TWI398515B - 電子材料用洗淨劑及洗淨方法 - Google Patents
電子材料用洗淨劑及洗淨方法 Download PDFInfo
- Publication number
- TWI398515B TWI398515B TW097148830A TW97148830A TWI398515B TW I398515 B TWI398515 B TW I398515B TW 097148830 A TW097148830 A TW 097148830A TW 97148830 A TW97148830 A TW 97148830A TW I398515 B TWI398515 B TW I398515B
- Authority
- TW
- Taiwan
- Prior art keywords
- acid
- group
- detergent
- cleaning
- carbon atoms
- Prior art date
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- 238000000034 method Methods 0.000 title claims description 34
- 239000012459 cleaning agent Substances 0.000 title claims description 8
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- WHFQAROQMWLMEY-UHFFFAOYSA-N propylene dimer Chemical compound CC=C.CC=C WHFQAROQMWLMEY-UHFFFAOYSA-N 0.000 description 1
- 230000005588 protonation Effects 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 150000003222 pyridines Chemical class 0.000 description 1
- 229940079877 pyrogallol Drugs 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- SBYHFKPVCBCYGV-UHFFFAOYSA-N quinuclidine Chemical compound C1CC2CCN1CC2 SBYHFKPVCBCYGV-UHFFFAOYSA-N 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 125000003548 sec-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- FDRCDNZGSXJAFP-UHFFFAOYSA-M sodium chloroacetate Chemical compound [Na+].[O-]C(=O)CCl FDRCDNZGSXJAFP-UHFFFAOYSA-M 0.000 description 1
- BEOOHQFXGBMRKU-UHFFFAOYSA-N sodium cyanoborohydride Chemical compound [Na+].[B-]C#N BEOOHQFXGBMRKU-UHFFFAOYSA-N 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- DGPIGKCOQYBCJH-UHFFFAOYSA-M sodium;acetic acid;hydroxide Chemical compound O.[Na+].CC([O-])=O DGPIGKCOQYBCJH-UHFFFAOYSA-M 0.000 description 1
- SUBJHSREKVAVAR-UHFFFAOYSA-N sodium;methanol;methanolate Chemical compound [Na+].OC.[O-]C SUBJHSREKVAVAR-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000001593 sorbitan monooleate Substances 0.000 description 1
- 235000011069 sorbitan monooleate Nutrition 0.000 description 1
- 229940035049 sorbitan monooleate Drugs 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000010421 standard material Substances 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 230000001180 sulfating effect Effects 0.000 description 1
- 230000019635 sulfation Effects 0.000 description 1
- 238000005670 sulfation reaction Methods 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Inorganic materials O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 1
- HIFJUMGIHIZEPX-UHFFFAOYSA-N sulfuric acid;sulfur trioxide Chemical compound O=S(=O)=O.OS(O)(=O)=O HIFJUMGIHIZEPX-UHFFFAOYSA-N 0.000 description 1
- DHCDFWKWKRSZHF-UHFFFAOYSA-N sulfurothioic S-acid Chemical compound OS(O)(=O)=S DHCDFWKWKRSZHF-UHFFFAOYSA-N 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- 125000001973 tert-pentyl group Chemical group [H]C([H])([H])C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 150000005621 tetraalkylammonium salts Chemical class 0.000 description 1
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 description 1
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 description 1
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical compound C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 description 1
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 description 1
- WJCNZQLZVWNLKY-UHFFFAOYSA-N thiabendazole Chemical compound S1C=NC(C=2NC3=CC=CC=C3N=2)=C1 WJCNZQLZVWNLKY-UHFFFAOYSA-N 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 150000003573 thiols Chemical class 0.000 description 1
- UAXOELSVPTZZQG-UHFFFAOYSA-N tiglic acid Natural products CC(C)=C(C)C(O)=O UAXOELSVPTZZQG-UHFFFAOYSA-N 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- 229960000984 tocofersolan Drugs 0.000 description 1
- 235000010384 tocopherol Nutrition 0.000 description 1
- 229930003799 tocopherol Natural products 0.000 description 1
- 239000011732 tocopherol Substances 0.000 description 1
- 229960001295 tocopherol Drugs 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- ILJSQTXMGCGYMG-UHFFFAOYSA-N triacetic acid Chemical compound CC(=O)CC(=O)CC(O)=O ILJSQTXMGCGYMG-UHFFFAOYSA-N 0.000 description 1
- 125000005270 trialkylamine group Chemical group 0.000 description 1
- 150000003918 triazines Chemical class 0.000 description 1
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 1
- GRNRCQKEBXQLAA-UHFFFAOYSA-M triethyl(2-hydroxyethyl)azanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CCO GRNRCQKEBXQLAA-UHFFFAOYSA-M 0.000 description 1
- YFNKIDBQEZZDLK-UHFFFAOYSA-N triglyme Chemical compound COCCOCCOCCOC YFNKIDBQEZZDLK-UHFFFAOYSA-N 0.000 description 1
- 239000013638 trimer Substances 0.000 description 1
