚染物質になるという致命的な問題が発生す
る。加えて、これらの蒸気洗浄方法は、電気部品、機械
部品、工具等の小さな対象物の外面洗浄に対しては有効
であるが、本発明が対象とするクロロシラン容器のよう
な大型対象物の、しかも内面洗浄に対しては、非常に大
きな処理槽が必要となる上、洗浄効果も十分とは言えな
い。なぜなら、処理槽内の容器の外面には十分な量の蒸
気を接触させることができるが、通ガス性の悪い容器の
内部に十分な量の蒸気を供給することが難しいからであ
る。Although the object is different, a vapor cleaning method in which the organic solvent for cleaning is evaporated in the processing tank and the vapor is condensed on the surface of the object in the processing tank is disclosed, for example, in Japanese Patent Laid-Open No. 2000-17
No. 8776 and Japanese Patent Application Laid-Open No. 2001-191039. When this vapor cleaning method is applied to the inner surface cleaning of a high-purity chlorosilane container, there is a fatal problem that the organic solvent remaining on the inner surface of the container becomes a contaminant. In addition, these vapor cleaning methods are effective for cleaning the outer surfaces of small objects such as electric parts, mechanical parts, and tools, but large objects such as chlorosilane containers targeted by the present invention, Moreover, for cleaning the inner surface, a very large processing tank is required, and the cleaning effect is not sufficient. This is because a sufficient amount of steam can be brought into contact with the outer surface of the container in the processing tank, but it is difficult to supply a sufficient amount of steam to the inside of the container having poor gas permeability.
【０００９】本発明の目的は、僅かな液量と簡単な設備
で容器内面を経済性よく効果的に洗浄できる高純度クロ
ロシラン容器洗浄方法を提供することにある。An object of the present invention is to provide a method for cleaning a high-purity chlorosilane container which is capable of economically and effectively cleaning the inner surface of the container with a small amount of liquid and simple equipment.
【００１０】[0010]
【課題を解決するための手段】上記目的を達成するため
に、本発明の高純度クロロシラン容器洗浄方法は、高純
度トリクロロシラン又は高純度四塩化珪素若しくはこれ
らの混合物を収容する容器の内面を洗浄するに当たり、
高純度トリクロロシラン又は高純度四塩化珪素若しくは
これらの混合物を洗浄液として、その蒸気を前記容器の
内面で凝集させ、凝集液を容器から排出することを技術
的特徴点としている。In order to achieve the above object, a method for cleaning a high-purity chlorosilane container according to the present invention is to clean the inner surface of a container containing high-purity trichlorosilane, high-purity silicon tetrachloride, or a mixture thereof. In doing
A technical feature is that high-purity trichlorosilane, high-purity silicon tetrachloride, or a mixture thereof is used as a cleaning liquid, the vapor thereof is aggregated on the inner surface of the container, and the aggregated liquid is discharged from the container.
【００１１】洗浄液の蒸気は容器の外から内部へ導入す
ることも可能であるが、効率的には、洗浄液を容器内に
少量入れ、容器下部を加熱し、容器上部を冷却すること
により、容器内で洗浄液の蒸気を発生させ、且つ、その
蒸気を容器の内面で凝集させるのが好ましい。The vapor of the cleaning liquid can be introduced from the outside to the inside of the container. However, efficiently, a small amount of the cleaning liquid is put in the container, the lower part of the container is heated and the upper part of the container is cooled. It is preferable to generate the vapor of the cleaning liquid inside and to agglomerate the vapor on the inner surface of the container.
【００１２】本発明の高純度クロロシラン容器洗浄方法
では、洗浄液の蒸気が容器の内面に接触し冷却され凝縮
して液体になる。その液体は重力により上から下へ容器
内面を伝って流下する。このとき、容器内面の汚染物が
流下する液体中に取り込まれ、容器底部に溜まる。容器
底部に溜まった液体を排出すれば、少量の洗浄液で容器
内面が洗浄されることになる。In the high-purity chlorosilane container cleaning method of the present invention, the vapor of the cleaning liquid comes into contact with the inner surface of the container and is cooled and condensed to become a liquid. The liquid flows down along the inner surface of the container due to gravity. At this time, the contaminants on the inner surface of the container are taken into the flowing liquid and collected at the bottom of the container. When the liquid accumulated at the bottom of the container is discharged, the inner surface of the container is cleaned with a small amount of cleaning liquid.
