JP3797775B2 - Wet cleaning device for electronic material and processing method for cleaning liquid for electronic material - Google Patents
Wet cleaning device for electronic material and processing method for cleaning liquid for electronic material Download PDFInfo
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- JP3797775B2 JP3797775B2 JP34143097A JP34143097A JP3797775B2 JP 3797775 B2 JP3797775 B2 JP 3797775B2 JP 34143097 A JP34143097 A JP 34143097A JP 34143097 A JP34143097 A JP 34143097A JP 3797775 B2 JP3797775 B2 JP 3797775B2
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Description
【０００１】
【発明の属する技術分野】
本発明は、電子材料用ウェット洗浄装置に関する。さらに詳しくは、本発明は、半導体用シリコン基板、液晶用ガラス基板などの電子材料の表面を清浄化するための電子材料用ウェット洗浄装置に関する。
【０００２】
【従来の技術】
電子材料用の洗浄液としては、過酸化水素をベースとするＲＣＡ洗浄液をはじめ、超純水自体や、酸、アルカリ、酸化剤、還元剤などを溶解し、pHや酸化還元電位を調整した超純水などが使用されている。バッチ式のウェット洗浄方式において、洗浄液の消費量を低減するために、洗浄槽から洗浄液をポンプにより引き抜き、フィルターによるろ過を経て再度洗浄槽に供給する循環システムが採用されている。近年、イオン交換機能を有する膜モジュールにより、洗浄液中の金属不純物も除去することができるようになり、循環システムの採用はますます広がっている。
電子材料用の洗浄液を用いて電子材料を洗浄するとき、気体が洗浄液に溶解する場合がある。特に、洗浄液が循環して使用される系においては、加圧又は減圧の状態が多かれ少なかれ生じ、洗浄液中に気泡が発生しやすい。また、洗浄液の成分が分解してガス化するものでは気泡が発生しやすい。例えば、過酸化水素を含有する洗浄液では、過酸化水素が自己分解して酸素となり、気泡が発生しやすくなる。
洗浄液中に気泡が発生すると、微細な気泡が被洗浄物である電子材料の表面に付着し、気泡の表面に集合する異物で被洗浄物を汚染してしまうという問題がある。特に、フッ化水素酸を含む洗浄液の場合は、洗浄された固体表面が疎水性になって、気泡が固体表面に付着しやすくなり、固体表面を再汚染することになりやすい。
【０００３】
【発明が解決しようとする課題】
本発明は、半導体用シリコン基板、液晶用ガラス基板などの電子材料の表面を清浄化するための電子材料用ウェット洗浄工程において、洗浄槽における気泡の発生を皆無にすることができる電子材料用ウェット洗浄装置を提供することを目的としてなされたものである。
【０００４】
【課題を解決するための手段】
本発明者らは、上記の課題を解決すべく鋭意研究を重ねた結果、洗浄槽と洗浄槽の液を引き抜いて再度洗浄槽に戻す洗浄液循環ラインとを有する電子材料用ウェット洗浄装置において、洗浄液循環ラインに脱気装置を設けて、洗浄液中に溶解している気体の量を大気圧における飽和度以下とすることにより、洗浄槽における気泡の発生を防止することが可能となることを見いだし、この知見に基づいて本発明を完成するに至った。
すなわち、本発明は、
（１）洗浄液として、過酸化水素を溶解した超純水、塩酸と過酸化水素を溶解した超純水、硫酸と過酸化水素を溶解した超純水、フッ化水素酸と過酸化水素を溶解した超純水、アンモニアと過酸化水素を溶解した超純水又はフッ化水素酸水溶液を用いる電子材料用ウェット洗浄装置であって、洗浄槽と、洗浄槽より洗浄液を引き抜いて再度洗浄槽に返送する洗浄液循環ラインとを有する電子材料用ウェット洗浄装置において、洗浄循環ラインに溶解した気体を除去するための気体透過膜モジュールと減圧系からなる脱気装置と、更に浄化装置を該脱気装置の下流側に設けたことにより洗浄槽内の微細な気泡の発生を抑制したことを特徴とする電子材料用ウェット洗浄装置、
（２）前記浄化装置がフィルター、イオン交換機能を有するフィルター、イオン交換器、又は紫外線照射装置を備えてなることを特徴とする第１項記載の電子材料用ウェット洗浄装置、
（３）前記脱気装置が、洗浄液中の気体から大気圧における飽和度を超えない濃度まで前記気体を脱気する脱気装置である第１項又は第２項記載の電子材料用ウェット洗浄装置、
（４）洗浄液として、過酸化水素を溶解した超純水、塩酸と過酸化水素を溶解した超純水、硫酸と過酸化水素を溶解した超純水、フッ化水素酸と過酸化水素を溶解した超純水、アンモニアと過酸化水素を溶解した超純水又はフッ化水素酸水溶液を用いる電子材料用ウェット洗浄方法であって、洗浄槽より引き抜いた洗浄液を、気体透過膜モジュールと減圧系からなる脱気装置により溶解した気体を脱気したのち、更に浄化して再度洗浄槽に返送することにより、洗浄槽内の微細な気泡の発生を抑制したことを特徴とする電子材料用洗浄液の処理方法、及び、
（５）洗浄液中の気体の飽和度を大気圧における飽和度を超えない濃度まで脱気することを特徴とする第４項に記載の電子材料用洗浄液の処理方法、
を提供するものである。
【０００５】
【発明の実施の形態】
本発明の電子材料用ウェット洗浄装置は、洗浄槽と、洗浄槽より洗浄液を引き抜いて再度洗浄槽に返送する洗浄液循環ラインとを有し、さらに洗浄液循環ラインに脱気装置が設けられてなるものである。