- PDSVZUAJOIQXRK-UHFFFAOYSA-N trimethyl(octadecyl)azanium Chemical compound CCCCCCCCCCCCCCCCCC[N+](C)(C)C PDSVZUAJOIQXRK-UHFFFAOYSA-N 0.000 description 1
- GLFDLEXFOHUASB-UHFFFAOYSA-N trimethyl(tetradecyl)azanium Chemical compound CCCCCCCCCCCCCC[N+](C)(C)C GLFDLEXFOHUASB-UHFFFAOYSA-N 0.000 description 1
- 125000003258 trimethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- ZNEOHLHCKGUAEB-UHFFFAOYSA-N trimethylphenylammonium Chemical compound C[N+](C)(C)C1=CC=CC=C1 ZNEOHLHCKGUAEB-UHFFFAOYSA-N 0.000 description 1
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 description 1
- IJGSGCGKAAXRSC-UHFFFAOYSA-M tris(2-hydroxyethyl)-methylazanium;hydroxide Chemical compound [OH-].OCC[N+](C)(CCO)CCO IJGSGCGKAAXRSC-UHFFFAOYSA-M 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000000230 xanthan gum Substances 0.000 description 1
- 229920001285 xanthan gum Polymers 0.000 description 1
- 235000010493 xanthan gum Nutrition 0.000 description 1
- 229940082509 xanthan gum Drugs 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 235000004835 α-tocopherol Nutrition 0.000 description 1
- 239000002076 α-tocopherol Substances 0.000 description 1
- 235000007680 β-tocopherol Nutrition 0.000 description 1
- 239000011590 β-tocopherol Substances 0.000 description 1
- FGYKUFVNYVMTAM-WAZJVIJMSA-N β-tocotrienol Chemical compound OC1=CC(C)=C2O[C@@](CC/C=C(C)/CC/C=C(C)/CCC=C(C)C)(C)CCC2=C1C FGYKUFVNYVMTAM-WAZJVIJMSA-N 0.000 description 1
- 239000002478 γ-tocopherol Substances 0.000 description 1
- QUEDXNHFTDJVIY-DQCZWYHMSA-N γ-tocopherol Chemical compound OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1 QUEDXNHFTDJVIY-DQCZWYHMSA-N 0.000 description 1
- 239000002446 δ-tocopherol Substances 0.000 description 1
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
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/04—Carboxylic acids or salts thereof
- C11D1/06—Ether- or thioether carboxylic acids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
-
- 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
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/14—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
- C11D1/143—Sulfonic acid esters
-
- 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
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/14—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
- C11D1/146—Sulfuric acid esters
-
- 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
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/34—Derivatives of acids of phosphorus
- C11D1/342—Phosphonates; Phosphinates or phosphonites
-
- 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
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/34—Derivatives of acids of phosphorus
- C11D1/345—Phosphates or phosphites
-
- 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
- C11D3/43—Solvents
-
- 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
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/40—Specific cleaning or washing processes
- C11D2111/46—Specific cleaning or washing processes applying energy, e.g. irradiation
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Detergent Compositions (AREA)
- Cleaning Or Drying Semiconductors (AREA)
Description
本發明是有關於一種電子材料用洗淨劑及洗淨方法。更詳細而言,本發明是有關於一種可較好地用於平面顯示器(flat panel display)基板、光罩(photomask)基板、硬碟(hard disk)基板或半導體(semiconductor)基板的洗淨劑及洗淨方法。
電子材料的洗淨技術中,在製造時殘留在基板上的微量有機物污漬、或玻璃屑(glass cullet)及砥粒(abrasive grain)等雜質會對電子材料的性能或良率造成大的影響,因此其管理變得極為重要。尤其是,由於成為洗淨對象的雜質變得微粒子(微粒,particle)化,與至今為止相比更容易附著、殘留在界面上,故而迫切需要確立高度洗淨技術。因此,為了防止這些微粒所造成的污染,提出有使用界面活性劑來提高微粒除去性的方法(參照日本專利特開2007-39627號公報、日本專利特開2004-2691號公報、日本專利特開2001-276759號公報、)。
但是,在製造平面顯示器、光罩、硬碟及半導體用的玻璃或矽基板的步驟中,存在如下問題:視需要自玻璃母板(mother glass)上切割適當大小的玻璃基板時所產生的玻璃切割屑(通稱為玻璃屑)、飛濺至無塵室(clean room)內的灰塵或加工油等有機物污漬、或者使基板表面粗糙化(texturing)的步驟中所使用的研磨劑或研磨屑等會牢固
地附著在基板表面上,而在洗淨步驟中無法將這些充分地除去。
由於以這些玻璃屑、有機物污漬、研磨劑及研磨屑為代表的微粒會牢固地附著在基板表面上,故而為了將這些微粒充分地除去,需要對基板或研磨劑表面稍加蝕刻,使微粒分散至液體中,並且使分散在液體中的微粒不會再次附著在基板表面上。但是,日本專利特開2007-39627號公報中所提出的洗淨劑是含有烷基葡萄糖苷(alkyl glucoside)、甘油醚(glyceryl ether)及烴的洗淨液,雖然可期待其對有機污漬的除去性,但存在玻璃屑除去性不充分的問題,進而藉由含有鹼性試劑,可期待藉由蝕刻來除去微粒,但存在洗淨後的基板表面變得粗糙的問題。另外,日本專利特開2004-2691號公報中提出有含有特定非離子性界面活性劑、特定二醇醚(glycol ether)化合物及烴的洗淨劑,以及含有烴、特定二醇醚、陰離子性界面活性劑及二甲基亞碸(dimethyl sulfoxide)的洗淨劑,前一洗淨劑為了提高微粒除去性能而使用非離子性界面活性劑,但由於界面活性劑成分容易殘留在電子材料表面上,故而存在沖洗(rinse)性不良,良率降低的問題;另外,後一洗淨劑為了提高滲透性而含有平均碳數為10~20的磺基琥珀酸(sulfosuccinic acid)型陰離子性界面活性劑等,雖然可見微粒除去性之改善,但起泡性極高,而且欠缺消泡性,故而於操作性方面存在問題。另外,日本專利特開2001-276759號公報中所提出的洗淨劑是溶解有氟化氫
(hydrogen fluoride)及臭氧(ozone)的洗淨液,雖然可期待將牢固地附著在基板表面上的微粒藉由蝕刻來除去的效果,但由於此洗淨劑含有氟離子,故而存在排水處理會消耗巨大成本的問題,並且由於無法控制強蝕刻性,故而存在於洗淨時有損基板的平坦性的問題。另外,日本專利特開2002-212597號公報中所提出的洗淨劑藉由使用陰離子性界面活性劑,可使防止微粒再次附著的效果獲得某種程度的改善,但由於此洗淨劑幾乎不具有蝕刻性,故而存在微粒除去性不充分,洗淨性不充分的問題。
