1327734 九、發明說明： 【發明所屬之技術領域】 本發明係涉及-種透明導電膜之製備方法，尤其涉及 一牙可應用於場發射器件内的透明導電膜之製備方法。 【先前技術】 明導電膜於場發射技術中有著—用，其 發射器件的陽極基板上，並與陰極的電子發射 明導==加電場，同時’焚光層發出的光透過透 =的==上使用的多爲氧化銦錫薄膜，係採用磁控 可實現大°該種製備氧化鋼錫薄膜的方法雖 批！生産，惟其所需的生產材料及製備過繼 率較供—㈣備過程較為簡單、效 得；之製備方法，該製備方法 【發明内容】…有缺的導電性及透光性。 下面將藉由實施例進—半 製備方法，㈣mf JL明—種透明導電膜之 低且具有較：效率二過程簡單、易於操作、成本較 膜具有較好的導電1二該製備方法得到的透明導電 ''種透明導賴之製備 所需的透明導電膜，該 件表面形成 下步輝·· 電膜之A備方法主要包括以 8 W/734 製備奈米碳管漿料； 將製備的奈米碳管漿料於玻璃元件表面形成一奈米碳 管漿料層； 反 將奈米破管漿料層供乾；以及 將形成有奈米碳管衆料層的玻璃元件於氮氣或情性氣 ，的保護下加熱至3GG〜50GT並保溫的時間，再降至 室溫’從而於玻璃元件的表面形成奈米碳管透明導電膜。 與先前技術相比較，本發明透明導電膜之製備方 玻璃表面間的吸附作用於玻璃元件上 成不h s《觸並將其加缺秘_元件 系的透明導f膜，製備過關單1 成斤 具有較高的效率；同時，因奈米 有 乂低且 具有較好的導電性能 具有較好的透光性，.同時亦 【實施方式】 -步：：:_對本發明透明導電膜之製備方法作進 請參閱圖！，本發明製 兀件表面形成所需的透明導月^電搞之方法係於玻璃 驟： 犋，該方法主要包括以下步 f驟（：)’製備奈米碳管襞料。 /丁'米石反官漿料中主要包含有 内的奈米碳管，該奈米碳管 ^載體及为散於有機載體 製備有機載體； 遽備方法包括以下步驟： 其中，該有機賴狀合劑，包_心 作局增塑劑的少量鄰苯二甲酸二 私柄、 乙基纖維素。有機載體的製備過程爲的少量 的條件下紅級維素簡雜油 I、及胁 ψ 叶τ，及，加入鄰茉_ 締油浴加熱的條件下持續攪拌—定時㈣ 鄰;甲？體。其中’優選地’松油醇、乙基纖維素及 ::Γ: 丁酿於混合劑中的質量百分比分別約爲 /。、5/0和5% ;加熱溫度爲8(Ml(rc，最優加献時間爲 0°c;持續麟時間爲闕小時，最優持續^^間爲 Z4小時。 將粉末狀奈米碳管於二氣乙烧中用破碎機分散後再進 行超聲分散形成奈米碳管溶液； 其中，奈米碳管可預先通過化學氣相沈積法、電弧放. 電法或鐳射蒸發法等傳統技術製備，奈米碳管長度優選爲 1 100微米，最優長度約爲10微米；直徑優選爲丨〜1〇〇納 求。奈米碳管與二氣乙院的比例優選爲：每兩克奈米碳管 而要約500毫升的二氣乙烧。破碎機分散的時間優選爲 5〜30分鐘，最優時間爲20分鐘；超聲分散的時間優選爲 仞〜仙分鐘，最優時間爲30分鐘。 過濾奈米碳管溶液； 其中，奈米碳管溶液可選用篩網過濾，最優地，選用 400目的篩網過濾'奈米碳管溶液從而可得到具有優選直徑 及長度的奈米碳管的溶液。 將奈米碳管溶液加入有機載體中並充分分散； 13277341327734 IX. Description of the Invention: [Technical Field] The present invention relates to a method for preparing a transparent conductive film, and more particularly to a method for preparing a transparent conductive film which can be applied to a field emission device. [Prior Art] The conductive film has a field emission technology, which is used on the anode substrate of the emitting device, and emits an electron with the electron emission of the cathode == an electric field, and the light emitted by the light-emitting layer passes through == = Most of the used indium tin oxide film, the use of magnetic control can achieve large ° this method of preparing oxidized steel tin film, although approved! Production, but the required production materials and preparation success rate are better than - (4) preparation process is relatively simple and effective; the preparation method, the preparation method [invention content] ... lack of conductivity and light transmission. In the following, by way of the embodiment, the semi-preparation method, (4) mf JL-type transparent conductive film is low and has the following advantages: the process is simple, easy to operate, and the cost is better than that of the film. Conductive ''transparent transparent conductive film required for the preparation of the transparent conductive film, the surface of the piece forming the next step · · electric film A preparation method mainly includes preparing the carbon nanotube slurry at 8 W / 734; The carbon nanotube slurry forms a carbon nanotube slurry layer on the surface of the glass component; the nanotube breaking slurry layer is supplied for drying; and the glass component forming the nanocarbon carbon nanotube layer is nitrogen or emotional Under the protection of gas, it is heated to 3GG~50GT and kept for a while, and then cooled to room temperature' to form a carbon nanotube transparent conductive film on the surface of the glass element. Compared with the prior art, the adsorption between the surface of the glass of the transparent conductive film of the present invention is applied to the glass element to form a transparent guide film of the component. It has high efficiency; at the same time, because of its low conductivity and good electrical conductivity, it has good light transmittance, and also [Embodiment] - Step:::_ Preparation method