本発明装置に用いる洗浄液には特に制限はなく、例えば、過酸化水素を溶解した超純水、塩酸と過酸化水素を溶解した超純水、硫酸と過酸化水素を溶解した超純水、フッ化水素酸と過酸化水素を溶解した超純水、アンモニアと過酸化水素を溶解した超純水、フッ化水素酸水溶液などを挙げることができる。
本発明装置の洗浄液循環ラインに設ける脱気装置には特に制限はなく、例えば、気相を減圧状態にした減圧タンクを設けることができ、あるいは、気体透過膜モジュールを設けることもできる。気体透過膜モジュールは、膜の一方の側に循環している洗浄液を通液し、膜の他方の側を真空ポンプで吸引して減圧とし、洗浄液中の気体を膜の液相側から気相側に透過させて分離するものである。脱気装置としては、気体透過膜モジュールと減圧系の組み合わせを好適に使用することができる。気体透過膜モジュールは、洗浄液中に含まれる薬品に対して耐久性を有するものであることが好ましい。
【０００６】
気体透過膜モジュールは、循環ポンプの吐き出し側に設置することが好ましい。気体透過膜モジュールの気相部を減圧することにより、薬液に大気圧における飽和度以上に溶解した気体成分、例えば、過酸化水素の分解により生成した酸素などを除去することができる。気相部を過度に減圧にすると、洗浄液中の薬剤の分解が促進される場合がある。洗浄液中の気体は、大気圧における飽和度を超えない濃度まで脱気されれば、洗浄槽において気泡を発生することがないので、大気圧における飽和度以下まで溶存気体を減らす程度の脱気にとどめることが好ましい。なお、洗浄液中の気体の飽和度とは、水中に溶解している気体の量を、大気圧、常温における気体の溶解量で除した値である。例えば、圧力１０5Ｐａ、温度２０℃で空気と接して平衡状態にある水は、窒素１５.４mg／リットル及び酸素８.８mg／リットルを溶解して飽和度１.０倍の状態となっているので、脱気により気体の溶解量を窒素１２.３mg／リットル、酸素７.０mg／リットルとした水の飽和度は、０.８倍である。洗浄液中の気体の飽和度を０.８倍程度とすることにより、洗浄槽における気泡の発生を確実に防止することができる。
本発明装置においては、洗浄液循環ラインに、洗浄液の浄化装置を設けることが好ましい。洗浄液の浄化装置には特に制限はなく、洗浄液中に含まれる汚染物に応じて適宜選択することができる。循環する洗浄液は、洗浄槽で被洗浄物に付着した汚染物を洗浄、除去したものであり、洗浄液中にその汚染物が含まれる。汚染物としては、例えば、微粒子、金属、有機物などが存在する。洗浄液の浄化装置としては、例えば、フィルター、イオン交換機能を有するフィルター、イオン交換器、紫外線照射装置を備えた有機物分解装置などを挙げることができる。洗浄液の浄化装置は、脱気装置の下流側に設けることが好ましい。洗浄液の浄化装置を脱気装置の下流側に設けることにより、脱気装置において微粒子などが発生した場合にも、洗浄液の浄化装置において除去することができる。
【０００７】
図１は、本発明の電子材料用ウェット洗浄装置の一態様の工程系統図である。本態様の装置は、バッチ式洗浄槽１と、洗浄槽より循環ポンプ２により洗浄液を引き抜いて、再度洗浄槽に返送する洗浄液循環ライン３とを有し、洗浄液循環ラインには脱気装置４と洗浄液の浄化装置５が設けられている。脱気装置は、気体透過膜モジュールに真空ポンプ６を接続したものであり、洗浄液の浄化装置にはフィルターが用いられている。
バッチ式洗浄槽から引き抜かれた洗浄液は、循環ポンプにより圧送され、脱気装置及び洗浄液の浄化装置を経て、再び洗浄槽に返送される。脱気装置を設けないと、引き抜きの際に巻き込んだ微量の気泡や、過酸化水素などの洗浄液成分の自己分解により発生した溶存気体は、ポンプの吐き出し側では一時的に加圧状態となるので洗浄液に溶解するが、大気圧の洗浄槽に戻されたのちには、飽和度を超える気体成分が気泡となり、被洗浄物の表面に付着する。洗浄液循環ラインに脱気装置を設けることにより、洗浄液中に溶解している気体成分を、大気圧における飽和度以下に低減して、洗浄槽における気泡の発生を抑止することができる。気泡の発生を抑止することにより、被洗浄物の表面に気泡が付着し、さらに気泡の表面に異物が集合して、被洗浄物が再汚染されることを防止することが可能となる。
【０００８】
【発明の効果】
本発明の電子材料用ウェット洗浄装置を用いることにより、洗浄槽内の洗浄液中で微細な気泡が発生することがなく、気泡に起因する被洗浄物の再汚染や、洗浄不良を防止することができる。
【図面の簡単な説明】
【図１】図１は、本発明の電子材料用ウェット洗浄装置の一態様の工程系統図である。
【符号の説明】
１ バッチ式洗浄槽
２ 循環ポンプ
３ 洗浄液循環ライン
４ 脱気装置
５ 洗浄液の浄化装置
６ 真空ポンプ[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a wet cleaning apparatus for electronic materials. More specifically, the present invention relates to an electronic material wet cleaning apparatus for cleaning the surface of an electronic material such as a semiconductor silicon substrate and a liquid crystal glass substrate.
[0002]
[Prior art]
