TW201144254A - Slurry composition for ceramic green sheet, ceramic green sheet, and multilayer ceramic capacitor - Google Patents
Slurry composition for ceramic green sheet, ceramic green sheet, and multilayer ceramic capacitor Download PDFInfo
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- TW201144254A TW201144254A TW099145524A TW99145524A TW201144254A TW 201144254 A TW201144254 A TW 201144254A TW 099145524 A TW099145524 A TW 099145524A TW 99145524 A TW99145524 A TW 99145524A TW 201144254 A TW201144254 A TW 201144254A
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- Prior art keywords
- ceramic green
- mol
- degree
- ceramic
- green sheet
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Classifications
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- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/08—Inorganic dielectrics
- H01G4/12—Ceramic dielectrics
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
- C04B35/465—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates
- C04B35/468—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates
- C04B35/4682—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates based on BaTiO3 perovskite phase
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62625—Wet mixtures
- C04B35/6264—Mixing media, e.g. organic solvents
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/6342—Polyvinylacetals, e.g. polyvinylbutyral [PVB]
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/636—Polysaccharides or derivatives thereof
- C04B35/6365—Cellulose or derivatives thereof
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/48—Isomerisation; Cyclisation
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/30—Stacked capacitors
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Description
201144254 六、發明說明: 【發明所屬之技術領域】 本發明係關於陶瓷胚片用漿料組成物, 合陶瓷電容器。 【先前技術】 在製造層合陶瓷電容器時,一般而言是 。首先,將聚乙烯縮醛樹脂等之黏合劑樹脂 於分散有陶瓷粉末之有機溶劑中,並藉由球 混合而調製出陶瓷胚片用漿料組成物,以流 調製之漿料組成物成形於聚對苯二甲酸乙二 支撐體上,並藉由加熱等來餾除溶劑等後, 離而製造出陶瓷胚片。 此等陶瓷胚片,.是從上述剝離性支撐體 首先,係交互地重疊複數片之藉由網版印刷 的表面形成有成爲內部電極之導電膏而成者 壓著而得層合體。接著藉由各步驟來形成層 爲既定形狀。然後在進行以熱分解來去除該 含之黏合劑成分等之處理,亦即進行所謂的 進行燒結而得陶瓷燒結物,並將外部電極燒 結物的端面上,藉由此步驟,來製造出層合 因此,上述陶瓷胚片,係要求陶瓷胚片用漿 製作業之良好的作業性,以及可承受此等加 強度。 陶瓷胚片及層 進行下列步驟 與可塑劑添加 磨機等均一地 體鑄膜法將所 酯等之剝離性 從支撐體中剝 中剝離使用。 等在陶瓷胚片 ,並進行加熱 合體,並裁切 層合體中所包 脫脂處理後, 結於該陶瓷燒 陶瓷電容器。 料組成物的調 工的各步驟之 -5- 201144254 近年來,隨著電子機器的多功能化和小型化,對於層 合陶瓷電容器亦要求大容量化、小型化。因應於此’陶瓷 胚片中所使用之陶瓷粉末,係採用〇.5μηι以下的細微粒徑 者,並嘗試在剝離性支撐體上可塗佈成5μπι以下的薄膜狀 者。 然而,當使用細微粒徑的陶瓷粉末時,由於充塡密度 和表面積增加,使所使用之黏合劑樹脂量增加,進而使陶 瓷胚片用漿料組成物的黏度亦增大,有時會難以塗佈或產 生陶瓷粉末本身的分散不良。另一方面,在陶瓷胚片製作 時的各步驟中,會受到拉伸和彎曲等之應力負荷,故需採 用具有可承受此般應力之充分強度的黏合劑。 爲了解決此問題,專利文獻1係揭示一種對鹼化度8 0 莫耳%以上之聚乙烯醇的乙烯醇單位,以0.005〜2莫耳%的 比率至少添加二醛來進行縮醛化而成之陶瓷胚片用陶瓷膏 ,而實現一種機械強度佳之陶瓷胚片用漿料組成物。 然而,當以二醛進行交聯時,分子間交聯變得過密, 所得之薄膜胚片的機械強度雖有所提升,但所得之交聯聚 乙烯縮醛樹脂的一部分不溶於有機溶劑,而具有殘存部分 未溶解份之問題。此外,由於交聯部位與未交聯部位的應 力緩和力不同’故具有薄膜胚片產生翹曲之問題。 [先前技術文獻] [專利文獻] 專利文獻1:日本特開2006-282490號公報 201144254 【發明內容】 (發明所欲解決之課題) 本發明係鑒於上述現狀而提供一種可製得具有充分的 機械強度且翹曲少之陶瓷胚片之陶瓷胚片用漿料組成物, 陶瓷胚片及層合陶瓷電容器。 (用以解決課題之手段) 本發明者們係進行精心探討,結果發現到藉由使用聚 合度超過1 000且爲4500以下、乙烯酯單位的含量小於1莫 耳%且縮醛化度爲60〜83莫耳%之聚乙烯縮醛樹脂作爲陶瓷 胚片用漿料組成物的黏合劑樹脂,可形成塗佈性佳之組成 物,即使將厚度薄化,亦可製得機械強度高且不易翹曲之 陶瓷胚片,因而完成本發明。 發明之效果: 能夠提供一種可製得具有充分的機械強度且翹曲少之 陶瓷胚片之陶瓷胚片用漿料組成物,陶瓷胚片及層合陶瓷 電容器》 【實施方式】 以下詳細說明本發明。 本發明中所使用之聚乙烯縮醛樹脂的聚合度,係超過 1000且爲45 00以下。聚合度爲1 000以下時,當製作厚度 2μπι以下的薄膜陶瓷胚片時,機械強度變得不足,聚合度 201144254 超過45 00時,無法充分地溶解於有機溶劑,或是溶液黏度 過高使塗佈性和分散性降低。聚乙烯縮醛樹脂之聚合度的 較佳下限爲1 500,上限爲3500。 上述聚合度,係從聚乙烯縮醛樹脂的製造時所使用之 聚乙烯醇樹脂的黏度平均聚合度,以及聚乙烯縮醛樹脂的 黏度平均聚合度兩者中求取。亦即,由於聚合度不會因縮 醛化而改變,所以聚乙烯醇樹脂與將該聚乙烯醇樹脂進行 縮醛化所得之聚乙烯縮醛樹脂的聚合度相同。雖無特別限 定,但聚乙烯醇樹脂的黏度平均聚合度是指根據ns K6726所求取之平均聚合度。此外,當混合2種以上的聚乙 烯醇樹脂作爲聚乙烯醇樹脂使用時,是指混合後之聚乙烯 醇樹脂全體的表觀黏度平均聚合度。另一方面,聚乙嫌縮 醛樹脂的聚合度,是指根據JIS Κ6728所記載的方法,來 測定將聚乙烯醇樹脂進行縮醛化後之黏度平均聚合度者。 上述聚乙嫌縮醒樹脂之乙嫌醋單位的含量係小於1莫 耳% ’較佳上限爲0 · 9 9莫耳%。爲1莫耳%以上時,薄膜的 胚片柔軟性過強,而使陶瓷胚片無法保有充分的機械強度 。乙稀酯單位的含量小於1莫耳%之聚乙烯縮醛樹脂,可藉 由將乙稀酯單位的含量小於1莫耳%之聚乙烯醇樹脂,亦即 驗化度高於99莫耳%之聚乙烯醇樹脂進行縮醛化而得。聚 乙烯醇樹脂之鹼化度的較佳下限爲99.01莫耳%。 上述聚乙烯縮醛樹脂之乙烯酯單位的含量之較佳下限 爲0.01莫耳%。乙烯酯單位的含量小於001莫耳%之聚乙烯 縮醒樹脂’可藉由將鹼化度高於99 99莫耳%之聚乙烯醇樹 201144254 脂進行縮醛化而得。鹼化度高於9 9 · 9 9莫耳%之聚乙烯醇, 工業上難以生產出,且對水的溶解性差,有時難以進行縮 醛化反應。因此’聚乙烯醇樹脂之鹼化度的較佳上限爲 9 9.9 9 莫耳 %。 上述聚乙烯縮醛樹脂之縮醛化度的下限爲60莫耳。/〇, 上限爲83莫耳%。未達60莫耳%時,聚乙烯縮醛樹脂的親 水性高,不易溶解於有機溶劑,對於陶瓷胚片用漿料組成 物的製造形成阻礙,超過8 3莫耳%時,殘存羥基變少,損 及聚乙烯縮醛樹脂的強韌性,就生產性、反應性之觀點來 看,工業上亦難以製得,而導致生產性的降低。