201206690 六、發明說明： 【發明所屬之技術領域】 本發明係有關於-種使乾燥㈣ 充到ϋ銶内部之方法 4以壓⑧狀態填 電池電極材料之陶& 種適。將如鐘離子 E鉢内部填充粉體之方法。 、s鉢内。P之向 【先前技術】 當使成為鐘離子電池及其他電子零件原料 性燒成時，一般俜使用埴 柘體工業 I係使用填充粉體到稱做£鉢之 益，在燒成爐内燒成之方法。A .、'谷 馬如问在此燒成步驟中之生 產效率，而要求盡量提高粉體填充龍鉢之效率。 提高粉體填充效率之機構，自先前有使用震動填充 在專利文獻1中，開示有當使粉體在成形模且内 部壓縮時’施加〇.5〜100Hz震動之方法。 …、 在此專利文獻1中，係使粉體a縮成均勾厚度。但h 當使用本發明者之檢討結果時，可知與其使粉體如專:文 獻Η吏粉體填充成均勾厚度，還不如使㈣中央部填充厚 度較溥且使周緣部較厚’如此才能提高燒成品質。其原因 在於：此種粉體之熱傳導率較低，所以，昆鉢中央；部之 昇溫速度相對較低，因為㈣内部之位置，粉體承受之燒 成溫度履歷會有參差，為均勾化燒成品質，使_中央部 填充厚度較薄，以使熱較容易傳導者比較有利。 但是’因為此種粉體厭惡水分’很多粉體無法進行渴 201206690 式填充，在乾燥狀態下係成輕飄飄狀態，所以，欲成形為 周緣部較高之形狀並*容易。㈣，當最初填充粉體_ 鉢内。卩時，粉體表面成平面狀，自此狀態使粉體上部往上 方增间，或者，在此形狀中，欲壓密化成整體中央凹陷狀 並不合易，因此我想先前技術完全無此種技術。 【先行技術文獻】 【專利文獻】 【專利文獻1】日本特公平7_1 1 2637號公報 【發明内容】 【發明所欲解決的課題】 因此，本發明之目的係解決上述先前技術之問題點， 提供1種使乾燥狀態之粉體成中央部較厚且周緣部較薄之 表面形狀’以壓密狀態填充到g銖内部之向B鉢内部填充 粉體之方法。 ' 【用於解決課題的手段】 為解決上述課題之本發明的特徵，係既定量供給乾燥 粉體到匣鉢内部後，一邊 〜 ， 降第1壓板到粉體表面直到既 定位置為止，一邊黨·叙厣奴 ®鉢’以使粉體表面隨著第1壓板 下表面形狀成形為中央 触士 勹τ央凹陷之形狀，接著，使成形後之粉 體表面藉第2壓板更加下壓 ^ 又加下7坚，以壓密化粉體。 如申請專利範圍第2項所-^ $所不’最好使粉體之供給、成 形及壓密化各步驟在減壓箱 相體内進行，在此情形下，如申 請專利範圍第3項所示，最杠& 被好使減壓箱體内之環境氣體與 201206690 燒成爐内之環境氣體相同。 又，如申請專利範圍第4項所示，最好第丄壓板盘第 2壓板具有相同之下表面形狀，"請專利範圍第5項所 不，最好第！壓板與第2壓板之下表面形狀，係中央部較 低且周緣部朝上之傾斜面。在此情形下，^請專利範圍 第6項所示，最好周緣部朝上之傾斜面使相對於£林底面 之夾角’小於粉體之安息角。 【發明效果】 當使用申請專利範圍第i項之發明時，在供給既定量 乾無後粉體龍鉢内部後’ 一邊施加震動到㈣，一邊使 21壓板朝向粉體表面以下降至既定位置。粉體藉震動而 :動化’在周緣部移動到比最初位置還要上方之位置隨 著第1壓板下表面之形；}大’成形為中央凹陷之形狀。但是 =原樣時，密度不充分，所以之後，#第2壓板更加下壓 粉體表面，⑽内部粉體被壓密化成概略均勻的密产。因 此，在燒成步驟中，升溫較慢之㈣中央部粉體也二容易 :傳熱，燒成品質就不會有參差…，能使匡鉢内之燒 成粉體重量比先前增加，能提高之後的燒成步驟之 率0 1又’先前係被填充到S鉢内部t粉體表面為自由狀 ^ ’填^密度之參差也是任其發展，但是當使用本發明 和，此官理粉體之表面狀態’所以，能消除每個匣鉢之參 差=’能獲得均句的燒成品質。而且，當使用本發明時，能 吏最初之粉體供給不施加過大壓力在粉體，所以，能有效 201206690 抑制混合之產生。 當使用申請專利範圍第2項之發明時，.因為在減壓條 件下，進行粉體之供給、成形及壓密化之各步驟，所以， 能去除存在粉體粒子間之空氣，僅此部分就能提高粉體之 填充密度。又’藉脫氣粉體中之空氣，能防止由空氣中之 氧氣或水分所致之燒成品質降低。而且，藉減壓也能同時 防止自粉體表面產生塵埃，能抑制粉體飛散所致之損失。 當使用申請專利範圍第3項之發明時，藉使減壓箱體 内之環境氣體與燒成爐内之環境氣體相同，能使粉體内部 之空氣較完全置換成環境氣體，能提高燒成品質。 當使用申請專利範圍第4項之發明時，能使藉第1壓 板成形之粉體表面形狀不崩潰地，藉第2壓板壓密。 ¥使用申凊專利範圍第5項之發明時，匣銖内部粉體 燒成品質之參差會減少，又，當使用申請專利範圍第6項 之發明時，藉第1壓板成形之粉體在移動中不會崩潰。 【實施方式】 以下’一邊參照圖面’一邊詳細說明本發明之實施形 態。 在本實施形態中，匣鉢係四角形之碳匣鉢，粉體係裡 離子電池正極材料用之陶瓷粉體。此粉體之粒徑係2〜】5 "m，其為嫌惡水分之物質。又，燒成係在氮氣環境氣體中 進行。但是，本發明並不侷限於此。 對於以滾輪輸送帶等適宜搬運機構（未圖示）搬運之 201206690 「T1:首先，'1圖所示，使粉體供給龍鈽内部。 起= 2㈣被支#，在心料降機構5舉 、 费者在具有粉體供給口 3之蓋體4上之位 狀態下’粉體自上方藉螺桿供料$ 6被供給 每個201206690 VI. Description of the Invention: [Technical Field of the Invention] The present invention relates to a method of filling a dry (four) into a crucible, and filling the battery electrode material with a pressure 8 state. A method of filling a powder such as a clock ion E钵. , s钵. Direction of P [Prior Art] When it is used as a raw material for the production of a clock-ion battery and other electronic parts, it is generally used in the industry of the body I to use the filler powder to be used in the firing furnace. The method of becoming. A., 'Gu Maru asks about the productivity in this firing step, and requires to increase the efficiency of filling the dragon's dragonfly as much as possible. The mechanism for improving the powder filling efficiency has been previously filled with vibration. Patent Document 1 discloses a method of applying a vibration of 〇5 to 100 Hz when the powder is compressed in a molding die and internally compressed. In this Patent Document 1, the powder a is reduced to a uniform thickness. However, when using the results of the