JPH0831781A - Washing chemicals - Google Patents
Washing chemicalsInfo
- Publication number
- JPH0831781A JPH0831781A JP18544894A JP18544894A JPH0831781A JP H0831781 A JPH0831781 A JP H0831781A JP 18544894 A JP18544894 A JP 18544894A JP 18544894 A JP18544894 A JP 18544894A JP H0831781 A JPH0831781 A JP H0831781A
- Authority
- JP
- Japan
- Prior art keywords
- wafer surface
- wafer
- hydrogen peroxide
- cleaning
- oxide film
- 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
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、半導体装置の製造工程
でウエハを洗浄する際に用いられる洗浄薬液に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a cleaning chemical solution used for cleaning a wafer in a semiconductor device manufacturing process.
【０００２】[0002]
【従来の技術】半導体装置の製造工程では、その殆ど全
ての工程中でパーティクルや金属不純物等の汚染物質が
発生してウエハ表面に付着する。ウエハ表面への上記汚
染物質の付着は、半導体装置の歩留りを低下させる要因
になる。このため、半導体装置の製造プロセスフロー中
には、様々な洗浄薬液によるウエハのウェット洗浄工程
が繰り返し行われる。2. Description of the Related Art In a semiconductor device manufacturing process, contaminants such as particles and metal impurities are generated and adhere to the wafer surface in almost all of the processes. Adhesion of the contaminants to the wafer surface causes a reduction in the yield of semiconductor devices. Therefore, the wet cleaning process of the wafer with various cleaning chemicals is repeatedly performed during the manufacturing process flow of the semiconductor device.
【０００３】上記洗浄薬液としては、例えば、アンモニ
ア−過酸化水素溶液からなるＳＣ−１、塩酸−過酸化水
素溶液からなるＳＣ−２，希フッ酸溶液からなるＤＨＦ
等が用いられている。そして、半導体装置の各製造工程
間では、これらの各洗浄薬液によるウエハ洗浄を組み合
わせたいわゆるＲＣＡ洗浄が広く行われている。Examples of the cleaning solution include SC-1 made of ammonia-hydrogen peroxide solution, SC-2 made of hydrochloric acid-hydrogen peroxide solution, and DHF made of dilute hydrofluoric acid solution.
Etc. are used. Then, so-called RCA cleaning, which is a combination of wafer cleaning with these cleaning chemicals, is widely performed between the respective semiconductor device manufacturing processes.
【０００４】上記洗浄薬液のうち、ＤＨＦを用いたウエ
ハ洗浄は、フッ酸でシリコンからなるウエハ表面の自然
酸化膜をエッチングすることによって、パーティクルや
自然酸化膜中に取り込まれやすい鉄（Ｆｅ），アルミニ
ウム（Ａｌ）等の金属をウエハ表面から除去することを
目的としている。また、金属に対する除去効果を得るた
めに、上記ＤＨＦ溶液に塩酸を添加した洗浄薬液も用い
られている。Among the cleaning chemicals described above, the wafer cleaning using DHF is performed by etching the natural oxide film on the surface of the wafer made of silicon with hydrofluoric acid, so that iron (Fe), which is easily incorporated into particles or natural oxide film, The purpose is to remove metal such as aluminum (Al) from the wafer surface. Further, in order to obtain the effect of removing metal, a cleaning chemical liquid in which hydrochloric acid is added to the DHF solution is also used.
【０００５】[0005]
【発明が解決しようとする課題】しかし、上記の塩酸を
含むＤＨＦからなる洗浄薬液には、以下の様な課題があ
った。すなわち、上記洗浄薬液を用いて洗浄を行ったウ
エハ表面は、表面層の自然酸化膜がエッチングされてい
わゆるベアシリコンが露出した状態になる。このベアシ
リコン表面は非常に活性であるため、汚染物質が吸着し
易い。このため、上記洗浄薬液中の塩酸やフッ酸によっ
てウエハ表面から除去された汚染物質のうち、特にベア
シリコンに対する吸着力が強いＣｕやパーティクル等の
汚染物質は、ベアシリコンが露出した時点で再びウエハ
表面に付着するという問題があった。However, the above-mentioned cleaning chemical liquid containing DHF containing hydrochloric acid has the following problems. That is, on the surface of the wafer that has been cleaned using the cleaning chemical solution described above, the natural oxide film of the surface layer is etched to expose the so-called bare silicon. Since this bare silicon surface is very active, contaminants are easily adsorbed. For this reason, among the contaminants removed from the wafer surface by the hydrochloric acid or hydrofluoric acid in the cleaning chemical, contaminants such as Cu and particles, which have a particularly strong adsorbing power to bare silicon, are re-exposed to the wafer when bare silicon is exposed. There was a problem of sticking to the surface.