本發明的目的在於提供一種電子材料用洗淨劑及洗淨方法,此電子材料用洗淨劑無損玻璃或矽基板表面的平坦性,可實現優異的微粒除去性,且低起泡性及經時穩定性優異。
本發明者等為解決上述課題而進行潛心研究,結果完成了本發明。即,本發明是有關於一種電子材料用洗淨劑及使用此洗淨劑的電子材料的洗淨方法,此電子材料用洗淨劑中的陰離子成分含有通式(1)所表示的陰離子性界面活性劑(A)、以及選自由碳數為6~18的烯烴及通式(2)所表示的有機溶劑所組成族群中的一種或一種以上的有機溶劑(B),且上述有機溶劑(B)的SP值(solubility parameter,溶解度參數)為6~13。
R1[-(OA1)a-Q-]b (1)
[式(1)中,R1表示碳數為1~10的烴基,A1表示碳
數為2~4的亞烷基,Q-表示-COO-、-OCH2COO-、-SO3 -、-OSO3 -或-OPO2(OR2)-,R2表示氫或碳數為1~10的烴基,a為平均值且為0~20,b為1~6的整數,當Q-為-COO-或-SO3 -時,a為0。]
R3[-(OA2)c-OH]d (2)
[式(2)中,R3表示碳數為1~12的烴基,A2表示碳數為2~4的亞烷基,c為平均值且為0~20,d為1~6的整數。]
本發明的電子材料用洗淨劑,在製造平面顯示器用、光罩用、硬碟用及半導體用的玻璃或矽基板的步驟中,無損基板表面的平坦性,可賦予經適度控制的蝕刻性,藉此可使被牢固地附著在基板表面上的微小微粒自基板表面脫離,進而使脫離的微粒穩定地分散在洗淨劑中,而實現優異的微粒除去性,可實現低起泡性及經時穩定性優異,可提高製造時的良率或在短時間進行洗淨的高效的高度洗淨。
為讓本發明之上述特徵和優點能更明顯易懂,下文特舉實施例,並配合所附圖式作詳細說明如下。
本發明的陰離子性界面活性劑(A)是含有陰離子成分及陽離子成分而成,陰離子成分是以上述通式(1)表示。
通式(1)中,R1表示碳數為1~10的烴基,R1例如可列舉:碳數為1~10的直鏈脂肪族烴基、碳數為3~10
的支鏈脂肪族烴基、及碳數為6~10的芳香族烴基。
碳數為1~10的直鏈脂肪族烴基可列舉:甲基、乙基、正丙基、正丁基、正戊基、正己基、正庚基、正辛基、正壬基及正癸基,以及自碳數為2~10的烷二醇(alkylene glycol)、甘油(glycerin)及山梨糖醇(sorbitol)等中除去羥基所剩餘的殘基等。
碳數為3~10的支鏈脂肪族烴基可列舉:異丙基、異丁基或第三丁基、異戊基或新戊基、異己基、異庚基、異辛基、異壬基或第二壬基、異癸基或第二癸基、1-乙基辛基及通式(3)所表示的烴基。
[式(3)中,R4及R5分別獨立表示碳數為1~6的烷基,且R4與R5的碳數合計為3~8,e為0~2的整數,當R4與R5的碳數合計為8時,e為0或1。]
通式(3)的R4及R5的具體例,例如可列舉:甲基、乙基、正丙基或異丙基、異丁基或正丁基、第二丁基或異丁基或第三丁基、正戊基、1-甲基丁基、2-甲基丁基、3-甲基丁基、1,1-二甲基丙基、1,2-二甲基丙基、2,2-二甲基丙基、正己基、1-甲基戊基、2-甲基戊基、3-甲基戊基、4-甲基戊基、1,1-二甲基丁基、1,2-二甲基丁基、1,3-二甲基丁基、2,2-二甲基丁基、2,3-二甲基丁基、3,3-二甲基丁
基、1,1-二甲基-2-甲基丙基、1-乙基丁基、2-乙基丁基、1-乙基-1-甲基丙基及1-乙基-2-甲基丙基。
碳數為6~10的芳香族烴基,可列舉通式(4)所表示的烴基。
[式中,f個R6分別獨立表示氫原子或碳數為1~4的烷基,且f個R6的碳數合計小於等於4,f為1~4的整數。]
通式(4)的R6,可列舉上述通式(3)的R4及R5所例示的烷基中的碳數為1~4的烷基。
就微粒除去性及低起泡性的觀點而言,這些R1中較好的是碳數為4~10的烴基,更好的是通式(3)或(4)所表示的烴基。
通式(1)中,A1表示碳數為2~4的亞烷基,A1可列舉:亞乙基,1,2-亞丙基或1,3-亞丙基,及1,2-亞丁基、1,3-亞丁基、2,3-亞丁基或1,4-亞丁基。就經時穩定性及低起泡性的觀點而言,這些A1中較好的是亞乙基、1,2-亞丙基,A1可單獨使用一種亞烷基,或併用兩種或兩種以上的亞烷基。
如下所述,(A1O)是藉由環氧烷(alkylene oxide)(以下,簡稱為AO)的亞烷基為A1者的加成反應而形成的,
故而這些環氧烷加成物的加成莫耳數具有分佈。因此,a是以平均值表示,通常為0~20,就經時穩定性的觀點而言,較好的是0~10,更好的是0~5,特別好的是0。
此外,當形成(A1O)時併用兩種或兩種以上的AO的情況下,可為嵌段加成(封端型(capped-type)、平衡型及活性次級型等),亦可為無規加成,亦可為兩者的混合體系[無規加成後,再進行封端的混合體系:分子中具有0~50%(較好的是5~40%)任意分佈的氧乙烯鏈,且0~30%(較好的是5~25%)的氧乙烯鏈在分子末端被封端的混合體系]。
上述及下述說明中,只要無特別規定,則%表示重量百分比。
通式(1)中,Q-表示-COO-、-OCH2COO-、-SO3 -、-OSO3 -或-OPO2(OR2)-,就洗淨劑沖洗性的觀點而言,較好的是-OSO3 -及-OPO2(OR2)-。
此外,當Q-為-COO-或-SO3 -時,上述a為0。
R2表示氫原子或碳數為1~10的烴基,碳數為1~10的烴基,可列舉與通式(1)的R1所例示的烴基相同的烴基,就微粒的分散穩定性的觀點而言,較好的是碳數為4~10的烴基,更好的是通式(3)或(4)所表示的烴基。
通式(1)中,b為1~6的整數,就洗淨後的表面平坦性的觀點而言,較好的是1~3,更好的是1。
構成陰離子性界面活性劑(A)的陰離子成分的具體例可列舉:自甲醇,乙醇,1-丙醇或2-丙醇,1-丁醇、2-
丁醇或第三丁醇,1-戊醇、2-戊醇或3-戊醇,2-甲基-1-丁醇,3-甲基-2-丁醇,1-己醇、2-己醇或3-己醇,2-甲基-1-戊醇,3-甲基-1-戊醇,4-甲基-2-戊醇,3,3-二甲基-2-丁醇,3-甲基-2-戊醇,1-庚醇、2-庚醇、3-庚醇或4-庚醇,2,4-二甲基-3-戊醇,3-甲基-1-己醇,5-甲基-2-己醇,1-辛醇、2-辛醇、3-辛醇或4-辛醇,6-甲基-2-庚醇,2,2-二甲基-3-己醇,2,5-二甲基-3-己醇,2-乙基-1-己醇,5-甲基-2-庚醇,5-甲基-3-庚醇,6-甲基-3-庚醇,2,2-二甲基-3-庚醇,1-壬醇、2-壬醇、3-壬醇、4-壬醇或5-壬醇,2-甲基-3-辛醇,1-癸醇、2-癸醇、3-癸醇、4-癸醇或5-癸醇,3,7-二甲基-1-辛醇,乙二醇,1,6-己二醇,1,10-癸二醇,甘油及山梨糖醇等醇以及這些醇的碳數為2~4的AO(環氧乙烷,1,2-環氧丙烷或1,3-環氧丙烷,及1,2-環氧丁烷、1,3-環氧丁烷、2,3-環氧丁烷或1,4-環氧丁烷等)加成物(加成莫耳數為1~20)的硫酸酯或磷酸酯中除去質子而成的陰離子;自丙酸,2-甲基丙酸,2,2-二甲基丙酸,丁酸,2-甲基丁酸或3-甲基丁酸,2-乙基丁酸,2,3-二甲基丁酸或3,3-二甲基丁酸,2-乙基-3-甲基丁酸、戊酸,2-甲基戊酸、3-甲基戊酸或4-甲基戊酸,2-乙基戊酸或3-乙基戊酸,2-正丙基戊酸或異丙基戊酸,2,4-二甲基戊酸,2,4,4-三甲基戊酸或3,4,4-三甲基戊酸,己酸,2-甲基己酸、3-甲基己酸、4-甲基己酸或5-甲基己酸,2-乙基己酸、3-乙基己酸或4-乙基己酸,2-正丙基己酸或3-正丙基己酸,2-異丙基己酸或3-異丙基己酸,2,5-二甲基己酸或3,5-二甲基己酸,2,5,5-三
甲基己酸或3,5,5-三甲基己酸,庚酸,2-甲基庚酸、3-甲基庚酸、4-甲基庚酸、5-甲基庚酸或6-甲基庚酸,2-乙基庚酸、3-乙基庚酸、4-乙基庚酸或5-乙基庚酸,2-正丙基庚酸、3-正丙基庚酸或4-正丙基庚酸,2-異丙基庚酸、3-異丙基庚酸或4-異丙基庚酸,2,6-二甲基庚酸或3,6-二甲基庚酸,2,6,6-三甲基庚酸、2,4,6-三甲基庚酸或3,6,6-三甲基庚酸,辛酸,2-甲基辛酸、3-甲基辛酸、4-甲基辛酸、5-甲基辛酸、6-甲基辛酸或7-甲基辛酸,2-乙基辛酸、3-乙基辛酸、4-乙基辛酸、5-乙基辛酸或6-乙基辛酸,2,7-二甲基辛酸或3,7-二甲基辛酸,壬酸及2-甲基壬酸、3-甲基壬酸、4-甲基壬酸、5-甲基壬酸、6-甲基壬酸、7-甲基壬酸或8-甲基壬酸中除去質子而成的陰離子;自1-甲基丙磺酸(1-methylpropanesulfonic acid)、1-甲基戊磺酸(1-methylpentanesulfonic acid)及1-乙基丁磺酸(1-ethylbutanesulfonic acid)中除去質子而成的陰離子;藉由上述醇或這些醇的碳數為2~4的AO加成物(加成莫耳數為1~20)與2-氯乙酸鹽(2-chloroacetate salt)(鉀鹽或鈉鹽)的反應而獲得的烷基醚羧酸鹽(alkyl ether carboxylate salt)的陰離子;自苯磺酸、甲苯磺酸、二甲苯磺酸、異丙苯磺酸(cumenesulfonic acid)及苯甲酸中除去質子而成的陰離子等。
就微粒除去性及低起泡性的觀點而言,這些構成陰離子性界面活性劑(A)的陰離子成分中,較好的是自1-丁醇、2-乙基-1-己醇、3-甲基-1-己醇、3,7-二甲基-1-辛醇及
這些醇的碳數為2~4的AO(環氧乙烷、1,2-或1,3-環氧丙烷及1,2-、1,3-、2,3-或1,4-環氧丁烷等)加成物(加成莫耳數為1~20)的硫酸酯或磷酸酯中除去質子而成的陰離子,以及自2-乙基戊酸、2-正丙基戊酸、2-異丙基戊酸、2,4,4-三甲基戊酸或3,4,4-三甲基戊酸、2-甲基己酸、2-乙基己酸、2-正丙基己酸、2-異丙基己酸、2-甲基庚酸、2-乙基庚酸、2-甲基辛酸、苯磺酸、甲苯磺酸及二甲苯磺酸中除去質子而成的陰離子;更好的是自2-乙基-1-己醇、3-甲基-1-己醇及3,7-二甲基-1-辛醇的硫酸酯或磷酸酯中除去質子而成的陰離子,以及自2-正丙基戊酸、2-異丙基戊酸、2,4,4-三甲基戊酸或3,4,4-三甲基戊酸、2-乙基己酸、2-甲基庚酸、對甲苯磺酸(paratoluenesulfonic acid)、鄰甲苯磺酸(orthotoluenesulfonic acid)、間二甲苯磺酸(metaxylenesulfonic acid)及對二甲苯磺酸(paraxylenesulfonic acid)中除去質子而成的陰離子;特別好的是自2-乙基-1-己醇的硫酸酯或磷酸酯中除去質子而成的陰離子,以及自辛酸、對甲苯磺酸及間二甲苯磺酸中除去質子而成的陰離子;最好的是自2-乙基-1-己醇的硫酸酯、對甲苯磺酸及間二甲苯磺酸中除去質子而成的陰離子。
構成本發明的陰離子性界面活性劑(A)的陽離子成分可列舉:鹼金屬陽離子、鹼土金屬陽離子、碳數為0~25的銨陽離子、將羥胺(hydroxyamine)質子化而成的陽離子、將碳數為1~36的脂肪族胺質子化而成的陽離子、
