TWI795547B - Silicon wafer cleaning method - Google Patents
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- TWI795547B TWI795547B TW108111633A TW108111633A TWI795547B TW I795547 B TWI795547 B TW I795547B TW 108111633 A TW108111633 A TW 108111633A TW 108111633 A TW108111633 A TW 108111633A TW I795547 B TWI795547 B TW I795547B
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- 238000004140 cleaning Methods 0.000 title claims abstract description 160
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 103
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 103
- 239000010703 silicon Substances 0.000 title claims abstract description 103
- 238000000034 method Methods 0.000 title claims abstract description 28
- 235000012431 wafers Nutrition 0.000 claims abstract description 106
- 239000000126 substance Substances 0.000 claims abstract description 84
- 230000001590 oxidative effect Effects 0.000 claims abstract description 20
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 28
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 abstract description 15
- 238000011156 evaluation Methods 0.000 description 30
- 239000000243 solution Substances 0.000 description 28
- 230000000052 comparative effect Effects 0.000 description 22
- 230000007547 defect Effects 0.000 description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000000203 mixture Substances 0.000 description 7
- 239000002184 metal Substances 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000005498 polishing Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 238000004519 manufacturing process Methods 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
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 230000005856 abnormality Effects 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 230000036962 time dependent Effects 0.000 description 1
Classifications
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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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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
-
- 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
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/02227—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process
- H01L21/0223—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate
- H01L21/02233—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate of the semiconductor substrate or a semiconductor layer
- H01L21/02236—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate of the semiconductor substrate or a semiconductor layer group IV semiconductor
- H01L21/02238—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate of the semiconductor substrate or a semiconductor layer group IV semiconductor silicon in uncombined form, i.e. pure silicon
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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
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Metallurgy (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Cleaning Or Drying Semiconductors (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Detergent Compositions (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
本發明係為一種矽晶圓的洗淨方法，係將矽晶圓予以進行SC1洗淨之後，以具有氧化能力的洗淨液進行洗淨，其中以具有氧化能力的該洗淨液將經藉由該SC1洗淨而形成於該矽晶圓的表面的化學氧化膜予以洗淨，藉此以進一步使該化學氧化膜的厚度成為1.0 nm以上的方式進行成長。藉此提供能夠有良好的微粒品質及形成安定的化學氧化膜的矽晶圓的洗淨方法。The present invention relates to a method for cleaning silicon wafers. After the silicon wafers are cleaned by SC1, they are cleaned with a cleaning solution with oxidizing ability, wherein the cleaning solution with oxidizing ability is used to The chemical oxide film formed on the surface of the silicon wafer by the SC1 cleaning is cleaned, and the chemical oxide film is further grown so that the thickness of the chemical oxide film becomes 1.0 nm or more. This provides a cleaning method for silicon wafers that can have good particle quality and form a stable chemical oxide film.
Description
本發明係關於一種矽晶圓的洗淨方法。The invention relates to a method for cleaning silicon wafers.
單晶矽晶圓的製造步驟之中，單晶矽晶圓之主表面在拋光步驟之中被精加工。進一步有為了將在拋光步驟中附著於矽晶圓表面的拋光劑及金屬雜質予以除去的洗淨步驟。在此洗淨步驟之中使用被稱為RCA洗淨的洗淨方法。此RCA洗淨係根據目的，將SC1（Standard Cleaning 1）洗淨、SC2（Standard Cleaning 2）洗淨及DHF（Diluted Hydrofluoric Acid）洗淨予以組合而進行的洗淨法。此SC1洗淨係以任意的比例混合氨水及雙氧水，藉由鹼性的洗淨液的矽晶圓表面的蝕刻而使附著微粒剝離，進一步利用矽晶圓與微粒的靜電反作用力抑制對矽晶圓的再附著而同時除去微粒的洗淨方法。再者，SC2洗淨係藉由以任意的比例混合鹽酸與雙氧水的洗淨液，將矽晶圓表面的金屬雜質予以溶解除去的洗淨方法。再者，DHF洗淨係藉由稀氟酸將矽晶圓表面的化學氧化膜予以除去的洗淨方法。進一步有亦使用具有強氧化力的臭氧水洗淨的場合，進行附著於矽晶圓表面的有機物的除去及DHF洗淨後的矽晶圓表面的化學氧化膜形成。矽晶圓的洗淨，根據目的組合這些洗淨而進行（專利文獻1~3）。 ［先前技術文獻］ ［專利文獻］In the manufacturing step of the single crystal silicon wafer, the main surface of the single crystal silicon wafer is finished in the polishing step. Furthermore, there is a cleaning step for removing the polishing agent and metal impurities adhering to the surface of the silicon wafer during the polishing step. In this cleaning step, a cleaning method called RCA cleaning is used. This RCA cleaning is a cleaning method that combines SC1 (Standard Cleaning 1) cleaning, SC2 (Standard Cleaning 2) cleaning, and DHF (Diluted Hydrofluoric Acid) cleaning according to the purpose. This SC1 cleaning is to mix ammonia water and hydrogen peroxide in any proportion, and use the alkaline cleaning solution to etch the surface of the silicon wafer to peel off the attached particles, and further use the electrostatic reaction force between the silicon wafer and the particles to suppress the damage to the silicon wafer. Cleaning method for circular reattachment while removing particles. Furthermore, SC2 cleaning is a cleaning method that dissolves and removes metal impurities on the surface of the silicon wafer by mixing a cleaning solution of hydrochloric acid and hydrogen peroxide in an arbitrary ratio. Furthermore, DHF cleaning is a cleaning method that removes the chemical oxide film on the surface of the silicon wafer by dilute hydrofluoric acid. In some cases, ozone water cleaning with strong oxidizing power is also used to remove organic matter adhering to the surface of the silicon wafer and to form a chemical oxide film on the surface of the silicon wafer after DHF cleaning. The cleaning of the silicon wafer is performed by combining these cleanings according to the purpose (Patent Documents 1 to 3). [Prior Technical Literature] [Patent Document]
［專利文獻1］日本特開2002-329691號公報 ［專利文獻2］日本特開平9-017765號公報 ［專利文獻3］日本特開平9-260328號公報 ［專利文獻4］日本特開2006-208314號公報[Patent Document 1] Japanese Patent Laid-Open No. 2002-329691 [Patent Document 2] Japanese Patent Application Laid-Open No. 9-017765 [Patent Document 3] Japanese Patent Application Laid-Open No. 9-260328 [Patent Document 4] Japanese Patent Laid-Open No. 2006-208314
［發明所欲解決之問題］ 作為洗淨後的重要的矽晶圓品質係有微粒品質。微粒係根據洗淨液的種類而對矽晶圓的附著容易度會變化。用於SC1洗淨的洗淨液為鹼性的緣故，而有微粒難以靜電地附著的特性。另一方面，用於SC2洗淨的洗淨液為酸性的緣故，而有容易靜電地附著的特性。進一步，在DHF洗淨之中將矽晶圓表面的化學氧化膜剝離的緣故，故為酸性且同時裸面露出，成為微粒非常容易附著的狀況。因此，一般而言，為了得到良好的微粒品質，會於洗淨後使矽晶圓表面為包覆有化學氧化膜的狀態。換言之，會成為SC1洗淨及SC2洗淨的組合。[Problem to be solved by the invention] The important silicon wafer quality after cleaning is particle quality. The degree of adhesion of particles to silicon wafers varies depending on the type of cleaning solution. Since the cleaning solution used for SC1 cleaning is alkaline, it has the characteristic that fine particles are difficult to adhere electrostatically. On the other hand, the cleaning solution used for SC2 cleaning has the property of being easy to electrostatically adhere because of its acidity. Furthermore, since the chemical oxide film on the surface of the silicon wafer is peeled off during DHF cleaning, it is acidic and at the same time the bare surface is exposed, making it very easy for particles to adhere. Therefore, in general, in order to obtain good particle quality, the surface of the silicon wafer is coated with a chemical oxide film after cleaning. In other words, it becomes a combination of SC1 cleaning and SC2 cleaning.
另一方面，雖然有各式各樣評估洗淨後的矽晶圓的品質的方法，其中作為評估表面品質的手段，有DSOD（Direct Surface Oxide Defect）評估。以此DSOD評估所評估的品質，受到矽晶圓表面缺陷、結晶缺陷、金屬汙染及在洗淨步驟中形成的化學氧化膜品質等的影響。因此，在明確的原因為不明的狀況下，也有DSOD品質惡化的場合或變動的場合。因此，為了提升DSOD品質，在改善表面缺陷及結晶缺陷的同時，必須使在洗淨步驟中形成的化學氧化膜品質安定。On the other hand, although there are various methods for evaluating the quality of cleaned silicon wafers, DSOD (Direct Surface Oxide Defect) evaluation is used as a method for evaluating the surface quality. The quality evaluated by this DSOD evaluation is affected by silicon wafer surface defects, crystal defects, metal contamination, and the quality of the chemical oxide film formed in the cleaning step. Therefore, even when the definite cause is unknown, the quality of DSOD may deteriorate or fluctuate. Therefore, in order to improve the quality of DSOD, it is necessary to stabilize the quality of the chemical oxide film formed in the cleaning step while improving the surface defects and crystal defects.
在RCA洗淨之中，在SC1洗淨步驟中形成的化學氧化膜非常地薄。SC1洗淨後的化學氧化膜厚度，藉由XPS（X射線光電子能譜學（X-ray photoelectron spectroscopy））而測量為0.7 nm左右。在此SC1洗淨中形成的化學氧化膜厚度，在矽晶圓的製造的現實的時間內之中，變更洗淨時間或洗淨液溫度也不會有變化，而得知了，SC1洗淨條件無法控制化學氧化膜厚度。如此非常薄的化學氧化膜，難以使化學氧化膜品質安定化，會阻礙DSOD品質的提升。Among the RCA cleaning, the chemical oxide film formed in the SC1 cleaning step is very thin. The thickness of the chemical oxide film after SC1 cleaning was measured by XPS (X-ray photoelectron spectroscopy) to be about 0.7 nm. The thickness of the chemical oxide film formed in this SC1 cleaning does not change even if the cleaning time or the temperature of the cleaning solution is changed within the actual time of silicon wafer manufacturing, and it is known that SC1 cleaning Conditions cannot control the chemical oxide film thickness. Such a very thin chemical oxide film is difficult to stabilize the quality of the chemical oxide film, which will hinder the improvement of DSOD quality.
