TW201319004A - 陶瓷顆粒及陶瓷顆粒之製造方法以及陶瓷成形體 - Google Patents

陶瓷顆粒及陶瓷顆粒之製造方法以及陶瓷成形體 Download PDF

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TW201319004A
TW201319004A TW101135451A TW101135451A TW201319004A TW 201319004 A TW201319004 A TW 201319004A TW 101135451 A TW101135451 A TW 101135451A TW 101135451 A TW101135451 A TW 101135451A TW 201319004 A TW201319004 A TW 201319004A
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weight
parts
ceramic
acrylic copolymer
copolymer resin
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Masaki Yoshino
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Toray Industries
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Abstract

本發明之陶瓷顆粒係含有由丙烯酸共聚樹脂(a-1)、聚乙烯醇(a-2)、聚伸烷基氧化物(a-3)及硬脂酸(a-4)所構成之有機成分(A)及陶瓷粉體(B)之陶瓷顆粒，其特徵為：相對於100重量份的丙烯酸共聚樹脂(a-1)，係含有25~35重量份的聚乙烯醇(a-2)、25~35重量份的聚伸烷基氧化物(a-3)、及15~25重量份的硬脂酸(a-4)。本發明提供在以生胚加工、用加壓成形製造必須要高密度、高強度之陶瓷成形體的製程中，有效率的加壓成形，且容易生胚加工之陶瓷顆粒及陶瓷顆粒之製造方法。

Description

陶瓷顆粒及陶瓷顆粒之製造方法以及陶瓷成形體
本發明係關於陶瓷顆粒及陶瓷顆粒之製造方法，與將陶瓷顆粒加以成形而成之陶瓷成形體，該陶瓷顆粒係於壓製成形高密度、高強度之陶瓷成形體的製程中，有效率的加壓成形，且容易生胚加工。
陶瓷被使用於粉碎機構件、工業用磁磚、刀具、及電子零件等，而特別是在粉碎機構件與工業用磁磚等正進行大型化。而此種結構用陶瓷的一般製造方法，眾所周知有加壓成形法。加壓成形法有在水中或油中將粉體填充至橡膠模具並施加壓力的冷間均壓成形法(以下稱為CIP法，Cold Isostatic Press)，與將粉末填充進金屬模具從上下或左右的一軸方向施加壓力予以成形之金屬模具加壓法等。
一般為了提高成形體的形狀保持性，而在原料粉末中含有有機物黏結劑，為了具有對模具填充時的流動性，而使用製成球狀顆粒的粉末。
使用此陶瓷顆粒到得到燒結體係進行：顆粒之製造步驟→成形步驟→成形體加工步驟(生胚加工)→脫脂步驟→燒結步驟，但於大的成形體或形狀複雜的成形體，在壓力釋放或脫模時成形體會有發生破損的情形，或在對形狀複雜的成形體作生胚加工時會有發生破損的情形，故陶瓷顆粒被要求要具成形時的成形性、形狀保持性、及脫模時的脫模性。
