TW202010725A - 陶瓷製造用顆粒之製造方法 - Google Patents
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Abstract
本發明之目的係提供陶瓷製造用顆粒之製造方法,其生產性高,將供給至加壓成形所得之加壓成形體進行燒製而製造陶瓷時,可得到抑制了物性降低之陶瓷。本發明之特徵係包含下列步驟:漿料製備步驟,製備由包含無機化合物之粉末、黏結劑及溶劑的混合物構成之漿料;造粒步驟,將前述漿料導入噴霧乾燥裝置,形成包含前述無機化合物之顆粒物;排氣步驟,使前述噴霧乾燥裝置內的環境氣體,經由表面為陶瓷製的旋風器而排氣;將在前述排氣步驟中旋風器所回收之微粉,混合於前述造粒步驟所得之顆粒物。
Description
本發明係關於包含無機化合物(例如氮化鋁)作為燒結用粒子之陶瓷製造用顆粒之製造方法。
氮化鋁所代表之無機材料係將包含溶劑、進一步因應需要而包含黏結劑等之漿料藉由噴霧乾燥而形成為顆粒狀,並將其燒製而作成堅硬的燒結物,即陶瓷。上述陶瓷可使用於各種用途。例如氮化鋁製陶瓷顯示高熱傳導性、高絕緣性,作為散熱材料、電氣絕緣材料,廣泛使用於電子儀器之散熱基板、電子電路基板等用途(專利文獻1及2)。
尤其如上述的顆粒狀成形體由於粒徑一致,因此適合藉由加壓成形而成形為規定形狀,藉由燒製這樣的成形體,可得到目的之形狀的陶瓷。
在前述藉由噴霧乾燥的顆粒之製造中,已造粒之顆粒係由噴霧乾燥裝置的下部回收,微粉係與排氣一同自噴霧乾燥裝置排出,以旋風器、袋濾器捕捉。
上述微粉係因在噴霧乾燥裝置中的乾燥過程中顆粒彼此碰撞、在將漿料進行噴霧時生成之微細的液滴之生成而生成。尤其若欲製作100μm以下的粒徑之顆粒,則其微粉之量相對地增加,有使所得之顆粒的產率降低之問題,而追求其改善。
[先前技術文獻]
[專利文獻]
專利文獻1:日本專利第3479160號
專利文獻2:日本專利第2525074號
[發明所欲解決課題]
因此,本發明之目的係提供在前述顆粒之製造方法中,生產性優異的陶瓷製造用顆粒之製造法。
[用來解決課題之手段]
根據本發明,可提供上述的陶瓷製造用顆粒之製造方法,其包含:
漿料製備步驟,製備由包含無機化合物之粉末及溶劑的混合物構成之漿料;
造粒步驟,將前述漿料導入噴霧乾燥裝置,形成包含前述無機化合物之顆粒物;
排氣步驟,使前述噴霧乾燥裝置內的環境氣體,經由表面為陶瓷製的旋風器而排氣;
將在前述排氣步驟中旋風器所回收之微粉,混合於前述造粒步驟所得之顆粒物的步驟。
在本發明中,作為前述無機化合物,可理想地使用氮化鋁。
[發明之效果]
根據本發明之前述製造方法,可提供在前述顆粒之製造方法中,回收排除作為微粉之生成物,混合於所得之顆粒而作成製品,藉此顯著提升產率之陶瓷製造用顆粒之製造法。
在本發明之製造方法中,最大的特徵係微粉之回收技術、與將回收之微粉混合於顆粒。
本發明者等注目於上述微粉之回收所使用之旋風器所致之微粉的污染,藉由以陶瓷構成上述旋風器之內面而達成污染極少的微粉之回收。再者,針對添加於藉由噴霧乾燥所得之顆粒物時的影響進行探討,結果見到所得之陶瓷製造用顆粒的重裝體積密度之上升,確認到不僅提升填充至成形模具之填充性,而且對於在成形後進行燒結所得之燒結物的特性、外觀幾乎不造成影響。又,由於微粉所包含之以鐵為中心的金屬雜質量少,因此可將微粉混合後的顆粒中的鐵含量維持在20ppm以下。