因此，在矽晶圓的洗淨之中，良好的微粒品質及形成安定的化學氧化膜則成為了對於晶圓品質提升的課題。 ［解決問題之技術手段］Therefore, in the cleaning of silicon wafers, good particle quality and the formation of a stable chemical oxide film have become issues for improving the quality of wafers. [Technical means to solve the problem]
為了達成上述目的，本發明提供一種矽晶圓的洗淨方法，係將矽晶圓予以進行SC1洗淨之後，以具有氧化能力的洗淨液進行洗淨，其中以具有氧化能力的該洗淨液將經藉由該SC1洗淨而形成於該矽晶圓的表面的化學氧化膜予以洗淨，藉此以進一步使該化學氧化膜的厚度成為1.0 nm以上的方式進行成長。In order to achieve the above object, the present invention provides a method for cleaning silicon wafers. After the silicon wafers are cleaned SC1, they are cleaned with a cleaning solution with oxidizing ability, wherein the cleaning method with oxidizing ability is used to clean the silicon wafers. By cleaning the chemical oxide film formed on the surface of the silicon wafer by the SC1 cleaning, the chemical oxide film is grown so that the thickness of the chemical oxide film becomes 1.0 nm or more.
若為如此的矽晶圓的洗淨方法，能夠將形成於矽晶圓的表面的化學氧化膜形成為較過去更厚的1.0 nm以上，而能夠提升矽晶圓表面品質。According to such a cleaning method of the silicon wafer, the chemical oxide film formed on the surface of the silicon wafer can be formed to be thicker than the past by 1.0 nm or more, and the surface quality of the silicon wafer can be improved.
再者，此時作為具有氧化能力的該洗淨液，使用臭氧水及／或雙氧水為佳。In this case, it is preferable to use ozone water and/or hydrogen peroxide as the cleaning liquid having oxidizing ability.
本發明的矽晶圓的洗淨方法，對於如此的場合特別有效。The silicon wafer cleaning method of the present invention is particularly effective in such a case.
再者，於進行該SC1洗淨之後，且以具有氧化能力的該洗淨液進行洗淨之前，進行SC2洗淨為佳。Furthermore, it is preferable to perform SC2 cleaning after performing the SC1 cleaning and before cleaning with the cleaning solution having oxidizing ability.
如為如此的矽晶圓的洗淨方法，藉由將矽晶圓表面的金屬雜質溶解除去，而能夠進一步提升矽晶圓表面品質。Such a silicon wafer cleaning method can further improve the surface quality of the silicon wafer by dissolving and removing metal impurities on the silicon wafer surface.
再者，進行該SC1洗淨的矽晶圓係為未進行DHF洗淨的矽晶圓為佳。Furthermore, it is preferable that the silicon wafer to be cleaned by SC1 is a silicon wafer that has not been cleaned by DHF.
若為如此的矽晶圓的洗淨方法，沒有預先除去化學氧化膜的緣故，而能夠得到充分的化學氧化膜厚度，能夠更確實地提升矽晶圓表面品質。 ［對照先前技術之功效］According to such a silicon wafer cleaning method, a sufficient thickness of the chemical oxide film can be obtained without removing the chemical oxide film in advance, and the surface quality of the silicon wafer can be improved more reliably. [Compared with the effect of previous technology]
若為本發明的矽晶圓的洗淨方法，能夠將形成於矽晶圓的表面的化學氧化膜形成為較過去更厚的1.0 nm以上，並且能夠安定並提升矽晶圓表面品質。According to the silicon wafer cleaning method of the present invention, the chemical oxide film formed on the surface of the silicon wafer can be formed to be 1.0 nm or more thicker than before, and the surface quality of the silicon wafer can be stabilized and improved.
以下，具體地說明本發明，但是本發明並非限定於此。Hereinafter, although this invention is demonstrated concretely, this invention is not limited to this.
如同上述，為了提升DSOD品質，必須在改善表面缺陷及結晶缺陷的同時，使洗淨步驟中形成的化學氧化膜品質安定化。然而，在RCA洗淨之中，在SC1洗淨中形成的化學氧化膜厚度非常地薄，如此的化學氧化膜，難以使化學氧化膜品質安定化，而阻礙了DSOD品質的提升。因此，在矽晶圓的洗淨之中，良好的微粒品質及形成安定的化學氧化膜則成為了對於晶圓品質提升的課題。As mentioned above, in order to improve the quality of DSOD, it is necessary to improve the quality of the chemical oxide film formed in the cleaning step while improving the surface defects and crystal defects. However, in RCA cleaning, the thickness of the chemical oxide film formed in SC1 cleaning is very thin. Such a chemical oxide film is difficult to stabilize the quality of the chemical oxide film, which hinders the improvement of DSOD quality. Therefore, in the cleaning of silicon wafers, good particle quality and the formation of a stable chemical oxide film have become issues for improving the quality of wafers.
