TWI254075B - Cleaning composition comprising ozone and hydrofluoroether fluorinated solvent and method of cleaning a substrate - Google Patents
Cleaning composition comprising ozone and hydrofluoroether fluorinated solvent and method of cleaning a substrate Download PDFInfo
- Publication number
- TWI254075B TWI254075B TW090105710A TW90105710A TWI254075B TW I254075 B TWI254075 B TW I254075B TW 090105710 A TW090105710 A TW 090105710A TW 90105710 A TW90105710 A TW 90105710A TW I254075 B TWI254075 B TW I254075B
- Authority
- TW
- Taiwan
- Prior art keywords
- group
- composition
- solvent
- ozone
- fluorinated
- Prior art date
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/39—Organic or inorganic per-compounds
- C11D3/3947—Liquid compositions
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/02—Inorganic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/50—Solvents
- C11D7/5004—Organic solvents
- C11D7/5018—Halogenated solvents
-
- 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
-
- 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
- H01L21/02082—Cleaning product to be cleaned
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/14—Hard surfaces
- C11D2111/22—Electronic devices, e.g. PCBs or semiconductors
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/263—Ethers
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/264—Aldehydes; Ketones; Acetals or ketals
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/265—Carboxylic acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/266—Esters or carbonates
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
- C11D7/3263—Amides or imides
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
- C11D7/3281—Heterocyclic compounds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S134/00—Cleaning and liquid contact with solids
- Y10S134/902—Semiconductor wafer
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Detergent Compositions (AREA)
- Cleaning Or Drying Semiconductors (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US09/540,590 US6372700B1 (en) | 2000-03-31 | 2000-03-31 | Fluorinated solvent compositions containing ozone |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| TWI254075B true TWI254075B (en) | 2006-05-01 |
Family
ID=24156103
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| TW090105710A TWI254075B (en) | 2000-03-31 | 2001-03-12 | Cleaning composition comprising ozone and hydrofluoroether fluorinated solvent and method of cleaning a substrate |
Country Status (9)
| Country | Link |
|---|---|
| US (2) | US6372700B1 (enExample) |
| EP (1) | EP1268734B1 (enExample) |
| JP (1) | JP4532806B2 (enExample) |
| KR (1) | KR100728845B1 (enExample) |
| AT (1) | ATE280214T1 (enExample) |
| AU (1) | AU2000268956A1 (enExample) |
| DE (1) | DE60015190T2 (enExample) |
| TW (1) | TWI254075B (enExample) |
| WO (1) | WO2001074985A1 (enExample) |
Families Citing this family (31)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6552090B1 (en) * | 1997-09-15 | 2003-04-22 | 3M Innovative Properties Company | Perfluoroalkyl haloalkyl ethers and compositions and applications thereof |
