TW563141B - High dielectric constant very low fired X7R ceramic capacitor, and powder for making - Google Patents

High dielectric constant very low fired X7R ceramic capacitor, and powder for making Download PDF

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Publication number
TW563141B
TW563141B TW091125273A TW91125273A TW563141B TW 563141 B TW563141 B TW 563141B TW 091125273 A TW091125273 A TW 091125273A TW 91125273 A TW91125273 A TW 91125273A TW 563141 B TW563141 B TW 563141B
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Galeb H Maher
Samir Maher
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Mra Lab Inc
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Description

563141 A7 B7 五、發明説明（1 ) 發明領域 本發明有關多層陶瓷電容器及用於製造該電容器之經 調配陶瓷粉末，其中該電容器節合電子工業協會（the Electronic Industrial Association ( “E.I.A”））之 X7R 性 能特徵，特別是有關一經調配陶瓷粉末，由彼可製造一介 電陶瓷體，其可於]，〇2 5 °C或以下燒結，而得以使用具有85 重量百分比或以上銀組成之高銀含量銀鈀合金電極。 先前技藝 有關製造低度燒製、高介電常數、X7R多層陶瓷電容 器及用於製造該電容器之經調配陶瓷粉末的硏究結果已廣 爲人知。例如，使介電體在約1，】00 °C下燒製或燒結之後， 充分具有標準X7R性能特徵與高介電常數之介電陶瓷組成 物揭不於本發明人之一G a 1 e b M a h e r的多篇專利當中。此等 專利包括Maher於I 991年4月23日申請之美國專利 5,0]0,443、Maher於]993年Π月2日申請之美國專利 5,258,338以及Maher等人於2000年3月28日申請之美國 專利6,0 4 3，] 74，此等專利全文係以提及的方式倂入本文中 ’而且其係S襄受予亦爲本文所揭示且主張權利之本發明所 有權之讓受人。 在M a h e r等人申請的美國專利6，0 4 3，] 7 4中，描述具有 高度接可受性之X7R調配陶瓷粉末混合物可於低至1，] 2〇 C之溫度調配之後燒結，得以使用由7 0 %銀與3 0 %鈀所組 成之電極。揭示於6, 〇 4 3 5〗74專利中之該種陶瓷粉末混合物 本紙張尺度適用中國國家標準（CNS ) Α4Ι^Γ( 2】0>( 297公楚) — --- (請先閲讀背面之注意事項再填寫本頁) C- 、11 經濟部智慧財產局员工消赀合作社印製 563141 A7 B7 五、發明説明（2 ) (請先M讀背面之注意事項再填寫本頁) 包括至少九十重量百分比（重量％)純鈦酸鋇粉末，其平均 粒徑自0.4至0.7微米，由0.] 5至2.5重量％矽酸鎘粉末助 熔劑、少量顆粒生長抑制劑化合物，諸如相對於鈦酸鋇數 量自0.89至2.7 2莫耳百分比之Nb203，以及約0.2至1.0 莫耳百分比鈣陽離子。目前本產業中製造並銷售由此種組 成物製得之多層陶瓷電容器，以及根據美國專利6,043,1 74 揭示所製得之經調配陶瓷粉末，其係由本案讓受人一 MRA Laboratories，Inc·，of Adams，MA，U.S.A.所銷售。 經濟部智¾財產g(工消费合作社印製 此等陶瓷粉末與由此等粉末所製得之多層陶瓷電容器 已達到高性能特徵，同時減少電極內之鈀數量。如眾所周 知’鈀的成本高使得必須減少銀鈀合金電極中之鈀數量， 並增加銀用量。藉由降低將陶瓷粉末自粉末轉變成黏結固 體或是成熟體而且不熔融該粉末之燒結溫度，可以增加銀 鈀電極中之銀的相對數量，同時減少鈀之數量。如前文所 述’ 6,〇43，]74專利中所揭示之陶瓷粉末可在介於]3]2〇°C 至]，]5 0 °C之溫度下燒結，如此電極中之鈀數量可以降低3 0 個百分比。已知本技術中，該陶瓷粉末的燒結溫度必須低 於該銀鈀電極的熔融溫度。另外，當該電極中之銀比例增 加時，該電極中之鈀比例降低，該電極的熔融溫度亦降低 。