Cleaning liquids for electronic materials include RCA cleaning liquids based on hydrogen peroxide, ultrapure water itself, acids, alkalis, oxidizing agents, reducing agents, etc., and adjusted to adjust pH and redox potential. Water is used. In the batch type wet cleaning system, in order to reduce the consumption of the cleaning liquid, a circulation system is employed in which the cleaning liquid is drawn out from the cleaning tank by a pump and supplied to the cleaning tank again through filtration by a filter. In recent years, it has become possible to remove metal impurities in the cleaning liquid by using a membrane module having an ion exchange function, and the adoption of a circulation system has been increasingly widespread.
When the electronic material is cleaned using the cleaning liquid for the electronic material, gas may be dissolved in the cleaning liquid. In particular, in a system in which the cleaning liquid is circulated, the state of pressurization or depressurization occurs more or less, and bubbles are easily generated in the cleaning liquid. In addition, bubbles are easily generated when the components of the cleaning liquid are decomposed and gasified. For example, in a cleaning solution containing hydrogen peroxide, hydrogen peroxide is self-decomposed into oxygen, and bubbles are likely to be generated.
When bubbles are generated in the cleaning liquid, there is a problem that fine bubbles adhere to the surface of the electronic material that is the object to be cleaned, and the object to be cleaned is contaminated with foreign substances that collect on the surface of the bubbles. In particular, in the case of a cleaning liquid containing hydrofluoric acid, the cleaned solid surface becomes hydrophobic, and air bubbles tend to adhere to the solid surface, and the solid surface tends to be recontaminated.
[0003]
[Problems to be solved by the invention]
The present invention provides a wet for electronic material that can eliminate the generation of bubbles in a cleaning tank in a wet cleaning process for an electronic material for cleaning the surface of an electronic material such as a silicon substrate for a semiconductor and a glass substrate for a liquid crystal. The purpose is to provide a cleaning device.
[0004]
[Means for Solving the Problems]
As a result of intensive studies to solve the above problems, the present inventors have developed a cleaning liquid in a wet cleaning apparatus for electronic materials having a cleaning tank and a cleaning liquid circulation line that draws out the liquid in the cleaning tank and returns it to the cleaning tank again. We found that it is possible to prevent the generation of bubbles in the cleaning tank by providing a degassing device in the circulation line and making the amount of gas dissolved in the cleaning liquid below the saturation level at atmospheric pressure, The present invention has been completed based on this finding.