【０００６】そこで本発明は、上記課題を解決する洗浄
薬液を供給することによって、ウエハ表面の清浄度を向
上させることを目的とする。Therefore, an object of the present invention is to improve the cleanliness of the wafer surface by supplying a cleaning chemical solution that solves the above problems.
【０００７】[0007]
【課題を解決するための手段】上記目的を達成するため
の本発明は、塩酸を含む希フッ酸溶液に過酸化水素を添
加した洗浄薬液である。The present invention for achieving the above object is a cleaning chemical solution in which hydrogen peroxide is added to a dilute hydrofluoric acid solution containing hydrochloric acid.
【０００８】[0008]
【作用】上記洗浄薬液には、塩酸を含む希フッ酸溶液に
過酸化水素が添加されていることから、上記洗浄薬液を
用いてシリコンウエハを洗浄した場合には、塩酸による
金属の溶解とフッ酸によるウエハ表面の自然酸化膜のエ
ッチングと過酸化水素によるウエハ表面の酸化とが同時
に進行する。このため、上記洗浄薬液中では、ウエハ表
面の金属除去と共に、自然酸化膜のエッチングと新たな
酸化膜の形成とが繰り返される。したがって、上記洗浄
では、ウエハ表面の活性化が抑制される。Since hydrogen peroxide is added to a dilute hydrofluoric acid solution containing hydrochloric acid in the above cleaning chemical solution, when a silicon wafer is cleaned using the above cleaning chemical solution, the metal is dissolved by the hydrochloric acid and the fluorine content is reduced. Etching of the natural oxide film on the wafer surface by acid and oxidation of the wafer surface by hydrogen peroxide proceed at the same time. For this reason, in the cleaning chemical, the removal of the metal on the wafer surface and the etching of the natural oxide film and the formation of a new oxide film are repeated. Therefore, in the above cleaning, activation of the wafer surface is suppressed.
【０００９】[0009]
【実施例】以下、本発明の洗浄薬液の実施例を説明す
る。洗浄薬液は、塩酸を含む希フッ酸溶液に過酸化水素
を添加した溶液である。上記塩酸を含む希フッ酸溶液
は、例えば、１７％塩酸：２５％フッ酸＝１溶：１溶を
水で１００倍に希釈した溶液である。そして、この希フ
ッ酸溶液に、過酸化水素を添加した溶液が上記洗浄薬液
になる。EXAMPLES Examples of the cleaning chemicals of the present invention will be described below. The cleaning chemical solution is a solution obtained by adding hydrogen peroxide to a dilute hydrofluoric acid solution containing hydrochloric acid. The dilute hydrofluoric acid solution containing hydrochloric acid is, for example, a solution in which 17% hydrochloric acid: 25% hydrofluoric acid = 1 solution: 1 solution is diluted 100 times with water. Then, a solution obtained by adding hydrogen peroxide to the diluted hydrofluoric acid solution becomes the cleaning chemical solution.
【００１０】上記洗浄薬液を用いてシリコンウエハ（以
下ウエハと記す）を洗浄する場合には、以下のように行
う。先ず、洗浄槽内に上記洗浄薬液を溜め、当該洗浄薬
液中にウエハを浸漬する。所定時間経過後、上記ウエハ
を洗浄薬液中から取り出して純水でリンスし、当該ウエ
ハ表面から上記洗浄薬液を除去する。その後、このウエ
ハを乾燥させる。When a silicon wafer (hereinafter referred to as a wafer) is cleaned using the above cleaning chemical solution, it is carried out as follows. First, the cleaning chemical solution is stored in the cleaning tank, and the wafer is immersed in the cleaning chemical solution. After a lapse of a predetermined time, the wafer is taken out of the cleaning chemical solution and rinsed with pure water to remove the cleaning chemical solution from the surface of the wafer. Then, the wafer is dried.
