546265 、發明說明(i) (一)幾_背景 〔發_之範疇〕 本發明乃針對鉻遮光層遮光方式之彩鱼濾光片不良 品之再奎回收:_供所需的方法及技術έ 特別以筆_型電腦(Nme Book PC);及工作站(Work StatiM),或移動交通工具之顯示器;或液晶電親所用之彩 色液晶顯示器。該彩色液晶顯示器生產製造所需之重要材 料-鉻遮光層彩色濾光片,其不良品之再生回收使用之方 法茇技術。 〔目前他人的技術〕 使用鉻與鉻化物來作顏色光阻(Cdor Resist)之遮光 方式的顏料分散法彩色濾光片,其製程爲:先將玻璃基板 上之鉻遮光層作格弐化(Patwrnhig:h苒順序的將紅(R); 綠(G);藍(B)三色顏鱼的樹脂格式化(Pattef_g)塗 著上。必要時再將ό/e之二氧化矽(Si02)膜塗佈成膜; 最後氧化銦錫物UTO)透明電極成膜後完成K特開平 9-86968 ;平成9年(1997) 3月31日;住友化學工業提 患)丨晃(特開平1142123 ;卒成11年(1999)2月26曰; 荒川化學工業_出) 最泜由於液晶顯示器(LCD)爲提高大量生產產能, 種璃基板必須大型化)即蔣已形成數個彩色濾光it (C/F) 之大型玻璃基板與同樣畫素電極之Affay玻璃基板模板 (Patteni)灌入液晶組合後而作成。特別指3.0世代以上 之大型玻璃基板。例如:取δ面之彩色濾先片,其不良率 就比以前取一片時6倍不良率大幅度的提高,也就是會產 禺大量不良_彩色濾光片。 546265 A6 B6 五、發明説明(2 ) (請先閲讀背面之注念事項再塡貧本頁) 使彩色濾光片生產時良率提高的方法爲:改善由於彩色 濾光片生產過程中所產生之不良的原因,有微塵粒(Particle) 等混入之不良;白黑點或缺色等之缺點,及玻璃基板不夠平 坦所造成的異常原因•但是要將上述異常完全排除乃非常 困難之事,且若在製造生產過程中採嚴重管理勢必排除的 話,其工業上所需付出成本也絕非有利之事· 因此,爲使彩色濾光片生產過程能達低成本化,就必須 將彩色濾光片之不良基板作處理•使得彩色濾光片之基版 得以再生使用•例如從最上層之ITO,利用鹽酸之酸性水溶 液去光阻處理後再用氫氧化鈉等鹼液去除彩色濾光層之處 理方法•但是用鹽酸酸性之水溶液及鹼液處理法時彩色濾 光層去光阻時間長且彩色濾光層去除的同時也會有侵腐到 玻璃基板等其他素材之問題發生•另外尙有利用乙醇等有 機溶媒與高純度硫酸於高溫下對彩色濾光層剝去之處理法, 但是,由於有機溶媒與高純度硫酸在高溫下處理時去光阻能 力低;將會造成彩色濾光層溶解度降低,而有剝離效果不確 實的情形發生·(特開平9-86968;住友化學工業提出)· 另外,僅使用硫酸之去ITO方式,會導致IT◦剝離不完全 (特開平11-52123;荒川化學工業提出)· (二)·發明槪述 [本發明所欲解決的課題]_ 經濟郎中央標率局员工消費合作社印製 上述所發生的不良彩色濾光片,若用前述的再生技術將 無法再使用·因此,大量昂貴的玻璃基板將於顏色樹脂或鉻 遮光層成膜狀態下被廢棄,無論從環保或經濟的觀點來看都 將是一大問題·爲此,本發明最大目的在於提供再生回收處 理過程中,從不良彩色濾光片再處理時,不使玻璃基板等其 規格(210 X 297公釐) 適用中國國家標準(CNS)甲4 546265 五、發明說明(3) 他素材受侵腐,且能殘留鉻遮光層以利於顏料光阻再塗佈 之彩色濾光片玻璃基板再生回收技術。 〔解決課題的方法〕 發明人團隊硏究後,提出達成上述課題方法之結果, 經以下列所述之特定處理,可達成前述課題之目的此乃本 發明宗旨。 本發明中,第一發明爲:將使用鉻遮光層之彩色濾光 片不良品,經(A)〜(C)製程處理。能使得使用鉻遮光 層之彩色濾光片玻璃基板得以再生使用。 (A) 將彩色濾光片浸泡於三價鐵鹽水溶液或三價鐵鹽水溶 液與硝酸之混合液中的浸泡(DIP)方式製程。 (B) 將彩色濾光片浸泡於硫酸如(A)製程後的浸泡(DIP) 方式製程。 (C) 上述彩色濾光片(B)製程後的毛刷洗淨之製程。 本^發明中另有第二之發明。特徵爲將使用鉻層之彩色 濾光片不良品經以下(B)〜(C)製程之處理,能獲得剩 下格狀鉻遮光層之彩色濾光片玻璃基板再生回收的方法。 (B) 將彩色濾光片浸泡於硫酸之浸泡(DIP)方式製程。 (C) 上述彩色濾光片(B)製程後的毛刷洗淨之製程。 本發明中ITO膜去除時單獨使用硫酸,會有ITO處理 後殘留現象。三價鐵鹽倂用時’可有效去除ΠΌ殘留現象。 (三).發明之詳細說明 〔發明之實際應用〕 適用於本發明之彩色濾光片不良品之定義爲:於玻璃 546265 五、發明說明(4 ) 基板上形成鉻遮光層且將紅(R)綠(G)藍(B)之畫素薄 膜成膜使成爲彩色濾光片;製程中有畫素未著色、晝素間之 分離不順造成滲色,或保護層(OverCoat)之成膜不良造成 平坦性不足、牛頓紋產生,或鉻遮光層與RGB位置不正’ 或ITO未達所定範圍之抗阻値,及製程上由於微塵粒混入造 成之不良品等。但本發明並未適用包括玻璃基板自身所造成 之傷痕或缺陷,若異常原因爲玻璃基板自身或鉻遮光層異常 時較無回收價値,需排除之。 總之,若遮光層爲正常時,該鉻遮光層基板再使用於彩 色濾光片之生產當會對生產廠商成本上較爲有利,此發明乃 針對此,作留下:鉻遮光層玻璃基板之再生回收方法。- ' ‘ ''1 ^ \ ,; ·- - t Θ首先對專利申請範圍第一項之再生回收方法作說明-{ .' · I: 由於彩色濾光片之最上層爲銦錫化合物( ITO)之成膜, 故需先將不良之彩色濾光片浸泡於三價鐵鹽水溶液或三價 鐵鹽水溶液與硝酸之混合液以去除ITO層。 三價鐵鹽水溶液或三價鐵鹽水溶液與硝酸之混合液乃 三價鐵鹽水溶液濃度爲5〜4〇重量%,硝酸濃度爲〇〜60重 量%之水溶液,適用於ITO之蝕刻。 浸泡的溫度爲〇c起用之水溶液沸點範圍,因太低溫 時,浸泡時間過長;太高溫時又因硝酸蒸氣大量發生,於安 全上不利。故一般限制於室溫〜85°c之間浸泡。浸泡時間可 由三價鐵鹽水溶液的溶液濃度與浸泡溫度條件作調整,直至 使IT0膜完全除去而設定之,通常爲數分鐘到數小時。 546265 五 發明說明(5) 由上述方法取得已去除ITO膜之不良彩色濾光片,接 著需去除顏色光阻層(以及保護層0/C層)。 顏色光阻層(以及保護層0/C層),一般爲壓克力系樹 脂與高分子(Polyimide)系樹脂;若爲單純之成膜物,僅 用硫酸就可去除,彩色濾光片用成膜後通常會作加熱理, 故需在硫酸浸泡後再用毛刷洗淨,使能確實去除顏色光阻 層,硫酸浸泡前可先做水洗製程,藉由水洗可防止三價鐵 鹽水溶液等混入硫酸中,各處理液之使用壽命也可延長。 此製程所使用的硫酸濃度爲60重量%以上。基於去 除能力與成本之考量,最好爲70〜98重量%之成分◊ 60 重量%以下時浸泡時間變長,不適於工業上量產使用。 浸泡溫度在常溫以上時,無特殊之限制,但爲使浸泡 時間縮短,可在製程上加熱。而浸泡時間因所用之液體濃 度,去除目的之顏色光阻層之種類,浸泡溫度及毛刷洗淨 條件之不同而異;重點在於考量前述各項條件組合後,能 完全的將顏色光阻層除去爲原則下即可。 本發明乃針對彩色濾光片之製程上不良玻璃基板,使 其經前述之去光阻劑方法,使不良之ITO膜與顏色光阻層 (以及保護層o/c層)從彩色濾光片用玻璃基板上剝去, 留下再生回收之鉻遮光層玻璃基板。彩色濾光片去除不 良膜之玻璃收納方法則較無特殊之限制,例如:將彩色濾 光片的不良基板收納於指定的治具中(Cassette)後再作 浸泡製程也可。而浸泡的同時,也可以作搖動,搭配去光 阻液循環或超音波處理等均可。 546265 五、發明說明(6 ) 毛刷洗淨可以用液晶顯示器(LCD)、或是大規模機體 迴路(LSI)、或彩色濾光片生產製程上所用之附毛刷之洗 淨機且也可經由人手來洗淨。毛刷洗淨所用的毛刷原則上 以柔軟布(Sponze),毛刷,紙輪,布及橡皮板等不會在玻 璃基板上留下傷痕之材料爲基本,無特別限定。另外毛刷 洗淨時,前述去光阻液或水同時灑注在基板上更好,於洗 淨液中實施毛刷洗淨效果會更好。另外毛刷洗淨前作去除 殘留去光阻液之水洗,可使毛刷洗淨效果更佳。之後,再 用純水洗淨;更進一步乾燥後,就可獲得再生回收之附有 鉻遮光層玻璃基板。 以上述再生回收方式得到之附有鉻遮光層玻璃基板可 再投入彩色濾光片生產線之顏料光阻塗佈工程再使用,供 給再使用於彩色濾光片之生產。 Θ接著敘述專利申請範圍第二項之再生回收方法- 彩色濾光片之最上層有銦錫化合物層(ΙΤΟ膜),萁下 方有顏料光阻層(以及o/c層),該成膜不良之彩色濾光片 浸泡於硫酸中,之後再施以毛刷洗淨,其ΙΤΟ層與顏料光 阻層(以及ο/e層)可同時除去。 