WO2013179569A1 - Method for cleaning semiconductor wafer - Google Patents

Method for cleaning semiconductor wafer Download PDF

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WO2013179569A1
WO2013179569A1 PCT/JP2013/002849 JP2013002849W WO2013179569A1 WO 2013179569 A1 WO2013179569 A1 WO 2013179569A1 JP 2013002849 W JP2013002849 W JP 2013002849W WO 2013179569 A1 WO2013179569 A1 WO 2013179569A1
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cleaning
semiconductor wafer
overwater
concentration
hydrogen peroxide
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PCT/JP2013/002849
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French (fr)
Japanese (ja)
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均 椛澤
阿部　達夫
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信越半導体株式会社
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02041—Cleaning
    • H01L21/02043—Cleaning before device manufacture, i.e. Begin-Of-Line process
    • H01L21/02052—Wet cleaning only

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  • the present invention relates to a method for cleaning a semiconductor wafer.
  • Patent Document 1 describes a silicon wafer cleaning method in which HF cleaning is performed after SC1 cleaning, and then SC1 cleaning is performed again.
  • the surface of the semiconductor wafer is usually oxidized with ozone water after HF cleaning.
  • the ozone water treatment tank of the immersion type cleaning device As described above, when cleaning with SC1 ⁇ HF ⁇ ozone water is performed, the ozone water is extremely unstable. Therefore, in the ozone water treatment tank of the immersion type cleaning device, the concentration is constantly lowered with time. . Originally, it is preferable that the ozone concentration in the cleaning tank is uniform, but in reality, there is a partial difference in concentration between the newly supplied ozone water and the ozone water in the cleaning tank whose concentration has been attenuated. Has occurred.
  • the present invention has been made in view of the above-described problems, and can reduce the unevenness of the surface roughness (haze) of the semiconductor wafer due to the cleaning, and can clean the semiconductor wafer effectively. It aims to provide a method.
  • the present invention provides a semiconductor wafer cleaning method, comprising: a first cleaning process for SC1 cleaning the semiconductor wafer; and a second cleaning process for cleaning the semiconductor wafer after the first cleaning process.
  • a semiconductor wafer cleaning method comprising: a cleaning step; and a third cleaning step of cleaning the semiconductor wafer with hydrogen peroxide after the second cleaning step.
  • the semiconductor wafer can be cleaned without causing unevenness in the surface roughness (haze) of the semiconductor wafer, and a higher quality semiconductor wafer can be obtained.
  • the temperature of the hydrogen peroxide solution is preferably 20 to 80 ° C.
  • the concentration of the hydrogen peroxide solution is preferably 0.1 to 30 wt%.
  • uneven oxidation on the surface of the semiconductor wafer due to cleaning can be reduced, and the semiconductor wafer can be cleaned without causing unevenness in the surface roughness (haze) of the semiconductor wafer.
  • FIG. 10 shows the particle level of the cleaned silicon wafer when the liquid temperature in the overwater cleaning in Examples 1 to 9 and Comparative Example 1 is changed.
  • the particle levels of the silicon wafer after cleaning when the solution concentration in the overwater cleaning is changed in Examples 10 to 15 and Comparative Example 1 are shown.
  • 7 shows the evaluation results of the haze map and the hazyness of the silicon wafer after the first to third cleaning steps in Examples 1 to 6 and Comparative Example 1.
  • FIG. FIG. 7 shows the evaluation results of the haze map and the hazyness of the silicon wafer after the first to third cleaning steps in Examples 7 to 13.
  • FIG. FIG. 14 shows the haze map and the evaluation results of the haze irregularity of the silicon wafer after the first to third cleaning steps in Examples 14 and 15.
  • the semiconductor wafer is SC1 cleaned with a mixed cleaning solution of ammonia, hydrogen peroxide, and water (first cleaning step).
  • SC1 cleaning particles attached to the surface of the semiconductor wafer by etching are lifted off and removed.
  • the mixing ratio of ammonia, hydrogen peroxide and water, and the temperature of the SC1 cleaning liquid are not particularly limited. Any of the commonly employed conditions can be applied.
  • the semiconductor wafer can be rinsed with pure water.
  • the SC1 cleaned semiconductor wafer is HF cleaned with an HF aqueous solution (second cleaning step).
  • the HF cleaning by removing the oxide film on the surface of the semiconductor wafer formed by the SC1 cleaning, particles on the surface of the semiconductor wafer strongly bonded to the oxide film are removed by lifting off, and heavy metals in the oxide film are also removed. be able to.
  • concentration of HF aqueous solution is not specifically limited.
  • the surface of the semiconductor wafer after HF cleaning is a hydrophobic surface and particles are likely to adhere. Therefore, in order to prevent particles from reattaching to the surface of the semiconductor wafer, in the present invention, the semiconductor wafer after HF cleaning is washed with hydrogen peroxide water to oxidize the surface (third cleaning step).
