TWI290634B - Manufacturing method of crystallined optical film with nano-sols - Google Patents

Manufacturing method of crystallined optical film with nano-sols Download PDF

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TWI290634B
TWI290634B TW94111397A TW94111397A TWI290634B TW I290634 B TWI290634 B TW I290634B TW 94111397 A TW94111397 A TW 94111397A TW 94111397 A TW94111397 A TW 94111397A TW I290634 B TWI290634 B TW I290634B
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nano
film
sol
optical
coating
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TW94111397A
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TW200636276A (en
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Jung-Jie Chen
Jeng-Jie Jang
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Nano Tech Chemical & System Lt
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Abstract

This invention relates to a manufacturing method of a crystallined optical film with nano-sols, forming the film by recoating on a surface of a substrate, i.e. a plastic material (including acrylics, polycarbonate, polystyrene and their derivatives) or glass by utilizing nanopowder sols with different index of refraction so as to form an optical film layer with particular optical characteristics. The manufacturing method utilizes a particular process to coat the surface of the processed substrate uniformly with a chosen nanopowder sol with crystallined metal oxide to form a film, which has a particular index of refraction, a compact structure, good absorption and complies with the preset thickness, on the surface of the substrate by utilizing a configured procedure of baking or microwaving, then repeat the above mentioned steps with a nanopowder sol with crystallined metal oxide having another index of refraction to form a film of another particular index of refraction on the original film so as to form the optical film layer of the particular optical characteristic on the processed substrate. Finally, the optical layer is finished with a protective membrane as needed. The optical film layer, depending on how its surface treatment, has various optical characteristics such as anti-reflection, anti-dazzling, semi-transmitting, blocking of ultraviolet transmitting and high-reflection, in addition, it has effects of being smooth on surface, less contaminated, highly light transmissive, highly absorptive, antistatic, and resistant to friction and scraping.

Description

1290634 九、發明說明: • 【發明所屬之技術領域】 本發明-種光學顏晶型絲轉製造法,是卵結晶型太 米溶膠製造光學膜的新流程,其作法是將結晶型二氧化鈦太米二 體溶膠(形成高折射率)及結晶型氧化銘、結晶型二氧化石夕奈 溶膠(形成低折射率)分別依設定程序’均勻塗佈於被處^材剩" 括壓克力、聚碳酸、聚苯乙稀及其衍生材料)表面/玻璃表面,並= 已元成的光學鍵膜層上依需要作保護膜處理,再經設定的妈^戈 • 微波處理程序後,即在被處理材料表面形成厚度合乎設定f吸= 良好而結構緻密、具特定光學特性的薄膜;更直接說,本發明是 利用設定化學處理程序,將二氧化鈦及二氧化矽、氧化鋁^兩= 不同折射率結晶型奈米粉體溶膠分別依設定程序,均勻塗佈於被 處理材料表面,並依需要進行特定的保護膜處理後,再經特定的 烘烤或微波處理程序後,使得奈米粉體溶膠轉化成吸附良好^緻 密的光學薄膜;所形成的光學薄膜,依其塗佈程序,分別具有抗 反射、抗眩光、半透射、防紫外光穿透、高反射等光學特性外二 瞻更有表面光滑、不易積垢、高透光度、高吸附力、抗靜電、耐磨、 耐刮等作用。 【先前技術】 基本上,光學鍍膜元件皆是由高、低折射率的光學膜層交互 堆疊形成,以達到特定的光學功能需求,由於,高、低折射率的 材料有限,在無機光學膜層多採二氧化矽、二氧化鈦為材料,至 於生產方式,目前工業界所用的光學膜製造,皆採用真空蒸鍍的 1290634 方式’基本上真空蒸鍍量產光學膜,已是成_生產製程,其產 品品質也相當安定,但是,真空蒸鍍量產製程本身相當多的問題 及限制,包括設備投資金額昂f、產量低、被鍍元件形狀必需固 疋、被鍍70件形狀不得有關、非平面元件光學膜厚度不均句等 問題’這些問題,在面對產品錄化的趨勢要求下及成本下降的 壓力時,造成真空蒸鍍量產製程,愈來愈有量產可行性的疑慮, 在此狀況下,_光學難作方法㈣求性日益提高,其主要作 法有兩大類··有機膜合成法及無機膜塗佈法; 有機膜合成法,主要是朗高分子聚合_光學特性,包括 U. S. Patent 6, 680, 899 ^ ^ silicon lubricant A Fluoro lubricant搭配而成的多層膜;中華民國專利第578〇16號,利用 射出成形,非晶態熱可塑型樹脂;中華民國專利第575_號,利 用低壓氣相沉積方式形成的有機膜;中華民國專利第572937號, _ 則以&成方式’產生環酯類聚亞醯胺薄膜;中華民國專利第166683 號,是以PDD高分子膜重複黏貼,形成不眩光的多層膜等皆屬於 此類’有機膜主要著重於光學特性,而不耐磨、祕為其共同缺 點此外’產品哥命短,亦是其推展的瓶頸所在,而有機膜合成 法的内容,皆和本發明無關; 無機膜部份,-般多以真空蒸鑛或濺鍍的方式進行多層膜的 合成’其中真空蒸鍍部份,包括中華民國專利第1223009號,利 用真空療鑛的方式將氟化約(CaFO和二氧化鈦(Ti〇2)分次成膜, 1290634 *成’、撥水功摘光學膜;中華民國專利第棚226號,則以真空 i鍍的方式將氟蝴(泌)和二氧切⑶⑹分:欠成膜,亦形 成'、撥水功恥的光學膜;中華民國專利第584742號,則利用真空 1谱的方式將氧化錯(聽)和二氧化♦⑶⑹分次成膜,形成 ’、;慮光作用的多層膜;中華民國專利第54_號,則直接利用真 空蒸鍍的方式將二氧化鈦⑽d形成高反賴 ;濺鍍部份,則有 春中華民國專利第侧⑷虎,以濺鑛方式將二氧化鈦⑽2) 和二 氧化夕(Si〇2)分次附著於基材表面,再經高溫燒結,形成低耗磨 的光學膜:·中華民國專利第122402號,以濺鍍方式石夕氧化物(Siia ne)和一氧化石夕(咖)在基材表面形成保護膜 ,以補強塑膠基材 不耐磨、易髒的特性,就真空蒸鍍或麟的生產應用而言,皆屬 録的生產技術,但設備成本高、產出效率低、處理元件的形狀 必而固疋(否則必需另作模具,而模具費用高昂。)