此製程所用的硫酸,濃度爲60〜95重量%,爲考量其 去除之性能,硫酸濃度最好選擇在70〜90重量%。因硫酸 濃度在60重量%以下時顏料光阻層(以及〇/〇層)之剝離 效果不佳,且硫酸濃度在95重量%以上時ΓΓ0層剝離不確 實。 五、發明說明(7 ) 浸泡之過程方法,浸泡時間,浸泡溫度以及毛刷洗淨 ^程之後等’完全與第一項所述之處理做法相同。 t下針對本發明作一個執行的例子,各個條件均作實驗數 ,化之實例。對本發明作一個更詳盡的說明,各例之百分 比不同,意指重量基準不同。 〈實例1〉. 由彩色濾光片不良品中挑出玻璃基板以及鉻遮光層 無問題者。先將該不良品置於38%,30t之三價鐵鹽水溶 液中浸泡1小時;之後,不改變其濕潤性的情況下,浸泡 於水中洗去過程之硫酸;再以PE製Sponze毛刷在25°C之 水溫的水沖洗下刷洗,接著以25°C水沖洗洗淨,放置於 100°C下乾燥1個小時後即可獲得附有鉻遮光層之再生回 收玻璃基板。再生回收玻璃基板以目視及光學顯微鏡觀察 該玻璃基板之ITO膜與顏料光阻層(以及o/c層)的去除 狀態。另外,用表面粗度計((株)日本真空)對玻璃基 板以及鉻遮光層部分的鈾刻狀態檢測,取玻璃基板以及鉻 遮光層上無傷痕或欠缺等缺點之玻璃檢測。 <實例2〜6以及比較例1〜11 > 表1所示爲實施例1 -其他實施例之評價結果。其他 實施例之條件,如表1所示,在去光阻劑之組成比或去光 阻成分,處理溫度略作變化’其他條件同實施例1。 546265 A6 B6 五、發明説明(8 ) <ITO剝離能力,去光阻剝離能力> 將彩色濾光片用玻璃基板的ΙΤΟ層及顏料光阻層之去 光阻效能,用顯微鏡(約50倍)作目視判定,定出以下供參考 基礎之判斷基準·546265, Description of the invention (i) (一) Several backgrounds [This category] This invention is aimed at the recovery of the defective products of the color fish filter of the chromium light-shielding method: _ the method and technology required In particular, pen-type computers (Nme Book PC); and workstations (Work StatiM), or mobile vehicle displays; or color LCD monitors used by LCD pro. The important material required for the manufacture of this color liquid crystal display-the chromium light-shielding layer color filter, and the method and technology for the recycling of defective products. [Current technology of others] The pigment dispersion method color filter using chromium and chrome compounds as a light shielding method for color photoresist (Cdor Resist), the process is as follows: first, the chromium light shielding layer on the glass substrate is formatted ( Patwrnhig: h 苒 order red (R); green (G); blue (B) resin-colored (Pattef_g) coating. If necessary, SiO / SiO2 (Si02) Film coating and film formation; Finally, indium tin oxide (UTO) transparent electrode is completed after completion of K JP 9-86968; Heisei 9 (1997) March 31; Sumitomo Chemical Industries raises concerns) 丨 Akira (JP 1142123; 11 years (1999) February 26th; Arakawa Chemical Industry_out) Mostly, in order to increase the mass production capacity of liquid crystal displays (LCDs), the glass substrate must be large.) That is, Jiang has formed several color filters it ( C / F) large glass substrate and Affay glass substrate template (Patteni) with the same pixel electrode are produced by pouring liquid crystal into a combination. Particularly refers to large glass substrates of 3.0 generations and above. For example, if the color filter of the δ plane is taken first, the defect rate is greatly increased by 6 times compared with the previous one, that is, a large number of defective_color filters will be produced. 546265 A6 B6 V. Description of the Invention (2) (Please read the notes on the back before diluting this page) The method to improve the yield of color filter production is: to improve the color filter production process. The reasons for the defects include the incorporation of fine particles (Particles), the disadvantages of white and black spots or lack of color, and the cause of abnormalities caused by the flatness of the glass substrate. However, it is very difficult to completely eliminate the above abnormalities. And if serious management in the manufacturing process is bound to exclude it, the industrial cost is definitely not a good thing. Therefore, in order to reduce the cost of the color filter production process, the color filter must be The bad substrate of the film is processed. • The base plate of the color filter can be reused. • For example, from the top layer of ITO, the acidic aqueous solution of hydrochloric acid is used to remove the photoresist