of transparent conductive film of the present invention Please refer to the picture! The method for forming the transparent guide electrode formed on the surface of the beryllium of the present invention is applied to the glass. The method comprises the following steps: (step) to prepare a carbon nanotube dip. /丁'米石反官浆 mainly comprises an inner carbon tube, the nano carbon tube ^ carrier and an organic carrier prepared by dispersing the organic carrier; the preparation method comprises the following steps: wherein the organic lame Mixture, package _ heart made plasticizer a small amount of phthalic acid two private handle, ethyl cellulose. The preparation process of the organic carrier is a small amount of conditions under the conditions of red-dimensional vitamins I and 胁 τ, and, after adding to the adjacent __ oil bath, the heating is continued under the condition of heating - timing (four) neighbor; body. Wherein 'preferably' terpineol, ethylcellulose and:::: the mass percentages in the mixture are about /, respectively. 5/0 and 5%; heating temperature is 8 (Ml (rc, optimal addition time is 0 °c; continuous lining time is 阙 hour, optimal duration is ^4 hour). Powdered nanocarbon The tube is dispersed in a two-gas sinter by a crusher and then ultrasonically dispersed to form a carbon nanotube solution; wherein the carbon nanotubes can be previously subjected to conventional techniques such as chemical vapor deposition, arc discharge, electrical or laser evaporation. For preparation, the length of the carbon nanotubes is preferably 1 100 micrometers, and the optimal length is about 10 micrometers; the diameter is preferably 丨~1〇〇纳. The ratio of the carbon nanotubes to the second gas hospital is preferably: every two grams. The carbon nanotubes are required to be about 500 ml of dioxane. The time for dispersing the crusher is preferably 5 to 30 minutes, and the optimum time is 20 minutes; the time for ultrasonic dispersion is preferably 仞~ cents, and the optimum time is 30 minutes. Filtering the carbon nanotube solution; wherein the carbon nanotube solution can be filtered by a mesh screen, and optimally, a 400 mesh sieve is used to filter the 'nanocarbon tube solution to obtain a carbon nanotube having a preferred diameter and length. Solution. The carbon nanotube solution is added to the organic carrier and fully dispersed; 1327 734
充分分今超聲辰4將奈米碳管減於有機載體+ ==湯的時間優選爲加分鐘。奈米碳管溶液 ::=機載體的質量比優選為m 到具有合;濃度以管溶液的有機載體到得 料中奈米碳管的遭度可影響:二二:==漿 的透光性能及導電性能。當襞 二得:丨的奈米碳管透明導電祺的透光率較 ： 透料賴的透騎較高而導電性能較弱。優選 地二當於上述製備過程中選用2克奈米碳管、㈤_毫升 的-亂乙烧及奈米碳管與有機載體的質量爲15 : !時，於 ^浴加熱下將混有命米.碳t溶液的有機載體蒸發得到侧 宅升的奈米碳管漿料。 其中，加熱溫度優選為9(TC。 步驟（二），將製備的奈米碳管漿料於玻璃元件的表面 形成一奈米碳管漿料層。 其中，於玻璃元件表面上形成奈米碳管漿料層的方法 依據玻璃元件的形狀而不同，如，當需要於平板玻璃的一 側表面形成透明導電膜時，形成奈米碳管漿料層的方法 爲：將製備的奈米碳管漿料放置於敞口容器内；將兩平板 玻璃重疊並豎直浸人奈米碳管漿料中；勾速提出平板玻 璃，藉由吸附作用即於兩重疊玻璃的兩相對表面各形成一 奈米碳管漿料層。當需要於玻璃管内壁形成透明導電膜 11 時，形成奈米碳管装料層的方法爲：將玻璃管一端封閉炎 將玻璃管的封閉端向下14放置；將奈米破管㈣倒入玻 璃官内’打開_管的封閉端，奈米碳管料藉由重力作 $ utT ’部分奈米祕通過㈣仙於玻璃管内 壁上形成一奈米碳管漿料層。形成奈米碳管漿料層 的過程 應於潔淨的環境⑽行，優選地，環㈣的灰塵度小於 1000mg/m3 〇 步驟（三）’將奈米碳管漿料層烘乾使得奈米碳管漿料 層固定於玻璃元件表面。 步驟（四）將形成有奈米碳管漿料層的玻璃元件於氮 氣或h性軋體的保護下加熱至3〇〇〜5〇(Tc並保溫一定的時 間，再降至室溫，從而於玻璃元件的表面形成奈米碳管透 明導電膜。 .. 其中，加熱溫度優選爲32(TC，保溫時間優選爲2〇分 鐘。 在貫驗中，藉由上述製備方法中的較優參數制得長度 約爲10厘米且寬度爲8厘米的透明導電膜，經測試，該奈 米碳管透明導電膜的透光率約爲70%，沿長度方向上的電 阻小於100千歐。 綜上所述，本發明確已符合發明專利之要件，遂依法 提出專利申請。惟，以上親者僅為本翻之健實關， 自不能以此限制本案之申請專利範圍。舉凡熟悉本案技藝 之人士援依本發明之精神所作之等效修飾或變化，皆應^ 蓋於以下申請專利範圍内。 12 1327734 【圖式簡單說明】 圖1係本發明實施例透明導電膜之製備方法的流程示 意圖。 