review by the inventors, it can be seen that instead of filling the powder as a special thickness, it is better to make the thickness of the center portion thicker and the peripheral portion thicker. Improve the quality of firing. The reason is that the thermal conductivity of the powder is low, so the temperature rise rate of the central part of the Kunyu is relatively low, because (4) the internal position, the burning temperature history of the powder is uneven, The quality of the firing is such that the thickness of the central portion is relatively thin, so that the heat is more easily conducted. However, because many of the powders are not suitable for moisture, many powders cannot be filled with the 201206690 type, and they are lightly floated in a dry state. Therefore, it is easy to form a shape with a high peripheral portion. (d), when initially filled with powder _ 钵. When 卩, the surface of the powder is flat, and the upper portion of the powder is increased upward from this state. Or, in this shape, it is not easy to press and densify into a central depression. Therefore, I think the prior art has no such thing. technology. [PRIOR ART DOCUMENT] [Patent Document 1] [Patent Document 1] Japanese Patent Publication No. 7_1 1 2637 SUMMARY OF INVENTION [Problems to be Solved by the Invention] Accordingly, an object of the present invention is to solve the problems of the prior art described above and provide A method of filling a powder in a dry state with a surface portion having a thick central portion and a thin peripheral portion, and filling the powder into the interior of the crucible in a pressure-tight state. [Means for Solving the Problem] In order to solve the above-described problems of the present invention, it is possible to quantitatively supply the dry powder to the inside of the crucible, and then lower the first platen to the surface of the powder until the predetermined position. · 厣 厣 钵 钵 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 粉 粉 粉 粉 粉 粉 粉 粉 粉 粉 粉 粉 粉 粉 粉 粉 粉 粉 粉 粉 粉 粉 粉 粉 粉 粉 粉 粉 粉 粉 粉Add 7 strong to compact the powder. For example, in the second paragraph of the patent application scope, it is preferable to carry out the steps of supplying, forming and compacting the powder in the decompression chamber phase. In this case, for example, the third item of the patent application scope As shown, the bar and the air are the same as the ambient gas in the 201206690 firing furnace. Further, as shown in the fourth item of the patent application, it is preferable that the second platen of the first platen plate has the same lower surface shape, and the patent scope is not the fifth item. The shape of the lower surface of the pressure plate and the second pressure plate is an inclined surface having a lower central portion and an upward peripheral portion. In this case, as shown in the sixth item of the patent range, it is preferable that the inclined surface with the peripheral portion facing upward is such that the angle θ with respect to the bottom surface of the forest is smaller than the angle of repose of the powder. [Effect of the Invention] When the invention of the invention of the scope of the invention is used, the vibration is applied to the (four) while the inside of the powder turkey is