為了解決這些問題已提議各種方法。例如，已提議有一種含有規定平均皂化度與聚合度之聚乙烯醇的肥粒鐵(ferrite)成形用顆粒(專利文獻1)。然而，因含有許多聚乙烯醇的顆粒會變成堅硬的顆粒，使顆粒的破碎性變差，特別在製造形狀複雜之成形體時會有困難的情形。
另外，已提議一種取得壓力傳遞性與顆粒的壓縮破壞性之平衡的陶瓷顆粒(專利文獻2)。然而，壓力傳遞性良好的顆粒，由於顆粒對模具的附著而會有讓操作性變差的情形。
另外，已提議有一種調整顆粒的含水率之陶瓷顆粒(專利文獻3)。然而，在顆粒的含水率變多的情形，由於顆粒對模具的附著而會有讓操作性變差的情形。
再者，已提議有一種適量添加潤滑劑用以成形大型製品之乾式加壓成形用陶瓷粉末(專利文獻4)。然而，在潤滑劑與其它黏合劑等的含量平衡不良的情形，會有形狀保持性變差、成形體龜裂之情形。
先前技術文獻 專利文獻
專利文獻1 日本特開2001-130969號公報
專利文獻2 日本特開2006-27914號公報
專利文獻3 日本特開2007-197265號公報
專利文獻4 日本特開2001-19558號公報
如上所述，專利文獻1中顆粒的破碎性差，為了解決這個問題，專利文獻2中試圖取得壓力傳遞性與顆粒的壓縮破壞性之平衡，但由於顆粒對模具的附著(脫模性差)而使操作性變差。另外，若如專利文獻3調整顆粒的含水率，則會有由於顆粒對模具的附著(脫模性差)而使操作性變差的情形，而若為了解決這個問題而如專利文獻4適量添加潤滑劑，則會有形狀保持性變差、成形體龜裂的情形。
本案發明者們欲解決對模具之附著的問題，讓脫模時的脫模性變好，而著眼於硬脂酸及與其組合的聚伸烷基氧化物，為了得到它們的適切調配比例而不斷專心努力，終於達成本發明。此處專利文獻2中雖有硬脂酸及聚伸烷基氧化物之記載，但關於適切的調合比例則沒記載。
本發明係關於以加壓成形、生胚加工製造高密度、高強度為必要的陶瓷成形體的製程中，有效率的加壓成形，且容易生胚加工，具優良的成形時的成形性、形狀保持性、及特別是脫模時的脫模性之陶瓷顆粒及陶瓷顆粒之製造方法，與將陶瓷顆粒加以成形而成之陶瓷成形體。
本發明為了解決這些課題，而具有以下構成。亦即，本發明係一種陶瓷顆粒，其係含有由丙烯酸共聚樹脂 (a-1)、聚乙烯醇(a-2)、聚伸烷基氧化物(a-3)及硬脂酸(a-4)所構成之有機成分(A)、與陶瓷粉體(B)之陶瓷顆粒，其特徵為：相對於100重量份的丙烯酸共聚樹脂(a-1)，其係含有25~35重量份的聚乙烯醇(a-2)、25~35重量份的聚伸烷基氧化物(a-3)、15~25重量份的硬脂酸(a-4)。
本發明之陶瓷顆粒，相對於陶瓷粉體(B)的總表面積，較佳係以3.2~5.3mg/m2之比例含有有機成分(A)。又，陶瓷粉體(B)係由氧化鋯(b-1)及氧化釔(b-2)所構成，而相對於100重量份的氧化鋯(b-1)，較佳含有3~10重量份的氧化釔(b-2)。
又本發明為一種陶瓷顆粒之製造方法，其係含有由丙烯酸共聚樹脂(a-1)、聚乙烯醇(a-2)、聚伸烷基氧化物(a-3)及硬脂酸(a-4)所構成之有機成分(A)、與陶瓷粉體(B)之陶瓷顆粒的製造方法，其特徵為：具有把陶瓷粉體(B)漿液化之步驟；把有機成分(A)添加至該漿液化的陶瓷粉體(B)，邊攪拌邊混合之步驟；把該經過混合的陶瓷粉體(B)及有機成分(A)加以造粒之步驟；其中，相對於100重量份的丙烯酸共聚樹脂(a-1)，有機成分(A)係含有25~35重量份的聚乙烯醇(a-2)、25~35重量份的聚伸烷基氧化物(a-3)、及15~25重量份的硬脂酸(a-4)之乳液。本發明之陶瓷顆粒之製造方法中，陶瓷粉體(B)的BET比表面積較佳為6~10m2/g。
又本發明係一種陶瓷成形體，其係將本發明之陶瓷顆粒加以成形而成。