【００１３】このように、本発明の高純度クロロシラン
容器洗浄方法では、容器自体が蒸気洗浄における処理槽
として利用されることにより、僅かの洗浄液により、格
別の設備なしに大量の蒸気が容器内面に供給される。し
かも、容器収容物が蒸気洗浄における洗浄液として使用
されることにより、洗浄液による二次汚染の問題が解決
される。また、容器収容物であるトリクロロシラン、四
塩化珪素の大気圧下における各沸点はそれぞれ約３２
℃、約５７℃と室温より若干高い程度であるため、容器
の底部をスチーム加熱する程度で簡単に蒸発させること
ができ、凝集についても容器外面を外気に曝して放冷す
るだけ、或いは容器外面に水をかけるだけで可能であ
り、いずれも簡単に実施できる。これらのため、僅かな
液量と簡単な設備で容器内面を経済性よく効果的に洗浄
することが可能となる。As described above, in the high-purity chlorosilane container cleaning method of the present invention, since the container itself is used as the processing tank in the steam cleaning, a large amount of steam can be transferred to the inner surface of the container without any special equipment with a slight cleaning liquid. Supplied. Moreover, since the container contents are used as the cleaning liquid in the steam cleaning, the problem of secondary contamination due to the cleaning liquid is solved. Further, the boiling points of trichlorosilane and silicon tetrachloride contained in the container are about 32 at atmospheric pressure.
℃, about 57 ℃, which is slightly higher than room temperature, so it can be evaporated easily by heating the bottom of the container with steam, and even for aggregation, just expose the container outer surface to the outside air and let it cool, or It can be done simply by sprinkling water on it. For these reasons, it becomes possible to economically and effectively clean the inner surface of the container with a small amount of liquid and simple equipment.
【００１４】洗浄液としては、容器に充填される液体の
種類に関係なく、高純度トリクロロシラン又は高純度四
塩化珪素若しくはこれらの混合物のいずれを使用しても
よい。高純度トリクロロシラン、高純度四塩化珪素、こ
れらの混合物のいずれも高純度に精製されているため、
いずれを使用しても金属不純物やリン、ボロンに対する
洗浄効果は同等である。As the cleaning liquid, high-purity trichlorosilane, high-purity silicon tetrachloride, or a mixture thereof may be used regardless of the kind of liquid filled in the container. Since high-purity trichlorosilane, high-purity silicon tetrachloride, and mixtures of these have been purified to high purity,
Whichever is used, the cleaning effect on metal impurities, phosphorus and boron is the same.
【００１５】しかし、高純度トリクロロシランの製品
（出荷品）には四塩化珪素の混入濃度に許容範囲があ
り、高純度四塩化珪素の製品（出荷品）にはトリクロロ
シランの混入濃度に許容範囲がある。このため、例えば
トリクロロシランの容器を四塩化珪素で洗浄すると、僅
かではあるが洗浄後に容器内に残った四塩化珪素が、充
填物であるトリクロロシラン中の四塩化珪素濃度を上昇
させてしまう。従って、容器に充填される液体と同じも
のを洗浄液として使用することが望まれる。However, the product (shipment product) of high-purity trichlorosilane has a permissible concentration range of silicon tetrachloride, and the product (shipment product) of high-purity silicon tetrachloride has a permissible concentration range of trichlorosilane. There is. For this reason, for example, when a container of trichlorosilane is washed with silicon tetrachloride, the silicon tetrachloride remaining in the container after the cleaning, although a little, raises the concentration of silicon tetrachloride in the filling material, trichlorosilane. Therefore, it is desirable to use the same liquid as the liquid filled in the container as the cleaning liquid.
