200900541 九、發明說明： 【發明所屬之技術領域】 本發明是有關於一種製備鋁•鐘化合物之方法，且特別 是有關於一種製備高鐘含量之銘-鐘化合物的方法。 【先前技術】 由於銘-裡（AlLi)化合物在製備上有一定的難度，盆製 、 成之合金成分不易控制’因此目前的應用尚不普遍。過去 的鐵·鋰（FeLi)化合物、銅-鐘（CuLi)化合物等製備方法，一 般都是在真空或具保護氣氛之反應室内進行球磨法製 備，強迫金屬粉末與鋰粒混合在一起，其製程不但耗時更 耗能源。此外，由於鋁粉及鋰粒皆具備高活性，以上述方 法製備#S -經化合物極具困難度，可行性低。 目前一般是將純鋰在真空環境下加入鋁熔湯製備鋁-鋰化合物，然而鋰金屬之活性強，周遭的些微濕氣皆可能 〇 造成鋰的瞬間氣化，使得熔煉過程不僅困難且危險性高。 此外，由於純鋰活性大，在運送、儲存的過程中極為 危險，因此純鋰的價格高低取決於運送的方式，對於不生 產鋰礦而需仰賴進口的地區來說，亦是無法降低成本的原 因之一。 【發明内容】 因此本發明就是在提供一種高鋰含量之鋁_鋰化合物 的製備方法’用以解決傳統鋁_鋰化合物製備方法之危險性 5 200900541 高、原料運送及儲存成本高的問題。 根據本發明之-種高鐘含量之銘·鋰化合物的製備方 法，包含提供一電解槽，其陰極為銘材，電解槽裝有一電 解液’電解液包含氯化鐘、氯化鉀及氯储。其中，氯化 經提供鐘來源，而氯化鉀主要作為助炼劑，藉以降低電解 液溫度，並增加電解液流動性。 在大氣環境下，施加電流密度為每單位陰極面積〇〇8 〜0.1安培之電流於380〜55(rc之電解液令，進行一電解 擴散反應。於尚溫下，電解液中所含之鋰原子可還原於陰 極之鋁表面’並擴散入陰極之鋁材内部，形成鋁-鋰化合物。 鋁陰極表面及次表面的鋰含量隨著時間而增加，當鋰 含量到達約50 Wt% (A1-50wt.% Li)時（以電解液溫度為 500 C為例），紹-鐘化合物為液態。利用銘-鐘液態金屬的 密度低於熔融的電解液密度，鋁-鋰液態金屬會浮在電解液 之液面上，將此鋁-鋰液態金屬撈出，使用模具或直接凝固 後即可得到高鐘含量之鋁-鐘化合物。 本發明提供一種製備高鋰含量之鋁-鋰化合物的方 法’以銘作為電化學反應之陰極，於含鋰之電解液中進行 電解反應，使鋰原子還原並沉積於陰極材料上，隨著鐘含 里增加’可形成铭_鍾液態金屬’凝固後即可得到高鐘含旦 之鋁-鋰化合物，為一種安全且簡便的製備方法，由於使用 之原料為氣化鋰’具有穩定的化學活性可方便運輸、儲 存’更可降低鋁-鋰化合物的生產成本，増加其應用範圍。 200900541 【實施方式】 請參照第1圖，係繪示本發明之實施例的一種製備高 鋰含量之鋁-鋰化合物的步驟流程圖。 依照本發明之實施例，製備高鋰含量之鋁-鋰化合物的 步驟包含提供一電解槽及一電解液，將電解液之溫度維持 在約380°C〜550°C以上之高温，施加一電流於電解液，電 流密度為每單位陰極面積（cm2)流通0.08〜0.1安培，進行 電解擴散反應，使電解液之鋰離子還原於陰極而形成鋰原 子，該鋰原子擴散入陰極鋁材内，當鋰含量愈來愈高而形 成鋰-鋁金屬液體浮於電解液之液面上，撈出該鋰-鋁金屬 液體，凝固後形成鋁-鋰化合物。 依照本發明之一實施例，電解槽包含一陰極及一陽 極，陰極之材料為鋁，用以使鋰原子還原於其上並形成鋁 -鍾化合物。 參照第2圖，為本發明之一實施例的電解槽結構示意 圖。電解槽200包含一外槽體210及一内層220，内層220 為高温隔熱材質，例如氧化鋁；外槽體210上方具有一頂 蓋211，頂蓋211為可動式。電解槽200中具有一支撐板 221，置於内層220内之底部，一容器230設於支撐板221 上。容器230可為鋼製，容器230中盛裝有上述之電解液 241 ° 容器230周緣設有一加熱器250，容器230内包含一 熱電偶260、一陽極242及一陰極243，加熱器250用以 加熱電解液241，使電解液維持在適當之工作溫度，促使 7 200900541 電解液中之鋰原子還原並擴散入陰極材料内。熱電偶260 置於容器230内並浸入電解液241中，用以偵測電解液241 之溫度。陽極242及陰極243設置於容器230内，並部分 浸置於電解液241中。陰極243以陰極支撐架244支撐。 陰極243之材料為一鋁材，陽極242之材料可為石墨棒、 高分子複合材料或合金。 依照本發明之一實施例，電解液可包含氯化鋰、氯化 鉀及氯化鈣。其中電解液之組成份包含20〜40 wt%之氯化 鍾、30〜50 wt%之氯化钟及10 wt°/〇以下之氯化#5。氯化鍾 係提供鋰來源，而氯化鉀主要作為助熔劑，藉以降低電解 液溫度，並增加電解液流動性。 依照本發明之一實施例，電解擴散反應進行之條件包 含：電流密度為每單位陰極面積（cm2)流通0.08安培，電 解液之溫度維持在約500°C，可使電解液之鋰原子還原於 陰極上。隨著鋁-鋰化合物之鋰濃度提高，達到約55%時會 形成鋁-鋰化合物之液態金屬。 由於鋁-鋰化合物之液態金屬密度小於熔融之電解 液，因此會浮在電解液液面上，將此銘-鍾化合物之液態金 屬撈出直接凝固或以模具成型，可得到成分介於 Al-40wt.°/〇 Li至Al-62wt.% Li之間的鋁-鋰化合物，由於鋰 含量相當高，無法以目前現有的儀器量測其含量，因此鋁 -鋰化合物之成分測定可根據相圖來推測。 參照第3圖，為鋁-鋰金屬之相圖，圖中縱軸為溫度， 下橫軸為链在紹中的原子百分比，而上橫軸為鋰在銘中的 8 200900541 重罝百分比；本發明實施例之内容皆採重量百分比來說 明。以本發明實施例所揭露最佳操作溫度範圍為例，如第 3圖二示’例如當溫度55〇〇c時，陰極紹材表面所含有的 鋰3置重s百分比達41%時，該鋁材表面已達第3圖中所 了、 A1液態區。由於紹密度為2.74 g/cm3，而鐘的密度 為〇. 54 g/cm3 ’因此可推測上述之Al_4丨％ u液態金屬的ς 度=1.84g/cm3,高於電解槽中液態鹽密度（約2g/cm3)， 故田Al-Li液態金屬於陰極表面產生時，因其密度較低而 浮出液面。所以持續的於電解槽中施加適當的電流密度， 貝J Al-Li液態金屬亦持續的產出而浮出電解液面，以供撈 取。 依上述方法製成之紹_鐘化合物的金屬性質穩定，可存 放於大氣％境下，大幅減低存放純鐘所需顧慮的安全問 通此外將尚鐘含量之鋁-鐘化合物放置於水中，隨著放 置時間渐增’成型之叙_鐘化合物會與水進行激烈之反應， 亦可證實高含量的鋰存在於鋁-鋰化合物中。 電解液中之其他成分，例如鉀，由於與鋁（陰極材料） =親和性極差’故依本發明方法製備之銘-鐘化合物的卸含 量小於50 ppn^鋁_鋰化合物可能具有少量之雜質，例如 鈉’為-般氣化鹽類中常見_f。經定量分析，以本發 明製備之鋁-鋰化合物的鈉含量小於3〇ppm。 雖然本發明已以一較佳實施例揭露如上，然其並非用 以限定本發明’任何熟習此技藝者，在不脫離本發明之精 神和範圍内，當可作各種之更動與潤飾，因此本發明之保 200900541 護範圍當視後附之申請專 專利範園所界定者為準。 【圖式簡單說明】 為讓本發明之上述和其他目的 能更明顯易f董，所附圖式之詳細說明如下、.優點與實施例 第1圖係績示表發明之實施例的—種製備高链 鋁·•鋰化合物的步騍流程圖。 夂 第2圖為本發明之〆實施例的電解槽結構示意圖 第3圖為|呂_鐘金屬之相圖。 210 :外槽體 220 ·•内層 230 :容器 242 :陽極 244 :陰極支撐架 260 :熱電偶 【主要元件符號說明】 200 :電解槽 211 :頂蓋 221 :支撐板 241 :電解液 243 :陽極 250 :加熱器200900541 IX. INSTRUCTIONS OF THE INVENTION: TECHNICAL FIELD OF THE INVENTION The present invention relates to a method of preparing an aluminum clock compound, and more particularly to a method of preparing a high clock content of an inscription-bell compound. [Prior Art] Since the Al-Li compound has difficulty in preparation, the composition of the pot and the alloy is difficult to control. Therefore, the current application is not yet widespread. In the past, iron-lithium (FeLi) compounds, copper-bell (CuLi) compounds