、處理元件的 _ I狀不得有凹凸或死㈣,為其制継,但不管如何,真空蒸 鍍及錢鍍製作乡層朗方式,皆和本發明無關; 目刖也有業界’以奈米粉體溶廣彡成多層賴方式在推廣中, 但其所使用的“奈米粉體溶膠,,,係所謂“反應型奈米粉體溶膠 (其奈米粉體溶膠為半成品,呈非晶態混合物。),和本發明所 i_ “結晶型奈米粉體溶膠”(奈米粉體溶膠已結膠完成,且 成完全結晶態)完全不同,魏麟計也差職大,特別要說明 的是’本發明由於採用已結晶完成的奈米粉體溶膠,藥液本身的 1290634 . 安定性很高’無論在生產管控上、品質安定上,皆較‘‘反應型奈 米粉體溶膠”安定性高很多。 —口上述’本發明H新而具新雛、進步性及競爭力的 應用技術發明。 【發明内容】 本發明一種光學膜結晶型奈米溶膠製造法,是運用一序列設 籲定的化工處理程序,將被處理材料經由前處理卜結晶型奈米粉體 /感塗佈2、保護膜處理3及後處理4等程序,使結晶型奈米粉體 /谷膠在獅表_成均自、緻密而韻良好的絲細,不但具 有抗反射、抗眩光、半透射、时外光穿透、高反射等個別光學 特性,更有表面光滑/不易積垢/提高透光度/抗靜電/耐磨/耐到/ 防紫外光穿透等作用;本發明被處理材料包括壓克力、聚碳酸、 聚苯乙稀及其衍生材料、玻璃材料等。 _ 鈿處理1主要疋在被處理材料表面進行表面改質,以幫助結 晶型奈米粉體溶膠塗佈及後處理的進行,·所使用的前處理劑為以 適當的溶劑或水為基礎,並依需要添加潤濕劑及分散劑;所使用 的溶劑包括乙醇、異丙醇、己烷、環己烷、苯、甲苯、丙_、環 己酮、醋酸、三乙基銨、三丙基銨、吡咯酮、甲基四氫吡嘻_等, 溶劑濃度為3〜100% ;所使用的分散劑視需要加入,種類以聚乙 一醇(PEG)或聚丙二醇(PPG)或壬基紛(NP)或天然醇為主,分子量 在100〜1500之間,添加量為5〜5000ppm為宜;潤濕劑則以葵酚 1290634 (Octyl Phen〇i,〇p)或〇leyl Mc〇h〇1或綿羊油為主,分子量 在150〜3500之間,添加量為5〜i〇〇〇ppm為宜;其中玻璃使用的 前處理劑除了上述物質外,另外視需要加入氟化氫錢,加入量為 5〜20克/升(g/L),處理時,可以浸泡或滾錢等方式將前處理劑 均勻附著於被處理材料表面,其中浸泡的時間為1〇秒〜3〇分鐘, 處理溫度為10〜9(TC,經水洗、烘乾後,即完成前處理程序。 結晶型奈米粉體溶膠塗佈2所使用的處理劑為以含結晶型二 氧化鈦、結晶型二氧化石夕、結晶型氧化紹的奈米粉體溶膠為主成 份,其粒徑分佈為2〜l〇〇nm(0. _〜〇· 1〇〇//m),含量為〇. 1% 〜30% ’比表φ積為1G〜5⑼mVg的細,並依需要添加潤濕劑及 刀政%I] ’其中礼難I]及分散劑的選用依結晶型奈米粉體溶膠種類 而變’其成份同前處理劑,處理方式是以浸泡或滚輪塗佈等方式 將處理劑依設定程序,均勻塗佈於被處理材料表面;被處理材料 包括玻璃材料、Μ克力、聚碳酸、聚苯乙烯等瓣㈣及其衍生 材料;其中,浸泡的溫度為5〜8(rc,浸泡時間為5秒至10分鐘, 浸泡後的拉昇速度為每秒董米/分鐘(麵/min),被處理 材料在完全泡入處理液及拉昇至末端脫離液面的瞬間會做暫停的 動作’暫停時間0〜60秒,滾輪塗佈的速度為〇. 5〜_董米/分 鐘(咖/miri),每塗佈-次,即進行烘乾,供乾後的膜層厚度為5 〜200奈米(簡),依操作條件而不同;其中,的條件依被處理 材料不同而定’烘乾的溫度為60〜25(rc,時間為u分鐘,供 1290634 乾完成即可進行第二次的塗佈;每一種結晶型奈米粉體溶膠塗佈 的次數,依膜層厚度需求而不同,為1〜9次;膜層厚度達到需求 值後,即可進行下一階段(另一種折射率的奈米粉體溶膠)的塗 佈,上述步驟經重覆實施後,即可在被處理物材料上形成具特定 光學特性的光學鍍膜層;其中不同折射率形成的奈米粉體薄膜層 數,依光學性質需要,單面可為1〜7層。 保§蒦膜處理3是將結晶型奈米粉體溶膠塗佈完成的被處理材 料,以高分子膠内含至少美耐敏、聚乙烯、聚丙烯等擔體粒子, 均勻塗佈於被處理材料表面上,形成保護膜;其中,使用的高分 子膠種類尚包括··亞克力膠、PU膠、聚碳酸及聚苯乙稀的單體等, 塗佈時的S1含量為〇· 1〜60%(依厚度需要調整),塗佈後的烘乾溫 度為60〜15G°C:,縣時㈣5〜120分鐘,烘乾後的保護膜厚度 為2〜500奈米(nm),保護膜塗佈完成的被處理材料,經烘乾後進 行後處理(Post-treatment)。 後處理4係依被處理材料特性、結晶型奈米粉體溶膠種類、 顆粒大小而變,以輯錢波在設找條件下進行賴作用;其 中烘烤的溫度為6G〜15Gt ’時間為5至12G分鐘;微波所使用的 微波頻率為〇. i〜4〇GHz,功率為1〇〜3〇, 〇謹;時間為5秒至昶 分鐘’依結晶型奈米粉體溶膠種類'顆粒大小及被處理材料性 而定。 1290634 射、防紫外光穿透、高反射等光學特性外,更有表面光滑、不易 積垢、高透光度高吸附力、抗靜電、耐磨、耐刮等作用。 【實施方式】 以下,舉出實施例以說明本發明一種光學膜結晶型奈米溶膠 製造法内容,但本發明之範圍並不只限於此等的例子: 筆 實施例一: 將玻璃材料,先經過鹼洗脫脂後,浸泡在前處理劑中,前處 理劑是以氣化氫錄水溶液為主,其中含氟化氫録5克/升,雙氧水 2%,乙二醇(PEG)2〇ppm,壬基紛(Νρ)1〇_ ;在常溫下浸泡時間五 分鐘’經吹乾後,將玻璃㈣泡域晶型二氧化鈦奈雜體溶膠 (其中二氧化鈦含量為〇. 3%,粒徑分佈為2〜施m,比表面積為2〇〇 〜500mVg) ’其中溶液溫度為3〇t,浸泡時間為1〇秒,浸泡完成 •,’以扣釐米/分鐘(fflm/min)的速度拉昇,並在末端脫離液面的 =間暫停10秒’拉昇完成,於靴的溫度供烤,烘烤時間為 二鐘’供烤完成的玻璃紐再泡人原轉溶液中,重複三次,即 凡成二氧化鈦的結晶型奈米粉體溶膠塗裝,然後將此玻璃材料泡 =晶型二氧化料米粉體溶膠(其中二氧切含量為㈣、粒徑 '為10〜30簡、比表面積為7〇〜施2/g),操作條件同結晶型 4化欽奈米粉體溶膠塗裝,但速度拉昇改為3G㈣/分鐘 (_•並重複四次,供烤後的玻璃材料經高溫強化 11 1290634 反射玻璃”。 實施例二: 處理步驟如實酬㈠,但在二氧歸錄完錢,再作一 次結晶型二氧化鈦奈米粉體轉塗佈,操作條件同第一次的結晶 型二氧化鈦奈米粉體溶膠塗佈程序,供烤後的玻璃材料經高溫強 化,即為“高反射玻璃,,。 實施例三: 將被處理材料壓克力基材,泡入異丙醇(IPA)中3〇秒,經吹 乾後’依次序以結晶型二氧化鈦奈綠齡觀結晶型二氧化 石夕奈米粉體溶膠中,其操作條件同實施例㈠,但烘烤條件改為 70 C /10分鐘,穿占姑、夺 疋成後,改入含美耐米膠的曱基乙基醇(MEA)溶液 •中了中美耐米膠固含量為5%,塗佈後的烘乾溫度為6〇°c,烘乾 夺間為30分鐘,即為成品,處理過的壓克力基材,即為具“抗反 射”的塑膠透光材料。 實施例四: 理步驟如實施例㈢,但在二氧化矿塗奴成後,再作一 型—氧化鈇奈米粉體溶膠塗佈,操作條件同第一次的結晶 i A化鈦奈米粉體溶膠塗佈程序,烘烤後的壓克力基材,即為 12 1290634 具“高反射”的塑膠透光材料。 實施例五: 操作步驟同如實施例(三),但被處理物改為聚碳酸(PC),各 步驟的烘乾溫度改為110°C,其餘相同;所得成品亦為具“抗反 射”的塑膠透光材料。 •實施例六: 操作步驟同如實施例(四),但被處理物改為聚碳酸(PC),各 步驟的烘乾溫度改為11(rc,其餘補;所得成 射,,的塑膠透光材料。1290634 IX. Description of the invention: • The technical field of the invention belongs to the invention. The invention relates to a method for producing an optical film by an egg crystal type taiji sol, which is a method for preparing a crystalline titanium dioxide. The two-body sol (forming a high refractive index) and the crystalline oxidized crystal, the crystalline smectite cerium sol (forming a low refractive index) are uniformly coated on the basis of the setting procedure, respectively, according to the setting procedure, including acrylic, Polycarbonate, polystyrene and its derivatives) surface/glass surface, and = the optical film layer that has been formed as a protective film treatment, and then set the Ma ^ Ge • microwave processing program, that is The surface of the material to be treated is formed into a film having a thickness corresponding to the set f absorption = good structure and having specific optical characteristics; more directly, the present invention utilizes a set chemical treatment procedure to TiO 2 and cerium oxide, aluminum oxide = two different refractive Rate crystallized nanometer powder sol is uniformly applied to the surface of the material to be treated according to the setting procedure, and subjected to a specific protective film treatment as needed, and then subjected to a specific baking or microwave processing procedure. After that, the nano-powder sol is converted into an optical film with good adsorption; the formed optical film has anti-reflection, anti-glare, semi-transmission, anti-ultraviolet light penetration, high reflection and the like according to the coating procedure thereof. The characteristics of the external view are more smooth, less fouling, high transparency, high adsorption, antistatic, abrasion resistance, scratch resistance and so on. [Prior Art] Basically, optical coating elements are formed by alternately stacking high and low refractive index optical film layers to achieve specific optical functional requirements due to limited high and low refractive index materials in inorganic optical film layers. More than cerium oxide and titanium dioxide are used as materials. As for the production method, the optical film manufacturing used in the industry is vacuum vapor-deposited 1290634. The vacuum optical vapor deposition mass production optical film is already a production process. The quality of the product is also quite stable. However, the vacuum evaporation mass production process itself has quite a few problems and limitations, including the investment amount of the equipment, low output, the shape of the plated component must be solid, the shape of the plated 70 is not relevant, non-planar Problems such as uneven thickness of optical film of components' These problems, in the face of the trend of product recording and the pressure of cost reduction, resulting in vacuum evaporation mass production process, more and more doubts about the feasibility of mass production, Under this circumstance, _ optical difficulty method (4) is increasingly improving, and its main methods are two major types: organic film synthesis method and inorganic film coating method; The synthesis method is mainly a high molecular polymerization _ optical property, including a multilayer film composed of US Patent 6, 680, 899 ^ ^ silicon lubricant A Fluoro; the Republic of China Patent No. 578〇16, using injection molding, amorphous Thermoplastic resin; Republic of China Patent No. 575_, an organic film formed by low pressure vapor deposition; Republic of China Patent No. 572937, _ to produce a cyclic ester polyimine film in a & The Republic of China Patent No. 166683 is a multi-layer film that is repeatedly affixed with PDD polymer film to form a non-glare film. The organic film mainly focuses on optical properties, and is not wear-resistant and secret. The short life is also the bottleneck of its development, and the content of the organic film synthesis method is not related to the present invention; the inorganic film part, generally multi-layer film synthesis by vacuum distillation or sputtering 'in which vacuum The vapor deposition part, including the Republic of China Patent No. 1223009, uses a vacuum treatment method to form a fluorinated (CaFO and titanium dioxide (Ti〇2) into a film, 1290634 * into ', water The optical film of the power picking; the No. 226 of the Republic of China Patent No. 226, the fluorine butterfly (secret) and the dioxotomy (3) (6) are divided into vacuum film, and the film is formed into a film, which also forms an optical film that makes water and shame; In the Republic of China Patent No. 584742, the oxidization error (hearing) and the oxidized ♦ (3) (6) were formed