【００１６】[0016]
【発明の実施の形態】以下に本発明の実施形態を図面に
基づいて説明する。図１は本発明の一実施形態を示す高
純度クロロシラン容器洗浄方法の工程図である。BEST MODE FOR CARRYING OUT THE INVENTION Embodiments of the present invention will be described below with reference to the drawings. FIG. 1 is a process diagram of a high-purity chlorosilane container cleaning method showing an embodiment of the present invention.
【００１７】本実施形態では、高純度四塩化珪素を収容
する容器のオーバーホール後の内面洗浄が、洗浄液とし
て高純度四塩化珪素を用いて実施される。In the present embodiment, the cleaning of the inner surface of the container containing the high-purity silicon tetrachloride after overhaul is carried out using high-purity silicon tetrachloride as the cleaning liquid.
【００１８】容器をオーバーホールした後、容器内を純
水洗浄する。容器内を乾燥後Ａｒ，Ｎ2 などの不活性ガ
スで置換する。そして、図１（ａ）に示すように、容器
容積で１／１０量程度の四塩化珪素２０を容器１０内に
洗浄液として入れる。ここで使用される四塩化珪素２０
は、容器１０に充填される内容物と同じ高純度四塩化珪
素である。また、洗浄液量は、容器容積の１／１００〜
１／２が好ましい。１／１００未満の場合は洗浄効果が
不足し、１／２を超える場合は、効果が飽和し、経済性
が悪化する。After the container is overhauled, the inside of the container is washed with pure water. After drying the inside of the container, it is replaced with an inert gas such as Ar or N 2 . Then, as shown in FIG. 1A, about 1/10 of the volume of the container is filled with silicon tetrachloride 20 as a cleaning liquid. Silicon tetrachloride used here 20
Is the same high-purity silicon tetrachloride as the content filled in the container 10. In addition, the amount of cleaning liquid is 1/100 to the container volume.
1/2 is preferable. If it is less than 1/100, the cleaning effect is insufficient, and if it exceeds 1/2, the effect is saturated and the economical efficiency is deteriorated.
【００１９】容器１０の内底面は、残液が底面中心部に
溜まるように、中心へ向けて下降傾斜を付与したすり鉢
形状になっている。１１は容器１０内への液体の出し入
れのために、容器１０内に深く挿入された液管であり、
その先端は容器内底面の最も低い中心部に僅かの距離を
残して対向している。また、１２は容器１０内の気体の
出し入れのために容器１０内に浅く挿入されたガス管で
ある。The inner bottom surface of the container 10 is shaped like a mortar with a downward inclination toward the center so that the residual liquid collects in the center of the bottom surface. Reference numeral 11 denotes a liquid pipe that is deeply inserted into the container 10 in order to take the liquid in and out of the container 10.
Its tip faces the lowest central portion of the bottom surface of the container with a slight distance. Further, reference numeral 12 is a gas pipe that is shallowly inserted into the container 10 for taking in and out the gas in the container 10.
【００２０】容器１０内への洗浄液の導入が終わると、
図１（ｂ）に示すように、容器１０の外面を大気に接触
させた状態で、容器１０の下部をスチームの吹き付けに
より加熱して、内部の四塩化珪素２０を蒸発させる。こ
のとき、容器１０の上部に設けられたガス管を開放して
おき、容器１０の内部に充填されていたイナートガス及
び四塩化珪素の蒸気の一部を外部へ排出する。排出ガス
は外部の中和装置により処理する。When the cleaning liquid has been introduced into the container 10,
As shown in FIG. 1B, with the outer surface of the container 10 in contact with the atmosphere, the lower portion of the container 10 is heated by spraying steam to evaporate the silicon tetrachloride 20 inside. At this time, the gas pipe provided in the upper part of the container 10 is opened, and a part of the inert gas and the vapor of silicon tetrachloride filled in the container 10 is discharged to the outside. The exhaust gas is processed by an external neutralizer.
