TW524787B - Barium titanate powder, semiconducting ceramic, and semiconducting ceramic electronic element - Google Patents

Barium titanate powder, semiconducting ceramic, and semiconducting ceramic electronic element Download PDF

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TW524787B
TW524787B TW088107690A TW88107690A TW524787B TW 524787 B TW524787 B TW 524787B TW 088107690 A TW088107690 A TW 088107690A TW 88107690 A TW88107690 A TW 88107690A TW 524787 B TW524787 B TW 524787B
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barium titanate
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titanate powder
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powder
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TW088107690A
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Mitsutoshi Kawamoto
Hideaki Niimi
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Murata Manufacturing Co
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Description

524787 A7 B7 五、發明説明（、） 1 發明詳述： 發明範圍 本發明有關一種鈦酸鋇粉末，更特別的是，有關一種用 以製造具有正溫度係數特性之半導體陶瓷。 發明背景 ’
用以控制溫度、限制電流、在常溫下產生熱等應用之電 子元件已使用一種具有正溫度係數特性（下文稱為PTC特性） 之半導體陶瓷，其中當溫度高於居里溫度時，其電阻大幅 提高。已廣泛使用鈦酸鋇陶瓷作為此種半導體陶瓷。 近年來，對於用於上述應用之半導體陶瓷電子元件之需 求提高，該元件具有高耐壓（即高介電強度），因此可於高 電壓下使用。特別是，用於電路之過電流保護元件中所使 用之半導體陶瓷元件必須具有高耐壓。 ij •i 有利於製得具有具有高介電強度半導體陶瓷的習知方法 之一係降低作為原材料之鈦酸鋇粉末粒子大小。因此，研 究焦點都集中在降低粒子大小。例如，日本專利公告 (kokoku)第60-25004號揭示藉由壓碎並混合鈦酸鋇與作為半 導體化劑之氧化銻；於受控制條件下鍛燒；於受控制條件 下粉壓；並於1350°C下燒製該粉壓坯製得顆粒大小為1-5微 米且最大介電強度為500伏/毫米之半導體陶瓷。 不過，習用鈦酸鋇與其半導體陶瓷涉及下列缺點1與2。 1 ·為了有效降低室溫下之電阻係數，於約1300°C燒製鈦酸 鋇粉末為佳。不過，當於此種溫度下燒製該粉末時，鈦酸 鋇顆粒會生長至約1 - 5微米之大小，因此無法達到標的耐電 本紙張尺度適用中國國家標準(CNS) A4規格(210X 297公釐) 524787 A7 B7 五、發明説明（ ） 2 壓性；及 2 .當鈦酸鋇粉末之粒子大小降至0 . 1微米或以下時，該陶 瓷之室溫下電阻係數容易隨產物變化，在某些實例中會隨 時間提高（即，隨著時間改變）。 本發明提出一種介電強度為800伏/毫米或以上且室溫下電 阻係數為100歐姆·厘米或以下之鈦酸鋇粉末，該室溫下之電 阻係數大致上無時程變化。本發明亦提出一種自鈦酸鋇粉 末製得之半導體陶瓷。本發明另外提供一種自該陶瓷製得 之半導體陶瓷電子元件。 發明概要 本發明提出一種介電強度為800伏/毫米或以上且室溫下電 阻係數為100歐姆·厘米或以下之鈦酸鋇粉末，該室溫下之電 阻係數大致上無時程變化。本發明亦提出一種自鈦酸鋇粉 末製得之半導體陶瓷。本發明另外提供一種自該陶瓷製得 之半導體陶瓷電子元件。 本發明第一方面中，提出一種立方晶系且平均粒子大小 為0.1微米或以下之鈦酸鋇粉末，其中經由X射線光電子光 譜（“XPS”）獲得以BaC03/Ba0所示之比率為0.42或以下；該 晶格常數為0.4020毫微米或以上；以Ba/Ti所示之比率為 0.988-0.995。 