into films by vacuum 1 spectrum method to form a multilayer film with a light effect; the Republic of China patent No. 54_ is directly The titanium dioxide (10)d is formed by vacuum evaporation to form a high reciprocal; the sputtering part is the spring side of the Republic of China (4) tiger, and the titanium dioxide (10) 2) and the cerium dioxide (Si〇2) are attached in a splashing manner. On the surface of the substrate, and then sintered at a high temperature to form a low-wear optical film: · Republic of China Patent No. 122402, on the surface of the substrate by sputtering Siia ne and oxidized stone (coffee) Forming a protective film to reinforce the plastic substrate is not wear-resistant, easy to dirty characteristics, in the vacuum evaporation or Lin production applications, are recorded production technology, but high equipment cost, low output efficiency, processing components The shape must be solid (otherwise it must be another mold, Die expensive. ), the _ I shape of the processing element must not have bumps or death (four), for its production, but no matter how, vacuum evaporation and money plating to make the township lang method, have nothing to do with the invention; see also the industry's nano-powder The solubilization method is widely used in the promotion, but the "nano powder sol," which is called "reactive nano-powder sol (the nano-powder sol is a semi-finished product, is an amorphous mixture.) And the invention i_ "crystalline nano powder sol" (the nano powder sol has been gelatinized and completed into a completely crystalline state) is completely different, Wei Lin is also a problem, especially in the description of the present invention Using the crystal powder sol that has been crystallized, the liquid of the liquid itself is 1290634. The stability is very high. 'In terms of production control and quality stability, it is much more stable than the 'reactive nano powder sol.' The present invention relates to a novel, progressive and competitive application technology invention. SUMMARY OF THE INVENTION An optical film crystalline nano sol manufacturing method of the present invention is a chemical process using a sequence of predetermined applications. The material to be treated is subjected to a procedure such as pretreatment, crystallized nano-powder/sensing coating 2, protective film treatment 3, and post-treatment 4, so that the crystalline nano-powder/gluten is in the lion's form and is dense and dense. Fine rhyme, not only anti-reflection, anti-glare, semi-transmission, external light penetration, high reflection and other individual optical characteristics, but also smooth surface / not easy to foul / improve transmittance / antistatic / wear / Resistant to / anti-ultraviolet light penetration; the material to be treated of the present invention includes acrylic, polycarbonate, polystyrene and its derivative materials, glass materials, etc. _ 钿 treatment 1 mainly 疋 surface on the surface of the material to be treated Modification to assist in the coating and post-treatment of crystalline nano-powder sol. · The pretreatment agent used is based on a suitable solvent or water, and a wetting agent and a dispersing agent are added as needed; The solvent includes ethanol, isopropanol, hexane, cyclohexane, benzene, toluene, propylene, cyclohexanone, acetic acid, triethylammonium, tripropylammonium, pyrrolidone, methyltetrahydropyridinium, and the like. The solvent concentration is 3 to 100%; the dispersant used is added as needed, The main type is polyethylene glycol (PEG) or polypropylene glycol (PPG) or sulfhydryl (NP) or natural alcohol, the molecular weight is between 100~1500, the amount is preferably 5~5000ppm; the wetting agent is sunflower Phenol 1290634 (Octyl Phen〇i, 〇p) or 〇leyl Mc〇h〇1 or lyn oil, molecular weight between 150~3500, the amount of addition is 5~i〇〇〇ppm; In addition to the above substances, the pretreatment agent may be added with hydrogen fluoride as needed, and the