因此，藉由降低該陶瓷粉末的燒結溫度，可以使用較高 比例銀與較低比例鈀製造電極，因鈀的成本明顯高於銀的 成本，故可以明顯地節約成本。 前述專利亦揭示本案人對於降低成本及加強多層電容 器用之經調配陶瓷粉末的性能特徵之進一步硏究成果。例 本紙張尺度適用中國國家標準（CNS ) Λ4規格（2]0X 297公釐) ~ 563141 A7 B7 五、發明説明（3 ) (請先閱讀背面之注意事項再填寫本頁) 如，美國專利6, (M3 5] 74亦揭示藉由在起始粉末中添加極少 而且臨界量之鈣化合物，諸如碳酸鈣或鈮酸鈣，可以省略 成本高昂的退火步驟，同時加速使用期限試驗中仍維持高 絕緣電阻，僅有介電常數略微降低。 雖然習知陶瓷粉末以及由該粉末製得之多層電容器顯 示出經改良性能，但是現有的粉末仍然受到明顯限制。例 如，已知該粉末中使用諸如CdO、PbO與Bi2 03等重金屬氧 化物作爲助熔劑。多層電容器中使用矽酸鎘助熔劑的優點 最早揭示由本案發明人之一 Gal eb Maher於]981年5月5 日所申請的美國專利4,26 6,2 65中。不過，諸如氧化鎘等重 金屬化合物已逐漸被視爲危險材料，因此其會造成與使用 包括鎘或其他危險重金屬氧化物之電容器的組件之使用及 廢棄相關重要成本問題。因此，如前述專利所揭示，燒結 包括矽酸鎘助熔劑的陶瓷粉末時，必須使用密閉式坩堝以 包容所有毒性鎘煙霧，以免污染在該坩堝附近的工作人員 〇 經濟部智¾¾產局負工消赀合作社印製 因此，需要一種多層陶瓷電容器以及不包括危險重金 屬氧化物，而且降低習知電容器成本之供製造該電容器用 的粉末。 發明內容 本發明包括一種介電陶瓷粉末混合物，其包括至少九 十重量百分比實質上純鈦酸鋇粉末，平均粒徑自0.2至].2 微米；自0.2至2.5重量百分比硼矽酸鋇鋰（“BLBS”）助 -6 - 本紙张尺度適用中國國家標準（CNS ) A4規格（2】OX297公漦） 563141 A7 五、發明説明（4 ) 熔劑；自〇.]至0.3重量百分比之]VhiC03 ;顆粒生長抑制齊lj (請先閱讀背面之注意事項再填寫本頁) ，諸如氧化鈮或鈮酸鹽化合物，如此於該粉末混合物中添 加氧化鈮或鈮酸鹽化合物時，產生〇 . 4至].5 0重量百分比 之Nb205 ;以及0.4至].2重量百分比之Gd203。 由於徹底硏究與實驗的結果，本案發明人發現意外產 生之釓的稀土金屬氧化物，而且極佳地形成細微顆粒結構 ;以及發現倂用Nb205或鈮酸鹽化合物作爲顆粒生長抑制 劑時，製得本技術中需要之核心外殼結構，其於95 0°C之低 溫燒製或燒結之後顯示出優良X7R性能特徵。 經濟部智悲財產局貨工消費合作社印焚 本發明另一實施樣態包括一種製造較佳介電陶瓷粉末 之方法，其包括製備上述所需要之起始粉末混合物，包括 0.4至].2重量百分比Gd2〇3 ;於約450°C至約5 5 0°C溫和地 煅燒該起始粉末混合物，製得由起始粉末之混合物的黏聚 物所組成的粉末，其中每個黏聚物具有與鈦酸鋇、硼矽酸 鋇鋰、N b 2 Ο 5、Μ n C Ο 3與氧化物釓（G d 2 0 3 )之起始粉末實 質上相同組成比率；以便提供可於開放式氧化錐耐火架子 中，以95〇°C至】，〇25°C燒結之粉末狀混合物，製造燒結密 度大於5.75 g/cm3、介電常數（“K”）大於2,500，且電容 器溫度係數（“tcc”）平順之介電陶瓷體，其中相對於25 °C溫度之K値，在dVC至]ht：溫度範圔內之κ値在 + / - ] 5 % 內。 本發明另一實施樣態包括一種製造符合X7R性能特徵 之多層陶瓷電容器體的方法，包括將包括〇 4至]2重量百 分比Gd2〇3之上述經煅燒起始粉末混合物分散於一種黏合 本紙张尺度適用中國國家標準（CNS ) A4規格（210X29^ ) 563141 Α7 _ Β7 五、發明说明（5 ) (請先閱讀背面之注意事項再填寫本頁) 齊Γ溶齊卜黏合劑系統中，形成該粉末混合物之淤漿；製備該 淤漿層；乾燥此等層；形成數層之堆疊體，並將銀鈀電極 墨水的經佈線膜插入次一對相鄰層之間；然後藉由在開放 空氣中’以95 0°C至]，〇2 5 t間之溫度下燒結3至5小時， 加熱使此等層之堆疊體完成，製造具有埋入式電極之緻密 陶瓷電容器體。 由此方法製得之多層陶瓷電容器證實K値大於2,500 與平順電容溫度係數（“TCC”）之前述較佳X7R性能特徵 ，其中K値於-5 5 °C至1 2 5 °C之間時在+/-】5 %內，散逸係數 (“DF”）小於2.5百分比，而125 °C下之絕緣電阻大於1〇〇 歐姆·法拉’在高溫與高電壓下之使用期限試驗期間，具有 長時間安定性。 經濟部智慈財產局貨工消骨合作社卬 因此’本發明目的係提供一種非常低度燒製、高介電 常數陶瓷電容器，以及用以製造該電容器之粉末，該粉末 包括一種氧化添加劑，而且不包括重金屬氧化物。所形 成粉末與陶瓷電容器具有平順X7R性能特徵，可於950 = 至]，02 5 °C之溫度燒製或燒結，而且不包括危險性廢棄產物 ’因而使製造與廢棄物處理成本最小化，同時得以使用銀 含量超過8 5百分比之高銀含量銀鈀電極。. ^ δ羊閱以下說明與附圖，將更明白本發明此等與其他目 的與優點。 