將碳數為4~10的脒(amidine)化合物質子化而成的陽離子、將碳數為1~23的烷醇胺(alkanolamine)質子化而成的陽離子及將碳數為6~20的芳香族或芳香脂肪族胺質子化而成的陽離子。這些陽離子成分可單獨使用,亦可併用兩種或兩種以上。
鹼金屬陽離子可列舉鈉陽離子及鉀陽離子等。
鹼土金屬陽離子可列舉鈣陽離子及鎂陽離子等。
碳數為0~25的銨陽離子可列舉:銨、四甲基銨、三甲基乙烯基銨、三甲基苯基銨、苄基三乙基銨、十二烷基三甲基銨、四丁基銨、三甲基十四烷基銨、苄基三丁基銨、四戊基銨、乙基十六烷基二甲基銨及十八烷基三甲基銨等。
將碳數為1~36的脂肪族胺質子化而成的陽離子中的碳數為1~36的脂肪族胺,可列舉:碳數為1~12的烷基胺、碳數為2~6的烷二胺(alkylenediamine)、碳數為3~7的環狀胺、多(n=2~6)亞烷基(碳數為2~6)多(n=3~7)胺及這些脂肪族胺的碳數為2~4的AO(環氧乙烷,1,2-環氧丙烷或1,3-環氧丙烷,及1,2-環氧丁烷、1,3-環氧丁烷、2,3-環氧丁烷或1,4-環氧丁烷等)加成物等。
碳數為1~12的烷基胺可列舉:碳數為1~6的單烷基胺(monoalkylamine)(甲胺、乙胺、丙胺、異丙胺、丁胺及己胺等)及碳數為2~12的二烷基胺(dialkylamine)(二甲基胺、乙基甲基胺、丙基甲基胺、丁基甲基胺、二乙基胺、丙基乙基胺、二異丙基胺及二己基胺等)等。
碳數為2~6的烷二胺可列舉:乙二胺
(ethylenediamine)、1,2-丙二胺(1,2-propylenediamine)或1,3-丙二胺(1,3-propylenediamine)、1,4-丁二胺(tetramethylenediamine)、1,5-戊二胺(pentamethylenediamine)及1,6-己二胺(hexamethylenediamine)等。
碳數為3~7的環狀胺可列舉:環丙胺、環己胺、哌啶(piperidine)、哌嗪(piperazine)、奎寧(quinuclidine)、2-吡啶胺(pyridineamine)、順式-3-甲基環己胺及1,4-二氮雜雙環[2.2.2]辛烷(DABCO,1,4-diazabicyclo[2.2.2]octane)等。
多(n=2~6)亞烷基(碳數為2~6)多(n=3~7)胺可列舉:二乙三胺、二丙三胺、二己三胺、三乙四胺、四乙五胺、五乙六胺及六乙七胺等。
將碳數為4~10的脒化合物質子化而成的陽離子中的碳數為4~10的脒化合物,可列舉:1,8-二氮雜雙環[5.4.0]-7-十一烯(以下,簡稱為DBU)、1,5-二氮雜雙環[4.3.0]-5-壬烯(以下,簡稱為DBN)、2-甲基咪唑(2-methylimidazole)、2-丁基苯并咪唑(2-butylbenzimidazole)及2-(4-噻唑基)苯并咪唑(2-(4-thiazolyl)benzimidazole)等。
將碳數為1~23的烷醇胺質子化而成的陽離子中的碳數為1~23的烷醇胺,可列舉:單乙醇胺、二乙醇胺、三乙醇胺、N-甲基二乙醇胺、N,N-二甲基乙醇胺、N,N-二乙基乙醇胺、2-胺基-2-甲基-1-丙醇、N-(胺基乙基)乙醇胺、
2-(2-胺基乙氧基)乙醇及這些烷醇胺的碳數為2~4的AO(環氧乙烷,1,2-環氧丙烷或1,3-環氧丙烷,及1,2-環氧丁烷、1,3-環氧丁烷、2,3-環氧丁烷或1,4-環氧丁烷等)加成物等。
碳數為6~20的芳香族或芳香脂肪族胺質子化而成的陽離子中的碳數為6~20的芳香族或芳香脂肪族胺,可列舉:苯胺、苯二胺(phenylenediamine)、甲苯二胺、亞甲基二苯胺(methylene dianiline)、二苯醚二胺(diphenylether diamine)、萘二胺(naphthalenediamine)、蒽二胺(anthracenediamine)、苄基胺(benzylamine)、苯二甲胺(xylylene diamine)及這些的碳數為2~4的AO(環氧乙烷,1,2-環氧丙烷或1,3-環氧丙烷,及1,2-環氧丁烷、1,3-環氧丁烷、2,3-環氧丁烷或1,4-環氧丁烷等)加成物等。
就微粒除去性的觀點而言,這些陽離子成分中,較好的是鹼金屬陽離子、將碳數為1~15的脂肪族胺質子化而成的一價陽離子、將碳數為4~10的脒化合物質子化而成的陽離子及將碳數為1~15的烷醇胺質子化而成的一價陽離子;更好的是鈉陽離子、鉀陽離子,以及將三甲基胺、DBU、DBN及二乙醇胺質子化而成的陽離子;特別好的是鈉陽離子、鉀陽離子、將DBU質子化而成的陽離子及將二乙醇胺質子化而成的陽離子。
通式(1)中,當Q-為-COO-、-SO3 -、-OSO3 -或-OPO2(OR2)-時,陰離子性界面活性劑(A),例如可藉由含有陰離子成分及質子的酸,與包含上述鹼金屬陽離子、鹼
土金屬陽離子、碳數為0~25的銨陽離子及羥基陰離子的鹼性化合物,或者上述碳數為1~15的胺或碳數為2~36的多元(2~7元)胺產生中和反應而獲得。中和反應的溫度通常為10~60℃,時間通常為30~200分鐘。中和度通常為95~100%,中和物的pH值(中和物的5%水溶液)通常為7~12。
通式(1)中,當Q-為-OSO3 -或-OPO2(OR2)-時,包含陰離子成分及質子的酸,例如可藉由以下(1)及(2)的反應來製造。
(1)AO的加成反應
藉由通常方法,在通式(1)的R1上取代有羥基的化合物的羥基上加成碳數為2~4的AO。具體而言,將上述含羥基化合物裝入加壓反應容器內,在無觸媒或觸媒的存在下(特別是,加成AO的後半段)吹入AO,於常壓或加壓條件下以一個階段或多個階段來進行反應。觸媒可列舉鹼觸媒,例如:鹼金屬(鋰、鈉、鉀及銫等)的氫氧化物;酸[過鹵酸(過氯酸、過溴酸及過碘酸)、硫酸、磷酸及硝酸等(較好的是過氯酸)]以及這些酸的鹽[較好的是2價或3價金屬(Mg、Ca、Sr、Ba、Zn、Co、Ni、Cu及Al等)的鹽]。
反應溫度通常為50~150℃,反應時間通常為2~20小時。
AO加成反應結束後,可視需要中和觸媒並利用吸附劑進行處理,而除去觸媒並進行精製。
(2)硫酸酯化反應或磷酸酯化反應
藉由將通式(1)的R1上取代有羥基的化合物或上述(1)中所獲得的AO加成物的末端羥基硫酸酯化或磷酸酯化,可獲得硫酸酯化物或磷酸酯化物。
酯化方法例如可列舉:(i)使用氯磺酸的方法、(ii)使用硫酸酐(sulfan)的方法、(iii)使用磺胺酸(sulfamic acid)的方法、(iv)使用硫酸的方法、以及(v)使用磷酸的方法等。(ii)的硫酸酐是利用乾燥氮氣等來加以稀釋後再進行使用。
當利用(i)及(ii)的方法時,反應溫度通常為-10~70℃,較好的是-5~40℃。當利用(iii)、(iv)及(v)的方法時,反應溫度通常為50~150℃,較好的是60~130℃。
酯化反應的結束點是56100/(酯化物的分子量)所表示的酸值(AV)達到理論值(theoretical value)的70~110%之時,較好的是達到理論值的80~105%之時。
通式(1)中,當Q-為-SO3 -時,包含陰離子成分及質子的酸,例如可藉由如下方法來製造:使鹵代烷或烷基硫酸鹽與亞硫酸鹼金屬鹽反應的方法;使用發煙硫酸,將烴直接磺化的方法;以及在紫外線照射下,使二氧化硫及氯與烴反應的方法等。
通式(1)中,當Q-為-COO-時,包含陰離子成分及質子的酸,例如可藉由利用高壓分解法(8~50個大氣壓)或崔其耳(Twitchell)分解法(添加崔其耳分解劑及少量
硫酸,而將脂肪酸瀝青(fatty acid pitch)除去)水解天然油脂來製造。
通式(1)中,當Q-為-OCH2COO-時,陰離子性界面活性劑(A)例如可藉由在鹼(氫氧化鈉及氫氧化鉀等)的存在下,將通式(1)的R1上取代有羥基的化合物或上述(1)中所獲得的AO加成物與單氯乙酸鹽(鈉鹽及鉀鹽等)羧甲基化來製造。
本發明的有機溶劑(B)可列舉:碳數為6~18的烯烴、通式(2)所表示的有機溶劑及這些的混合物。
碳數為6~18的烯烴,可列舉碳數為6~18的直鏈烯基或支鏈烯烴,具體而言可列舉:1-己烯、2-庚烯、3-辛烯、4-壬烯、5-癸烯、1-十一烯、1-十二烯、1-十三烯、1-十四烯、1-十五烯、1-十六烯、1-十七烯、1-十八烯、丁烯二聚物、丁烯三聚物、丁烯四聚物、異丁烯三聚物、丙烯二聚物、丙烯三聚物、丙烯四聚物及丙烯五聚物等。
通式(2)中,R3表示碳數為1~12的烴基,就有機物污漬除去性能的觀點而言,較好的是氫或碳數為1~8的烴基。
碳數為1~12的烴基可列舉:上述通式(1)的R1中所例示的碳數為1~10的烴基,正十一烷基、第二-十一烷基或異十一烷基,及正十二烷基、第二-十二烷基或異十二烷基等。
通式(2)中,A2表示碳數為2~4的亞烷基(亞乙基,1,2-亞丙基或1,3-亞丙基,及1,2-亞丁基、1,3-亞丁基、2,3-
亞丁基或1,4-亞丁基等),就經時穩定性及低起泡性的觀點而言,較好的是亞乙基及1,2-亞丙基,A2可單獨使用一種亞烷基,或併用兩種或兩種以上的亞烷基。
(A2O)是以與通式(1)的(A1O)相同的方式形成,故而A2O的加成莫耳數具有分佈。因此,c以平均值表示,通常為0~20,就經時穩定性的觀點而言,較好的是0~10。
通式(2)中,d為1~6的整數,就洗淨後的沖洗性的觀點而言,較好的是1~3,更好的是1。
通式(2)所表示的有機溶劑的具體例可列舉:異丙醇、正戊醇、2-乙基己醇、甲基溶纖劑(methyl cellosolve)、丁基溶纖劑(butyl cellosolve)、甲基卡必醇(methyl carbitol)、乙基卡必醇、丁基卡必醇、己基卡必醇、三乙二醇單甲醚、四乙二醇單甲醚、三乙二醇二甲醚、三乙二醇單乙醚、四乙二醇單乙醚、甲醇環氧乙烷(methyl alcohol ethylene oxide)(10莫耳)加成物、異丙醇環氧乙烷(5莫耳)加成物、烯丙醇環氧乙烷(5莫耳)環氧丙烷(15莫耳)嵌段加成物、甘油環氧乙烷(15莫耳)環氧丙烷(2莫耳)無規加成物及山梨糖醇環氧乙烷(2莫耳)加成物等。
就微粒除去性的觀點而言,有機溶劑(B)中,較好的是1-十二烯、1-十三烯、1-十四烯、1-十五烯、異丁烯三聚物、丙烯四聚物、丙烯五聚物、2-乙基己醇、丁基卡必醇、己基卡必醇及三乙二醇單甲醚,更好的是1-十二烯、異丁烯三聚物、丙烯四聚物、丙烯五聚物、丁基卡必醇、
己基卡必醇及三乙二醇單甲醚。
有機溶劑(B)可單獨使用碳數為6~18的烯烴及通式(2)所表示的有機溶劑中的一種,亦可併用兩種或兩種以上。
有機溶劑(B)的SP值通常為6~13,較好的是7~12,更好的是8~11。若SP值小於6或大於13,則有機污漬除去性會變差。
另外,SP值是藉由「Polymer Engineering and Science,Vol.14,No.2,p147~154(1974)」中所記載的Fedors法進行計算而獲得的值。
