JP2015106647A - Method of manufacturing silicon wafer - Google Patents
Method of manufacturing silicon wafer Download PDFInfo
- Publication number
- JP2015106647A JP2015106647A JP2013248106A JP2013248106A JP2015106647A JP 2015106647 A JP2015106647 A JP 2015106647A JP 2013248106 A JP2013248106 A JP 2013248106A JP 2013248106 A JP2013248106 A JP 2013248106A JP 2015106647 A JP2015106647 A JP 2015106647A
- Authority
- JP
- Japan
- Prior art keywords
- cleaning
- silicon wafer
- hydrochloric acid
- aqueous solution
- containing aqueous
- 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
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 86
- 239000010703 silicon Substances 0.000 title claims abstract description 86
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 26
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 170
- 238000004140 cleaning Methods 0.000 claims abstract description 121
- 239000007864 aqueous solution Substances 0.000 claims abstract description 67
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 39
- 238000005406 washing Methods 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 12
- -1 fluorine ions Chemical class 0.000 abstract description 25
- 229910052731 fluorine Inorganic materials 0.000 abstract description 23
- 239000011737 fluorine Substances 0.000 abstract description 23
- 239000000243 solution Substances 0.000 abstract description 5
- XJKVPKYVPCWHFO-UHFFFAOYSA-N silicon;hydrate Chemical compound O.[Si] XJKVPKYVPCWHFO-UHFFFAOYSA-N 0.000 abstract 2
- 235000012431 wafers Nutrition 0.000 description 78
- 230000000052 comparative effect Effects 0.000 description 11
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 238000005498 polishing Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 4
- 239000000460 chlorine Substances 0.000 description 4
- 229910021645 metal ion Inorganic materials 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 229910021642 ultra pure water Inorganic materials 0.000 description 3
- 239000012498 ultrapure water Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 239000003929 acidic solution Substances 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004255 ion exchange chromatography Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
Landscapes
- Cleaning Or Drying Semiconductors (AREA)
Abstract
Description
本発明は、シリコンウェーハの製造方法に関するものであり、詳しくは、ＨＦ洗浄を含む洗浄工程を経てシリコンウェーハを製造するにあたり、シリコンウェーハ表面における残留フッ素量の低減が可能なシリコンウェーハの製造方法に関するものである。 The present invention relates to a method for manufacturing a silicon wafer, and more particularly, to a method for manufacturing a silicon wafer capable of reducing the amount of residual fluorine on the surface of the silicon wafer when the silicon wafer is manufactured through a cleaning process including HF cleaning. Is.
シリコンウェーハの製造プロセスは、一般に、シリコンインゴットからのウェーハの切り出し（スライシング）、研磨やエッチング等の表面処理、洗浄工程、更にウェーハの用途に応じて必要により行われる後工程（アニール、エピタキシャル層形成等）を含む。 In general, the manufacturing process of a silicon wafer includes cutting a wafer from a silicon ingot (slicing), surface treatment such as polishing and etching, a cleaning process, and a post process (annealing, epitaxial layer formation) that is performed according to the application of the wafer. Etc.).
上記洗浄工程は、通常、ＳＣ−１洗浄、ＳＣ−２洗浄等により行われ、フッ化水素酸による洗浄（以下、「ＨＦ洗浄」ともいう。）が行われることもある（例えば特許文献１参照）。 The cleaning step is usually performed by SC-1 cleaning, SC-2 cleaning, or the like, and cleaning with hydrofluoric acid (hereinafter also referred to as “HF cleaning”) may be performed (for example, see Patent Document 1). ).
近年、シリコンウェーハの洗浄工程において、シリコンウェーハ表面の高清浄度化を実現するために、最終洗浄処理にフッ化水素酸（ＨＦ洗浄）を使用する方式が適用されている。しかし、ＨＦ洗浄後のシリコンウェーハ表面には、通常、フッ素イオン（Ｆ-）が残留している。フッ素イオンが表面に残留したシリコンウェーハを用いて半導体デバイスを製造すると、製造プロセス初期に実施されるゲート酸化膜形成処理時に、酸化膜形成異常（膜厚低下）を引き起こすおそれがある。そのため、ＨＦ洗浄を施したシリコンウェーハにおける残留フッ素イオン量を低減することが求められている。 In recent years, in a silicon wafer cleaning process, a method using hydrofluoric acid (HF cleaning) has been applied to the final cleaning process in order to achieve high cleanliness of the silicon wafer surface. However, fluorine ions (F − ) usually remain on the surface of the silicon wafer after HF cleaning. When a semiconductor device is manufactured using a silicon wafer in which fluorine ions remain on the surface, an oxide film formation abnormality (thickness reduction) may occur during a gate oxide film formation process performed in the initial stage of the manufacturing process. Therefore, it is required to reduce the amount of residual fluorine ions in a silicon wafer subjected to HF cleaning.
そこで本発明の目的は、ＨＦ洗浄を含み、かつフッ素イオンの残留の少ないシリコンウェーハを得ることのできるシリコンウェーハの製造方法を提供することにある。 SUMMARY OF THE INVENTION An object of the present invention is to provide a method for producing a silicon wafer, which includes a HF cleaning and can obtain a silicon wafer with little residual fluorine ions.