這樣的陶瓷製造用顆粒可有效地避免混入金屬雜質所致之燒結性的降低、外觀的惡化,而且,由於大量包含源自微粉的微粒成分,因此重裝體積密度提高。結果為,將該顆粒供給至加壓成形時,所得之加壓成形體成為粒子間隙小之緻密者。因此,將這樣的加壓成形體藉由加熱至高溫的燒結而製作陶瓷時,可有效地抑制粒子間隙所致之燒結性的偏差,可得到安定的物性之陶瓷。
參照圖1之流程圖,本發明之陶瓷製造用顆粒之製造步驟大致而言具有準備燒結材料的無機化合物之粉末、溶劑及適當使用之任意材料作為原材料,使用此等原材料而製備漿料(漿料製備步驟),將所得之漿料供給至噴霧乾燥裝置而造粒(造粒步驟),因應需要而使所得之顆粒物流動化(流動化步驟)之步驟,進一步設置使用旋風器之微粒成分回收及混合至前述顆粒物之混合步驟。
原材料:
在本發明中,使用作為原材料的無機化合物係燒結材料,係形成最終製造之陶瓷的骨架之成分,使用因應目的之陶瓷的種類之無機化合物。
作為這樣的無機化合物,可使用有燒結物之特性、外觀惡化之虞的金屬雜質少,其中又可使用其中之一的鐵之含量抑制在20ppm以下的高純度者,只要是這樣的高純度,則可使用各種無機化合物,而以使用電子設備等的電子電路基板等所使用之氮化鋁為最佳。作為金屬雜質少的無機化合物,其中又可理想地使用藉由還原氮化法而製造之氮化鋁。
又,製備供給至噴霧乾燥之漿料所使用之無機化合物之粉末,通常平均粒徑為5μm以下,尤其在0.5~3μm左右的範圍的話,從得到具有均勻的粒度分布之顆粒的觀點為佳。該平均粒徑例如可藉由利用雷射繞射法的粒度分布測定裝置而測定。
與上述的無機化合物粉末一同使用之溶劑,係製備漿料及藉由噴霧乾燥的造粒所必需之成分,取決於無機化合物之種類而使用水或揮發性的有機溶劑。
作為這樣的有機溶劑,並未限定於此,而例如可例示:丙酮、甲乙酮及甲基異丁基酮等酮類;乙醇、丙醇及丁醇等醇類;苯、甲苯及二甲苯等芳香族烴類;或者三氯乙烯、四氯乙烯及氯溴甲烷等鹵化烴類等,此等有機溶劑可混合2種以上而使用。
該溶劑係以例如以所得之漿料在20℃的黏度成為0.02~2000mPa・s的範圍之量使用為佳,例如以每100質量份的前述無機化合物粉末而言20~200質量份之量使用。
又,作為適當使用之其它成分,可列舉陶瓷之成形所使用之周知的摻合劑,例如可列舉:黏結劑(binder)、界面活性劑、燒結助劑等。
黏結劑係使用顆粒的陶瓷之成形所使用者,係為了在燒結以前,粒子不散亂地成形為規定形狀的成形體而使用者,係以往周知的摻合劑。
作為這樣的黏結劑之例,不限制於此,而通常可使用:聚乙烯縮丁醛等聚乙烯縮醛;聚甲基丙烯酸甲酯、聚甲基丙烯酸乙酯、聚甲基丙烯酸2-乙基己酯、聚甲基丙烯酸丁酯、聚丙烯酸酯、纖維素乙酸丁酸酯等丙烯酸系樹脂;硝化纖維素、甲基纖維素、羥基甲基纖維素、聚乙烯醇、聚氧乙烯氧化物(polyoxyethylene oxide)及聚環氧丙烷等含氧有機高分子物;石油樹脂、聚乙烯、聚丙烯、聚苯乙烯等烴系合成樹脂;聚氯乙烯;蠟及其乳液等有機高分子物,此等可混合2種以上而使用。