本發明的電子材料用洗淨劑藉由含有以下鹼成分(C),而進一步提高蝕刻性及沖洗性。
鹼成分(C)可列舉:氨水、羥基胺、氫氧化四級銨(C-1)、碳數為1~36的脂肪族胺(C-2)、無機鹼(C-3)、碳數為1~23的烷醇胺(C-4)、碳數為4~10的脒化合物(C-5)及這些的混合物。
(C-1)可列舉:四甲基氫氧化銨、乙基三甲基氫氧化銨、四乙基氫氧化銨、三乙基甲基氫氧化銨、四丙基氫氧化銨、四丁基氫氧化銨、四戊基氫氧化銨、四己基氫氧化銨、羥乙基三甲基氫氧化銨、三乙基羥乙基氫氧化銨、二(羥乙基)二甲基氫氧化銨及三(羥乙基)甲基氫氧化銨等。
(C-2)可列舉:與構成上述陰離子性界面活性劑(A)的陽離子成分的記載中所例示的碳數為1~36的脂肪族胺相同的脂肪族胺。
(C-3)可列舉:氫氧化鋰、氫氧化鈉、氫氧化鉀、氫氧化鈣及氫氧化鎂等。
(C-4)可列舉:與構成上述陰離子性界面活性劑(A)的陽離子成分的記載中所例示的碳數為1~23的烷醇胺相同的烷醇胺。
(C-5)可列舉:與構成上述陰離子性界面活性劑(A)的陽離子成分的記載中所例示的碳數為4~10的脒化合物相同的脒化合物。
就蝕刻性及洗淨後相對於水的接觸角(沖洗性)的觀點而言,鹼成分(C)中,較好的是(C-2)、(C-3)、(C-4)、(C-5)及這些的混合物,更好的是氫氧化鉀、氫氧化鈉、DBU、丁胺、己胺、環己胺、三乙醇胺、N-甲基二乙醇胺、環己胺環氧乙烷(2莫耳)加成物、環己胺環氧丙烷(2莫耳)加成物、N,N-二甲基乙醇胺、三乙醇胺環氧乙烷(5莫耳)加成物、三乙醇胺環氧丙烷(5莫耳)加成物、N,N-二甲基乙醇胺環氧乙烷(3莫耳)加成物、N,N-二甲基乙醇胺環氧乙烷(3莫耳)加成物及這些的混合物。
本發明的電子材料用洗淨劑,可更含有選自由以下高分子型分散劑(D)及螯合劑(E)所組成族群中的一種或一種以上。
本發明的電子材料用洗淨劑藉由含有高分子型分散劑(D),而進一步提高微粒分散性及防止再污染性。
高分子型分散劑(D)可列舉:重量平均分子量(以下,簡稱為Mw)為2,500~800,000的具有磺酸(鹽)基
的高分子型陰離子性界面活性劑(D-1)、具有硫酸酯(鹽)基的高分子型陰離子性界面活性劑(D-2)、具有磷酸酯(鹽)基的高分子型陰離子性界面活性劑(D-3)、具有膦酸(鹽)基的高分子型陰離子性界面活性劑(D-4)、具有羧酸(鹽)基的高分子型陰離子性界面活性劑(D-5)、以及多糖類及其衍生物(D-6)等。
高分子分散劑(D)的具體例可列舉如下的例子。
具有磺酸(鹽)基的高分子型陰離子性界面活性劑(D-1):聚苯乙烯磺酸(polystyrene sulphonic acid)、苯乙烯/苯乙烯磺酸共聚物、聚[2-(甲基)丙烯醯胺基-2,2-二甲基乙磺酸]、2-(甲基)丙烯醯胺基-2,2-二甲基乙磺酸/苯乙烯共聚物、2-(甲基)丙烯醯胺基-2,2-二甲基乙磺酸/丙烯醯胺共聚物、2-(甲基)丙烯醯胺基-2,2-二甲基乙磺酸/(甲基)丙烯酸共聚物、2-(甲基)丙烯醯胺基-2,2-二甲基乙磺酸/(甲基)丙烯酸/丙烯醯胺共聚物、2-(甲基)丙烯醯胺基-2,2-二甲基乙磺酸/苯乙烯/丙烯醯胺共聚物、2-(甲基)丙烯醯胺基-2,2-二甲基乙磺酸/苯乙烯/(甲基)丙烯酸共聚物、萘磺酸-甲醛(naphthalenesulfonic acid-formaldehyde)縮合物、甲基萘磺酸-甲醛縮合物、二甲基萘磺酸-甲醛縮合物、蒽磺酸-甲醛縮合物、三聚氰胺磺酸-甲醛縮合物及胺基苯磺酸-苯酚-甲醛縮合物等,以及這些的鹽;具有硫酸酯(鹽)基的高分子型陰離子性界面活性劑(D-2):
聚[(甲基)丙烯酸-2-羥基乙酯硫酸酯]、丙烯酸-2-羥基乙酯/丙烯酸-2-羥基乙酯硫酸酯共聚物、甲基丙烯酸-2-羥基乙酯/甲基丙烯酸-2-羥基乙酯硫酸酯共聚物、聚[(甲基)丙烯酸-2-羥基乙酯]的硫酸酯化物、聚[(甲基)丙烯醯氧基聚環氧烷硫酸酯]、(甲基)丙烯醯氧基聚環氧烷硫酸酯/丙烯酸共聚物及纖維素、甲基纖維素或乙基纖維素的硫酸酯化物等,以及這些的鹽類;具有磷酸酯(鹽)基的高分子型陰離子性界面活性劑(D-3):聚[(甲基)丙烯酸-2-羥基乙酯磷酸酯]、丙烯酸-2-羥基乙酯/丙烯酸-2-羥基乙酯磷酸酯共聚物、甲基丙烯酸-2-羥基乙酯/甲基丙烯酸-2-羥基乙酯磷酸酯共聚物、聚[(甲基)丙烯酸-2-羥基乙酯]的磷酸酯化物、聚[(甲基)丙烯醯氧基聚環氧烷磷酸酯]、(甲基)丙烯醯氧基聚環氧烷磷酸酯/丙烯酸共聚物及纖維素、甲基纖維素或乙基纖維素的磷酸酯化物等,以及這些的鹽類;具有膦酸(鹽)基的高分子型陰離子性界面活性劑(D-4):聚[(甲基)丙烯醯氧基乙基膦酸]、丙烯酸-2-羥基乙酯/丙烯醯氧基乙基膦酸共聚物及甲基丙烯酸-2-羥基乙酯/甲基丙烯醯氧基乙基膦酸共聚物、萘膦酸-甲醛縮合物、甲基萘膦酸-甲醛縮合物、二甲基萘膦酸-甲醛縮合物、蒽膦酸-甲醛縮合物及苯胺膦酸-苯酚-甲醛縮合物等,以及這些的鹽;
具有羧酸(鹽)基的高分子型陰離子性界面活性劑(D-5):聚(甲基)丙烯酸、(甲基)丙烯酸-順丁烯二酸共聚物、(甲基)丙烯酸-衣康酸共聚物、(甲基)丙烯酸-反丁烯二酸共聚物、(甲基)丙烯酸/乙酸乙烯酯共聚物、甲基丙烯酸-2-羥基乙酯/(甲基)丙烯酸共聚物、聚[(甲基)丙烯酸-2-羥基乙酯]的羧甲基化物、羧甲基纖維素、羧甲基甲基纖維素、羧甲基乙基纖維素、苯甲酸-甲醛縮合物及苯甲酸-苯酚-甲醛縮合物等,以及這些的鹽類;多糖類及其衍生物(D-6):可列舉羥乙基纖維素、陽離子化纖維素、羥甲基纖維素、羥丙基纖維素、瓜爾膠(guar gum)、陽離子化瓜爾膠、三仙膠(xanthan gum)、海藻酸鹽(alginate)、陽離子化澱粉等,聚乙烯醇(poval)以及磷酸酯[植酸(phytic acid)、二(聚氧乙烯)烷基醚磷酸及三(聚氧乙烯)烷基醚磷酸等]等。
高分子分散劑(D)形成鹽時的反離子(counter ion)並無特別限定,例如可列舉:鹼金屬鹽(鈉鹽及鉀鹽等)、銨鹽、1級胺鹽(甲胺、乙胺及丁胺等烷基胺,單乙醇胺,以及胍等)、2級胺鹽(二甲基胺、二乙基胺及二丁基胺等二烷基胺,以及二乙醇胺等)、3級胺鹽(三甲基胺、三乙基胺及三丁基胺等三烷基胺,三乙醇胺,DBU,DBN,以及DABCO等)以及四級銨鹽(四烷基銨鹽等)。
就微粒分散性的觀點而言,高分子型分散劑(D)中,
較好的是(D-1)及(D-5),更好的是聚苯乙烯磺酸、苯乙烯/苯乙烯磺酸共聚物、聚(甲基)丙烯酸及(甲基)丙烯酸-順丁烯二酸共聚物以及這些的鹽,特別好的是聚(甲基)丙烯酸及(甲基)丙烯酸-順丁烯二酸共聚物以及這些的鹽。
就防止微粒再次附著及低起泡性的觀點等而言,高分子型分散劑(D)的Mw較好的是3,000~400,000,更好的是4,000~80,000,特別好的是5,000~40,000。
本發明的Mw是藉由凝膠滲透層析法(gel filtration chromatography),以聚環氧乙烷為標準物質,在40℃下進行測定[例如,裝置本體:HLC-8120(東曹(TOSOH)股份有限公司製造);管柱:東曹股份有限公司製造的TSKgel α6000、G3000 PWXL;檢測器:內置於裝置本體中的示差折射儀(differential refractometer)檢測器;溶離液:0.5%的乙酸鈉-水/甲醇(體積比為70/30);溶離液流量:1.0 ml/min;管柱溫度:40℃;試樣:0.25%的溶離液溶液;注入量:200 μl;標準物質:東曹股份有限公司公司製造的TSK TANDARD POLYETHYLENE OXIDE;資料處理軟體:GPC-8020 model Ⅱ(東曹股份有限公司製造)。
本發明的電子材料用洗淨劑藉由含有螯合劑(E),而進一步容易地控制基板的蝕刻性,亦進一步提高微粒分散穩定性。
螯合劑(E)可列舉:胺基多羧酸(鹽)(E-1)[例如,乙二胺四乙酸(鹽)(EDTA)、二乙三胺五乙酸(鹽)(DTPA)、三乙四胺六乙酸(鹽)(TTHA)、羥乙基乙二
胺三乙酸(鹽)(HEDTA)、二(羥乙基)乙二胺四乙酸(鹽)(DHEDDA)、氮川乙酸(Nitriloacetic acid)(鹽)(NTA)、羥乙基亞胺基二乙酸(鹽)(HIDA)、β-丙胺酸二乙酸(鹽)、天冬醯胺酸二乙酸(鹽)、甲基甘胺酸二乙酸(鹽)、亞胺基二琥珀酸(鹽)、絲胺酸二乙酸(鹽)、羥基亞胺基二琥珀酸(鹽)、二羥乙基甘胺酸(鹽)、天冬醯胺酸(鹽)及麩胺酸(鹽)];羥基羧酸(鹽)(E-2)[例如,羥基乙酸(鹽)、酒石酸(鹽)、檸檬酸(鹽)及葡萄糖酸(鹽)];醚羧酸(鹽)(E-3)[例如,羧甲基酒石酸(carboxy methyl tartronate)、羧甲基氧基琥珀酸、氧基二琥珀酸、酒石酸單琥珀酸及酒石酸二琥珀酸];其他羧酸(鹽)(E-4)[例如,順丁烯二酸衍生物及草酸(鹽)];膦酸(鹽)(E-5)[例如,甲烷二膦酸(methane diphosphonic acid)(鹽)、胺基三(亞甲基膦酸)](amino tri(methylene phosphonic acid))(鹽)、1-羥基亞乙基-1,1-二膦酸(鹽)、乙二胺四(亞甲基膦酸)(鹽)、己二胺四(亞甲基膦酸)(鹽)、丙二胺四(亞甲基膦酸)(鹽)、二乙三胺五(亞甲基膦酸)(鹽)、三乙四胺六(亞甲基膦酸)(鹽)、三胺基三乙基胺六(亞甲基膦酸)(鹽)、反式-1,2-環己二胺四(亞甲基膦酸)(鹽)、二醇醚二胺四(亞甲基膦酸)(鹽)及四乙五胺七(亞甲基膦酸)(鹽)];縮合磷酸(鹽)(E-6)[例如,偏磷酸(鹽)、三聚磷
酸(鹽)及六偏磷酸(鹽)]等。
此外,螯合劑(E)形成鹽時的反離子,可列舉上述高分子型分散劑(D)中所例示的反離子。另外,此等反離子可單獨使用,亦可併用兩種或兩種以上。
就基板的蝕刻性控制及洗淨性能的觀點而言,螯合劑(E)中,較好的是(E-1)、(E-2)、(E-4)、(E-5)及(E-6),更好的是(E-1)、(E-2)、(E-5)及(E-6),特別好的是乙二胺四乙酸(鹽)(EDTA)、二乙三胺五乙酸(鹽)(DTPA)、二羥乙基乙二胺四乙酸(鹽)(DHEDDA)、天冬醯胺酸二乙酸(鹽)、天冬醯胺酸(鹽)、麩胺酸(鹽)、檸檬酸(鹽)、胺基三(亞甲基膦酸)(鹽)、1-羥基亞乙基-1,1-二膦酸(鹽)、乙二胺四(亞甲基膦酸)(鹽)、偏磷酸(鹽)及六偏磷酸(鹽),特別好的是檸檬酸(鹽)、胺基三(亞甲基膦酸)(鹽)、1-羥基亞乙基-1,1-二膦酸(鹽)、乙二胺四(亞甲基膦酸)(鹽)及六偏磷酸(鹽)。
另外,本申請案發明的陰離子性界面活性劑(A)中的環羧酸(鹽)[例如,均苯四甲酸(鹽)、苯并多羧酸(鹽)及環戊烷四甲酸(鹽)],亦具有作為螯合劑的效果。
本發明的電子材料用洗淨劑,亦可於無損洗淨劑效果的範圍內,更含有其他添加劑(F)。其他添加劑(F)可列舉:還原劑、抗氧化劑、防銹劑、pH值調節劑、緩衝劑、消泡劑、防腐劑及水溶助劑(hydrotropic agent)等。