本発明者は上記目的を達成するために鋭意検討を重ねた結果、ＨＦ洗浄後の次工程の湿式処理として塩酸含有水溶液による洗浄（すすぎ洗い）を行うことにより、ＨＦ洗浄後のシリコンウェーハ表面に残留したフッ素イオンを高度に除去することが可能であることを新たに見出した。この点について、本発明者は以下のように推察している。
フッ素イオンＦ-は、電気陰性度が最も高いイオンであり、シリコンウェーハ表面で強固なイオン結合を形成しウェーハ表面に留まるが、塩酸含有水溶液によりすすぎ洗いすることで、Ｆ-の存在を抑制し、ウェーハ表面に留まっていたフッ素を中性状態のＨＦとして除去することができる。ただし、ＨＦ洗浄の次工程の湿式処理として、塩酸含有水溶液による洗浄以外の処理、例えば水洗や他の薬液による洗浄を行うと、シリコンウェーハ表面からフッ素イオンを高度に除去することは困難であることも、本発明者の検討の結果、明らかとなった。
本発明は、以上の知見に基づき完成された。
As a result of intensive studies to achieve the above object, the present inventor performed cleaning (rinsing) with a hydrochloric acid-containing aqueous solution as a wet process in the next step after HF cleaning, so that the surface of the silicon wafer after HF cleaning It was newly found that the remaining fluorine ions can be removed to a high degree. About this point, this inventor guesses as follows.
Fluorine ion F − is the ion with the highest electronegativity and forms a strong ionic bond on the silicon wafer surface and stays on the wafer surface. Rinse with an aqueous solution containing hydrochloric acid suppresses the presence of F −. The fluorine remaining on the wafer surface can be removed as neutral HF. However, it is difficult to remove fluorine ions from the silicon wafer surface to a high degree when wet processing of the next step of HF cleaning is performed other than cleaning with an aqueous solution containing hydrochloric acid, such as cleaning with water or other chemicals. As a result of the study by the present inventor, it became clear.
The present invention has been completed based on the above findings.
即ち、上記目的は、
シリコンウェーハを準備する工程と、
前記シリコンウェーハの表面を洗浄する工程と、
を含むシリコンウェーハの製造方法であって、
前記洗浄工程は、
フッ化水素酸による洗浄と、
フッ化水素酸による洗浄の次工程の湿式処理として塩酸含有水溶液による洗浄と、
を含む、シリコンウェーハの製造方法、
により達成された。
That is, the above purpose is
Preparing a silicon wafer;
Cleaning the surface of the silicon wafer;
A method for producing a silicon wafer comprising:
The washing step includes
Cleaning with hydrofluoric acid,
As a wet treatment of the next step of washing with hydrofluoric acid, washing with an aqueous solution containing hydrochloric acid,
Including a method for manufacturing a silicon wafer,
Achieved by.
一態様では、上記塩酸含有水溶液は、酸成分として塩酸のみを含む水溶液である。 In one embodiment, the hydrochloric acid-containing aqueous solution is an aqueous solution containing only hydrochloric acid as an acid component.
一態様では、上記塩酸含有水溶液は、塩酸を質量基準で０．０１ｐｐｍ以上含む。 In one aspect | mode, the said hydrochloric acid containing aqueous solution contains 0.01 ppm or more of hydrochloric acid on a mass basis.
一態様では、上記塩酸含有水溶液は、塩酸を質量基準で１０００ｐｐｍ以下含む。 In one aspect | mode, the said hydrochloric acid containing aqueous solution contains 1000 ppm or less of hydrochloric acid on a mass basis.
一態様では、上記塩酸含有水溶液による洗浄時間は、５分以下である。 In one aspect | mode, the washing | cleaning time by the said hydrochloric acid containing aqueous solution is 5 minutes or less.
一態様では、前記フッ化水素酸による洗浄の前にＳＣ−１洗浄および水洗からなる群から選択される一種以上の洗浄を行う。 In one aspect, at least one type of cleaning selected from the group consisting of SC-1 cleaning and water cleaning is performed before the cleaning with hydrofluoric acid.
一態様では、上記塩酸含有水溶液による洗浄の後に、水洗およびオゾン水による洗浄からなる群から選択される一種以上の洗浄を行う。 In one aspect, after washing with the hydrochloric acid-containing aqueous solution, one or more kinds of washing selected from the group consisting of washing with water and washing with ozone water are performed.
本発明によれば、ＨＦ洗浄を経ているにもかかわらずフッ素イオンの残留が少ないシリコンウェーハを提供することができる。 According to the present invention, it is possible to provide a silicon wafer with little fluorine ion residue despite HF cleaning.
本発明は、シリコンウェーハを準備する工程と、前記シリコンウェーハの表面を洗浄する工程と、を含むシリコンウェーハの製造方法に関する。本発明のシリコンウェーハの製造方法において、上記洗浄工程は、フッ化水素酸による洗浄（ＨＦ洗浄）と、フッ化水素酸による洗浄の次工程の湿式処理として塩酸含有水溶液による洗浄と、を含む。
以下、本発明のシリコンウェーハの製造方法について、更に詳細に説明する。
The present invention relates to a method for manufacturing a silicon wafer, including a step of preparing a silicon wafer and a step of cleaning the surface of the silicon wafer. In the method for producing a silicon wafer of the present invention, the cleaning step includes cleaning with hydrofluoric acid (HF cleaning) and cleaning with a hydrochloric acid-containing aqueous solution as a wet process in the next step of cleaning with hydrofluoric acid.
Hereafter, the manufacturing method of the silicon wafer of this invention is demonstrated in detail.
シリコンウェーハを準備する工程
洗浄工程が施されるシリコンウェーハは、公知の方法により準備することができる。例えば、ＣＺ法等により育成されたシリコンインゴットからのウェーハを切り出し（スライシング）、得られたシリコンウェーハを、粗研磨（ラッピング）、エッチング、研磨（ポリッシング）等の表面処理に付すことにより、洗浄工程が施されるシリコンウェーハを準備することができる。ただし本発明は、上記の方法に特に限定されるものではない。また、市販のシリコンウェーハを入手することも、シリコンウェーハを準備する工程の一態様として、本発明に包含されるものとする。
A silicon wafer subjected to a process cleaning step for preparing a silicon wafer can be prepared by a known method. For example, a cleaning process is performed by cutting out (slicing) a wafer from a silicon ingot grown by the CZ method or the like, and subjecting the obtained silicon wafer to surface treatment such as rough polishing (lapping), etching, or polishing (polishing). Can be prepared. However, the present invention is not particularly limited to the above method. In addition, obtaining a commercially available silicon wafer is also included in the present invention as one aspect of a process for preparing a silicon wafer.