amount of addition is 5 to 20 g/L (g/L). When the treatment is performed, the pretreatment agent may be uniformly attached to the material to be treated by soaking or rolling money. The surface, wherein the immersion time is 1 sec. to 3 〇 minutes, the treatment temperature is 10 〜9 (TC, after washing and drying, the pretreatment process is completed. The treatment used for the crystallization of the nanometer powder sol coating 2 The agent is a nanometer powder sol containing crystalline titanium dioxide, crystalline silica dioxide, and crystalline oxide, and has a particle size distribution of 2 to 1 〇〇 nm (0. _~〇·1〇〇/ /m), the content is 〇. 1% ~ 30% 'the ratio of the table φ is 1G~5(9)mVg, and if necessary, add wetting agent and knife%1] The difficulty of I] and the choice of dispersant vary according to the type of crystalline nano-powder sol. The composition is the same as the pre-treatment agent. The treatment method is uniform coating on the treatment agent according to the setting procedure by soaking or roller coating. The surface of the material to be treated; the material to be treated includes glass material, acryl, polycarbonate, polystyrene, etc. (4) and its derivative materials; wherein the immersion temperature is 5~8 (rc, soaking time is 5 seconds to 10 minutes) After the immersion, the pulling speed is dongm/min (face/min), and the material to be treated will pause when it is completely immersed in the treatment liquid and pulled to the end to escape from the liquid surface. 'Pause time 0~60 Seconds, the speed of roller coating is 〇. 5~_ Dongmi/min (coffee/miri), every coating-time, that is, drying, the thickness of the film after drying is 5~200 nm (simplified) Depending on the operating conditions; the conditions are different depending on the material being processed. 'The drying temperature is 60~25 (rc, the time is u minutes, for 1290634 dry to complete the second coating; each The number of times a crystalline nano-powder sol is coated, depending on the thickness of the film layer The same, 1~9 times; after the film thickness reaches the required value, the next stage (the other refractive index of the nano-powder sol) can be applied, and the above steps can be processed after repeated implementation. An optical coating layer having specific optical characteristics is formed on the material; wherein the number of layers of the nano powder film formed by different refractive indexes is required according to optical properties, and one side may be 1 to 7 layers. The 蒦 蒦 film treatment 3 is a material to be processed by coating a crystalline nano sol sol, and the polymer gel contains at least a carrier particle such as methicone, polyethylene, or polypropylene, and is uniformly applied to the material to be treated. On the surface, a protective film is formed; among them, the type of polymer glue used includes acrylic monomers, PU glue, polycarbonate, and polystyrene monomers, and the S1 content during coating is 〇·1 to 60%. (Adjusted according to the thickness), the drying temperature after coating is 60~15G °C: 5 times to 120 minutes in the county (four), the protective film thickness after drying is 2~500 nanometers (nm), protective film coating The finished material to be processed is subjected to post-treatment after drying. The post-treatment 4 series is changed according to the characteristics of the material to be treated, the type of crystalline nano-powder sol, and the particle size, and the granulation is carried out under the conditions of setting; the baking temperature is 6G~15Gt 'time is 5 to 12G minutes; microwave frequency used for microwave is 〇. i~4〇GHz, power is 1〇~3〇, 〇 ;; time is 5 seconds to 昶 minutes 'depending on crystal type nano powder sol type' particle size and It depends on the materiality. 