然後，本發明人等為了解決上述的課題而反覆努力探討的結果，發現：於SC1洗淨後，或SC1洗淨後進行SC2洗淨的洗淨流程後，以具有氧化力的洗淨液進行化學氧化，藉由此化學氧化，而能夠使化學氧化膜厚度成長為1.0 nm，能夠使矽晶圓表面品質安定而提升，進而達成了本發明。Then, as a result of the inventors' repeated efforts to solve the above-mentioned problems, it was found that after SC1 cleaning, or after SC1 cleaning, the cleaning process of SC2 cleaning was performed with a cleaning solution having oxidative power. Chemical oxidation, through this chemical oxidation, the thickness of the chemical oxide film can be grown to 1.0 nm, and the surface quality of the silicon wafer can be stabilized and improved, thereby achieving the present invention.
亦即，本發明提供一種矽晶圓的洗淨方法，係將矽晶圓予以進行SC1洗淨之後，以具有氧化能力的洗淨液進行洗淨，其中以具有氧化能力的該洗淨液將經藉由該SC1洗淨而形成於該矽晶圓的表面的化學氧化膜予以洗淨，藉此以使該化學氧化膜的厚度成為1.0 nm以上的方式進行成長。That is to say, the present invention provides a method for cleaning a silicon wafer. After the silicon wafer is cleaned SC1, it is cleaned with a cleaning solution with oxidizing ability, wherein the cleaning solution with oxidizing ability will By cleaning the chemical oxide film formed on the surface of the silicon wafer by the SC1 cleaning, the chemical oxide film is grown so as to have a thickness of 1.0 nm or more.
若為如此的矽晶圓的洗淨方法，能夠將形成於矽晶圓的表面的化學氧化膜形成為較過去更厚的1.0 nm以上並使其安定，而能夠提升矽晶圓表面品質。According to such a silicon wafer cleaning method, the chemical oxide film formed on the surface of the silicon wafer can be formed to be thicker than the conventional one by 1.0 nm or more and stabilized, thereby improving the surface quality of the silicon wafer.
以下說明本發明的矽晶圓的洗淨方法。The cleaning method of the silicon wafer of the present invention will be described below.
本發明之中的矽晶圓的洗淨，首先將矽晶圓進行SC1洗淨。藉此，藉由鹼性的洗淨液的矽晶圓表面的蝕刻而使附著微粒剝離，進一步利用矽晶圓與微粒的靜電反作用力抑制對矽晶圓的再附著而同時除去微粒。再者，藉由SC1洗淨，於矽晶圓的表面形成薄的化學氧化膜。In the cleaning of the silicon wafer in the present invention, firstly, the silicon wafer is cleaned by SC1. In this way, the adhered particles are peeled off by etching the surface of the silicon wafer with an alkaline cleaning solution, and the particles are removed while suppressing reattachment to the silicon wafer by utilizing the electrostatic reaction force between the silicon wafer and the particles. Furthermore, by cleaning with SC1, a thin chemical oxide film is formed on the surface of the silicon wafer.
之後，將經SC1洗淨的矽晶圓以具有氧化力的洗淨液進行洗淨，而進行化學氧化。如此一來，於SC1洗淨之後，以具有氧化力的洗淨液進行洗淨，藉此使化學氧化膜的厚度形成為較過去更厚的1.0 nm以上（1.2 nm以下為佳）。Afterwards, the silicon wafer cleaned by SC1 is cleaned with an oxidizing cleaning solution for chemical oxidation. In this way, after SC1 cleaning, cleaning with an oxidizing cleaning solution can make the thickness of the chemical oxide film 1.0 nm or more (preferably 1.2 nm or less) thicker than before.
再者，此時，作為具有氧化力的該洗淨液，使用臭氧水及／或雙氧水為佳。使用如此的洗淨液的場合，本發明特別有效。In this case, it is preferable to use ozone water and/or hydrogen peroxide as the cleaning liquid having oxidizing power. The present invention is particularly effective when such a cleaning solution is used.
再者，作為具有氧化力的洗淨液，使用臭氧水的場合，臭氧的濃度係10ppm上為佳。若臭氧水濃度大於10ppm，矽晶圓表面內的氧化會變得均一而為佳。Furthermore, when ozone water is used as the cleaning solution having oxidizing power, the concentration of ozone is preferably on the order of 10 ppm. If the concentration of ozone water is greater than 10ppm, the oxidation on the surface of the silicon wafer will become uniform, which is better.