圖式簡要說明 圖】係根據本發明構成之多層陶瓷電容器的橫剖面圖 本紙張尺度剌巾關家標準（CNS ) Α4規格（2)(}>< 297公發） -8- 563141 A7 B7 五、發明説明（7) 瓷粉末調配物的硏究性能資料。 圖12(包括圖12-1及12-2)係表9,顯示在95(TC下燒製 3小時之實施例92-97陶瓷粉末調配物的硏究性能資料。 圖13(包括圖13— 1及13— 2)係表10，顯示實施例98-99之具有85%銀-15%鈀內部電極之多層陶瓷電容器結構在 不同溫度下燒製3小時之硏究性能資料。 圖14(包括圖14— 1及14 一 2)係表11，顯示實施例 100-101之具有85%銀-15%鈀內部電極之多層陶瓷電容器結 構在不同溫度下燒製3小時之硏究性能資料。 圖15(包括圖15-1、15-2、15-3及15-4)係表12，顯示 實施例1 02- 1 05之具有85%銀-15%鈀內部電極之多層陶瓷 電容器結構在不同溫度下燒製3小時之硏究性能資料。 圖16(包括圖16— 1及16-2)係表13，顯示實施例 1 0 6- 1 07之具有85 %銀-15%鈀內部電極之多層陶瓷電容器結 構在不同溫度下燒製3小時之硏究性能資料。 圖17(包括圖17-1及17— 2)係表14，顯示在95(rc下 燒製實施例1 08-1 1 0陶瓷粉末調配物之硏究性能資料。 圖18係表15，顯示實施例111之具有7 0%銀-3 0%鈀 內部電極之多層陶瓷電容器結構在l，〇〇〇t下燒製3小時之 硏究性能資料。 主要元件對照表 10 電容器 12 陶瓷體 14 電極 16 電極 18 外部終端 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐〉 _ 1〇 - (請先閲讀背面之注意事項再填寫本頁) 衣. 訂 經濟部智慧財產局8工消費合作社印製 563141 A7 B7 經濟部智慧財產苟8工消費合作社印製 五、發明説明（8 ) 實施方式 此此將說明由廣泛實驗所形成之陶瓷粉末混合物的較 佳具體實施例。以實驗單層結構形式試驗至少9 7個實施例 ，發展該較佳陶瓷粉末調配物。表1至9 (圖3 - ] 2 )中列 出實施例1至97的性能資料。然後，將較佳陶瓷粉末調配 物用於實施例98- 1 07之多層陶瓷電容器，而且實施例之性 ㉟資料係顯不於表10-12(圖13_16)。圖1中顯示多層陶 瓷電容器，而且通常以參考數字10表示。電容器10包括 一陶瓷體1 2、埋在陶瓷體1 2內之第一組電極I 4、埋在該 陶瓷體1 2內，與第一組電極1 4具有電容關係之第二組電 極1 6、與第一組電極1 4連接之第一外部終端1 8，以及與 第二組電極I 6連接之第二外部電極。製備5 0克一批之下 文與表1至9 (圖3-]2 )所述陶瓷調配物、使用200 cc塑 膠罐與500克經氧化釔安定之氧化鉻碾磨介質，製得實施 例]至97之單層結構電容器。將約20克之有機黏合劑/溶 劑分散劑溶液添加於該罐中，然後球磨碾磨約]2小時。然 後’將該淤漿澆鑄在一紙板上，以乾燥該溶劑。將乾燥餅 狀物粒化，並以]5,000 PSI壓製成九狀。然後，在一氧化 鉻耐火架子上燒結該九狀物。該單層結構的經燒製尺寸係 直徑約1 cm，厚度0· 1 cm。使用阿基米德原理測量經燒製 密度之後，在該圓盤物的正反面塗覆銀墨水，形成具有電 容關係之電極。然後，以約7 5 0°C燒製該結構]0分鐘。然 後，在25°C下以]KHz、] Vms陳化24小時之後，測量其 電性質。 (請先閲讀背面之注意事項再填寫本頁) 訂 f 本紙張尺度適用中國國家標準（CNS ) A4規格（2】0X 297公釐） -11- ^14!
<、發明説明（9) 所有單層結構實例（實施例]-97)之起始粉末混合物 保至少九十重量百分比實質上純鈦酸鋇粉末（BaTi03 )， 其平均粒徑自0.2至].2微米（大部分實例包括介於ο.' 〇·9微米之BaTi03)、自0.2至2.5重量百分比之硼矽酸鋇 _，以及自〇.〗至0.3重量百分比之MnC03。 該硼矽酸鋇鋰（“BLBS”）之較佳組成係描述於本案發 明人之共待審美國專利申請案中，其係以（3Ba0.]B2 03 ) + ( Ba0.B203 )相之獨特組成爲基礎，當以約1:1比率混 合時，獲得低共熔混合物之熔融溫度約972 °C。（該共待審 獒國專利申請案係申請案序號第〇9/65 2,562，於08/31/00 所申請，該案全文係以提及的方式倂入本文中）。當此比 率進一步與矽酸鋰Li4 Si 04混合時，熔融溫度更降至75 〇t 以下。較佳組成物係由（〇·5ιτι之Ba0.B2 03 + 〇.5ηι之 3Ba0.B203 + ]m之Li4，Si04)組成，或以氧化物之莫耳比 形式表示；2BaO，]B2〇3，2Li205 ]Si02。 BLB S助熔劑添力ϋ齊[|之影響 如圖3所示，表1提供實施例]至7之性能資料。表] 說明具有不同量BLB S助熔劑燒結助劑之單層裝置。由此 資料可以看出，將細微顆粒BaTi03之燒結溫度降至950°C 僅需要添加]重量％BLBS，燒製密度超過理論値的96%。 當此種組成物不具有該添加劑時，則需要1 25 0 °C以上以達 到相同密度，此時其效果極爲明顯。雖然該燒製顆粒相當 小（例如，小於]微米），但是該電容器溫度係數（“TCC” (請先閱讀背面之注意事項再填寫本頁)
