JPH03243688A - Method for cleaning siox with chlorine fluoride gas - Google Patents
Method for cleaning siox with chlorine fluoride gasInfo
- Publication number
- JPH03243688A JPH03243688A JP4048990A JP4048990A JPH03243688A JP H03243688 A JPH03243688 A JP H03243688A JP 4048990 A JP4048990 A JP 4048990A JP 4048990 A JP4048990 A JP 4048990A JP H03243688 A JPH03243688 A JP H03243688A
- Authority
- JP
- Japan
- Prior art keywords
- chlorine fluoride
- siox
- fluoride gas
- cleaning
- gas
- 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.)
- Granted
Links
- OMRRUNXAWXNVFW-UHFFFAOYSA-N fluoridochlorine Chemical compound ClF OMRRUNXAWXNVFW-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000004140 cleaning Methods 0.000 title claims description 18
- 101100441092 Danio rerio crlf3 gene Proteins 0.000 claims abstract description 9
- 229910052814 silicon oxide Inorganic materials 0.000 abstract description 14
- 229910020323 ClF3 Inorganic materials 0.000 abstract description 8
- 239000000203 mixture Substances 0.000 abstract description 8
- JOHWNGGYGAVMGU-UHFFFAOYSA-N trifluorochlorine Chemical compound FCl(F)F JOHWNGGYGAVMGU-UHFFFAOYSA-N 0.000 abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 229910021419 crystalline silicon Inorganic materials 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 26
- 238000006243 chemical reaction Methods 0.000 description 14
- 239000011521 glass Substances 0.000 description 6
- 238000002309 gasification Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 239000011538 cleaning material Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000005297 pyrex Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- Physical Vapour Deposition (AREA)
- Chemical Vapour Deposition (AREA)
- Drying Of Semiconductors (AREA)
- Cleaning Or Drying Semiconductors (AREA)
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明は、単結晶シリコン製造装置内等に発生するＳｉ
ＯＸ＆［ｌ戒の堆積物または付着物を、フッ化塩素系の
ガスを用いてクリーニングする方法に関するものである
。[Detailed Description of the Invention] [Industrial Application Field] The present invention is directed to the treatment of Si generated in single crystal silicon manufacturing equipment, etc.
This invention relates to a method of cleaning OX&[l precepts or deposits using a chlorine fluoride gas.
［従来技術１
従来より半導体製造等の薄膜形成プロセス、すなわちＣ
ＶＤ、真空薫着、ＰＶＤ、シリコンエピタキシー等にお
いては、薄膜を形成すべき目的物のみでなく装置部部材
、各種治具等にも多量の堆積物、付着物が生成すること
が知られているが、シリコンの単結晶を製造する装置に
おいても容器からの由来と考えられる酸素により、同様
に必ずしも組成のはっきりしないＳｉＯＸ組戒の組成物
や付着物が生成する。[Prior art 1] Conventionally, thin film formation processes such as semiconductor manufacturing, that is, C
It is known that in VD, vacuum smoke deposition, PVD, silicon epitaxy, etc., a large amount of deposits and deposits are generated not only on the object on which a thin film is to be formed, but also on equipment parts, various jigs, etc. However, even in equipment for producing silicon single crystals, SiOX compositions and deposits, whose compositions are not necessarily clear, are similarly generated due to oxygen that is thought to originate from the container.
従来は、上記ＳｉＯＸ組威の堆積物を除去する手段とし
てアルカリ等による洗浄しか有効でないとされており、
アルカリ溶液を使用した湿式のクリーニング法が実施さ
れていた。Conventionally, it has been thought that cleaning with alkali or the like is the only effective means of removing the SiOX deposits.
Wet cleaning methods using alkaline solutions were practiced.
しかし、アルカリ等による洗浄においては長期間装置を
停止する必要があるほか操作が煩雑で、装置、治具自体
が損傷を受けやすいという問題点があった。However, cleaning with alkali or the like requires the equipment to be stopped for a long period of time, is complicated to operate, and has problems in that the equipment and jigs themselves are easily damaged.
［問題点を解決するための具体的手段］本発明者らは従
来法の問題点に鑑み鋭意検討の結果、上記堆積物の除去
にフッ化塩素ガスが有効であることを見出し、本発明に
到達したものである。[Specific means for solving the problem] As a result of intensive study in view of the problems of the conventional method, the present inventors found that chlorine fluoride gas is effective in removing the above deposits, and the present invention has been developed. It has been reached.
