1290535 九、發明說明： 【發明所屬之技術領域】 本發明「高純度石墨碳材之製造方法」旨在提供一 用乂‘ &向純度石墨碳材之方法，藉以獲得更能符合機 械、冶金、化學、電氣、航太以及核工業使用需求之石 墨碳材。 【先前技術】 按，石墨乃雖然屬於非金屬礦物，但卻具有金屬化 合物之特性，茲就石墨之特性客觀、簡要說明如下·· 1、耐高溫及特殊的熱性能，石墨的熔點為385(rc， 1點為425(TC，比高溫之王鎢高得多，石墨在超高溫之 备、件下不軟化，而且強度反而增高，在252〇它時，其抗 拉強度比常溫高-倍，另外，石墨的熱膨脹係數很小，在 溫度驟變時，體積變化不大，具有良好的抗熱震性能，故 成為最耐高溫的輕質元素之一。 2、優良的導電和導熱性，石墨的導電導熱性不亞於 金屬’它比不錄鋼大4倍，比碳素鋼大2倍，比錯大3〜 3· 5倍，比其他非金屬約高1〇 〇倍，其導電導熱性和 石墨化程度有關，石墨化純度越高，導電性能越好，但石 墨的導熱性又和金屬不同，隨荽、、w> , B 、、 · + υ I返者μ度的升高，導熱係數不 疋增加而疋減小’在極高、黑_主 、， 孤度#，則趨於絕熱狀態，如將 石墨置於磁場中，加溫力σ屡則可制 ^^^ ^^ 衣成定向石墨，其順向的 導電率比反向導電率高1〇〇Ω 丄υ υ υ倍，稱之為各向異性。 1290535 3、 潤滑性，石墨的潤滑性能類似於二硫化錮，在潤 滑介質中石墨的摩擦係數為〇 . 1以下，鱗片越大摩擦係 數越小，潤滑性能越好，在氣體、液體、韌體物質或結晶 狀物質中，均具有良好的对磨性，而且潤滑性能不受溫度 影響。 4、 塗敷性及可塑性，石墨能牢固地黏附在固體表面 不易脫落，粒度越小黏力越強，另外石墨的可塑性很好， 可加工成複雜之形狀。 5、 化學穩定性，石墨在常溫下具有良好之化學穩定 性，能耐任何強酸、強鹼及有機溶劑之浸蝕，其化學穩定 性和其純度、溫度有關，石墨在低溫時氧化速度較慢，當 溫度達到400°C時開始氧化，溫度越高氧化速度越快，因 此在空氣中石墨製品的使用溫度不宜超過500°C。 6、 其他，石墨是一種脆性材料，其抗沖擊及抗拉強 度較差，如此之性能取決於石墨之種類及加工方法，一般 石墨製品的強度為抗壓強度〉抗彎強度〉抗拉強度，其差值 為二的倍數，由於測定抗壓強度較為方便，因此一般只測 其抗壓強度，石墨又軟又硬，水平方向硬度為二可在紙上 劃出條痕，而垂直方向硬度很高，硬到可使金鋼石刀具損 壞。 也因為石墨具有上述優異之特性，而使得石墨製品廣 泛應用於機械、冶金、化學、電氣、航太以及核工業，甚 至於可做成玻璃及造紙業的拋光劑、防腐塗料、防銹、鍋 爐防垢、油漆填充料、覆寫紙、鞋油等原料。 1290535 再者，由於石墨碳材之純度將直接影響其性能之表 現，因此業界不斷的在研發可以製造高純度石墨碳材之方 法，而目前業界所知悉者如：台灣專利公告號424079號「高 強度、高密度大型石墨碳材之製造方法」，其係一種利用 在液晶介向粉末中混合適罝經過碳化處理之液晶介相粉 末並壓結成型，再依序進行真空低溫碳化、高溫碳化以及 最後石墨化處理之方法，以期能提高大型石墨碳材之機械 強度及密度，並降低大型粉末壓結胚體碳化時間及避免碳 化破裂現象。 惟，其液晶介相粉末與液晶介相碳化粉末係未經純 化處理便直接進行碳化，將使得成品因雜質多而純度不 夠，且其成份本身内含之雜質將隨碳化之氣體造成氣 泡，其氣泡所形成之空洞將使石墨碳材之強度降低。 【發明内容】 本發明「高純度石墨碳材之製造方法」，乃係先分別 將焦碳微粒加熱，以及將瀝青加熱，接著將焦碳微粒與瀝 青以9. 8 : 1之比例均勻混合並壓成胚料，並將胚料以真空 加熱方式加熱令胚料内之結晶均勻化之後，將胚料放置於 氣氛爐中加熱使之再純化，該純化後之胚料則在經過含浸 瀝青，再經持續加熱至石墨化後，最後緩慢冷卻至常溫即 可成為南純度之石墨碳材。 尤其，胚料係在内部結晶均勻化之後，再放置於氣氛 爐中加熱至2000°C以進行再純化，並且將再純化之胚料 !29〇535 構強Ι填補胚料表面之”，增加胚料結 以及^至於可反覆進行胚料内部結晶均勾化、再純化 度。胚料含浸遞青之步驟，藉以增加整體石墨碳材之密 【實施方式】 敕使θ番查委員清楚本發明之結構組成，以及 正脰運作方式，茲配合圖式說明如下： 本兔明「咼純度石墨碳材之製造方法」，1整f π f 驟： 私如弟一圖所示，係依序包括下列步 係由ttr微粒加熱至8啊〜麵，其焦碳微粒 隹^私末粉碎至以粒度約在0 001〜0 003_ 焦石反被粒所加熱而成。 B、 將瀝青加熱至5〇〇°c〜7〇〇π C、 將焦碳微粒與瀝青以9.8: 1之比例均勻混人， 亚以85,34G〜113,78_心之屋力加麼成胚料。ϋ D、 將胚料以真空加熱方式加熱至i彻。c〜⑽代 知績二十四小時，令胚料内之結晶均勻化。 200(TC令其胚料再2化之胚似置於氣氛爐中加熱至 F 純化之胚料含浸青，因為㈣在純化過程 :表：胃因為氣泡作用而形成空洞，故可藉由瀝青埴補 胚料之空洞，以增加胚料結構強度。 1290535 G、將含浸瀝青後之胚料加熱至2500°C〜3000°C持 續一百二十小時，令胚料石墨化。 Η、將石墨化之胚料以每小時100°C之冷卻速率緩慢 冷卻至常溫即獲得純度為99. 9%以上之高純度石墨碳材。 如上所述，由於胚料在内部結晶均勻化之後，係再放 置於氣氛爐中加熱至2000°C以進行再純化，並且將再純化 之胚料含浸瀝青，以利用瀝青填補胚料表面之空洞，增加 胚料結構強度，甚至於可反覆進行胚料内部結晶均勻化、 再純化以及胚料含浸瀝青之步驟，藉以增加整體石墨碳材 之密度，因此可獲得強度為150Mpa以上之高強度、密度為 1.85〜1.95g/cm3之高密度石墨碳材，而可應用於機械工業 之潤滑、冶金工業之耐火材料、化學工業之反應爐、電氣 工業之電極或碳管、核工業之減速劑、航太工業之喷嘴等 範圍，而更能符合機械、冶金、化學、電氣、航太以及核 工業使用之需求。 以上之實施說明及圖式所示，係本發明較佳實施例之 一者，並非以此侷限本發明，是以，舉凡與本發明之構造、 裝置、特徵等近似、雷同者，均應屬本發明之創設目的及 申請專利範圍之内。 1290535 【圖式簡單說明】 第一圖係為本發明一較佳實施例之製造流程圖。 