還原劑可列舉:碳數為6~70的還原酮(reductone)類[例如,L-抗壞血酸(ascorbic acid)(鹽)、異抗壞血酸
(鹽)、5,6-亞烷基-L-抗壞血酸{5,6-異亞丙基-L-抗壞血酸、5,6-(丁烷-2-亞基)-L-抗壞血酸及5,6-(戊烷-3-亞基)-L-抗壞血酸等}(鹽)、L-抗壞血酸-6-羧酸酯(L-抗壞血酸-6-乙酸酯及L-抗壞血酸-6-丙酸酯等)(鹽)、抗壞血酸硫酸酯(鹽)、抗壞血酸磷酸酯(鹽)、抗壞血酸葡萄糖苷(鹽)、抗壞血酸異棕櫚酸酯(鹽)、異抗壞血酸(鹽)、異抗壞血酸磷酸酯(鹽)、異抗壞血酸棕櫚酸酯(鹽)及異抗壞血酸四異棕櫚酸酯(鹽)];碳數為6~9的芳香族胺(對苯二胺及對胺基苯酚等);碳數為6~30的苯酚化合物[一元苯酚化合物{3-羥基黃酮(3-hydroxy flavone)及生育酚(tocopherol)(α-生育酚、β-生育酚、γ-生育酚、δ-生育酚、ε-生育酚或η-生育酚)等}及多酚(3,4,5-三羥基苯甲酸、鄰苯二酚(pyrocatechol)、間苯二酚(resorcinol)、對苯二酚(hydroquinone)、萘間二酚(Naphthalenediol)、鄰苯三酚(pyrogallol)及間苯三酚(phloroglucinol)等)等];磷系還原劑(三(2-羧基乙基)膦等);醛(甲醛、乙醛、丙醛及乙烯基醛等);硼烷系錯合物(硼烷-第三丁基胺錯合物、硼烷-N,N-二乙基苯胺錯合物及硼烷-三甲基胺錯合物等);硫醇系還原劑(L-半胱胺酸及胺基乙烷硫醇等);羥基胺系還原劑(羥基胺及二乙基羥基胺等);無機還原劑[亞硫酸(鹽)、二亞硫酸(鹽)、二亞硫磺酸(鹽)、硫代硫酸(鹽)、二硫磺酸(鹽)、多硫磺酸(鹽)、亞磷酸(鹽)、亞磷酸氫酸(鹽)、次亞磷酸(鹽)、硫酸亞鐵、氯化錫、氰基硼氫化鈉及硼氫化鈉等];等。
還原劑形成鹽時的反離子,可使用與上述高分子型分散劑(D)中所例示的反離子相同的反離子。還原劑可單獨使用,亦可併用兩種或兩種以上。另外,作為上述鹼成分(C)而例示的(C-2)、(C-4)及(C-5),亦具有作為還原劑的效果。
抗氧化劑可列舉:苯酚系抗氧化劑(2,6-二-叔丁基苯酚、2-叔丁基-4-甲氧基苯酚及2,4-二甲基-6-叔丁基苯酚等)、胺系抗氧化劑(單辛基二苯基胺、單壬基二苯基胺等單烷基二苯基胺;4,4'-二丁基二苯基胺、4,4'-二戊基二苯基胺等二烷基二苯基胺;四丁基二苯基胺、四己基二苯基胺等多烷基二苯基胺;α-萘胺及苯基-α-萘胺等萘胺等)、硫系化合物[啡噻嗪(phenothiazine)、季戊四醇-四-(3-十二烷基硫代丙酸酯)及雙(3,5-第三丁基-4-羥基苄基)硫醚等]及磷系抗氧化劑[雙(2,4-二-叔丁基苯基)季戊四醇二磷酸酯、亞磷酸苯基二異癸基酯、磷酸二苯基二異辛基酯及磷酸三苯基酯等]等。
防銹劑可列舉:苯并三唑(benzotriazole)、甲基苯并三唑(tolyltriazole)、含有碳數為2~10的烴基的苯并三唑、苯并咪唑、含有碳數為2~20的烴基的咪唑、含有碳數為2~20的烴基的噻唑及2-巰基苯并噻唑(2-mercaptobenzothiazole)等含氮有機防銹劑;十二烯基琥珀酸半酯、十八烯基琥珀酸酐及十二烯基琥珀醯胺等烷基或烯基琥珀酸;山梨糖醇酐單油酸酯、甘油單油酸酯及季戊四醇單油酸酯等多元醇部分酯等。這些防銹劑可單獨
使用,亦可併用兩種或兩種以上。
pH值調節劑可列舉:無機酸(鹽酸、硫酸、硝酸及磺胺酸等)、有機酸(檸檬酸、草酸及乳酸等)以及上述說明中所例示的鹼成分(C)等,這些pH值調節劑可單獨使用,亦可併用兩種或兩種以上。
緩衝劑可列舉:具有緩衝作用的碳數為1~10的有機酸(乙酸、甲酸、葡萄糖酸、羥乙酸、酒石酸、反丁烯二酸、乙醯丙酸(levulinic acid)、戊酸、順丁烯二酸及苦杏仁酸(Mandelic Acid)等)、無機酸(磷酸及硼酸等)以及這些酸的鹽。此外,緩衝劑形成鹽時的反離子,可列舉與上述高分子型分散劑(D)中所例示的反離子相同的反離子。這些緩衝劑可單獨使用,亦可併用兩種或兩種以上。
消泡劑可列舉:聚矽氧(silicone)消泡劑(以二甲基聚矽氧、氟化聚矽氧及聚醚聚矽氧等作為構成成分的消泡劑等)等。這些消泡劑可單獨使用,亦可併用兩種或兩種以上。
防腐劑可列舉:三嗪(triazine)衍生物[六氫-1,3,5-三(2-羥乙基)均三嗪等]、異噻唑啉(isothiazoline)衍生物(1,2-苯并異噻唑啉-3-酮、2-甲基-4-異噻唑啉-3-酮及5-氯-2-甲基-4-異噻唑啉-3-酮等)、吡啶衍生物[吡啶-吡啶硫醇-1-氧化物(鹽)等]、嗎啉(morpholine)衍生物[4-(2-硝基丁基)嗎啉及4,4-(2-乙基-2-硝基三亞甲基)-二嗎啉等]、苯并咪唑衍生物[2-(4-噻唑基)苯并咪唑等]、聚[氧乙烯(二甲基亞胺基)亞乙基(二甲基亞胺基)亞乙基]二氯化物、對氯
間二苯甲酚、苯氧基乙醇、苯氧基丙醇、乙醯氧基二甲基二氧陸圜、異丙基甲基苯酚、四氯間苯二甲腈(tetrachloro isophthalonitrile)、雙溴乙醯氧基乙烷、3-碘-2-丙炔基丁基胺基甲酸酯及2-溴-2-硝基丙烷-1,3-二醇等。這些防腐劑可單獨使用,亦可併用兩種或兩種以上。
水溶助劑可列舉:間苯二酚及水楊酸(鹽)等。此外,水溶助劑形成鹽時的反離子,可列舉與上述高分子型分散劑(D)中所例示的反離子相同的反離子。這些水溶助劑可單獨使用,亦可併用兩種或兩種以上。此外,作為陰離子性界面活性劑(A)列舉的甲苯磺酸(鹽)、二甲苯磺酸(鹽)、異丙苯磺酸(鹽)及苯甲酸(鹽),亦具有作為水溶助劑的效果。
如上所述,本發明的電子材料用洗淨劑含有陰離子性界面活性劑(A)、有機溶劑(B),及視需要的鹼成分(C)、高分子型分散劑(D)、螯合劑(E)及其他添加劑(F),亦可更含有水,特別是離子交換水(導電率小於等於0.2 μS/cm)或超純水(電阻率大於等於18 MΩ.cm)。
於本發明中,有效成分是指除了水以外的成分。
就蝕刻性及沖洗性的觀點而言,本發明的電子材料用洗淨劑用作洗淨液時,在有效成分濃度下並且在25℃下的pH值較好的是10~14,更好的是11~13。
另外,使用pH計(股份有限公司堀場製作所製造,M-12)來測定本發明的洗淨劑在溫度25℃下的pH值。
使用本發明的電子材料用洗淨劑來洗淨玻璃時,水對
於玻璃的接觸角小於等於20°,較好的是小於等於15°。
於本發明中,接觸角是使用接觸角儀對玻璃進行測定[裝置本體:PD-W(協和界面化學公司製造);玻璃板:玻璃板#1737(康寧(Corning)公司製造);檢測條件:自動檢測;測定條件:自滴在玻璃板上起10秒後,測定接觸角]。
就微粒除去性及低起泡性的觀點而言,基於電子材料用洗淨劑的有效成分的重量,陰離子性界面活性劑(A)的含量較好的是0.5~99%,更好的是1~95%,特別好的是2~90%,最好的是5~80%。
就微粒除去性的觀點而言,基於電子材料用洗淨劑的有效成分的重量,有機溶劑(B)的含量較好的是1~99.5%,更好的是2~95%,特別好的是5~90%,最好的是10~85%。
就蝕刻性及沖洗性的觀點而言,基於電子材料用洗淨劑的有效成分的重量,鹼成分(C)的含量較好的是0~55%,更好的是1~55%,特別好的是3~50%,最好的是5~45%。
就微粒分散性及防止再污染性的觀點而言,基於電子材料用洗淨劑的有效成分的重量,高分子型分散劑(D)的含量較好的是0~25%,更好的是0.1~20%,特別好的是0.5~15%,最好的是1~10%。
就基板的蝕刻性控制及分散穩定性的觀點而言,基於電子材料用洗淨劑的有效成分的重量,螯合劑(E)的含量較好的是0~10%,更好的是0.01~7%,特別好的是0.05
~5%,最好的是0.1~3%。
基於電子材料用洗淨劑的有效成分的重量,其他添加劑(F)即還原劑、抗氧化劑、防銹劑、緩衝劑及水溶助劑的各自含量,較好的是0~20%,更好的是0.1~15%,特別好的是0.5~10%,最好的是1~5%。另外,消泡劑的含量較好的是0~2%,更好的是0.01~1.5%,特別好的是0.02~1%,最好的是0.05~0.5%。
基於電子材料用洗淨劑的有效成分的重量,其他添加劑(F)的合計含量較好的是0~25%,更好的是0.5~20%,特別好的是1~15%,最好的是2~10%。
另外,當上述任意成分(C)~(F)間的組成相同而發生重複時,這些成分的合計含量並非是單純地將各個任意成分的含量加以合計,而是考慮到同時發揮各自作為其他任意成分的效果,根據使用目的來調整這些任意成分的含量。
本發明的電子材料用洗淨劑的有效成分濃度,通常為1~100%,就使用時的操作性或運輸效率的觀點而言,較好的是2~90%,更好的是5~70%,特別好的是10~50%。
本發明的電子材料用洗淨劑,例如可藉由如下方式製造:將陰離子性界面活性劑(A)、有機溶劑(B),及視需要的任意成分(C)~(F)及水,在10~40℃下混合溶解30~300分鐘。
用於混合溶解的裝置,並無特別限定,例如可使用安裝有槳型葉片的攪拌混合裝置,或安裝有螺旋型葉片的攪
拌混合裝置。
於將電子材料用洗淨劑用作洗淨液時,就操作性及成本的觀點而言,較好的是視需要使用水,特別是使用離子交換水(導電率小於等於0.2 μS/cm)或超純水(電阻率大於等於18 MΩ.cm)而使有效成分濃度達到0.1~15%,尤其好的是達到0.5~10%。
另外,當本發明的洗淨劑中使用上述碳數為6~18的烯烴時,就對有機物污漬的除去性的觀點而言,上述烯基較好的是以分散狀態存在於洗淨液中。
就對基板的濡濕擴散性的觀點而言,上述洗淨液對於玻璃的接觸角較好的是小於等於10°,更好的是小於等於8°,特別好的是小於等於5°,最好的是小於等於1°。
用水來稀釋電子材料用洗淨劑的方法,並無特別限定,例如可列舉如下方法:使用安裝有槳型葉片的攪拌混合裝置或安裝有螺旋型葉片的攪拌混合裝置等,將電子材料用洗淨劑與水,在10~40℃下混合溶解30~300分鐘。
本發明的電子材料的洗淨方法是使用上述電子材料用洗淨劑,利用選自由超音波洗淨、噴淋洗淨(shower cleaning)、噴霧洗淨(spray cleaning)、毛刷洗淨(brush cleaning)、浸漬洗淨、浸漬揺動及單片式洗淨所組成族群中的至少一種洗淨方法來進行洗淨的方法。
就洗淨性的觀點而言,洗淨溫度較好的是10~80℃,更好的是15~60℃,特別好的是20~50℃。
以本發明的洗淨方法加以洗淨後的玻璃表面的表面
粗糙度(Ra),較好的是小於等於1.0 nm,更好的是0.75 nm,特別好的是小於等於0.5 nm。若Ra小於等於1.0 nm,則在其後的步驟中,藉由濺鍍等來形成膜時可形成均勻的膜,故而可提高良率。
此外,Ra可使用SII Nano Technology公司製造的E-sweep,並在下述條件下進行測定。
測定模式:DFM(tapping mode,輕敲模式)
掃描區域:10 μm×10 μm
掃描線數:256條(在Y方向上掃描)
修正:有X、Y方向上的平坦修正
