TWI488943B - Etching paste composition and the application thereof - Google Patents
Etching paste composition and the application thereof Download PDFInfo
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本發明是有關於一種蝕刻膏組成物，特別是指一種適用於絲網印刷的蝕刻膏組成物。The present invention relates to an etching paste composition, and more particularly to an etching paste composition suitable for screen printing.
觸控面板、薄膜電晶體或太陽能電池的結構中，常藉由化學氣相沉積(Chemical Vapor Deposition，CVD)或濕式化學塗佈等方式，藉以形成氧化矽或氮化矽層，於多數情況下，常作為抗反射層或鈍化層之使用。In the structure of a touch panel, a thin film transistor or a solar cell, a layer of yttrium oxide or tantalum nitride is often formed by chemical vapor deposition (CVD) or wet chemical coating, in most cases. Next, it is often used as an antireflection layer or a passivation layer.
移除氧化矽或氮化矽層之特定部份的步驟稱為蝕刻，習知技術包括採用雷射支持蝕刻法(laser-supported etching method)，或在光阻形成遮罩圖案後，藉由濕式蝕刻法(wet-chemical method)或乾式蝕刻法(dry-etching method)選擇性地進行蝕刻。The step of removing a specific portion of the tantalum oxide or tantalum nitride layer is referred to as etching, and conventional techniques include using a laser-supported etching method or by forming a mask pattern after the photoresist is formed by wet etching. The etching is selectively performed by a wet-chemical method or a dry-etching method.
就雷射支持蝕刻法來說，雖具有高度精密性，但其逐點逐行地掃描蝕刻圖案的工作方式需要大量的工作時間，不利工業上量產。乾式蝕刻法或濕式蝕刻法，需先使用光阻製作出遮罩圖案，之後，乾式蝕刻法是於真空裝置中予以電漿蝕刻或利用反應性氣體在流動反應器中蝕刻 ，製程複雜且設備昂貴，而濕式蝕刻法則是以具有蝕刻活性的化學藥劑浸泡並蝕刻出圖案，最後將光阻遮罩圖案以溶劑剝除，並於清水沖洗後乾燥。In terms of the laser-assisted etching method, although it is highly precise, the operation of scanning the etching pattern line by line by line requires a large amount of work time, which is disadvantageous for mass production in the industry. Dry etching or wet etching requires first using a photoresist to create a mask pattern. Thereafter, the dry etching method is plasma etching in a vacuum device or etching in a flow reactor using a reactive gas. The process is complicated and the equipment is expensive, and the wet etching method soaks and etches the pattern with the etch-active chemical agent, and finally the photoresist mask pattern is solvent-stripped, and dried after washing with water.
JP2012-129346揭示一種蝕刻液組成物，特別適用於蝕刻氧化銦系被膜，係由含有下述成分的水溶液所構成：(A)2-羥基乙磺酸或其鹽依2-羥基乙磺酸換算為5~20 wt%；以及(B)從氫氟酸、氟化銨、氟化鉀、氟化鈉及氟化鋰所構成群組中選擇之至少1種氟化化合物0.05~5 wt%。但濕式蝕刻法相當耗時且複雜，所用的化學原料更具有毒性及高腐蝕性。JP 2012-129346 discloses an etching liquid composition which is particularly suitable for etching an indium oxide-based coating film, and is composed of an aqueous solution containing the following components: (A) 2-hydroxyethanesulfonic acid or a salt thereof in terms of 2-hydroxyethanesulfonic acid 5 to 20 wt%; and (B) 0.05 to 5 wt% of at least one fluorinated compound selected from the group consisting of hydrofluoric acid, ammonium fluoride, potassium fluoride, sodium fluoride, and lithium fluoride. However, the wet etching method is quite time consuming and complicated, and the chemical materials used are more toxic and highly corrosive.
目前有更高度自動化且更高產量的作法，是透過印刷技術將蝕刻膏轉移至待蝕刻的表面並進行蝕刻，不需要進行光阻遮罩圖案的製作步驟，例如移印方法、壓印方法、噴墨印刷方法，或手動印刷等。At present, there is a more highly automated and higher-yield method of transferring the etching paste to the surface to be etched by etching and etching, without the need for a photoresist mask patterning step, such as a pad printing method, an imprint method, Inkjet printing methods, or manual printing, and the like.
由上述可知，就經濟效益來說，一種適用於印刷技術且品質良好的蝕刻膏組成物，是有迫切需求的。From the above, it is known that there is an urgent need for an etching paste composition which is suitable for printing technology and of good quality in terms of economic efficiency.
因此，本發明之第一目的，即在於提供一種適用於絲網印刷且經時安定性佳的蝕刻膏組成物。Accordingly, a first object of the present invention is to provide an etching paste composition which is suitable for screen printing and which has good stability over time.
於是，本發明蝕刻膏組成物，包含：含氟化合物(A)；溶劑(B)，包括芳香醇類溶劑(B-1)、水(B-2)及其他溶劑(B-3)；微粒(C)，是選自於聚合物微粒(C-1)、無機化合物微粒 (C-2)，或此等之一組合；有機增稠劑(D)；及酸(E)，是選自於有機酸(E-1)、無機酸(E-2)，或此等之一組合。Thus, the etching paste composition of the present invention comprises: a fluorine-containing compound (A); a solvent (B) comprising an aromatic alcohol solvent (B-1), water (B-2), and other solvents (B-3); (C) is selected from the group consisting of polymer particles (C-1) and inorganic compound particles. (C-2), or a combination thereof; an organic thickener (D); and an acid (E) selected from the group consisting of organic acids (E-1), inorganic acids (E-2), or the like One combination.
本發明另一目的，在於提供一種蝕刻方法。Another object of the present invention is to provide an etching method.
本發明蝕刻方法，包含：提供一觸控面板，包括一基板，以及一設置於該基板上的氧化矽層或氮化矽層；將如前所述的蝕刻膏組成物絲網印刷於該氧化矽層或氮化矽層上；進行一蝕刻步驟；及進行一清洗步驟。The etching method of the present invention comprises: providing a touch panel comprising a substrate, and a ruthenium oxide layer or a tantalum nitride layer disposed on the substrate; and screen printing the etch paste composition as described above on the oxidized layer On the tantalum layer or the tantalum nitride layer; performing an etching step; and performing a cleaning step.