、1T 經濟部智怂財產局肖工消費合作社印製 尺度適用中國國家標準(TcNS ) A4規格（2]0X 297公t ) ~ 一 563141 A7 B7 五、發明説明（1C)) )不符合+Λ ]5% X7R規格。顯示出最佳BLBS水準在2.0 重量％左右。 (請先閱讀背面之注意寧項再填寫本頁) 稀土金屬氧化物之影響（effect ) 藉由形成核心外殼結構使T C C曲線平順之嘗試當中， 已試驗過各種稀土金屬氧化物。表2 (圖4)中所記錄之實 施例8至1 3性能資料顯示出在2重量％BLB S時，添加 Nd2〇3之影響。添加Nd203，會藉由與BaTi03形成固溶體 ’並造成居里溫度向下平移，使燒製密度提高至接近理論 値。高於2.0°/。時，該顆粒會變細，但是TCC仍然在 + /-]5%限制以外。高於2.5%，如實施例]3、]4所示，該 樣本呈孔狀，緻密度低。
Gd203之影響 經濟部智慈財產局員工消费合作社印災 如表3 (圖5 )所示，氧化釓（Gd203 )與大部分稀土 金屬氧化物不同，其獨特之處係可以產生範圍廣泛的添加 劑細微顆粒結構。實施例]5至]9顯示此種添加之效果。 如圖2所示，其他稀土金屬氧化物具有較大離子半徑，而 具有小離子半徑者不如氧化釓般有效。其顯示出約0. S重量 %接近最佳値，但是其TCC仍在X7R限制以外。
Nb205添力口之影響 表4 (圖6 )中，硏究在BaTi03中添加Nb205。已知將 Nb205添加於BaTi03中會產生核心外殼結構，並且獲得平 -13- 本紙ί長尺度適用中國國家標準（CNS ) A4規格（2】OX 297公釐） 563141 A7 _B7 五、發明説明（11 ) (#先閱讀背面之注意寧項再填寫本頁) 順電容溫度係數。實施例（20-24)顯示出Nb205對於包含 約 97 重量 ％ BaTi03、0.8 重量。/〇Gd203、2 重量 °/〇BLBS 助熔 劑與〇. 1 MnC03之組成物的影響。少量（例如，少於0.6重 量％ Nb205時），燒製密度非常低（例如，低於5.5 g/cm3 )，且超常顆粒生長超過]〇微米。於0.8重量％時，密度 會提高至大於理論値的9S%，不過有若干固溶體之痕跡。 於1重量。/〇 Nb205時（實施例24 )，達到高密度與平順 TCC。其亦適用於以高達1 .5重量％ Nb2 05之進行其他試驗 。亦可使用諸如 BaNb206、CaNb206、MgNb206 或 LiNb2〇6 等鈮酸鹽化合物所進行之其他試驗，此等鈮酸鹽化合物數 量可以產生相當於該陶瓷粉末混合物總重量之0.4重量％至 ]·5 重量 ％的 Nb2 05。 經濟部^¾財產工消费合作社印製 另外，對於熟悉本技術之技術人士而言，已習知Ta205 (五氧化鉅）或鉅化合物的表現與N b 2 〇 5相似，而且使用 與Nb2〇5相同莫耳基礎時產生相似結果◊前述〇.4重量％至 ].5重量。/〇範圍之N b2 0 $吴耳當量的T a 2 Ο 5或鉅化合物相同 莫耳比例係Ta2〇5之重量百分比，自0.66重量％至2.50重 量％。因此，就此處目的而言，較佳顆粒生長顆粒生長抑制 劑係指選自鈮化合物 Nb205 ' BaNb206、（：aNb206、 M g N b 2 Ο 6、L i N b Ο 3或其混合物，其使N b 2 〇 5之重量百分比 自Ο.4重量％至].50重量％ :或是鉅化合物或其混合物，其 使Ta2〇5之重量百分比自〇·66重量。/〇至2.50重量。/。；或鈮 與鉅化合物之莫耳當量混合物。顆粒生長抑制劑之「重量 百分比」係指相對於添加該顆粒生長抑制劑之整體混合物 木紙張尺度適用中國國家標準（CNS ) A4規格（210X297公漦） -14- 563141 A7 ____ B7__ 五、發明説明（12 ) 重量的重量百分比。 均在975 °C下燒結之具有2重量°/〇BLBS助熔劑、：I % Nb205 、0.1%MnC〇3與0.2重量％(6&〇.]32〇3)之各種稀土金屬氧 化物添加劑的影響 表5 (圖7、8 )中，一組實施例（25-62 )淸楚地顯示 出Gd203與具有較小與較大離子半徑之其他稀土金屬氧化 物比較時之意外獨特特質。實施例27的組成同樣是〇.8重 量％ Gd203，其顯示出最高密度、低散逸係數（“D.F.”）， 而且TCC在+Λ I5%內。圖2圖示說明在975 °C燒製之後， 此等不同添加劑對於密度的影響。