【００１１】上記洗浄薬液には、塩酸とフッ酸と過酸化
水素とが含有されている。このことから、ウエハを上記
洗浄薬液に浸漬すると、塩酸による金属の溶解とフッ酸
によるウエハ表面の自然酸化膜のエッチングと過酸化水
素によるウエハ表面の酸化とが同時に進行してウエハ表
面が洗浄される。The cleaning chemical solution contains hydrochloric acid, hydrofluoric acid, and hydrogen peroxide. From this, when the wafer is immersed in the above cleaning chemical, the dissolution of the metal with hydrochloric acid and the etching of the natural oxide film on the wafer surface with hydrofluoric acid and the oxidation of the wafer surface with hydrogen peroxide simultaneously proceed to clean the wafer surface. It
【００１２】ここで、上記洗浄薬液中の過酸化水素の添
加量を、例えば、以下のように設定する。図１には、銅
（Ｃｕ）と鉄（Ｆｅ）とのウエハ表面への吸着評価のグ
ラフを示す。ここで、Ｃｕは表面の自然酸化膜が除去さ
れたベアシリコンに対して特に吸着し易い物質であり、
Ｆｅは酸化膜に取り込まれ易い物質である。このグラフ
は、故意にＣｕとＦｅとをそれぞれ１０ｐｐｂのづつ添
加した上記洗浄薬液を用意し、この薬液中にウエハを３
分間浸漬させた際に当該洗浄薬液からウエハ表面に吸着
するＣｕとＦｅとの原子数を示している。グラフの横軸
は洗浄薬液中の過酸化水素濃度であり、縦軸はＣｕ，Ｆ
ｅの吸着数である。測定は全反射蛍光Ｘ線分析装置によ
って行った。このグラフから、過酸化水素濃度が高い
程、洗浄薬液中の過酸化水素によるウエハ表面の酸化力
が強まって酸化膜が成膜され易くなり、ウエハ表面の活
性化が抑えられて当該表面に吸着するＣｕの原子数が少
なくなることが確認される。また、過酸化水素による酸
化作用によってウエハ表面に新たに形成された酸化膜に
対するＦｅの吸着量は、上記過酸化水素の濃度に依存し
ないことが確認される。Here, the amount of hydrogen peroxide added to the cleaning chemical liquid is set as follows, for example. FIG. 1 shows a graph of evaluation of adsorption of copper (Cu) and iron (Fe) on the wafer surface. Here, Cu is a substance that is particularly easily adsorbed to bare silicon from which the native oxide film on the surface has been removed,
Fe is a substance that is easily taken into the oxide film. This graph shows that the above cleaning chemical solution was prepared by intentionally adding Cu and Fe at 10 ppb each, and 3 wafers were placed in this chemical solution.
The number of atoms of Cu and Fe adsorbed on the wafer surface from the cleaning chemical solution when immersed for a minute is shown. The horizontal axis of the graph is the hydrogen peroxide concentration in the cleaning chemical, and the vertical axes are Cu and F.
It is the adsorption number of e. The measurement was performed by a total reflection X-ray fluorescence analyzer. From this graph, the higher the concentration of hydrogen peroxide, the stronger the oxidizing power of the hydrogen peroxide in the cleaning liquid on the wafer surface and the easier it becomes for an oxide film to be formed. It is confirmed that the number of Cu atoms is reduced. Further, it is confirmed that the amount of Fe adsorbed to the oxide film newly formed on the wafer surface by the oxidizing action of hydrogen peroxide does not depend on the concentration of hydrogen peroxide.
【００１３】また、図２には、Ｓｉウエハ表面へのパー
ティクル吸着評価のグラフを示す。このグラフは、故意
にパーティクルを添加した上記洗浄薬液を用意し、この
薬液中にウエハを３分間浸漬させた際に当該洗浄薬液か
らウエハ表面に吸着するパーティル数を示している。グ
ラフの横軸は洗浄薬液中の過酸化水素濃度であり、縦軸
はパーティクル吸着数である。パーティクルとしては、
Ｓｉクズを用い、０．３μｍ以上の粒子径のパーティク
ルについてカウントした。このグラフから、洗浄薬液中
の過酸化水素濃度が０．１〜０．２％程度の場合に、ウ
エハ表面に吸着するパーティクル数が少なくなることが
確認される。Further, FIG. 2 shows a graph of particle adsorption evaluation on the Si wafer surface. This graph shows the number of particles adsorbed to the wafer surface from the cleaning chemical solution when the cleaning chemical solution to which particles are intentionally added is prepared and the wafer is immersed in this chemical solution for 3 minutes. The horizontal axis of the graph is the hydrogen peroxide concentration in the cleaning chemical solution, and the vertical axis is the particle adsorption number. As particles,
Particles having a particle diameter of 0.3 μm or more were counted using Si scraps. From this graph, it is confirmed that the number of particles adsorbed on the wafer surface decreases when the concentration of hydrogen peroxide in the cleaning chemical solution is about 0.1 to 0.2%.