| US6372700B1 (en) * | 2000-03-31 | 2002-04-16 | 3M Innovative Properties Company | Fluorinated solvent compositions containing ozone |
| TWI250206B (en) * | 2000-06-01 | 2006-03-01 | Asahi Kasei Corp | Cleaning agent, cleaning method and cleaning apparatus |
| US6678082B2 (en) | 2001-09-12 | 2004-01-13 | Harris Corporation | Electro-optical component including a fluorinated poly(phenylene ether ketone) protective coating and related methods |
| JP3914842B2 (ja) * | 2001-10-23 | 2007-05-16 | 有限会社ユーエムエス | 有機被膜の除去方法および除去装置 |
| DE10229041A1 (de) * | 2002-06-28 | 2004-01-22 | Solvay Fluor Und Derivate Gmbh | Herstellung homogener Gasgemische |
| CN1678961B (zh) * | 2002-08-22 | 2010-05-05 | 大金工业株式会社 | 剥离液 |
| US7087805B2 (en) * | 2002-10-22 | 2006-08-08 | Steris Inc. | Use of an ozone containing fluid to neutralize chemical and/or biological warfare agents |
| EP1563952B1 (en) * | 2002-11-06 | 2013-06-26 | Nomura Plating Co., Ltd | Surface treatment method for vacuum vessel or pipe |
| US20040117918A1 (en) * | 2002-12-11 | 2004-06-24 | The Procter & Gamble Company | Fluorine-containing solvents and compositions and methods employing same |
| US6884338B2 (en) | 2002-12-16 | 2005-04-26 | 3M Innovative Properties Company | Methods for polishing and/or cleaning copper interconnects and/or film and compositions therefor |
| US7147767B2 (en) | 2002-12-16 | 2006-12-12 | 3M Innovative Properties Company | Plating solutions for electrochemical or chemical deposition of copper interconnects and methods therefor |
| US6858124B2 (en) | 2002-12-16 | 2005-02-22 | 3M Innovative Properties Company | Methods for polishing and/or cleaning copper interconnects and/or film and compositions therefor |
| DE602004013154T2 (de) | 2003-06-27 | 2009-05-14 | Asahi Glass Co., Ltd. | Reinigungs/spülverfahren |
| US20050106774A1 (en) * | 2003-11-13 | 2005-05-19 | Dmitri Simonian | Surface processes in fabrications of microstructures |
| US7071154B2 (en) * | 2003-12-18 | 2006-07-04 | 3M Innovative Properties Company | Azeotrope-like compositions and their use |
| JP2005217262A (ja) * | 2004-01-30 | 2005-08-11 | Matsushita Electric Ind Co Ltd | 化合物半導体装置の製造方法 |
| KR100627139B1 (ko) * | 2004-06-18 | 2006-09-25 | 한국전자통신연구원 | 미세기전 구조물 그 제조방법 |
| JP4559250B2 (ja) * | 2005-02-16 | 2010-10-06 | シチズンファインテックミヨタ株式会社 | アクチュエータ、及びその製造方法 |
| JP2006278966A (ja) * | 2005-03-30 | 2006-10-12 | Toshiba Corp | 半導体製造装置 |
| US20070129273A1 (en) * | 2005-12-07 | 2007-06-07 | Clark Philip G | In situ fluoride ion-generating compositions and uses thereof |
| JP4803821B2 (ja) * | 2007-03-23 | 2011-10-26 | 大日本スクリーン製造株式会社 | 基板処理装置 |
| JP2010529670A (ja) * | 2007-06-07 | 2010-08-26 | レール・リキード−ソシエテ・アノニム・プール・レテュード・エ・レクスプロワタシオン・デ・プロセデ・ジョルジュ・クロード | 半導体適用のための非可燃性溶媒 |
| US8071816B2 (en) * | 2008-06-30 | 2011-12-06 | 3M Innovative Properties Company | Hydrofluoroacetal compounds and processes for their preparation and use |
| TWI558876B (zh) * | 2010-07-05 | 2016-11-21 | 大陽日酸股份有限公司 | 表面氧化處理方法及表面氧化處理裝置 |
| US20120039796A1 (en) * | 2010-08-15 | 2012-02-16 | Demetrios Markou | Novel method for creating, suspending and stabilizing electronically modified oxygen derivatives, along with creating, suspending and stabilizing electronically modified reaction intermediates, in a bio compatible fluorocarbon suspension, for the purpose of inducing a cascading immune response in mammalian patients |