That is, the present invention
(1) As a cleaning solution, ultrapure water in which hydrogen peroxide is dissolved, ultrapure water in which hydrochloric acid and hydrogen peroxide are dissolved, ultrapure water in which sulfuric acid and hydrogen peroxide are dissolved, hydrofluoric acid and hydrogen peroxide are dissolved Wet cleaning equipment for electronic materials using ultrapure water, ammonia and hydrogen peroxide dissolved ultrapure water, or hydrofluoric acid aqueous solution, withdrawing the cleaning liquid from the cleaning tank and the cleaning tank and returning it to the cleaning tank again In the wet cleaning apparatus for electronic materials having a cleaning liquid circulation line, a gas permeable membrane module for removing gas dissolved in the cleaning circulation line, a deaeration device comprising a decompression system, and a purification device are further provided. Wet cleaning device for electronic materials characterized by suppressing generation of fine bubbles in the cleaning tank by being provided on the downstream side,
(2) The wet cleaning apparatus for electronic materials according to the first aspect, wherein the purification device includes a filter, a filter having an ion exchange function, an ion exchanger, or an ultraviolet irradiation device,
(3) The wet cleaning apparatus for electronic materials according to claim 1 or 2, wherein the degassing apparatus is a degassing apparatus for degassing the gas from a gas in the cleaning liquid to a concentration not exceeding saturation at atmospheric pressure. ,
(4) As a cleaning solution, ultrapure water in which hydrogen peroxide is dissolved, ultrapure water in which hydrochloric acid and hydrogen peroxide are dissolved, ultrapure water in which sulfuric acid and hydrogen peroxide are dissolved, hydrofluoric acid and hydrogen peroxide are dissolved The wet cleaning method for electronic materials using ultrapure water, ultrapure water in which ammonia and hydrogen peroxide are dissolved, or a hydrofluoric acid aqueous solution, wherein the cleaning liquid drawn from the cleaning tank is removed from the gas permeable membrane module and the decompression system. After the gas dissolved by the degassing device is degassed, it is further purified and returned to the cleaning tank again , thereby suppressing the generation of fine bubbles in the cleaning tank, and processing the cleaning liquid for electronic materials Method and
(5) The method for treating a cleaning liquid for electronic materials according to
Is to provide.
[0005]
DETAILED DESCRIPTION OF THE INVENTION
The wet cleaning apparatus for electronic materials according to the present invention has a cleaning tank, a cleaning liquid circulation line that draws the cleaning liquid from the cleaning tank and returns it to the cleaning tank, and is further provided with a degassing device in the cleaning liquid circulation line. It is.
The cleaning liquid used in the apparatus of the present invention is not particularly limited. For example, ultrapure water in which hydrogen peroxide is dissolved, ultrapure water in which hydrochloric acid and hydrogen peroxide are dissolved, ultrapure water in which sulfuric acid and hydrogen peroxide are dissolved, and fluorine. Examples thereof include ultrapure water in which hydrofluoric acid and hydrogen peroxide are dissolved, ultrapure water in which ammonia and hydrogen peroxide are dissolved, and a hydrofluoric acid aqueous solution.
The deaeration device provided in the cleaning liquid circulation line of the apparatus of the present invention is not particularly limited. For example, a depressurization tank in which the gas phase is depressurized can be provided, or a gas permeable membrane module can be provided. The gas permeable membrane module passes the cleaning liquid circulating on one side of the membrane, sucks the other side of the membrane with a vacuum pump to depressurize the gas in the cleaning liquid from the liquid phase side of the membrane to the gas phase Permeate to the side and separate. As a deaeration device, a combination of a gas permeable membrane module and a decompression system can be suitably used. It is preferable that the gas permeable membrane module has durability against chemicals contained in the cleaning liquid.
[0006]
The gas permeable membrane module is preferably installed on the discharge side of the circulation pump. By depressurizing the gas phase part of the gas permeable membrane module, it is possible to remove gas components dissolved in the chemical solution at a degree of saturation or higher at atmospheric pressure, for example, oxygen generated by decomposition of hydrogen peroxide. If the pressure in the gas phase is excessively reduced, decomposition of the drug in the cleaning liquid may be accelerated. If the gas in the cleaning liquid is degassed to a concentration that does not exceed the saturation level at atmospheric pressure, bubbles will not be generated in the cleaning tank. It is preferable to stay. The gas saturation in the cleaning liquid is a value obtained by dividing the amount of gas dissolved in water by the amount of gas dissolved at atmospheric pressure and room temperature. For example, water in contact with air at a pressure of 10 5 Pa and a temperature of 20 ° C. is in a state of equilibrium of 1.0 times by dissolving 15.4 mg / liter of nitrogen and 8.8 mg / liter of oxygen. Therefore, the degree of saturation of water in which the amount of dissolved gas is 12.3 mg / liter of nitrogen and 7.0 mg / liter of oxygen by degassing is 0.8 times. By setting the degree of saturation of the gas in the cleaning liquid to about 0.8 times, generation of bubbles in the cleaning tank can be reliably prevented.