以下,藉由實施例更詳細地說明本發明,但本發明並非限定於此。只要無特別限定,則以下的份表示重量份。此外,以下使用的超純水的比電阻值大於等於18 MΩ.cm。
向附帶攪拌裝置及溫度控制裝置的玻璃製反應裝置內,添加2-乙基己醇256份,在攪拌下冷卻至0℃,一面將系統內溫度保持在0℃,一面以3小時滴加氯磺酸229份,而獲得硫酸酯。接著,緩慢添加48%的氫氧化鉀水溶液252份及離子交換水583份,在20℃下混合60分鐘將其中和,而獲得有效成分濃度為40%的陰離子性界面活性劑(A-1)1248份。
向附帶攪拌裝置及溫度控制裝置的玻璃製反應裝置
內,添加正丁醇148份,在攪拌下將溫度調整為70℃,一面將系統內溫度保持在70℃,一面以2小時滴加磷酸98份,接著在70℃下繼續攪拌4小時,而獲得磷酸酯。接著,將系統內冷卻至30℃,緩慢添加30%的氫氧化鈉水溶液133份及離子交換水201份,在20℃下混合60分鐘將其中和,而獲得有效成分濃度為40%的陰離子性界面活性劑(A-2)580份。
將2-乙基己醇換成3,7-二甲基-1-辛醇,將氯磺酸的份數換成189份,將48%的氫氧化鉀水溶液253份換成DBU271份,將離子交換水的份數換成912份,除此以外以與製造例1相同的方式獲得有效成分濃度為40%的陰離子性界面活性劑(A-3)1568份。
將2-乙基己酸144份及離子交換水395份添加至燒杯內,在20℃下攪拌15分鐘將其均勻混合後,緩慢添加N-甲基二乙醇胺119份,在20℃下混合60分鐘將其中和,而獲得有效成分濃度為40%的陰離子性界面活性劑(A-4)658份。
向附帶攪拌裝置及溫度控制裝置的不鏽鋼製高壓釜(autoclave)內,添加1-辛醇130份及28%的甲醇鈉甲醇(sodium methylate methanol)溶液8份,在攪拌下並且在室溫(20℃)下用氮氣置換系統內的氣相部,其後在減壓
條件下(錶壓:-0.0025 MPa),在120℃下以2小時進行脫甲醇後,接著在減壓條件下(錶壓:-0.05 MPa),在反應溫度120℃下,開始吹入環氧乙烷88份,一面控制錶壓達到0.1~0.3 MPa,一面進行反應直至系統內無壓力變化為止,而獲得1-辛醇的環氧乙烷2莫耳加成物218份。向附帶攪拌裝置及溫度控制裝置的玻璃製反應裝置內,添加上述1-辛醇的環氧乙烷2莫耳加成物164份、單氯乙酸鈉96份及甲苯200份,一面將溫度保持在50℃,一面緩慢提高減壓度直至達到-0.01 MPa後,一面進行減壓脫水,一面以2小時添加顆粒狀的氫氧化鈉38份,接著熟化6小時後,添加離子交換水300份,用鹽酸將其調節為酸性,藉由靜置、分液而脫鹽後,進行脫甲苯,而獲得結構式為C8H17O(CH2CH2O)2CH2COOH的醚羧酸。向附帶攪拌裝置及溫度控制裝置的玻璃製反應裝置內,添加水323份,緩慢添加顆粒狀的氫氧化鈉30份並將其溶解,在60℃下添加上述醚羧酸208份,而獲得有效成分濃度為40%的陰離子性界面活性劑(A-5)561份。
向附帶攪拌裝置及溫度控制裝置的不鏽鋼製高壓釜內,添加2-乙基己醇113份及氫氧化鉀3份,在攪拌下並且在室溫(20℃)下用氮氣置換系統內的氣相部,在減壓條件下(錶壓:-0.05 MPa)並且在反應溫度120℃下開始吹入環氧乙烷384份,一面控制錶壓達到0.1~0.3 MPa,一面進行反應直至系統內無壓力變化為止,而獲得2-乙基
己醇的環氧乙烷10莫耳加成物497份。
將2-乙基己醇256份換成上述2-乙基己醇的環氧乙烷10莫耳加成物497份,將氯磺酸的份數換成102份,將48%的氫氧化鉀水溶液的份數換成112份,將離子交換水的份數換成833份,除此之外以與製造例1相同的方式獲得有效成分濃度為40%的陰離子性界面活性劑(A-6)1512份。
向附帶攪拌裝置及溫度控制裝置的不鏽鋼製高壓釜內,添加環己胺297份,在攪拌下並且在室溫(20℃)下用氮氣置換系統內的氣相部,在減壓條件下(錶壓:-0.05 MPa)並且在反應溫度100℃下開始吹入環氧乙烷264份,一面控制錶壓達到0.1~0.3 MPa,一面進行反應直至系統內壓力無變化為止,而獲得環己胺環氧乙烷(2莫耳)加成物561份。
使用燒杯,在20℃下,根據表1所記載的調配份數,將表1所記載的各成分均勻混合,而製作實施例1~29及比較例1~7的洗淨劑。其中,表1所記載的(A)~(F)的份數是有效成分的份數,超純水的份數包括(A-1)~(A-6)及下述(D)的PANa中的水。
另外,表1中的成分的簡稱如下。
.MeXSNa:間二甲苯磺酸鈉鹽(北星興業股份有限公司製造)
.SDS:十二烷基硫酸鈉(Nacalai Tesque股份有限公
司製造:比較用的陰離子界面活性劑)
.PELSNa:聚氧乙烯十二烷基醚硫酸鈉(Sandet EN,三洋化成工業股份有限公司製造:比較用的陰離子界面活性劑)
.D2ehNa:磺基琥珀酸二(2-乙基己基)酯鈉(東京化成工業股份有限公司製造:比較用的陰離子界面活性劑)
.HC:己基卡必醇(SP值為10.2)
.PP-15:丙烯五聚物(SP值為7.6)
.TEG-M:三乙二醇單甲醚(SP值為10.8)
.FA:甲醯胺(SP值為19.2:比較用的溶劑)
.KOH:氫氧化鉀
.DBU:1,8-二氮雜雙環[5.4.0]-7-十一烯[SAN-APRO股份有限公司製造]
.MDEA:N-甲基二乙醇胺
.CHNEG:上述製造例7所獲得的環己胺環氧乙烷(2莫耳)加成物
.PANa:聚丙烯酸鈉[Calibon L-400,43%的水溶液,三洋化成工業股份有限公司製造]
.EDTA:乙二胺四乙酸
.Cys:L-半胱胺酸
以原本的濃度將實施例1~29及比較例1~7的洗淨劑直接用作洗淨液,對pH值、洗淨性-1、洗淨性-2、洗淨性-3、洗淨性-4、洗淨性-5、蝕刻性、洗淨後相對於水的接觸角、洗淨液的接觸角、表面粗糙度、起泡性及經時穩
定性進行測定或評價,將測定及評價結果示於表2。
此外,pH值、洗淨性-1、洗淨性-2、洗淨性-3、洗淨性-4、洗淨性-5、蝕刻性、洗淨後相對於水的接觸角、洗淨液的接觸角、表面粗糙度、起泡性及經時穩定性的測定或評價是藉由以下方法來進行。
使用pH計(堀場製作所股份有限公司製造,M-12),於測定溫度25℃下測定pH值。
在70℃的加熱板(PMC Industries公司製造,數位式加熱板系列(Digital Hot Plate Series)730)上,以1分鐘將作為樣本汚染物質的正三十酸(triacontan)(東京化成工業股份有限公司製造)10 mg融著在市售的玻璃基板(康寧公司製造,玻璃板#1737,長10 cm×寬10 cm)上,藉此製作汚染基板。然後,取洗淨液1000 g置於2 L玻璃製燒杯內,將所製作的汚染基板浸漬在其中,在超音波洗淨機(200 kHz)內,在30℃下洗淨5分鐘。洗淨後,取出基板,用超純水充分沖洗後,吹入氮氣進行乾燥,然後根據下述評價點,利用微分干擾顯微鏡(Differential Interference Microscopy)(Nikon公司製造,OPTIPHOT-2,倍率為400倍)評價基板表面的洗淨性。此外,為了防止受到空氣汚染,本評價是在潔淨等級(class)為1,000(FED-STD-209D,美國聯邦標準,1988年)的無塵室內實施的。
◎:幾乎可完全除去。
O:大致可洗淨。
△:殘留有少許粒子。
×:幾乎無法洗淨。
除了塗佈有鄰苯二甲酸二辛酯(東京化成工業股份有限公司製造)10 mg作為樣本汚染物質以外,以與洗淨性-1相同的方式進行評價。
於市售的玻璃基板(康寧公司製造,玻璃板#1737,長10 cm×寬10 cm)上,散布切割玻璃板(斷裂)時的玻璃粉5 mg,在105℃的加熱板(PMC Industries公司製造,數位式加熱板系列730)上加熱1小時,藉此製作汚染基板,除此以外,以與洗淨性-1相同的方式進行評價。
使用作為研磨劑的市售二氧化矽溶膠(colloidal silica)漿料(KEMIRA公司製造,VI-80)及研磨布,對市售玻璃基板(康寧公司製造,玻璃板#1737,長10 cm×寬10 cm)進行研磨後,用超純水沖洗表面並吹入氮氣,藉此製作汚染基板,除此以外,以與洗淨性-1相同的方式進行評價。
使用作為研磨劑的市售氧化鈰漿料(Fujimi Incorporated公司製造,CEPOL-120)及研磨布,對市售玻璃基板(康寧公司製造,玻璃板#1737,長10 cm×寬10 cm)
進行研磨後,用超純水沖洗表面並吹入氮氣,藉此製作汚染基板,除此以外,以與洗淨性-1相同的方式進行評價。
取洗淨液10 g置於50 ml聚丙烯製容器內,將溫度調節為50℃後,放入將市售玻璃基板(康寧公司製造,玻璃板#1737)切割成長2 cm×寬2 cm大小的基板,在50℃下浸漬並靜置24小時後,採集洗淨液,利用ICP光譜分析裝置(VARIAN公司製造,Varian 730-ES)測定洗淨液中的Si含量。此外,亦以相同的方式預先測定試驗前的洗淨液中的Si含量,求出兩者的差,藉此求得試驗中所溶出的Si含量(ppb)。此溶出的Si含量越多,則蝕刻性越高。
使用全自動接觸角儀[協和界面科學股份有限公司製造,PD-W],對剛經過上述洗淨性-1的評價的基板測定此基板相對於水的接觸角(25℃、10秒後)。
將市售玻璃基板(康寧公司製造,玻璃板#1737,長10 cm×寬10 cm)用超純水充分沖洗後,在25℃下吹入氮氣進行乾燥後,立即使用全自動接觸角儀[協和界面科學股份有限公司製造,PD-W],對基板測定洗淨液的接觸角(25℃、10秒後)。
取洗淨液10 g置於20 ml玻璃製容器內,將溫度調節為50℃後,放入將市售玻璃基板(康寧公司製造,玻璃板
#1737)切割成長2 cm×寬2 cm大小的基板,在50℃下浸漬並靜置5小時後,使用鑷子取出基板,用超純水充分沖洗而除去洗淨液後,在25℃下吹入氮氣進行乾燥,然後使用原子力顯微鏡(SII Nano Technology股份有限公司製造,E-Sweep)來測定基板表面的表面粗糙度(Ra)。Ra越小,表面平坦性越優異。
向100 ml的玻璃製有栓量筒(measuring cylinder)(作為JIS R3504「化學用體積儀玻璃原材料」的有栓量筒而規定尺寸的量筒)內,放入洗淨液20 ml,並在恆溫水槽中將溫度調節為25℃後,蓋上有栓量筒的蓋子,用30秒將量筒上下激烈振盪60次,測定振盪剛結束後及1分鐘後的氣泡量(ml)。振盪剛結束後的氣泡量越少,則起泡性越低,1分鐘後的氣泡量越少,則消泡性越高。
取洗淨液45 ml置於50 ml的玻璃容器內,在5℃及50℃的條件下靜置保存6個月,根據下述評價點,評價經時穩定性。
◎:在5℃及50℃下,均無外觀變化。
O:在5℃或50℃下,雖有少許分離,但輕微搖晃,便可變均勻。
△:於5℃或50℃下,雖分離較多,但輕微搖晃,便可變均勻。
×:於5℃、50℃下,均有分離,即使輕微搖晃,亦無
法變均勻。
[表1]