作為這樣的黏結劑,係以聚乙烯縮醛、丙烯酸系樹脂為較佳,具體而言,可列舉:積水化學工業(股)製S-LEC B、Kuraray(股)製Mowital、東亞合成(股)製Aron系列、共榮社化學(股)製Olycox KC系列、日新化成(股)製NSK系列、Taisei Fine Chemical(股)製KWE系列。
從有效地進行燒結前的成形的觀點來看,該黏結劑通常以每100質量份的無機化合物粉末而言0.1~30重量份之量使用為較佳。
界面活性劑係為了使無機化合物粉末均勻地分散於漿料中而使用者,可使用其本身周知者,而通常可理想地使用HLB在4.5~18,尤其6.0~10.0的範圍之非離子系界面活性劑。
作為這樣的非離子界面活性劑之例,可列舉:羧化三氧乙烯十三醚、二甘油單油酸酯、二甘油單硬脂酸酯、羧化七氧乙烯十三醚、四甘油單油酸酯、六甘油單油酸酯、聚氧乙烯山梨醇酐單月桂酸酯、聚氧乙烯山梨醇酐單油酸酯等,此等亦可混合2種以上而使用。
該界面活性劑之使用量通常以每100質量份的無機化合物粉末而言0.01~10質量份,尤其0.02~3.0質量份的範圍為較佳。
再者,燒結助劑係為了促進製造陶瓷時之燒結而使用者,可因應無機化合物粉末之種類,使用其本身周知者。例如當使用氮化鋁粉末時,作為燒結助劑,係以氧化鈣、氧化鍶等鹼土類金屬氧化物;氧化釔、氧化鑭等稀土類氧化物;鋁酸鈣等複合氧化物等為佳,以在與氮化鋁粉末之合計量中所佔的比例而言0.1~10質量%的範圍使用。
製備漿料:
上述的各種原材料可使用周知的混合裝置而混合,作為該混合裝置,通常係以球磨機為代表的滾磨機。藉此,可得到無機化合物粉末均勻分布之漿料。
所得之漿料可因應需要而進行過濾,去除漿料中的粗粒成分後,暫時保存於漿料槽。
此外,上述的過濾通常可藉由使漿料通過孔徑為10~100μm的濾材而進行。
如此進行,可得到較佳為在20℃之黏度在0.02~2000mPa・s的範圍之漿料。
藉由噴霧乾燥的造粒:
如上述進行所得之漿料係導入到噴霧乾燥裝置而進行造粒,而當使用氮化鋁作為無機金屬化合物時,係以使該漿料通過磁性過濾器而供給至噴霧乾燥裝置為佳。
亦即,由於氮化鋁粉末非常堅硬,因此包含該氮化鋁粉末之材料的運送配管會摩耗,有摩耗粉作為雜質混入之虞。儘管使用例如不鏽鋼製者作為運送配管,然而其結果為有包含Fe、Ni、Cr等之摩耗粉混入漿料中之虞。因此,藉由使上述漿料通過磁性過濾器而供給,可理想地自漿料中去除這樣的摩耗粉,可有效地避免例如在所得之顆粒中之金屬雜質含量大於20ppm之不理想的情況。
此外,藉由磁性過濾器去除摩耗粉亦可在造粒後進行,而由於造粒後的去除效率低,因此以在即將將漿料供給至噴霧乾燥裝置之前通過磁性過濾器而進行摩耗粉之去除為佳。亦即,這是因為比起將藉由造粒所得之顆粒物(粒狀物)通過磁性過濾器,將漿料通過磁性過濾器者可更緊密地接觸磁性過濾器。
在本發明中,噴霧乾燥裝置係自其上部將前述製備之漿料噴霧至經適當加熱之乾燥氣流(例如空氣、氮氣)中,藉此去除溶劑,得到包含無機化合物之粒狀物。