  • the temperature of the hydrogen peroxide solution is preferably 20 to 80 ° C.
  • the temperature of the hydrogen peroxide solution is 20 ° C. or higher, the effect of preventing the reattachment of particles can be maintained, so that the particle level after cleaning becomes better.
  • the temperature of the hydrogen peroxide solution is 80 ° C. or lower, the evaporation amount of the cleaning liquid can be kept constant and bubbles can be prevented from increasing in the cleaning liquid, so that hazy irregularities occur in the semiconductor wafer after cleaning. This can be suppressed more effectively.
  • the concentration of the hydrogen peroxide solution is preferably 0.1 to 30 wt%.
  • the concentration of the hydrogen peroxide solution is 0.1 wt% or more, it is possible to suppress the occurrence of hazyness in the semiconductor wafer by the cleaning, and the particle level after the cleaning becomes good.
  • the concentration of the hydrogen peroxide solution is 30 wt% or less, the evaporation amount of hydrogen peroxide from the cleaning liquid can be kept appropriate, and the burden on the exhaust equipment can be prevented from increasing.
  • Example 1 First, a silicon wafer having a diameter of 300 mm, a crystal orientation ⁇ 100>, and a P-type 10 ⁇ cm was cleaned with SC1 (first cleaning step), rinsed with ultrapure water, then washed with HF (second cleaning step), Washing with water (third washing step) was performed continuously. Then, the silicon wafer that had been cleaned after the third cleaning step was dried. Particles ( ⁇ 41 nm) and haze of the dried silicon wafer were measured with a particle counter.
  • the SC1 cleaning liquid used had a mixing ratio of ammonia, superwater, and water of 1: 1: 10, and the temperature of the SC1 cleaning liquid was 70 ° C.
  • the first to third cleaning steps were performed with the HF concentration in the second cleaning step being 1.5%, the overwater concentration in the third cleaning step being 3.0 wt%, and the temperature of the overwater being 10 ° C.
  • Example 2 The first to third washing steps were performed in the same manner as in Example 1 except that the temperature of the overwater in the overwater washing was 20 ° C.
  • Example 3 The first to third washing steps were performed in the same manner as in Example 1 except that the temperature of the overwater in the overwater washing was 30 ° C.
  • Example 4 The first to third washing steps were performed in the same manner as in Example 1 except that the temperature of the overwater in the overwater washing was 40 ° C.
  • Example 5 The first to third washing steps were performed in the same manner as in Example 1 except that the temperature of the overwater in the overwater washing was 50 ° C.
  • Example 6 The first to third washing steps were carried out in the same manner as in Example 1 except that the temperature of the overwater in the overwater washing was 60 ° C.
  • Example 7 The first to third washing steps were performed in the same manner as in Example 1 except that the temperature of the overwater in the overwater washing was set to 70 ° C.
  • Example 8 The first to third washing steps were performed in the same manner as in Example 1 except that the temperature of the overwater in the overwater washing was 80 ° C.
  • Example 9 The first to third washing steps were performed in the same manner as in Example 1 except that the temperature of the overwater in the overwater washing was 90 ° C.
  • Example 10 The first to third washing steps were performed in the same manner as in Example 1 except that the temperature of the overwater in the overwater washing was 80 ° C. and the concentration of the overwater was 0.03 wt%.
  • Example 11 The first to third cleaning steps were performed in the same manner as in Example 10 except that the concentration of overwater was 0.1 wt%.
  • Example 12 The first to third cleaning steps were performed in the same manner as in Example 10 except that the concentration of overwater was 0.3 wt%.
  • Example 13 The first to third cleaning steps were performed in the same manner as in Example 10 except that the concentration of overwater was 1.0 wt%.
  • Example 14 The first to third cleaning steps were carried out in the same manner as in Example 10 except that the concentration of overwater was 10.0 wt%.
  • Example 15 The first to third cleaning steps were performed in the same manner as in Example 10 except that the concentration of overwater was 30.0 wt%.
  • Example 1 The first and second cleaning steps were performed in the same manner as in Example 1. Thereafter, the silicon wafer was cleaned with 10 ppm of ozone water instead of cleaning with excess water.
  • the number of particles on the surface of the silicon wafer after washing with water was as small as about 15.
  • the number of particles was as good as 17 particles.
  • Comparative Example 1 As shown in FIGS. 2 and 3, the number of particles on the surface of the silicon wafer after cleaning was not significantly different from that of the Example. However, as shown in FIG. 4, since the hazyness was generated on the surface of the silicon wafer after the ozone water cleaning, the quality of the silicon wafer after the cleaning was poor.
  • the present invention is not limited to the above embodiment.
  • the above-described embodiment is an exemplification, and the present invention has substantially the same configuration as the technical idea described in the claims of the present invention, and any device that exhibits the same function and effect is the present invention. It is included in the technical scope of the invention.