すなわち本発明は、ＣＩＦ、ＣｌＦ３、ＣＩＦ、のうち
、少なくとも１種以上を含有するフッ化塩素ガスをＳｉ
ＯＸ （１≦ｘ〈２）と接触させることを特徴とするフ
ッ化塩素ガスによるＳｉＯＸのクリーニング方法、およ
び上記方法において室温以上でフッ化塩素の分圧が５０
ｔｏｒｒ以上でかつ空搭速度が２０ｃｍ／ｍｉｎ以上の
条件による流通方式で行うこと、もしくは１００°Ｃ以
上でかつフッ化塩素の分圧が７６０ ｔｏｒｒ以上の条
件による静置方式で行うことを特徴とするフッ化塩素ガ
スによるＳｉＯＸのクリーニング方法を提供するもので
ある。That is, the present invention uses chlorine fluoride gas containing at least one of CIF, ClF3, and CIF to Si.
A method for cleaning SiOX with chlorine fluoride gas characterized by contacting with OX (1≦x<2), and in the above method, the partial pressure of chlorine fluoride is 50
It is characterized by carrying out by a flow method under the conditions of a temperature of 100° C. or more and an empty loading speed of 20 cm/min or more, or a static method under the conditions of a temperature of 100° C. or more and a partial pressure of chlorine fluoride of 760 torr or more. The present invention provides a method for cleaning SiOX using chlorine fluoride gas.
本発明でクリーニングの対象となる化合物は、完全な５
ｉ０２とは異なるＳｉＯＸ （１≦ｘ＜２）ｍ戒の珪素
酸化物である。この化合物は、黄かっ色ではっきりした
結晶性を示さず、Ｘ線分析による観察でもＸが２に近く
なるに従いクリストバライトのブロードなピークが観察
されるだけであるが、これらの組成物はＳｉＯが部分的
に酸化されたものだと考えられる。The compound to be cleaned in the present invention is a complete 5
It is a silicon oxide with a precept of SiOX (1≦x<2) which is different from i02. This compound is yellowish-brown and does not show clear crystallinity, and even when observed by X-ray analysis, only a broad peak of cristobalite is observed as X approaches 2; however, these compositions show that SiO is It is thought to have been partially oxidized.
本発明で使用するガスは、ＣＩＦ、 ＣｌＦ３、Ｃｌ
Ｆ５であり、これらは単独で使用しても、２種以上を混
合して使用してもよいが、ＣｌＦ３を単独で使用するか
、または主成分として使用するのが好ましい。また、こ
れらフッ化塩素ガスはそのまま装置内に導入してクリー
ニングを行ってもよいが、窒素、アルゴン、ヘリウム等
の不活性ガスで希釈して用いてもよい。Gases used in the present invention include CIF, ClF3, Cl
F5, and these may be used alone or in combination of two or more types, but it is preferable to use ClF3 alone or as the main component. Furthermore, these chlorine fluoride gases may be introduced into the apparatus as they are for cleaning, but they may also be used after being diluted with an inert gas such as nitrogen, argon, helium, or the like.
クリーニングの方法としては、一定の温度、疏速で装置
内にガスを流通させるいわゆる流通方式か、または装置
内に上記ガスを封入して一定の温度に保ついわゆる静置
方式かの二つの方法をとることができる。There are two cleaning methods: the so-called circulation method, in which gas is passed through the device at a constant temperature and speed, and the so-called static method, in which the gas is sealed inside the device and maintained at a constant temperature. You can take it.
本発明でクリーニングガスと堆積物の反応は、フッ化塩
素によりＳｉＯＸ組底物が分解されて、Ｓｉのハロゲン
化物と酸素が発生する反応であると考えられるが、−旦
発生した酸素が気相中または固相中のいずれかを遣って
拡散し、非常にエツチングされにくいＳｉＯ□に変化す
る場合があるため、反応の条件を検討する必要がある。In the present invention, the reaction between the cleaning gas and the deposit is thought to be a reaction in which SiOX composite is decomposed by chlorine fluoride and Si halide and oxygen are generated. It is necessary to consider the reaction conditions because it may diffuse into SiO□, which is very difficult to etch, by diffusion either in the medium or in the solid phase.
すなわち、フッ化塩素ガスが一定以上の濃度で常にクリ
ーニング材料表面に供給される必要があり、流通方式で
クリーニングを行う場合は、フッ化塩素ガスの圧力が５
０ｔｏｒｒ以上でかつその空搭速度が２０ｃｍ／ｓｉｎ
以上であれば室温でガス化反応は進行し、完全にクリー
ニングを行うことができる。In other words, chlorine fluoride gas must always be supplied to the surface of the cleaning material at a concentration higher than a certain level, and when cleaning is performed using the circulation method, the pressure of chlorine fluoride gas must be
0 torr or more and its empty speed is 20 cm/sin
If it is above, the gasification reaction will proceed at room temperature, and complete cleaning can be performed.