supplied, and the 21-plate is lowered to a predetermined position toward the surface of the powder. The powder is shaken by vibration: the movement is moved to a position above the initial position at the peripheral portion along the lower surface of the first platen; the large shape is formed into a shape of a central depression. However, when the density is not sufficient, the #2nd platen is further pressed down on the surface of the powder, and (10) the internal powder is compacted into a uniform and uniform production. Therefore, in the firing step, the temperature rise is slower. (4) The powder in the central portion is also easy: heat transfer, and the quality of the firing is not staggered... and the weight of the calcined powder in the crucible can be increased. The rate of the firing step after the increase is 0 1 and 'the previous system is filled into the interior of the S. The surface of the powder is free. ^ The density of the filling is also allowed to develop, but when using the present invention, this official powder The surface state of the body 'so, it can eliminate the stagger of each = = ' can get the firing quality of the average sentence. Further, when the present invention is used, the initial powder supply can be applied without applying excessive pressure to the powder, so that it is effective to suppress the occurrence of mixing in 201206690. When the invention of claim 2 is used, since the steps of supplying, forming, and compacting the powder are performed under reduced pressure, the air between the powder particles can be removed, and only this portion It can increase the packing density of the powder. Further, by using the air in the degassed powder, it is possible to prevent the deterioration of the firing quality caused by oxygen or moisture in the air. Moreover, by decompression, dust can be prevented from being generated from the surface of the powder at the same time, and the loss due to powder scattering can be suppressed. When the invention of claim 3 is used, if the ambient gas in the decompression chamber is the same as the ambient gas in the firing furnace, the air inside the powder can be completely replaced with the ambient gas, and the firing can be improved. quality. When the invention of the fourth application of the patent application is used, the shape of the surface of the powder formed by the first press plate can be compacted by the second pressure plate without collapse. When using the invention of the fifth paragraph of the patent application, the variation in the quality of the internal powder is reduced, and when the invention of the sixth application of the patent application is used, the powder formed by the first plate is moving. It won't crash. [Embodiment] Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings. In the present embodiment, the tantalum is a carbon powder of a square shape, and the ceramic powder for the positive electrode material of the ion battery in the powder system. The particle size of the powder is 2~5"m, which is a substance that is irritating to moisture. Further, the firing was carried out in a nitrogen atmosphere. However, the invention is not limited to this. For the 201206690 "T1: First, as shown in the figure 1", the powder is supplied to the inside of the dragon's raft. The up = 2 (four) is supported by #, and the heart drop mechanism 5 is lifted. In the position of the cover body 4 having the powder supply port 3, the powder is supplied from the top by the screw supply $6.