Abstract

This method for cleaning a semiconductor wafer has: a first cleaning step (1) for performing SC1 cleaning with respect to the semiconductor wafer; a second cleaning step (2) for performing HF cleaning with respect to the semiconductor wafer after the first cleaning step (1); and a third cleaning step (3) for cleaning the semiconductor wafer using a hydrogen peroxide solution after the second cleaning step (2). Consequently, nonuniformity of the surface roughness (haze) of the semiconductor wafer due to cleaning is reduced, and the semiconductor wafer can be effectively cleaned.

Description

半導体ウェーハの洗浄方法Semiconductor wafer cleaning method
　本発明は、半導体ウェーハの洗浄方法に関する。 The present invention relates to a method for cleaning a semiconductor wafer.
　半導体ウェーハの洗浄方法としては、アンモニア水、過酸化水素水（以下、過水ともいう）、超純水の混合洗浄液による洗浄（ＳＣ１洗浄）、塩酸、過水、超純水の混合洗浄液による洗浄（ＳＣ２洗浄）、及びこれらにＨＦによる洗浄を組み合わせたＲＣＡ洗浄等の洗浄プロセスが多く用いられている。例えば、特許文献１では、シリコンウェーハの洗浄方法であって、ＳＣ１洗浄後にＨＦ洗浄を行い、その後、ＳＣ１洗浄を再び行うことが記載されている。 As cleaning methods for semiconductor wafers, cleaning with a mixed cleaning solution of ammonia water, hydrogen peroxide solution (hereinafter also referred to as excess water) and ultrapure water (SC1 cleaning), cleaning with a mixed cleaning solution of hydrochloric acid, excess water and ultrapure water. (SC2 cleaning) and cleaning processes such as RCA cleaning combining these with HF cleaning are often used. For example, Patent Document 1 describes a silicon wafer cleaning method in which HF cleaning is performed after SC1 cleaning, and then SC1 cleaning is performed again.
　ＳＣ１洗浄によって、半導体ウェーハのパーティクル除去を行った後、ＳＣ１洗浄によって生じた酸化膜及び酸化膜中の重金属を、ＨＦ洗浄で除去を行った場合、半導体ウェーハの表面に再びパーティクルが付着することを防ぐため、ＨＦ洗浄後に、通常はオゾン水によって半導体ウェーハの表面を酸化している。 After removing particles of the semiconductor wafer by SC1 cleaning, if the oxide film and heavy metal in the oxide film generated by SC1 cleaning are removed by HF cleaning, particles adhere to the surface of the semiconductor wafer again. In order to prevent this, the surface of the semiconductor wafer is usually oxidized with ozone water after HF cleaning.
特開平１１－８７２８１号公報Japanese Patent Laid-Open No. 11-87281
　このように、ＳＣ１→ＨＦ→オゾン水による洗浄を行った場合、オゾン水は極めて不安定であるため、浸漬型洗浄装置のオゾン水処理槽では、絶えず時間と共に、分解による濃度低下が起きている。本来、洗浄槽内のオゾン濃度は均一であることが好ましいが、現実的には、新しく供給されるオゾン水と、濃度が減衰した洗浄槽内のオゾン水との間で、部分的に濃度差が生じている。この結果、オゾン水で、ＨＦ処理後のベア面に酸化を行うと、オゾン水の濃度ムラによって酸化にムラができ、この酸化ムラによって半導体ウェーハの表面粗さ（ヘイズ）にムラが生じている。 As described above, when cleaning with SC1 → HF → ozone water is performed, the ozone water is extremely unstable. Therefore, in the ozone water treatment tank of the immersion type cleaning device, the concentration is constantly lowered with time. . Originally, it is preferable that the ozone concentration in the cleaning tank is uniform, but in reality, there is a partial difference in concentration between the newly supplied ozone water and the ozone water in the cleaning tank whose concentration has been attenuated. Has occurred. As a result, when the bare surface after HF treatment is oxidized with ozone water, the unevenness of the oxidation is caused by the uneven concentration of ozone water, and the unevenness of the surface roughness (haze) of the semiconductor wafer is caused by this unevenness of oxidation. .
　本発明は、上記問題点に鑑みてなされたものであって、洗浄による半導体ウェーハの表面粗さ（ヘイズ）のムラを低減し、効果的に半導体ウェーハの洗浄を行うことができる半導体ウェーハの洗浄方法を提供することを目的とする。 The present invention has been made in view of the above-described problems, and can reduce the unevenness of the surface roughness (haze) of the semiconductor wafer due to the cleaning, and can clean the semiconductor wafer effectively. It aims to provide a method.