treatment, and then the color filter layer is removed by an alkali solution such as sodium hydroxide. Treatment method • However, when the acidic aqueous solution of hydrochloric acid and alkaline solution are used for treatment, the color filter layer has a long photoremoval time and the color filter layer is removed. At the same time, it will also invade the glass substrate, etc. Problems with the material • In addition, there is no treatment method that uses an organic solvent such as ethanol and high-purity sulfuric acid to strip the color filter layer at high temperature. However, the organic solvent and high-purity sulfuric acid have low photoresistance removal ability when processed at high temperature. ; It will cause the solubility of the color filter layer to decrease, and the peeling effect may be insecure. (Japanese Patent Application Laid-Open No. 9-86968; proposed by Sumitomo Chemical Industries). In addition, the use of sulfuric acid to remove ITO will cause IT. Complete (Japanese Patent Application Laid-Open No. 11-52123; proposed by Arakawa Chemical Industries) · (II) · Description of Invention [Problems to be Solved by the Invention] Sheet, it can no longer be used if the aforementioned recycling technology is used. Therefore, a large number of expensive glass substrates will be discarded when the color resin or chrome light-shielding layer is formed. This will be a big problem from an environmental or economic point of view. For this reason, the main purpose of the present invention is to provide a glass substrate and other specifications (210 X 297 mm) when reprocessing from a defective color filter during the recycling process. ) Applies China National Standard (CNS) A five 4,546,265, described invention (3) involvement he rot material, and can facilitate the residual chromium light-shielding layer of the color filter glass substrate and then photoresist coating pigments of recuperation technique. [Methods of Solving the Problem] After researching by the inventor team, the results of the method for achieving the above-mentioned problems are proposed, and the above-mentioned problems can be achieved by the specific treatment described below. This is the object of the present invention. In the present invention, the first invention is that a defective color filter using a chromium light-shielding layer is processed through (A) to (C). The color filter glass substrate using the chromium light-shielding layer can be reused. (A) A process of immersion (DIP) in which a color filter is immersed in an aqueous solution of a ferric iron salt or a mixed solution of a ferric iron salt solution and nitric acid. (B) The immersion (DIP) process after immersing the color filter in sulfuric acid such as (A). (C) The process of brush cleaning after the above-mentioned color filter (B). There is another second invention in the present invention. It is characterized by the method of regenerating the color filter glass substrate with the remaining grid-shaped chromium light-shielding layer by processing the defective color filter using the chromium layer through the following processes (B) to (C). (B) The process of dipping the color filter in sulfuric acid (DIP). (C) The process of brush cleaning after the above-mentioned color filter (B). In the present invention, sulfuric acid is used alone when removing the ITO film, and there is a residual phenomenon after ITO treatment. Trivalent iron salt can effectively remove the residual phenomenon of ΠΌ. (3) Detailed description of the invention [Practical application of the invention] The definition of the defective color filter suitable for