1290634 In addition to the optical characteristics of shooting, anti-ultraviolet light penetration and high reflection, it has the functions of smooth surface, difficult to scale, high transparency, high adsorption, antistatic, abrasion resistance and scratch resistance. [Embodiment] Hereinafter, examples of the method for producing an optical film crystallized nano sol according to the present invention will be described, but the scope of the present invention is not limited to these examples: Pen Example 1: The glass material is passed first. After the alkali elutes the fat, it is immersed in the pretreatment agent. The pretreatment agent is mainly composed of a vaporized hydrogen recording aqueous solution, wherein the hydrogen fluoride is recorded in 5 g/L, the hydrogen peroxide is 2%, and the ethylene glycol (PEG) is 2 〇 ppm.纷(Νρ)1〇_ ; soaking time at normal temperature for five minutes' After drying, the glass (four) bubble-domain crystalline titanium dioxide nano sol (where the titanium dioxide content is 〇. 3%, the particle size distribution is 2~ m, specific surface area is 2〇〇~500mVg) 'where the solution temperature is 3〇t, the soaking time is 1〇 second, the soaking is completed•, 'pulled at a speed of decimation cm/min (fflm/min), and at the end Disengaged from the liquid level = pause for 10 seconds 'pull up is completed, the temperature of the boot is baked, and the baking time is two minutes'. The glass spring is added to the original solution of the roasting, which is repeated three times, that is, the titanium dioxide is added. Crystalline nano-powder sol coating, and then soaking the glass material = crystal type dioxide rice powder sol (where the dioxygen content is (4), the particle size 'is 10~30, the specific surface area is 7〇~2/g), and the operating conditions are the same as the crystalline type 4 capsules. Sol coating, but the speed is increased to 3G (four) / minute (_• and repeated four times, the glass material after roasting is strengthened by high temperature 11 1290634 reflective glass.) Example 2: Processing steps such as remuneration (a), but in dioxane After the registration of the money, another crystalline titanium dioxide nano-powder powder coating is applied, and the operating conditions are the same as the first crystalline titanium dioxide nano-powder sol coating procedure, and the glass material after roasting is strengthened by high temperature, which is "high". Reflective glass,. Example 3: The acrylic substrate to be treated is immersed in isopropanol (IPA) for 3 sec seconds, and after being blown dry, the sequential crystallization of titanium dioxide nano-age crystals In the oxidized stone sulphite powder sol, the operating conditions were the same as those in the example (1), but the baking condition was changed to 70 C /10 minutes. After wearing the scorpion and the scorpion, the thiol ethyl group containing the methicillin was changed. Alcohol (MEA) solution • 5% of China-US Nami cement content, after coating The temperature is 6〇°c, and the drying interval is 30 minutes, which is the finished product, and the treated acrylic substrate is a plastic light-transmitting material with “anti-reflection”. Embodiment 4: The steps are as follows. (3), but after the smear of the sulphuric acid ore, it is further coated with a type of yttrium oxide nano-powder sol, and the operating conditions are the same as the first crystallization of the titanium oxide nano-sol sol coating procedure, after baking The acrylic substrate is 12 1290634 plastic light transmissive material with "high reflection". Embodiment 5: The operation steps are the same as in the embodiment (3), but the treated object is changed to polycarbonate (PC), each step The drying temperature was changed to 110 ° C, and the others were the same; the finished product was also a plastic light-transmitting material with "anti-reflection". Example 6: The operation procedure was the same as in the embodiment (4), but the treated material was changed to polycarbonate. (PC), the drying temperature of each step is changed to 11 (rc, the rest of the; the resulting injection, plastic light transmissive material.