藉由本發明，能提供以加壓成形、生胚加工製造高密度、高強度為必要的陶瓷成形體的製程中，有效率的加壓成形，且容易生胚加工，具優良的成形時的成形性、形狀保持性、及特別是脫模時的脫模性之陶瓷顆粒及將該陶瓷顆粒加以成形而成之陶瓷成形體。
實施發明之形態
本發明的一實施態樣之陶瓷顆粒係含有由丙烯酸共聚樹脂(a-1)、聚乙烯醇(a-2)、聚伸烷基氧化物(a-3)及硬脂酸(a-4)所構成之有機成分(A)與陶瓷粉體(B)之陶瓷顆粒，係由相對於100重量份的丙烯酸共聚樹脂(a-1)，含有25~35重量份的聚乙烯醇(a-2)、25~35重量份的聚伸烷基氧化物(a-3)、及15~25重量份的硬脂酸(a-4)之陶瓷顆粒所構成。
本實施態樣的陶瓷顆粒係含有有機成分(A)，有機成分(A)具有作為黏結劑之任務。作為有機成分(A)，成形時的成形性、形狀保持性、自模具的脫模性係必要的，故含有丙烯酸共聚樹脂(a-1)、聚乙烯醇(a-2)、聚伸烷基氧化物(a-3)及硬脂酸(a-4)係重要的。
此處，因丙烯酸共聚樹脂(a-1)係柔軟的，藉由使用它能使顆粒容易粉碎。又，若是玻璃轉移溫度為-20~30℃的丙烯酸共聚樹脂，因可減少調配量，可防止脫脂時的破損、成形體之變形，故為優選。
雖然若使用聚乙烯醇(a-2)會有讓顆粒變堅實的傾向，但會讓形狀保持性、生胚加工性變好。其中較佳為平均聚合度300~1000之聚乙烯醇。若在此範圍內，則壓縮破壞強度不會變得過高，且讓黏著力不足的情形變少。
聚伸烷基氧化物(a-3)係賦予顆粒可塑性，並可進一步賦與優良的壓力傳遞性。其中較佳使用數量平均分子量1000~3萬之聚伸烷基氧化物。聚伸烷基氧化物的數量平均分子量若超過3萬則會看不到可塑性的提升效果。另一方面，在數量平均分子量少於1000之情形，因在室溫會變成液狀，造成粉末凝聚，而有粉末對模具的填充性惡化的情形。進一步為了提升顆粒的低壓崩壞，藉由添加數量平均分子量10萬~15萬之聚伸烷基氧化物，因能賦予適當的壓縮破壞性，能進一步讓成形體的空隙變小。聚伸烷基氧化物的數量平均分子量若小於10萬，則崩潰性之賦予過少，見不到添加的效果，而若使用超過15萬者，則崩潰性會惡化，有壓縮破壞強度變過高的情況。
此處說的聚環氧乙烷係一種聚乙二醇。但是相對於上述的數量平均分子量1000~3萬之聚乙二醇係將環氧乙烷縮合開環聚合於乙二醇而成，聚環氧乙烷係將環氧乙烷配位開環聚合而成，聚乙二醇係以下式(1)表示，聚環氧乙烷係以下式(2)表示。
HO-(CH2-CH2-O-)mH………(1)
HO~(CH2-CH2-O-)n~H………(2)
(式(1)中，m表示23~682之整數，式(2)中，n表示2273~3409之整數。)
硬脂酸(a-4)能讓與加壓金屬模具的金屬模具、橡膠壓模機的心軸之脫模滑順的進行。
本實施態樣之陶瓷顆粒，將其適量組合之黏結劑係重要的，相對於100重量份的丙烯酸共聚樹脂(a-1)，聚乙烯醇(a-2)的含有比例為25~35重量份，且聚伸烷基氧化物(a-3)的含有比例為25~35重量份，且硬脂酸(a-4)的含有比例為15~25重量份係重要的。
相對於100重量份的丙烯酸共聚樹脂(a-1)，若聚乙烯醇(a-2)的含有比例比35重量份多，則顆粒會變得過於堅實，有可能顆粒無法順利的粉碎，產生低密度的成形體。又，若相對於100重量份的丙烯酸共聚樹脂(a-1)，聚乙烯醇(a-2)的含有比例比25重量份少，則有可能顆粒變得太柔軟而產生破損，於生胚加工時發生龜裂。更佳為，相對於100重量份的丙烯酸共聚樹脂(a-1)，聚乙烯醇(a-2)的含有比例為25~30重量份。
