200407939 玖、發明說明 内容、實、 屬之技術領域'先前技術 【發明領域】 本發及-種燈絲及其製備方法，_涉及—種使 材 料之燈絲及其製備方法。 丁丁 g柯 【發明背景】 砂技射之電燈燈絲錢天然之多晶、無定形或非晶材料 但這些材料長時間處於較高溫度下會變脆而易碎。 、真=^__之金_在__，由於其晶耱 :•麵於較高溫 ^及·壽命日Γ 、、、、°晶’從而增大金屬燈絲之易碎性而降低強 錢燈絲之另-缺點係電阻率較低，有時為提高其電阻，需相當長: 之金屬燈絲，同時為減小燈泡之大小，要將金屬燈絲緊密纏繞，纏繞之 部分相互糾結，因此燈絲發光面積減小，燈絲發光效率降低。金屬燈絲 尤其係鎢絲還具有電阻/溫度係數較高之缺點，從室溫到刪。c之範· 其電阻值提高六倍’從而為得到相同之發光效率，其雜之電能更 多0 【發明目的】 一斤1C本I月之目的在於提供一種於較高溫度下具有高穩定 性、咼比表面積之燈絲。 本發明之另—目的在於提供—種具有高穩親、高比表燈絲之 製備方法。 、 6 200407939 【發明特徵】 本發明提供之燈絲包含有碳奈料絲及二 電極間。 發明說明、續頁 電極，該碳奈米管 絲纏繞 破奈米管陣継嫩議； 極間，得到燈絲 【較佳實施例】 請參閱第-圖，本發明之燈絲屬包含有碳奈米管絲咖及二電. 30，該碳奈米管絲204纏繞於該二電極3〇間。 私 、、糸204與二電極3〇相接觸 作為本發明之進一步改進，可以於碳奈米管 處點上銀點膠32以降低接觸點之電阻。 本發明提供-種碳奈米管燈絲之製備方法，其包括如下步驟： 步驟1 :請參閱第二圖，製備碳奈米管陣列2〇，具體過程如下。 準備基底22，該基底22包括-個直徑為5· lcm、厚為·麵之石夕晶片 222，該矽晶片222上面沈積有8〇〇nm厚之二氧化石夕層224，該二氧化石夕| 224之表面被處理成平整光滑以適合生長大賴碳奈米管陣列旧電子束 沈積方法於基底22上形成-層厚為5nm之鐵細24，隨後於溫度細〜侧 C之間退火處理約10小時形成鐵的氧化物膜，再用氳氣或氨氣將此鐵的 氧化物膜還原為單質鐵膜24作催化劑使用；將該沈積有催化劑鐵薄膜24 之基底22切成矩形小塊，將其中一塊放入石英反應舟（圖未示），再將此 石英反應舟送至2. 54cm石英反應爐（圖未示）之中心；通入氬氣，同時加 熱反應爐至650〜700 C ;然後通入30sccm乙炔與300sccm氬氣之混合氣 7 200407939 發明說明續頁 體；反應5俯鐘後’將反應爐冷卻至室溫，碳奈料陣卿於該絲 22上生成。 ， V&2 π ’閱第―圖，從上述碳奈米管陣列2◦中拉出碳奈米管絲 204。製得碳奈米管陣·後，用抽拉卫具如鑷子（圖未示），夾住一束碳 奈米管2G2抽拉，由於碳奈米管之間的凡德瓦爾力作用，碳奈米管束观 端部首尾連接於一起，形成碳奈米管絲2〇4。 步驟3 :請參閱第-圖，用均勻外力將碳奈米管絲2〇4纏繞於作為二 電極3暖用彼此相距一定間距之二根金屬導線上，優遷間距編之嫣夢 導線。然後於縣米管職慎二電極3_鋪處點上銀點職以降低接 觸點之電阻，即獲得於外加電壓下可發光之燈絲細。 要獲得能抽拉出碳奈米管絲2〇4之碳奈米管陣，需滿足固. 生長條件： 一 a·基底表面平整光滑； b·碳奈米管之生長速率高； c·碳源氣之分壓低。 | 基底表面平縣_於生長峻高密度之碳奈料物，從而近距 離碳奈米管間之凡德瓦爾力可保證碳奈料聚集成束並拉成絲。 生長條件b及e可縣於提高碳奈綺生長速較同轉低無定型碳 之生長速率’因此可避免於生長碳奈米管之同時於其管壁上生長出益定 型碳而減小碳奈米純之凡德瓦_力。因碳奈料之生長稱與反應 及催化獻溫差成正比，所以需要温差足夠灿提高碳奈綺之生長^ 率通书至少要控制反應爐及催化劑之溫差在5〇。匸以上。操作時，催化 200407939 發明說明H胃~ 」之/皿度可通過;^源氣之、來控制，而反應爐之溫度可直接控 制。碳源氣之分壓可通過調整碳源氣及氬氣之流速流量比來控制，通常、 碳源氣之分壓不高於〇· 2，優選不高於〇. J。 〃碳奈米管絲204之寬度由抽拉工具之尖端尺寸決定，尖端尺寸越小， 狻传的奴奈米官絲204寬度越小。抽拉碳奈米管絲2〇4用力之大小由碳奈 米吕絲204之見度決定，寬度越大，所需力越大。碳奈米管絲謝之長度 取決於碳奈米管陣列20之面積。 另外生長碳奈米管陣·時也可用其他惰性氣體，如氮氣、氦氣夢 來代替氬氣作為保護氣使用，也可用其他過渡金屬，如姑、錄等代替鐵 作為催化劑使用’也可用其他碳氫化合物，如甲垸、乙婦等代替乙块作 為碳源氣使用。 . 將由上述步所得祕施置於—健力為5xi『3pa之纽系統. I ’於二電極30間外加電壓後’碳奈米管燈絲2〇6開始發出白織光，並隨 著电疋之:^加电光冗度增加’電流也持續增加，碳奈米管燈絲施於 .8V(、勺lGmA)日$可持_發出白熾光丨丨小時。將碳奈米管燈絲施取p 後，奴奈米官燈絲206比未發光前更堅硬及具有彈性。 由於發光過程中之高溫熱處理過程使碳奈米管燈絲施之抗張強度 及導電性能都有增強，因此可通制量發光前後碳奈米管燈職kiv 曲線及抗張強度研究碳奈米管燈絲206之變化。 重複上述步驟1〜3得到另一根碳奈米管燈絲。請參閱第四圖，將其於 =中未發光前之卜V曲線(如曲齡所示）用吉時卿制濁測 里儀。己錄下來’紐’外加冒之直流電壓使其發献小時，再次測量其 200407939 ^曲線’發現沒有明顯變化(如曲細所示）；再· 光=先期輸隨時間之增長持續增加，細、時後 始^ 冷卻，再次測量其卜叫舆未發光前之1娜相比 二Γ禮4加約13%(如曲線C所示）。由變形測量儀測得發光前後使碳 示/、官燈纖_所需力分縣_及6.姻，由此表明，碳奈米管燈絲 206於外加7㈣之直流電愿發光3小時後其抗張強度增加約6倍。、 由於發光前後碳奈米管燈絲之結構發生變化，同時於發光過程中， =碳奈米管_4之相鄰碳奈米管細之接觸處（請參閱第三圖）之# 间電阻/溫度係數會產生較高之溫度，從而更易於引起結構發生變化，因 此發光前後碳奈歸燈·6之導條能及抗張财均有所增強。 本發明之碳奈米管㈣具有低電阻率、貞溫度電_數及高比表面. 狀優點’為_—蚊之白熾溫度及發光亮度，本發g狀碳奈米管燈. 糸車乂白矣五屬k絲需求之電能更少’而且碳奈米管具有六圓環狀之穩定 結構’其於較向溫度下也不胃發生變化而能穩定存在。 綜上所述’本發明符合發明專利要件，爰依法提出專利申請。惟| 以上所述者僅為本發明之較佳實關，舉凡熟悉本案技藝之人士，於援 依本案發明精神所作之等效修飾賴化，皆應包含於町之申請專利範 圍内。 & □續次頁（發明說明頁不敷使用時，請註記並使用續頁） 10200407939 发明, Description of the invention Content, actuality, and belonging to the technical field 'Prior art' [Field of the invention] The present invention relates to a filament and a method for preparing the same, and relates to a filament for a material and a method for preparing the same. Tintin g Ke [Background of the Invention] Sand lamp light filaments are naturally polycrystalline, amorphous or amorphous materials, but these materials become brittle and fragile at high temperatures for a long time. ， 真 = ^ __ 的 金 _ 在 __, because