由圖2與表5的性能資 料清楚地看出’氧化釓與其他稀土金屬氧化物不同，其提 供實質上經改良性能，因此產生意料外之有價値結果。 添力[]W03與Mo03之影響 表6 (圖9 )顯示出，實施例63-70中添加少量W03 ( 例如，少於1重量％)亦會影響該固溶體與該系統之顆粒生 長。實施例6 3 W 6顯示此添加作用對於電性質的影響。添 力口 〇 · 2至0.6重量％時，可達到相當高密度、細微顆粒以及 平順TCC，但是介電常數（“K”）稍微下降。添加相當莫耳 部分之Mo03可提供幾乎相同結果，如實施例67· 70所示。 添加Mg2Ti04與V205之影響 表7 (圖]〇 )顯示添加少量MgsTi〇4 (例如，少於〇.2 尺度適用中國國家標準（CNS) A4規格（210X 297公釐) "~~~ (請先閱讀背面之注意事項再填寫本頁)
563141 A7 B7 五、發明説明（13) (請先閱讀背面之注意事項再填寫本頁) 重量％ )亦對於燒製密度與電性質有重大正面影響。實施例 7]-74顯示高於〇.]%之密度與K値降得非常迅速。實施例 7 5 - 7 7亦顯示添加少量V 2 0 5 (例如，少於0,2重量％ )提供 非常平順T C C，但是K値降低。 添加（BLBS)對於燒製溫度與電性質之影響 表8 (圖]1)中，使用最佳添加量1.0重量％Nb205、 0.8重量％Gd203與0.1 MnC03，並檢測BLBS含量在].25 與2.5重量％之間變動的影響。實施例78-9]顯示是爲900 °C、95 0 °C與97 5 °C燒製溫度之函數的性質。不過，必須注 意的是，此組結果與前述實施例略有不同，尤其是其組成 具有2重量％助熔劑（實施例8 ]與8 7 )。此一差異的原因 是BaTi03種類所致。此組當中，BaTi03之粒徑約爲0.4微 米，而前述實施例所使用之BaTi03爲0.7至0.9微米。 其他添加劑之影響 經濟部智^对產局8工消費合作社印％ 表9 (圖]2 )顯示其他添加劑的影響，已檢查不存在 Nb205時，此等添加劑對於核心外殻結構之效用。實施例 92-94顯示出Zr02之影響，而實施例95-97顯示出Sb203 之影響。在此二實例下，觀察到顆粒生長與明顯的固溶體 。因此，可以歸納出Nb2 0 5是優良顆粒生長抑制劑的結論 多層陶瓷電容器（“MLCC”）之實例 -16 - 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） 563141 A7 B7_ 五、發明説明（14) 前述實施例]-97中之單層樣本足以界定本發明之較佳 組成範圍。例如，實施例24 (表4-圖6 ) 、27 ' 28 ' 29 ( (請先閲讀背面之注意事項再填寫本頁} 表 5-圖 7)與 64、65、66、67、68、69(表 6-圖 9)顯示 在非常低度燒製或燒結陶瓷粉末中，介電常數大於2500且 具有特別的X7R性能特徵。 然後使用上述介電陶瓷粉末之經驗證較佳組成範圍製 造多層陶瓷電容器實例，以顯示該介電粉末在具有高銀含 量銀鈀（“Ag/Pd”）電極系統之MLCC型結構中的物理與電 性質。大部分情況中，該MLCC係由]0至20層交錯之介 電膜與Ag/Pd電極所組成。該Ag/Pd之組成可自〇%鈀至最 高達20鈀，其餘部分爲銀。該電容電極內之介電質的經燒 製層厚度介於]5與30微米之間。於25t陳化24小時之後 ，在]KHz、] Vrms下測量容器與散逸係數（DF )。其他 電性質諸如T C C、絕緣擊穿電壓、於1 2 5 °C之絕緣電阻以及 於加速溫度與電壓下之使用期限試驗亦描述於表]0- ] 3 (圖 ]3-16 ) ° 經濟部智认？w/i^s(工消赀合作社印製 表1 0中之實施例9 S提供具有3層2 5微米主動層以及 由85重量°/〇Ag/】5重量(3/〇^(1系統所組成之內部電極的多層 陶瓷電容器結構（3. Ox 2.5 mm)之資料。於97 5 t：燒製此 等MLCC時，達到良好K値、D.F.與TCC。不過，]25°C與 3 00 V之絕緣電阻（某種程度惡化。此結果對電容 器的長期性能是不良的結果。理想狀態是，I.R.隨時間的變 化很小或是不隨時間變化。 實施例99實質上與實施例98相同，但是其MnC03含 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -17- 563141 Μ Β7 五、發明説明（15) (請先閱讀背面之注意寧項再填寫本頁) 量增加至〇. 2重量％。氧化錳增加可提供長時間非常安定之 1.R·。不過，其似乎亦對於燒結條件有影響，而且觀察到某 些固溶體。 表1 1 (圖]4 )所顯示之實施例1 〇〇與]〇 ]顯示出相之 ML C C結構，但是其爲】0層燒製層厚度爲2 5微米的主動層 。此等實施例中，檢查Zr02與Ti〇2之影響。此等實施例顯 示稍微調整相對於鈦酸鋇之化學計量（Ba0/Ti02 )，並且 顯示出可接受之性能特徵。 