　上記目的を達成するために、本発明は、半導体ウェーハの洗浄方法であって、前記半導体ウェーハをＳＣ１洗浄する第一洗浄工程と、前記第一洗浄工程後に、前記半導体ウェーハをＨＦ洗浄する第二洗浄工程と、前記第二洗浄工程後に、前記半導体ウェーハを過酸化水素水により洗浄する第三洗浄工程と、を有することを特徴とする半導体ウェーハの洗浄方法を提供する。 To achieve the above object, the present invention provides a semiconductor wafer cleaning method, comprising: a first cleaning process for SC1 cleaning the semiconductor wafer; and a second cleaning process for cleaning the semiconductor wafer after the first cleaning process. There is provided a semiconductor wafer cleaning method comprising: a cleaning step; and a third cleaning step of cleaning the semiconductor wafer with hydrogen peroxide after the second cleaning step.
　このように、第三洗浄工程において過酸化水素水により洗浄（過水洗浄）することで、半導体ウェーハ表面のパーティクルの再付着、及び、酸化ムラを抑制できる。そのため、半導体ウェーハの表面粗さ（ヘイズ）にムラを生じることなく、半導体ウェーハを洗浄することができ、より高品質な半導体ウェーハを得ることができる。 As described above, by cleaning with hydrogen peroxide water (overwater cleaning) in the third cleaning step, re-adhesion of particles on the surface of the semiconductor wafer and uneven oxidation can be suppressed. Therefore, the semiconductor wafer can be cleaned without causing unevenness in the surface roughness (haze) of the semiconductor wafer, and a higher quality semiconductor wafer can be obtained.
　このとき、前記過酸化水素水の温度を２０～８０℃とすることが好ましい。
　これにより、洗浄後の半導体ウェーハ表面におけるパーティクルの再付着、及び、酸化ムラの発生をより効果的に抑制できる。 At this time, the temperature of the hydrogen peroxide solution is preferably 20 to 80 ° C.
Thereby, the reattachment of particles on the surface of the semiconductor wafer after cleaning and the occurrence of uneven oxidation can be more effectively suppressed.
　このとき、前記過酸化水素水の濃度を０．１～３０ｗｔ％とすることが好ましい。
　これにより、洗浄後に半導体ウェーハの酸化ムラが発生することをより確実に抑制でき、過酸化水素の蒸発による排気設備への負担を低減できる。 At this time, the concentration of the hydrogen peroxide solution is preferably 0.1 to 30 wt%.
Thereby, it is possible to more reliably suppress the occurrence of uneven oxidation of the semiconductor wafer after cleaning, and to reduce the burden on the exhaust facility due to evaporation of hydrogen peroxide.
　以上のように、本発明によれば、洗浄による半導体ウェーハ表面の酸化ムラを低減し、半導体ウェーハの表面粗さ（ヘイズ）にムラを生じることなく、半導体ウェーハを洗浄することができる。 As described above, according to the present invention, uneven oxidation on the surface of the semiconductor wafer due to cleaning can be reduced, and the semiconductor wafer can be cleaned without causing unevenness in the surface roughness (haze) of the semiconductor wafer.
本発明における半導体ウェーハの洗浄フロー図である。It is a cleaning flowchart of a semiconductor wafer in the present invention. 実施例１～９及び比較例１における、過水洗浄での液温を変化させた場合の、洗浄後のシリコンウェーハのパーティクルレベルを示している。10 shows the particle level of the cleaned silicon wafer when the liquid temperature in the overwater cleaning in Examples 1 to 9 and Comparative Example 1 is changed. 実施例１０～１５及び比較例１における、過水洗浄での溶液濃度を変化させた場合の、洗浄後のシリコンウェーハのパーティクルレベルを示している。The particle levels of the silicon wafer after cleaning when the solution concentration in the overwater cleaning is changed in Examples 10 to 15 and Comparative Example 1 are shown. 実施例１～６及び比較例１における、第一～第三洗浄工程後のシリコンウェーハのヘイズマップ及びヘイズムラの評価結果である。7 shows the evaluation results of the haze map and the hazyness of the silicon wafer after the first to third cleaning steps in Examples 1 to 6 and Comparative Example 1. FIG. 実施例７～１３における、第一～第三洗浄工程後のシリコンウェーハのヘイズマップ及びヘイズムラの評価結果である。FIG. 7 shows the evaluation results of the haze map and the hazyness of the silicon wafer after the first to third cleaning steps in Examples 7 to 13. FIG. 実施例１４，１５における、第一～第三洗浄工程後のシリコンウェーハのヘイズマップ及びヘイズムラの評価結果である。FIG. 14 shows the haze map and the evaluation results of the haze irregularity of the silicon wafer after the first to third cleaning steps in Examples 14 and 15. FIG.
　以下、本発明について、実施態様の一例として、図を参照しながら詳細に説明するが、本発明はこれに限定されるものではない。 Hereinafter, the present invention will be described in detail as an example of an embodiment with reference to the drawings, but the present invention is not limited thereto.