In the apparatus of the present invention, it is preferable to provide a cleaning liquid purification device in the cleaning liquid circulation line. There is no restriction | limiting in particular in the purification apparatus of a washing | cleaning liquid, According to the contaminant contained in a washing | cleaning liquid, it can select suitably. The circulating cleaning liquid is obtained by cleaning and removing contaminants attached to the object to be cleaned in the cleaning tank, and the cleaning liquid contains the contaminants. Examples of contaminants include fine particles, metals, and organic substances. Examples of the cleaning liquid purifier include a filter, a filter having an ion exchange function, an ion exchanger, and an organic substance decomposing apparatus equipped with an ultraviolet irradiation device. The cleaning liquid purifier is preferably provided downstream of the deaerator. By providing the cleaning liquid purification device on the downstream side of the deaeration device, even if fine particles or the like are generated in the deaeration device, the cleaning liquid purification device can remove them.
[0007]
FIG. 1 is a process flow diagram of one embodiment of a wet cleaning apparatus for electronic materials according to the present invention. The apparatus of this embodiment has a batch type cleaning tank 1 and a cleaning
The cleaning liquid drawn out from the batch type cleaning tank is pumped by a circulation pump and is returned to the cleaning tank again through a degassing device and a cleaning liquid purification device. Without a degassing device, a small amount of bubbles entrained during extraction and dissolved gas generated by self-decomposition of cleaning liquid components such as hydrogen peroxide are temporarily pressurized on the pump discharge side. Although dissolved in the cleaning liquid, after returning to the cleaning tank at atmospheric pressure, the gas component exceeding the saturation becomes bubbles and adheres to the surface of the object to be cleaned. By providing a degassing device in the cleaning liquid circulation line, the gas component dissolved in the cleaning liquid can be reduced to a degree of saturation or less at atmospheric pressure, and the generation of bubbles in the cleaning tank can be suppressed. By suppressing the generation of air bubbles, it is possible to prevent air bubbles from adhering to the surface of the object to be cleaned, and foreign matters to collect on the surface of the air bubbles, thereby recontaminating the object to be cleaned.
[0008]
【The invention's effect】
By using the wet cleaning apparatus for electronic materials according to the present invention, fine bubbles are not generated in the cleaning liquid in the cleaning tank, and it is possible to prevent recontamination of objects to be cleaned and cleaning defects caused by the bubbles. it can.
[Brief description of the drawings]
FIG. 1 is a process flow diagram of one embodiment of a wet cleaning apparatus for electronic materials according to the present invention.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 Batch type washing tank 2
Claims (5)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34143097A JP3797775B2 (en) | 1997-12-11 | 1997-12-11 | Wet cleaning device for electronic material and processing method for cleaning liquid for electronic material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34143097A JP3797775B2 (en) | 1997-12-11 | 1997-12-11 | Wet cleaning device for electronic material and processing method for cleaning liquid for electronic material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH11176794A JPH11176794A (en) | 1999-07-02 |
| JP3797775B2 true JP3797775B2 (en) | 2006-07-19 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP34143097A Expired - Fee Related JP3797775B2 (en) | 1997-12-11 | 1997-12-11 | Wet cleaning device for electronic material and processing method for cleaning liquid for electronic material |
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| JP (1) | JP3797775B2 (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3595441B2 (en) * | 1997-12-29 | 2004-12-02 | 三菱電機株式会社 | Cleaning method using hydrogen peroxide |
| JP2002370060A (en) * | 2001-06-13 | 2002-12-24 | Fuji Photo Film Co Ltd | Deaeration system of coating liquid and deaeration method for coating liquid |
| JP5243849B2 (en) * | 2008-06-03 | 2013-07-24 | 芝浦メカトロニクス株式会社 | Substrate processing apparatus and substrate processing method |
| JP6770823B2 (en) * | 2016-04-13 | 2020-10-21 | オルガノ株式会社 | Degassing method and equipment for chemicals |
| US10935896B2 (en) * | 2016-07-25 | 2021-03-02 | Applied Materials, Inc. | Cleaning solution mixing system with ultra-dilute cleaning solution and method of operation thereof |
-
1997
- 1997-12-11 JP JP34143097A patent/JP3797775B2/en not_active Expired - Fee Related
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| Publication number | Publication date |
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| JPH11176794A (en) | 1999-07-02 |
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