钵之粉體供給量為-定，能在供給路徑=每個E 闕等之定量供給機構。如第i圖所一途中’置切斷間 第1圖所不，㈣在 而且，當供給與後段燒成爐之環境氣體相同之氮氣到 減壓箱體2内部時’在粉體之供給階段中，粉體粒子間之 …與氮氣置換’所以在燒成階段中，粉體與氧氣接觸 之y能性會降低。此氮氣可在爐體間循環使用。在此實施 形態中，不施加過大壓力到粉體地向匣鉢丨内填充，所以， 能抑制混合之發生。又，在減壓狀態中進行粉體之… 所以，能抑制粉塵飛散所致之粉體損失。但是，也有因粉 體種類而在氧化條件下進行燒成者，在此情形下，當然: 要使減壓箱體2内部減壓即可。 接著，被供給既定量粉體之！Ψ7^ 遛艾匣鉢1係藉匣鉢升降機構 被載置到滾輪輸送帶等適宜之搬運機構上，被搬運到第^ 圖所示之成形位置。在此成形位置，㈣i被載置到具有 振動產生器11的支樓座12上。且支撐座12被具有彈脊 13之基座14所支稽，藉升降機構15被舉起到既定高度為 止。而且，在此成形位置也設有減壓箱體2 ^ 在㈣1上方，第1壓板16藉壓板升降機構17支撑。 第1壓板1 6之尺寸係比匣鉢1内側尺寸僅小些許，其下表 201206690 面形狀係中央部較低，周緣部係朝上之傾斜面18。最好中 央部與其係完全平面狀’如圖所示，寧可事先做成少許彎 曲面，則較容易移動粉體。周緣部之朝上傾斜面18與昆鉢 1底面之夾角α，係事先使其比粉體安息角還要小。 在被搬運到第2圖所示之成形位置期間，因為震動等 之影響’如第4(A)圖所示，匣鉢！内之粉體表面概略成 平面仁疋在第2圖所示之成形位置中，一邊使第1壓 板16藉[板升降機才冓17朝粉體表面下降，一邊藉震動產 生器11施加震動到£鉢i。其震動頻率如專利文獻i所示， 只要0.5〜ΐ〇〇Ηζ即可，只要對應粉體之特性狀況（流動 性、凝集性及粒度等）適宜設定即可。 粉體藉此震動成為可流動之狀態，所以，周緣部之粉 體能移動到比最初高度還要高之位置，當使第i壓板以下 降到比粉體最初高度還要低之位置時，如第4⑷圖所示， 粉體表面被成形為沿著第1壓板16下表面之形狀，亦即， 中央凹陷之形狀。而且此時’為防止自第1壓板16與匠鉢 1之間㈣漏粉體’第i壓板16之周緣部最好做成平直狀。 接著，帛1壓板16係藉屢板升降機構17被舉起，g 鉢1被載置到滾輪輸送帶等適宜之搬運機構上，被搬運到 :3圖所示之加壓位置。第1麼板16係決定粉體之表面形 ，並非特別施加壓力之物件。因此’當舉起第i壓板Μ 時’雖然粉體形狀有崩潰之可能性’但是如上所述，使周 :部之朝上傾斜面18_#1底面之夹角。小於粉體安息 角’藉此，能防止表面形狀崩潰。 $The powder supply amount of 钵 is set to be a quantitative supply mechanism in the supply path = each E 阙. In the middle of the figure i, the first section of the cut-off room is not shown. (4) In addition, when supplying the same nitrogen gas as the ambient gas of the subsequent-stage firing furnace to the inside of the decompression chamber 2, the supply phase in the powder is In the middle, the powder particles are replaced with nitrogen. Therefore, in the firing stage, the y energy of the powder in contact with oxygen is lowered. This nitrogen can be recycled between furnaces. In this embodiment, the excessive pressure is applied to the powder to fill the crucible, so that the occurrence of mixing can be suppressed. Further, the powder is subjected to the pressure reduction state. Therefore, the powder loss due to the dust scattering can be suppressed. However, there are cases in which the firing is performed under oxidizing conditions depending on the type of the powder. In this case, of course, the inside of the decompression chamber 2 may be decompressed. Then, it is supplied with the same amount of powder! Ψ7^ 遛 匣钵 匣钵 1 匣钵 匣钵 匣钵 匣钵 被 被 被 被 被 被 被 被 被 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 At this forming position, (d) i is placed on the stand 12 having the vibration generator 11. The support base 12 is supported by the base 14 having the ridge 13 and lifted by the lift mechanism 15 to a predetermined height. Further, at this forming position, a decompression chamber 2 ^ is provided above the (four) 1, and the first platen 16 is supported by the platen elevating mechanism 17. The size of the first platen 16 is smaller than the inner dimension of the crucible 1, and the surface of the first form 201206690 has a lower central portion and an inclined portion 18 with the peripheral portion facing upward. Preferably, the central part and its system are completely flat. As shown in the figure, it is