the present invention is: on glass 546265 5. Description of the invention (4) A chromium light-shielding layer is formed on the substrate and red (R ) Green (G) Blue (B) pixel film is formed into a color filter; in the process, there are uncolored pixels, irregular separation between pixels, which causes bleeding, or poor film formation of the protective layer (OverCoat). It may result in insufficient flatness, Newtonian texture, or the position of the chrome shading layer and RGB is not correct, or the resistance of ITO is less than the specified range, and the defective products caused by the incorporation of dust particles in the process. However, the present invention is not applicable to include the flaws or defects caused by the glass substrate itself. If the abnormality is caused by the abnormality of the glass substrate itself or the chrome shading layer, there is no recovery price, which needs to be ruled out. In short, if the light-shielding layer is normal, reusing the chromium light-shielding layer substrate for the production of color filters will be more cost-effective for manufacturers. This invention aims at this, leaving: Recycling method. -'' '' 1 ^ \ , ·--t Θ First of all, we will explain the recycling method of the first item in the scope of patent application- {. '· I: Because the top layer of the color filter is indium tin compound (ITO ) Film formation, it is necessary to first immerse the defective color filter in a trivalent iron salt aqueous solution or a mixed solution of a trivalent iron salt aqueous solution and nitric acid to remove the ITO layer. The trivalent iron salt aqueous solution or a mixed solution of the trivalent iron salt aqueous solution and nitric acid is an aqueous solution containing a trivalent iron salt aqueous solution having a concentration of 5 to 40% by weight and a nitric acid concentration of 0 to 60% by weight, and is suitable for etching of ITO. The immersion temperature is within the boiling point range of the aqueous solution used at 0 ° C. When the temperature is too low, the immersion time is too long; when the temperature is too high, a large amount of nitric acid vapor occurs, which is disadvantageous for safety. Therefore, it is generally limited to immersion between room temperature and 85 ° c. The immersion time can be adjusted by the solution concentration of the ferric iron salt solution and the immersion temperature conditions until the IT0 film is completely removed, and it is usually several minutes to several hours. 546265 5 Description of the invention (5) Obtain the defective color filter from which the ITO film has been removed by the above method, and then remove the color photoresist layer (and the protective layer 0 / C layer). The color photoresist layer (and the protective layer 0 / C layer) is generally acrylic resin and polymer (Polyimide) resin; if it is a simple film-forming product, it can be removed only with sulfuric acid, and used for color filters After film formation, it is usually heated, so it needs to be washed with a brush after soaking in sulfuric acid to ensure the removal of the color photoresist layer. The water washing process can be performed before soaking in sulfuric acid. Water washing can prevent the trivalent iron salt aqueous solution. When mixed into sulfuric acid, the service life of each treatment liquid can be extended. The sulfuric acid concentration used in this process is 60% by weight or more. Based on the consideration of removal capacity and cost, it is best to use 70 to 98% by weight of ingredients. When the weight is below 60% by weight, the soaking time becomes