洗浄工程
本発明のシリコンウェーハの製造方法における洗浄工程は、少なくとも、ＨＦ洗浄と、ＨＦ洗浄の次工程の湿式処理として行われる塩酸含有水溶液による洗浄と、を含む。ここで、フッ化水素酸による洗浄（ＨＦ洗浄）の次工程の湿式処理として塩酸含有水溶液による洗浄を含むとは、ＨＦ洗浄の後に、水、洗浄液等の液体をＨＦ洗浄後のシリコンウェーハ表面に接触させる処理を行わずに、塩酸含有水溶液による洗浄を行うことをいうものとする。このように、ＨＦ洗浄後の次工程の湿式処理として塩酸含有水溶液による洗浄を行うことにより、ＨＦ処理後にシリコンウェーハ表面に残留したフッ素イオンを高度に除去することができる。
Cleaning Step The cleaning step in the method for producing a silicon wafer of the present invention includes at least HF cleaning and cleaning with a hydrochloric acid-containing aqueous solution performed as a wet process in the next step of HF cleaning. Here, the wet process in the next step of cleaning with hydrofluoric acid (HF cleaning) includes cleaning with a hydrochloric acid-containing aqueous solution. After HF cleaning, liquids such as water and cleaning liquid are applied to the silicon wafer surface after HF cleaning. It shall mean washing with a hydrochloric acid-containing aqueous solution without performing the contact treatment. Thus, by performing cleaning with a hydrochloric acid-containing aqueous solution as a wet process in the next step after HF cleaning, fluorine ions remaining on the silicon wafer surface after HF processing can be highly removed.
（ｉ）ＨＦ洗浄
ＨＦ洗浄は、シリコンウェーハに通常施されるＨＦ洗浄と同様に行うことができる。例えば、弗酸濃度０．０１〜５質量％程度のフッ化水素酸（ＨＦ水溶液）をシリコンウェーハ表面と接触させることにより、シリコンウェーハ表面をフッ化水素酸により洗浄することができる。シリコンウェーハ表面とフッ化水素酸との接触は、例えば、フッ化水素酸を含む液槽にシリコンウェーハを浸漬することにより行うことができる。洗浄時のフッ化水素酸は、常温であっても加熱または冷却してもよく、液温は特に限定されるものではない。なお常温とは、温度制御（加熱または冷却）がされていない状態の温度をいうものとする。シリコンウェーハとフッ化水素酸との接触時間（洗浄時間）も特に限定されるものではなく、一例として、例えば０．５〜１０分程度とすることができる。なおＨＦ洗浄によりシリコンウェーハ表層の自然酸化膜（ＳｉＯ2膜）を完全に除去してもよく、一部を残してよい。自然酸化膜を完全に除去すると、ウォーターマークの発生等によりＬＰＤ（Light Point Defect）品質が低下することがあるため、ＨＦ洗浄後に自然酸化膜をわずかに（例えば膜厚０．５ｎｍ以下程度）残すことが好ましい場合もあるが、本発明では、特に限定されるものではない。自然酸化膜が残留しているシリコンウェーハ表面は親水性が高いためフッ素イオンがより残留しやすい傾向があるが、そのような場合であっても本発明によれば、後述のアンモニア系洗浄液による洗浄によりフッ素イオンを除去し、残留フッ素イオンの少ないシリコンウェーハを提供することができる。
(I) HF cleaning HF cleaning can be performed in the same manner as HF cleaning that is normally performed on silicon wafers. For example, the silicon wafer surface can be cleaned with hydrofluoric acid by bringing hydrofluoric acid (HF aqueous solution) having a hydrofluoric acid concentration of about 0.01 to 5% by mass into contact with the silicon wafer surface. The contact between the silicon wafer surface and hydrofluoric acid can be performed, for example, by immersing the silicon wafer in a liquid bath containing hydrofluoric acid. Hydrofluoric acid at the time of washing may be at room temperature or heated or cooled, and the liquid temperature is not particularly limited. The normal temperature refers to a temperature in which temperature control (heating or cooling) is not performed. The contact time (cleaning time) between the silicon wafer and hydrofluoric acid is not particularly limited, and can be, for example, about 0.5 to 10 minutes. The natural oxide film (SiO 2 film) on the surface layer of the silicon wafer may be completely removed by HF cleaning, or a part thereof may be left. If the natural oxide film is completely removed, the quality of the LPD (Light Point Defect) may deteriorate due to the generation of a watermark, etc., so that the natural oxide film remains slightly after the HF cleaning (for example, about 0.5 nm or less). In some cases, the present invention is not particularly limited. Although the surface of the silicon wafer where the natural oxide film remains is highly hydrophilic, fluorine ions tend to remain more easily. Even in such a case, according to the present invention, cleaning with an ammonia-based cleaning liquid described later is performed. By removing fluorine ions, a silicon wafer with little residual fluorine ions can be provided.
（ｉｉ）塩酸含有水溶液による洗浄
本発明のシリコンウェーハの製造方法では、上記ＨＦ洗浄が施されたシリコンウェーハに、ＨＦ洗浄の次工程の湿式処理として、塩酸含有水溶液による洗浄を施す。これにより、ＨＦ洗浄後のシリコンウェーハ表面に残留したフッ素イオンを高度に除去し、残留フッ素イオン量の少ないシリコンウェーハを提供することが可能となる。
(Ii) Cleaning with hydrochloric acid-containing aqueous solution In the method for producing a silicon wafer according to the present invention, the silicon wafer subjected to the HF cleaning is cleaned with a hydrochloric acid-containing aqueous solution as a wet process in the next step of HF cleaning. As a result, it is possible to highly remove fluorine ions remaining on the surface of the silicon wafer after HF cleaning and provide a silicon wafer with a small amount of residual fluorine ions.