相對於100重量份的丙烯酸共聚樹脂(a-1)，若聚伸烷基氧化物(a-3)的含有比例比35重量份多，則會妨害到黏著性，而有成形體發生龜裂的情形。相對於100重量份的丙烯酸共聚樹脂(a-1)，若聚伸烷基氧化物(a-3)的含有比例比25重量份少，則會有可塑性的效果變少，而無法成形複雜的形狀之情形。更佳為，相對於100重量份的丙烯酸共聚樹脂(a-1)，聚伸烷基氧化物(a-3)的含有比例為25~30重量份。
相對於100重量份的丙烯酸共聚樹脂(a-1)，若硬脂酸(a-4)的含有比例比25重量份多，則會妨害到黏著性，而有成形體發生龜裂的情形。相對於100重量份的丙烯酸共聚樹脂(a-1)，若硬脂酸(a-4)的含有比例比15重量份少，則會有脫模性的效果變少，而無法成形複雜的形狀之情形。更佳為，相對於100重量份的丙烯酸共聚樹脂(a-1)，硬脂酸(a-4)的含有比例為15~20重量份。
相對於陶瓷粉體(B)的總表面積，較佳以3.2~5.3mg/m2之比例含有有機成分(A)。有機成分的含有比例係以「含有比例=有機物重量÷陶瓷粉體重量÷陶瓷粉體的BET比表面積」的數學式來求取。此處，有機物重量能作為將陶瓷顆粒在大氣中以800℃燒成3小時之際，燒成前後的重量差來求取。陶瓷粉體重量能作為將陶瓷顆粒在大氣中以800℃燒成3小時之際的燒成後重量來求取。
陶瓷粉體的BET比表面積，能使用將陶瓷顆粒在大氣中以800℃燒成3小時後的陶瓷粉體，依據JIS-R1626「使用精密陶瓷粉體之氣體吸附BET法的比表面積之測定方法」，以BET 1點法求取。黏結劑等有機成分的量係支配形成顆粒之粒子的表面積。有機成分若少於3.2mg/m2，則在成形步驟的減壓時或脫模際會有破損。又在生胚加工時會有成形體的邊緣龜裂、破損的情形。若超過5.3mg/m2，則因會發生對金屬模具附著、產生脫脂破損，產生拉長脫脂時間的必要。又，在生胚加工時，會有成形體的黏性過高，無法順利加工的情形。另外， 在將成形體閒置期間會有變形的情況。有機成分的含有比例更佳為3.6~4.5mg/m2。
構成本實施態樣之陶瓷顆粒的陶瓷粉體(B)之種類無特別限定，因必須要有緻密且高強度之性能，較佳分別單獨使用氧化鋁、氧化鋯、氧化釔、氮化矽、碳化矽、碳化鎢、氮化鈦、莫來石、SiAloN、矽酸鈣、堇青石、鋰輝石、沸石、鋯石等，或使用它們複合而成之物。其中，更佳為使用泛用性高的氧化鋁、氧化鋯及其混合物。
特別是陶瓷粉體(B)係含有氧化鋯(b-1)及氧化釔(b-2)，且相對於100重量份的氧化鋯(b-1)，氧化釔(b-2)的含有比例較佳為3~10重量份，更佳為4~8重量份。氧化釔(b-2)的含有比例若為3~10重量份，則更可展現氧化鋯(b-1)的高強度性、高韌性。
構成本實施態樣之陶瓷顆粒的陶瓷粉體(B)之平均凝聚粒徑較佳為0.1~2μm，更佳為0.3~1μm。若在此範圍內，則在構成顆粒時顆粒會變密，壓縮破壞強度不會變得太高，也不會有燒結性悪化，在與顆粒性質無關的燒結體內存在大量空隙而變成低燒結體密度的情況。藉由讓平均凝聚粒徑在0.1~2μm，作為陶瓷的燒結性優良，並可使有機成分均勻的分散於顆粒內，及減少燒結體中的殘留空隙。
下面舉例說明本實施態樣的陶瓷顆粒之製造方法。
本實施態樣的陶瓷顆粒之製造方法，係含有由丙烯酸共聚樹脂(a-1)、聚乙烯醇(a-2)、聚伸烷基氧化物(a-3)及硬脂酸(a-4)所構成之有機成分(A)及陶瓷粉體(B)的陶 瓷顆粒之製造方法，其係具有：把陶瓷粉體(B)漿液化之步驟；把有機成分(A)添加至該漿液化的陶瓷粉體(B)邊攪拌邊混合之步驟；把該經過混合的陶瓷粉體(B)及有機成分(A)加以造粒之步驟；其中，(A)有機成分相對於100重量份的丙烯酸共聚樹脂(a-1)，係含有25~35重量份的聚乙烯醇(a-2)、25~35重量份的聚伸烷基氧化物(a-3)、15~25重量份的硬脂酸(a-4)之乳液。