longer, which is not suitable for industrial mass production. When the immersion temperature is above normal temperature, there are no special restrictions, but in order to shorten the immersion time, it can be heated in the manufacturing process. The immersion time varies depending on the concentration of the liquid used, the type of color photoresist layer to be removed, the immersion temperature, and the cleaning conditions of the brush; the key point is that after considering the combination of the foregoing conditions, the color photoresist layer can be completely It can be removed under the principle. The present invention is directed to the defective glass substrate in the process of color filter, so that the defective ITO film and the color photoresist layer (and the protective layer o / c layer) are removed from the color filter through the aforementioned photoresist removing method. The glass substrate was peeled off, leaving the chrome light-shielding layer glass substrate that was recycled. There are no special restrictions on the glass storage method for removing the defective film from the color filter. For example, the defective substrate of the color filter can be stored in a specified fixture (Cassette) and then immersed. While soaking, it can also be shaken. It can be used with photoresist circulation or ultrasonic treatment. 546265 V. Description of the invention (6) Brush cleaning can be done with liquid crystal display (LCD), large-scale body circuit (LSI), or color filter production process with brush cleaning machine Wash by hand. In principle, the brushes used for cleaning the brushes are based on materials such as soft cloths (sponze), brushes, paper wheels, cloths, and rubber plates that do not leave scratches on the glass substrate, and are not particularly limited. In addition, when the brush is cleaned, it is better to spray the aforementioned photoresist solution or water on the substrate at the same time, and it is better to perform the brush cleaning in the cleaning solution. In addition, the brush is washed with water to remove the residual photoresist solution before washing, which can make the brush better. After that, it was washed with pure water; after further drying, a recycled glass substrate with a chromium light-shielding layer was obtained. The glass substrate with a chromium light-shielding layer obtained by the above-mentioned recycling method can be re-used in the pigment photoresist coating process of a color filter production line for reuse in the production of color filters. Θ Next describes the second recycling method of the scope of the patent application-the top layer of the color filter has an indium tin compound layer (ITO film), and the pigment photoresist layer (and o / c layer) under the 萁, the film formation is poor The color filter is immersed in sulfuric acid, and then washed with a brush. The ITO layer and the pigment photoresist layer (and ο / e layer) can be removed at the same time. The concentration of sulfuric acid used in this process is 60 to 95% by weight. In consideration of its removal performance, the concentration of sulfuric acid is preferably selected to be 70 to 90% by weight. When the sulfuric acid concentration is 60% by weight or less, the peeling effect of the pigment photoresist layer (and the 0/0 layer) is not good, and when the sulfuric acid concentration is 95% by weight or more, the peeling of the ΓΓ0 layer is not sure. V. Description of the invention (7) The method of soaking, the soaking time, the soaking temperature, and the cleaning process of the brush, etc. are completely the same as the treatment