縮醛化度 的較佳下限爲65莫耳%,較佳上限爲75莫耳%。 上述聚乙烯縮醛樹脂中所使用之醛類爲單醛(於一分 子內有1個醛基)。當以具有2個以上的醛基之化合物進行 縮醛化時,由於交聯部位與未交聯部位的應力緩和力不同 ’所以在乾燥後從聚對苯二甲酸乙二酯剝離後,有時會產 生翹曲。因此,所使用之醛類較佳爲單醛,即使是使用具 有2個以上的醛基之化合物,相對於聚乙烯醇樹脂的乙烯 醇單位,較佳爲添加少於0.005莫耳%的量,尤佳爲少於 0.003莫耳%的量。 本發明中所使用之聚乙烯縮醛樹脂,通常是以聚乙烯 醇樹脂爲原料來製造出。上述聚乙烯醇樹脂,可藉由以往 所知的手法,亦即使乙烯酯系單體聚合,並將所得之聚合 物進行鹼化而得。使乙烯酯系單體聚合之方法,可使用溶 液聚合法、塊狀聚合法、懸浮聚合法、乳化聚合法等之以 -9 - 201144254 往所知的方法。聚合起始劑,可因應聚合方法來適當地選 擇偶氮系起始劑、過氧化物系起始劑、還原氧化系起始劑 等。鹼化反應,可適用採用有以往所知的鹼觸媒或酸觸媒 之醇解 '水解等,當中,以甲醇爲溶劑並採用氫氧化鈉( NaOH )之鹼化反應較簡便,故最佳。 乙烯酯系單體,例如可列舉出甲酸乙烯酯、乙酸乙烯 酯、丙酸乙烯酯、丁酸乙烯酯、異丁酸乙烯酯、戊酸乙烯 酯、叔碳酸乙烯酯、己酸乙烯酯、辛酸乙烯酯、月桂酸乙 烯酯、棕櫚酸酸乙烯酯、硬脂酸乙烯酯、油酸乙烯酯、苯 甲酸乙烯酯等,尤佳爲乙酸乙烯酯。 此外,當使前述乙烯酯系單體聚合時,在不損及本發 明的主旨之範圍內,亦可與該他單體共聚合。因此,本發 明之聚乙烯醇樹脂,亦含有由乙烯醇單位與該他單體單位 所構成之槪念。該他單體的例子,例如可列舉出乙烯、丙 烯、正丁烯等之α_烯烴:丙烯酸及該鹽類;丙烯酸甲酯、 丙烯酸乙酯、丙烯酸正丙酯、丙烯酸異丙酯、丙烯酸正丁 酯、丙烯酸異丁酯、丙烯酸三級丁酯、丙烯酸2-乙基己酯 、丙烯酸十二烷酯、丙烯酸十八烷酯等之丙烯酸酯類;甲 基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸正丙酯、甲 基丙烯酸異丙酯、甲基丙烯酸正丁酯、甲基丙烯酸異丁酯 、甲基丙烯酸三級丁酯、甲基丙烯酸2-乙基己酯、甲基丙 烯酸十二烷酯、甲基丙烯酸十八烷酯等之甲基丙烯酸酯類 :丙烯醯胺' Ν-甲基丙烯醯胺' Ν-乙基丙烯醯胺、Ν,Ν-二 甲基丙烯醯胺、二丙酮丙烯醯胺、丙烯醯胺丙烷磺酸及該 10· 201144254 鹽類、丙烯醯胺丙基二甲基胺或該酸鹽類或雷 N-羥甲基丙烯醯胺及該衍生物等之丙烯醯胺衍 丙烯醯胺、N -甲基甲基丙烯醯胺、N -乙基甲基 甲基丙烯醯胺丙烷磺酸及該鹽類、甲基丙烯醯 基胺或該酸鹽類或該4級鹽類、N -羥甲基甲基 該衍生物等之甲基丙烯醯胺衍生物;甲基乙烯 烯醚、正丙基乙烯醚、異丙基乙烯醚、正丁基 丁基乙烯醚、三級丁基乙烯醚、十二基乙烯醚 烯醚等之乙烯醚類;丙烯腈、甲基丙烯腈等之 烯、氟乙烯等之鹵化乙烯;偏二氯乙烯、偏二 偏二鹵化乙烯;乙酸烯丙酯、氯化烯丙基等之 物;馬來酸及該鹽類或該酯類或該酐類;乙烯 烷等之乙烯矽烷化合物;乙酸異丙烯酯等。此 對於乙烯酯系單體,通常是以未達10莫耳%的t 縮醛化所使用之酸觸媒並無特別限定,可 或無機酸,例如可列舉出乙酸、對甲苯磺酸、 、鹽酸等。此等當中,較佳爲使用鹽酸、硫酸 佳爲使用鹽酸。 本發明之聚乙烯縮醛樹脂’可藉由下列方 先將3〜1 5質量%濃度的聚乙烯醇樹脂水溶液調 t的溫度範圍,在10~60分鐘間逐漸冷卻該溫 降低至-10〜40 °C時,添加醛及酸觸媒,一邊將 定並在10〜300分鐘間進行縮醛化反應。然後在 間將反應液升溫至45~80°C,並保持該溫度60 〔4級鹽類、 生物:甲基 丙烯醯胺、 胺丙基二甲 丙烯醯胺及 醚、乙基乙 乙烯醚、異 、十八基乙 腈類;氯乙 氟乙烯等之 烯丙基化合 基三甲氧矽 等單體,相 ;:率使用。 使用有機酸 硝酸、硫酸 、硝酸,特 法製得。首 整至80〜100 度》當溫度 溫度保持一 30~200分鐘 ~ 3 6 0分鐘間 -11 - 201144254 。反應的熟化溫度(升溫厚的溫度)較佳爲45°c 4 5 °C更低時,所得之聚乙烯縮醛樹脂的溶液黏度 陶瓷胚片用漿料組成物的分散性降低。接著將該 卻,較佳爲冷卻至室溫,水洗後添加鹼等之中和 行洗淨、乾燥,藉此可得目的之聚乙烯縮醛樹脂 縮醛化度調整爲60〜83莫耳%,必須適當地調整醛 乙烯醇樹脂之添加量,以及添加醛及酸觸媒後的 等。此外,相對於聚乙烯醇100質量份,較佳爲费 質量份的醛。 本發明中,用以將聚乙烯醇樹脂進行縮醛化 無特別限定,例如可列舉出乙醛(包含對乙醛) 丁醛、戊醛、己醛、庚醛、2-乙基己醛、環己醛 醛、苯甲醛、2-甲基苯甲醛、3-甲基苯甲醛、4-醛、對羥基苯甲醛、間羥基苯甲醛、苯基乙醛、 醛等。當中,就生產性與特性均衡之觀點來看, 醛、丁醛。