TW557453B - Semiconductor ceramic having a negative temperature coefficient of resistance and negative temperature coefficient thermistor - Google Patents
Semiconductor ceramic having a negative temperature coefficient of resistance and negative temperature coefficient thermistor Download PDFInfo
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- TW557453B TW557453B TW090124989A TW90124989A TW557453B TW 557453 B TW557453 B TW 557453B TW 090124989 A TW090124989 A TW 090124989A TW 90124989 A TW90124989 A TW 90124989A TW 557453 B TW557453 B TW 557453B
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Description
557453
發明背景 ι_.發明領祕 本發明有關-種具有負電阻溫度係數的半導性陶曼及一 種負溫度係數熱敏電阻器。 之.相關括藝描述 近年來,-直要求更精㈣負溫度係數熱敏電阻器,主 要用—作感溫ϋ。_還要求將電阻變化㈣在正或負i百分 範圍内傳 '、’先上,這類負溫度係數熱敏電阻器中係使用 由Μη與Zn、Mg#〇A1中至少一種元素之固態溶液及除了 以外的過渡元素⑴、v、Cr、Fe、c〇 Ni Cup^ 得之尖晶石複合氧化物作為半導性陶瓷。然而一般知道, 複合氧化物會造成耐環境性能的問題。相信該項問題是Μη 離子因為環境溫度與氧分壓變化而改變其氧化態且在格點 間遷移所造成。 為了解決此項問題,開展了研究工作,而在B Giu〇t等人 的論文(Solid State I〇nics,48,93-99,1991)和 人的論文(Journal of the European Ceramic Society,13 185-95,1994)中,報道了一種在輸入原料時添加鋇的方 法。根據這些論文,由於鋇的離子半徑大於過渡元素的離 子半仏鋇然法固;谷於災晶石相中而存在於晶粒邊界,因 為形成不同的相而位於三相點。由於形成了這種結構,因 而在1 2 5 C的高溫環境中,大幅抑制電阻的變化。 此外,在曰本經審查專利申請案公告No. 6-48641中,陳 述藉著在由Μη與Ni的氧化物所製得之熱敏電阻器元件中添 -4 - 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公釐) 557453
加稀土元素氧化物或铭與稀土元素氧化物,可在125。(:高温 環境中控制·電阻變化。 然而’根據上述論文和專利申請公告所描述的方法,由 於游離水☆性鋇離子容易保留在原料與燒結物巾,黏合劑 進行膠凝化,破壞模製性,而且未進行反應之稀土元素的 氧化物會殘留。結果,帛製體因為吸濕而潤脹,在高濕度 ί哀境中產生新的性能問題。本發明者和其它人所進行的試 驗已釐清此等事實。 發明概述 因此本發明一個目的是提供一種具有負電阻溫度係數 的半導|±陶瓷和種負溫度係數熱敏電阻器,它們在高濕 度環境中具有良好的模製性與高可信度。 為達成刖述目的,在本發明具有負電阻溫度係數的半導 性陶瓷中,添加約O.iSM莫耳百分比的ΑΜη〇3 (八表示 Ca、Sr、Ba、La、Pr、Nd、Sm、Eu、Gd、Tb、^與
Ho中的至少一種)於包含Mn與Ti、V、Cr、Fe、Co、 、Cu、Zn、Mg和Ai元素中至少一種元素之固態溶液的 尖晶石複合氧化物中。 此外,在本發明的負溫度係數熱敏電阻器中,在包含半 導性陶曼的元件組合體的表面或内部提供至少一對電極。 在生產半導性陶曼時添加Ca、Sr、Ba、La、Pr、Nd、 Sm、Eu、Gd、Tb、Dy與Ho方面,由於藉著選擇碎鈦礦 Μη複合氡化物,使游離水溶性離子與稀土元素氡化物在燒 成及繞結之後還原,所以可得到特性變化很小的負溫度係 本紙張尺度適用中國國家標準(CNS) Α4規格(210 X 297公釐)