再者，作為具有氧化力的洗淨液，使用雙氧水的場合，雙氧水（30wt%）及水的混合比例為H2 O2 ：H2 O=1：20~1：5且溫度為60℃以上為佳。藉由使用如此的洗淨液，矽晶圓的氧化充分，能夠更確實地使化學氧化膜形成為較過去更厚。Furthermore, when hydrogen peroxide is used as the cleaning liquid with oxidizing power, the mixing ratio of hydrogen peroxide (30wt%) and water is H2O2 : H2O =1:20~1:5 and the temperature is 60°C or higher. better. By using such a cleaning solution, the silicon wafer is sufficiently oxidized, and the chemical oxide film can be formed thicker than in the past more reliably.
再者，能夠於進行該SC1洗淨之後且以具有氧化力的該洗淨液進行洗淨之前，進行SC2洗淨。若為如此的矽晶圓的洗淨方法，藉由將矽晶圓表面的金屬雜質溶解除去，而能夠進一步提升矽晶圓表面品質。Furthermore, SC2 cleaning can be performed after performing the SC1 cleaning and before cleaning with the cleaning solution having oxidative power. According to such a cleaning method of the silicon wafer, the surface quality of the silicon wafer can be further improved by dissolving and removing the metal impurities on the surface of the silicon wafer.
再者，進行該SC1洗淨的矽晶圓為未進行DHF洗淨的矽晶圓為佳。若為如此的矽晶圓的洗淨方法，沒有預先除去形成於矽晶圓的表面的化學氧化膜的緣故，而能夠得到充分的化學氧化膜厚度，能夠更確實地提升矽晶圓表面品質。 ［實施例］Furthermore, it is preferable that the silicon wafer to be cleaned by SC1 is a silicon wafer that has not been cleaned by DHF. According to such a silicon wafer cleaning method, a sufficient thickness of the chemical oxide film can be obtained without removing the chemical oxide film formed on the surface of the silicon wafer in advance, and the surface quality of the silicon wafer can be improved more reliably. [Example]
以下表示實施例及比較例而更具體地說明本發明，但是本發明並非限定於這些實施例。Although Examples and Comparative Examples are shown below and the present invention will be described more specifically, the present invention is not limited to these Examples.
［比較例一］ 首先進行評估用矽晶圓的準備。準備：鏡面拋光後的乾淨的不具有被稱為COP及DSOD的結晶缺陷的300mm矽晶圓。COP係為：於藉由被稱為SC1洗淨的氨水與雙氧水的混合液將鏡面拋光後的矽晶圓予以洗淨後，在矽晶圓表面檢測出的結晶起因的凹坑狀的缺陷。此凹坑狀的缺陷，以微粒計數器的矽晶圓表面的測量而與微粒共同被檢測出。再者，COP係為使作為氧化膜的信賴性評估所進行的GOI（Gate Oxide Integrity）評估的TDDB（Time Dependent Dielectric Breakdown）及TZDB（Time Zero Dielectric Breakdown）劣化的原因。再者，Cu沉積法的DSOD評估也會作為DSOD缺陷而被檢測出。評估用矽晶圓為三片，其中二片用於DSOD評估，剩餘一片用於XPS的化學氧化膜厚度評估。[Comparative Example 1] First, silicon wafers for evaluation are prepared. Preparation: Mirror polished clean 300mm silicon wafer without crystal defects called COP and DSOD. COP is a pit-shaped defect caused by crystallization detected on the surface of a silicon wafer after the mirror-polished silicon wafer is cleaned by a mixture of ammonia and hydrogen peroxide called SC1 cleaning. The pit-like defects are detected together with the particles by the particle counter's measurement of the silicon wafer surface. Furthermore, COP is a cause of deterioration of TDDB (Time Dependent Dielectric Breakdown) and TZDB (Time Zero Dielectric Breakdown) of GOI (Gate Oxide Integrity) evaluation performed as an oxide film reliability evaluation. Furthermore, the DSOD evaluation of the Cu deposition method is also detected as a DSOD defect. There are three silicon wafers for evaluation, two of which are used for DSOD evaluation, and the remaining one is used for XPS evaluation of chemical oxide film thickness.
＜矽晶圓的洗淨＞ 將所準備的矽晶圓進行DHF洗淨，之後進行臭氧水的洗淨，進一步進行SC1洗淨。臭氧水的洗淨係以臭氧（O3 ）=10ppm，在25℃實施10min。SC1洗淨係以氨水（NH4 OH）：雙氧水（H2 O2 ）：H2 O=1：1：10的混合液作為洗淨液，在80℃實施10min。於DHF洗淨，使用HF為3.0wt%的洗淨液。混合液的調整所使用的藥品的濃度係NH4 OH為28wt%，H2 O2 為30wt%。<Cleaning of Silicon Wafer> The prepared silicon wafer is cleaned with DHF, then with ozone water, and then with SC1. Cleaning with ozone water is carried out at 25°C for 10 minutes with ozone (O 3 ) = 10 ppm. SC1 cleaning system uses ammonia water (NH 4 OH):hydrogen peroxide (H 2 O 2 ):H 2 O=1:1:10 mixture as the cleaning solution, and implements it at 80°C for 10 minutes. Wash in DHF, using 3.0wt% HF cleaning solution. The concentrations of the chemicals used in the adjustment of the mixed solution were 28 wt% for NH 4 OH and 30 wt% for H 2 O 2 .