| JP5862353B2 (ja) * | 2011-08-05 | 2016-02-16 | 東京エレクトロン株式会社 | 半導体装置の製造方法 |
| JP5630679B1 (ja) * | 2013-09-08 | 2014-11-26 | 株式会社E・テック | 揮発性消毒剤、揮発性消毒剤の製造方法 |
| US9321635B2 (en) * | 2013-11-28 | 2016-04-26 | Solid State System Co., Ltd. | Method to release diaphragm in MEMS device |
| JP2016164977A (ja) * | 2015-02-27 | 2016-09-08 | キヤノン株式会社 | ナノインプリント用液体材料、ナノインプリント用液体材料の製造方法、硬化物パターンの製造方法、光学部品の製造方法、回路基板の製造方法、および電子部品の製造方法 |
| WO2017165637A1 (en) * | 2016-03-24 | 2017-09-28 | Avantor Performance Materials, Llc | Non-aqueous tungsten compatible metal nitride selective etchants and cleaners |
Family Cites Families (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3235335A (en) * | 1958-01-30 | 1966-02-15 | Olin Mathieson | Stabilized liquid ozone |
| DE1298514B (de) | 1965-12-02 | 1969-07-03 | Hoechst Ag | Verfahren zur Herstellung von Perfluoralkyl-alkyl-aethern |
| FR2287432A1 (fr) | 1974-10-10 | 1976-05-07 | Poudres & Explosifs Ste Nale | Nouveaux ethers fluores et leur procede de preparation |
| US4182663A (en) | 1978-03-13 | 1980-01-08 | Vaseen Vesper A | Converting oxygen to ozone by U.V. radiation of a halogen saturated hydrocarbon liquid containing dissolved or absorbed oxygen |
| JP3016301B2 (ja) * | 1992-04-15 | 2000-03-06 | 三菱電機株式会社 | 洗浄方法 |
| JP2589930B2 (ja) | 1993-03-05 | 1997-03-12 | 工業技術院長 | メチル 1,1,2,2,3,3−ヘキサフルオロプロピル エーテル及びその製造方法並びにこれを含有する洗浄剤 |
| JP2551522B2 (ja) * | 1993-06-29 | 1996-11-06 | 株式会社白洋舎 | 漂白・脱臭・殺菌方法 |
| US5658962A (en) | 1994-05-20 | 1997-08-19 | Minnesota Mining And Manufacturing Company | Omega-hydrofluoroalkyl ethers, precursor carboxylic acids and derivatives thereof, and their preparation and application |
| US5603750A (en) | 1995-08-14 | 1997-02-18 | Minnesota Mining And Manufacturing Company | Fluorocarbon fluids as gas carriers to aid in precious and base metal heap leaching operations |
| WO1997022683A1 (en) * | 1995-12-15 | 1997-06-26 | Minnesota Mining And Manufacturing Company | Cleaning process and composition |
| US5750797A (en) | 1996-04-15 | 1998-05-12 | Minnesota Mining And Manufacturing Company | Process for the production of hydrofluoroethers |
| DE19701971C1 (de) | 1997-01-22 | 1998-11-26 | Invent Gmbh Entwicklung Neuer Technologien | Verfahren und Vorrichtung zur Reinigung von Substratoberflächen |
| US5882425A (en) | 1997-01-23 | 1999-03-16 | Semitool, Inc. | Composition and method for passivation of a metallization layer of a semiconductor circuit after metallization etching |
| US6552090B1 (en) | 1997-09-15 | 2003-04-22 | 3M Innovative Properties Company | Perfluoroalkyl haloalkyl ethers and compositions and applications thereof |
| JP4299966B2 (ja) | 1997-09-23 | 2009-07-22 | エスイーゼツト・アクチエンゲゼルシヤフト | 改善された化学的乾燥及び清浄化システム |
| US6046368A (en) | 1998-03-17 | 2000-04-04 | 3M Innovative Properties Company | Catalytic process for making hydrofluoroethers |
| US5914003A (en) | 1998-06-09 | 1999-06-22 | Mach I, Inc. | Cellulose oxidation |
| JP4107720B2 (ja) * | 1998-07-07 | 2008-06-25 | スリーエム カンパニー | 半導体製造装置における汚染物の洗浄方法 |