首先，以濕式或乾式粉碎陶瓷粉體，使其分散於水中並漿液化。濕式粉碎較佳為珠磨機或研磨機等介質媒體型攪拌法。而在乾式粉碎較佳是以噴射研磨機或乾式研磨機等粉碎/混合，以球磨機或攪拌型分散混合機在水中均勻分散。此處，係調節粉碎時間讓以BET 1點法測定之BET比表面積落入6~10m2/g之範圍，較佳為7~9m2/g。
接著相對於100重量份的丙烯酸共聚樹脂(a-1)，將25~35重量份的聚乙烯醇(a-2)、25~35重量份的聚伸烷基氧化物(a-3)、及15~25重量份的硬脂酸(a-4)之乳液添加至有機成分。較佳為使此有機成分的比例為3.2~5.3mg/m2之方式將有機成分添加至漿液，邊充分攪拌邊混合。更佳為有機成分的比例為3.6~4.5mg/m2。
其次，把漿液與有機成分攪拌混合而成之物，以噴霧乾燥機等使用噴霧乾燥法製出平均顆粒直徑10~90μm之造粒體。關於顆粒直徑之調整，在圓盤式的情形係調整圓盤的轉速，而在雙流體噴嘴式的情形則係藉由調整空氣壓力與供給量來進行。而關於噴霧乾燥機的乾燥溫 度，若殘存的水分能保持陶瓷顆粒的形狀即可，較佳讓水分殘存率在0.1~2重量份之範圍，通常設定於70℃~120℃即可。自所得到的顆粒以篩將200μm以上的顆粒或凝集物去除，以磁石等將來自裝置的鐵的雜質除去，得到陶瓷顆粒。
下面舉例說明本實施態樣之陶瓷成形體及其製造方法。本實施態樣之陶瓷成形體能藉由將上述本實施態樣的陶瓷顆粒加以成形、把本實施態樣之陶瓷顆粒填充至成形用金屬模具之方法、或填充至圓柱狀橡膠模具，以98~343MPa的壓力予以加壓成形來得到。如此進行所得到的陶瓷成形體之密度係2.9~3.3g/cm3，成為成形體強度2.8~5.7MPa之高強度成形體。
而如此進行所得到的陶瓷成形體可燒成成為燒結體。燒結條件依使用的陶瓷粉末之種類而不同。例如，在使用氧化鋯粉末之情形，較佳為1300~1500℃、1~5小時。而在使用氧化鋁粉末之情形，較佳為1500~1700℃、1~5小時。
[實施例]
下面以實施例具體說明本發明。但是本發明不受此等實施例任何限制。
實施例的各物性之測定及評價係如下述般進行。
(1)BET比表面積
BET比表面積之測定係使用將陶瓷顆粒在大氣中以800℃燒成3小時而成的陶瓷粉體，依照JIS-R1626「使用精密陶瓷粉體之氣體吸附BET法的比表面積之測定方法」，以BET 1點法進行。
(2)有機物量
將陶瓷顆粒在大氣中以800℃燒成3小時，求取其前後的重量差。
(3)陶瓷粉體重量
將陶瓷顆粒在大氣中以800℃燒成3小時，求取燒成後的重量。
(4)有機成分的含有比例
以「有機物重量÷陶瓷粉體重量÷陶瓷粉體的BET比表面積」之數學式求取。
(5)平均凝聚粒徑
於300cc的燒杯中加入導電度5μS/cm之純水210g、添加有機性成分前的漿液90g，仔細攪拌後，於超音波產生機歷經10分鐘製作調製液。使用粒度分布計，測定調製液的凝聚粒子直徑，取累積分布相當於50%，亦即中值粒徑為平均凝聚粒徑。粒度分布計係使用堀場製作所製LA200。
(6)平均顆粒直徑
使用田中化學機械(股)製R-2型振篩機，以標準篩測定。取累積分布相當於50%，亦即中值粒徑為平均顆粒直徑。
(7)聚乙烯醇之平均聚合度測定
依JISK6726(1994年改正)的聚乙烯醇的平均聚合度之試驗方法測定。
(8)丙烯酸共聚樹脂之玻璃轉移溫度測定