由表2的結果可知,本發明的電子材料用洗淨劑無損基板表面的平坦性,具有經適度控制的蝕刻性,並且有機物污漬、玻璃屑及研磨劑等微粒的除去性及防止再次污染性優異。
本發明的電子材料用洗淨劑,適合以油分、來自人體的污漬(指紋等)、樹脂、增塑劑(鄰苯二甲酸二辛酯等)、有機微粒等有機物,及無機微粒(玻璃粉末、砥粒、陶瓷粉末及金屬粉末等)等作為對象進行洗淨。
因此,本發明的電子材料用洗淨劑,可較好地用於各種電子材料[例如,平面顯示器用基板(液晶面板用的玻璃基板、彩色濾光器(color filter)基板、陣列(array)基板、電漿顯示器(plasma display)用基板及有機EL(organic electroluminescence)用基板等)、光罩用基板、硬碟用基板(鋁基板、Nip基板、玻璃基板、磁光碟(magnetic disk)及磁頭(magnetic head)等)、半導體用基板(半導體元件及矽晶圓(silicon wafer)等)、光學透鏡(optical lens)、印刷配線基板、光通訊用電纜(optical telecommunication cable)、LED、太陽電池用基板以及晶體振盪器(crystal oscillator)]的製造步驟中的洗淨步驟。
另外,本發明的電子材料的洗淨方法,特別適合於平面顯示器用基板、光罩用基板、硬碟用基板或半導體用基板的電子材料。
雖然本發明已以實施例揭露如上,然其並非用以限定本發明,任何所屬技術領域中具有通常知識者,在不脫離
本發明之精神和範圍內,當可作些許之更動與潤飾,故本發明之保護範圍當視後附之申請專利範圍所界定者為準。
Claims (12)
- 一種電子材料用洗淨劑,其陰離子成分是含有通式(1)所表示的陰離子性界面活性劑(A)、以及選自由碳數為6~18的烯烴及以通式(2)所表示的有機溶劑所組成族群中的一種或一種以上的有機溶劑(B)而成,且上述(B)的SP值為6~13,R1[-(OA1)a-Q-]b (1)式(1)中,R1表示碳數為1~10的烴基,A1表示碳數為2~4的亞烷基,Q-表示-COO-、-OCH2COO-、-SO3 -、-OSO3 -或-OPO2(OR2)-,R2表示氫或碳數為1~10的烴基,a為平均值且為0~20,b為1~6的整數,當Q-為-COO-或-SO3 -時,a為0,R3[-(OA2)c-OH]d (2)式(2)中,R3表示碳數為1~12的烴基,A2表示碳數為2~4的亞烷基,c為平均值且為0~20,d為1~6的整數,且該電子材料用洗淨劑更含有鹼成分(C),且在用作洗淨液時的有效成分濃度下的25℃時的pH值為10~14。
- 如申請專利範圍第1項所述的電子材料用洗淨劑,其中陰離子性界面活性劑(A)的陽離子成分是選自由鹼金屬陽離子、碳數為1~15的脂肪族胺上加成有質子的一價陽離子、碳數為4~10的脒化合物上加成有質子的陽離子、及碳數為1~15的烷醇胺上加成有質子的一價陽離子所組成族群中的一種或一種以上的陽離子。
- 如申請專利範圍第1項所述的電子材料用洗淨劑,其中通式(1)中,R1表示通式(3)或通式(4)所表示的烴基,
- 如申請專利範圍第1項所述的電子材料用洗淨劑,其中通式(1)中,a為0且b為1,上述鹼成分(C)是選自由碳數為1~36的脂肪族胺(C-2)、無機鹼(C-3)、碳數為1~23的烷醇胺(C-4)、及碳數為4~10的脒化合物(C-5)所組成族群中的一種或一種以上的鹼成分。
- 如申請專利範圍第1項所述的電子材料用洗淨劑,其中基於電子材料用洗淨劑的有效成分的重量,上述(A)的含量為1~95重量%,上述(B)的含量為2~95重量%,以及上述(C)的含量為1~55重量%。
- 如申請專利範圍第1項所述的電子材料用洗淨劑,其更含有選自由高分子型分散劑(D)及螯合劑(E)所組成族群中的一種或一種以上。
- 如申請專利範圍第1項至第6項中任一項所述的電子材料用洗淨劑,其用作洗淨液時的有效成分濃度為0.1~15重量%,洗淨液相對於玻璃的接觸角小於等於10°。
- 如申請專利範圍第1項至第6項中任一項所述的電子材料用洗淨劑,其中相對於使用上述電子材料用洗淨劑來洗淨的玻璃,水的接觸角小於等於20°。
- 如申請專利範圍第1項至第6項中任一項所述的電子材料用洗淨劑,其是用於洗淨平面顯示器基板、光罩基板、硬碟基板或半導體基板。
- 一種電子材料的洗淨方法,其使用如申請專利範圍第1項至第6項中任一項所述的電子材料用洗淨劑。
- 如申請專利範圍第10項所述的電子材料的洗淨方法,其是使用選自由超音波洗淨、噴淋洗淨、噴霧洗淨、毛刷洗淨、浸漬洗淨、浸漬搖動洗淨及單片式洗淨所組成族群中的至少一種或一種以上的洗淨方法來進行洗淨。
- 如申請專利範圍第10項所述的洗淨方法,其中上述電子材料是平面顯示器基板、光罩基板、硬碟基板或半導體基板。
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CN102639686B (zh) * | 2009-07-29 | 2014-09-03 | 东友Fine-Chem股份有限公司 | 清洁组成物及使用该组成物清洁面板的方法 |
JP5500911B2 (ja) * | 2009-08-26 | 2014-05-21 | ライオン株式会社 | ハードディスク基板用洗浄剤組成物、およびハードディスク基板の洗浄方法 |
KR20110028239A (ko) * | 2009-09-11 | 2011-03-17 | 동우 화인켐 주식회사 | 평판표시장치 제조용 기판의 세정액 조성물 |
WO2011031092A2 (ko) * | 2009-09-11 | 2011-03-17 | 동우 화인켐 주식회사 | 평판표시장치 제조용 기판의 세정액 조성물 |
JP5515588B2 (ja) * | 2009-10-05 | 2014-06-11 | 栗田工業株式会社 | ウエハ用洗浄水及びウエハの洗浄方法 |
JP5585076B2 (ja) * | 2009-12-24 | 2014-09-10 | 栗田工業株式会社 | 洗浄方法 |
JP5401359B2 (ja) * | 2010-02-16 | 2014-01-29 | 花王株式会社 | 硬質表面用アルカリ洗浄剤組成物 |
JP5774330B2 (ja) * | 2011-02-28 | 2015-09-09 | 三洋化成工業株式会社 | 電子材料用洗浄剤 |
WO2012161270A1 (ja) * | 2011-05-24 | 2012-11-29 | 旭硝子株式会社 | 洗浄剤およびガラス基板の洗浄方法 |
TW201323102A (zh) * | 2011-12-15 | 2013-06-16 | Dongwoo Fine Chem Co Ltd | 清洗製造有機el裝置的氣相沉積掩模的方法及清洗液 |
JP6123334B2 (ja) | 2012-02-17 | 2017-05-10 | 三菱化学株式会社 | 半導体デバイス用洗浄液及び半導体デバイス用基板の洗浄方法 |
CN102911821B (zh) * | 2012-10-25 | 2015-01-28 | 东莞市伟思化学科技有限公司 | 一种水基光学透镜清洗剂组合物 |
JP6234673B2 (ja) * | 2012-12-05 | 2017-11-22 | 花王株式会社 | ガラス基板の洗浄方法 |
WO2014208353A1 (ja) * | 2013-06-24 | 2014-12-31 | 三菱電機株式会社 | 太陽光発電装置用基板の製造方法および太陽光発電装置用基板の製造装置 |
JP6208575B2 (ja) * | 2013-12-24 | 2017-10-04 | 花王株式会社 | 洗浄剤組成物 |
JP2016037606A (ja) * | 2014-08-08 | 2016-03-22 | 三洋化成工業株式会社 | 電子材料用洗浄剤組成物及び電子材料の製造方法 |
CN107532115A (zh) | 2015-06-24 | 2018-01-02 | 花王株式会社 | 玻璃制硬盘基板用清洗剂组合物 |
MY187480A (en) * | 2015-11-30 | 2021-09-23 | Kao Corp | Polishing liquid composition for magnetic disk substrate |
CN109196113B (zh) * | 2016-02-11 | 2022-10-04 | 奇根科学有限责任公司 | 合成测序中的多酚添加剂 |
CN105714585B (zh) * | 2016-04-12 | 2017-10-31 | 张家港市德宝化工有限公司 | 一种用于合成纤维的还原清洗剂、其制备方法及应用 |
EP3523241A4 (en) * | 2016-10-06 | 2020-05-13 | FujiFilm Electronic Materials USA, Inc. | CLEANING FORMULATIONS FOR REMOVING RESIDUES ON SEMICONDUCTOR SUBSTRATES |
CN106753865A (zh) * | 2016-11-29 | 2017-05-31 | 洛阳新巨能高热技术有限公司 | 电子材料清洗剂 |
CN106800982A (zh) * | 2016-11-29 | 2017-06-06 | 洛阳新巨能高热技术有限公司 | 一种电子材料用清洗剂 |
CN106847691B (zh) * | 2016-12-11 | 2020-05-22 | 安徽兆利光电科技有限公司 | 一种整流二极管清洗方法 |
JPWO2018174092A1 (ja) * | 2017-03-22 | 2020-01-30 | 三菱ケミカル株式会社 | 半導体デバイス用基板の洗浄液、半導体デバイス用基板の洗浄方法、半導体デバイス用基板の製造方法及び半導体デバイス用基板 |
KR101955597B1 (ko) * | 2017-05-17 | 2019-05-31 | 세메스 주식회사 | 세정액 제조 장치 및 방법 |
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KR102029442B1 (ko) * | 2018-01-04 | 2019-10-08 | 삼성전기주식회사 | 드라이필름 레지스트 제거용 박리조성물 및 이를 이용한 드라이필름 레지스트의 박리방법 |
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WO2009078123A1 (ja) | 2009-06-25 |
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