上記洗浄に用いる塩酸含有水溶液は、塩酸ＨＣｌの濃度が、質量基準で０．００１ｐｐｍ以上であることが好ましく、シリコンウェーハ表面からフッ素イオンをより効率的に除去する観点からは、０．０１ｐｐｍ以上であることが好ましい。塩酸濃度が高いほど、フッ素イオンの除去効率の点からは好ましいが、塩酸濃度が高いほど、塩素イオンＣｌ-が、ウェーハ表面に付着していた金属イオンや水溶液中に含まれていた金属イオンと塩を形成することにより、ウェーハ表面のパーティクル発生頻度が高まる。一般に、塩素イオン濃度が１×１０11ａｔｏｍｓ／ｃｍ2以上になるとパーティクル発生頻度が高まるため、塩酸濃度は、系内の塩素イオン濃度が１×１０11ａｔｏｍｓ／ｃｍ2以上にならないように設定することが好ましい。この点から、上記塩酸含有水溶液の塩酸濃度は、質量基準で１０００ｐｐｍ以下とすることが好ましい。ただし、キレート剤の使用による金属イオンの除去等の手段により系内の金属イオン量を低減することができれば、塩酸濃度が１０００ｐｐｍを超える塩酸含有水溶液の使用も可能である。この点から、上記塩酸含有水溶液の塩酸濃度は、例えば３０００ｐｐｍ以下であっても、２０００ｐｐｍ以下であってもよい。 The hydrochloric acid-containing aqueous solution used for the cleaning preferably has a hydrochloric acid HCl concentration of 0.001 ppm or more on a mass basis, and from the viewpoint of more efficiently removing fluorine ions from the silicon wafer surface, the concentration is 0.01 ppm or more. Preferably there is. Higher concentration of hydrochloric acid is high, is preferable from the viewpoint of removal efficiency of fluoride ions, the higher the concentration of hydrochloric acid, chlorine ions Cl - is a metal ion contained in the metal ion and the aqueous solution adhering to the wafer surface By forming the salt, the frequency of particle generation on the wafer surface is increased. In general, when the chlorine ion concentration becomes 1 × 10 11 atoms / cm 2 or more, the frequency of particle generation increases. Therefore, the hydrochloric acid concentration is set so that the chlorine ion concentration in the system does not become 1 × 10 11 atoms / cm 2 or more. It is preferable. From this point, the hydrochloric acid concentration of the hydrochloric acid-containing aqueous solution is preferably 1000 ppm or less on a mass basis. However, if the amount of metal ions in the system can be reduced by means such as removal of metal ions by using a chelating agent, it is possible to use a hydrochloric acid-containing aqueous solution having a hydrochloric acid concentration exceeding 1000 ppm. From this point, the hydrochloric acid concentration of the hydrochloric acid-containing aqueous solution may be, for example, 3000 ppm or less or 2000 ppm or less.
上記塩酸含有水溶液には、塩酸以外の酸成分が共存していてもよく、共存していなくてもよい。塩酸以外の酸が共存する酸性溶液では、
・共存する酸が、ウェーハ表面に留まっていたフッ素イオンと酸性溶液に含まれていた酸により生成されたＨＦとともに、シリコンウェーハ表面をエッチングし面荒れを起こす；
・共存する酸がシリコンウェーハ表面に強固に付着してしまう；
・共存する酸が酸化力が強いものであると配管部材等の腐食の原因となる；
といった現象が発生する場合がある。これに対し、酸成分として塩酸のみを含む酸性水溶液であれば、上記現象の発生なく、ＨＦ洗浄後にシリコンウェーハ表面に残留したフッ素イオンを除去することが可能となる。したがって上記塩酸含有水溶液は、酸成分として塩酸のみを含む水溶液であることが好ましい。また、上記塩酸含有水溶液には、酸成分以外の成分も含まれていてもよい。そのような成分としては、例えば非イオン性界面活性剤、増粘剤（水溶性高分子）等の、塩酸とフッ素イオンとのＨＦ生成反応を妨げない成分が好ましい。
In the hydrochloric acid-containing aqueous solution, an acid component other than hydrochloric acid may or may not coexist. In acidic solutions where acids other than hydrochloric acid coexist,
The coexisting acid etches the surface of the silicon wafer together with the fluorine ions remaining on the wafer surface and the HF generated by the acid contained in the acidic solution to cause surface roughness;
-The coexisting acid adheres firmly to the silicon wafer surface;
-If the coexisting acid has strong oxidizing power, it may cause corrosion of piping members, etc .;
Such a phenomenon may occur. In contrast, an acidic aqueous solution containing only hydrochloric acid as an acid component can remove fluorine ions remaining on the surface of the silicon wafer after HF cleaning without the above phenomenon. Therefore, the hydrochloric acid-containing aqueous solution is preferably an aqueous solution containing only hydrochloric acid as an acid component. The hydrochloric acid-containing aqueous solution may also contain components other than the acid component. As such a component, a component that does not interfere with the HF generation reaction between hydrochloric acid and fluoride ions, such as a nonionic surfactant and a thickener (water-soluble polymer), is preferable.