依JISK7121(1987年制定)塑膠的轉移溫度測定法之熱機械分析法(TMA)測定。
(9)聚環氧乙烷之數量平均分子量測定
以四氫呋喃為溶媒予以溶解，測定凝膠滲透層析法(GPC)。
(10)CIP成形時的破損、龜裂
將所得到的陶瓷顆粒填充進內徑30cm×高度30cm的圓柱狀橡膠模具，以CIP法取設定壓力為98MPa，以5分鐘升壓至設定壓力，保持30秒後，以5秒減壓。取出本成形體時，以目視判定成形體的破損與龜裂的程度。破損/龜裂的程度係把成形體從內部開始破損，或邊緣部分從上面起龜裂3cm以上者龜裂者當成×、除此之外當成○。
(11)生胚加工性
將所得到的陶瓷顆粒填充進內徑30cm×高度30cm的圓柱狀橡膠模具，以CIP法取設定壓力為98MPa，以5分鐘升壓至設定壓力，保持30秒後，以5秒減壓。從所得到的成形體裁切出直徑10cm×長度20cm之圓柱成形體，置於車床上，重複切下0.5mm之切削，在50次以內邊緣龜裂者為×、在此之上者為○。實驗進行2次，以平均值判斷。
(12)燒結相對密度
使用CIP裝置以1ton/cm2之條件將陶瓷粉末加以成形，將其成形體加工成Φ25×L25mm之圓柱，以特定溫度 度燒結2小時。將燒結體的實測密度除以理論密度，把將其以百分比表示之值當成燒結相對密度。此處陶瓷燒結體的實測密度係以阿基米德法測定。而相對於100重量份的氧化鋯，以5.7重量份之比例含有氧化釔之部分安定化鋯粉末的理論密度係設為6.08g/cm3。
(13)抗彎強度
使用CIP裝置以1ton/cm2之條件將陶瓷粉末加以成形，以特定溫度將其成形體燒結2小時。自燒結體裁切出3×4×約40mm之試料片，按照JIS-R 1601「精密陶瓷之抗彎強度試驗方法」，測定3點抗彎強度。
(14)成形體密度
以98.343MPa之壓力將所得到的陶瓷顆粒加壓成形，製作陶瓷成形體(48mm×6.5mm×5.4mm)，測定尺寸至微米，以電子天秤測定重量再計算。
(15)成形體強度
以98.343MPa之壓力將所得到的陶瓷顆粒加壓成形，製作陶瓷成形體(48mm×6.5mm×5.4mm)，使用萬能試驗機依照JIS R1601所規定之方法測定成形體強度。
(實施例1)
作為陶瓷粉末，將相對於100重量份的氧化鋯，以5.7重量份之比例含有氧化釔的部分安定化鋯粉末，以濕式研磨機粉碎2小時予以漿液化。接著作為有機成分，相對於100重量份的陶瓷粉末，添加以下的量。
玻璃轉移溫度為負8℃的丙烯酸共聚樹脂：1.8重量份
平均聚合度500的聚乙烯醇：0.5重量份(相對於100重量份的丙烯酸共聚樹脂係28重量份)
數量平均分子量10萬的聚環氧乙烷：0.5重量份(相對於100重量份的丙烯酸共聚樹脂係28重量份)
硬脂酸乳液：0.4重量份(相對於100重量份的丙烯酸共聚樹脂係23重量份)
用噴霧乾燥機以乾燥溫度100℃將本漿液噴霧乾燥，經由進行過篩、去鐵，得到實施例1之陶瓷顆粒。
對本顆粒以上述方法測定成形體密度、成形體強度，以CIP法成形確認破損，評價生胚加工性。另以設定溫度1400℃燒結2小時製作燒結體，測定燒結相對密度、抗彎強度。結果示於表1。
(實施例2)
作為陶瓷粉末，將相對於100重量份的氧化鋯，以5.7重量份之比例含有氧化釔的部分安定化鋯粉末，以濕式研磨機粉碎2小時予以漿液化。接著作為有機成分，相對於100重量份的陶瓷粉末，添加以下的量。
玻璃轉移溫度為負8℃的丙烯酸共聚樹脂：2.5重量份
平均聚合度500的聚乙烯醇：0.7重量份(相對於100重量份的丙烯酸共聚樹脂係28重量份)
