JPH08117706A - Method for filling liquid into recesslike structural space - Google Patents
Method for filling liquid into recesslike structural spaceInfo
- Publication number
- JPH08117706A JPH08117706A JP25705194A JP25705194A JPH08117706A JP H08117706 A JPH08117706 A JP H08117706A JP 25705194 A JP25705194 A JP 25705194A JP 25705194 A JP25705194 A JP 25705194A JP H08117706 A JPH08117706 A JP H08117706A
- Authority
- JP
- Japan
- Prior art keywords
- liquid
- gas
- dioxide
- recesslike
- soluble
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Cleaning By Liquid Or Steam (AREA)
- Cleaning Or Drying Semiconductors (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は凹状構造空間に液体を充
填する方法に関する。更に詳しくは、液体による濡れ性
の悪い材質から成る微細凹状構造空間内、及びあらかじ
め構造空間に存在するガスと液体との置換が起こりにく
い微細凹状構造空間内に効率良く液体を充填する方法に
関する。本発明は特に、微細加工された半導体基板表面
の洗浄に利用される。FIELD OF THE INVENTION The present invention relates to a method for filling a concave structure space with a liquid. More specifically, the present invention relates to a method for efficiently filling a liquid in a fine concave structure space made of a material having poor wettability with a liquid, and in a fine concave structure space in which gas and liquid existing in advance in the structure space are unlikely to be replaced. The present invention is particularly used for cleaning the surface of a microfabricated semiconductor substrate.
【０００２】[0002]
【従来の技術】近年、エレクトロニクス技術の著しい進
歩に伴い、半導体製品の高集積化が必須となってきた。
その結果、使用される半導体素子に極めて微細な加工が
施される様になる。一方、微細加工された基板表面を従
来の微細加工のない基板表面と同じく、薬液で洗浄する
ことは素子の性能向上のために必須である。2. Description of the Related Art In recent years, with the remarkable progress of electronics technology, high integration of semiconductor products has become essential.
As a result, the semiconductor element used is subjected to extremely fine processing. On the other hand, it is indispensable to wash the finely processed substrate surface with a chemical solution in order to improve the performance of the device, like the conventional substrate surface without fine processing.
【０００３】しかし、著しく微細な表面加工を施された
基板に対する洗浄効率については種種の問題がある。即
ち、固体表面及び液体の両者の間に生まれる表面張力の
ために微細凹状構造空間内部の曲率の大きい部分又は微
細な部分に気泡が付着し、これが液体による濡れを妨げ
る。更に、微細凹状構造空間の径が小さくなるほどまた
微細凹状構造空間の深さが大きくなるほど、微細凹状構
造空間内部への液の完全な到達が困難となる。However, there are various problems regarding the cleaning efficiency for a substrate having a remarkably fine surface treatment. That is, due to the surface tension generated between both the solid surface and the liquid, bubbles adhere to a large curvature portion or a fine portion inside the fine concave structure space, which prevents the liquid from getting wet. Furthermore, as the diameter of the fine concave structure space becomes smaller and the depth of the fine concave structure space becomes larger, it becomes more difficult for the liquid to completely reach the inside of the fine concave structure space.
【０００４】これに対し、半導体基板を水蒸気を含む雰
囲気内に置き、表面を結露させることによって濡らす方
法や超音波振動を与えることによって微細凹状構造空間
内部に液体を充填させる方法が今日までに発表されてい
る。しかし、従来開発されたこれらの技術では微細凹状
構造空間内部への液の完全な到達は困難である。On the other hand, to date, a method of placing a semiconductor substrate in an atmosphere containing water vapor and wetting the surface by dew condensation and a method of applying ultrasonic vibration to fill the inside of the micro concave structure space with a liquid have been announced to date. Has been done. However, it is difficult to completely reach the inside of the fine concave structure space with these techniques that have been conventionally developed.
【０００５】すなわち、従来開発されている技術では将
来予想される、より微細化を目指した加工技術に対応す
ることができず、微細凹状構造空間に対する新規な液体
の充填技術の開発が必要となっている。In other words, the conventionally developed technology cannot support the processing technology aiming for further miniaturization, which is expected in the future, and it is necessary to develop a new liquid filling technology for the fine concave structure space. ing.
【０００６】[0006]
【発明が解決しようとする課題】本発明の目的は、凹状
構造空間内に液体を充填する技術の提供である。本発明
のもう一つの目的は、微細加工された半導体基板の凹状
構造空間内に液体を充填する方法の提供である。SUMMARY OF THE INVENTION An object of the present invention is to provide a technique for filling a liquid in a concave structure space. Another object of the present invention is to provide a method for filling a liquid into the concave structure space of a microfabricated semiconductor substrate.
【０００７】[0007]
【課題を解決するための手段】本発明者らは上記の目的
を達成すべく鋭意検討を行った結果、凹状構造空間内部
ガスの液への溶解性に着目し、液体に可溶性のガスを該
構造空間内に充満させた後、当該ガスを溶解する液体を
該構造空間内に注入することにより微細な凹状構造空間
においてもその底部にまで液体を充填させることができ
ることを見いだし、本発明を完成するに至った。Means for Solving the Problems As a result of intensive studies to achieve the above object, the present inventors have focused on the solubility of the gas inside the concave structure space in the liquid and The present invention has been completed by finding that even after filling the structure space with a liquid that dissolves the gas, the bottom of the structure space can be filled with the liquid by injecting the liquid into the structure space. Came to do.
【０００８】本発明においては、まず、凹状構造空間に
液体に可溶性のガスを該構造空間内に充満させ、次い
で、当該ガスを溶解する液体を該構造空間内に注入す
る。ここで、充満した気体が注入した液体に物理的に溶
解してその容積を失うのであれば、どのような気体及び
液体の組合せを選定しても随意である。具体的には、処
理温度における当該ガスの液体への溶解度が液体100ml
当たり0.005g以上、好ましくは0.1g以上であるような組
合せを選定する。In the present invention, first, the concave structure space is filled with a gas soluble in the liquid, and then the liquid that dissolves the gas is injected into the structure space. Here, any combination of gas and liquid is optional as long as the filled gas physically dissolves in the injected liquid and loses its volume. Specifically, the solubility of the gas in the liquid at the processing temperature is 100 ml of the liquid.
A combination is selected so that the amount is 0.005 g or more, preferably 0.1 g or more.
【０００９】具体的には、注入する液体が水又は水溶液
である場合は、充満させる気体はアンモニア、塩化水
素、臭化水素、フッ化水素、塩素、臭素、二酸化炭素、
二酸化硫黄、三酸化硫黄、一酸化窒素、二酸化窒素、炭
素数１〜３のアルコール、炭素数３〜４のケトン及び炭
素数２〜４のエステルが例示される。炭素数１〜３のア
ルコールとしてはメタノール、エタノール、イソプロピ
ルアルコールが例示され、炭素数３〜４のケトンとして
はアセトンが例示され、炭素数２〜４のエステルとして
はギ酸メチル、酢酸エチルが例示される。中でもアンモ
ニア、塩化水素、フッ化水素、二酸化硫黄、三酸化硫黄
又は二酸化窒素が好ましい。ガスを溶解する液体とし
て、過酸化水素を好ましくは0.1 〜20重量％、より好ま
しくは0.5 〜10重量％含有する水溶液を注入することも
また好ましい。Specifically, when the liquid to be injected is water or an aqueous solution, the gas to be filled is ammonia, hydrogen chloride, hydrogen bromide, hydrogen fluoride, chlorine, bromine, carbon dioxide,
Examples thereof include sulfur dioxide, sulfur trioxide, nitric oxide, nitrogen dioxide, alcohols having 1 to 3 carbon atoms, ketones having 3 to 4 carbon atoms, and esters having 2 to 4 carbon atoms. Examples of the alcohol having 1 to 3 carbon atoms include methanol, ethanol and isopropyl alcohol, examples of the ketone having 3 to 4 carbon atoms include acetone, and examples of the ester having 2 to 4 carbon atoms include methyl formate and ethyl acetate. It Among them, ammonia, hydrogen chloride, hydrogen fluoride, sulfur dioxide, sulfur trioxide or nitrogen dioxide is preferable. It is also preferable to inject an aqueous solution containing hydrogen peroxide of preferably 0.1 to 20% by weight, more preferably 0.5 to 10% by weight, as the gas dissolving liquid.
【００１０】注入する液体が過酸化水素水溶液、水酸化
ナトリウム等の金属水酸化物水溶液、硫酸ナトリウム等
の金属塩水溶液、フッ化アンモニウム等のアンモニウム
塩水溶液や硫酸水溶液等の水溶液である場合は、充満さ
せる気体に水蒸気を選択することも好ましい。前記注入
する水溶液の濃度に制限は無いが、５重量％以上が好ま
しく、２０重量％以上の高濃度がより好ましい。When the liquid to be injected is an aqueous solution of hydrogen peroxide, an aqueous solution of metal hydroxide such as sodium hydroxide, an aqueous solution of metal salt such as sodium sulfate, an aqueous solution of ammonium salt such as ammonium fluoride or an aqueous solution of sulfuric acid, It is also preferable to select water vapor as the gas to be filled. The concentration of the aqueous solution to be injected is not limited, but is preferably 5% by weight or more, and more preferably 20% by weight or more.
【００１１】注入する液体がイソプロピルアルコールに
代表されるアルコール類、ジエチルエーテルに代表され
るエーテル類、メチルイソブチルケトンに代表されるケ
トン類、酢酸エチルに代表されるエステル類、アミン
類、クロロホルムに代表されるハロゲン化炭化水素、炭
素数６〜12の芳香族又は脂肪族炭化水素等の有機溶媒で
ある場合は、充満させる気体は一酸化炭素、二酸化炭
素、アンモニア、二酸化硫黄、又はメタン、アセチレ
ン、エチレン等の炭素数１〜６の脂肪族炭化水素、又は
ジメチルエーテル等の炭素数２〜６のエーテル類、又は
アセトン等の炭素数３〜６のケトン類、又はギ酸メチル
等の炭素数２〜６のエステル類、又は塩化メチレン等の
炭素数１〜６のハロゲン化炭化水素が好適である。Liquids to be injected are alcohols typified by isopropyl alcohol, ethers typified by diethyl ether, ketones typified by methyl isobutyl ketone, esters typified by ethyl acetate, amines, typified by chloroform. In the case of an organic solvent such as a halogenated hydrocarbon, an aromatic or aliphatic hydrocarbon having 6 to 12 carbon atoms, the gas to be filled is carbon monoxide, carbon dioxide, ammonia, sulfur dioxide, or methane, acetylene, C1-C6 aliphatic hydrocarbons such as ethylene, C2-C6 ethers such as dimethyl ether, C3-C6 ketones such as acetone, or C2-C6 such as methyl formate. Are preferred, or halogenated hydrocarbons having 1 to 6 carbon atoms such as methylene chloride.
【００１２】本発明に使用される気体及び液体は、通
常、気体及び液体が微細凹状構造を成す物質に対して反
応性を有しないものが選択されるが、基板又は基板の凹
状構造空間内部の化学的研磨を意図する場合は基板を成
す物質に対して反応性を有するものを選択しても良い。The gas and liquid used in the present invention are usually selected so that the gas and the liquid are not reactive with the substance forming the fine concave structure. When chemical polishing is intended, a material having reactivity with the substance forming the substrate may be selected.
【００１３】ガスを溶解する液体を凹状構造空間内に注
入する際の温度は、通常−10〜150℃、注入する際の圧
力は通常１mmHg〜５atm 、好ましくは１〜３atm から選
ばれる。The temperature for injecting the liquid that dissolves the gas into the concave structure space is usually -10 to 150 ° C, and the pressure for injecting is usually 1 mmHg to 5 atm, preferably 1 to 3 atm.