ＨＦ洗浄と同様、上記塩酸含有水溶液による洗浄は、例えば、上記塩酸含有水溶液をシリコンウェーハ表面と接触させることによって行うことができる。シリコンウェーハ表面と上記塩酸含有水溶液との接触は、例えば、上記塩酸含有水溶液を含む液槽にシリコンウェーハを浸漬することにより行うことができる。洗浄時の塩酸含有水溶液は、常温であっても加熱または冷却してもよく、液温は特に限定されるものではない。シリコンウェーハと上記塩酸含有水溶液との接触時間（洗浄時間）は、例えば５分以下であることが好ましく、フッ素イオンを効率的に除去する観点からは、２分以上であることが好ましい。 As with the HF cleaning, the cleaning with the hydrochloric acid-containing aqueous solution can be performed, for example, by bringing the hydrochloric acid-containing aqueous solution into contact with the silicon wafer surface. The contact between the silicon wafer surface and the hydrochloric acid-containing aqueous solution can be performed, for example, by immersing the silicon wafer in a liquid bath containing the hydrochloric acid-containing aqueous solution. The hydrochloric acid-containing aqueous solution at the time of washing may be heated or cooled at room temperature, and the liquid temperature is not particularly limited. The contact time (cleaning time) between the silicon wafer and the hydrochloric acid-containing aqueous solution is preferably 5 minutes or less, for example, and preferably 2 minutes or more from the viewpoint of efficiently removing fluorine ions.
（ｉｉｉ）任意の洗浄
本発明のシリコンウェーハの洗浄工程は、上述のＨＦ洗浄と、ＨＦ洗浄の次工程の湿式処理として行われる塩酸含有水溶液による洗浄を必須の洗浄処理として含むが、これら必須の洗浄処理の前後に、他の洗浄処理を行うこともできる。他の洗浄処理としては、半導体基板の洗浄処理として従来公知の各種洗浄処理、例えば、ＳＣ−１洗浄、オゾン水による洗浄、水洗等の１つ以上を行うことができる。ここでＳＣ−１洗浄とは、アンモニア水／Ｈ2Ｏ2／Ｈ2Ｏが混合されたＳＣ１液による洗浄処理をいうものとする。ＳＣ１液は、常温であっても加熱または冷却されていてもよい。また、洗浄に用いるオゾン水のオゾン濃度は、質量基準で２〜２０ｐｐｍ程度とすることが好適である。水洗に用いる水およびオゾン水は、常温であっても、加熱または冷却してもよい。処理時間は、特に限定されるものではない。上記塩酸含有水溶液による洗浄の後に任意に行う洗浄処理としては、水洗およびオゾン水による洗浄のいずれかまたは両方の洗浄が好ましい。また、ＨＦ洗浄前に任意に行う洗浄処理としては、表面に存在するパーティクル成分除去の点から、ＳＣ−１洗浄および水洗のいずれかまたは両方が好ましい。
(Iii) Arbitrary cleaning The silicon wafer cleaning process of the present invention includes the above-described HF cleaning and cleaning with a hydrochloric acid-containing aqueous solution performed as a wet process in the next process of HF cleaning as essential cleaning processes. Other cleaning processes can be performed before and after the cleaning process. As another cleaning process, one or more of various conventionally known cleaning processes such as SC-1 cleaning, cleaning with ozone water, and water cleaning can be performed as the semiconductor substrate cleaning process. Here, the SC-1 cleaning refers to a cleaning process using an SC1 solution in which ammonia water / H 2 O 2 / H 2 O is mixed. The SC1 solution may be at room temperature or heated or cooled. The ozone concentration of ozone water used for cleaning is preferably about 2 to 20 ppm on a mass basis. Water used for washing and ozone water may be heated or cooled at room temperature. The processing time is not particularly limited. As the washing treatment optionally performed after washing with the hydrochloric acid-containing aqueous solution, either or both of washing with water and washing with ozone water are preferable. In addition, as the cleaning treatment that is optionally performed before HF cleaning, either or both of SC-1 cleaning and water cleaning are preferable from the viewpoint of removing particle components present on the surface.
洗浄処理後のシリコンウェーハは、任意に乾燥等の後処理に付すことができ、また必要に応じてアニール等の用途に応じた後工程に付すことができる。 The silicon wafer after the cleaning treatment can be optionally subjected to a post-treatment such as drying, and can be subjected to a post-process corresponding to the application such as annealing as necessary.
以上説明した本発明のシリコンウェーハの製造方法によれば、ＨＦ洗浄後の残留フッ素イオン量の少ないシリコンウェーハを提供することができる。 According to the method for producing a silicon wafer of the present invention described above, a silicon wafer having a small amount of residual fluorine ions after HF cleaning can be provided.
以下、本発明を実施例に基づき更に説明する。ただし、本発明は実施例に示す態様に限定されるものではない。また、以下に記載の「ｐｐｍ」、「％」は、いずれも質量基準である。また、特記しない限り、各操作は温度制御せず室温（約２５℃）で実施した。以下に記載の常温とは、室温下に置かれていたことを意味する。また、以下に記載の塩酸含有水溶液としては、酸成分として塩酸のみを添加した水溶液を用いた。 Hereinafter, the present invention will be further described based on examples. However, this invention is not limited to the aspect shown in the Example. Further, “ppm” and “%” described below are based on mass. Unless otherwise specified, each operation was performed at room temperature (about 25 ° C.) without temperature control. The normal temperature described below means being placed at room temperature. Moreover, as the hydrochloric acid-containing aqueous solution described below, an aqueous solution in which only hydrochloric acid was added as an acid component was used.
［実施例１］
１．第一段階（ＳＣ−１洗浄）
仕上研磨を施した後のシリコンウェーハ（直径：３００ｍｍ）を準備した。準備したシリコンウェーハを、６０℃の２９質量％アンモニア水：３０質量％Ｈ2Ｏ2：Ｈ2Ｏ ＝ ０．５：１：１０（体積比）で調合した溶液にて４分間間洗浄した。
２・第二段階（水洗）
第一段階の処理を行ったシリコンウェーハを、常温の超純水にて４分間、連続注水方式でリンス処理を行った。
３．第三段階（ＨＦ洗浄）
第二段階の処理を行ったシリコンウェーハを、常温の０．０５質量％ＨＦ溶液（フッ化水素酸）に４分間浸漬し、ＨＦ洗浄を行った。
４．第四段階（塩酸含有水溶液による洗浄）
第三段階の処理を行ったシリコンウェーハを、他の湿式処理を行うことなく直ちに、塩酸濃度が質量基準で０．００５ｐｐｍの常温の塩酸含有水溶液に４分間浸漬し、洗浄処理を行った。
５．第五段階（水洗）
第一段階の処理を行ったシリコンウェーハを、常温の超純水にて４分間、連続注水方式でリンス処理を行った。
[Example 1]
1. First stage (SC-1 cleaning)
A silicon wafer (diameter: 300 mm) after finishing polishing was prepared. The prepared silicon wafer was washed for 4 minutes with a solution prepared by 29% by mass ammonia water at 60 ° C .: 30% by mass H 2 O 2 : H 2 O = 0.5: 1: 10 (volume ratio).