　鏡面研磨後の研磨剤等を除去する洗浄において、本発明では、図１に示すように、まず、半導体ウェーハをアンモニア、過酸化水素、水の混合洗浄液によりＳＣ１洗浄する（第一洗浄工程）。ＳＣ１洗浄では、エッチングによって半導体ウェーハ表面に付着したパーティクルをリフトオフして除去を行う。尚、ＳＣ１洗浄における、アンモニア、過酸化水素、水の混合比、及び、ＳＣ１洗浄液の温度は特に限定されない。一般に採用されている条件のいずれをも適用することができる。また、ＳＣ１洗浄を施した後、半導体ウェーハは、純水でリンスすることができる。 In the cleaning for removing the polishing agent and the like after mirror polishing, in the present invention, as shown in FIG. 1, first, the semiconductor wafer is SC1 cleaned with a mixed cleaning solution of ammonia, hydrogen peroxide, and water (first cleaning step). In SC1 cleaning, particles attached to the surface of the semiconductor wafer by etching are lifted off and removed. In the SC1 cleaning, the mixing ratio of ammonia, hydrogen peroxide and water, and the temperature of the SC1 cleaning liquid are not particularly limited. Any of the commonly employed conditions can be applied. In addition, after the SC1 cleaning, the semiconductor wafer can be rinsed with pure water.
　次に、ＳＣ１洗浄を施した半導体ウェーハを、ＨＦ水溶液によりＨＦ洗浄する（第二洗浄工程）。ＨＦ洗浄では、ＳＣ１洗浄で形成された半導体ウェーハ表面の酸化膜を除去することにより、酸化膜と強く結びついた半導体ウェーハ表面上のパーティクルをリフトオフして除去するとともに、酸化膜中の重金属も除去することができる。尚、ＨＦ水溶液の濃度は特に限定されない。 Next, the SC1 cleaned semiconductor wafer is HF cleaned with an HF aqueous solution (second cleaning step). In the HF cleaning, by removing the oxide film on the surface of the semiconductor wafer formed by the SC1 cleaning, particles on the surface of the semiconductor wafer strongly bonded to the oxide film are removed by lifting off, and heavy metals in the oxide film are also removed. be able to. In addition, the density | concentration of HF aqueous solution is not specifically limited.
　ＨＦ洗浄後の半導体ウェーハ表面は、疎水面となり、パーティクルが付着しやすい状態となる。そのため、半導体ウェーハ表面にパーティクルが再付着することを防ぐために、本発明では、ＨＦ洗浄後の半導体ウェーハを過酸化水素水により過水洗浄し、その表面を酸化させる（第三洗浄工程）。 The surface of the semiconductor wafer after HF cleaning is a hydrophobic surface and particles are likely to adhere. Therefore, in order to prevent particles from reattaching to the surface of the semiconductor wafer, in the present invention, the semiconductor wafer after HF cleaning is washed with hydrogen peroxide water to oxidize the surface (third cleaning step).
　従来、半導体ウェーハ表面をオゾン水（１０ｐｐｍ）で洗浄した場合には、洗浄後の半導体ウェーハ表面に酸化ムラによるヘイズムラが発生していた。
　これに対し、本発明では、オゾン水に代えて過酸化水素水により過水洗浄することで、半導体ウェーハ表面のパーティクルの再付着低減とともに、酸化ムラを抑制できる。そのため、半導体ウェーハの表面粗さ（ヘイズ）にムラを生じることなく、半導体ウェーハを洗浄することができ、より高品質な半導体ウェーハを得ることができる。 Conventionally, when the surface of a semiconductor wafer is cleaned with ozone water (10 ppm), haisminess due to uneven oxidation has occurred on the surface of the semiconductor wafer after cleaning.
On the other hand, in this invention, it replaces with ozone water and wash | cleans with hydrogen peroxide water, and it can suppress the non-uniformity of oxidation while reducing the reattachment of the particle on the semiconductor wafer surface. Therefore, the semiconductor wafer can be cleaned without causing unevenness in the surface roughness (haze) of the semiconductor wafer, and a higher quality semiconductor wafer can be obtained.
　また、本発明の第三洗浄工程では、過酸化水素水の温度を２０～８０℃とすることが好ましい。
　このように、過酸化水素水の温度が２０℃以上であれば、パーティクルの再付着を防止する効果を維持できるため、洗浄後のパーティクルレベルがより良好となる。また、過酸化水素水の温度が８０℃以下であれば、洗浄液の蒸発量を一定に保ち、洗浄液中に気泡が増加することを防ぐことができるため、洗浄後の半導体ウェーハにヘイズムラが発生することをより効果的に抑制できる。 In the third cleaning step of the present invention, the temperature of the hydrogen peroxide solution is preferably 20 to 80 ° C.
Thus, if the temperature of the hydrogen peroxide solution is 20 ° C. or higher, the effect of preventing the reattachment of particles can be maintained, so that the particle level after cleaning becomes better. Further, if the temperature of the hydrogen peroxide solution is 80 ° C. or lower, the evaporation amount of the cleaning liquid can be kept constant and bubbles can be prevented from increasing in the cleaning liquid, so that hazy irregularities occur in the semiconductor wafer after cleaning. This can be suppressed more effectively.