装 訂
線 557453 A7 ______B7____ 一 五、發明説明(3 ) 數熱敏電阻器,其中因為黏合劑之反應與吸水性所造成的 模製體潤脹得以抑制,高濕度環境下的可信度良好。 根據本發明,可使用CaMn03、SrMn03、BaMn〇3、 L a Μ η Ο 3、p r μ η Ο 3、N d Μ η Ο 3、S m Μ η Ο 3、E u Μ η Ο 3、 GdMn03、TbMn03、DyMn03 和 ΗοΜη03 作為鈣敛礦 Μη 複合氧化物,可以使用其中的一種或同時使用兩種或多 種。 添加ΑΜη03的量限於約〇. 1至20莫耳百分比的理由在 於’當添加量小於約〇 · 1莫耳百分比時,就不能實現添加效 果’當添加量大於約20莫耳百分比時,則電阻值與Β常數 變得過大。此外,在高濕度環境下的電阻有較大之變化。 1_式簡單說明 圖1是表示本發明第一種負溫度係數熱敏電阻器的透視 圖;且 圖2是表示本發明第二種負溫度係數熱敏電阻器的剖視 圖。 毯佳具體會你丨始沭 下文描述本發明半導性陶瓷與負溫度係數熱敏電阻器的 具體實例。 星二AJ溫度係數熱敏電阻器,圖1 圖1示出本發明的第一種負溫度係數熱敏電阻器,其 中元件組合體11係使用具有負電阻溫度係數的半導性陶兗 形成,在該元件組合體11的兩個主表面上設置電極丨2與 13° 本紙張尺度適用中國國家標準(CNS) Α4規格(210X 297公釐) 557453 A7 ___ _B7 五、發明説明(4 ) 在該具有負電阻溫度係數的半導性陶曼中,在包含Mll與 丁1、乂、(^、?6、(:〇、>^、(:11、711、1^§及八1中至少一 種之固態溶液的矣晶石族複合氧化物中,添加約〇 1至2 〇莫 耳至少一種下列氧化物:CaMn03 、SrMn〇3 、
BaMn03、LaMn03、PrMn03、NdMn03、SmMn03、 EuMn03、GdMn03、TbMn03、DyMn03和HoMn03。 以下具體實例1至4中詳細描述這些材料與製造方法。 電極1 2及1 3以應用厚膜材料諸如印刷等方法或應用薄膜 材料諸如蒸發、濺射等方法形成,其中使用了一般已知的 電極材料,而形成電極的材料與方法可視情況使用。 复二種$溫唐係數熱敏電阻器,圖2 圖2示出本發明的第二種負溫度係數熱敏電阻器2〇,其 中内部電極22與23設置在元件組合體21内部,而組合體21 包括多片由具有負電阻溫度係數的半導性陶瓷構成之板 片,外部電極24與25係設置在元件組合體21的表面上。 具有負電阻溫度係數的半導性陶瓷與第一種負溫度係數 熱敏電阻器1 0中的相同,在具體實例5中詳細描述該材料 和方法。 例如’該内部電極2 2及2 3係藉著在一板片上塗覆導電材 料糊而形成,其它板片藉壓力黏合形成層積體,將該層積 體進行焙烘。另外,在層積體兩末端部分塗覆銀糊,並進 行焙烘,可形成外部電極24與25。而且,製造商可自行選 擇用以形成電極22至25的材料與方法。 具體實例1 本紙張尺度適用中國國家搮準(CNS) A4規格(210 X 297公釐) 557453 A7 -------B7 五、發明説明(5 ) Μπ3〇4與BaC〇3進行混合,使Ba/M的原子比變成i而製 備成原料。在以1 3 0 〇 °c燒制2小時後,原料用粉碎機壓 碎,再用球磨機精磨2〇小時,得到BaMn〇3細粉。 接著如表1所列,將B a μ n 〇 3粉加到重量比為5 〇 : 3 〇 : 2 〇 的Mn3〇4、Ni〇和Fe2〇3裏,用球磨機混合16小時。原料 以900°C燒制2小時,用粉碎機壓碎。接著將1〇%重量作為 有機黏合劑之聚乙烯醇、〇 5重量百分比作為增塑劑之甘油 和1.0重1百分比聚乙稀分散劑加到已壓碎的原料裏,混合 1 6小時。然後,用2 5 0目篩網除去粗粒,得到板片形成性 之漿料。用刮刀將該漿料成形為5〇|1111厚的陶瓷生片。 把陶瓷生片衝壓成固定尺寸,再把生片層積成厚, 於厚度方向加壓至2噸/厘米2之壓力。以U5(rc燒制2小時 後,將層積體拋光至厚度0.5 mm,在層積體兩主表面塗上 銀糊,以70 0。(:焙烘10分鐘。然後,用切鋸將層積體切成 2父2111111大小的板片,得到尺寸為20><2〇><〇5111111的負 /JHL度係數熱放電阻元件(參照圖1 )。