| US6297308B1 (en) * | 1999-10-07 | 2001-10-02 | 3M Innovative Properties Company | Chemical compositions |
| US6372700B1 (en) * | 2000-03-31 | 2002-04-16 | 3M Innovative Properties Company | Fluorinated solvent compositions containing ozone |
| US6310018B1 (en) * | 2000-03-31 | 2001-10-30 | 3M Innovative Properties Company | Fluorinated solvent compositions containing hydrogen fluoride |
-
2000
- 2000-03-31 US US09/540,590 patent/US6372700B1/en not_active Expired - Lifetime
- 2000-08-08 AU AU2000268956A patent/AU2000268956A1/en not_active Abandoned
- 2000-08-08 EP EP00957319A patent/EP1268734B1/en not_active Expired - Lifetime
- 2000-08-08 WO PCT/US2000/021598 patent/WO2001074985A1/en not_active Ceased
- 2000-08-08 AT AT00957319T patent/ATE280214T1/de not_active IP Right Cessation
- 2000-08-08 JP JP2001572661A patent/JP4532806B2/ja not_active Expired - Fee Related
- 2000-08-08 DE DE60015190T patent/DE60015190T2/de not_active Expired - Lifetime
- 2000-08-08 KR KR1020027012923A patent/KR100728845B1/ko not_active Expired - Fee Related
-
2001
- 2001-03-12 TW TW090105710A patent/TWI254075B/zh not_active IP Right Cessation
-
2002
- 2002-01-07 US US10/041,924 patent/US6537380B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| US6372700B1 (en) | 2002-04-16 |
| EP1268734B1 (en) | 2004-10-20 |
| KR20020081595A (ko) | 2002-10-28 |
| JP2003529925A (ja) | 2003-10-07 |
| US20020107160A1 (en) | 2002-08-08 |
| WO2001074985A1 (en) | 2001-10-11 |
| AU2000268956A1 (en) | 2001-10-15 |
| KR100728845B1 (ko) | 2007-06-14 |
| JP4532806B2 (ja) | 2010-08-25 |
| US6537380B2 (en) | 2003-03-25 |
| EP1268734A1 (en) | 2003-01-02 |
| ATE280214T1 (de) | 2004-11-15 |
| DE60015190T2 (de) | 2006-03-09 |
| DE60015190D1 (de) | 2004-11-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| TWI254075B (en) | Cleaning composition comprising ozone and hydrofluoroether fluorinated solvent and method of cleaning a substrate | |
| JP4786111B2 (ja) | 弗化水素を含有する弗素化溶媒組成物 | |
| TWI299360B (en) | Processing of substrates with dense fluids comprising acetylenic diols and/or alcohols | |
| TWI379174B (en) | Nanoelectronic and microelectronic cleaning compositions | |
| KR102434147B1 (ko) | 반도체 기판상의 잔류물을 제거하기 위한 세정 제형 | |
| US10626353B2 (en) | Cleaning formulations | |
| TW200846462A (en) | Liquid cleaner for the removal of post-etch residues | |
| KR102490840B1 (ko) | 반도체 기판상의 잔류물을 제거하기 위한 세정 조성물 | |
| TW200913046A (en) | Method for removing contamination with fluorinated compositions | |
| TW200521222A (en) | Lactam compositions for cleaning organic and plasma etched residues for semiconductor devices | |
| TWI882010B (zh) | 包含氫氟醚的溶劑及使用包含氫氟醚之溶劑的基板處理方法 | |
| JP2021519836A (ja) | 洗浄用組成物 | |
| JP6010894B2 (ja) | 洗浄乾燥剤およびそれを用いた基板の洗浄乾燥方法 | |
| KR100734342B1 (ko) | 아세틸렌계 디올 및/또는 알콜을 포함하는 고밀도 유체를사용한 기판의 처리 | |
| US20210157242A1 (en) | Photoresist-removing liquid and photoresist-removing method | |
| CN101326262A (zh) | 就地生成氟离子的组合物及其用途 | |
| KR20160051184A (ko) | 포스트-에칭 포토레지스트 에칭 중합체 및 잔류물을 제거하기 위한 스트리퍼 조성물 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| MM4A | Annulment or lapse of patent due to non-payment of fees |