and the like are generally prepared by ball milling in a vacuum or protective atmosphere, forcing metal powder and lithium particles to be mixed together. Not only is it time consuming and energy consuming. In addition, since aluminum powder and lithium particles have high activity, it is extremely difficult to prepare #S-processed compounds by the above method, and the feasibility is low. At present, pure lithium is added to aluminum melt in a vacuum environment to prepare an aluminum-lithium compound. However, the activity of lithium metal is strong, and some micro-humidity around it may cause instantaneous vaporization of lithium, making the melting process not only difficult and dangerous. high. In addition, due to the high activity of pure lithium, it is extremely dangerous in the process of transportation and storage. Therefore, the price of pure lithium depends on the mode of transportation. For regions that do not rely on imports for producing lithium ore, it is impossible to reduce costs. one of the reasons. SUMMARY OF THE INVENTION Accordingly, the present invention is to provide a method for preparing a high lithium content aluminum-lithium compound to solve the problem of the conventional aluminum-lithium compound preparation method. 5 200900541 High, high material transportation and storage cost. The method for preparing a lithium compound according to the present invention comprises the provision of an electrolytic cell, the cathode of which is a name material, and the electrolytic cell is provided with an electrolyte. The electrolyte contains a chlorination clock, potassium chloride and chlorine storage. . Among them, chlorination provides a clock source, and potassium chloride is mainly used as a refining agent to lower the temperature of the electrolyte and increase the fluidity of the electrolyte. In the atmosphere, the current density is 〇〇8 ～0.1 amps per unit cathode area at 380~55 (rc electrolytic solution, an electrolytic diffusion reaction is carried out. At room temperature, the lithium contained in the electrolyte The atom can be reduced to the aluminum surface of the cathode and diffused into the aluminum of the cathode to form an aluminum-lithium compound. The lithium content of the surface and subsurface of the aluminum cathode increases with time, when the lithium content reaches about 50 Wt% (A1- 50wt.% Li) (for example, the electrolyte temperature is 500 C), the Shao-Chung compound is liquid. The density of the liquid metal in the Ming-Qing is lower than the density of the molten electrolyte, and the aluminum-lithium liquid metal floats on the electrolysis. On the liquid surface of the liquid, the aluminum-lithium liquid metal is taken out, and the aluminum-bell compound having a high clock content can be obtained by using a mold or directly solidified. The present invention provides a method for preparing a high lithium content aluminum-lithium compound. Taking Ming as the cathode of the electrochemical reaction, the electrolytic reaction is carried out in the lithium-containing electrolyte to reduce and deposit the lithium atoms on the cathode material, and the solidification of the clock can be formed by the addition of the liquid crystal Get high clock The aluminum-lithium compound is a safe and simple preparation method, and the raw material used is gasified lithium, which has stable chemical activity, can be conveniently transported and stored, and can reduce the production cost of the aluminum-lithium compound, and the application range thereof. [0086] [Embodiment] Referring to Figure 1, there is shown a flow chart of a process for preparing a high lithium content aluminum-lithium compound according to an embodiment of the present