easier to move the powder by making a slightly curved surface in advance. The angle α between the upwardly inclined surface 18 of the peripheral portion and the bottom surface of the Kunming 1 is made smaller than the powder angle of repose in advance. During the conveyance to the forming position shown in Fig. 2, the influence of vibration or the like is as shown in Fig. 4(A), 匣钵! The surface of the powder inside is roughly flattened in the forming position shown in Fig. 2, while the first platen 16 is lowered by the [plate lifter 17] toward the surface of the powder, and the shock is applied by the vibration generator 11 to £.钵i. The vibration frequency is as long as 0.5 to ΐ〇〇Ηζ as shown in the patent document i, and it is only necessary to appropriately set the characteristics (fluidity, aggregability, particle size, etc.) of the powder. The powder is vibrated by this vibration, so that the powder at the peripheral portion can be moved to a position higher than the initial height, and when the i-th pressure plate is lowered to a position lower than the initial height of the powder, As shown in Fig. 4(4), the surface of the powder is shaped to follow the shape of the lower surface of the first platen 16, that is, the shape of the central depression. Further, at this time, it is preferable to prevent the peripheral portion of the i-th pressure plate 16 from being between the first pressure plate 16 and the smith 1 (four) powder leakage body. Next, the 帛1 pressure plate 16 is lifted by the repeating plate elevating mechanism 17, and the 钵1 is placed on a suitable transport mechanism such as a roller conveyor belt, and transported to the pressurizing position shown in Fig. 3. The first board 16 determines the surface shape of the powder, and is not an object to which pressure is particularly applied. Therefore, 'when the ith platen 举 is lifted, the powder shape has a possibility of collapse', but as described above, the angle of the bottom surface of the upwardly inclined surface 18_#1 of the circumference is increased. Less than the powder rest angle ', thereby preventing the surface shape from collapsing. $
S 201206690 在第3圖所示之加壓位置中，在減壓箱體2内部設有 第堅板21，下壓在前步驟成形之粉體表面。"壓板21 被如壓缸之下壓機構22支標。又，其下表面形狀最好與第 1壓板16之下表面形狀相同。 設於第2圖所示成形位置之壓板升降機構17,係具有 降第1 [板16直到其行程終點之功能，設於第3圖所示 加壓位置之下壓機肖22係用於施加既定壓力之物件。因 此’如第4(C)圖所示’ w 1内部之粉體表面被下壓， 整體被壓密。當宽01 ^板21下表面形狀與第1壓板16下 表面形狀相㈣，能使成形粉體表面形狀 密整體。 而且’在此實施形態下’雖然使㈣】自帛2圖所示 成形位置移動到第3圖所示加壓位置，但是，也可以在相 5置並D又第1壓板16與第2壓板21，在相同位置實施 此兩步驟。 當上升第2壓板21時，如第4(D)圖所示，粉體在 匿鉢1内部被遂密成中央凹陷之形狀，在此狀態下，搬運 到燒成爐以在氮氣環境氣體中進行燒成。在處理之考量 下’雖'然有使此搬運區間做成對大氣開放之㈣，但是， 粉體表面被壓密化’所以空氣很難侵入，燒成品質不會降 低。 當填充粉體成如第4 (D)圖所示之剖面形狀以進行燒 成時’爐内之熱也很容易傳導到匣鉢i中央底#，所以， 與如第4 (A)圖所示之先前填充狀態下燒成者相比較下， 201206690 升溫速度變均勻，能使匣鉢1内各處粉體之燒成品質不再 有參差。又，整體被壓密化，所以，當使用本發明時，能 使一個E鉢的粉體重量增加2〇〜30%，能提高燒成步驟之 生產效率。 如上所述，當使用本發明時，能使乾燥狀態粉體的表 面形狀成為中央部厚度較薄且周緣部厚度較厚，且以壓密 狀態填充到匣鉢内冑，具有能提高燒成步驟生產效率及燒 成品質之效果。 【圖式簡單說明】 步驟說明圖。 之說明圖。 之說明圖。 之匣鉢内部粉體 表 第1圖係表示供給粉體到匣鉢之供給 第2圖係由第1壓板所做之成形步驟 第3圖係由第2壓板所做之壓密步驟 第4(A)〜（d)圖係表示各步驟中 面形狀變化之放大剖面圖。 