此等醛可單獨使用或倂用2種以上。 所使用之聚乙烯縮醛樹脂,爲使用碳數2〜6的醛 使用碳數2〜4的醛之聚乙烯縮醛樹脂,當中就陶 機械強度、塗佈性之觀點來看,較佳爲使用正丁 烯縮醛樹脂。 本發明之聚乙烯縮醛樹脂中之上述α-烯烴鏈 ’較佳下限爲1莫耳%,較佳上限爲20莫耳%。當 段的含量未達1莫耳%時,含有上述α-烯烴之效果 過2 0莫耳%時’疏水性過強’使陶瓷粉末的分散 以上。較 增高,使 反應液冷 劑,並進 。爲了將 相對於聚 反應時間 I加46〜74 之單醛並 、丙醛、 、咲喃甲 甲基苯甲 β-苯基丙 較佳爲乙 本發明中 ,尤其是 瓷胚片的 醛之聚乙 段的含量 α-烯烴鏈 不足,超 性降低, 201144254 或是由於聚乙烯醇樹脂的溶解性降低,而使縮醛化反應難 以進行。 此外’本發明之陶瓷胚片用漿料組成物,黏合劑樹脂 ’除了上述聚乙烯縮醛樹脂外,亦可含有丙烯酸系樹脂、 纖維素系樹脂。當含有丙烯酸系樹脂、纖維素系樹脂等作 爲黏合劑樹脂時,上述聚乙烯縮醛樹脂於黏合劑樹脂全體 中所佔有之含量的較佳下限爲30質量%。未達30質量%時 ’可能使所得之陶瓷胚片的機械強度變得不足。 本發明中所使用之聚乙烯縮醛樹脂,可藉由將聚合度 超過1〇〇〇且爲4500以下之聚乙烯醇樹脂以醛進行縮醛化而 製造出。當混合使用2種以上的聚乙烯醇樹脂時,各樹脂 之聚合度的平均値爲超過1000且爲4500以下即可。聚合度 的平均値之較佳下限爲1500,上限爲3500» 上述陶瓷粉末並無特別限定,例如可列舉出氧化鋁、 氧化銷、矽酸鋁、氧化鈦、氧化鋅、鈦酸鋇、氧化鎂、賽 隆(SiAlON )、只匕。木厶小歹彳卜、碳化矽、氮化矽、氮 化鋁等粉末。此等陶瓷粉末可單獨使用或併用2種以上。 陶瓷粉末相對於本發明之陶瓷胚片用漿料組成物的全體量 之含量的上限爲80質量%,下限爲30質量%。當陶瓷粉末 的含量少於3 0質量%時,黏度變得過低,使陶瓷胚片成形 時的處理性變差,當多於80質量%時,陶瓷胚片用漿料組 成物的黏度變得過高,捏揉性有降低之傾向。 上述有機溶劑並無特別限定,例如可列舉出丙酮、丁 酮、二丙酮、二異丁酮等之酮類;甲醇、乙醇、異丙醇、 -13- 201144254 丁醇等之醇類;甲苯、二甲苯等之芳香族烴類;丙酸甲酯 、丙酸乙酯、丙酸丁酯、丁酸甲酯、丁酸乙酯、丁酸丁酯 、戊酸甲酯、戊酸乙酯、戊酸丁酯、己酸甲酯、己酸乙酯 、己酸丁酯、乙酸2-乙基己酯、丁酸2-乙基己酯等之酯類 ;甲基溶纖劑、乙基溶纖劑、丁基溶纖劑、α -松油醇'丁 基溶纖劑乙酸酯、丁基卡必醇乙酸酯等。此等有機溶劑可 單獨使用或倂用2種以上。有機溶劑相對於本發明之陶瓷 胚片用漿料組成物的全體量之含量的上限爲80質量%,下 限爲20質量%。位於上述範圍內時,可將適度的捏揉性賦 予至本發明之陶瓷胚片用漿料組成物。當多於80質量%時 ,黏度變得過低,使陶瓷胚片成形時的處理性變差,少於 2 0質量%時,陶瓷胚片用漿料組成物的黏度變得過高,捏 揉性有降低之傾向。 陶瓷胚片用漿料組成物,在不損及本發明的效果之範 圍內,可含有丙烯酸樹脂、纖維素系樹脂等之黏合劑樹脂 、可塑劑、潤滑劑、分散劑、防帶電劑、抗氧化劑等之以 往所知的添加劑。 本發明之陶瓷胚片用漿料組成物,可因應必要添加可 塑劑。所添加之可塑劑的種類並無特別限定,例如可列舉 出鄰苯二甲酸二辛酯、鄰苯二甲酸苯甲基丁酯、鄰苯二甲 酸二丁酯、鄰苯二甲酸二己酯、鄰苯二甲酸二(2-乙基己 基)酯CDOP)、鄰苯二甲酸二(2-乙基丁基)酯等之鄰 苯二甲酸系可塑劑;己二酸二己酯、己二酸二(2_乙基己 基)酯(DO A )等之己二酸系可塑劑;乙二醇、二乙二醇 201144254 、三乙二醇等之二醇系可塑劑;三乙二醇二丁酯、三乙二 醇二(2-乙基丁酯)、三乙二醇二(2-乙基己酯)等之二 醇酯系可塑劑等,此等亦可組合2種以上使用。可塑劑的 使用量並無特別限定,相對於本發明之陶瓷胚片用漿料組 成物的全體量,較佳爲使用〇_1〜10質量%,尤佳爲1~8質量 %。當中就揮發性低且容易保持薄片的柔軟性來看,較佳 爲DOP、DOA、三乙二醇2-乙基己酯。 製造出本發明之使用聚乙烯縮醛樹脂之陶瓷胚片用漿 料組成物的方法並無特別限定,例如可列舉出使用球磨機 、摻合機、三軋輥機等之各種混合機,將含有上述聚乙烯 縮醛樹脂之黏合劑樹脂、陶瓷粉末、有機溶劑、及因應必 要所添加之各種添加劑予以混合之方法。 本發明之陶瓷胚片用漿料組成物,由於具有上述構成 ,即使厚度爲2μ1Ώ以下,亦可製造出具有充分的機械強度 之薄膜陶瓷胚片。如此,使用本發明之陶瓷胚片用漿料組 成物所製得之陶瓷胚片且爲厚度2μιη以下之陶瓷胚片,亦 爲本發明之一。 本發明之陶瓷胚片的製造方法並無特別限定,可藉由 以往所知的製造方法製造,例如可列舉出以流體鑄膜法將 本發明之陶瓷胚片用漿料組成物成形於聚對苯二甲酸乙二 酯等之剝離性支撐體上,並藉由加熱等來餾除溶劑等後, 從支撐體中剝離之方法。 