本發明之功效在於：該蝕刻膏組成物，透過含有特定成分及比例的溶劑調控其揮發性和均勻程度，後續應用於絲網印刷時，黏度經時安定性良好，且不易有塞網的情形發生。The effect of the invention is that the composition of the etching paste regulates the volatility and uniformity of the solvent through a solvent containing a specific component and a ratio, and the viscosity is stable and stable over time when applied to the screen printing, and the plugging net is not easy. occur.
本發明蝕刻膏組成物，包含：含氟化合物(A)；溶劑(B)，包括芳香醇類溶劑(B-1)、水(B-2)及其他溶劑(B-3)； 微粒(C)，是選自於聚合物微粒(C-1)、無機化合物微粒(C-2)，或此等之一組合；有機增稠劑(D)；及酸(E)，是選自於有機酸(E-1)、無機酸(E-2)，或此等之一組合。The etching paste composition of the present invention comprises: a fluorine-containing compound (A); a solvent (B) comprising an aromatic alcohol solvent (B-1), water (B-2) and other solvents (B-3); The fine particles (C) are selected from the group consisting of polymer microparticles (C-1), inorganic compound microparticles (C-2), or a combination thereof; organic thickener (D); and acid (E), which are selected From organic acid (E-1), inorganic acid (E-2), or a combination of these.
該蝕刻膏組成物透過溶劑組成的調節，可以控制該蝕刻膏組成物的揮發性和均勻程度，後續應用於絲網印刷時，具有經時安定性佳且不塞網的優點。The composition of the etching paste can control the volatility and uniformity of the composition of the etching paste by adjusting the composition of the solvent, and the subsequent application to the screen printing has the advantages of good stability over time and no netting.
以該含氟化合物(A)為100重量份計，該溶劑(B)之用量為350至2000重量份，該微粒(C)的用量為300至2000重量份，該有機增稠劑(D)的用量為10至200重量份，該酸(E)的用量為30至600重量份。The solvent (B) is used in an amount of from 350 to 2000 parts by weight, based on 100 parts by weight of the fluorine-containing compound (A), and the fine particles (C) are used in an amount of from 300 to 2000 parts by weight, the organic thickener (D) The amount used is 10 to 200 parts by weight, and the acid (E) is used in an amount of 30 to 600 parts by weight.
較佳地，以該含氟化合物(A)為100重量份計，該溶劑(B)之用量為450至1800重量份，該微粒(C)的用量為400至1800重量份，該有機增稠劑(D)的用量為15至180重量份，該酸(E)的用量為40至550重量份。Preferably, the solvent (B) is used in an amount of from 450 to 1800 parts by weight based on 100 parts by weight of the fluorine-containing compound (A), and the fine particles (C) are used in an amount of from 400 to 1800 parts by weight, the organic thickening The agent (D) is used in an amount of 15 to 180 parts by weight, and the acid (E) is used in an amount of 40 to 550 parts by weight.
更佳地，以該含氟化合物(A)為100重量份計，該溶劑(B)之用量為500至1500重量份，該微粒(C)的用量為500至1500重量份，該有機增稠劑(D)的用量為20至150重量份，該酸(E)的用量為50至500重量份。More preferably, the solvent (B) is used in an amount of 500 to 1500 parts by weight based on 100 parts by weight of the fluorine-containing compound (A), and the fine particles (C) are used in an amount of 500 to 1500 parts by weight, the organic thickening The agent (D) is used in an amount of 20 to 150 parts by weight, and the acid (E) is used in an amount of 50 to 500 parts by weight.
該芳香醇類溶劑(B-1)因為揮發性低，能調節該蝕刻膏組成物的黏度並減少因溶劑揮發所造成的黏度改變；若未使用，則會有黏度經時安定性不佳以及絲網印刷時塞網等問題產生。若未使用水(B-2)，該蝕刻膏組成物於使 用時可能有塞網的問題產生。若未使用其他溶劑(B-3)，則會有經時黏度安定性不佳的問題。The aromatic alcohol solvent (B-1) can adjust the viscosity of the etching paste composition and reduce the viscosity change caused by the solvent volatilization because of low volatility; if not used, the viscosity will be unstable over time and Problems such as plugging the net during screen printing. If water (B-2) is not used, the etching paste composition is There may be problems with the plugged network when using it. If no other solvent (B-3) is used, there is a problem that the stability of the viscosity over time is not good.
以該含氟化合物(A)為100重量份計，該芳香醇類溶劑(B-1)的用量為100至500重量份，水(B-2)的用量為50至300重量份，其他溶劑(B-3)的用量為200至1200重量份。The aromatic alcohol solvent (B-1) is used in an amount of 100 to 500 parts by weight, and the water (B-2) is used in an amount of 50 to 300 parts by weight, based on 100 parts by weight of the fluorine-containing compound (A), and other solvents. (B-3) is used in an amount of from 200 to 1200 parts by weight.
較佳地，該含氟化合物(A)為100重量份計，該芳香醇類溶劑(B-1)的用量為150至450重量份，水(B-2)的用量為60至270重量份，其他溶劑(B-3)的用量為250至1000重量份。Preferably, the fluorine-containing compound (A) is used in an amount of from 150 to 450 parts by weight based on 100 parts by weight of the aromatic alcohol solvent (B-1), and the amount of water (B-2) is from 60 to 270 parts by weight. The other solvent (B-3) is used in an amount of from 250 to 1,000 parts by weight.
更佳地，以該含氟化合物(A)為100重量份計，該芳香醇類溶劑(B-1)的用量為200至400重量份，水(B-2)的用量為70至250重量份，其他溶劑(B-3)的用量為300至800重量份。More preferably, the aromatic alcohol solvent (B-1) is used in an amount of 200 to 400 parts by weight, and the water (B-2) is used in an amount of 70 to 250 parts by weight based on 100 parts by weight of the fluorine-containing compound (A). The other solvent (B-3) is used in an amount of from 300 to 800 parts by weight.