表12(圖15)中，實施例]02顯示具有0.25重量 %MnC03之最佳組成物的性質。MnC03之增力□使得此實施 例於9 5 0 °C燒製時具有良好性質，但是於9 7 5 °C燒製時顯示 出少許固溶體。實施例]0 3、] 0 4與1 〇 5實質是相同組成物 ，但是少量添加 〇.2重量％ BaO.B2〇3 + 0.2 Zr03 (]03)、 0.15 重量。/〇V2〇5 ( 104)與 0·6 重量 ％Mg2Ti〇4 ( 105)。 表]3 (圖16)中之實施例106與107顯示出添加W03 之影響。於0.4重量％ (] 0 6 )時，觀察到良好電性質。不 過，於0.6重量％ ( ]07)時，觀察到I.R.稍微變差。
經濟部智恶財1苟肖工消費合作社印K 雖然本文中本發明人的硏究主要有關陶瓷粉末以及由 敌符合X 7 R性能特徵之陶瓷粉末所製得的多層電容器，但 是於硏究期間，本發明人亦發現特定組成物可用於與TCC (電容之溫度係數）有關之Y5V性能特徵。該Y5v TCC的 必要條件是，在溫度範圍爲· 3 0 °C與+ 8 5 °C之間時，介電常 數（“K”）的改變必須在-80%與+22%內（相對於25°C之K 値）。在符合Y5 V特徵之組成物中，鈦酸鋇或鈦酸鉻酸鋇 本紙张尺度適用中國國家標準（CNS ) A4規格（210X 297公釐） -18- 563141 A7 B7 五、發明説明（16) 與添加劑之間的固溶體最好達到必要之高介電常數値β 實施例]08-Π1 (圖17與18)描述些此符合Y5V性能 特徵之組成物與相對應電性質。表]4中所示之實施例]08 、：I 0 9與Π 0表示單層樣本，由鈦酸銷酸鋇 (BaTi.8Zr.2) 〇3(“BTZ”） + ( N d2〇3 ) + BLBS 助溶劑 與Μη C03所組成。由表14可以看出，實施例i〇8提供大 於8,000之高K値（介電常數），且TCC符合Y5V特徵。 實施例Π1 (圖18，表15)顯示出具有1.5% BLBS助熔劑 之組成物於多層陶瓷電容器（“MLC”）中之性質。實例1 Π 亦顯示良好電性質，包括於150 V及125 °C下之高且安定絕 緣電阻。本發明人正對於此等陶瓷粉末進行進一步硏究。 由本發明人之徹底硏究與本文所列出之資料淸楚地看 出，經由起始粉末的最佳組成，已達成製備高介電常數、 非常低溫燒製X7R陶瓷電容器，其中該起始粉末包括：至 少九十重量百分比實質上純鈦酸鋇粉末，其平均粒徑自0.2 至1.2微米；自0.2至2.5重量百分比之硼矽酸鋇鋰；自 〇.]至0.3重量百分比之MnCO3;0·4至1.50重量百分比 Nb205或由鈮酸鹽形式，諸如 BaNb206、CaNb206、 MgNb206、LiNb206所導出之等量Nb205的最佳顆粒生長抑 制劑；以及0.4至].2重量百分比Gd203。此調配物之陶瓷 粉末與由該調配物所製得之多層電容器不包括有毒重金屬 氧化物，而且可以使用銀含量自W%至100%之銀鈀合金。 如上述，已發現倂用Gd203與〇.6至1.5重量°/〇之其他 稀土金屬氧化物與至].50重量％範圍內之顆粒生長抑 -19- (諳先間讀背面之注意事項再填寫本頁) 本紙張尺度適用中國國家標準（CMS ) A4規格（210X 297公漦） 563141 A7 B7 五、發明説明（10
(請先閱讀背面之>1意事項再填寫本頁J 制劑Nb2〇5是獲得所需電性質的基本條件。此等性質包括 K値大於25 00之介電常數、小於2.5%之散逸係數（DF ) 以及在-55°C與125°C之間，TCC在+/- ]5%內。此外，已發 現至多0.3重量。/〇之呈MnC03添加劑形式的氧化錳數量愈 多，可以提供高絕緣電阻，以及在高溫與高電壓下之使用 期限試驗的長期安定性。 因此’本發明包括一種介電陶瓷起始粉末混合物，其 包括至少九十重量百分比實質上純鈦酸鋇粉末，其平均粒 徑自0.2至1.2微米；自〇.2至2.5重量百分比之硼矽酸鋇 鋰；自0」至0.3重量百分比之MnC03 ;顆粒生長抑制劑， 其 5^1 自 I尼化合物 Nb2〇5、BaNb2〇<s、CaNb2〇6、MgNb2〇6 ' LiNb03或其混合物，如此使Nb2 05重量百分比自0.4至 ].50重量百分比，或鉅化合物，或其混合物，如此使Ta2〇5 之重量百分比自0.66重量％至2.50重量％，或鈮與鉅化合 物之莫耳當量的混合物；以及〇. 4至】.2重量百分比之 G d 2 〇 3 0 本發明另一實施樣態包括一種製造較佳介電陶瓷粉末 之方法’其包括以下步驟：混合物上述起始粉末混合物； 在約4 5 0 °C至約55〇t下溫和地煅燒該起始粉末混合物，製 得由起始粉末之混合物的黏聚物所組成之粉末，其中該黏 聚物具有與該鈦酸鋇、硼矽酸鋇鋰、Nb205 ' MnC03與氧化 ( GchCh )之起始粉末實質上相同組成比率；以提供一種 可在開放式氧化鉻耐火架子中，以9 5 〇它至]，〇2 5力燒結之 粉末狀混合物’以製造燒製密度大於5 7 5 g/cni3、介電常數 本紙張尺度適用中國國家標準（CNS ) Λ4規格（2】OX 297公釐） -20- 563141 A7 B7 五、發明説明（18) (#先閱讀背面之注意事項再填寫本頁) (“K”）大於2,500，且TCC平順之介電陶瓷體，其中在 -55°C至]25°C溫度範圍內，相對於25°C溫度之K値，該K 値在]5%內。 