軸本齡以六項實施例揭露如上’財並非㈣限定本創 作此應用者,在不脫離本創作之精神和範嘴内,當可 範圍所狀者為準。 ” 青專利 【圖式簡單說明】 第一圖為本發明處理程序流程圖。 【主要元件符號說明】 前處理1 結晶型奈米粉體溶膠塗佈2 13 1290634 保護膜處理3 後處理4The age of the shaft is disclosed in the six examples. The above is not the limit of (4) the creation of this application, and the scope of the scope of the creation is subject to the spirit and scope of the creation.青专利 [Simple description of the diagram] The first diagram is the flow chart of the processing procedure of the present invention. [Description of main components] Pretreatment 1 Crystalline nano powder sol coating 2 13 1290634 Protective film treatment 3 Post treatment 4

Claims (1)

1290634 十、申請專利範園:1290634 X. Applying for a patent garden: 1、一種光學膜結晶型奈米溶膠製造法,是利用結晶型奈米溶膠製 造光學膜的新流程,其作法是將被處理材料經過前處理程序進 行表面改質後,將清潔、改質完成的被處理材料經由結晶型奈 米粉體溶膠塗佈、保護膜處理及後處理等程序,使結晶型狀奈 米粉體溶膠在被處理材料表面,塗佈形成均勻、緻密而吸附^ 好的光學薄膜;本發明被處理材料包括壓克力、聚碳酸、聚苯 乙稀,其衍生材料、玻璃材料等,·其中,結晶型奈米粉體溶膠 塗佈是以魏歧齡料料縣晶型雜奈米轉均勾塗 佈於被處理材料表面;倾膜處酬以高分子勒含至少美耐 敏、聚乙烯、聚丙稀等擔體粒子,均勻塗佈於被處理材料表面 上’形成保護膜;後處理是以烘烤或微波在設定的條件下進行 ^膜作用;經過上述處理的被處理材料,表面會形成均句、緻 密而吸附良好的光學薄膜及保護層’不但分別具有抗反射、抗 眩光、半透射、防紫外光穿透、高反射等光學特性外,更有表 面光滑、不易積垢、高透光度高吸附力、抗靜電、 等作用。 2·=申喷專她圍第丨摘述之光學麟晶型奈米溶膠製造法, 二:、、、。aa型奈米粉體溶膠塗佈所使用的處理劑為以水溶液中含 Hi二氧化鈦、結晶型二氧化梦、結晶型氧化_奈米結晶 以合膠為主成份,其粒徑分佈為卜⑽咖⑽⑽鄉〜1〇〇 ,,含量為◦.1%〜識,比表面積為10〜500mVg的範圍, 要添蝴關及分_ ;表面__对是以浸泡或 矣“、’、佈等方式將處糊依設定程序,均㈣佈於被處理材料 表面,其中,浸泡的溫度為5〜8(rc,浸泡時間為5秒至1〇分 15 12906341. An optical film crystal type nano sol manufacturing method, which is a new process for manufacturing an optical film by using a crystalline nano sol, which is characterized in that after the surface of the material to be processed is subjected to a pretreatment process, the surface is modified, and the cleaning and upgrading are completed. The material to be treated is coated on the surface of the material to be processed to form a uniform, dense, and well-adsorbed optical film via a process such as crystalline nano-sol sol coating, protective film treatment, and post-treatment. The material to be treated according to the present invention includes acrylic, polycarbonate, polystyrene, derivative materials, glass materials, etc., wherein the crystalline nano-sol sol coating is a kind of crystal-type hybrid rice of Weiqiling material county. All of them are coated on the surface of the material to be treated; the plastic film contains at least the carrier particles such as methicone, polyethylene, polypropylene, etc., and is evenly coated on the surface of the material to be treated to form a protective film; The film is treated by baking or microwave under the set conditions; the treated material subjected to the above treatment forms a uniform film, a dense and well-adsorbed optical film and a protective layer. Not only have anti-reflection, anti-glare, a semi-transmissive, anti-UV penetration, highly reflective outer optical characteristics, etc., more smooth surface, easy to fouling, high transparency and high adhesive force, anti-static, and so on. 2·=Shenpeng specializes in the production of optical cylindrical nano sols, which are described by Dien, Di, 2:,,,. The treatment agent used for coating aa type nano powder sol is a solution containing Hi titanium dioxide in an aqueous solution, a crystalline dioxide dioxide dream, and a crystalline oxidation-nano crystal as a main component, and the particle size distribution thereof is (10) coffee (10) (10) Township ~ 1 〇〇, the content is ◦.1% ~ knowledge, the specific surface area is 10~500mVg range, to add a butterfly and points _; surface __ pairs are soaked or 矣 ", ', cloth, etc. At the paste setting procedure, all are placed on the surface of the material to be treated, wherein the temperature of the soaking is 5~8 (rc, soaking time is 5 seconds to 1 minute 15 1290634) 鐘’浸泡後的拉昇速度為每秒1〜1800釐米/分鐘(mm/min), 被處理材料在完全泡入處理液及拉昇至末端脫離液面的瞬間會 做暫停的動作,暫停時間〇〜6〇秒,滾輪塗佈的速度為〜 6000釐米/分鐘(mm/min),每塗佈一次,即進行烘乾,烘乾後 的膜層厚度為5〜200奈米(nm),依操作條件而不同;其中,烘 乾的條件依被處理材料不同而定,烘乾的溫度為60〜250°C,時 間為1〜30分鐘,烘乾完成即可進行第二次的塗佈,每一種奈 米粉體溶膠塗佈的次數,依膜層厚度需求而不同,為1〜9次, 膜層厚度達到需求值後,即可進行下一p皆段(另一種折射率的 奈米粉體溶膠)的塗佈,上述步驟經重覆實施後,即可在被處 理材料上形成具特定光學特性的光學鍍膜層,其中不同折射率 形成的奈米粉體薄膜層數,依光學性質需要,單面可為丨〜7層。 