【主要元件代表符號說明】 41290535 IX. Description of the Invention: [Technical Field of the Invention] The "manufacturing method of high-purity graphite carbon material" of the present invention aims to provide a method for purifying graphite carbon material by using 乂' & to obtain a more suitable mechanical, metallurgical Graphite carbon materials used in chemical, electrical, aerospace and nuclear industries. [Prior Art] According to the fact that graphite is a non-metallic mineral, it has the characteristics of a metal compound. The objective and brief description of the characteristics of graphite is as follows: 1. High temperature resistance and special thermal properties. The melting point of graphite is 385 ( Rc, 1 point is 425 (TC, much higher than the king of high temperature tungsten, graphite does not soften under ultra-high temperature, and the strength is increased, at 252 〇, its tensile strength is higher than normal temperature - times In addition, graphite has a small coefficient of thermal expansion, has little change in volume when the temperature suddenly changes, and has good thermal shock resistance, so it is one of the lightest elements with the highest temperature resistance. 2. Excellent electrical and thermal conductivity, The electrical and thermal conductivity of graphite is no less than that of metal. It is 4 times larger than non-recorded steel, 2 times larger than carbon steel, 3 to 3.5 times larger than the error, and about 1 times higher than other non-metals. The thermal conductivity is related to the degree of graphitization. The higher the graphitization purity, the better the conductivity. However, the thermal conductivity of graphite is different from that of metal. With the increase of μ degree, w, w> , B , , · + υ I return , the thermal conductivity does not increase and the 疋 decreases 'at very high, black _ main , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , 1〇〇Ω 丄υ υ υ times, called anisotropy. 1290535 3, Lubricity, graphite lubrication performance is similar to bismuth disulfide, the friction coefficient of graphite in the lubricating medium is 〇. 1 or less, the larger the scale The smaller the friction coefficient, the better the lubrication performance, and the good the grinding property in gas, liquid, tough substance or crystalline material, and the lubrication performance is not affected by temperature. 4. Coating and plasticity, graphite energy Firmly adhered to the solid surface, it is not easy to fall off. The smaller the particle size, the stronger the viscosity. In addition, the plasticity of graphite is very good and can be processed into a complex shape. 5. Chemical stability, graphite has good chemical stability at normal temperature and can withstand any The corrosion of strong acid, strong alkali and organic solvent is related to its chemical stability and its temperature. The oxidation rate of graphite is slow at low temperature. When the temperature reaches 400 °C, oxidation begins. The higher the temperature, the faster the oxidation rate. The use temperature of the graphite product in the air should not exceed 500 ° C. 6. Other, graphite is a brittle material, its impact resistance and tensile strength is poor, such performance depends on the type and processing method of graphite, general graphite products The strength is compressive strength>bending strength>tensile strength, and the difference is a