【主要元件符號說明】 1 匣鉢 2 減壓箱體 3 粉體供給口 4 蓋體 5 S鉢升降機構 6 螺桿供料器 7 供給路徑 201206690 11 震動產生器 12 支撐座 13 彈簧 14 基座 15 升降機構 16 第1壓板 17 壓板升降機構 18 傾斜面 21 第2壓板 22 下壓機構S 201206690 In the pressurizing position shown in Fig. 3, the first plate 21 is provided inside the decompression chamber 2, and the surface of the powder formed in the previous step is pressed down. " Platen 21 is supported by a pressing mechanism 22 such as a cylinder. Further, the shape of the lower surface thereof is preferably the same as the shape of the lower surface of the first pressure plate 16. The platen lifting and lowering mechanism 17 provided at the forming position shown in Fig. 2 has a function of lowering the first [plate 16 up to the end of its stroke, and is provided under the pressing position shown in Fig. 3, and the press machine 22 is used for application. An object of established pressure. Therefore, as shown in Fig. 4(C), the surface of the powder inside the w 1 is pressed down, and the whole is compacted. When the shape of the lower surface of the width of the plate 21 is the same as the shape of the lower surface of the first platen 16, the surface shape of the formed powder can be made dense. Further, 'in this embodiment', although (4) is moved from the molding position shown in Fig. 2 to the pressing position shown in Fig. 3, the first platen 16 and the second platen may be placed in the phase 5 and D. 21. Perform these two steps in the same location. When the second pressure plate 21 is raised, as shown in Fig. 4(D), the powder is dented into a central depression in the interior of the concealer 1, and in this state, it is transported to a firing furnace for use in a nitrogen atmosphere. Perform baking. Under the consideration of the treatment, although the transportation section is opened to the atmosphere (4), the surface of the powder is densified. Therefore, the air is hard to intrude and the quality of the firing is not lowered. When the powder is filled into a cross-sectional shape as shown in Fig. 4(D) for firing, the heat in the furnace is also easily conducted to the center of the 匣钵i, so, as shown in Fig. 4(A) Compared with the burned ones in the previous filled state, the heating rate of 201206690 becomes uniform, and the firing quality of the powders in the crucible 1 is no longer uneven. Further, since the whole is densified, when the present invention is used, the weight of one E 钵 powder can be increased by 2 〇 to 30%, and the production efficiency of the firing step can be improved. As described above, when the present invention is used, the surface shape of the powder in the dry state can be made thinner at the center portion, thicker at the peripheral portion, and filled in the crucible in a compacted state, thereby improving the firing step. Production efficiency and firing quality. [Simple description of the diagram] Step description diagram. Description of the figure. Description of the figure. Fig. 1 shows the supply of the powder to the crucible. Fig. 2 shows the molding step by the first pressure plate. Fig. 3 shows the compacting step by the second pressure plate. A) to (d) are enlarged cross-sectional views showing changes in the shape of the surface in each step. [Description of main components] 1 匣钵2 Decompression chamber 3 Powder supply port 4 Cover 5 S钵 Lifting mechanism 6 Screw feeder 7 Supply path 201206690 11 Vibration generator 12 Support base 13 Spring 14 Base 15 Lift Mechanism 16 first pressure plate 17 pressure plate lifting mechanism 18 inclined surface 21 second pressure plate 22 pressing mechanism