invention. According to an embodiment of the present invention, a high lithium content aluminum is prepared. The step of the lithium compound comprises providing an electrolytic cell and an electrolyte, maintaining the temperature of the electrolyte at a high temperature of about 380 ° C to 550 ° C or higher, applying a current to the electrolyte, and the current density is per unit cathode area (cm 2 ). Circulating 0.08~0.1 amps, performing electrolytic diffusion reaction, reducing lithium ions of the electrolyte to the cathode to form lithium atoms, the lithium atoms diffusing into the cathode aluminum material, and forming a lithium-aluminum metal liquid float when the lithium content is higher and higher The lithium-aluminum metal liquid is removed from the liquid surface of the electrolyte and solidified to form an aluminum-lithium compound. According to an embodiment of the invention, the electrolytic cell comprises a cathode and The material of the anode and the cathode is aluminum for reducing lithium atoms thereon and forming an aluminum-bell compound. Referring to Fig. 2, there is shown a schematic structural view of an electrolytic cell according to an embodiment of the present invention. The electrolytic cell 200 comprises an outer tank body. 210 and an inner layer 220, the inner layer 220 is a high temperature heat insulating material, such as alumina; the top of the outer tank body 210 has a top cover 211, and the top cover 211 is movable. The electrolytic cell 200 has a support plate 221 disposed on the inner layer 220. A container 230 is disposed on the support plate 221. The container 230 may be made of steel, and the container 230 is filled with the electrolyte 241 °. The periphery of the container 230 is provided with a heater 250, and the container 230 includes a thermocouple 260. An anode 242 and a cathode 243 are used to heat the electrolyte 241 to maintain the electrolyte at an appropriate operating temperature to cause the lithium atoms in the electrolyte to be reduced and diffused into the cathode material. The thermocouple 260 is placed in the container 230 and immersed in the electrolyte 241 to detect the temperature of the electrolyte 241. The anode 242 and the cathode 243 are disposed in the vessel 230 and partially immersed in the electrolyte 241. The cathode 243 is supported by a cathode support frame 244. The material of the cathode 243 is an aluminum material, and the material of the anode 242 may be a graphite rod, a polymer composite or an alloy. According to an embodiment of the invention, the electrolyte may comprise lithium chloride, potassium chloride and calcium chloride. The composition of the electrolyte comprises 20 to 40 wt% of a chlorination clock, 30 to 50 wt% of a chlorination clock, and 10 wt/min of chlorination #5. Chlorination clocks provide a source of lithium, while potassium chloride acts primarily as a flux to lower the temperature of the electrolyte and increase electrolyte fluidity. According to an embodiment of the present invention, the conditions for performing the electrolytic diffusion reaction include: a current density of 0.08 amps per unit cathode area (cm 2 ), and a temperature of the electrolyte maintained at about 500 ° C to reduce lithium atoms of the electrolyte On the cathode. As the lithium concentration of the aluminum-lithium compound increases, a liquid metal of an aluminum-lithium compound is formed when it reaches about 55%. Since the liquid metal density of the aluminum-lithium compound is lower than that of the molten electrolyte, it floats on the liquid surface of the electrolyte, and the liquid metal of the inventor compound is directly solidified or molded by a mold to obtain a composition of Al- The aluminum-lithium compound between 40wt.