該含氟化合物(A)是至少一種選自於由下列所構成群組的化合物：氟化氫銨(Ammonium bifluoride)、氟化銨(Ammonium fluoride)、氟化氫鈉(Sodium bifluoride)、氟化鈉(Sodium fluoride)、氟化氫鉀(Potassium bifluoride)、氟化鉀(Potassium fluoride)、氟化鋇(Barium fluoride)，及氟硼酸銨(Ammonium Fluoborate)。The fluorine-containing compound (A) is at least one selected from the group consisting of ammonium hydrogen fluoride (Ammonium bifluoride), ammonium fluoride (Ammonium fluoride), sodium hydrogen fluoride (Sodium bifluoride), sodium fluoride (Sodium fluoride). ), Potassium bifluoride, Potassium fluoride, Barium fluoride, and Ammonium Fluoborate.
較佳地，該含氟化合物(A)是至少一種選自於由下列所構成群組的化合物：氟化氫銨、氟化氫鈉及氟化鋇。Preferably, the fluorine-containing compound (A) is at least one selected from the group consisting of ammonium hydrogen fluoride, sodium hydrogen fluoride, and barium fluoride.
該芳香醇類溶劑(B-1)是至少一種選自於下列所 構成群組的化合物：苯甲醇、(2-羥基苯基)甲醇、(甲氧基苯基)甲醇、(3,4-二羥基苯基)甲醇、4-(羥甲基)苯-1,2-二醇、(4-羥基-3-甲氧基苯基)甲醇、(3,4-二甲氧基苯基)甲醇、(4-異丙基苯基)甲醇、2-苯乙醇、1-苯乙醇、2-苯基-1-丙醇、對甲苯基醇、2-(4-羥基-3-甲氧基苯基)甲烷-1-醇、2-(3,4-二甲氧基苯基)甲烷-1-醇、3-苯基-丙烷-1-醇、2-苯基-丙烷-2-醇、肉桂醇、3-(4-羥基-3-甲氧基苯基)丙-2-烯-1-醇、3-(4-羥基-3,5-甲氧基苯基)丙-2-烯-1-醇、聯苯甲醇、三苯甲醇、1,2-聯苯甲烷-1,2-二醇，1,1,2,2-四苯基甲烷-1,2-二醇、苯-1,2-二甲醇、苯-1，3-二甲醇，及苯-1,4-二甲醇。The aromatic alcohol solvent (B-1) is at least one selected from the group consisting of the following Compounds constituting the group: benzyl alcohol, (2-hydroxyphenyl)methanol, (methoxyphenyl)methanol, (3,4-dihydroxyphenyl)methanol, 4-(hydroxymethyl)benzene-1, 2-diol, (4-hydroxy-3-methoxyphenyl)methanol, (3,4-dimethoxyphenyl)methanol, (4-isopropylphenyl)methanol, 2-phenylethanol, 1-phenylethanol, 2-phenyl-1-propanol, p-tolyl alcohol, 2-(4-hydroxy-3-methoxyphenyl)methane-1-ol, 2-(3,4-dimethyl Oxyphenyl)methane-1-ol, 3-phenyl-propan-1-ol, 2-phenyl-propan-2-ol, cinnamyl alcohol, 3-(4-hydroxy-3-methoxyphenyl )prop-2-en-1-ol, 3-(4-hydroxy-3,5-methoxyphenyl)prop-2-en-1-ol, biphenylmethanol, triphenylmethanol, 1,2- Biphenylmethane-1,2-diol, 1,1,2,2-tetraphenylmethane-1,2-diol, benzene-1,2-dimethanol, benzene-1,3-dimethanol, and Benzene-1,4-dimethanol.
較佳地，該芳香醇類溶劑(B-1)是至少一種選自於下列所構成群組的化合物：苯甲醇、(2-羥基苯基)甲醇及(4-異丙基苯基)甲醇。Preferably, the aromatic alcohol solvent (B-1) is at least one compound selected from the group consisting of benzyl alcohol, (2-hydroxyphenyl)methanol, and (4-isopropylphenyl)methanol. .
該其他溶劑(B-3)是至少一種選自於由下列所構成群組的溶劑：不具芳香基的醇類溶劑、醚類溶劑、羧酸之酯類溶劑，及酮類溶劑。The other solvent (B-3) is at least one selected from the group consisting of a solvent having no aromatic group, an ether solvent, an ester solvent of a carboxylic acid, and a ketone solvent.
該不具芳香基的醇類溶劑是至少一種選自於由下列所構成群組的溶劑：丙三醇、1,2-丙二醇、1,4-丁二醇、1,3-丁二醇、1,5-戊二醇、2-乙基-1-己烯醇、乙二醇、二乙二醇、二丙二醇、甲醇、乙醇、異丙醇、正丙醇、戊醇、1-十六醇、1,2,3,4-丁四醇、丙-2-烯-1-醇、2-丙炔-1-醇、3,7-二甲基庚-2,6-二烯-1-醇、木糖醇，及甘露醇。The non-aromatic alcohol solvent is at least one selected from the group consisting of glycerol, 1,2-propanediol, 1,4-butanediol, 1,3-butanediol, 1 , 5-pentanediol, 2-ethyl-1-hexenol, ethylene glycol, diethylene glycol, dipropylene glycol, methanol, ethanol, isopropanol, n-propanol, pentanol, 1-hexadecanol 1,2,3,4-butanetetraol, prop-2-en-1-ol, 2-propyn-1-ol, 3,7-dimethylheptane-2,6-diene-1- Alcohol, xylitol, and mannitol.