method described in the first item. An example of implementation of the present invention is given below t, and each condition is an example of experiment number. For a more detailed explanation of the present invention, the percentages of the examples are different, which means that the weight basis is different. <Example 1> The glass substrate and the chrome shading layer were selected from the defective color filters. First immerse the defective product in a 38%, 30t trivalent iron salt solution for 1 hour; then, immerse it in water without changing its wettability to remove sulfuric acid during the process; then use a PE-made Sponze brush to Rinse under 25 ° C water temperature, then rinse with 25 ° C water. After drying at 100 ° C for 1 hour, a recycled glass substrate with a chromium light-shielding layer can be obtained. The state of removal of the ITO film and the pigment photoresist layer (and the o / c layer) of the glass substrate was observed with a visual and optical microscope. In addition, the surface roughness meter (Japan Vacuum Co., Ltd.) was used to detect the uranium engraved state of the glass substrate and the chrome shading layer, and the glass substrate and the chrome shading layer were inspected without any flaws or defects. < Examples 2 to 6 and Comparative Examples 1 to 11 > Table 1 shows the evaluation results of Example 1-other examples. The conditions of the other examples are shown in Table 1. The composition temperature of the photoresist removing agent or the photoresist removing component is slightly changed. The other conditions are the same as those of the first embodiment. 546265 A6 B6 V. Explanation of the invention (8) < ITO peeling ability, photoresistance peeling ability > The photoresist removal efficiency of the ITO layer of the color filter glass substrate and the pigment photoresist layer was measured with a microscope (about 50 Times) Make a visual judgment and determine the following judgment criteria for reference.
◎ ΔX 確實的剝離成功 稍許殘留· 大部分殘留· <鉻遮光層玻璃基板的狀態> 將彩色濾光片用玻璃基板的鉻遮光層以及玻璃基板部 之蝕刻效能,用顯微鏡(約50倍)作目視判定,定出以下供參 考基礎之判斷基準· 鉻遮光層◎ ΔX has been peeled off successfully. Most of the residues remain. ≪ State of the glass substrate of the chromium light-shielding layer > The etching efficiency of the chromium light-shielding layer of the glass substrate for color filters and the glass substrate portion was measured with a microscope (about 50 times ) Make a visual judgment and determine the following reference standards for reference. Chromium shading layer
◎ ΔX 鉻遮光層蝕刻量10Α以下· 鉻遮光層蝕刻量10〜100又· .絡遮光層餓刻量ιοοΑ以上· 玻璃基板部◎ ΔX Etching amount of chromium light-shielding layer is 10A or less. Etching amount of chromium light-shielding layer is 10 to 100..
◎ ΔX 玻璃基板蝕刻量10A以下· 玻璃基板蝕刻量10〜ιοοΑ · 玻璃基板蝕刻量100又以上 <表一實測値參考下頁: (請先閲讀背面.^注念事項再塡寫本頁,) 部 中 央 標 準 消 沓 谷 作 本紙张尺度適用中國國家標準(CNS)甲4規格(210 X 297公釐) 546265 五、發明說明(9) m II〜1爹鎰另9〜I Ms?« 基板的狀態 玻璃基板 ◎ ◎ ◎ ◎ ◎ ◎ ◎ ◎ ◎ ◎ X ◎ ◎ ◎ ◎ ◎ ◎ 鉻遮光層 ◎ ◎ ◎ ◎ ◎ ◎ X ◎ ◎ ◎ ◎ ◎ ◎ ◎ ◎ ◎ 除去的效果 光阻 剝離性 ◎ ◎ ◎ ◎ ◎ ◎ ◎ ◎ ◎ ◎ ◎ X X X X X X ITO 剝離性 ◎ ◎ ◎ ◎ ◎ ◎ ◎ ◎ X X ◎ ◎ ◎ ◎ ◎ ◎ ◎ 毛刷 洗淨 有無 碟 顏色光阻(保護層)去光阻 1 ^ rH rH r-t τΗ r-H rH rH rH rH rH rH rH ▼Η rH 溫度 ec S S S S S s s S 成份 wt% 8 g? 〇 8 rH 8 rH 8 S 成份 硫酸 硫酸 硫酸 硫酸| ___1 硫酸 硫酸 硫酸 硫酸 i硫酸 硫酸 苟性鹼 硝酸 1 丙酮 硫酸 硫酸 硫酸 氧化銦錫物剝離條件 1 ^ rH r-H r-i rH rH τΗ rH rH 1—^ 1—ί r—ί r-4 rH rH rH 溫度 °c S SS S S S 8 s S 8 s 氧化銦錫物(ITO)去光阻劑 成份B wt% 1 1 1 I LO CO 1 1 1 1 1 I 1 i 1 成份A wt% S 1〇 % 2 Ξ S s ?S S s 成份 B ! 1 1 ! 