2. Second stage (washing with water)
The silicon wafer subjected to the first stage treatment was rinsed by continuous water injection for 4 minutes with ultrapure water at room temperature.
3. Third stage (HF cleaning)
The silicon wafer subjected to the second stage treatment was immersed in a 0.05 mass% HF solution (hydrofluoric acid) at room temperature for 4 minutes to perform HF cleaning.
4). Fourth stage (cleaning with hydrochloric acid-containing aqueous solution)
The silicon wafer subjected to the third stage treatment was immediately immersed in a hydrochloric acid-containing aqueous solution having a hydrochloric acid concentration of 0.005 ppm on a mass basis for 4 minutes without performing another wet treatment, and was subjected to a washing treatment.
5. 5th stage (washing)
The silicon wafer subjected to the first stage treatment was rinsed by continuous water injection for 4 minutes with ultrapure water at room temperature.
［実施例２］
第四段階において用いる塩酸含有水溶液を、塩酸濃度０．０１ｐｐｍの塩酸含有水溶液に変更した点以外、実施例１と同様の処理を実施した。
[Example 2]
The same treatment as in Example 1 was performed except that the hydrochloric acid-containing aqueous solution used in the fourth stage was changed to a hydrochloric acid-containing aqueous solution having a hydrochloric acid concentration of 0.01 ppm.
［実施例３］
第四段階において用いる塩酸含有水溶液を、塩酸濃度１ｐｐｍの塩酸含有水溶液に変更した点以外、実施例１と同様の処理を実施した。
[Example 3]
The same treatment as in Example 1 was performed except that the hydrochloric acid-containing aqueous solution used in the fourth stage was changed to a hydrochloric acid-containing aqueous solution having a hydrochloric acid concentration of 1 ppm.
［実施例４］
第四段階において用いる塩酸含有水溶液を、塩酸濃度１０００ｐｐｍの塩酸含有水溶液に変更した点以外、実施例１と同様の処理を実施した。
[Example 4]
The same treatment as in Example 1 was performed, except that the hydrochloric acid-containing aqueous solution used in the fourth stage was changed to a hydrochloric acid-containing aqueous solution having a hydrochloric acid concentration of 1000 ppm.
［実施例５］
第四段階において用いる塩酸含有水溶液を、塩酸濃度２０００ｐｐｍの塩酸含有水溶液に変更した点以外、実施例１と同様の処理を実施した。
[Example 5]
The same treatment as in Example 1 was performed except that the hydrochloric acid-containing aqueous solution used in the fourth stage was changed to a hydrochloric acid-containing aqueous solution having a hydrochloric acid concentration of 2000 ppm.
［比較例１］
第四段階の塩酸含有水溶液による洗浄を実施しなかった点以外、実施例１と同様の処理を実施した。
[Comparative Example 1]
The same treatment as in Example 1 was performed, except that the fourth stage hydrochloric acid-containing aqueous solution was not washed.
［比較例２］
第四段階の塩酸含有水溶液による洗浄を、オゾン濃度１０ｐｐｍのオゾン水にて４分間、連続供給方式で行う洗浄処理に変更した点以外、実施例１と同様の処理を実施した。
[Comparative Example 2]
The same treatment as in Example 1 was carried out except that the washing with the hydrochloric acid-containing aqueous solution in the fourth stage was changed to a washing treatment performed by ozone water having an ozone concentration of 10 ppm for 4 minutes by a continuous supply method.
［比較例３］
第三段階のＨＦ洗浄と第四段階の塩酸含有水溶液による洗浄との間に、常温の超純水にて４分間、連続注水方式でリンス処理を行った点以外、実施例１と同様の処理を実施した。
[Comparative Example 3]
The same treatment as in Example 1 except that the rinsing treatment was performed by continuous water injection for 4 minutes with ultrapure water at room temperature between the third stage HF washing and the fourth stage washing with hydrochloric acid-containing aqueous solution. Carried out.
［比較例４］
第三段階のＨＦ洗浄と第四段階の塩酸含有水溶液による洗浄との間に、オゾン濃度１０ｐｐｍのオゾン水にて４分間、連続供給方式で洗浄処理を行った点以外、実施例１と同様の処理を実施した。
[Comparative Example 4]
The same as in Example 1 except that the cleaning process was performed in a continuous supply system for 4 minutes with ozone water having an ozone concentration of 10 ppm between the third stage HF cleaning and the fourth stage hydrochloric acid-containing aqueous solution. Processing was carried out.
＜評価方法＞
１．フッ素イオン（Ｆ-）濃度、塩素イオン（Ｃｌ-）濃度の測定
洗浄後のシリコンウェーハ表面に存在するフッ素イオン濃度および塩素イオン濃度を、イオンクロマトグラフ法により測定した。
２．ヘイズ値の測定
ヘイズ値は、洗浄後のシリコンウェーハ表面をパーティクルカウンター（KLA-Tencor社製ＳＰ−２）により測定し、ＤＷＯモードで得られる値により確認した。
<Evaluation method>
1. Measurement of Fluorine Ion (F − ) Concentration and Chlorine Ion (Cl − ) Concentration The fluorine ion concentration and the chlorine ion concentration present on the cleaned silicon wafer surface were measured by ion chromatography.