【００１４】特に、液体に可溶性のガスがアンモニア、
塩化水素、臭化水素、フッ化水素、塩素、臭素、二酸化
炭素、二酸化硫黄、三酸化硫黄、一酸化窒素、二酸化窒
素、炭素数１〜３のアルコール及び炭素数３〜４のケト
ンからなる群から選ばれた少なくとも１種であり、当該
ガスを物理的に溶解する液体が水である場合の温度は、
０〜100 ℃、好ましくは５〜40℃である。In particular, the gas soluble in the liquid is ammonia,
Group consisting of hydrogen chloride, hydrogen bromide, hydrogen fluoride, chlorine, bromine, carbon dioxide, sulfur dioxide, sulfur trioxide, nitric oxide, nitrogen dioxide, alcohol having 1 to 3 carbon atoms and ketone having 3 to 4 carbon atoms. The temperature when the liquid that physically dissolves the gas is water is at least one selected from
The temperature is 0 to 100 ° C, preferably 5 to 40 ° C.
【００１５】特に、液体に可溶性のガスが水蒸気であ
り、当該ガスを物理的に溶解する液体が過酸化水素、金
属水酸化物、金属塩、アンモニウム塩又は硫酸の水溶液
である場合の温度は、70〜150 ℃、好ましくは80〜110
℃である。Particularly, when the gas soluble in the liquid is water vapor and the liquid which physically dissolves the gas is an aqueous solution of hydrogen peroxide, metal hydroxide, metal salt, ammonium salt or sulfuric acid, the temperature is 70-150 ℃, preferably 80-110
° C.
【００１６】特に、液体に可溶性のガスが一酸化炭素、
二酸化炭素、アンモニア、塩化水素、フッ化水素、二酸
化硫黄、三酸化硫黄、二酸化窒素、並びに、炭素数１〜
６の炭化水素、エーテル類、ケトン類及びエステル類か
らなる群から選ばれた少なくとも１種であり、当該ガス
を物理的に溶解する液体が有機溶媒である場合の温度
は、−10〜70℃、好ましくは０〜40℃である。In particular, the gas soluble in the liquid is carbon monoxide,
Carbon dioxide, ammonia, hydrogen chloride, hydrogen fluoride, sulfur dioxide, sulfur trioxide, nitrogen dioxide, and carbon number 1 to
6 is at least one selected from the group consisting of hydrocarbons, ethers, ketones and esters, and the temperature when the liquid that physically dissolves the gas is an organic solvent is -10 to 70 ° C. , Preferably 0 to 40 ° C.
【００１７】ガスを溶解する液体を凹状構造空間内に注
入する際には、該構造体に振動波を加えながら行うこと
も好ましい。注入時の液体の温度を気体の温度より低く
して本発明を実施することも可能である。本発明におい
ては、更に、液体に界面活性剤などの濡れ性向上剤又は
キレート剤を添加することも好ましい。When the liquid that dissolves the gas is injected into the concave structure space, it is also preferable to add a vibration wave to the structure. It is also possible to carry out the present invention by making the temperature of the liquid at the time of injection lower than the temperature of the gas. In the present invention, it is also preferable to add a wettability improver such as a surfactant or a chelating agent to the liquid.