【００２１】容器１０の下部の加熱を開始してから例え
ば１時間後にその加熱を停止する。容器１０の下部を加
熱する間、容器１０内で発生した四塩化珪素の蒸気は容
器１０の内面に接触する。容器１０の下部を除く部分は
放冷により冷却されている。このため、容器１０の内面
に接触した蒸気が凝縮し、四塩化珪素の液体に戻る。液
体に戻った四塩化珪素は、容器１０の内面に沿って流下
し、底部に戻る。底部に戻った四塩化珪素２０は再度蒸
発する。このサイクルが繰り返されることにより、容器
１０の内面は、流下する四塩化珪素の液体によって洗浄
され、汚染物質が除去される。The heating of the lower portion of the container 10 is stopped, for example, 1 hour after the heating is started. While heating the lower portion of the container 10, the vapor of silicon tetrachloride generated in the container 10 contacts the inner surface of the container 10. The part of the container 10 excluding the lower part is cooled by cooling. Therefore, the vapor contacting the inner surface of the container 10 is condensed and returns to the liquid of silicon tetrachloride. The silicon tetrachloride that has returned to the liquid flows down along the inner surface of the container 10 and returns to the bottom. The silicon tetrachloride 20 returned to the bottom is evaporated again. By repeating this cycle, the inner surface of the container 10 is washed with the liquid of silicon tetrachloride flowing down to remove contaminants.
【００２２】容器１０の下部を加熱する時間（蒸気洗浄
時間）は、容器１０の内表面積１ｍ 2 当たり５〜３００
分が好ましい。これが５分未満だと洗浄効果が小さく、
３００分を超えると、逆に洗浄効果が小さくなり、経済
性が悪化する。Time for heating the lower part of the container 10 (steam cleaning
Time) is the inner surface area of the container 1m 25 to 300
Minutes are preferred. If this is less than 5 minutes, the cleaning effect is small,
If it exceeds 300 minutes, the cleaning effect will decrease and the economy
Sex deteriorates.
【００２３】容器１０の冷却中は、ガス管１２から容器
１０内にアルゴン、窒素等の不活性ガスを導入して、容
器１０内が大気圧より低い負圧になることを防止する。
そして、冷却後、図１（ｃ）に示すように、容器１０内
をアルゴン、窒素等の不活性ガスで０．１ＭＰａＧ程度
に加圧する。これにより、容器１０の底部に溜まってい
る四塩化珪素２０を液管１１から容器１０の外へ排出す
る。During the cooling of the container 10, an inert gas such as argon or nitrogen is introduced into the container 10 through the gas pipe 12 to prevent the inside of the container 10 from having a negative pressure lower than the atmospheric pressure.
Then, after cooling, as shown in FIG. 1C, the inside of the container 10 is pressurized to about 0.1 MPaG with an inert gas such as argon or nitrogen. As a result, the silicon tetrachloride 20 accumulated at the bottom of the container 10 is discharged from the liquid pipe 11 to the outside of the container 10.
【００２４】このようにして容器１０の内面洗浄を終え
た後、その容器１０内に収容物として四塩化珪素を充填
する。After the inner surface of the container 10 has been cleaned in this manner, the container 10 is filled with silicon tetrachloride as a contained item.
【００２５】本発明の実施例として、上記方法により、
高純度四塩化珪素容器のオーバーホール後の内面洗浄を
実施した。容器に充填する前の四塩化珪素中の不純物濃
度と、洗浄後の容器に充填した後の四塩化珪素中の不純
物濃度とを、半導体で重要視されるリン、ボロンについ
て調査した。結果を表１に示す。調査は、それぞれの四
塩化珪素を用いて小型の水素還元炉により多結晶シリコ
ンを製造し、製造された多結晶シリコンを用いて製造し
た単結晶のサンプルをフォトルミネッセンス法によって
分析することにより行った。As an embodiment of the present invention, by the above method,
The inner surface of the high-purity silicon tetrachloride container was cleaned after overhaul. The impurity concentration in silicon tetrachloride before filling the container and the impurity concentration in silicon tetrachloride after filling the container after cleaning were investigated for phosphorus and boron, which are important in semiconductors. The results are shown in Table 1. The investigation was carried out by producing polycrystalline silicon using a small hydrogen reduction furnace using each silicon tetrachloride, and analyzing a single crystal sample produced using the produced polycrystalline silicon by a photoluminescence method. .