【００１４】そして、図３には、ＣｕとＦｅとのウエハ
表面からの除去評価のグラフを示す。このグラフは、故
意にＣｕとＦｅとを吸着させたウエハを上記洗浄薬液で
洗浄した後に、ウエハ表面に残留しているＣｕとＦｅの
原子数を示している。グラフの横軸は洗浄薬液中の過酸
化水素濃度であり、縦軸は洗浄後にウエハ表面に残った
ＣｕとＦｅとの残数である。このグラフから、上記０．
１〜０．２％程度の過酸化水素が添加された洗浄薬液で
は、過酸化水素によるウエハ表面の酸化が洗浄薬液中の
塩酸によるウエハ表面のＣｕの除去を妨げないことが確
認される。また、上記０．１〜０．２％程度の過酸化水
素が添加された洗浄薬液では、過酸化水素によるウエハ
表面の酸化がフッ酸によるウエハ表面の自然酸化膜のエ
ッチングを妨げることはなく、当該自然酸化膜中のＦｅ
がウエハ表面から除去されることが確認される。FIG. 3 shows a graph of evaluation of removal of Cu and Fe from the wafer surface. This graph shows the numbers of Cu and Fe atoms remaining on the surface of the wafer after cleaning the wafer on which Cu and Fe are intentionally adsorbed with the cleaning solution. The horizontal axis of the graph is the hydrogen peroxide concentration in the cleaning chemical solution, and the vertical axis is the remaining number of Cu and Fe remaining on the wafer surface after cleaning. From this graph,
It has been confirmed that in a cleaning chemical solution to which hydrogen peroxide of about 1 to 0.2% is added, the oxidation of the wafer surface by hydrogen peroxide does not hinder the removal of Cu on the wafer surface by hydrochloric acid in the cleaning chemical solution. In addition, in the above-mentioned cleaning chemical solution to which about 0.1 to 0.2% of hydrogen peroxide is added, the oxidation of the wafer surface by hydrogen peroxide does not hinder the etching of the natural oxide film on the wafer surface by hydrofluoric acid. Fe in the natural oxide film
Are removed from the wafer surface.
【００１５】上記各グラフから、上記洗浄薬液中の過酸
化水素濃度を、例えば０．１〜０．２％の間に設定す
る。From the above graphs, the hydrogen peroxide concentration in the cleaning chemical solution is set to, for example, 0.1 to 0.2%.
【００１６】上記のように、過酸化水素の濃度が設定さ
れた洗浄薬液では、ウエハ表面の金属汚染が塩酸によっ
て除去される。また、自然酸化膜のエッチングによっ
て、ウエハ表面の自然酸化膜に取り込まれている汚染物
質が除去される。また、ウエハ表面の酸化によって、ベ
アシリコン表面に酸化膜が形成され、ウエハ表面の活性
化が抑えられる。これによって、ウエハ表面への汚染物
質の吸着が防止される。したがって、ウエハ洗浄工程の
最後に上記洗浄薬液を用いた洗浄を行うことによって、
上記洗浄薬液による洗浄及びその後工程でシリコンウエ
ハ表面の清浄度が保たれる。As described above, in the cleaning chemical solution in which the concentration of hydrogen peroxide is set, the metal contamination on the wafer surface is removed by hydrochloric acid. Further, by etching the natural oxide film, contaminants taken in by the natural oxide film on the wafer surface are removed. Further, the oxidation of the wafer surface forms an oxide film on the bare silicon surface, which suppresses the activation of the wafer surface. This prevents the adsorption of contaminants on the wafer surface. Therefore, by performing the cleaning using the cleaning chemical solution at the end of the wafer cleaning process,
The cleanliness of the surface of the silicon wafer is maintained in the cleaning with the cleaning chemical solution and the subsequent steps.
【００１７】上記実施例では、上記洗浄薬液中の過酸化
水素濃度を、０．１〜０．２％とした。しかし、過酸化
水素濃度は洗浄薬液中のフッ酸による自然酸化膜のエッ
チンング速度と過酸化水素によるシリコンの酸化速度と
に基づいて設定される値である。このため、上記過酸化
水素濃度は、０．１〜０．２％に限るものではなく、希
フッ酸溶液のフッ酸濃度に対応させて選択する。In the above embodiment, the hydrogen peroxide concentration in the cleaning chemical solution is set to 0.1 to 0.2%. However, the hydrogen peroxide concentration is a value set based on the etching rate of the natural oxide film by the hydrofluoric acid in the cleaning chemical solution and the oxidation rate of silicon by hydrogen peroxide. Therefore, the hydrogen peroxide concentration is not limited to 0.1 to 0.2%, and is selected according to the hydrofluoric acid concentration of the dilute hydrofluoric acid solution.