of its crystal 耱: • at higher temperatures ^ and · life days Γ ,,,, ° crystals, thereby increasing the fragility of metal filaments and reducing strong money filaments The other disadvantage is that the resistivity is low. Sometimes in order to increase its resistance, it takes a long time: to reduce the size of the bulb, the metal filament must be tightly wound, and the entangled parts are tangled with each other, so the light emitting area of the filament Reduced, the filament luminous efficiency is reduced. Metal filaments, especially tungsten filaments, also have the disadvantage of higher resistance / temperature coefficients, from room temperature to deletion. The range of c. The resistance value is increased by six times, so that in order to obtain the same luminous efficiency, the amount of miscellaneous electric energy is more 0. [Objective of the Invention] A pound of 1C The purpose of this month is to provide a high stability at higher temperatures Filament with specific surface area. Another object of the present invention is to provide a method for preparing a filament with high stability and high ratio. 6 200407939 [Inventive Features] The filament provided by the present invention includes a carbon nanowire and two electrodes. Description of the invention, continuation of the electrode, the carbon nanotube wire is wound to break the nano tube array; between the poles, a filament is obtained [preferred embodiment] Please refer to the figure-the filament of the present invention contains carbon nano 30. The carbon nano tube 204 is wound between the two electrodes 30. As a further improvement of the present invention, it is possible to apply silver dispensing 32 at the carbon nanotube to reduce the resistance of the contact point. The invention provides a method for preparing a carbon nanotube tube filament, which includes the following steps: Step 1: Refer to the second figure to prepare a carbon nanotube tube array 20, and the specific process is as follows. A substrate 22 is prepared. The substrate 22 includes a stone wafer 222 with a diameter of 5.1 cm and a thickness of 1200. The silicon wafer 222 is deposited with a 800 nm-thick dioxide dioxide layer 224. The silicon dioxide Xi | 224 surface is processed to be flat and smooth to suit the growth of carbon nanotube arrays. The old electron beam deposition method was formed on the substrate 22-iron thickness 24 with a layer thickness of 5nm, and then annealed between the temperature and the side C. It is treated for about 10 hours to form an iron oxide film, and then this iron oxide film is reduced to elemental iron film 24 using radon gas or ammonia gas as a catalyst; the substrate 22 on which the catalyst iron thin film 24 is deposited is cut into a rectangular shape. Block, put one of them into a quartz reaction boat (not shown), and then send this quartz reaction boat to the center of a 2.54cm quartz reaction furnace (not shown); pass in argon while heating the reaction furnace to 650 ~ 700 C; then pass in a mixture of 30 sccm acetylene and 300 sccm argon 7 200407939 Description of the invention; continuation sheet; after 5 minutes of reaction, the reaction furnace is cooled to room temperature, and carbon nanomaterials are formed on the wire 22. , V & 2 π ′, as shown in the first