　更に、本発明の第三洗浄工程では、過酸化水素水の濃度は０．１～３０ｗｔ％とすることが好ましい。
　このように、過酸化水素水の濃度が０．１ｗｔ％以上であれば、当該洗浄により半導体ウェーハにヘイズムラが発生することを抑制でき、かつ、洗浄後のパーティクルレベルが良好となる。また、過酸化水素水の濃度が３０ｗｔ％以下であれば、洗浄液中からの過酸化水素の蒸発量を適正に保つことができ、排気設備への負担が増大することを防ぐことができる。 Further, in the third cleaning step of the present invention, the concentration of the hydrogen peroxide solution is preferably 0.1 to 30 wt%.
As described above, when the concentration of the hydrogen peroxide solution is 0.1 wt% or more, it is possible to suppress the occurrence of hazyness in the semiconductor wafer by the cleaning, and the particle level after the cleaning becomes good. Further, if the concentration of the hydrogen peroxide solution is 30 wt% or less, the evaporation amount of hydrogen peroxide from the cleaning liquid can be kept appropriate, and the burden on the exhaust equipment can be prevented from increasing.
　以下、実施例及び比較例を示して本発明をより具体的に説明するが、本発明はこれらに限定されるものではない。
（実施例１）
　まず、直径３００ｍｍ、結晶方位＜１００＞、Ｐ型１０ΩｃｍのシリコンウェーハをＳＣ１による洗浄を行い（第一洗浄工程）、超純水でリンスを行った後、ＨＦ洗浄（第二洗浄工程）、過水による洗浄（第三洗浄工程）を連続して行った。そして、第三洗浄工程終了後に洗浄が完了したシリコンウェーハを乾燥させた。乾燥後のシリコンウェーハのパーティクル（≧４１ｎｍ）、及び、ヘイズをパーティクルカウンターで測定した。 EXAMPLES Hereinafter, although an Example and a comparative example are shown and this invention is demonstrated more concretely, this invention is not limited to these.
Example 1
First, a silicon wafer having a diameter of 300 mm, a crystal orientation <100>, and a P-type 10 Ωcm was cleaned with SC1 (first cleaning step), rinsed with ultrapure water, then washed with HF (second cleaning step), Washing with water (third washing step) was performed continuously. Then, the silicon wafer that had been cleaned after the third cleaning step was dried. Particles (≧ 41 nm) and haze of the dried silicon wafer were measured with a particle counter.
　このとき、使用したＳＣ１洗浄液は、アンモニア、過水、水の混合比を１：１：１０、ＳＣ１洗浄液の温度は７０℃とした。また、第二洗浄工程におけるＨＦ濃度は１．５％、第三洗浄工程における過水濃度は３．０ｗｔ％、過水の温度は１０℃として、第一～第三洗浄工程を実施した。 At this time, the SC1 cleaning liquid used had a mixing ratio of ammonia, superwater, and water of 1: 1: 10, and the temperature of the SC1 cleaning liquid was 70 ° C. In addition, the first to third cleaning steps were performed with the HF concentration in the second cleaning step being 1.5%, the overwater concentration in the third cleaning step being 3.0 wt%, and the temperature of the overwater being 10 ° C.
（実施例２）
　過水洗浄での過水の温度を２０℃とした以外は、実施例１と同様に、第一～第三洗浄工程を実施した。 (Example 2)
The first to third washing steps were performed in the same manner as in Example 1 except that the temperature of the overwater in the overwater washing was 20 ° C.
（実施例３）
　過水洗浄での過水の温度を３０℃とした以外は、実施例１と同様に、第一～第三洗浄工程を実施した。 (Example 3)
The first to third washing steps were performed in the same manner as in Example 1 except that the temperature of the overwater in the overwater washing was 30 ° C.
（実施例４）
　過水洗浄での過水の温度を４０℃とした以外は、実施例１と同様に、第一～第三洗浄工程を実施した。 (Example 4)
The first to third washing steps were performed in the same manner as in Example 1 except that the temperature of the overwater in the overwater washing was 40 ° C.
（実施例５）
　過水洗浄での過水の温度を５０℃とした以外は、実施例１と同様に、第一～第三洗浄工程を実施した。 (Example 5)
The first to third washing steps were performed in the same manner as in Example 1 except that the temperature of the overwater in the overwater washing was 50 ° C.
（実施例６）
　過水洗浄での過水の温度を６０℃とした以外は、実施例１と同様に、第一～第三洗浄工程を実施した。 (Example 6)
The first to third washing steps were carried out in the same manner as in Example 1 except that the temperature of the overwater in the overwater washing was 60 ° C.