該醚類溶劑是至少一種選自於由下列所構成群組的溶劑：四氫呋喃、乙二醇單丁醚、三乙二醇單甲醚、 二乙二醇單丁醚、二丙二醇單甲醚、乙二醇單丙醚、乙二醇單甲醚、乙二醇單***、乙二醇丁醚醋酸酯、乙二醇***醋酸酯、乙二醇甲醚醋酸酯、二乙二醇單甲醚、二乙二醇單***、二乙二醇二甲醚、二乙二醇二***、二乙二醇甲***、二丙二醇單***、二丙二醇二甲醚、二丙二醇二***、二丙二醇甲***、丙二醇單甲醚、丙二醇單***、丙二醇單丙醚、丙二醇單丁醚、丙二醇甲醚醋酸酯、丙二醇***醋酸酯、丙二醇丙醚醋酸酯、丙二醇丁醚醋酸酯、丙二醇甲醚丙酸酯、丙二醇***丙酸酯、丙二醇丙醚丙酸酯，及丙二醇丁醚丙酸酯。The ether solvent is at least one selected from the group consisting of tetrahydrofuran, ethylene glycol monobutyl ether, triethylene glycol monomethyl ether, Diethylene glycol monobutyl ether, dipropylene glycol monomethyl ether, ethylene glycol monopropyl ether, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol butyl ether acetate, ethylene glycol ethyl ether acetate, B Glycol methyl ether acetate, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol dimethyl ether, diethylene glycol diethyl ether, diethylene glycol methyl ethyl ether, dipropylene glycol monoethyl ether, two Propylene glycol dimethyl ether, dipropylene glycol diethyl ether, dipropylene glycol methyl ether, propylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol monopropyl ether, propylene glycol monobutyl ether, propylene glycol methyl ether acetate, propylene glycol diethyl ether acetate, propylene glycol propyl ether acetate , propylene glycol butyl ether acetate, propylene glycol methyl ether propionate, propylene glycol diethyl ether propionate, propylene glycol propyl ether propionate, and propylene glycol butyl ether propionate.
該羧酸之酯類溶劑是至少一種選自於由下列所構成群組的溶劑：2-(2-正丁氧基乙氧基)乙酸乙酯、碳酸丙烯酯、γ-丁內酯、γ-戊內酯、δ-戊內酯、乙酸甲酯、乙酸乙酯、乙酸丙酯、乙酸丁酯、2-羥基丙酸乙酯、2-羥基-2-甲基丙酸甲酯、2-羥基-2-甲基丙酸乙酯、羥乙酸甲酯、羥乙酸乙酯、羥乙酸丁酯、乳酸甲酯、乳酸丙酯、乳酸丁酯、3-羥基丙酸甲酯、3-羥基丙酸乙酯、3-羥基丙酸丙酯、3-羥基丙酸丁酯、2-羥基-3-甲基丁酸甲酯、甲氧基乙酸甲酯、甲氧基乙酸乙酯、甲氧基乙酸丁酯、乙氧基乙酸甲酯、乙氧基乙酸乙酯、乙氧基乙酸丙酯、乙氧基乙酸丁酯、丙氧基乙酸甲酯、丙氧基乙酸乙酯、丙氧基乙酸丙酯、丙氧基乙酸丁酯、丁氧基乙酸甲酯、丁氧基乙酸乙酯、丁氧基乙酸丙酯、丁氧基乙酸丁酯、3-甲氧基丁基乙酸酯、2-甲氧基丙酸甲酯、2-甲氧基丙酸乙酯、2-甲氧基丙酸丙酯、2-甲氧 基丙酸丁酯、2-乙氧基丙酸甲酯、2-乙氧基丙酸乙酯、2-乙氧基丙酸丙酯、2-乙氧基丙酸丁酯、2-丁氧基丙酸甲酯、2-丁氧基丙酸甲酯、2-丁氧基丙酸乙酯、2-丁氧基丙酸丙酯、2-丁氧基丙酸丁酯、3-甲氧基丙酸甲酯、3-甲氧基丙酸乙酯、3-甲氧基丙酸丙酯、3-甲氧基丙酸丁酯、3-乙氧基丙酸甲酯、3-乙氧基丙酸乙酯、3-乙氧基丙酸丙酯、3-乙氧基丙酸丁酯、3-丙氧基丙酸甲酯、3-丙氧基丙酸乙酯、3-丙氧基丙酸丙酯、3-丙氧基丙酸丁酯、3-丁氧基丙酸甲酯、3-丁氧基丙酸乙酯、3-丁氧基丙酸丙酯，及3-丁氧基丙酸丁酯等。The ester solvent of the carboxylic acid is at least one selected from the group consisting of ethyl 2-(2-n-butoxyethoxy)acetate, propylene carbonate, γ-butyrolactone, γ -valerolactone, δ-valerolactone, methyl acetate, ethyl acetate, propyl acetate, butyl acetate, ethyl 2-hydroxypropionate, methyl 2-hydroxy-2-methylpropionate, 2- Ethyl hydroxy-2-methylpropionate, methyl hydroxyacetate, ethyl hydroxyacetate, butyl glycolate, methyl lactate, propyl lactate, butyl lactate, methyl 3-hydroxypropionate, 3-hydroxypropane Ethyl acetate, propyl 3-hydroxypropionate, butyl 3-hydroxypropionate, methyl 2-hydroxy-3-methylbutanoate, methyl methoxyacetate, ethyl methoxyacetate, methoxy Butyl acetate, methyl ethoxyacetate, ethyl ethoxyacetate, propyl ethoxyacetate, butyl ethoxyacetate, methyl propoxyacetate, ethyl propoxyacetate, propoxyacetic acid Propyl ester, butyl propoxyacetate, methyl butoxyacetate, ethyl butoxyacetate, propyl butoxyacetate, butyl butoxyacetate, 3-methoxybutyl acetate, 2 Methyl methoxypropionate, ethyl 2-methoxypropionate, 2-methoxypropionate, 2-methoxy Butyl propyl propionate, methyl 2-ethoxypropionate, ethyl 2-ethoxypropionate, propyl 2-ethoxypropionate, butyl 2-ethoxypropionate, 2-butoxy Methyl propyl propionate, methyl 2-butoxypropionate, ethyl 2-butoxypropionate, propyl 2-butoxypropionate, butyl 2-butoxypropionate, 3-methoxy Methyl propyl propionate, ethyl 3-methoxypropionate, propyl 3-methoxypropionate, butyl 3-methoxypropionate, methyl 3-ethoxypropionate, 3-ethoxy Ethyl propyl propionate, propyl 3-ethoxypropionate, butyl 3-ethoxypropionate, methyl 3-propoxypropionate, ethyl 3-propoxypropionate, 3-propoxy Propyl propyl propionate, butyl 3-propoxypropionate, methyl 3-butoxypropionate, ethyl 3-butoxypropionate, propyl 3-butoxypropionate, and 3-butyl Butyl oxypropionate and the like.