室温においてフッ化塩素ガスの圧力が５０ｔｏｒｒより
低いか、または空搭速度が２０ｃｍ／ｌｌ１ｎ未満の場
合は、最初はガス化反応が進行するが、次第に表面が５
ｉ０２に変化し、反応は停止してしまうため、温度をさ
らに上げる必要がある。しかし、反応の温度が上がるに
従い、必要なフッ化塩素ガスの圧力または空搭速度も低
下する。If the pressure of chlorine fluoride gas is lower than 50 torr or the empty loading velocity is lower than 20 cm/ll1n at room temperature, the gasification reaction will initially proceed, but gradually the surface
Since the reaction changes to i02 and the reaction stops, it is necessary to further raise the temperature. However, as the temperature of the reaction increases, the required pressure or emptying rate of chlorine fluoride gas also decreases.
一方、フッ化塩素ガスを装置内に封入する静置方式にお
いては、材料表面にフッ化塩素ガスが供給されにくいた
めガス圧力および反応温度を高く設定する必要があり、
温度１００“Ｃ以上でかつフッ化塩素分圧７６０ ｔｏ
ｒｒ以上で初めてガス化反応が進行する。上記条件を満
たさない場合は、５ｉ０２が生威し、反応は進行しない
、ただし、温度が上がるに従い、必要なフッ化塩素ガス
の圧力は低下していく。On the other hand, in the stationary method where chlorine fluoride gas is sealed inside the device, it is difficult to supply chlorine fluoride gas to the material surface, so the gas pressure and reaction temperature must be set high.
At a temperature of 100"C or higher and a partial pressure of chlorine fluoride of 760 to
The gasification reaction progresses only when the temperature exceeds rr. If the above conditions are not met, 5i02 will survive and the reaction will not proceed.However, as the temperature rises, the required pressure of chlorine fluoride gas decreases.
上記した条件では雰囲気温度が余り高くないため、装置
材料は殆ど腐食せず、装置自体を傷つけることなしにク
リーニングを行うことができる。Under the above conditions, the ambient temperature is not so high that the material of the device hardly corrodes, and cleaning can be performed without damaging the device itself.
このように、前記したような条件を設定することにより
、従来ガスによる乾式クリーニングが難しいとされてい
たＳｉＯＸＭｉ或の堆積物を、フッ化塩素ガスを用いて
クリーニングできるものである。By setting the above-mentioned conditions in this way, it is possible to clean SiOXMi deposits, which have conventionally been difficult to dry clean using gas, using chlorine fluoride gas.
［実施例〕 以下、実施例により本発明の詳細な説明する。[Example〕 Hereinafter, the present invention will be explained in detail with reference to Examples.
実施例１〜６、比較例１．２
シリコン単結晶製造装置内で発生したＳｉＯＸ＆ｉ或（
ｘ−１，３）の堆積物を採取したちの０．２ｇをニッケ
ル製の容器に入れ、この容器をパイレンクスガラス管（
直径５０＋ｕ＋、長さ７００＋＊＋＊）内に設置した。Examples 1 to 6, Comparative Example 1.2 SiOX&i or (
x-1, 3), put 0.2 g of the sample into a nickel container, and place the container into a Pyrex glass tube (
It was installed within a diameter of 50+u+ and a length of 700+**+*.
但し、実施例６だけはＳｉＯＸの組成は（ｘ ＝ １．
７）である。次に、ガラス管の両端は、５ＩＪＳ３１６
製でガスが導入できるように導入口を有する金属製容器
で密封されている。このガラス管の周囲に管状電気炉を
設け、反応温度を任意に設定できるようにした。However, only in Example 6, the composition of SiOX was (x = 1.
7). Next, both ends of the glass tube are 5IJS316
It is sealed in a metal container with an inlet to allow gas to be introduced. A tubular electric furnace was installed around this glass tube, so that the reaction temperature could be set arbitrarily.
次に、Ｃ］Ｆ３ボンベとＡｒボンへからガラス管内に混
合ガスが導入できるようガス管を設置し、出口より排気
ポンプで排気しながら所定の圧力、疏量でＣｌＦ３ガス
単独かまたはＡｒとのγ昆合ガスをガラス管に導入し、
２時間反応を行った。結果を第１表に示す。Next, install a gas pipe so that a mixed gas can be introduced into the glass tube from the C]F3 cylinder and Ar cylinder, and while evacuating from the outlet with an exhaust pump, ClF3 gas alone or with Ar is introduced at a predetermined pressure and amount. Introducing γ-containing gas into a glass tube,
The reaction was carried out for 2 hours. The results are shown in Table 1.
この結果より、室温でもＣｌＦ３の分圧が５Ｑｔｏｒｒ
以上、流量が２０ｃｍ／＊ｉｎ以上であれば、サンプル
を完全にガス化させ、クリーニングできることがわかる
。From this result, even at room temperature, the partial pressure of ClF3 is 5Qtorr.