（実施例７）
　過水洗浄での過水の温度を７０℃とした以外は、実施例１と同様に、第一～第三洗浄工程を実施した。 (Example 7)
The first to third washing steps were performed in the same manner as in Example 1 except that the temperature of the overwater in the overwater washing was set to 70 ° C.
（実施例８）
　過水洗浄での過水の温度を８０℃とした以外は、実施例１と同様に、第一～第三洗浄工程を実施した。 (Example 8)
The first to third washing steps were performed in the same manner as in Example 1 except that the temperature of the overwater in the overwater washing was 80 ° C.
（実施例９）
　過水洗浄での過水の温度を９０℃とした以外は、実施例１と同様に、第一～第三洗浄工程を実施した。 Example 9
The first to third washing steps were performed in the same manner as in Example 1 except that the temperature of the overwater in the overwater washing was 90 ° C.
（実施例１０）
　過水洗浄での過水の温度を８０℃、過水の濃度を０．０３ｗｔ％とした以外は、実施例１と同様に、第一～第三洗浄工程を実施した。 (Example 10)
The first to third washing steps were performed in the same manner as in Example 1 except that the temperature of the overwater in the overwater washing was 80 ° C. and the concentration of the overwater was 0.03 wt%.
（実施例１１）
　過水の濃度を０．１ｗｔ％とした以外は、実施例１０と同様に、第一～第三洗浄工程を実施した。 (Example 11)
The first to third cleaning steps were performed in the same manner as in Example 10 except that the concentration of overwater was 0.1 wt%.
（実施例１２）
　過水の濃度を０．３ｗｔ％とした以外は、実施例１０と同様に、第一～第三洗浄工程を実施した。 Example 12
The first to third cleaning steps were performed in the same manner as in Example 10 except that the concentration of overwater was 0.3 wt%.
（実施例１３）
　過水の濃度を１．０ｗｔ％とした以外は、実施例１０と同様に、第一～第三洗浄工程を実施した。 (Example 13)
The first to third cleaning steps were performed in the same manner as in Example 10 except that the concentration of overwater was 1.0 wt%.
（実施例１４）
　過水の濃度を１０．０ｗｔ％とした以外は、実施例１０と同様に、第一～第三洗浄工程を実施した。 (Example 14)
The first to third cleaning steps were carried out in the same manner as in Example 10 except that the concentration of overwater was 10.0 wt%.
（実施例１５）
　過水の濃度を３０．０ｗｔ％とした以外は、実施例１０と同様に、第一～第三洗浄工程を実施した。 (Example 15)
The first to third cleaning steps were performed in the same manner as in Example 10 except that the concentration of overwater was 30.0 wt%.
（比較例１）
　第一、第二洗浄工程に関しては、実施例１と同様に行った。その後、過水洗浄の代わりに、オゾン水１０ｐｐｍでシリコンウェーハの洗浄を行った。 (Comparative Example 1)
The first and second cleaning steps were performed in the same manner as in Example 1. Thereafter, the silicon wafer was cleaned with 10 ppm of ozone water instead of cleaning with excess water.
　実施例１～１５及び比較例１の結果を図２～６に示した。 The results of Examples 1 to 15 and Comparative Example 1 are shown in FIGS.
　図４～６に示すように、シリコンウェーハをＳＣ１洗浄、ＨＦ洗浄、過水洗浄の順に洗浄したことで、実施例１～１５では、洗浄後のシリコンウェーハ表面のヘイズムラが低減できた。実施例９の場合に、過水洗浄後のシリコンウェーハ表面にヘイズムラが発生したのは、過水の温度が９０℃と高かったためである。また、実施例１０の場合に、過水洗浄後のシリコンウェーハ表面にヘイズムラが発生したのは、過水の濃度が０．０３ｗｔ％と低かったためである。ただし、比較例１よりは、実施例９，１０の方がヘイズムラが抑制されていた。 As shown in FIGS. 4 to 6, by cleaning the silicon wafer in the order of SC1 cleaning, HF cleaning, and overwater cleaning, in Examples 1 to 15, it was possible to reduce the haze on the surface of the silicon wafer after cleaning. In the case of Example 9, the reason why haismura occurred on the surface of the silicon wafer after the overwater cleaning was that the temperature of the overwater was as high as 90 ° C. Further, in the case of Example 10, the reason why hazyness was generated on the surface of the silicon wafer after the overwater cleaning was that the concentration of overwater was as low as 0.03 wt%. However, Heismura was suppressed more in Examples 9 and 10 than in Comparative Example 1.