本發明另一實施樣態包括一種製造符合X7R性能特徵 之多層陶瓷電容器體的方法。該方法包括以下步驟：形成 上述經煅燒起始粉末混合物的淤漿；製備該淤漿層；乾燥 此等層；形成數層之堆疊體，並將銀鈀電極墨水的經佈線 膜插入次一對相鄰層之間，其中該銀鈀電極墨水包括85% 重量％以上之銀；然後藉由在開放空氣中，以9 5 0 °C至 1，02 5 °C間之溫度下燒結3至5小時，加熱使此等層之堆疊 體完成，製造具有埋入式電極之緻密陶瓷電容器體。本發 明亦包括如此製得之多層陶瓷電容器。 雖然已根據特定實施例與具體實施例說明與解釋本發 明，但是應明白本發明不受限於所述之實施例。例如，雖 然較佳實施例（例如，實施例27、63-69 )說明氧化纟L ( GdsO3 )之較佳重量百分比爲“0.8”，但須明白「約0.8重量 百分比」一句意指〇 · 8重量百分比加減2 0%，儘量說明套佳 比例或具體實施例。本文中，「約―一重量百分比」一句的 相同意義亦適用於以此種句型說明之其他化合物。另外， 本發明包括藉由「將該混合物分散於黏合劑-溶劑-分散系統 」「形成該粉末之淤漿」，由所述之介電陶瓷粉末之較佳 具體實施例製造電容器。不過，必須明白，可以本技術中 習知之任何方法「形成該粉末淤漿」。因此，主要必須參 考附錄之主張權項決定本發明範圍’而非參考前述說明跑 本纸张尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -21 - 563141 A7 B7五、發明説明（19)實例。 (請先閱讀背面之注意事項再填寫本頁) 訂 經濟部智您財1局员工消費合作社印製 本紙乐尺度適用中國國家標準（CMS ) A4規格（210父297公釐） -22-

Claims (1)

  1. 563141 a/t/A 絛正/更五/麵九 B8’ C8 ^___D8 、申請專禾ϋ -- 附件4a: 第91125273號專利申請案 修正後無劃線之中文申請專利範圍替換本 民國92年10月2日修正 I 一種介電陶瓷起始粉末，其包括： a •至少九十重量百分比實質上純鈦酸鋇，其平均粒徑 自〇·2至1.2微米； b·自〇·2至2·5重量百分比之硼矽酸鋇鋰； c*自0.1至〇·3重量百分比之MnC03 ; d·顆粒生長抑制劑，其係選自鈮化合物Nb205、 BaNb2〇6、CaNb2〇6、MgNb2〇6、LiNb〇3 或其混合物，如此 使Nb2〇5重量百分比自〇·4至ι·5〇重量百分比，或鉅化合 物’或其混合物，如此使Ta205之重量百分比自0.66重量 %至2.50重量％，或鈮與鉅化合物之莫耳當量的混合物；以 及 e· 0.4至1.2重量百分比氧化釓。 2.如申請專利範圍第1項之介電陶瓷起始粉末，其中 該氧化釓之重量百分比約0.8百分比。 3 ·如申請專利範圍第1項之介電陶瓷起始粉末，其中 該顆粒生長抑制劑之重量百分比約1 ·〇百分比Nb205。 4.如申請專利範圍第1項之介電陶瓷起始粉末，進一 步包括自0.2至0.6重量百分比之W03。 5 .如申請專利範圍第1項之介電陶瓷起始粉末’進一 步包括自〇·〇7至〇·2重量百分比之Mo〇3。 6. —種用以製造介電陶瓷粉末之方法’包括步驟： 本紙張尺度逋用中國國家樣準（CNS ) A4規格（210 X 297公釐） (請先閲讀背面之注意事項再填寫本頁)
    經濟部智慧財產局員工消費合作社印製 563141 A8 B8 C8 D8 六、申請專利範圍 a·製備介電陶瓷起始粉末之混合物，其包括至少九十 (請先閲讀背面之注意事項再填寫本頁) 重量百分比實質上純鈦酸鋇，其平均粒徑自0.2至1.2微米 :自0.2至2.5重量百分比之硼矽酸鋇鋰；自0.1至0.3重 量百分比之MnC03 ;顆粒生長抑制劑，其選自鈮化合物 Nb205、BaNb206、CaNb206、MgNb206、LiNb03 或其混合 物，如此使Nb205重量百分比自0.4至1.50重量百分比， 或鉬化合物，或其混合物，如此使Ta205之重量百分比自 0.66重量％至2.50重量％，或鈮與鉅化合物之莫耳當量的 混合物；以及0.4至1.2重量百分比之氧化釓； b·在約450°C至約550°C下溫和地煅燒該介電陶瓷起 始粉末混合物’製得由起始粉末之混合物的黏聚物所組成 之介電陶瓷粉末，其中每個黏聚物具有與該鈦酸鋇、硼矽 酸鋇鋰、Nb205、MnC03與氧化釓之起始粉末實質上相同組 成比率；以提供一種可在開放式空氣中於95 0°C至1，025 °C 下燒結之介電陶瓷粉末，以製得符合X7R電容器性能特徵 之介電陶瓷體。 