°/〇Li and Al-62wt.% Li, because the lithium content is quite high, cannot be measured by the existing instruments, so the composition of the aluminum-lithium compound can be determined according to the phase diagram. To speculate. Referring to Fig. 3, it is a phase diagram of aluminum-lithium metal, in which the vertical axis is temperature, the lower horizontal axis is the atomic percentage of the chain, and the upper horizontal axis is the percentage of lithium in the name of 200900541. The contents of the embodiments of the invention are all described by weight percentages. Taking the optimal operating temperature range disclosed in the embodiment of the present invention as an example, as shown in FIG. 3, 'for example, when the temperature is 55 〇〇c, when the percentage of lithium 3 s contained in the surface of the cathode material is 41%, The surface of the aluminum has reached the liquid area of A1 as shown in Figure 3. Since the density is 2.74 g/cm3 and the density of the clock is 54.54 g/cm3', it can be inferred that the above-mentioned Al_4丨% u liquid metal has a mobility of 1.84 g/cm3, which is higher than the liquid salt density in the electrolytic cell ( About 2g/cm3), when the Al-Li liquid metal is produced on the surface of the cathode, it floats out of the liquid surface due to its low density. Therefore, the appropriate current density is continuously applied to the electrolytic cell, and the liquid metal of the shell J Al-Li is continuously produced to float out of the electrolyte surface for fishing. The metal compound prepared according to the above method has stable metal properties and can be stored in the atmosphere, greatly reducing the safety concerns of storing the pure clock. In addition, the aluminum-bell compound of the Shangzhong content is placed in the water, Increasing the standing time, the forming compound, reacts violently with water, and it can also be confirmed that high levels of lithium are present in the aluminum-lithium compound. Other components in the electrolyte, such as potassium, have a very low affinity with aluminum (cathode material). Therefore, the deuterium compound prepared by the method of the present invention has a charge-removing content of less than 50 ppn. The aluminum-lithium compound may have a small amount of impurities. For example, sodium 'is common in gasification salts _f. After quantitative analysis, the aluminum-lithium compound prepared by the present invention has a sodium content of less than 3 〇 ppm. Although the present invention has been described above in terms of a preferred embodiment, it is not intended to limit the invention to those skilled in the art, and various modifications and changes may be made without departing from the spirit and scope of the invention. The insurance coverage of the invention 200900541 is subject to the definition of the patent application park attached to the application. BRIEF DESCRIPTION OF THE DRAWINGS In order to make the above and other objects of the present invention more obvious, the detailed description of the drawings is as follows. Advantages and Embodiments Fig. 1 shows an example of the embodiment of the invention. A step-by-step flow chart for the preparation of high-chain aluminum·•lithium compounds.夂 Fig. 2 is a schematic view showing the structure of an electrolytic cell according to an embodiment of the present invention. Fig. 3 is a phase diagram of a metal of Lu_zhong. 210 : outer tank body 220 · inner layer 230 : container 242 : anode 244 : cathode support frame 260 : thermocouple [ main component symbol description ] 200 : electrolytic cell 211 : top cover 221 : support plate 241 : electrolyte 243 : anode 250 :heater