【００２６】[0026]
【表１】 [Table 1]
【００２７】表１から分かるように、容器に充填する前
の四塩化珪素と、容器に充填した後の四塩化珪素との間
に、不純物濃度の差はなく、容器の内面洗浄が完全であ
ることが確認された。As can be seen from Table 1, there is no difference in the impurity concentration between the silicon tetrachloride before being filled in the container and the silicon tetrachloride after being filled in the container, and the inner surface of the container is completely cleaned. It was confirmed.
【００２８】比較例として以下の洗浄を実施し、上記実
施例のときと同様に、洗浄後の容器に充填した後の四塩
化珪素中の不純物濃度を調査した。結果を表２に示す。As a comparative example, the following cleaning was carried out, and the impurity concentration in silicon tetrachloride after filling the container after cleaning was examined in the same manner as in the above-mentioned example. The results are shown in Table 2.
【００２９】（１）オーバーホール後の容器を純水洗浄
し、容器内を乾燥し、不活性ガスにより置換した後、高
純度四塩化珪素による内面洗浄を行わずに、収容物であ
る高純度四塩化珪素を容器内に充填した。
（２）オーバーホール後の容器を純水洗浄し、容器内を
乾燥し、不活性ガスにより置換した後、容器容積で１／
１０量の高純度四塩化珪素を容器内に洗浄液として入
れ、蒸気洗浄を行うことなくその高純度四塩化珪素を容
器外へ排出した。その後、収容物である高純度四塩化珪
素を容器内に充填した。
（３）オーバーホール後の容器を純水洗浄し、容器内を
乾燥し、不活性ガスにより置換した後、洗浄液としての
高純度四塩化珪素により、容器内を満杯にし、その高純
度四塩化珪素を容器外へ排出した。その後、収容物であ
る高純度四塩化珪素を容器内に充填した。(1) After the overhaul, the container was washed with pure water, the inside of the container was dried, and the inside of the container was replaced with an inert gas. The container was filled with silicon chloride. (2) After the overhaul, the container is washed with pure water, the inside of the container is dried, and the atmosphere is replaced with an inert gas.
10 volumes of high-purity silicon tetrachloride was put into the container as a cleaning liquid, and the high-purity silicon tetrachloride was discharged out of the container without performing steam cleaning. Then, the container was filled with high-purity silicon tetrachloride, which is the contained material. (3) After the overhaul, the container is washed with pure water, the inside of the container is dried, and the container is replaced with an inert gas. Then, the inside of the container is filled with high-purity silicon tetrachloride as a cleaning liquid, and the high-purity silicon tetrachloride It was discharged to the outside of the container. Then, the container was filled with high-purity silicon tetrachloride, which is the contained material.
【００３０】[0030]
【表２】 [Table 2]
【００３１】表２から分かるように、本発明の実施例に
よると、１／１０量の高純度四塩化珪素を使用するにも
かかわらず、容器内を高純度四塩化珪素で満杯にしたと
きと同等の洗浄効果を得ることができる。As can be seen from Table 2, according to the examples of the present invention, the case where the container was filled with high-purity silicon tetrachloride despite the use of 1/10 amount of high-purity silicon tetrachloride was used. The same cleaning effect can be obtained.