7 .如申請專利範圍第6項之製造介電陶瓷粉末的方法 ，其中該氧化釓之重量百分比約0.8百分比。 經濟部智慧財產局員工消費合作社印製 8 ·如申請專利範圍第6項之製造介電陶瓷粉末的方法 ，其中該顆粒生長抑制劑之重量百分比約1.0百分比Nb205 〇 9·如申請專利範圍第6項之製造介電陶瓷粉末的方法 ，其中該製備混合物步驟進一步包括在該混合物中混合0.2 至0.6重量百分比之W03，以及在該混合物中混合〇.〇7至 本紙張尺度適用中國國家樣準（CNS ) A4規格（210X297公釐） 563141 A8 B8 C8 D8 六、申請專利範圍 0.2重量百分比之m〇03。 10. —種製造符合X7R電容器性能特徵之多層陶瓷電 容器的方法，包括步驟： a•製備介電陶瓷起始粉末之混合物，其包括至少九十 重量百分比實質上純鈦酸鋇，其平均粒徑自0.2至1.2微米 •，自0.2至2.5重量百分比之硼矽酸鋇鋰；自〇·1至〇.3重 量百分比之MnC03 ;顆粒生長抑制劑，其選自鈮化合物 Nb205、BaNb2Q6、CaNb206、MgNb206、LiNb03 或其混合 物，如此使Nb2Ο5重量百分比自0.4至1.50重量百分比， 或鉬化合物，或其混合物，如此使Ta205之重量百分比自 0.66重量％至2.5 0重量％，或鈮與鉬化合物之莫耳當量的 混合物；以及0.4至1.2重量百分比之氧化釓； b ·在約4 5 0 °C至約5 5 0 °C下溫和地鍛燒該介電陶瓷起 始粉末，製得由起始粉末之混合物的黏聚物所組成之介電 陶瓷粉末，其中每個黏聚物具有與該鈦酸鋇、硼矽酸鋇鋰 、Nb205、MnC03與氧化釓之起始粉末實質上相同組成比率 c. 形成該經煅燒陶瓷粉末之淤漿； d. 製備該淤漿之層； ^ e·形成數層與至少一個插入相鄰層之間的銀鈀電極之 堆疊體； f·加熱以熟化該層之堆疊體，其係藉由於9 5 0 °C至 1，〇2 5 °C溫度下，在開放式空氣中燒結，以製造具有至少一 個埋入式電極之多層陶瓷電容器體。 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公嫠） -3 - (請先閲讀背面之注意事項再填寫本頁)
    經濟部智慧財產局員工消費合作社印製 563141 A8 B8 C8 ---_ D8 六、申請專利範圍 11 ·如申請專利範圍第1 〇項之製造多層陶瓷電容器的 方法，其中該銀鈀電極包括85重量百分比以上的銀。 (請先閲讀背面之注意事項再填寫本頁) 1 2.如申請專利範圍第1 1項之製造多層陶瓷電容器的 方法，其中該氧化釓之重量百分比約0.8百分比。 1 3 ·如申請專利範圍第1 2項之製造多層陶瓷電容器的 方法，其中該顆粒生長抑制劑Nb205之重量百分比係約1 .0 霆纛百分比Nb205。 14. 如申請專利範圍第13項之製造多層陶瓷電容器的 方法，其中該製備混合物步驟進一步包括在該混合物中混 合0·2至0.6重量百分比之W03，以及在該混合物中混合 〇·〇7至0.2重量百分比之Mo03。 15. —種符合X7R電容器性能特徵之多層陶瓷電容器 ’其具有至少一個埋入該電容器體內之電極，與一個與該 經濟部智慧財產局員工消費合作社印製 至少一個電極連接之外部終端，該電容器體包括： a·至少九十重量百分比實質上純鈦酸鋇； b_自〇·2至2.5重量百分比之硼砂酸鋇鋰； c.自〇.1至0.3重量百分比之MnC03 ; d· —種顆粒生長抑制劑，其選自鈮化合物Nb205、· BaNb206、CaNb206、MgNb206、LiNb03 或其混合物，如此 使Nb2〇5重量百分比自〇·4至1.50重量百分比，或鉅化合 物，或其混合物，如此使Ta205之重量百分比自0.66重量 °/。至2.50重量％，或鈮與鉅化合物之莫耳當量的混合物；以 及 e·自0.4至1.2重量百分比之氧化釓。 本^張尺度適用中國國家梂準（CNS ) A4规格（210X297公釐） - 563141 A8 B8 C8 D8 六、申請專利範圍 16. 如申請專利範圍第15項之多層陶瓷電容器，其中 該電極包括一個銀含量爲85重量百分比以上之銀鈀電極。 17. 如申請專利範圍第15項之多層陶瓷電容器，其中 該氧化釓之重量百分比約〇. 8重量百分比。 1 8 .如申請專利範圍第1 5項之多層陶瓷電容器，其中 該顆粒生長抑制劑之重量百分比約1·〇百分比Nb205 ° 19.如申請專利範圍第15項之多層陶瓷電容器，進一 步包括0.2至0.6重量百分比之W03，以及〇·07至0·2重 量百分比之Μ〇〇3。 (請先閲讀背面之注意事項再填寫本頁) 經濟部智慧財產局員工消費合作社印製 本紙張尺度適用中國國家揉準（CNS ) Α4規格（210X297公釐）
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