＜化學氧化膜評估方法（DSOD評估）＞ 以Cu沉積法的DSOD評估進行洗淨後的矽晶圓的化學氧化膜評估。關於Cu沉積法的DSOD評估，記載於專利文獻4，如以下進行。藉由上述矽晶圓的洗淨而使化學氧化膜（氧化絕緣膜）形成於矽晶圓表面，將形成於矽晶圓表層的缺陷部位上的氧化絕緣膜予以破壞。然後，於經破壞的氧化膜部位使Cu沉積（deposition）而特定出缺陷。在存在有Cu離子的溶液之中，一旦對形成於矽晶圓表面的氧化膜施加電壓，電流會流向氧化膜有劣化的部分，Cu離子則會成為Cu而沉積。觀察此沉積的Cu而判斷為DSOD。此DSOD除了結晶缺陷的檢出以外，也能夠檢測出拋光及洗淨等的對矽晶圓表面品質造成影響的刮痕或金屬汙染等的處理異常。＜Chemical Oxide Film Evaluation Method (DSOD Evaluation)＞ The evaluation of the chemical oxide film on the cleaned silicon wafer was performed by the DSOD evaluation of the Cu deposition method. The evaluation of DSOD by the Cu deposition method is described in Patent Document 4 and performed as follows. A chemical oxide film (oxidation insulating film) is formed on the surface of the silicon wafer by cleaning the above-mentioned silicon wafer, and the oxide insulating film formed on the defective part of the surface layer of the silicon wafer is destroyed. Then, Cu is deposited on the damaged oxide film to identify defects. In a solution containing Cu ions, when a voltage is applied to the oxide film formed on the surface of the silicon wafer, current flows to the degraded part of the oxide film, and Cu ions are deposited as Cu. Observation of this deposited Cu was judged as DSOD. In addition to the detection of crystal defects, this DSOD can also detect processing abnormalities such as scratches and metal contamination that affect the surface quality of silicon wafers such as polishing and cleaning.
＜化學氧化膜評估方法（化學氧化膜厚度評估）＞ 再者，矽晶圓的化學氧化膜厚度係以XPS進行測量。XPS係對試料表面照射X光，並計測自試料表面放出的光電子的運動能量，藉此分析構成試料表面的元素的組成及化學結合狀態的手法。＜Chemical Oxide Film Evaluation Method (Chemical Oxide Film Thickness Evaluation)＞ Furthermore, the chemical oxide film thickness of the silicon wafer is measured by XPS. XPS is a technique that irradiates the surface of a sample with X-rays and measures the kinetic energy of photoelectrons emitted from the surface of the sample to analyze the composition and chemical bonding state of the elements constituting the surface of the sample.
化學氧化膜評估的結果，比較例一之中的化學氧化膜厚度為0.7 nm，關於進行DSOD評估的二片，DSOD個數分別為31、36個。As a result of the evaluation of the chemical oxide film, the thickness of the chemical oxide film in Comparative Example 1 was 0.7 nm, and the number of DSODs in the two pieces evaluated for DSOD were 31 and 36, respectively.
［比較例二］ 在矽晶圓的洗淨之中，除了SC1洗淨的洗淨液為NH4 OH：H2 O2 ：H2 O=1：1：20的混合液以外，與比較例一同樣地實施。 化學氧化膜評估的結果，比較例二之中的化學氧化膜厚度為0.7 nm，關於進行DSOD評估的二片，DSOD個數分別為34、39個。[Comparative Example 2] In the cleaning of silicon wafers, except that the cleaning solution for SC1 cleaning is a mixture of NH 4 OH:H 2 O 2 :H 2 O=1:1:20, the same as in Comparative Example Implement in the same way. As a result of the evaluation of the chemical oxide film, the thickness of the chemical oxide film in Comparative Example 2 is 0.7 nm, and the number of DSODs of the two pieces evaluated for DSOD are 34 and 39, respectively.
［比較例三］ 在矽晶圓的洗淨之中，除了於SC1洗淨後進行SC2洗淨以外，與比較例一同樣地實施。SC2洗淨係以鹽酸（HCl）：H2 O2 ：H2 O=1：1：100的混合液作為洗淨液，在80℃實施10min。 化學氧化膜評估的結果，比較例三之中的化學氧化膜厚度為0.7 nm，關於進行DSOD評估的二片，DSOD個數分別為29、35個。[Comparative Example 3] Cleaning of the silicon wafer was carried out in the same manner as in Comparative Example 1, except that SC2 cleaning was performed after SC1 cleaning. SC2 cleaning system uses a mixture of hydrochloric acid (HCl): H 2 O 2 : H 2 O = 1:1:100 as the cleaning solution, and implements it at 80°C for 10 minutes. As a result of the evaluation of the chemical oxide film, the thickness of the chemical oxide film in Comparative Example 3 is 0.7 nm, and the number of DSODs for the two pieces evaluated for DSOD are 29 and 35, respectively.