【００１８】[0018]
【実施例】以下に実施例により本発明を説明する。 実施例１〜９ 下端にコックを取り付け上端に円錐状の漏斗を取り付け
た、内径0.05mm、長さ30cmのテフロン製の管に試験気体
を流し、完全に管の中を試験気体で置換した。次に、コ
ックを閉じ、直ちに試験液体を漏斗に注いだ。１atm 、
10℃で30分静置後、管内の液滴の下端位置を調べた。液
体の下端がコックにまで到達したことが確認された場合
を○、液滴の下端とコックとの間に空間部分が残った場
合を×として表１に示した。結果が○であることは管内
の隅々にまで液体が充填されたことを意味する。EXAMPLES The present invention will be described below with reference to examples. Examples 1 to 9 A test gas was passed through a Teflon tube having an inner diameter of 0.05 mm and a length of 30 cm, which was equipped with a cock at the lower end and a conical funnel at the upper end, and the inside of the tube was completely replaced with the test gas. The cock was then closed and the test liquid was immediately poured into the funnel. 1 atm,
After standing at 10 ° C. for 30 minutes, the lower end position of the droplet in the tube was examined. The results are shown in Table 1 as ◯ when it was confirmed that the lower end of the liquid reached the cock, and as × when the space portion remained between the lower end of the droplet and the cock. A result of ◯ means that the liquid was filled in every corner of the tube.
【００１９】[0019]
【表１】 気体 液体 結果 実施例１ アンモニア ３重量％過酸化水素水溶液 ○ 実施例２ 塩素 水 ○ 実施例３ 塩化水素 水 ○ 実施例４ フッ化水素 水 ○ 実施例５ 二酸化硫黄 ８重量％過酸化水素水溶液 ○ 実施例６ 二酸化窒素 水 ○ 実施例７ メタノール 水 ○ 実施例８ アセトン 水 ○ 実施例９ エチレン ヘキサン ○ [Table 1] Gas Liquid Result Example 1 Ammonia 3 wt% hydrogen peroxide aqueous solution ○ Example 2 chlorine water ○ Example 3 hydrogen chloride water ○ Example 4 hydrogen fluoride water ○ Example 5 Sulfur dioxide 8 wt% peroxide Aqueous hydrogen solution ○ Example 6 Nitrogen dioxide water ○ Example 7 Methanol water ○ Example 8 Acetone water ○ Example 9 Ethylene hexane ○
【００２０】実施例１０〜１１ 気体と液体の組合せを変更し、105 ℃で30分静置した他
は、実施例１〜９と同様の実験を繰り返した。結果を表
２に示す。Examples 10 to 11 The same experiments as in Examples 1 to 9 were repeated, except that the combination of gas and liquid was changed and the mixture was allowed to stand at 105 ° C for 30 minutes. Table 2 shows the results.
【００２１】[0021]
【表２】 気体 液体 結果 実施例１０ 水蒸気 30重量％硫酸水溶液 ○ 実施例１１ 水蒸気 40重量％過酸化水素水溶液 ○ [Table 2] Gas liquid Result Example 10 Water vapor 30 wt% sulfuric acid aqueous solution ○ Example 11 Water vapor 40 wt% hydrogen peroxide aqueous solution ○
【００２２】比較例１〜３ 気体と液体の組合せを変更した他は、実施例１〜９と同
様の実験を繰り返した。結果を表３に示す。Comparative Examples 1 to 3 The same experiments as in Examples 1 to 9 were repeated except that the combination of gas and liquid was changed. The results are shown in Table 3.