可藉由將塗佈有導電膏之薄層層合於本發明之陶瓷胚 片,而製作出層合陶瓷電容器。如此,使用本發明之陶瓷 -15- 201144254 胚片與導電膏所製得之層合陶瓷電容器,亦爲本發明之一 〇 本發明之層合陶瓷電容器的製造方法並無特別限定, 可藉由以往所知的製造方法製造,例如可列舉出交互地重 疊複數片之藉由網版印刷等在本發明之陶瓷胚片的表面形 成有成爲內部電極之導電裔而成者,並進行加熱壓著而得 層合體,然後在進行以熱分解來去除該層合體中所包含之 黏合劑成分等之處理(脫脂處理)後,進行燒結而得陶瓷 燒結物,並將外部電極燒結於該陶瓷燒結物的端面之方法 等。 此外,上述導電臂的製造方法並無特別限定,可藉由 以往所知的製造方法製造,例如可列舉出將金屬等之導電 性粉末、分散劑、可塑劑、溶劑等混合於聚乙烯縮醛樹脂 之方法等。 以下係列舉出實施例來更詳細地說明本發明,但本發 明並不限定於此等實施例。以下的實施例中,「%」及「 份」在無特別說明時,係意味著「質量%」及「質量份」 〇 聚乙烯縮醛樹脂及抗氧化劑之諸項特性的測定,係依 循下列方法來進行。 (聚乙烯縮醛樹脂的乙烯酯單位含量) 根據JIs K672 8所記載的方法來測定。 (聚乙烯縮醛樹脂的乙烯醇單位含量) 根據JIS K67 28所記載的方法來測定》 -16- 201144254 實施例 (實施例1 ) (聚乙烯縮醛樹脂的調製) 將離子交換水1295g、聚乙烯醇(PVA-1 :聚合度1050 、鹼化度99.2莫耳% ) 105g裝入於具備回流冷卻器、溫度 計及錨型攪拌翼之內容積2公升的玻璃製容器,將全體升 溫至98 °C使聚乙烯醇完全溶解,而形成聚乙烯醇水溶液( 濃度7.5質量% )。將所形成之聚乙烯醇水溶液,一邊以轉 速120rpm持續攪拌並在約30分鐘間逐漸冷卻至5°C後,將 丁醛70g以及作爲丁醛化觸媒的酸觸媒之濃度20質量%的鹽 酸100ml添加於該水溶液中,開始聚乙烯醇的丁醛化。進 行3 0分鐘的丁醛化後,在120分鐘間將全體升溫至70 °C, 並在70 °C下保持180分鐘後,冷卻至室溫。將藉由冷卻所 析出之樹脂過濾後,以離子交換水(相對於樹脂爲1 00倍 量之離子交換水)洗淨複數次,爲了中和而加入0.3質量% 的氫氧化鈉溶液,在70°C下保持5小時後,進行離心脫水 ’再以100倍量的離子交換水洗淨複數次,脫水後,在40 °C、減壓下進行1 8小時的乾燥,而得聚乙烯丁醛樹脂( PVB-1 )。所得之聚乙烯丁醛樹脂(pvB-丨),丁醛化度 爲7 1.0莫耳%,乙烯酯單位的含量爲0.8莫耳%,乙烯醇單 位的含量爲2 8.2莫耳%。 將所得之聚乙烯丁醛樹脂10質量份加入於甲苯20質量 份與乙醇20質量份之混合溶劑中,進行攪拌溶解,加入作 -17- 201144254 爲可塑劑之DOP8質量份,進行攪拌溶解。將作爲陶瓷粉 末之鈦酸鋇(堺化學工業公司製,BT-03(平均粒徑〇.3μιη) )1〇〇質量份加入於所得之樹脂溶液,以球磨機混合48小 時’而製得陶瓷胚片用漿料組成物。 (實施例2 ) 除了使用聚乙烯醇(PVA-2 :聚合度1 700、鹼化度 9 9.6莫耳% )來取代pvA-l之外,其他與實施例!相同而製 得聚乙烯丁醛樹脂(1^8-2)。?乂8-2的丁醛化度爲69.8莫 耳%’乙稀酯單位的含量爲〇.4莫耳%,乙烯醇單位的含量 爲2 9.8莫耳%。接著與實施例1相同地製得陶瓷胚片用漿料 組成物。 (實施例3 ) 除了使用聚乙烯醇(PVA-3 :聚合度24〇〇、鹼化度 "•9莫耳%)來取代PVA-1之外’其他與實施例1相同而製 知聚乙烯丁醛樹脂(pVB_3) 〇ρνΒ_3的丁醛化度爲743莫 耳%乙稀醋單位的含量爲〇. 1莫耳%,乙烯醇單位的含量 爲2 5.6莫耳% °接著與實施例1相同地製得陶瓷胚片用漿料 組成物。 (實施例4 ) 除了使用聚乙烯醇(pVA_4:聚合度35〇〇、鹼化度 99’8莫耳% )來取代PVA-1之外,其他與實施例1相同而製 •18- 201144254 得聚乙烯丁醛樹脂(PVB·4)。pvB-4的丁醒化度爲73.2莫 耳%’乙烯酯單位的含量爲〇·2莫耳%,乙烯醇單位的含量 爲2 6.6莫耳%。接著與實施例1相同地製得陶瓷胚片用漿料 組成物。 (實施例5 ) 除了使用聚乙烯醇(PVA-5:聚合度42〇0、鹼化度 99.9莫耳%)來取代pva-〗之外,其他與實施例1相同而製 得聚乙烯丁醛樹脂(PVB-5) 。pvB-5的丁醛化度爲69.0莫 耳%,乙嫌醋單位的含量爲〇.丨莫耳%,乙締醇單位的含量 爲30.9莫耳%。接著,除了添加聚乙烯丁醛樹脂8質量份與 作爲可塑劑之D Ο A 8質量份之外,其他與實施例1相同地製 得陶瓷胚片用漿料組成物。 (實施例6 ) 除了使用聚乙烯醇(PVA-6 :聚合度1*700、鹼化度 99.95莫耳%)來取代pva-1之外,其他與實施例1相同而製 得聚乙烯丁醛樹脂(PVB-6) °pVB-6的丁醛化度爲74_25 莫耳%,乙烯酯單位的含量爲0.05莫耳%,乙烯醇單位的含 量爲25.70莫耳%。