【００３２】[0032]
【発明の効果】以上に説明したとおり、本発明の高純度
クロロシラン容器洗浄方法は、高純度トリクロロシラン
又は高純度四塩化珪素若しくはこれらの混合物を収容す
る容器の内面を洗浄するに当たり、高純度トリクロロシ
ラン又は高純度四塩化珪素若しくはこれらの混合物を洗
浄液として、その蒸気を前記容器の内面で凝集させ、凝
集液を容器から排出することことにより、容器自体を蒸
気洗浄における処理槽として利用でき、且つ、容器収容
物を蒸気洗浄における洗浄液として使用できるので、僅
かな液量と簡単な設備で容器内面を経済性よく効果的に
洗浄することができる。As described above, the method for cleaning a high-purity chlorosilane container of the present invention is a method for cleaning a high-purity trichlorosilane, a high-purity silicon tetrachloride, or a mixture thereof in order to clean a high-purity chlorosilane container. Chlorosilane or high-purity silicon tetrachloride or a mixture thereof is used as a cleaning liquid, the vapor is aggregated on the inner surface of the container, and the aggregated liquid is discharged from the container, so that the container itself can be used as a treatment tank in vapor cleaning, and Since the container contents can be used as a cleaning liquid in the steam cleaning, the inner surface of the container can be economically and effectively cleaned with a small amount of liquid and simple equipment.
【図１】本発明の一実施形態を示す高純度クロロシラン
容器洗浄方法の工程説明図である。FIG. 1 is a process explanatory diagram of a high-purity chlorosilane container cleaning method showing an embodiment of the present invention.
１０ 容器 ２０ 四塩化珪素（洗浄液） 10 containers 20 Silicon tetrachloride (cleaning liquid)
Claims (3)
化珪素若しくはこれらの混合物を収容する容器の内面を
洗浄するに当たり、高純度トリクロロシラン又は高純度
四塩化珪素若しくはこれらの混合物を洗浄液として、そ
の蒸気を前記容器の内面で凝集させ、凝集液を容器から
排出することを特徴とする高純度クロロシラン容器洗浄
方法。1. When cleaning the inner surface of a container containing high-purity trichlorosilane or high-purity silicon tetrachloride or a mixture thereof, the high-purity trichlorosilane, high-purity silicon tetrachloride or a mixture thereof is used as a cleaning liquid, and its vapor is used. Is condensed on the inner surface of the container, and the aggregated liquid is discharged from the container.
部を加熱し、容器上部を冷却することにより、容器内で
洗浄液の蒸気を発生させ、且つ、その蒸気を容器の内面
で凝集させる請求項１に記載の高純度クロロシラン容器
洗浄方法。2. A small amount of the cleaning liquid is put in a container, a lower part of the container is heated, and an upper part of the container is cooled to generate vapor of the cleaning liquid in the container, and the vapor is condensed on the inner surface of the container. Item 1. A high-purity chlorosilane container cleaning method according to Item 1.
じ種類である請求項１に記載の高純度クロロシラン容器
洗浄方法。3. The high-purity chlorosilane container cleaning method according to claim 1, wherein the cleaning liquid is of the same type as the liquid filled in the container.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002128692A JP3952281B2 (en) | 2002-04-30 | 2002-04-30 | High purity chlorosilane container cleaning method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002128692A JP3952281B2 (en) | 2002-04-30 | 2002-04-30 | High purity chlorosilane container cleaning method |
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| Publication Number | Publication Date |
|---|---|
| JP2003321217A true JP2003321217A (en) | 2003-11-11 |
| JP3952281B2 JP3952281B2 (en) | 2007-08-01 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2020164348A (en) * | 2019-03-28 | 2020-10-08 | 三菱マテリアル株式会社 | Method for producing high-purity polycrystalline silicon |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2020164348A (en) * | 2019-03-28 | 2020-10-08 | 三菱マテリアル株式会社 | Method for producing high-purity polycrystalline silicon |
| JP7165304B2 (en) | 2019-03-28 | 2022-11-04 | 三菱マテリアル株式会社 | Method for producing high-purity polycrystalline silicon |
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| Publication number | Publication date |
|---|---|
| JP3952281B2 (en) | 2007-08-01 |
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