數量平均分子量10萬的聚環氧乙烷：0.7重量份(相對於100重量份的丙烯酸共聚樹脂係28重量份)
硬脂酸乳液：0.55重量份(相對於100重量份的丙烯酸共聚樹脂係22重量份)
用噴霧乾燥機以乾燥溫度100℃將本漿液噴霧乾燥，經由進行過篩、去鐵，得到實施例2之陶瓷顆粒。
對本顆粒以上述方法測定成形體密度、成形體強度，以CIP法成形確認破損，評價生胚加工性。另以設定溫度1400℃燒結2小時製作燒結體，測定燒結相對密度、抗彎強度。結果示於表1。
(實施例3)
將99.9%的高純度氧化鋁粉末以濕式研磨機粉碎2小時予以漿液化。接著作為有機成分，相對於100重量份的陶瓷粉末，添加以下的量。
玻璃轉移溫度為負8℃的丙烯酸共聚樹脂：1.8重量份
平均聚合度500的聚乙烯醇：0.5重量份(相對於100重量份的丙烯酸共聚樹脂係28重量份)
數量平均分子量10萬的聚環氧乙烷：0.5重量份(相對於100重量份的丙烯酸共聚樹脂係28重量份)
硬脂酸乳液：0.4重量份(相對於100重量份的丙烯酸共聚樹脂係23重量份)
用噴霧乾燥機以乾燥溫度100℃將本漿液噴霧乾燥，經由進行過篩、去鐵，得到實施例3之顆粒。
對本顆粒以上述方法測定成形體密度、成形體強度，以CIP法成形確認破損，評價生胚加工性。另以設定溫度1600℃燒結2小時製作燒結體，測定燒結相對密度、抗彎強度。結果示於表1。
(實施例4)
作為陶瓷粉末，將相對於100重量份的氧化鋯，以5.7重量份之比例含有氧化釔的部分安定化鋯粉末，以濕式研磨機粉碎1小時予以漿液化。接著作為有機成分，相對於100重量份的陶瓷粉末，添加以下的量。
玻璃轉移溫度為負8℃的丙烯酸共聚樹脂：1.3重量份
平均聚合度500的聚乙烯醇：0.35重量份(相對於100重量份的丙烯酸共聚樹脂係28重量份)
數量平均分子量10萬的聚環氧乙烷：0.35重量份(相對於100重量份的丙烯酸共聚樹脂係28重量份)
硬脂酸乳液：0.3重量份(相對於100重量份的丙烯酸共聚樹脂係23重量份)
用噴霧乾燥機以乾燥溫度100℃將本漿液噴霧乾燥，經由進行過篩、去鐵，得到實施例4之陶瓷顆粒。
對本顆粒以上述方法測定成形體密度、成形體強度，以CIP法成形確認破損，評價生胚加工性。另以設定溫度1400℃燒結2小時製作燒結體，測定燒結相對密度、抗彎強度。結果示於表1。
(實施例5)
作為陶瓷粉末，將相對於100重量份的氧化鋯，以5.7重量份之比例含有氧化釔的部分安定化鋯粉末，以濕式研磨機粉碎2小時予以漿液化。接著作為有機成分，相對於100重量份的陶瓷粉末，添加以下的量。
玻璃轉移溫度為負8℃的丙烯酸共聚樹脂：1.8重量份
平均聚合度500的聚乙烯醇：0.5重量份(相對於100重量份的丙烯酸共聚樹脂係28重量份)
數量平均分子量10萬的聚環氧乙烷：0.5重量份(相對於100重量份的丙烯酸共聚樹脂係28重量份)
硬脂酸乳液：0.3重量份(相對於100重量份的丙烯酸共聚樹脂係16重量份)
用噴霧乾燥機以乾燥溫度100℃將本漿液噴霧乾燥，經由進行過篩、去鐵，得到實施例5之陶瓷顆粒。
對本顆粒以上述方法測定成形體密度、成形體強度，以CIP法成形確認破損，評價生胚加工性。另以設定溫度1400℃燒結2小時製作燒結體，測定燒結相對密度、抗彎強度。結果示於表1。
(比較例1)
作為陶瓷粉末，將相對於100重量份的氧化鋯，以5.7重量份之比例含有氧化釔的部分安定化鋯粉末，以濕式研磨機粉碎2小時予以漿液化。接著作為有機成分，相對於100重量份的陶瓷粉末，添加以下的量。
玻璃轉移溫度為負8℃的丙烯酸共聚樹脂：1.8重量份
平均聚合度500的聚乙烯醇：0.5重量份(相對於100重量份的丙烯酸共聚樹脂係28重量份)