接著與實施例1相同地製得陶瓷胚片用 漿料組成物。 (實施例7 ) 除了使用聚乙烯醇(PVA-7 :聚合度1 700、鹼化度 -19- 201144254 99.9莫耳%)來取代PVA-1之外,其他與實施例1相同而製 ί守聚乙嫌丁酸樹脂(ρνΒ·7) .pvb-7的丁醛化度爲80.6莫 耳°/。’乙嫌醋單位的含量爲〇1莫耳%,乙烯醇單位的含量 爲19.3莫耳%。接著與實施例1相同地製得陶瓷胚片用漿料 組成物。 (實施例8 ) 除了使用聚乙烯醇(PVA-8 :聚合度1 700、鹼化度 99_8莫耳% )來取代ρνΑ·1之外,其他與實施例1相同而製 得聚乙稀丁醛樹脂(1>乂84)。?乂8-8的丁醛化度爲65.2莫 耳%’乙稀酯單位的含量爲0.2莫耳%,乙烯醇單位的含量 爲3 4 · 6莫耳%。接著與實施例1相同地製得陶瓷胚片用漿料 組成物。 (比較例1 ) 除了使用聚乙烯醇(PVA-A :聚合度850、鹼化度99.2 莫耳% )來取代PVA- 1之外,其他與實施例1相同而製得聚 乙烯丁醛樹脂(PVB-A) 。PVB-A的丁醛化度爲71_0莫耳% ’乙烯酯單位的含量爲〇.8莫耳%,乙烯醇單位的含量爲 28.2莫耳%。接著與實施例丨相同地製得陶瓷胚片用漿料組 成物。 (比較例2 ) 除了使用聚乙稀醇(PVA-B:聚合度1700、驗化度99 -20- 201144254 莫耳% )來取代pVA-1之外,其他與實施例1相同而製得聚 乙烯丁醛樹脂(PVB_B) 。PVB-B的丁醛化度爲70莫耳% ’乙烯酯單位的含量爲1莫耳%,乙烯醇單位的含量爲29莫 耳% °接著與實施例1相同地製得陶瓷胚片用漿料組成物。 (比較例3 ) 除了使用聚乙烯醇(PVA-C :聚合度3 500、鹼化度 98.5莫耳%)來取代pvA_i之外,其他與實施例1相同而製 得聚乙烯丁醛樹脂(;!^8_(:)。?^-(:的丁醛化度爲71.5 莫耳%’乙烯酯單位的含量爲1.5莫耳%,乙烯醇單位的含 量爲2?莫耳%。接著與實施例1相同地製得陶瓷胚片用漿料 組成物。 (比較例4 ) 除了使用聚乙烯醇(PVA-D :聚合度4800、鹼化度 99.9莫耳% )來取代PVA-1之外,其他與實施例1相同而製 得聚乙烯丁醛樹脂(!^8-0)。?乂8-0的丁醛化度爲71.9 莫耳%’乙烯酯單位的含量爲0.1莫耳%,乙烯醇單位的含 量爲28莫耳%。接著與實施例1相同地製得陶瓷胚片用漿料 組成物’但漿液的黏度高,塗佈性差,而在胚片中觀察到 粒子分散性的不均一。 (比較例5 ) 除了使用聚乙烯醇(PVA-E :聚合度2400、鹼化度 -21 - 201144254 99.9莫耳%)來取代pvA-i,並與丁醛同時添加戊二醛 0.08 g之外’其他與實施例1相同而製得聚乙烯丁醛樹脂( PVB-E) 。PVB-E的丁醛化度爲71.9莫耳%,乙烯酯單位的 含量爲0.1莫耳% ’乙烯醇單位的含量爲28莫耳%。接著與 實施例1相同地製得陶瓷胚片用漿料組成物。 (比較例6 ) 除了使用聚乙烯醇(PVA-F :聚合度1 700、鹼化度 9 9.5莫耳% )來取代p v A -1之外,其他與比較例5相同而製 得聚乙烯丁醛樹脂(PVB-F) "PVB-F的丁醛化度爲71.0莫 耳%’乙烯酯單位的含量爲〇_5莫耳%,乙烯醇單位的含量 爲2 8 _ 5莫耳%。接著與實施例1相同地製得陶瓷胚片用漿料 組成物。 使用塗佈棒,將實施例1〜8及比較例1〜6中所製作之陶 瓷胚片用漿料組成物,以使乾燥厚度成爲2μηι之方式塗佈 在經脫模處理後的聚酯薄膜上,在常溫下進行1小時的風 乾後,以熱風乾燥機在80 °C下進行3小時,接著在120。(:下 進行2小時的乾燥而製得陶瓷胚片。 (評估) (機械強度的評估) 從聚酯薄膜中將所得之陶瓷胚片剝離,觀察陶瓷胚片 的狀態。並以下列2階段進行評估。 〇:陶瓷胚片上未觀察到斷裂或破損 -22- 201144254 X :雖僅有些微但已觀察到斷裂或破損 (胚片評估) 從聚對苯二甲酸乙二酯中,將陶瓷胚片裁切爲6 0mm X 5 0 m m的大小,在2 0 °C下放置3分鐘後,以光學顯微鏡觀測 薄片的側面。並以下列2階段進行評估。 〇:未觀察到陶瓷胚片的翹曲 X:雖僅有些微但已在陶瓷胚片上觀察到翹曲 機械強度的評估與胚片評估之結果如第1表所示。 -23- 201144254 [第1表] 願 O O 0 0 ο 0 〇 〇 0 〇 ο 0 X X 擗 m 锻 m o 〇 0 ο ο ο 〇 0 X X X X 0 ο 趙呂 1 i膜 摧 摧 堞 鹿 壊 摧 鹿 壊 m 壊 壊 m 擗 诹 m s 8 s s 8 s S S s s S 含 g δ •«e ο ΚΙ ?: s J5 ro s S LA <0 P: o P: f= Ρ: m m 躍 s o § o ο ο s o ο ο g o 〇 〇 S 〇 s d 8 s ο ο ο ο S ο 跋 K) a赵? gSi s s s s 芑 o S o o ο ο δ 蔽 s s s s R a 〇> a 〇> CM S3 οό CM οό eg η <π s o o ο o t£? Ο § o s 〇 〇 s o o s Ο 9 1 ο m cvi CO m 1ι -L CM ± CO ± I ΙΑ -1 Ϊ 00 Λ ί Ϊ 2 1 UJ % I l I Έ I έ g 安 〇. I 1 g 1 t 1 m i CSl C9 m 握 寸 10 (0 卜 S 00 i N CD 寸 U) to 闺 握 辑 辑 闺 闺 辑 鎰 鎰 鎰 鑑 鎰 鎰 M 佩 1¾ Μ 卹 IK Μ Μ Μ a 產業上之可利用性: 根據本發明,能夠提供一種可製得具有充分的機械強 -24- 201144254 度且翹曲少之陶瓷胚片之陶瓷胚片用漿料組成物,陶瓷胚 片及層合陶瓷電容器。
Claims (1)
- 201144254 七、申請專利範圍: 1. 一種陶瓷胚片用漿料組成物’其係含有:聚乙燃 縮醛樹脂、陶瓷粉末、及有機溶劑,其中前述聚乙烯縮醛 樹脂係將聚合度超過1 〇〇〇且爲45 00以下、乙烯酯單位的含 量小於1莫耳%之聚乙烯醇樹脂以單醛進行縮醛化而得’且 縮酸化度爲6 0〜8 3莫耳% * 2 ·—種陶瓷胚片,爲使用如申請專利範圍第1項之陶 瓷胚片用漿料組成物而得之陶瓷胚片,其特徵爲: 厚度爲2μιη以下。 3· —種層合陶瓷電容器,其特徵爲: 使用如申請專利範圍第2項之陶瓷胚片與導電膏而得 -26- 201144254 四 指定代表圖: (一) 本案指定代表圖為:無 (二) 本代表圖之元件代表符號簡單說明:無 201144254 五 本案若有化學式時,請揭示最能顯示發明特徵的化學 式·無
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JP2010014011 | 2010-01-26 |
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TW099145524A TW201144254A (en) | 2010-01-26 | 2010-12-23 | Slurry composition for ceramic green sheet, ceramic green sheet, and multilayer ceramic capacitor |
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JP (1) | JP5702311B2 (zh) |
KR (1) | KR101780839B1 (zh) |
CN (1) | CN102822117A (zh) |
TW (1) | TW201144254A (zh) |
WO (1) | WO2011092963A1 (zh) |
Cited By (1)
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TWI496852B (zh) * | 2012-12-26 | 2015-08-21 | Murata Manufacturing Co | Ceramic embryo chip and its manufacturing method |
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WO2011102197A1 (ja) * | 2010-02-16 | 2011-08-25 | 株式会社クラレ | セラミックグリーンシート用ポリビニルアセタール樹脂、およびその製造方法、スラリー組成物、セラミックグリーンシート及び積層セラミックコンデンサ |
TWI557096B (zh) * | 2011-09-28 | 2016-11-11 | 可樂麗股份有限公司 | 漿料組成物、陶瓷坯片及積層陶瓷電容器 |
EP3109263A4 (en) * | 2014-02-17 | 2018-02-14 | Kuraray Co., Ltd. | Binder for formation of ceramic or for use in conductive paste, and use of same |
EP3327730A4 (en) * | 2015-07-22 | 2019-04-03 | Shoei Chemical Inc. | BINDER RESIN FOR PASTES CONTAINING DISPERSED INORGANIC PARTICLES AND PASTE CONTAINING DISPERSIBLE INORGANIC PARTICLES |