硝酸 硝酸1 t 鹽酸 1 1 丨 i 1 1 1 1 1 成份A 三價鐵鹽 三價鐵鹽 三價鐵鹽 三價鐵鹽 三價鐵鹽 三價鐵鹽 鹽酸 i三價鐵鹽 硝酸 硝酸 三價鐵鹽 三價鐵鹽 三價鐵鹽 三價鐵鹽 三價鐵鹽 三價鐵鹽 三價鐵鹽 實施例1 實施例2 實施例3 實施例4 實施例5 ________________1 實施例6 比較例1 比較例2 比較例3 比較例4 比較例5 比較例6 比較例7 j 比較例8 比較例9 比較例10 比較例11 裝 —訂 546265 B6 五、發明説明(1〇) <實例7> 由彩色濾光片不良品中挑出玻璃基板以及鉻遮光層無 問題者•先將該不良品至於30°C,9〇%之硫酸中浸泡1小時; 之後,不改變其濕潤性的情況下,移改於25°C水中沖洗去硫酸; 再以PE製Spcmze毛刷在25°C之純水沖洗下刷洗,接著以25°C 水沖洗洗淨,放置於l〇〇°C下乾燥1個小時後即可獲得附有鉻遮 光層之再生回收玻璃基板·再生回收玻璃基板以目視及光學顯 微鏡觀察該玻璃基板之ITO膜與顏料光阻層(以及〇/c層)的去 除狀態•另外,用表面粗度計((株)日本真空)對玻璃基板以 及鉻遮光層部分的蝕刻狀態檢測,取玻璃基板以及鉻遮光層 上無傷痕或欠缺等缺點之玻璃檢測· <實例8〜10以及比較例12〜15> 表2所示爲實施例7與其他實施例之評價結果•其他 實施例之條件,如表1所示,在去光阻劑之組成比或去光阻 成分,處理溫度略作變化,其他條件同實施例7 · 表2實測値 請 先 閲 面 之- 注 % 事 寫. 本 I. tk 濟 部 中 央 標 準 局 η 工 消 备 社 印 *製 實施例7〜10比較例12〜L5 _顏色光阻(保護層)去光阻劑 洗淨 除去的效果 基板的狀態 成份 成份 wt% 溫度 °c 時間 hr 效果 IT0 剝離性 光阻 剝離性 鉻 遮光層 基板 實施例-7 _硫酸 90 30 1 有 〇 ◎ ◎ ◎ 實施例-8 硫酸 90 50 1 有 ◎ 〇 ◎ 〇 實施例-9 硫酸 80 ao 1 有 〇 〇 〇 ◎ 實施例-10 硫酸 _70 30 1 有 〇 ◎ 〇 ◎ 比較例-12 硫酸 98 30 1 有 X 〇 〇 ◎ 比較例-13 硫酸 90 30 1 無 ◎ X 〇 〇 比較例-14 硫酸 90 一· , 50 1 無 〇 X ◎ 〇 比較例-15 硫酸— 50 ^----- 30 1 有 〇 X 〇 ◎ 本紙張从適用中國國家標準(CNS)甲4規格(21G χ 297公货) 546265 A6 B6 五、發明説明(11 ) (請先閲讀背面t注念事項再敬寫本K-) [發明之成果] 經過本發明之處理,可將彩色濾光片之不良玻璃基板在 不侵腐玻璃基板等其他素材的情況下,確實有效率的能將 ITO層及顏料光阻層(以及ο/e層)剝去,提供出鉻遮光層 之彩色濾光片用再生回收基板,能再次的供予彩色濾光片廠 商生產使用,對於彩色濾光片大量生產成本之降低有莫大功 勞•此外,在日益艱困之環境保護政策下,也能爲國內減少 玻璃,重金屬等高污染性產業廢棄物,成效可謂一舉數得 [簡單的圖面說明] <圖 1·> 鉻遮光層之彩色遮光片斷面圖· <符號說明> 1.玻璃基板 2·鉻遮光層(Black/Matrix) 3·彩色濾光層(顏料光阻膜) 4. (0/C 層),Ovgr Coat 二氧化矽層,Si〇2 層 5·銦錫化合物(ITO膜) 部 中 央 標 準 沓 谷 社 印 •製 本紙張尺及適用中國國家標準(CNS)甲4規格(210 X 297公资) 546265 五、發明說明(12)中英文名詞對照:◎ ΔX glass substrate etched less than 10A · glass substrate etched 10 ~ ιοοΑ · glass substrate etched 100 or more < Table 1 actual measurement 値 Refer to the next page: (Please read the back. ^ Notes before writing this page, ) The central standard eliminates the grain size of the paper. The paper size is applicable to the Chinese National Standard (CNS) A4 specification (210 X 297 mm) 546265. 5. Description of the invention (9) m II ~ 1 father and 9 ~ I Ms? « State glass substrate ??? rH rH rH rH rH rH rH ▼ Η rH Temperature ec SSSSS ss S Ingredient wt% 8 g? 〇8 rH 8 rH 8 S Ingredient sulfuric acid sulfuric acid sulfuric acid sulfuric acid | ___1 sulfuric acid sulfuric acid Acid sulfuric acid i sulfuric acid sulfuric acid alkali alkali nitric acid 1 acetone sulfuric acid sulfuric acid sulfuric acid indium tin oxide stripping conditions 1 ^ rH rH ri rH rH τΗ rH rH 1— ^ 1—ί r—ί r-4 rH rH rH temperature ° c S SS SSS 8 s S 8 s Indium tin oxide (ITO) photoresist component B wt% 1 1 1 I LO CO 1 1 1 1 1 I 1 i 1 Component A wt% S 10% 2 Ξ S s? SS s ingredient B! 1 1! nitric acid nitric acid 1 t hydrochloric acid 1 1 丨 i 1 1 1 1 1 1 ingredient A trivalent iron salt trivalent iron salt trivalent iron salt trivalent iron salt trivalent iron salt hydrochloric acid i three Valence iron salt Nitrate nitrate Trivalent iron salt Trivalent iron salt Trivalent iron salt Trivalent iron salt Trivalent iron salt Trivalent iron salt Trivalent iron salt Example 1 Example 2 Example 3 Example 4 Example 5 ________________1 Implementation EXAMPLE 6 COMPARATIVE EXAMPLE 1 COMPARATIVE EXAMPLE 2 COMPARATIVE EXAMPLE 3 COMPARATIVE EXAMPLE 4 COMPARATIVE EXAMPLE 5 COMPARATIVE EXAMPLE 6 COMPARATIVE EXAMPLE 7 J COMPARATIVE EXAMPLE 8 COMPARATIVE EXAMPLE 9 COMPARATIVE EXAMPLE 10 COMPARATIVE EXAMPLE 11 Binding—Binding 546265 B6 V. Description of the Invention (1〇) & lt Example 7 > Pick out the glass substrate and the chrome light-shielding layer from the defective color filter. 