3·如申請專利範圍第丨項所述之光學膜結晶型奈米轉製造法, 保護膜處理是將結晶型奈米粉體溶雜佈完成的賊理材料, 以高分子膠内含至少美耐敏、聚乙烯、聚丙烯等擔體粒子,均 勻塗佈於被處理材料表面上,形成保護膜,塗佈時的固含量為 。0.1〜60%(依厚度需要調整),塗佈後的烘乾溫度為⑼〜bo °c 烘乾時間為5〜12()分鐘,烘乾後的保護膜厚度為2〜_ 奈米(nm),保護膜塗佈完成的被處理材料,經烘乾後進行後處 理程序(Post-treatment);其中高分子膠尚包括··亞克力膠处 PU膠、聚碳酸及聚苯乙稀的單體等。 / 4·如申請專利細第〗項所述之光學膜結晶型奈米轉法, 其中後處理程序雜被處輯料特性、結晶型奈米粉體溶勝 類、顆粒大小而變,以烘烤或微波在設定的條 ^ 用;其帽烤的溫度:嶋7G〜靴,時間為3^= 16 1290634 % ' 鐘;玻璃為450〜6000°C,時間為5至30分鐘;若使用微波作 •後處理,所使用的微波頻率為2. 45GHz,功率為10〜1,500W ; 時間為5秒至30分鐘,依結晶型奈米粉體溶膠種類、顆粒大小 及被處理材料性質而定。The pulling speed of the bell after soaking is 1~1800 cm/min (mm/min) per second, and the material to be treated will pause when it is completely bubbled into the treatment liquid and pulled to the end to escape from the liquid surface. 〇~6 〇 seconds, the speed of roller coating is ~ 6000 cm / min (mm / min), drying once every coating, the thickness of the film after drying is 5 ~ 200 nm (nm), Depending on the operating conditions, the drying conditions are determined by the materials to be processed. The drying temperature is 60 to 250 ° C, the time is 1 to 30 minutes, and the second coating can be performed after drying. The number of coatings of each type of nano-powder sol varies from 1 to 9 times depending on the thickness of the film layer. After the film thickness reaches the required value, the next p-stage can be carried out (the other refractive index of the nano-powder) Coating of the body sol), after the above steps are repeated, an optical coating layer having specific optical characteristics can be formed on the material to be processed, wherein the number of layers of the nano-powder film formed by different refractive indexes is required according to optical properties. One side can be 丨~7 layers. 3. The optical film crystal type nano-transfer manufacturing method as described in the scope of the patent application, the protective film treatment is a thief material which completes the crystalline nano-powder-dissolving cloth, and the polymer glue contains at least the melon The carrier particles such as sensitive, polyethylene, and polypropylene are uniformly coated on the surface of the material to be treated to form a protective film, and the solid content at the time of coating is. 0.1~60% (adjusted according to thickness), the drying temperature after coating is (9)~bo °c, the drying time is 5~12() minutes, and the thickness of the protective film after drying is 2~_nm (nm The treated material coated with the protective film is subjected to post-treatment after drying; wherein the polymer adhesive still includes the monomer of PU glue, polycarbonate and polystyrene at the acrylic glue. Wait. / 4 · The optical film crystal type nano-transfer method as described in the patent application, wherein the post-treatment process is characterized by the characteristics of the material, the crystal type of the nano-powder, and the particle size to be baked. Or microwave in the set bar; its cap baking temperature: 嶋7G~boots, time is 3^= 16 1290634 % 'clock; glass is 450~6000 °C, time is 5 to 30 minutes; if using microwave • Post-treatment, using a microwave frequency of 2.45 GHz, a power of 10 to 1,500 W; a time of 5 seconds to 30 minutes, depending on the type of crystalline nano-sol sol, the particle size, and the nature of the material being treated. 17 1290634 七、指定代表圖: (一) 本案指定代表圖為:第(一)圖。 (二) 本代表圖之元件符號簡單說明: 前處理1 結晶型奈米粉體溶膠塗佈2 保護膜處理3 後處理417 1290634 VII. Designated representative map: (1) The representative representative of the case is: (1). (2) A brief description of the symbol of the representative figure: Pretreatment 1 Crystalline nano powder sol coating 2 Protective film treatment 3 Post treatment 4 八、本案若有化學式時,請揭示最能顯示發明特徵的化學式:8. If there is a chemical formula in this case, please disclose the chemical formula that best shows the characteristics of the invention:
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