KR20190038864A (ko) * | 2016-07-28 | 2019-04-09 | 주식회사 쿠라레 | 세라믹 그린 시트 및 도포 시트 |
CN113227246B (zh) * | 2018-12-25 | 2023-09-12 | 住友金属矿山株式会社 | 导电性浆料、电子部件以及叠层陶瓷电容器 |
KR20210118408A (ko) * | 2019-01-29 | 2021-09-30 | 카오카부시키가이샤 | 세라믹 성형체로부터의 유기물 성분의 제거 방법 |
TW202102554A (zh) | 2019-03-29 | 2021-01-16 | 日商積水化學工業股份有限公司 | 陶瓷生片用樹脂組成物、陶瓷生片及積層陶瓷電容器 |
CN112028625A (zh) * | 2020-07-31 | 2020-12-04 | 深圳陶陶科技有限公司 | 氧化锆陶瓷材料及其制备方法和用途 |
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JP3279392B2 (ja) * | 1993-06-17 | 2002-04-30 | 積水化学工業株式会社 | グリーンシート成形用セラミック泥漿物及びグリーンシート |
DE60302504T2 (de) * | 2002-07-23 | 2006-07-06 | KURARAY CO., LTD, Kurashiki | Polyvinylacetal und dessen Verwendung |
EP1447416B1 (en) * | 2003-01-23 | 2010-03-03 | Kuraray Co., Ltd. | Polyvinyl acetal and its use |
JP4870919B2 (ja) * | 2004-09-27 | 2012-02-08 | 積水化学工業株式会社 | セラミックグリーンシート用スラリー組成物、セラミックグリーンシート及び積層セラミックコンデンサ |
JP4829518B2 (ja) * | 2005-04-05 | 2011-12-07 | 積水化学工業株式会社 | セラミックグリーンシート用セラミックペースト |
EP2006308B1 (en) * | 2006-04-05 | 2010-09-01 | The Nippon Synthetic Chemical Industry Co., Ltd. | Polyvinyl acetal-based resin |
JP2008133371A (ja) * | 2006-11-28 | 2008-06-12 | Sekisui Chem Co Ltd | ポリビニルアセタール樹脂及びセラミックグリーンシート |
-
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- 2010-12-15 KR KR1020127021222A patent/KR101780839B1/ko active IP Right Grant
- 2010-12-15 CN CN2010800625116A patent/CN102822117A/zh active Pending
- 2010-12-15 WO PCT/JP2010/072563 patent/WO2011092963A1/ja active Application Filing
- 2010-12-15 JP JP2011551705A patent/JP5702311B2/ja active Active
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TWI496852B (zh) * | 2012-12-26 | 2015-08-21 | Murata Manufacturing Co | Ceramic embryo chip and its manufacturing method |
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JP5702311B2 (ja) | 2015-04-15 |
JPWO2011092963A1 (ja) | 2013-05-30 |
KR20120127596A (ko) | 2012-11-22 |
CN102822117A (zh) | 2012-12-12 |
WO2011092963A1 (ja) | 2011-08-04 |
KR101780839B1 (ko) | 2017-09-21 |
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