　また、図２に示すように、過水の温度が２０～８０℃の場合には、過水洗浄後のシリコンウェーハ表面のパーティクルの数が、オゾン水洗浄を行った比較例１と同程度で少なかった。更に、過水の温度が２０℃よりも下がると、パーティクルが増加する傾向が見られた。これは、過水の温度が下がることにより、パーティクルが再びシリコンウェーハに付着することを防止する効果が低下したためである。このため、実施例１では、パーティクルの数は４７個と悪化していたが、前述のように、ＨＦ洗浄後にオゾン水洗浄を行う場合はヘイズムラが顕在化するし、ＨＦ洗浄後に過水洗浄を行わない場合よりは改善されていた。 In addition, as shown in FIG. 2, when the temperature of the overwater is 20 to 80 ° C., the number of particles on the surface of the silicon wafer after the overwater cleaning is about the same as that in Comparative Example 1 in which the ozone water cleaning was performed. There were few. Furthermore, when the temperature of overwater fell below 20 degreeC, the tendency for a particle to increase was seen. This is because the effect of preventing the particles from adhering to the silicon wafer again due to the decrease in the temperature of the overwater. For this reason, in Example 1, the number of particles deteriorated to 47. However, as described above, when ozone water cleaning is performed after HF cleaning, haismura becomes obvious, and overwater cleaning is performed after HF cleaning. It was improved compared to the case where it was not performed.
　また、図３に示すように、実施例８，１０～１５では、過水洗浄後のシリコンウェーハ表面のパーティクルの数が１５個前後と少なかった。例えば、実施例８では、パーティクルの数は１７個と良好であった。 Further, as shown in FIG. 3, in Examples 8 and 10 to 15, the number of particles on the surface of the silicon wafer after washing with water was as small as about 15. For example, in Example 8, the number of particles was as good as 17 particles.
　このように、シリコンウェーハをＳＣ１洗浄、ＨＦ洗浄、過水洗浄の順に洗浄することで、パーティクル及びヘイズムラが発生することを低減できた。更に、過水洗浄の際に、過水の温度が２０～８０℃、濃度が０．１～３０ｗｔ％であれば、洗浄後のパーティクルをより効果的に低減でき、排気設備への負担も軽減できた。 Thus, by cleaning the silicon wafer in the order of SC1 cleaning, HF cleaning, and overwater cleaning, it was possible to reduce the occurrence of particles and haismura. In addition, if the water temperature is 20 to 80 ° C and the concentration is 0.1 to 30 wt%, the particles after cleaning can be reduced more effectively and the burden on the exhaust equipment is reduced. did it.
　一方、比較例１では、図２，３に示すように、洗浄後におけるシリコンウェーハの表面上のパーティクルの数は実施例と大差なかった。しかし、図４に示すように、オゾン水洗浄後のシリコンウェーハの表面にヘイズムラが発生していたため、洗浄後のシリコンウェーハの品質は悪かった。 On the other hand, in Comparative Example 1, as shown in FIGS. 2 and 3, the number of particles on the surface of the silicon wafer after cleaning was not significantly different from that of the Example. However, as shown in FIG. 4, since the hazyness was generated on the surface of the silicon wafer after the ozone water cleaning, the quality of the silicon wafer after the cleaning was poor.
　なお、本発明は、上記実施形態に限定されるものではない。上記実施形態は、例示であり、本発明の特許請求の範囲に記載された技術的思想と実質的に同一な構成を有し、同様な作用効果を奏するものは、いかなるものであっても本発明の技術的範囲に包含される。 Note that the present invention is not limited to the above embodiment. The above-described embodiment is an exemplification, and the present invention has substantially the same configuration as the technical idea described in the claims of the present invention, and any device that exhibits the same function and effect is the present invention. It is included in the technical scope of the invention.

Claims (3)

  1. 　半導体ウェーハの洗浄方法であって、
    　前記半導体ウェーハをＳＣ１洗浄する第一洗浄工程と、
    　前記第一洗浄工程後に、前記半導体ウェーハをＨＦ洗浄する第二洗浄工程と、
    　前記第二洗浄工程後に、前記半導体ウェーハを過酸化水素水により洗浄する第三洗浄工程と、
    　を有することを特徴とする半導体ウェーハの洗浄方法。     A method for cleaning a semiconductor wafer,
    A first cleaning step of SC1 cleaning the semiconductor wafer;
    A second cleaning step of HF cleaning the semiconductor wafer after the first cleaning step;
    A third cleaning step for cleaning the semiconductor wafer with hydrogen peroxide after the second cleaning step;
    A method for cleaning a semiconductor wafer, comprising:
  2. 　前記過酸化水素水の温度を２０～８０℃とすることを特徴とする請求項１に記載の半導体ウェーハの洗浄方法。 2. The method of cleaning a semiconductor wafer according to claim 1, wherein the temperature of the hydrogen peroxide solution is 20 to 80 ° C.
  3. 　前記過酸化水素水の濃度を０．１～３０ｗｔ％とすることを特徴とする請求項１又は請求項２に記載の半導体ウェーハの洗浄方法。 3. The method for cleaning a semiconductor wafer according to claim 1, wherein the concentration of the hydrogen peroxide solution is 0.1 to 30 wt%.
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JP2019161161A (en) * 2018-03-16 2019-09-19 栗田工業株式会社 Device and method for washing substrate
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