本發明第二方面提出一種半導體陶瓷，其係由燒結包含 該鈦酸鋇粉末與半導體化劑之半導體材料製得。具有此種 結構使得該鈦酸鋇之顆粒大小即使於約1300°C燒製後仍保 持很小，因此半導體陶瓷具有高介電強度，而且降低室溫 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公釐) 524787 A7 B7 五、發明説明（，） ό 下之電阻係數，該室溫下之電阻係數大致上無時程變化。 本發明第三方面中，提出一種半導體陶瓷電子元件，其 包括一種本發明第二方面所述之半導體陶瓷以及於其上形 成之電極。具有此種結構使得該半導體陶瓷電子元件可以 作為具有PTC特性之熱變電阻器，特別是一種適用於電路用 之過電流保護之元件。 發明詳述 除了 BaTi〇3粉末之外，本發明之鈦酸鋇粉末亦可包括一種 鈦酸鋇粉末為底質物質之粉末，其中B a被S r、C a、P b、Y 、一種稀土元素等部分取代，或者Ti被Sn、Zr、Nb、W、 S b等部分取代。 可於一種用以製造本發明半導體陶资之含鈥酸鋇半導體 材料中添加適量之Mn02、Si02、Ti02、Al2〇3等。 本發明中，“大致上無時程變化”、一辭係指燒製結束1000 小時後於室溫下之電阻係數與燒製後立即測得之電阻係數 比為1.05或以下。 下文將以實施例方式更詳細描述本發明。 實施例 實施例1 t 下文係用以製造本發明鈦酸鋇粉末之實例方法。 首先，製備具有各種Ba含量之氫氧化鋇水溶液與Ti含量 為2.655莫耳之以丁丨（0“？1〇4表示烷氧化錫之異丙醇（下文稱 為IPA)溶液。其次，將以LaCl3.6.3H20 (2·385克）表示之氯化 鑭溶解於乙醇（形成溶液體積為100立方厘米，La含量： -6- 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公釐) 524787 A7 B7 五、發明説明（/ ) 4 0.00664莫耳）之溶液均句於混入該烷氧化錫之IPA溶液。 其次，混合各種氫氧化鎖之水溶液與該氯化_之乙醇溶 液混合物及該烷氧化鈦之IPA溶液，使所形成混合物反應形 成一種淤漿。將該淤漿倒入一個陳化槽。隨後，使該經陳 化淤漿脫水形成一個經脫水餅，其於1 l〇°C乾燥三小時。壓 碎該經乾燥餅，如此製得一種含La之鈦酸鋇粉末。 進行測量以獲得含La之鈇酸鋇粉末之粒子大小、 BaC03/Ba0比、Ba/Ti比、晶系及晶格常數。該粒子大小、 BaC03/Ba0比、Ba/Ti比、晶系及晶格常數分別經由SEM、 XPS、螢光X射線分析及XRD測得。該粒子大小意指利用 SEM測量至少十個粒子之直徑獲得之平均粒子大小。 為形成粒化粉末，於該製得之含L a之鈦酸鋇粉末或是於 800- 1000°C鍛燒上述粉末製得之粉末添加一種黏合劑諸如醋 酸乙晞酯。利用單軸壓製方式模製該粒化粉末，如此形成 一個直徑為10毫米且厚度為1毫米之碟形粉壓坯。然後，在 1200- 1300°C下於空氣中乾燥該粉壓坯兩小時，形成一半導 體陶瓷。於該半導體陶瓷兩個主要表面上塗覆一種用以製 造In-Ga電極之糊漿，並乾燥整體製得一個半導體陶瓷電極 元件。
I 測量具有以上述方式製造半導體陶瓷電子元件之各種B a 含量氫氧化鋇溶液之半導體陶瓷中的室溫下電阻係數、介 電強度、半導體陶瓷表面以BaC03/Ba0表示之比率及室溫下 電阻係數之時程變化比。使用一個數位式電壓計以四點探 針方法測量2 5 °C之室溫下電阻係數。測量樣本斷裂前一刻 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公釐) 524787 A7 B7 五、發明説明（e ) 5 所施加最大電壓，並將該電壓除以介於兩個貼附在該樣本 上之電極間距離求得介電強度。該室溫下之電阻係數時程 變化比率表示燒製結束後1000小時於室溫下之電阻係數對 燒製後立即測得之電阻係數比。 對照實例 於每種作為鈦酸鋇粉末之熱液合成粉末BT-01與BT-02( 由Sakai Chemical Industry Co.，Ltd.所製）中添加硝酸_溶液形 式之鑭。經由蒸發作用乾燥所形成混合物，如此製得含L a 鈦酸鋇粉末。以類似實施例1之方式進行後續步騾與測量。 實施例1與對照實例進行之測量結果示於表1。標有*之樣 本在本發明範圍外。根據對照實例1與2，“陶瓷顆粒大小” 、記錄“1，數十（微米）”之襴係指顆粒大小為數十微米之陶 瓷顆粒於顆粒大小為1微米之陶瓷顆粒中之分散情形。 