The above shows that if the flow rate is 20 cm/*in or more, the sample can be completely gasified and cleaned.
（Ｊ）、 Ｔ ｆ−ＬＪ］
第
表
実施例７〜１１、比較例３．４
実施例１〜６と同し装置を使用し、同し組成のＳｉＯＸ
（ｘ ＝ １．３＞を使用してクリーニングを実施し
たが、ガラス管の出口はバルブを閉し、所定の圧力にな
るよう εＩＦ、単独またはＡｒとの混合ガスを封入し
て２時間保ち、反応状態をチエ、りした。(J), T f-LJ] Table Examples 7 to 11, Comparative Example 3.4 Using the same equipment as Examples 1 to 6, SiOX of the same composition
(x = 1.3>), the valve at the outlet of the glass tube was closed, and εIF, alone or a mixture of gas with Ar, was sealed for 2 hours to maintain the specified pressure. I checked the reaction status.
結果を第２表に示す、この結果より、温度が１００℃以
上、分圧が７６０ ｔｏｒｒ以上であればガス化が進行
し、クリーニングできることがわかる。The results are shown in Table 2. From the results, it can be seen that gasification progresses and cleaning is possible when the temperature is 100° C. or higher and the partial pressure is 760 torr or higher.
第２表
化合物を極めて良好に取り除き、りＩ；ることかできる
。The compounds of Table 2 can be removed and removed very well.
ニングすNingsu
Claims (3)
とも１種以上を含有するフッ化塩素ガスをＳｉＯ＿Ｘ（
１≦Ｘ＜２）と接触させることを特徴とするフッ化塩素
ガスによるＳｉＯ＿Ｘのクリーニング方法。(1) Chlorine fluoride gas containing at least one of ClF, ClF_3, and ClF_5 is converted into SiO_X (
1≦X<2) A method for cleaning SiO_X using chlorine fluoride gas.
＿Ｘのクリーニング方法において、室温以上でフッ化塩
素の分圧が５０ｔｏｒｒ以上でかつ空搭速度が２０ｃｍ
／ｍｉｎ以上の条件による流通方式で行うことを特徴と
するフッ化塩素ガスによるＳｉＯ＿Ｘのクリーニング方
法。(2) SiO using chlorine fluoride gas according to claim (1)
In the cleaning method of _X, the partial pressure of chlorine fluoride is 50 torr or more at room temperature or higher and the empty loading speed is 20 cm.
A method for cleaning SiO_X using chlorine fluoride gas, characterized in that it is carried out in a flow system under conditions of at least /min.
＿Ｘのクリーニング方法において、１００℃以上でかつ
フッ化塩素の分圧が７６０ｔｏｒｒ以上の条件による静
置方式で行うことを特徴とするフッ化塩素ガスによるＳ
ｉＯ＿Ｘのクリーニング方法。(3) SiO using chlorine fluoride gas according to claim (1)
In the cleaning method of
How to clean iO_X.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4048990A JP2836891B2 (en) | 1990-02-21 | 1990-02-21 | Cleaning method of SiOx with chlorine fluoride gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4048990A JP2836891B2 (en) | 1990-02-21 | 1990-02-21 | Cleaning method of SiOx with chlorine fluoride gas |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03243688A true JPH03243688A (en) | 1991-10-30 |
| JP2836891B2 JP2836891B2 (en) | 1998-12-14 |
Family
ID=12582000
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4048990A Expired - Fee Related JP2836891B2 (en) | 1990-02-21 | 1990-02-21 | Cleaning method of SiOx with chlorine fluoride gas |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2836891B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5888906A (en) * | 1996-09-16 | 1999-03-30 | Micron Technology, Inc. | Plasmaless dry contact cleaning method using interhalogen compounds |
| WO2000022660A1 (en) * | 1998-10-14 | 2000-04-20 | Tokyo Electron Limited | Method and apparatus for surface treatment |
-
1990
- 1990-02-21 JP JP4048990A patent/JP2836891B2/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5888906A (en) * | 1996-09-16 | 1999-03-30 | Micron Technology, Inc. | Plasmaless dry contact cleaning method using interhalogen compounds |
| US6503842B2 (en) * | 1996-09-16 | 2003-01-07 | Micron Technology, Inc. | Plasmaless dry contact cleaning method using interhalogen compounds |
| WO2000022660A1 (en) * | 1998-10-14 | 2000-04-20 | Tokyo Electron Limited | Method and apparatus for surface treatment |
| US7094703B2 (en) | 1998-10-14 | 2006-08-22 | Tokyo Electron Limited | Method and apparatus for surface treatment |
| US7146744B2 (en) | 1998-10-14 | 2006-12-12 | Tokyo Electron Limited | Method and apparatus for surface treatment |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2836891B2 (en) | 1998-12-14 |
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