另外,亦製備添加 B a C 03而不是添加B a Μ η 03的樣品,以作為對照組。標有 星號的樣品與本發明的樣品不同。 通過隨機取樣,選出一百片以此方法得到的負溫度係數 熱敏電阻器元件,測量它們在25°C溫度時的阻值(r25)和在 5 0°C溫度時的阻值(Rw),根據測得的值計算比電阻(p25) 與數(B25/50)。而且’用25C溫度的阻值(R25)與元件 尺寸確定比電阻。此外,通過下述公式(表達式)用25t的 阻值(R25)和5 0°C的阻值(R5〇)確定B常數。 ’ 本紙張尺度適用中國》家標準(CNS) A4規格(210 X 297公釐) 557453 A7 B7 五、發明説明(6 ) 公式1 B 常數(K) = 1ηΚ25(Ω) = ίηΚ5〇_(Ω) 1/298.15-1/323.15 接著,把被測試 >片置於125 °C的恒溫爐和設置為60°C 與95%RH的恒溫浴中歷時1 0 0 0小時,再測量阻值變 化率。測量值列於表1。 由表1可理解,藉著添加BaMn〇3而非BaCo〇3,明顯改 善了高濕環境條件下的電阻變化率。再者,當BaMn03的 添加量約為0.1莫耳百分比或更少時,看不出添加效果,而 當添加量約為2 0莫耳百分比或更多時,可看出電阻急劇增 大,電阻變化率在高濕環境條件下增大了。 表1 No BaMn〇3 (莫耳百 分比) BaC03 (莫耳百分 比) 原始特性 高溫環境試驗 高濕環境試驗 p25/n.cm B常數/K ar25/% △r25/% 1* 0 0 3852 3457 +5.1 +0.2 2* 0.05 0 3860 3458 +4.4 +0.2 3 0.1 0 3863 3458 +0.8 +0.4 4 0.5 0 3868 3460 +0.8 +0.4 5 1 0 3868 3460 +0.7 +0.3 6 5 0 3880 3465 +0.2 ,+0.1 7 10 0 3886 3466 +0.2 +0.2 8 20 0 3892 3468 +0.3 +0.5 9* 25 0 5723 3563 +1.9 +2.9 10* 0 1 3924 3480 +0.6 +2.1 11* 0 10 4020 3495 +0.3 +2.8 12* 0 20 4106 3520 +4.0 +3.7 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公釐) 557453 A7 B7 五、發明説明(7 ) 具體實例2 混合 Mn304、CaC03、SrCO 與 BaC03 ,使 Ca/Mn、
Sr/Mn與Ba/Mn的原子比變成1而製備成原料。以13〇〇t 燒制2小時後,用粉碎機壓碎原料,再用球磨機細磨2〇小 時而得到 CaMn03、SrMn03、BaMn03 細粉。 接著如表2所列,將CaMn03、SrMn03與BaMn03粉加 到重量比為45:25:30的Μπ3〇4、NiO、C0O4裏,用球磨 機混合1 6小時。將原料以900 °C燒制2小時,用粉碎機壓 碎。接著,將1 0重量百分比作為有機黏合劑之聚乙烯醇、 0.5重量百分比作為增塑劑之甘油和1 〇重量百分比聚乙烤 分散劑加到壓碎的原料裏,混合1 6小時。然後,用2 5 〇目 篩網除去粗粒而得到片形漿料,用刮刀將該槳料形成5〇|1111 厚的陶瓷生片。 陶瓷生片被衝壓成固定尺寸,生片層積到1 mm厚,以厚 度方向加壓2噸/厘米2。以1200°C燒制2小時後,將層積體 抛光成0.5 mm厚度’在層積體兩表面上塗布銀糊,以700 培烘10分鐘。然後,用切鋸將層積體切成2X2 mm的小片 尺寸’得到尺寸為2.0X2.0X0.5 mm的負溫度係數熱敏電 阻器元件(參照圖1)。另外,亦製備添加CaC〇3、51>(:〇3與