figure, the carbon nanotube wire 204 is pulled out from the carbon nanotube array 2. After the carbon nanotube array is obtained, use a pull-out fixture such as tweezers (not shown) to clamp a bundle of carbon nanotubes 2G2 to pull. Due to the van der Waals force between the carbon nanotubes, the carbon The ends of the nano tube bundle are connected end to end to form a carbon nano tube wire 204. Step 3: Please refer to Figure-. Use a uniform external force to wind carbon nano tube wire 204 on two metal wires that are used as the two electrodes 3 at a certain distance from each other. Then place a silver dot on the 3rd electrode of the county's rice tube to reduce the resistance of the contacts, that is, obtain a thin filament that can emit light under an applied voltage. To obtain a carbon nano tube array that can pull out carbon nano tube filaments 204, it is necessary to meet the solid. Growth conditions: a. The surface of the substrate is flat and smooth; b. The growth rate of the carbon nano tube is high; c. Carbon The partial pressure of source gas is low. | Pingxian, the base surface _ Yu grows high-density carbon nanomaterials, so the close vandval force between the carbon nanotubes can ensure that the carbon nanomaterials are gathered into bundles and drawn into filaments. The growth conditions b and e can increase the growth rate of the carbon nanotubes and lower the growth rate of the amorphous carbon. Therefore, it is possible to avoid growing carbon nanotubes on the wall of the carbon nanotubes while reducing the carbon growth. Nano pure van der Waals force. Because the growth of carbon nanomaterials is proportional to the temperature difference between the reaction and the catalytic donation, the temperature difference needs to be sufficiently high to increase the growth of carbon nanomaterials. The rate book must at least control the temperature difference between the reaction furnace and the catalyst to 50%.匸 Above. During operation, the catalysis of 200407939 shows that the stomach temperature can be controlled by the source gas, and the temperature of the reaction furnace can be directly controlled. The partial pressure of the carbon source gas can be controlled by adjusting the flow rate and flow ratio of the carbon source gas and the argon gas. Generally, the partial pressure of the carbon source gas is not higher than 0.2, preferably not higher than 0.1 J. The width of the carbon nano tube wire 204 is determined by the tip size of the drawing tool. The smaller the tip size, the smaller the width of the conventional slave nano wire 204. The strength of pulling carbon nanotube wire 204 is determined by the visibility of carbon nanotube 204. The larger the width, the greater the force required. The length of the carbon nanotube wire depends on the area of the carbon nanotube array 20. In addition, when growing carbon nanotube arrays, other inert gases such as nitrogen and helium can be used instead of argon as a protective gas, and other transition metals, such as iron and copper, can be used instead of iron as a catalyst. Hydrocarbons, such as formazan, otochi, etc., are used instead of block B as the carbon source gas. Put the secret obtained from the above step in the Jianli 5xi "3pa of the button system. I" After applying voltage between