數量平均分子量10萬的聚環氧乙烷：0.5重量份(相對於100重量份的丙烯酸共聚樹脂係28重量份)
用噴霧乾燥機以乾燥溫度100℃將本漿液噴霧乾燥，經由進行過篩、去鐵，得到比較例1之陶瓷顆粒。
對本顆粒以上述方法測定成形體密度、成形體強度，以CIP法成形確認破損，評價生胚加工性。另以設定溫度1400℃燒結2小時製作燒結體，測定燒結相對密度、抗彎強度。結果示於表1。
(比較例2)
作為陶瓷粉末，將相對於100重量份的氧化鋯，以5.7重量份之比例含有氧化釔的部分安定化鋯粉末，以濕式研磨機粉碎2小時予以漿液化。接著作為有機成分，相對於100重量份的陶瓷粉末，添加以下的量。
玻璃轉移溫度為負8℃的丙烯酸共聚樹脂：1.8重量份
平均聚合度500的聚乙烯醇：0.5重量份(相對於100重量份的丙烯酸共聚樹脂係28重量份)
數量平均分子量10萬的聚環氧乙烷：0.5重量份(相對於100重量份的丙烯酸共聚樹脂係28重量份)
硬脂酸乳液：0.4重量份(相對於100重量份的丙烯酸共聚樹脂係23重量份)
用噴霧乾燥機以乾燥溫度100℃將本漿液噴霧乾燥，經由進行過篩、去鐵，得到比較例2之陶瓷顆粒。
對本顆粒以上述方法測定成形體密度、成形體強度，以CIP法成形確認破損，評價生胚加工性。另以設定溫度1400℃燒結2小時製作燒結體，測定燒結相對密度、抗彎強度。結果示於表1。
產業利用性
本發明之陶瓷顆粒及陶瓷顆粒之製造方法能利用於以生胚加工、用加壓成形製造必須要高密度、高強度之陶瓷成形體的製程。

Claims (6)

  1. 一種陶瓷顆粒，其係含有由丙烯酸共聚樹脂(a-1)、聚乙烯醇(a-2)、聚伸烷基氧化物(a-3)及硬脂酸(a-4)所構成之有機成分(A)、與陶瓷粉體(B)之陶瓷顆粒，其特徵為：相對於100重量份的丙烯酸共聚樹脂(a-1)，其係含有25~35重量份的聚乙烯醇(a-2)、25~35重量份的聚伸烷基氧化物(a-3)、及15~25重量份的硬脂酸(a-4)。
  2. 如申請專利範圍第1項之陶瓷顆粒，其相對於陶瓷粉體(B)的總表面積，係以3.2~5.3mg/m2之比例含有有機成分(A)。
  3. 如申請專利範圍第1或2項之陶瓷顆粒，其中陶瓷粉體(B)係由氧化鋯(b-1)及氧化釔(b-2)所構成，且相對於100重量份的氧化鋯(b-1)，其係含有3~10重量份的氧化釔(b-2)。
  4. 一種陶瓷顆粒之製造方法，其係含有由丙烯酸共聚樹脂(a-1)、聚乙烯醇(a-2)、聚伸烷基氧化物(a-3)及硬脂酸(a-4)所構成之有機成分(A)、與陶瓷粉體(B)之陶瓷顆粒的製造方法，其特徵為：具有把陶瓷粉體(B)漿液化之步驟；把有機成分(A)添加至該漿液化的陶瓷粉體(B)，邊攪拌邊混合之步驟；把該經過混合的陶瓷粉體(B)及有機成分(A)加以造粒之步驟；其中，相對於100重量份的丙烯酸共聚樹脂(a-1)，有機成分(A)係含有25~35重量份的聚乙烯醇(a-2)、25~35重量份的聚伸烷基氧化物(a-3)、及15~25重量份的硬脂酸(a-4)之乳液。
  5. 如申請專利範圍第4項之陶瓷顆粒之製造方法，其中陶瓷粉體(B)的BET比表面積為6~10m2/g。
  6. 一種陶瓷成形體，其係將如申請專利範圍第1至3項中任一項之陶瓷顆粒加以成形而成。
TW101135451A 2011-09-29 2012-09-27 陶瓷顆粒及陶瓷顆粒之製造方法以及陶瓷成形體 TW201319004A (zh)

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