BaC03 而不添加 CaMn03、SΓMn03與BaMn03 的樣品。 標有星號的樣品不同於本發明的樣品。 通過隨機取樣,選出一百片這樣得到的負溫度係數熱敏 電阻器元件,測量它們在25°C溫度時的阻值(R25)和在5〇t 溫度時的阻值(R 5 〇 ),根據測得的值計算比電阻(P 2 5 )與B常 -10 - 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公釐) 557453 A7 B7 五、發明説明(8 數(Bn/so) u接著用用25 C溫度的阻值(民25)與元件尺寸確 疋比電阻。於是,通過上述公式(表達式,用“艽的阻值 (R25)和50°C的阻值(R5〇)確定b常數。 接著,將被測試小片置於1 2 5。(:恒溫爐和置成6 0它與9 5 /ό R Η的恒>jcl恒濕浴中1 〇 〇 〇小時,然後測量電阻變化率, 測量結果也列於表2。 從表2可見,藉著添加CaMn03、SrMn03與BaMn03而 不疋C a C 0 3、S r C 0 3與B a C 0 3,明顯改善了高濕環境條件 下的電阻變化率。另外,當CaMn03、SrMn03與 BaMnOs的添加量約為0.1莫耳百分比或更少時,看不出添 加效果’而當CaMn03、SrMn03與BaMn03的添加量超 過約20莫耳百分比時,可看出電阻增大了,而且在高濕環 境條件下增大了電阻變化率。 表2 No CaMn〇3 (莫耳百 分比) SrMn03 (莫耳百 分比) BaMn03 (莫耳百分 比) 原始特性 高溫環境試 驗 高濕環境試 驗 Ρ25/ΩΧΠ1 B常數/K △R25/% △R:25〆% 1* 0 0 0 1247 3820 +7.5 +0.3 2* 0.05 0 0 1247 3819 +7.1 +0.3 3 0.05 0.05 0 1250 3822 +0.9 +0.3 — 4 0 1 1 1253 3223 +0.7 +0.4 5 3 0 2 1260 3826 +0.4 +0.4 6 2 2 2 1258 3825 +0.4 +0.3 7 5 5 0 1270 3830 ^ +0.3 +0.3 8 5 5 5 1284 3835 +0.3 +0.4 9 10 2 3 1281 3833 +0.3 +0.4 10 5 10 5 1296 3846 +0.4 +0.4 11* 10 10 5 2689 4030 +1.1 +1.7 12* 10 20 0 2814 4102 +1.1 +1.9 -11 - 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公釐) 557453
具體實例3
LhO3與Μη"4經混合,使La/Mn的原子比變成ι而製 備成原料。以8〇〇t燒制2小時後,用粉碎機壓碎原料,再 用球磨機細磨20小時得到LaMn〇3細粉。 接著,按表3所示比率將LaMll〇3粉加到重量比為 50:3 0:20的Mn304、Nl0與卜2〇3裏,用球磨機混合16小 時。該材料以9〇〇t燒制2小時,用粉碎機壓碎。接著,將 10重量百分比作為有機黏合劑之聚乙歸醇、重量百分比 作為增塑劑之甘油與1,0重量百分比聚乙料散劑加到壓碎 的原料裏混合16小時。然後,用25〇目篩網除去粗粒而得 到片形漿料,再用刮刀將該漿料形成5〇μιη厚的陶瓷生片。 將該陶曼生片衝壓成固定尺寸,生片層積成總厚度 1 mm,於厚度方向加壓2噸/厘米2。以丨丨5 〇 t燒制2小時 後,將層積體拋光成0.5 mm厚度,在層積體兩表面上塗布 銀糊,以700°C焙烘1〇分鐘。然後,用切鋸將層積體切成 2X2 mm小片尺寸,得到尺寸為2 〇χ2 〇χ〇5爪爪的負溫 度係數熱敏電阻益疋件(參照圖丨)另外,亦製備以La2〇^< 替LaMn〇3的樣品以作為對照組。表3中標星號的樣品不同 於本發明的樣品。 通過隨機取樣’選出-百片這樣得到的負溫度係數熱敏 電阻器元件,測量它們在25t溫度時的阻值(R25)和在5〇t 溫度時的阻值(Rw),根據測得的值計算比電阻((^5)與8常 數(Bu/w)。接著用用25。(:溫度的阻值(R25)與元件尺寸確 定比電阻。於是,通過上述公式(表達式)用25。(:的阻值
557453 A7 B7
數(Bh/w)。另外,用25t溫度的阻值(R25)與元件尺寸確 定比電阻。此外,通過上述公式(表達式)用25 t的阻值 (R25)和5〇°C的阻值(R5〇)確定b常數。 接著,將被測試小片放在125t恒溫爐和設置成6〇t與 9 5 R Η的恒溫恒濕浴中1 〇 〇 〇小時,然後測量電阻變化 率,測量值列於表5。 由表5可知,即使在層積型片狀熱敏電阻器元件中,當添 加C a Μ η 03而不是c a C 03時,仍然大幅改善電阻在高濕環 i兄下的變化率。
裝 訂