the two electrodes 30 "carbon nanotube filament 206 began to emit white weave light, and with the electric power No .: ^ Increased power redundancy increases the current and the current continues to increase. Carbon nanotube filaments are applied at .8V (, spoon 1GmA) per day and can be held _ emitting incandescent light 丨 丨 hours. After the carbon nanotube filament is applied to p, the slave nanofilament filament 206 is harder and more flexible than before the light is emitted. Since the high temperature heat treatment process in the luminescence process enhances the tensile strength and electrical conductivity of carbon nanotube filaments, the kiv curve and tensile strength of carbon nanotube lamps before and after luminescence can be researched. Changes in filament 206. Repeat steps 1 to 3 to obtain another carbon nanotube filament. Please refer to the fourth figure, and use the turbidity measuring instrument made by Ji Shiqing to compare the V curve (as shown by Qu Ling) before the light emission. I have recorded the "new button" plus the DC voltage to make it donate hours, and measured the 200407939 ^ curve again and found that there is no significant change (as shown in the curve); then, the light = the previous input continues to increase over time. After that, let it cool down, and then measure its Na Na before the luminescence before the luminous phase, plus about 13% compared to the two Γ Li 4 (as shown in curve C). Measured by the deformation measuring instrument before and after the light emission, the carbon indicator, and the official lamp fiber _ required force points _ and 6. marriage, which shows that the carbon nanotube filament 206 plus 7 ㈣ DC power is willing to emit light for 3 hours after its resistance The tensile strength is increased about 6 times. 、 As the structure of the carbon nanotube filament changes before and after light emission, at the same time, during the light emission process, the contact between the thin carbon nanotube tube_4 and the adjacent carbon nanotube tube (see the third figure) The temperature coefficient will produce a higher temperature, which is more likely to cause structural changes. Therefore, the carbon nano-reduction lamp · 6's guide bar energy and Zhang Cai's resistance are enhanced before and after light emission. The carbon nanotube of the present invention has a low resistivity, a high temperature and a high specific surface. The advantages are: the incandescent temperature and luminous brightness of mosquitoes, the g-shaped carbon nanotube lamp of the present invention.矣 The five k-wires require less electricity 'and the carbon nanotube has a six-ring-shaped stable structure', which can stably exist even if the stomach does not change at higher temperatures. In summary, the present invention complies with the elements of the invention patent, and the patent application is filed according to law. However, the above is only a good practice of the present invention. For those who are familiar with the skills of this case, the equivalent modification of Lai Hua in accordance with the spirit of the invention of this case should be included in the scope of Macao's patent application. & □ continued page (if the description page of the invention is insufficient, please note and use the continued page) 10