該酮類溶劑是至少一種選自於由下列所構成群組的溶劑：苯乙酮、甲基-2-己酮、2-辛酮、4-羥基-4-甲基-2-戊酮、1-甲基-2-吡咯啶酮、甲乙酮、環己酮、環庚酮、氮-甲基吡咯烷酮、2-庚酮、3-庚酮，及二丙酮醇。The ketone solvent is at least one selected from the group consisting of acetophenone, methyl-2-hexanone, 2-octanone, 4-hydroxy-4-methyl-2-pentanone, 1-methyl-2-pyrrolidone, methyl ethyl ketone, cyclohexanone, cycloheptanone, nitrogen-methyl pyrrolidone, 2-heptanone, 3-heptanone, and diacetone alcohol.
較佳地，該其他溶劑(B-3)是至少一種選自於由下列所構成群組的溶劑：乙二醇、乙二醇單丁醚，及碳酸丙烯酯。Preferably, the other solvent (B-3) is at least one selected from the group consisting of ethylene glycol, ethylene glycol monobutyl ether, and propylene carbonate.
該聚合物微粒(C-1)是至少一種選自於由下列所構成群組的聚合物：聚乙烯、聚苯乙烯、聚丙烯酸、聚醯胺、聚醯亞胺、聚甲基丙烯酸酯、三聚氰胺、胺基甲酸酯、苯并鳥嘌呤、酚醛樹脂、聚矽氧樹脂、氟化聚合物(例如聚四氟乙烯(Poly-tetrafluoroethylene)或聚偏氟乙烯(Polyvinylidene fluoride))，微粉化纖維素及微粉化蠟(micronised wax)；其中，該聚乙烯之市售商品例如Dupont 公司出品之「Coathylene HX 1681」。較佳地，該聚合物微粒(C-1)是聚四氟乙烯、聚乙烯，或酚醛樹脂。The polymer microparticles (C-1) are at least one polymer selected from the group consisting of polyethylene, polystyrene, polyacrylic acid, polyamine, polyimine, polymethacrylate, Melamine, urethane, benzoguanine, phenolic resin, polyoxyxylene resin, fluorinated polymer (such as poly-tetrafluoroethylene or polyvinylidene fluoride), micronized fiber And micronised wax; among them, commercially available products of the polyethylene such as Dupont The company produced "Coathylene HX 1681". Preferably, the polymer microparticles (C-1) are polytetrafluoroethylene, polyethylene, or a phenolic resin.
較佳地，該無機化合物微粒(C-2)是至少一種選自於由下列所構成群組的化合物：氧化鋁、氟化鈣、氧化硼、氧化鈦、氧化鋯、氯化鉀、氯化鎂、氯化鈣，及氯化鈉。Preferably, the inorganic compound fine particles (C-2) are at least one selected from the group consisting of alumina, calcium fluoride, boron oxide, titanium oxide, zirconium oxide, potassium chloride, magnesium chloride, Calcium chloride, and sodium chloride.
更佳地，該無機化合物微粒(C-2)是氟化鈣、氧化鋁，或氧化硼。More preferably, the inorganic compound fine particles (C-2) are calcium fluoride, aluminum oxide, or boron oxide.
該聚合物微粒(C-1)的粒徑範圍為10 nm至3000 nm，較佳地，該聚合物微粒(C-1)的粒徑範圍為100 nm至2000 nm，更佳地，該聚合物微粒(C-1)的粒徑範圍為500nm至1500nm。The polymer microparticles (C-1) have a particle diameter ranging from 10 nm to 3000 nm, and preferably, the polymer microparticles (C-1) have a particle diameter ranging from 100 nm to 2000 nm, and more preferably, the polymerization The particle size of the fine particles (C-1) ranges from 500 nm to 1500 nm.
該無機化合物微粒(C-2)的粒徑範圍為10 nm至3000 nm，較佳地，該無機化合物微粒(C-2)的粒徑範圍為100nm至2000nm，更佳地，該無機化合物微粒(C-2)的粒徑範圍為500nm至1500nm。The inorganic compound fine particles (C-2) have a particle diameter ranging from 10 nm to 3000 nm, and preferably, the inorganic compound fine particles (C-2) have a particle diameter ranging from 100 nm to 2000 nm, and more preferably, the inorganic compound fine particles The particle diameter of (C-2) ranges from 500 nm to 1500 nm.
上述聚合物微粒(C-1)及該無機化合物微粒(C-2)有助於提升該蝕刻膏組成物的蝕刻速率及蝕刻深度。The above polymer fine particles (C-1) and the inorganic compound fine particles (C-2) contribute to an increase in the etching rate and etching depth of the etching paste composition.
該有機增稠劑(D)是至少一種選自於由下列所構成群組的化合物：水溶性纖維素醚、多醣及水溶性聚合物。The organic thickener (D) is at least one compound selected from the group consisting of water-soluble cellulose ethers, polysaccharides, and water-soluble polymers.
該水溶性纖維素醚是選自於：烷基纖維素，例如纖維素、甲基纖維素，或乙基纖維素等；羥烷基纖維素，例如羥丙基甲基纖維素、羥乙基纖維素，或羥丙基纖維 素等；或是羧烷基纖維素，例如羧甲基纖維素等。The water-soluble cellulose ether is selected from the group consisting of: alkyl cellulose, such as cellulose, methyl cellulose, or ethyl cellulose; hydroxyalkyl cellulose, such as hydroxypropyl methyl cellulose, hydroxyethyl Cellulose, or hydroxypropyl fiber Or the like; or a carboxyalkyl cellulose, such as carboxymethyl cellulose.
該多醣是選自於殼聚醣、藻酸、瓜耳膠、黃原膠，或鼠李聚糖膠(Rhamsan Gum)。The polysaccharide is selected from the group consisting of chitosan, alginic acid, guar gum, xanthan gum, or rhamsan Gum.
該水溶性聚合物是選自於聚乙烯醇、聚乙烯吡咯烷酮(polyvinylpyrrolidone)。The water-soluble polymer is selected from the group consisting of polyvinyl alcohol and polyvinylpyrrolidone.
較佳地，該有機增稠劑(D)是選自於纖維素、聚乙烯吡咯烷酮，或殼聚醣。Preferably, the organic thickener (D) is selected from the group consisting of cellulose, polyvinylpyrrolidone, or chitosan.