【００２３】[0023]
【表３】 気体 液体 結果 比較例１ 空気 水 × 比較例２ 窒素 水 × 比較例３ 空気 ヘキサン × Table 3 Gas / Liquid Results Comparative Example 1 Air Water × Comparative Example 2 Nitrogen Water × Comparative Example 3 Air Hexane ×
【００２４】[0024]
【発明の効果】本発明によれば、凹状構造内部の隅々に
まで液体を完全に充填することができ、該構造内部と液
体との接触による様々な作用を生む基礎を作り上げるこ
とが出来る。According to the present invention, it is possible to completely fill every corner inside the concave structure with a liquid, and it is possible to construct a foundation that produces various actions due to the contact between the inside of the structure and the liquid.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 吉田 寛史 東京都葛飾区新宿６丁目１番１号 三菱瓦 斯化学株式会社東京研究所内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Hiroshi Yoshida 6-1-1, Shinjuku, Katsushika-ku, Tokyo Mitsubishi Gas Chemical Co., Ltd. Tokyo Laboratory
Claims (6)
て、あらかじめ液体に可溶性のガスを凹状構造空間内に
充満させた後、当該ガスを物理的に溶解する液体を該構
造空間内に注入することを特徴とする、液体の充填方
法。1. A method of filling a liquid in a concave structure space, wherein a gas soluble in the liquid is filled in the concave structure space in advance, and then a liquid that physically dissolves the gas is injected into the structure space. A method for filling a liquid, which is characterized in that
素、臭化水素、フッ化水素、塩素、臭素、二酸化炭素、
二酸化硫黄、三酸化硫黄、一酸化窒素、二酸化窒素、炭
素数１〜３のアルコール、炭素数３〜４のケトン及び炭
素数２〜４のエステルからなる群から選ばれた少なくと
も１種であり、当該ガスを物理的に溶解する液体が水で
ある請求項１記載の方法。2. A liquid-soluble gas is ammonia, hydrogen chloride, hydrogen bromide, hydrogen fluoride, chlorine, bromine, carbon dioxide,
At least one selected from the group consisting of sulfur dioxide, sulfur trioxide, nitric oxide, nitrogen dioxide, alcohol having 1 to 3 carbon atoms, ketone having 3 to 4 carbon atoms, and ester having 2 to 4 carbon atoms, The method according to claim 1, wherein the liquid that physically dissolves the gas is water.
を含有する水溶液である請求項２記載の方法。3. The method according to claim 2, wherein the liquid that physically dissolves the gas is an aqueous solution containing hydrogen peroxide.
素、フッ化水素、二酸化硫黄、三酸化硫黄又は二酸化窒
素である請求項２記載の方法。4. The method according to claim 2, wherein the gas soluble in the liquid is ammonia, hydrogen chloride, hydrogen fluoride, sulfur dioxide, sulfur trioxide or nitrogen dioxide.
ガスを物理的に溶解する液体が過酸化水素、金属水酸化
物、金属塩、アンモニウム塩又は硫酸の水溶液である請
求項１記載の方法。5. The gas according to claim 1, wherein the gas soluble in the liquid is water vapor, and the liquid which physically dissolves the gas is an aqueous solution of hydrogen peroxide, metal hydroxide, metal salt, ammonium salt or sulfuric acid. Method.
炭素、アンモニア、塩化水素、フッ化水素、二酸化硫
黄、三酸化硫黄、二酸化窒素、並びに、炭素数１〜６の
脂肪族炭化水素、エーテル類、ケトン類及びエステル類
からなる群から選ばれた少なくとも１種であり、当該ガ
スを物理的に溶解する液体が有機溶媒である請求項１記
載の方法。6. A liquid-soluble gas comprising carbon monoxide, carbon dioxide, ammonia, hydrogen chloride, hydrogen fluoride, sulfur dioxide, sulfur trioxide, nitrogen dioxide, and an aliphatic hydrocarbon having 1 to 6 carbon atoms, The method according to claim 1, wherein the liquid is at least one selected from the group consisting of ethers, ketones, and esters, and the liquid that physically dissolves the gas is an organic solvent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25705194A JPH08117706A (en) | 1994-10-21 | 1994-10-21 | Method for filling liquid into recesslike structural space |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25705194A JPH08117706A (en) | 1994-10-21 | 1994-10-21 | Method for filling liquid into recesslike structural space |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH08117706A true JPH08117706A (en) | 1996-05-14 |
Family
ID=17301062
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP25705194A Pending JPH08117706A (en) | 1994-10-21 | 1994-10-21 | Method for filling liquid into recesslike structural space |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH08117706A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023166697A1 (en) * | 2022-03-04 | 2023-09-07 | 株式会社荏原製作所 | Substrate pre-wet processing method and pre-wet module |
-
1994
- 1994-10-21 JP JP25705194A patent/JPH08117706A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023166697A1 (en) * | 2022-03-04 | 2023-09-07 | 株式会社荏原製作所 | Substrate pre-wet processing method and pre-wet module |
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