【００１８】[0018]
【発明の効果】以上、説明したように本発明の洗浄薬液
によれば、塩酸を含む希フッ酸溶液に過酸化水素を添加
することによって、上記洗浄薬液によるＳｉウエハの洗
浄の際にウエハ表面の自然酸化膜のエッチングと同時に
酸化膜の形成を進行させることが可能になる。このた
め、Ｓｉウエハの洗浄で、ウエハ表面の金属汚染と自然
酸化膜中に取り込まれている汚染物質とを除去すると共
に、上記ウエハ表面の活性化を抑えて汚染物質の再吸着
を防止することができる。したがって、上記洗浄薬液に
よる洗浄及びその後工程で、シリコンウエハ表面の清浄
度を確保することが可能になる。As described above, according to the cleaning chemical of the present invention, by adding hydrogen peroxide to a dilute hydrofluoric acid solution containing hydrochloric acid, the surface of the wafer is cleaned when the Si wafer is cleaned by the cleaning chemical. It becomes possible to proceed with the formation of the oxide film simultaneously with the etching of the natural oxide film. Therefore, by cleaning the Si wafer, the metal contamination on the wafer surface and the contaminants taken in the natural oxide film are removed, and the activation of the wafer surface is suppressed to prevent the re-adsorption of the contaminants. You can Therefore, it becomes possible to secure the cleanliness of the surface of the silicon wafer in the cleaning with the cleaning chemical solution and the subsequent steps.
【図１】Ｃｕ，Ｆｅ吸着評価のグラフである。FIG. 1 is a graph of Cu and Fe adsorption evaluation.
【図２】パーティクル吸着評価のグラフである。FIG. 2 is a graph of particle adsorption evaluation.
【図３】Ｃｕ，Ｆｅ除去評価のグラフである。FIG. 3 is a graph of Cu and Fe removal evaluation.
Claims (1)
添加してなることを特徴とする洗浄薬液。1. A cleaning chemical liquid comprising hydrogen peroxide added to a dilute hydrofluoric acid solution containing hydrochloric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18544894A JPH0831781A (en) | 1994-07-13 | 1994-07-13 | Washing chemicals |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18544894A JPH0831781A (en) | 1994-07-13 | 1994-07-13 | Washing chemicals |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0831781A true JPH0831781A (en) | 1996-02-02 |
Family
ID=16170978
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP18544894A Pending JPH0831781A (en) | 1994-07-13 | 1994-07-13 | Washing chemicals |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0831781A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6245650B1 (en) | 1999-01-28 | 2001-06-12 | Nec Corporation | Process for production of semiconductor device |
| US6432836B1 (en) * | 1998-09-17 | 2002-08-13 | Nec Corporation | Cleaning method for semiconductor substrate and cleaning solution |
| US6727187B2 (en) | 2000-04-27 | 2004-04-27 | Renesas Technology Corp. | Fabrication method for semiconductor device |
| US7165560B2 (en) * | 2003-02-20 | 2007-01-23 | Matsushita Electric Industrial Co., Ltd. | Etching method, etching apparatus, and method for manufacturing semiconductor device |
| US7306681B2 (en) * | 2004-05-12 | 2007-12-11 | United Microelectronics Corp. | Method of cleaning a semiconductor substrate |
| EP1354197B1 (en) * | 2001-01-16 | 2010-03-24 | Universite Catholique De Louvain | Surface chemical modification of optical elements |
-
1994
- 1994-07-13 JP JP18544894A patent/JPH0831781A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6432836B1 (en) * | 1998-09-17 | 2002-08-13 | Nec Corporation | Cleaning method for semiconductor substrate and cleaning solution |
| US6245650B1 (en) | 1999-01-28 | 2001-06-12 | Nec Corporation | Process for production of semiconductor device |
| US6727187B2 (en) | 2000-04-27 | 2004-04-27 | Renesas Technology Corp. | Fabrication method for semiconductor device |
| EP1354197B1 (en) * | 2001-01-16 | 2010-03-24 | Universite Catholique De Louvain | Surface chemical modification of optical elements |
| US7165560B2 (en) * | 2003-02-20 | 2007-01-23 | Matsushita Electric Industrial Co., Ltd. | Etching method, etching apparatus, and method for manufacturing semiconductor device |
| US7306681B2 (en) * | 2004-05-12 | 2007-12-11 | United Microelectronics Corp. | Method of cleaning a semiconductor substrate |
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