2. Measurement of haze value The haze value was confirmed by measuring the surface of the cleaned silicon wafer with a particle counter (SP-2 manufactured by KLA-Tencor) and checking the value obtained in the DWO mode.
以上の結果を、表１に示す。 The results are shown in Table 1.
表１に示すように、ＨＦ洗浄後の次工程の湿式処理として塩酸含有水溶液による洗浄を行った実施例１〜５では、ＨＦ処理後の次工程の湿式処理として塩酸含有水溶液による洗浄を行わず水洗を行った比較例１と比べて、フッ素イオン濃度が低減された。
また、ＨＦ洗浄後に塩酸含有水溶液による洗浄に代えてオゾン水による洗浄を行った比較例２では、オゾン水による洗浄を行わなかった比較例１よりも高いフッ素イオン濃度が確認された。
一方、ＨＦ洗浄と塩酸含有水溶液による洗浄との間に、他の湿式処理を行った比較例３、４（比較例３；水洗、比較例４；オゾン水による洗浄）では、実施例１〜５のようにシリコンウェーハ表面からフッ素イオンを高度に除去することはできなかった。
以上の結果から、ＨＦ洗浄の次工程の湿式処理として塩酸含有水溶液による洗浄を行うことで、ＨＦ処理後にシリコンウェーハ表面に残留したフッ素イオンを高度に除去できることが確認された。
また、実施例１〜５では、比較例と比べてヘイズの値は同程度以下であったことから、表面を大きく荒らすことなく、ＨＦ処理後にシリコンウェーハ表面に残留したフッ素イオンを効率的に除去できることも確認された。
更に、実施例同士の対比から、フッ素イオンをより効率的に除去する観点からは、塩酸を質量基準で０．０１ｐｐｍ以上含む塩酸含有水溶液を用いることが好ましいこと（実施例２〜５）、およびシリコンウェーハ表面の残留塩素イオン量低減の観点からは、塩酸を質量基準で１０００ｐｐｍ以下含む塩酸含有水溶液を用いることが好ましいこと（実施例１〜４）も確認できる。
As shown in Table 1, in Examples 1 to 5 in which cleaning with a hydrochloric acid-containing aqueous solution was performed as a wet process in the next step after HF cleaning, cleaning with a hydrochloric acid-containing aqueous solution was not performed as a wet processing in the next step after HF processing. Compared with the comparative example 1 which washed with water, the fluorine ion concentration was reduced.
Further, in Comparative Example 2 in which cleaning with ozone water was performed instead of cleaning with a hydrochloric acid-containing aqueous solution after HF cleaning, a higher fluorine ion concentration was confirmed than in Comparative Example 1 in which cleaning with ozone water was not performed.
On the other hand, in Comparative Examples 3 and 4 (Comparative Example 3; water washing, Comparative Example 4; washing with ozone water) in which another wet treatment was performed between the HF cleaning and the hydrochloric acid-containing aqueous solution, Examples 1 to 5 Thus, fluorine ions could not be removed from the silicon wafer surface to a high degree.
From the above results, it was confirmed that fluorine ions remaining on the surface of the silicon wafer after HF treatment can be highly removed by washing with an aqueous solution containing hydrochloric acid as a wet treatment in the next step of HF cleaning.
Moreover, in Examples 1-5, since the value of haze was comparable or less compared with a comparative example, the fluorine ion which remained on the silicon wafer surface after HF processing was removed efficiently, without greatly roughening the surface. It was also confirmed that it was possible.
Furthermore, it is preferable to use a hydrochloric acid-containing aqueous solution containing 0.01 ppm or more of hydrochloric acid on a mass basis from the viewpoint of more efficiently removing fluorine ions from the comparison between Examples (Examples 2 to 5), and From the viewpoint of reducing the amount of residual chlorine ions on the silicon wafer surface, it can also be confirmed that it is preferable to use a hydrochloric acid-containing aqueous solution containing 1000 ppm or less of hydrochloric acid on a mass basis (Examples 1 to 4).
本発明は、半導体基板の製造分野において有用である。 The present invention is useful in the field of manufacturing semiconductor substrates.