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公釐) 524787 A7 B7 五 、發明説明（ 表1 樣本 鈦酸鋇粉末之物理性: 半導體陶瓷之物理性質 編號 粒子大 小(微米) BaC03/ BaO比 晶格常數 (毫微米） Ba/Ti 比 陶瓷顆粒 大小(微米) 室溫下之電阻係 數(歐姆·厘米） 介電強度 (伏/毫米) 時程變 化比 1 0.05 0.40 0.4025 0.991 0.8 100 1000 1.03 2 0.05 0.42 0.4020 0.995 1.0 77 833 1.02 3 0.05 0.37 0.4030 0.988 0.9 84 925 1.05 ※斗 0.05 0.48 0.4023 0.995 0.8 90 825 5.0 ※5 0.05 0.42 0.4024 0.997 0.9 95 840 3.5 ※6 0.05 0.40 0.4035 0.985 5.0 10 230 1.01 對照 實例1 0.1 0.38 0.4010 0.994 1，數十 500 250 1.02 對照 實例2 0.2 0.34 0.4005 0.994 1，數十 1000 200 1.01 ※標有*之樣本在本發明範圍外
訂 如表1所示，確認鈦酸鋇粉末之粒子大小為0 · i微米或以 下；經由XPS求得之BaCCVBaO比為〇42或以下；晶格常數 為0.4020愛微米或以下；Ba/Ti比為0 988-0.995，製造介電 強度為800伏/耄米或以上之半導體陶瓷+室溫下之電阻係數 為100歐姆·厘米或以下；其時程變化比為105或以下。 其次’描述限制本發明欽酸鋇粉末粒子大小、以XPS求得 之BaC03/Ba0、晶格常數及Ba/Ti比之原因。 在對照實例2情況下，當鈦酸鋇粉末之粒子大小超過〇 . i 微米時’室溫下之電阻係數不當地超過1〇〇歐姆·厘米，而該 介電強度不當地小於800伏/毫米。因此，鈦酸鋇粉末之粒子 大小限制在0 · 1微米或以下。 -9- 本紙張尺度適用中國國家標竿(CNS) A4規格(210 X 297公釐) 524787 A7 B7 五、發明説明（7 ) 在樣本4之情況下，當經由XPS求得之BaC03/Ba0比超過 0.42時，時程變化比不當地大於1.05。因此，將BaC03/Ba0 比限制在0.42或以下。 當對照實例1與2之晶格常數小於0.4020毫微米時，室溫下 之電阻係數不當地高於100歐姆·厘米，該介電強度不當地小 於800伏/毫米。因此，將晶格常數限制於0.4020 ;毫微米或 以下。 當樣本6中之Ba/Ti比小於0.988時，該介電強度不當地小 於800伏/毫米，然而當其超過0.995時，該時程變化比不當 地超過1.05。因此將Ba/Ti比限制在0.988-0.995。 雖然本實施例中使用La作為半導體化劑，但是該半導體 化劑並無特殊限制。例如，可使用稀土元素，諸如Y、S m 、Ce或Dy ;或是過渡金屬元素，諸如Nb、Ta或W。 氺氺氺 如上述，本發明之鈦酸鋇粉末具有立方晶系，而且粒子 大小為0.1微米或以下，其中經由XPS求得以BaC03/Ba0表 示之比率為0.42或以下；該晶格常數為0.4020毫微米或以上 •，以 Ba/Ti 表示之比為 0.988-0.995。 本發明之半導體陶瓷係由上述鈦酸鋇粉末與半導體化劑 形成，因此提供800伏/毫米或以上之介電強度及100歐姆·厘 米或以下之電阻係數，該室溫下之電阻係數大致上無時程 變化。 本紙張尺度適用中國國家標準(CNS) A4規格(210X297公釐)
葶 訂

Claims (1)

  1. 524787 A8 第088107690號專利申請案 別 中文申請專利莽凰修足本(91年,.mj ) 08 {f 「、申請專利: -告本 年月日/ ϋ汍2分… 1 . 一種平均粒子大小為0 · 1微米或以下之立方晶系鈦酸鋇 粉末，其中經由XPS獲得以BaC03/Ba0所示之比率為 0.42或以下；晶格常數為0.4020毫微米或以上；以Ba/Ti 所示之比率為0.988-0.995。 2. 一種供形成半導體陶瓷之混合物，其係包含如申請專利 範圍第1項之鈦酸鋇粉末及一種半導體化劑。 3. 如申請專利範圍第2項之混合物，其係包含含鑭之鈦酸 鋇粉末。 4. 一種半導體陶瓷，其係燒結包含如申請專利範圍第3項 之混合物之燒結物。 5. 一種半導體陶瓷電子元件，其包括一種如申請專利範圍 第4項之半導體陶瓷與其上形成之電極。 6. 一種半導體陶瓷，其係包含如申請專利範圍第2項之混 合物之燒結物。 7. 一種半導體陶瓷電子元件，其包括一種如申請專利範圍 第6項之半導體陶瓷與其上形成之電極。 -11 - 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公釐)
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