30 ° C, soaked in 90% sulfuric acid for 1 hour; afterwards, without changing its wettability, transfer to 25 ° C water to rinse the sulfuric acid; then use a PE-made Spcmze brush at 25 ° C pure water Brush under washing, then rinse with 25 ° C water, and place at 100 ° C to dry for 1 hour to obtain recycled recycled glass substrate with chromium light-shielding layer. Recycled recycled glass substrate for visual and optical microscope Observe the removal status of the ITO film and pigment photoresist layer (and 〇 / c layer) of the glass substrate. In addition, use a surface roughness meter (Nippon Vacuum Co., Ltd.) to detect the etching status of the glass substrate and the chrome shading layer. Glass inspection without defects such as flaws or defects on the glass substrate and the chromium light-shielding layer. ≪ Examples 8 to 10 and Comparative Examples 12 to 15 > Table 2 shows the evaluation results of Example 7 and other examples. Other Examples The conditions are as shown in Table 1. The composition temperature of the photoresist remover or photoresist removal component is slightly changed. The other conditions are the same as those in Example 7. · Table 2 is measured. Please read the above-Note% Write . I. tk Central Bureau of Standards, Ministry of Economic Affairs Example 7 to 10 produced by Bisha * Comparative Example 12 to L5 _ Color photoresist (protective layer) removal effect of photoresist cleaning and removal of the substrate state component content wt% temperature ° c time hr effect IT0 peeling photoresist Example of a peelable chromium light-shielding layer substrate -7 sulfuric acid 90 30 1 Yes ○ ◎ ◎ Example -8 sulfuric acid 90 50 1 Yes ◎ ○ ◎ Example -9 sulfuric acid 80 ao 1 Yes 〇〇〇 ◎ Example -10 Sulfuric acid_70 30 1 Yes 〇 ◎ 〇 ◎ Comparative Example-12 Sulfuric acid 98 30 1 Yes X 〇〇 ◎ Comparative Example-13 Sulfuric acid 90 30 1 No ◎ X 〇〇Comparative Example-14 Sulfuric acid 90 -1, 50 1 No 〇X ◎ 〇 Comparative Example-15 Sulfuric acid — 50 ^ ----- 30 1 Yes 〇X ○ ◎ This paper is from China National Standard (CNS) A4 specification (21G χ 297 public goods) 546265 A6 B6 V. Description of the invention ( 11) (Please read the note on the back t before writing this K-) [Achievements of the invention] After the treatment of the present invention, the defective glass substrate of the color filter can be used without damaging the glass substrate and other materials. , Indeed, it can effectively make ITO layer and pigment photoresist layer And ο / e layer) peeled off, providing a recycled recycling substrate for color filters that provides a chromium light-shielding layer, which can be re-used by color filter manufacturers for production. It has contributed a lot to reducing the cost of mass production of color filters. • In addition, under the increasingly difficult environmental protection policy, it can also reduce the waste of highly polluting industries such as glass and heavy metals in China. The effect can be described in one fell swoop [simple illustration] < Figure 1 · > Chrome shading Layered view of colored light-shielding fragments · < Description of symbols > 1. Glass substrate 2 · Chrome light-shielding layer (Black / Matrix) 3 · Color filter layer (pigment photoresist film) 4. (0 / C layer), Ovgr Coat Silicon dioxide layer, Si〇2 layer 5. Indium tin compound (ITO film) Ministry of Standards printed by Kariya Co., Ltd. • Paper ruler and applicable Chinese National Standard (CNS) A4 specification (210 X 297 public capital) 546265 5. Description of the invention (12) Comparison of Chinese and English nouns:
彩色濾光片- Color Filter 黑色遮光膜- Black Matrix 顏色光阻- Color Resist 格式化- Patterning 保護膜- o/c 二氧化砂- Sio2 氧化銦錫物- ITO 電樞- Array 微塵粒- Particle 液晶顯示器- LCD ( Liquid Chrystal Display ) 浸泡- DIPColor Filter-Color Filter-Black Matrix-Black Matrix Color Resistor-Color Resist Formatting-Patterning Protective Film-o / c Sand Dioxide-Sio2 Indium Tin Oxide-ITO Armature-Array Dust Particles-Particle LCD -LCD (Liquid Chrystal Display) immersion-DIP