【主要元件符號說明】 13It is preferable to add the minute to the time when the ultrasonic tube 4 is used to reduce the carbon nanotubes to the organic carrier + == soup. The carbon nanotube solution::=the mass ratio of the machine carrier is preferably m to have a combination; the concentration of the organic carrier of the tube solution to the yield of the carbon nanotubes in the material can be affected: 22:== Performance and electrical conductivity. When 襞二得: 透光's carbon nanotube transparent conductive 祺 light transmittance: the permeability of the permeable material is higher and the conductivity is weaker. Preferably, when 2 g of carbon nanotubes, (5)_ml of the chaotic baking and the mass of the organic carbon carrier and the organic carrier are 15:: in the above preparation process, the mixture will be mixed under the heating of the bath. The organic carrier of the m. carbon t solution is evaporated to obtain a side carbon nanotube slurry. Wherein, the heating temperature is preferably 9 (TC. Step (2), the prepared carbon nanotube slurry forms a carbon nanotube slurry layer on the surface of the glass element. Among them, the formation of nano carbon on the surface of the glass element The method of the tube slurry layer differs depending on the shape of the glass element. For example, when it is required to form a transparent conductive film on one side surface of the flat glass, the method of forming the carbon nanotube slurry layer is: preparing the carbon nanotube The slurry is placed in the open container; the two flat glass are overlapped and vertically immersed in the slurry of the human carbon nanotube; the flat glass is lifted, and the opposite surfaces of the two overlapping glass are formed by adsorption. The carbon nanotube slurry layer. When the transparent conductive film 11 needs to be formed on the inner wall of the glass tube, the method for forming the carbon nanotube charging layer is: sealing the end of the glass tube to the lower end 14 of the glass tube; The nano tube (4) is poured into the glass door to open the closed end of the tube. The carbon nanotube material is made by gravity for $ utT 'partial nanometer secret (4) to form a carbon nanotube slurry on the inner wall of the glass tube. Layer forming a layer of carbon nanotube slurry The process should be in a clean environment (10). Preferably, the dust of the ring (4) is less than 1000 mg/m3. Step (3) Drying the layer of the carbon nanotube slurry to fix the layer of the carbon nanotube slurry on the surface of the glass element Step (4) The glass element forming the slurry layer of the carbon nanotubes is heated to 3 〇〇 5 〇 under the protection of nitrogen or a h-rolling body (Tc and kept for a certain period of time, and then cooled to room temperature, Thereby forming a carbon nanotube transparent conductive film on the surface of the glass element. wherein the heating temperature is preferably 32 (TC, the holding time is preferably 2 〇 minutes. In the test, by the above preferred parameters in the preparation method A transparent conductive film having a length of about 10 cm and a width of 8 cm was obtained. After testing, the transparent conductive film of the carbon nanotube has a light transmittance of about 70%, and the electric resistance along the length direction is less than 100 kΩ. As described above, the present invention has indeed met the requirements of the invention patent, and has filed a patent application according to law. However, the above relatives are only a practical one, and cannot limit the scope of the patent application in this case. Those who are familiar with the skill of the case According to the spirit of the present invention The equivalent modifications or variations are to be included in the following claims. 12 1327734 BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a schematic flow chart showing a method of preparing a transparent conductive film according to an embodiment of the present invention.