在噴霧乾燥裝置內進行噴霧之方法有噴嘴式、或圓盤式,而本發明之粒徑較小的陶瓷顆粒係以圓盤式為佳。
又,在本發明中,藉由造粒所得之顆粒物係自噴霧乾燥裝置之下部回收,微粉係與排氣一同自噴霧乾燥裝置排出,以旋風器、袋濾器捕捉。
此外,亦考慮不介隔旋風器而直接以袋濾器回收所有生成物之方法,然而根據本發明者等之確認,有顆粒物變形、或微粉頑強地附著於表面而得到重裝體積密度降低者的問題。
前述旋風器所捕捉之微粉,係粒徑比在噴霧乾燥機下捕捉之顆粒物更小者,其粒徑係以40μm以下者為較佳。無法以旋風器捕捉之粒徑更小者係以袋濾器捕捉。
又,該微粉係混合於藉由噴霧乾燥所得之粒狀物者。由於是在旋風器內微粉進行離心分離,碰撞壁面而在之後因重力而落下,累積於下部之機制,因此旋風器之內面易於摩耗。因此,作為旋風器,可使用其內面經陶瓷塗布者。藉此,可確實地避免金屬雜質混入藉由旋風器所回收之微粉中,可有效地避免該微粉混合於藉由造粒所得之粒狀物時混入金屬雜質。作為前述無機化合物,當使用氮化鋁時,係以氮化鋁陶瓷、氧化鋁陶瓷塗布者為佳。
又,自噴霧乾燥裝置排出之粒狀物,係以通過篩(例如振動篩等)而去除粗粒成分(例如粒徑為300μm以上的粒子)為較佳。
微粉之混合:
在本發明中,係將上述的旋風器所回收之微粉混合於如前述進行所得之顆粒物,而以粒徑為40μm以下的微粒成分所佔之比例成為10~25質量%的範圍之方式混合微粉為較佳。關於該混合方法並未限制,而以與後述的流動化處理一同進行為較佳。
流動化處理:
如上述進行而混合了微粉之顆粒物,係以供給至使顆粒(顆粒物與微粉之混合物)滯留在亂流的氣體中之步驟(流動化步驟),達成流動性之提升、顆粒物之強度提升及顆粒物與旋風器所回收之微粉的進一步均勻化為較佳。
作為陶瓷製造用顆粒,若以氮化鋁顆粒為例,該流動化所使用之氣體係以與氮化鋁粉末、黏結劑等添加劑實質上不反應的氣體為較佳,例如可列舉:空氣、氧氣、氮氣等。又,供給之氣體的風速只要是顆粒之流動化所必要的風速即可。顆粒之流動化所必要的風速例如可任意地選自:化學工學協會編「化學工學便覽改訂4版」之176頁所記載之流動化起始速度的式子與1056頁所記載之結束速度的式子所計算之値的範圍。又,顆粒物之滯留時間係以選自1分鐘~36小時的範圍為較佳。供給之氣體的溫度可採用任意的溫度,而為了得到具有適當的破壞強度之氮化鋁顆粒,係以選自0~250℃的範圍較佳。藉由該流動化步驟,自噴霧乾燥機下捕捉之顆粒物與旋風器所捕捉之微粉均勻混合。又,可調整顆粒物之流動性、強度。
上述流動化步驟,通常係使用具備流動床之裝置,以分批進行,而在於上述流動化步驟供給顆粒物之藉由噴霧乾燥的造粒步驟中,從裝置之操作來看,係以連續進行運轉為較佳。此時,為了避免使造粒步驟中的運轉與流動化步驟一同以分批進行,亦可在造粒步驟與流動化步驟之間,設置成為緩衝的漏斗、或槽,一邊連續地進行造粒步驟,一邊以分批進行前述流動化步驟,且為較佳的態樣。
經流動化步驟所得之顆粒適當地通過篩,藉此,進一步去除粗粒成分,回收作為具有規定的平均粒徑及微粒含量之本發明之陶瓷製造用顆粒。
陶瓷製造用顆粒:
藉由本發明之方法所製造之陶瓷製造用顆粒,係每一無機化合物的金屬雜質含量為0.1質量%以下的極高純度。其中又因可將金屬雜質之一的鐵之含量抑制在以元素換算而言20ppm以下,因此可有效地避免這樣的金屬雜質所致之燒結物的特性、外觀之惡化。
又,為了作成適合加壓成形的陶瓷製造用顆粒,係以前述陶瓷製造用顆粒之平均粒徑成為60~100μm的範圍之方式,進行前述顆粒物之製造條件的調整、前述微粉之混合量的調整等為較佳。亦即,與顆粒物一同包含之微粉由於作為粒徑小的顆粒發揮功能,填補大的粒子之間隙,因此極適合經過加壓成形之燒結。亦即,將該顆粒填充於規定的模具內而進行加壓成形時,所得之加壓成形體由於粒子彼此緊密接合,因此在藉由接下來進行之高溫加熱而燒結時,可有效地避免存在空隙所致之燒結性的降低。
此外,在本發明中,顆粒等粒子之平均粒徑、微粒成分含量係藉由雷射繞射散射法而測定。
本發明之陶瓷製造用顆粒可例如藉由填充於規定的模具內之加壓成形而成形為所欲的形狀,其次,因應使用之無機化合物的種類之加熱而燒結(例如氮化鋁之情形為600℃以上),有效地調節燒結不良所致之各種特性的降低,得到具有安定的特性之陶瓷。
因此,當使用氮化鋁粉末作為原材料的無機化合物粉末時,最終製品的陶瓷係極高品質,廣泛使用作為各種電子儀器之電路基板、散熱板。
[實施例]
為了更具體地說明本發明而在以下列舉實施例及比較例,惟本發明並未限定於此等實施例。
此外,以下的實施例及比較例中的各種物性之測定係藉由下述方法進行。
(1)氮化鋁粉末之平均粒徑
氧化鋁粉末、氮化鋁粉末、氮化鋁與未反應原料氧化鋁的混合粉末之平均粒徑,係將試料以均質機分散於焦磷酸鈉水溶液中,使用日機裝股份有限公司製MICROTRAC HRA藉由雷射繞射法而測定。
(2)比表面積
氮化鋁粉末之比表面積係使用島津製作所(股)製流動式表面積自動測定裝置FlowSorb 2300藉由BET法而測定。
(3)氧含量
氮化鋁粉末中的總氧含量係使用堀場製作所(股)製陶瓷中氧氮分析裝置EMGA-620W而測定。
(4)碳含量
氮化鋁粉末中的碳含量係使用堀場製作所(股)製金屬中碳分析裝置「EMIA-110」,使粉末在氧氣流中燃燒,由產生之CO、CO2
氣體量進行定量。
(5)氮化鋁粉末之金屬元素含量
氮化鋁粉末之鋁以外的金屬元素含量係在0.8g的試料添加2mL的硝酸、10mL的磷酸而在380℃加熱分解20分鐘,使用島津製作所(股)製ICPS-1000-II藉由ICP發光光譜分析法而測定。
(6)顆粒之平均粒徑
使用日機裝股份有限公司製MICROTRAC MT3300EX,藉由雷射繞射法而測定。
(7)氮化鋁顆粒之金屬雜質量
氮化鋁顆粒中的金屬元素含量係將顆粒在600℃加熱5小時、脫脂後作為試料。在0.8g的試料添加2mL的硝酸、10mL的磷酸而在380℃加熱分解20分鐘,使用島津製作所(股)製ICPS-1000-II藉由ICP發光光譜分析法而測定。
(8)重裝體積密度
使用筒井理化學機械(股)製「A・B・D粉體特性測定器」而測定重裝體積密度。
(9)加壓成形體密度
由加壓成形體之尺寸與重量,計算加壓成形體密度而求出。
(10)燒結物密度
使用東洋精機製作所(股)製「高精度比重計D-H」,藉由阿基米德法而求出。
(11)體積電阻率