表5 ---- No CaMn03 (莫耳百 分比) CaC〇3 (莫耳百分 原始特性 而溫環境試 驗 高濕環境試 驗 比) Ρ25/Ωχιη Β常數 /Κ ar25/% ar25/% 1* 0 0 68210 4084 +3.4 +0.2 2 5 0 71540 4098 +0.1 +0.2 3* 0 5 70920 4095 +0.3 +2.1 由前文描述可知,在燒制與燒結以後,水溶性離子並不 留在本發明具有負電阻溫度係數的半導性陶瓷中,因而能 抑制黏合劑在模制時的反應和電阻在高濕環境下的變化。 此外’大幅改善可信度,且在本發明負溫度係數熱敏電阻 器中得到電阻偏差小的高精密度裝置。 k 17 - 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公釐)
Claims (1)
- 557453 A8 B8 C8 D8 第090124989號專利申請案 中文申請專利範圍替換本(92年4月) --—-- ; 申請專利範圍 1 ·種具有負電阻溫度係數的半導性陶瓷,其包括: 一尖晶石複合氧化物,包含Mn和至少一種選自包括 Τι、V、Cr、Fe、Co、Ni、Cu、Zn、Mg 及 A1 之群的元 素之固態溶液;及 約0.1至20莫耳百分比的AMn〇3,其中A是至少一種選 自包括 Ca、Sr、Ba、La、Pr、Nd、Sm、Eu、Gd、 Tb、Dy及Ho之群的元素。 2 ·如申請專利範圍第1項之具有負電阻溫度係數的半導性陶〜 瓷,其中 該尖晶石複合氧化物係包括Μη及至少一種選自包括 Fe、Co、Ni和Α1之群的元素之固態溶液;且 A表示Ca、Sr、Ba和La中的至少一種元素。 3 .如申請專利範圍第1項之具有負電阻溫度係數的半導性陶 瓷,其中 該尖晶石複合氧化物係包含Μ η、N i和至少一種選自包 括Fe、Co與A1之群的元素之固態溶液;且 A表示Ca、Sr、Ba與La中的至少一種元素。 4 ·如申請專利範圍第1項之具有負電阻溫度係數的半導性陶 瓷’其中 ΑΜη03 係為 BaMn03、LaMn03、Sr0 05La0.95MnO3 、CaMn03、SrMn03或其混合物。 5 ·如申請專利範圍第4項之具有負電阻溫度係數的半導性陶 瓷,其係為元件組合體形式,具有一表面及位在該元件組 合體表面上的一對分隔電極,而形成一負溫度係數熱敏電 阻器。 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公釐) 5574536 .如申清專利範圍第4項之具有負電阻溫度係數的半導性陶 瓷,其係為元件組合體形式,具有一表面及位在該元件組 合體内部的-對分隔電極,而形成一負溫度係數熱敏電阻 7 ·如申请專利範圍第3項之具有負電阻溫度係數的半導性陶 瓷,其係為元件組合體形式,具有一表面及位在該元件組 口此表面上的一對分隔電極,而形成一負溫度係數熱敏電 阻器。 8.如申請專利範圍第3項之具有負電阻溫度係數的半導性陶 瓷,其係為元件組合體形式,具有一表面及位在該元件組 合缸内部的一對分隔電極,而形成一負溫度係數熱敏電阻 9 ·如申凊專利範圍第2項之具有負電阻溫度係數的半導性陶 竞,其係為元件組合體形式,具有一表面及位在該元件組 合體表面上的-對分隔電極,而形成一負溫度係數熱敏電 阻器。 10. 如申Μ專利範圍第2項之具有負電阻溫度係數的半導性陶 资,其係為元件組合體形式,具有一表面及位在該元件組 合體内部的-對分隔電極,而形成—負溫度係數熱敏電阻 器。 11. 如申明專利範圍第i項之具有負電阻溫度係數的半導性陶 竞,其係為元件組合體形式,具有—表面及位在該元件組 合體表面上的一對分隔電極,而形成一負溫度係數熱敏電 阻器。 -2-557453 A8 B8 C8 D8 六、申請專利範圍 12.如申請專利範圍第1項之具有負電阻溫度係數的半導性陶 瓷,其係為元件組合體形式,具有一表面及位在該元件組 合體内部的一對分隔電極,而形成一負溫度係數熱敏電阻 器0 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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JP (1) | JP3711857B2 (zh) |
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US6469612B2 (en) | 2002-10-22 |
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