multiple of two. Since the compressive strength is convenient, generally only the compressive strength is measured, the graphite is soft and hard, and the hardness in the horizontal direction is two. Streaks can be drawn on the paper, and the hardness in the vertical direction is very high, so that the diamond cutter can be damaged. Because graphite has the above-mentioned excellent characteristics, the graphite products are widely used in machinery, metallurgy, chemical, electrical, and aviation. Taihe and the nuclear industry can even be used as polishing agents, anti-corrosion coatings, anti-rust, boiler anti-scaling, paint filling materials, overwriting paper, shoe polish and other raw materials in the glass and paper industry. 1290535 Furthermore, since the purity of graphite carbon material will directly affect the performance of its performance, the industry is constantly developing methods for producing high-purity graphite carbon materials, and the industry is known as: Taiwan Patent Bulletin No. 424079 "High A method for producing a high-density large-sized graphite carbon material, which is a liquid crystal phase-phase powder which is mixed with a carbonized medium in a liquid crystal-mediated powder and is subjected to kneading, followed by vacuum low-temperature carbonization, high-temperature carbonization, and the like. Finally, the method of graphitization is to improve the mechanical strength and density of large graphite carbon materials, and reduce the carbonization time of large powder compacted body and avoid carbonization cracking. However, the liquid crystal phase-phase powder and the liquid crystal phase-phase carbonized powder are directly carbonized without purification, which causes the finished product to be insufficiently pure due to impurities, and the impurities contained in the component itself will cause bubbles with the carbonized gas. The void formed by the bubbles will reduce the strength of the graphite carbon material. The present invention is a method for producing a high-purity graphite carbon material, which is to separately heat the coke particles and heat the asphalt, and then uniformly mix the coke particles with the pitch at a ratio of 9.8:1. After pressing into a billet and heating the billet by vacuum heating to homogenize the crystal in the billet, the billet is placed in an atmosphere furnace and heated to be repurified, and the purified billet is subjected to impregnated asphalt. After continuous heating to graphitization, it is finally cooled to normal temperature to become a graphite carbon material of southern purity. In particular, after the internal crystals are homogenized, they are placed in an atmosphere furnace and heated to 2000 ° C for re-purification, and the re-purified billet is added to the surface of the billet. The billet knot and the re-purification of the internal crystal of the billet can be repeated. The step of impregnating the billet to increase the density of the whole graphitic carbon material [embodiment] The structural composition and the correct operation mode are as follows: The rabbit Ming "How to make 咼 purity graphite carbon material", 1 whole f π f Step: As shown in the figure of the brother, the system includes The following steps are heated by ttr particles to 8 ah ~ face, and the coke particles 私 私 私 私 私 私 私 私 私 私 私 私 私 私 私 私 私 私 私 私 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 B. Heat the asphalt to 5〇〇°c~7〇〇π C, mix the coke particles and asphalt in a ratio of 9.8:1, and add 85,34G~113,78_heart to the house. Seed material. ϋ D. Heat the billet to a vacuum by vacuum heating. c~(10) Generation The performance is 24 hours, which makes the crystal in the billet uniform. 200 (TC makes the embryo of the billet re-formed in the atmosphere furnace to be heated to F. The purified billet is impregnated with blue, because (4) in the purification process: Table: The stomach forms a cavity due to the action of bubbles, so it can be made by asphalt Fill the void of the blank to increase the structural strength of the blank. 1290535 G. Heat the billet after impregnating the asphalt to 2500 ° C ~ 3000 ° C for one hundred and twenty hours to make the billet graphitized. The raw material is slowly cooled to a normal temperature at a cooling rate of 100 ° C per hour to obtain a high-purity graphite carbon material having a purity of 99.9% or more. As described above, since the billet is internally crystallized, it is placed again. The atmosphere furnace is heated to 2000 ° C for re-purification, and the re-purified billet is impregnated with bitumen to fill the voids on the surface of the billet with asphalt, increase the structural strength of the billet, and even repeat the internal crystal homogenization of the billet. And re-purification and the step of impregnating the aggregate with the bitumen to increase the density of the whole graphite carbon material, thereby obtaining a high-density graphite carbon material having a high strength of 150 Mpa or more and a density of 1.85 to 1.95 g/cm 3 , which can be applied to mechanical Lubrication in the industry, refractory materials in the metallurgical industry, reactors in the chemical industry, electrodes or carbon tubes in the electrical industry, speed reducers in the nuclear industry, nozzles in the aerospace industry, etc., and more in line with mechanical, metallurgical, chemical, electrical, Aerospace and the needs of the nuclear industry. The above description and the drawings are shown as one of the preferred embodiments of the present invention, and are not intended to limit the present invention, so that the structure, device, and features of the present invention are The approximation and the similarity are all within the scope of the invention and the scope of the patent application. 1290535 [Simplified description of the drawings] The first figure is a manufacturing flow chart of a preferred embodiment of the present invention. Description] 4
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