［比較例四］ 在矽晶圓的洗淨之中，除了SC2洗淨的洗淨液為HCl：H2 O2 ：H2 O=1：1：50的混合液以外，與比較例三同樣地實施。 化學氧化膜評估的結果，比較例四之中的化學氧化膜厚度為0.7 nm，關於進行DSOD評估的二片，DSOD個數分別為31、33個。[Comparative Example 4] In the cleaning of silicon wafers, except that the cleaning solution for SC2 cleaning is a mixture of HCl:H 2 O 2 :H 2 O=1:1:50, it is the same as Comparative Example 3 implemented. As a result of the evaluation of the chemical oxide film, the thickness of the chemical oxide film in Comparative Example 4 is 0.7 nm, and the number of DSODs for the two pieces evaluated for DSOD are 31 and 33, respectively.
［比較例五］ 在矽晶圓的洗淨之中，除了在DHF洗淨之中使用HF為1.0wt%的洗淨液以外，與比較例一同樣地實施。 化學氧化膜評估的結果，比較例五之中的化學氧化膜厚度為0.7 nm，關於進行DSOD評估的二片，DSOD個數分別為35、40個。[Comparative Example 5] Cleaning of the silicon wafer was carried out in the same manner as in Comparative Example 1 except that a cleaning solution having 1.0 wt % of HF was used for DHF cleaning. As a result of the evaluation of the chemical oxide film, the thickness of the chemical oxide film in Comparative Example 5 is 0.7 nm, and the number of DSOD for the two pieces evaluated for DSOD is 35 and 40, respectively.
［實施例一］ 除了將矽晶圓的洗淨改為於SC1洗淨後藉由臭氧水進行洗淨以外，與比較例一同樣地實施。 化學氧化膜評估的結果，實施例一之中的化學氧化膜厚度為1.0 nm，關於進行DSOD評估的二片，DSOD個數分別為13、16個。[Example 1] Except for changing the cleaning of the silicon wafer to cleaning with ozone water after the SC1 cleaning, it was carried out in the same manner as Comparative Example 1. As a result of the evaluation of the chemical oxide film, the thickness of the chemical oxide film in Example 1 is 1.0 nm, and the number of DSOD for the two pieces evaluated for DSOD is 13 and 16 respectively.
［實施例二］ 在矽晶圓的洗淨之中，除了使用臭氧（O3 ）＝30 ppm的洗淨液作為臭氧水以外，與實施例一同樣地實施。 化學氧化膜評估的結果，實施例二之中的化學氧化膜厚度為1.0 nm，關於進行DSOD評估的二片，DSOD個數分別為11、17個。[Example 2] Cleaning of a silicon wafer was carried out in the same manner as in Example 1 except that a cleaning liquid having ozone (O 3 )=30 ppm was used as ozone water. As a result of the evaluation of the chemical oxide film, the thickness of the chemical oxide film in Example 2 is 1.0 nm, and the number of DSODs for the two pieces evaluated for DSOD are 11 and 17, respectively.
［實施例三］ 在矽晶圓的洗淨之中，除了將藉由臭氧水的洗淨的時間定為1 min以外，與實施例二同樣地實施。 化學氧化膜評估的結果，實施例三之中的化學氧化膜厚度為1.0 nm，關於進行DSOD評估的二片，DSOD個數分別為15、17個。[Embodiment 3] Cleaning of the silicon wafer was carried out in the same manner as in Example 2 except that the time for cleaning with ozone water was set to 1 min. As a result of the evaluation of the chemical oxide film, the thickness of the chemical oxide film in Example 3 is 1.0 nm, and the number of DSODs for the two pieces evaluated for DSOD are 15 and 17 respectively.
［實施例四］ 在矽晶圓的洗淨之中，除了於SC1洗淨後且以臭氧水的洗淨之前進行SC2洗淨以外，與實施例一同樣地實施。SC2洗淨係與比較例三同樣地實施。 化學氧化膜評估的結果，實施例四之中的化學氧化膜厚度為1.0 nm，關於進行DSOD評估的二片，DSOD個數分別為16、18個。[Example 4] Cleaning of the silicon wafer was carried out in the same manner as in Example 1, except that SC2 cleaning was performed after SC1 cleaning and before cleaning with ozone water. SC2 cleaning was performed in the same manner as in Comparative Example 3. As a result of the evaluation of the chemical oxide film, the thickness of the chemical oxide film in Example 4 is 1.0 nm, and the number of DSODs for the two pieces evaluated for DSOD is 16 and 18, respectively.
［實施例五］ 在矽晶圓的洗淨之中，除了將以臭氧水的洗淨替換成進行以雙氧水的洗淨以外，與實施例一同樣地實施。以雙氧水的洗淨，洗淨液為H2 O2 ：H2 O＝1：10的混合液，在80℃實施10min。 化學氧化膜評估的結果，實施例五之中的化學氧化膜厚度為1.0 nm，關於進行DSOD評估的二片，DSOD個數分別為17、19個。[Example 5] Cleaning of the silicon wafer was carried out in the same manner as in Example 1, except that the cleaning with ozone water was replaced with the cleaning with hydrogen peroxide. Washing with hydrogen peroxide, the washing solution is a mixture of H 2 O 2 :H 2 O=1:10, and it is carried out at 80°C for 10 minutes. As a result of the evaluation of the chemical oxide film, the thickness of the chemical oxide film in Example 5 is 1.0 nm, and the number of DSODs of the two pieces evaluated for DSOD are 17 and 19 respectively.