該有機酸(E-1)具有C1 至C10 的直鏈或支鏈烷基，且是至少一種選自於由下列所構成群組的酸：烷基羧酸、羥基羧酸及二羧酸。The organic acid (E-1) has a C 1 to C 10 linear or branched alkyl group, and is at least one selected from the group consisting of an alkyl carboxylic acid, a hydroxycarboxylic acid, and a dicarboxylic acid. acid.
該有機酸(E-1)是至少一種選自於由下列所構成群組的酸：草酸、甲酸、乙酸、丙酸、丁酸、戊酸、己酸、庚酸、辛酸、壬酸、癸酸、檸檬酸、一氯乙酸二氯乙酸、三氯乙酸、三氟乙酸、及乳酸。較佳地，該有機酸(E-1)是選自於甲酸、乙酸、或乳酸。The organic acid (E-1) is at least one selected from the group consisting of oxalic acid, formic acid, acetic acid, propionic acid, butyric acid, valeric acid, caproic acid, heptanoic acid, octanoic acid, decanoic acid, hydrazine. Acid, citric acid, monochloroacetic acid dichloroacetic acid, trichloroacetic acid, trifluoroacetic acid, and lactic acid. Preferably, the organic acid (E-1) is selected from the group consisting of formic acid, acetic acid, or lactic acid.
該無機酸(E-2)是至少一種選自於由下列所構成群組的酸：氫氯酸、氫溴酸、氫碘酸、亞磷酸、次磷酸、磷酸、硫酸、亞硫酸、硼酸、偏硼酸，及硝酸。The inorganic acid (E-2) is at least one selected from the group consisting of hydrochloric acid, hydrobromic acid, hydroiodic acid, phosphorous acid, hypophosphorous acid, phosphoric acid, sulfuric acid, sulfurous acid, boric acid, Metaboric acid, and nitric acid.
較佳地，該無機酸(E-2)是選自於硝酸、磷酸，或硫酸。Preferably, the mineral acid (E-2) is selected from the group consisting of nitric acid, phosphoric acid, or sulfuric acid.
該蝕刻膏組成物的黏度範圍為1~500Pa．s，較佳地，該蝕刻膏組成物的黏度範圍為3~300Pa．s，更佳地，該蝕刻膏組成物的黏度範圍為5~200Pa．s。The etching paste composition has a viscosity ranging from 1 to 500 Pa. s, preferably, the composition of the etching paste has a viscosity ranging from 3 to 300 Pa. s, more preferably, the viscosity of the etching paste composition ranges from 5 to 200 Pa. s.
該蝕刻膏組成物的製備方法是將含氟化合物 (A)、溶劑(B)、微粒(C)、有機增稠劑(D)及酸(E)彼此混合，攪拌足夠時間至形成具有觸變性質的黏性糊狀物。攪拌可以在室溫或升溫至合適溫度的情況下進行。The etching paste composition is prepared by using a fluorine-containing compound (A), solvent (B), fine particles (C), organic thickener (D) and acid (E) are mixed with each other and stirred for a sufficient time to form a viscous paste having thixotropic properties. Stirring can be carried out at room temperature or by warming to a suitable temperature.
本發明蝕刻方法，包含：提供一觸控面板，包括一基板，以及一設置於該基板上的氧化矽層或氮化矽層；將如前所述的蝕刻膏組成物絲網印刷於該氧化矽層或氮化矽層上；進行一蝕刻步驟；及進行一清洗步驟。The etching method of the present invention comprises: providing a touch panel comprising a substrate, and a ruthenium oxide layer or a tantalum nitride layer disposed on the substrate; and screen printing the etch paste composition as described above on the oxidized layer On the tantalum layer or the tantalum nitride layer; performing an etching step; and performing a cleaning step.
該基板的材質並沒有特別限制，一般的材質均可以適用。The material of the substrate is not particularly limited, and general materials can be applied.
所謂氧化矽層，除了玻璃或石英的純SiO2 之外，亦包含所有基於SiO2 的系統，包含由SiO2 離散及/或聯結成SiO4 所構成的系統，亦可以含有其他組份。由SiO2 離散及/或聯結成SiO4 所構成的系統可例如焦矽酸鹽、雙矽酸鹽、環矽酸鹽、鏈矽酸鹽、頁矽酸鹽、網矽酸鹽，該其它組份例如鈣、鈉、鋁、鉛、鋰、鎂、鋇、鉀、硼、鈹、磷、鎵、砷、銻、鑭、鋅、釷、銅、鉻、錳、鐵、鈷、鎳、鉬、釩、鈦、金、鉑、鈀、銀、鈰、銫、鈮、鉭、鋯、釹、鐠等元素，且該等元素不限於以氧化物、碳酸鹽、硝酸鹽、磷酸鹽、硫酸鹽及/或鹵化物的形式存在於SiO2 的系統中或作為摻雜元素。The so-called yttrium oxide layer, in addition to pure SiO 2 of glass or quartz, also contains all SiO 2 -based systems, including systems consisting of SiO 2 discrete and/or bonded to SiO 4 , and may also contain other components. Systems consisting of SiO 2 discrete and/or bonded to SiO 4 may be, for example, pyroantimonate, dicaprate, cyclic citrate, stearate, decanoate, reticulate, the other groups Parts such as calcium, sodium, aluminum, lead, lithium, magnesium, barium, potassium, boron, strontium, phosphorus, gallium, arsenic, antimony, bismuth, zinc, antimony, copper, chromium, manganese, iron, cobalt, nickel, molybdenum, Elements such as vanadium, titanium, gold, platinum, palladium, silver, iridium, ruthenium, osmium, iridium, zirconium, osmium, iridium, and the like, and the elements are not limited to oxides, carbonates, nitrates, phosphates, sulfates, and the like. / or the form of a halide is present in the system of SiO 2 or as a doping element.
所謂氮化矽層是指結晶及部分結晶(通常稱為 微晶)系統，包括α-Si3 N4 及β-Si3 N4 改質的Si3 N4 ，及所有結晶及部分結晶的SiNx 及SiNx ：H。除了結晶的氮化矽還可以包含其它元素，諸如硼、鋁、鎵、銦、磷、砷或銻等。The tantalum nitride layer refers to a crystalline and partially crystalline (commonly referred to as microcrystalline) system, including α-Si 3 N 4 and β-Si 3 N 4 modified Si 3 N 4 , and all crystalline and partially crystalline SiN. x and SiN x :H. In addition to the crystalline tantalum nitride, other elements such as boron, aluminum, gallium, indium, phosphorus, arsenic or antimony may be contained.
本發明蝕刻方法並不限於絲網印刷，所屬技術領域具有通常知識者可以通過已知的印刷方法將該蝕刻膏組成物施加到待蝕刻區域上，例如通過移印方法、壓印方法、噴墨印刷方法，或手動印刷等。The etching method of the present invention is not limited to screen printing, and those skilled in the art can apply the etching paste composition to a region to be etched by a known printing method, for example, by a pad printing method, an imprint method, an inkjet method. Printing method, or manual printing.
絲網印刷是透過含有印刷模板的細目絲網或金屬蝕刻絲網與該基板上氧化矽層或氮化矽層的接觸，而將該蝕刻膏組成物轉移至該基板上氧化矽層或氮化矽層來進行該蝕刻步驟。所用的絲網材質並沒有特別限制，通常由塑料或金屬絲製成。Screen printing is carried out by contacting a ruthenium oxide layer or a tantalum nitride layer on the substrate through a fine mesh or metal etching screen containing a printing template, and transferring the etching paste composition to the yttrium oxide layer or nitriding on the substrate. The enamel layer is used to perform the etching step. The material of the screen used is not particularly limited and is usually made of plastic or metal wire.
於應用時，該蝕刻膏組成物可以施加到整個區域，或以合適的方式選擇性地施加到待蝕刻的氧化矽層或氮化矽層表面上，例如使用已知的印刷方法選擇性地施加到需要蝕刻的區域。如果必要的話，可以輸入能量來活化該蝕刻膏組成物，具體作法是將該蝕刻膏組成物於能量下暴露10秒至15分鐘，較佳地是暴露30秒至2分鐘。該蝕刻膏組成物的蝕刻溫度範圍為20至500℃，較佳地為25至400℃，更佳地為30至300℃。When applied, the etch paste composition can be applied to the entire area or selectively applied to the surface of the yttria layer or the tantalum nitride layer to be etched in a suitable manner, for example, selectively applied using known printing methods. To the area where etching is required. If necessary, energy can be input to activate the etch paste composition by exposing the etch paste composition to energy for 10 seconds to 15 minutes, preferably for 30 seconds to 2 minutes. The etching paste composition has an etching temperature in the range of 20 to 500 ° C, preferably 25 to 400 ° C, more preferably 30 to 300 ° C.
當整個區域或在選擇性印刷區域中的蝕刻完成時，可以通過進一步加熱進行摻雜，或使用溶劑或混合溶劑洗去用過的蝕刻膏組成物，或是通過加熱將用過的蝕刻 膏組成物燒除。較佳地，蝕刻完成後以水進行清洗。When the etching in the entire region or in the selective printing region is completed, the doping may be performed by further heating, or the used etching paste composition may be washed away using a solvent or a mixed solvent, or the used etching may be performed by heating. The paste composition is burned off. Preferably, the cleaning is performed with water after the etching is completed.
本發明將就以下實施例來作進一步說明，但應瞭解的是，該實施例僅為例示說明之用，而不應被解釋為本發明實施之限制。The present invention will be further illustrated by the following examples, but it should be understood that this embodiment is intended to be illustrative only and not to be construed as limiting.
<實施例1至9及比較例1至6><Examples 1 to 9 and Comparative Examples 1 to 6>
[實施例1][Example 1]
在一1公升之聚丙烯杯中，於室溫下，加入100重量份的氟化氫銨(A-1)、100重量份的(4-異丙基苯基)甲醇(B-1-3)、100重量份的水(B-2)、300重量份的乙二醇(B-3-1)及30重量份的甲酸(E-1-1)均勻攪拌5分鐘後，在一邊攪拌的同時加入300重量份的聚四氟乙烯(C-1-1)，並攪拌5分鐘最後加入10重量份的纖維素(D-1)，於轉速500rmp下攪拌60分鐘，即可製得實施例1之製備蝕刻膏組成物。100 parts by weight of ammonium hydrogen fluoride (A-1) and 100 parts by weight of (4-isopropylphenyl)methanol (B-1-3) were added to a 1 liter polypropylene cup at room temperature. 100 parts by weight of water (B-2), 300 parts by weight of ethylene glycol (B-3-1), and 30 parts by weight of formic acid (E-1-1) were uniformly stirred for 5 minutes, and then added while stirring. 300 parts by weight of polytetrafluoroethylene (C-1-1), and stirred for 5 minutes, and finally added 10 parts by weight of cellulose (D-1), and stirred at 500 rpm for 60 minutes to obtain Example 1 An etching paste composition is prepared.
[實施例2至9及比較例1至6][Examples 2 to 9 and Comparative Examples 1 to 6]
實施例2至9及比較例1至6是以與實施例1相同的步驟來製備該蝕刻膏組成物，不同的地方在於：改變化學品的種類及其使用量，該化學品的種類及其使用量如表1及表2所示。Examples 2 to 9 and Comparative Examples 1 to 6 were prepared in the same manner as in Example 1 except that the type of the chemical and the amount thereof were changed, and the kind of the chemical and its The usage amounts are shown in Tables 1 and 2.
<檢測項目><test item>
將實施例1至9及比較例1至6的蝕刻膏組成物進行下列檢測，並將結果記錄於表1及表2。The etching paste compositions of Examples 1 to 9 and Comparative Examples 1 to 6 were subjected to the following tests, and the results are reported in Tables 1 and 2.
1.黏度經時安定性測試1. Viscosity stability test
於25℃下，以黏度機分別量測該等蝕刻膏組成物靜置鐘，再分別以黏度機測定靜置後之黏度，記為μ2 ，並依下列公式計算黏度變化率，藉以該等蝕刻膏組成物的評價黏度經時安定性。At 25 ° C, the etching paste composition was measured by a viscosity machine, and the viscosity after standing was measured by a viscosity machine, and recorded as μ 2 , and the viscosity change rate was calculated according to the following formula. The viscosity of the etching paste composition was evaluated for stability over time.
黏度變化率=|μ2 -μ1 |/μ1 ×100%Viscosity change rate=|μ 2 -μ 1 |/μ 1 ×100%
○：黏度變化率<10%○: viscosity change rate <10%
X：黏度變化率≧10%X: viscosity change rate ≧10%
2.塞網測試2. Plug test
將配製好之蝕刻膏組成物，分別使用網印機(東遠科技出品，型號AT-45PA)配合網目數180目/cm2 的網版於室溫下進行網印測試，該網版上具有500μm線寬的印刷圖樣，於重覆五次印刷後，觀察印刷圖樣是否有蝕刻膏殘留的塞網情況發生。The prepared etching paste composition is respectively screen-printed at room temperature using a screen printing machine (produced by Dongwon Technology, model AT-45PA) with a screen mesh of 180 mesh/cm 2 , which has a screen printing test on the screen. The printing pattern of the line width of 500 μm was observed after repeated printing for five times, and it was observed whether or not the printed pattern had a residue of the etching paste remaining.
○：無蝕刻膏殘留○: no etching paste residue
X：有蝕刻膏殘留X: There is etching paste residue
如表1所示，比較例4至6僅使用單一種類的溶劑(B)，黏度經時安定性不佳，且會有塞網問題。比較例1至3是搭配使用兩種溶劑，其中比較例1僅使用水(B-2)及其他溶劑(B-3)，不含有芳香醇類溶劑(B-1)，黏度經時安定性不佳且塞網測試的結果不合乎需求；比較例2未使用水(B-2)，有塞網問題產生；比較例3未使用其他溶劑，黏度經時安定性不佳。As shown in Table 1, Comparative Examples 4 to 6 used only a single type of solvent (B), the viscosity was poor in stability over time, and there was a problem of plugging. Comparative Examples 1 to 3 were used in combination with two solvents, wherein Comparative Example 1 used only water (B-2) and other solvents (B-3), and did not contain an aromatic alcohol solvent (B-1), and the viscosity was stable over time. Poor and the results of the plugging test were not satisfactory; Comparative Example 2 did not use water (B-2), and there was a problem with the plugging net; Comparative Example 3 did not use other solvents, and the viscosity was not stable over time.
實施例1至9的溶劑(B)包括芳香醇類溶劑(B-1)、水(B-2)及其他溶劑(B-3)，該等蝕刻膏組成物黏度經時安定性良好，且用於絲網印刷時不會有塞網問題產生。The solvent (B) of Examples 1 to 9 includes an aromatic alcohol solvent (B-1), water (B-2), and other solvents (B-3), and the etching paste compositions have good viscosity stability over time, and There is no plugging problem when used for screen printing.
綜上所述，本發明蝕刻膏組成物透過選用特定組成的溶劑，黏度經時安定性佳，特別適用於採用絲網印刷的蝕刻方法，且不會有塞網問題產生，故確實能達成本發明之目的。In summary, the etching paste composition of the present invention has a viscosity stability over time by using a solvent having a specific composition, and is particularly suitable for an etching method using screen printing, and there is no problem of plugging the net, so the present invention can be achieved. The purpose of the invention.
惟以上所述者，僅為本發明之較佳實施例而已，當不能以此限定本發明實施之範圍，即大凡依本發明申請專利範圍及專利說明書內容所作之簡單的等效變化與修飾，皆仍屬本發明專利涵蓋之範圍內。The above is only the preferred embodiment of the present invention, and the scope of the present invention is not limited thereto, that is, the simple equivalent changes and modifications made by the patent application scope and patent specification content of the present invention, All remain within the scope of the invention patent.
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| CN109722248A (en) * | 2018-01-03 | 2019-05-07 | 厦门蓝科电子科技有限公司 | A kind of etching paste and preparation method thereof |
| CN110240906A (en) * | 2018-03-07 | 2019-09-17 | 中国科学院苏州纳米技术与纳米仿生研究所 | Group III-V semiconductor etching liquid and its preparation method and application |
| CN110129056B (en) * | 2019-04-08 | 2021-04-06 | 上海舸海科技有限公司 | Etchant composition for integrated circuits |
| CN110218563B (en) * | 2019-06-11 | 2021-04-06 | 厦门市豪尔新材料股份有限公司 | Etching slurry, preparation method and application thereof, and manufacturing method of solar cell |
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| US5965465A (en) * | 1997-09-18 | 1999-10-12 | International Business Machines Corporation | Etching of silicon nitride |
| CN101528884A (en) * | 2006-11-01 | 2009-09-09 | 默克专利股份有限公司 | Etching paste containing particles for silicon surfaces and layers |
| WO2012083082A1 (en) * | 2010-12-15 | 2012-06-21 | Sun Chemical Corporation | Printable etchant compositions for etching silver nanoware-based transparent, conductive film |
| CN102893421A (en) * | 2010-05-21 | 2013-01-23 | 默克专利股份有限公司 | Selectively etching of a carbon nano tubes (cnt) polymer matrix on a plastic substructure |
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| JP5700784B2 (en) * | 2010-12-15 | 2015-04-15 | 株式会社Adeka | Etching solution composition |
| JP5519728B2 (en) * | 2011-05-17 | 2014-06-11 | 富士フイルム株式会社 | Etching method, etching solution used therefor, and method for manufacturing semiconductor device using the same |
| CN102254814B (en) * | 2011-08-16 | 2013-12-25 | 中国科学院电工研究所 | Silicon oxide selective etching solution, preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5965465A (en) * | 1997-09-18 | 1999-10-12 | International Business Machines Corporation | Etching of silicon nitride |
| CN101528884A (en) * | 2006-11-01 | 2009-09-09 | 默克专利股份有限公司 | Etching paste containing particles for silicon surfaces and layers |
| CN102893421A (en) * | 2010-05-21 | 2013-01-23 | 默克专利股份有限公司 | Selectively etching of a carbon nano tubes (cnt) polymer matrix on a plastic substructure |
| WO2012083082A1 (en) * | 2010-12-15 | 2012-06-21 | Sun Chemical Corporation | Printable etchant compositions for etching silver nanoware-based transparent, conductive film |
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