利用根據JIS C2141之方法,以Advantest(股)製體積電阻率測定裝置R8340進行測定。
(12)熱傳導率
製作之AlN燒結物的熱傳導率係使用京都電子工業(股)製LFA-502藉由雷射閃光法而測定。
>實施例1>
在內容積500L的旋轉球磨機放入內含鐵心的耐綸球,其次,投入120kg的表1所示之還原氮化法所製造之氮化鋁粉末(德山(股)製H級No.1)、6kg的氧化釔、0.1kg的六甘油單油酸酯、4kg的聚甲基丙烯酸丁酯、120kg的甲苯溶劑,充分進行球磨機混合後,得到白色的漿料。
將如此所得之漿料藉由噴霧乾燥機而以噴霧器轉速5000rpm進行造粒。造粒結束後,將100kg的在噴霧乾燥機下捕捉之顆粒(顆粒物)、與25kg的在造粒中旋風器所捕捉之顆粒(微粉)導入流動乾燥機,在室溫進行2小時的流動化處理,製作氮化鋁顆粒。旋風器之內部係使用以氧化鋁陶瓷塗布者。
>實施例2>
除了在實施例1將噴霧器轉速設為8000rpm以外,與實施例1同樣地進行造粒。造粒結束後,將88kg的在噴霧乾燥機下捕捉之顆粒(顆粒物)、與35kg的在造粒中旋風器所捕捉之顆粒(微粉)導入流動乾燥機,在室溫進行2小時的流動化處理,製作氮化鋁顆粒。
>比較例1>
除了在實施例1中使用旋風器之內部不以氧化鋁陶瓷塗布之不鏽鋼製者以外,與實施例1同樣地進行造粒。造粒結束後,將101kg的在噴霧乾燥機下捕捉之顆粒(顆粒物)、與24kg的在造粒中旋風器所捕捉之顆粒(微粉)導入流動乾燥機,在室溫進行2小時的流動處理,製作氮化鋁顆粒。
>參考例1>
與實施例1同樣地進行造粒後,將100kg的在噴霧乾燥機下捕捉之顆粒(顆粒物)導入流動乾燥機,在室溫進行2小時的流動化處理,製作氮化鋁顆粒。
測定藉由上述的實施例、比較例、參考例所得之顆粒物及微粉的粒徑及金屬雜質(Fe、Cr、Ni)。又,針對混合此等所得之顆粒,測定粒徑、金屬雜質(Fe、Cr、Ni)、重裝體積密度。將此等結果示於表2。
再者,將30g的混合了顆粒物與微粉所得之顆粒導入φ100mm的金屬模具,以100MPa的壓力進行加壓成形,製作厚度約2mm的加壓成形體,測定加壓成形密度。此後,使該加壓成形體在空氣中580℃、5小時之條件下進行脫脂。其次,將該加壓成形體放入內面以氮化硼塗布之碳製坩堝,在氮氣環境下以1800℃燒製5小時,得到燒結物。研磨該燒結物表面後,確認外觀(有無混入金屬雜質所致之變色),測定密度、體積電阻率、熱傳導率。將結果示於表2。
無
[圖1]表示本發明之陶瓷製造用顆粒之製造方法的過程之流程圖。
Claims (2)
- 一種陶瓷製造用顆粒之製造方法,其特徵為包含: 漿料製備步驟,製備由包含無機化合物之粉末、黏結劑及溶劑的混合物構成之漿料; 造粒步驟,將該漿料導入噴霧乾燥裝置,形成包含該無機化合物之顆粒物; 排氣步驟,使該噴霧乾燥裝置內的環境氣體,經由表面為陶瓷製的旋風器而排氣; 將在該排氣步驟中旋風器所回收之微粉,混合於該造粒步驟所得之顆粒物。
- 如申請專利範圍第1項之陶瓷製造用顆粒之製造方法,其中該無機化合物為氮化鋁。
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