［實施例六］ 在矽晶圓的洗淨之中，除了將以雙氧水的洗淨的洗淨液改為H2 O2 ：H2 O＝1：20的混合液以外，與實施例五同樣地實施。 化學氧化膜評估的結果，實施例六之中的化學氧化膜厚度為1.0 nm，關於進行DSOD評估的二片，DSOD個數分別為13、15個。[Example 6] In the cleaning of the silicon wafer, except that the cleaning solution used for cleaning with hydrogen peroxide is changed to a mixed solution of H 2 O 2 : H 2 O = 1:20, the same as in Example 5 implemented. As a result of the evaluation of the chemical oxide film, the thickness of the chemical oxide film in Example 6 is 1.0 nm, and the number of DSODs of the two pieces evaluated for DSOD are 13 and 15 respectively.
［實施例七］ 在矽晶圓的洗淨之中，除了於SC1洗淨後且以臭氧水的洗淨之前進行SC2洗淨，並在60℃實施以雙氧水的洗淨以外，與實施例五同樣地實施。SC2洗淨係與比較例三同樣地實施。 化學氧化膜評估的結果，實施例七之中的化學氧化膜厚度為1.0 nm，關於進行DSOD評估的二片，DSOD個數分別為12、16個。[Embodiment 7] Cleaning of the silicon wafer was carried out in the same manner as in Example 5, except that SC2 cleaning was performed after SC1 cleaning and before cleaning with ozone water, and cleaning with hydrogen peroxide was performed at 60°C. SC2 cleaning was performed in the same manner as in Comparative Example 3. As a result of the evaluation of the chemical oxide film, the thickness of the chemical oxide film in Example 7 is 1.0 nm, and the number of DSOD of the two pieces evaluated for DSOD is 12 and 16 respectively.
【表1】
比較例一至五的化學氧化膜厚度為0.7 nm，實施例一至七的化學氧化膜厚度為1.0 nm。相對於比較例的化學氧化膜厚度為0.7 nm，實施例的化學氧化膜厚度為較比較例更厚的1.0 nm，推測是因為：由於比較例的化學氧化膜係以SC1洗淨所形成，SC1洗淨係氧化與蝕刻的平衡反應，故化學氧化膜在飽和之前就達到平衡狀態。另一方面，推測：由於在實施例之中，將以SC1洗淨所形成的化學氧化膜，以具有氧化力的洗淨液（臭氧水、雙氧水）進一步進行氧化，故能夠使化學氧化膜厚度形成為厚厚的1.0 nm。 另外，要將化學氧化膜厚度在此之上再增厚，則在矽晶圓的製造之中在現實的時間內係為困難。The thickness of the chemical oxide film in Comparative Examples 1 to 5 is 0.7 nm, and the thickness of the chemical oxide film in Examples 1 to 7 is 1.0 nm. Compared with the thickness of the chemical oxide film of the comparative example which is 0.7 nm, the thickness of the chemical oxide film of the embodiment is 1.0 nm which is thicker than that of the comparative example. Cleaning is an equilibrium reaction of oxidation and etching, so the chemical oxide film reaches an equilibrium state before saturation. On the other hand, it is speculated that: in the embodiment, the chemical oxide film formed by cleaning with SC1 is further oxidized with a cleaning solution (ozone water, hydrogen peroxide) with oxidative power, so the thickness of the chemical oxide film can be reduced. Formed to a thickness of 1.0 nm. In addition, it is difficult to increase the thickness of the chemical oxide film beyond this in real time in the manufacture of silicon wafers.
進一步，藉由使用如同本發明的矽晶圓的洗淨方法，能夠使實施例之中藉由DSOD評估所測量的DSOD的個數大幅地減少成比較例之中藉由DSOD評估所測量的DSOD的個數的約一半至一半以下，而能夠將洗淨所致的矽晶圓品質的惡化予以抑制。Further, by using the cleaning method of the silicon wafer as in the present invention, the number of DSODs measured by DSOD evaluation in Examples can be significantly reduced to the DSOD measured by DSOD evaluation in Comparative Examples About half to less than half of the number of silicon wafers can suppress the deterioration of the quality of silicon wafers caused by cleaning.
此外，本發明並不限定於上述的實施例。上述實施例為舉例說明，凡具有與本發明的申請專利範圍所記載之技術思想實質上同樣之構成，產生相同的功效者，不論為何物皆包含在本發明的技術範圍內。In addition, this invention is not limited to the above-mentioned Example. The above-mentioned embodiments are for illustration, and those who have substantially the same structure and produce the same effect as the technical idea recorded in the patent application scope of the present invention, no matter what they are, are included in the technical scope of the present invention.
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