Claims (7)
前記シリコンウェーハの表面を洗浄する工程と、
を含むシリコンウェーハの製造方法であって、
前記洗浄工程は、
フッ化水素酸による洗浄と、
フッ化水素酸による洗浄の次工程の湿式処理として塩酸含有水溶液による洗浄と、
を含む、シリコンウェーハの製造方法。 Preparing a silicon wafer;
Cleaning the surface of the silicon wafer;
A method for producing a silicon wafer comprising:
The washing step includes
Cleaning with hydrofluoric acid,
As a wet treatment of the next step of washing with hydrofluoric acid, washing with an aqueous solution containing hydrochloric acid,
A method for manufacturing a silicon wafer.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2013248106A JP6529715B2 (en) | 2013-11-29 | 2013-11-29 | Method of manufacturing silicon wafer |
| TW103129307A TWI615896B (en) | 2013-11-29 | 2014-08-26 | 矽 Wafer manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2013248106A JP6529715B2 (en) | 2013-11-29 | 2013-11-29 | Method of manufacturing silicon wafer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2015106647A true JP2015106647A (en) | 2015-06-08 |
| JP6529715B2 JP6529715B2 (en) | 2019-06-12 |
Family
ID=53436603
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2013248106A Active JP6529715B2 (en) | 2013-11-29 | 2013-11-29 | Method of manufacturing silicon wafer |
Country Status (2)
| Country | Link |
|---|---|
| JP (1) | JP6529715B2 (en) |
| TW (1) | TWI615896B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111199869A (en) * | 2018-11-19 | 2020-05-26 | 长鑫存储技术有限公司 | Wafer cleaning method |
| CN114669546A (en) * | 2022-04-18 | 2022-06-28 | 广东先导微电子科技有限公司 | Method for cleaning indium phosphide polycrystal material |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107863288A (en) * | 2016-09-22 | 2018-03-30 | 中芯国际集成电路制造(上海)有限公司 | A kind of method for cleaning Semiconductor substrate |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05226315A (en) * | 1992-02-10 | 1993-09-03 | Sharp Corp | Manufacture of semiconductor device |
| JPH07263392A (en) * | 1994-03-18 | 1995-10-13 | Fujitsu Ltd | Manufacture of semiconductor device |
| JPH11204478A (en) * | 1998-01-19 | 1999-07-30 | Mitsubishi Electric Corp | Method and apparatus for cleaning semiconductor substrate |
| JP2000290693A (en) * | 1999-04-12 | 2000-10-17 | Japan Organo Co Ltd | Cleaning of electronic parts and members |
| JP2006270115A (en) * | 2006-05-22 | 2006-10-05 | Dainippon Screen Mfg Co Ltd | Substrate treatment apparatus and substrate treatment method |
| JP2006295189A (en) * | 2005-04-13 | 2006-10-26 | Samsung Electronics Co Ltd | Semiconductor substrate processing equipment, equipment and method for cleaning semiconductor substrate |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6368416B1 (en) * | 1999-07-01 | 2002-04-09 | Lam Research Corporation | Method for validating pre-process adjustments to a wafer cleaning system |
-
2013
- 2013-11-29 JP JP2013248106A patent/JP6529715B2/en active Active
-
2014
- 2014-08-26 TW TW103129307A patent/TWI615896B/en active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05226315A (en) * | 1992-02-10 | 1993-09-03 | Sharp Corp | Manufacture of semiconductor device |
| JPH07263392A (en) * | 1994-03-18 | 1995-10-13 | Fujitsu Ltd | Manufacture of semiconductor device |
| JPH11204478A (en) * | 1998-01-19 | 1999-07-30 | Mitsubishi Electric Corp | Method and apparatus for cleaning semiconductor substrate |
| JP2000290693A (en) * | 1999-04-12 | 2000-10-17 | Japan Organo Co Ltd | Cleaning of electronic parts and members |
| JP2006295189A (en) * | 2005-04-13 | 2006-10-26 | Samsung Electronics Co Ltd | Semiconductor substrate processing equipment, equipment and method for cleaning semiconductor substrate |
| JP2006270115A (en) * | 2006-05-22 | 2006-10-05 | Dainippon Screen Mfg Co Ltd | Substrate treatment apparatus and substrate treatment method |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111199869A (en) * | 2018-11-19 | 2020-05-26 | 长鑫存储技术有限公司 | Wafer cleaning method |
| CN114669546A (en) * | 2022-04-18 | 2022-06-28 | 广东先导微电子科技有限公司 | Method for cleaning indium phosphide polycrystal material |
| CN114669546B (en) * | 2022-04-18 | 2023-08-22 | 广东先导微电子科技有限公司 | Method for cleaning indium phosphide polycrystal material |
Also Published As
| Publication number | Publication date |
|---|---|
| JP6529715B2 (en) | 2019-06-12 |
| TWI615896B (en) | 2018-02-21 |
| TW201521105A (en) | 2015-06-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP6575643B2 (en) | Silicon wafer manufacturing method | |
| JP3219020B2 (en) | Cleaning agent | |
| JP5589968B2 (en) | Semiconductor wafer cleaning method | |
| TWI520197B (en) | Method of cleaning semiconductor wafers | |
| JP4744228B2 (en) | Semiconductor substrate cleaning liquid and semiconductor substrate cleaning method | |
| JP2006253552A (en) | Method and device for washing semiconductor | |
| CN112928017A (en) | Cleaning method for effectively removing metal on surface of silicon wafer | |
| JP3624809B2 (en) | Cleaning composition, cleaning method and use thereof | |
| JP6529715B2 (en) | Method of manufacturing silicon wafer | |
| WO2013179569A1 (en) | Method for cleaning semiconductor wafer | |
| JP4933071B2 (en) | Cleaning method of silicon wafer | |
| JP4817887B2 (en) | Semiconductor substrate cleaning method | |
| JP4857738B2 (en) | Semiconductor wafer cleaning method and manufacturing method | |
| TW200915405A (en) | Process for cleaning a semiconductor wafer | |
| JP2011508981A (en) | Reduction of watermarks in HF processing of semiconductor substrates | |
| JP6206173B2 (en) | Semiconductor wafer cleaning method | |
| JP6405618B2 (en) | Silicon wafer manufacturing method | |
| JP2008153272A (en) | Method of cleaning semiconductor device manufacturing component, and cleaning solution composition | |
| KR20140091327A (en) | Method for cleaning wafer | |
| JP6200273B2 (en) | Manufacturing method of bonded wafer | |
| WO2023032488A1 (en) | Method for cleaning silicon wafer and method for producing silicon wafer | |
| JP5463740B2 (en) | Cleaning method for polished quartz glass substrate | |
| KR100732775B1 (en) | Cleaning bath for regenerating a dummy wafer and method of cleaning the dummy wafer using the same | |
| JP2004327878A (en) | Method of washing silicon wafer | |
| JPH07321080A (en) | Method for cleaning silicon wafer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20160902 |
|
| A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20170609 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20170627 |
|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20170817 |
|
| A02 | Decision of refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A02 Effective date: 20180116 |
|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20180409 |
|
| A911 | Transfer to examiner for re-examination before appeal (zenchi) |
Free format text: JAPANESE INTERMEDIATE CODE: A911 Effective date: 20180417 |
|
| A912 | Re-examination (zenchi) completed and case transferred to appeal board |
Free format text: JAPANESE INTERMEDIATE CODE: A912 Effective date: 20180525 |
|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20190315 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20190515 |
|
| R150 | Certificate of patent or registration of utility model |
Ref document number: 6529715 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |