TW460414B - Methods to partially reduce a niobium metal oxide and oxygen reduced niobium oxides - Google Patents

Methods to partially reduce a niobium metal oxide and oxygen reduced niobium oxides Download PDF

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Publication number
TW460414B
TW460414B TW088116008A TW88116008A TW460414B TW 460414 B TW460414 B TW 460414B TW 088116008 A TW088116008 A TW 088116008A TW 88116008 A TW88116008 A TW 88116008A TW 460414 B TW460414 B TW 460414B
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niobium
scope
patent application
niobium oxide
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TW088116008A
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James A Fife
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Cabot Corp
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Priority claimed from US09/154,452 external-priority patent/US6391275B1/en
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Description

< 告本 460414 ㈣說♦相-- 此專利申請案是1998年9月16曰提出申請的美國專利申 請案第09/154, 452號及19 98年9月16日提出申請的美國專 利申請案6 0 / 1 0 0，6 2 9號的接續申請案。 發明背景 本發明係關於鈮及其氧化物，更特別係關於鈮氧化物及 至少部份還原鈮氧化物之方法，另係關於氧減少的鈮。 發明概述 根據此處所表現及描述之本發明之目的，本發明传關於 至少部份還原銳氧化物的方法…二本 料存在時，於能夠使得鈮氧化物中的氧原子轉移至吸氣材 料的環境中，熱處理此鈮氧化物達足夠的時間和溫度，以 形成氧減少的銳氧化物。 本發明亦係關於氧減少的鈮氧化物，其有利地具有一些 優良性質二尤其是製成電解用電容器陽極之時。例如，由 本發明之氧減少的鈮氧化物製得的電容器 2 0 0,0 0 0 CV/克或以上。此外，电合罝同至 #从制π认兩m 外，由本發明之氧減少的鈮氧 化物I付的電解用電容器陽極之叱 ^容器眺漏失由約G.5毫微安培八 量= 提2:=化物之電容器的電容 能夠使得銳氧化物中的氧原存在時，於 熱f理此銳氧化物達足約的時間和溫度氧 化物，成氧減她氣化物，此氧減少： = 4 6〇4 1 4
製成電容器陽極時，具有減少的DC漏失和/或提高的電容 $ 。 應瞭解前述概述和下列詳述僅作為例子和說明，欲如申 請專利範圍中所提出者進一步說明本發明。 jf寸圖簡述 附圖卜11是本發明的多個氧減少的鈮氧化物於不同放大 倍數下得到的SEM。 發明詳述 本發明的實施例中，本發明係關於部份還原鈮氧化物的 方法。一般而言’此方法包括在有吸氣材料存在的情況 下，於能夠將鈮氧化物中的氧原子轉移至吸氣材料的環境 中’熱處理此起始銳氧化物達足夠的溫度和時間，以形成 氧減少的鈮氧化物。 就本發明的目的’鈮氧化物可以是鈮金屬和/或它們的 合金之乳化物中之至少一者。起始銳氧化物的特定例子是
Nb205。 本發明所用的鈮氧化物可為任何形狀或尺寸。較佳情況 中，此鈮氧化物為粉末或各種顆粒形式D可兹利用的粉末 類型的例子包括片、角形、結節狀及它們的混合物或各種 變化，但不在此限。較佳情況中’此鈮氧化物是能夠更有 效地形成氧減少的鈮氧化物之粉末形式者。 此較佳鈮氧化物粉末例包括尺寸由約6 〇 /丨〇 〇至約 100/32 5和由約60/100至約200/325網目者。其他尺寸範圍 是40網目至約32 5網目。換言之’此較佳鈮氧化物粉末的
第6頁 ^ 6Q41 ά_ 五、發明說明（3) 顆粒尺寸由約150/250至約45/150微米，及由約150/250至 約45/75微米。另一較佳尺寸範圍由約35 5微米至約45微 米。 用於本發明之目的的吸氣材料是能夠還原鈮氧化物的任 何材料。較佳情況中，吸氣材料包含钽、鈮或二者。其他 例子包括，鎂和類似物。但不在此限。可以使用任何對於 氧之親和力比對於鈮氧化物之親和力來得大的吸氣材料。 更佳情況中，此吸氣材料是鈮。用於本發明之目的的鈮吸 氧材料是任何能夠移除或部份還原在銳氧化物中之氧之含 鈮金屬的材料。因此，此銳吸氣材料可以是含銳金屬與他 種成份之混合物的合金或材料。較佳情況中，銳吸氣材料 即使不全為銳金屬，也是以銳金屬為主要成份者。銳吸氣 材料純度並不重要，但以由高純度鈮構成吸氣材料為佳， 以免在熱處理期間内引入其他雜質。據此，鈮吸氣材料中 的鈮純度以至少約98%為佳，至少約9 9%更佳。鈮吸氣材料 中的氧量可以是任何量。較佳情況中，會影響DC漏失的雜 質（如：鐵、錄、鉻和碳）的量低於約100 ppm。更佳情況 中，此吸氣材料是鈮金屬片，此以電容量高者為佳，如： 超過約75, 00 0 CV /克，約1 0 0, 0 0 0 CV /克或以上更佳， 如約2 0 0，0 〇 〇 CV /克。此吸氣材料亦以具有高表面積為 佳，如：BET由約5至約3 0平方求/克，約2 0至約3 〇平方米 /克更佳。 ' 此艇吸氣材料可為任何形狀或尺寸。例如，此銳吸氣材 料可為含有欲還原之鈮氧化物的盤狀形式或可以是顆粒或
第7頁 f * 4604 1 4 五、發明說明（4) ^ 粉末尺寸。較佳情況中，鈮吸氣材料為粉末形式，以具有 用以還原此銳氧化物的隶有效表面積。因此，此起吸氣材 料可以是片狀、角形、結節形或其變化之組合，如：粗 粒，如：14/40網目粒，其可藉過篩而簡便地與粉末產物 分離。 類似地，此吸氣材料可以 論之用於组吸氣材料之相同 吸氣材料可單獨使用或與纽 他種材料可構成吸氣材料的 吸氣材料在使用之後，可 如果吸氣材料和氧減少的銳 氣材料與鈮氧化物的基礎金 似形狀和尺寸。此外，以使 度吸氣材料為佳，此乃因這 氧化物相同或類似的氧化態 氧減少的鈮氧化物產率丨〇〇% 作為吸氣材料也可以留下成 份。 通常’足量的吸氣材料存 鈮氧化物。此外，吸氣材料 定。例如，如果希望稍微還 常以符合化學計量的量存在 化物中所存在的氧來還原鈮 是2至5倍於化學計量。一個 是 鈮 之 類 且 可 以 具 有 前 面 的 較 佳 參 數 和 / 或 性 質 〇 他 或 鈮 吸 氣 材 料 併 用 0 同 樣 地 — 部 份 0 以 移 除 或 留 下 〇 較 佳 情 況 中 氧 化 物 一 起 留 下 那 麼 希 望 屬 相 同 並 且 與 鈮 氧 化 物 具 有 用 南 純 度 、 南 表 面 積 和 高 孔 樣 的 材 料 會 得 到 與 氧 減 少 的 之 故 0 因 此 此 方 法 可 以 達 的 程 度 0 此 吸 氣 材 料 因 此 可 為 氧 減 少 的 鈮 氧 化 物 中 的 在 以 至 少 部 份 還 原 經 熱 處 理 量 視 鈮 氧 化 物 所 須 還 原 程 度 原 此 鈮 氧 化 物 Ϊ 則 吸 氣 材 料 0 類 似 地 J 如 果 實 質 上 依鈮 氧 化 物 > 則 吸 氣 材 料 的 存 在 例 子 中 吸 氣 材 料 存 在 量
46041 4 五、發明說明（5) (如：钮吸氣材料為10 0%组）使得吸氣材科與存在的鈮氧化 物量之間的比例由約2 : 1至約10 : i。此吸氣材料以鱼起 始起氧化物在能夠使得鈮氧化物中的氧原子轉移至吸器材 料的環境（如：氫氣氛）中摻合或混合為佳，其溫度以^ 1 1 0 〇 °C 至約 1 5 0 0 °C 為佳。 Λ ' 此外’吸氣材料量亦可視欲還原的鈮氧化物類型而定。 例如，要還原的鈮氧化物是NbJ5時，吸氣材料量以5 : } 佳°同樣地，起始物是Ν^2〇5時，使用符合化學旦二 Μ μ 丨匕子叶里的銳金 喝片，以達到0· 89份金屬/1份氧化物。 起始鈮氧化物的熱處理可以在任何熱處理梦 今、 牧罝或常用於 连屬（如：鈮和钽）之熱處理的爐中進行。鎚& 材枓存在下進行的熱處理是於足夠溫度進行 夕的銳氧化物的時間。熱處理的溫度和時間 這些因素如：銳氧化物的還原f、吸 吸 料類型和鈮氧化物類型。通常，鈮氧化物的叙 度由約8 0 0 °c或以下至約1 9 0 0 °c ，以約1 0 0 0它至約14 f 為佳，約11 0 0 °C至約1 25 Ot最佳。詳細言之， A 純1化物是 3纽的氧化物時，熱處理溫度將由約1 〇 0 〇它至約 ， 約1100 eC至約1 2 50。(：更佳，處理時間由約5分鐘至Cp 鐘，約30分鐘至約60分鐘更佳。本說明書的慣例' = 使得嫻於此技術者毫無困難地控制熱處理時 、 ^ 」和溫度’以 使錕氧化物得到適當或所欲還原程度。 此熱處理於能夠使得鈮氧化物中的氧原子韃 将移至嗯氧材 料的環境下進行。此熱處理通常於含氫的環 兄、以僅含氫 460414 五、發明說明（6) 者為佳）中進行。他種氣體（如：惰性氣體）亦可與氫一起 存在’只要他種氣體不會與氫反應即可。較佳情況中，熱 處理期間内存在的氫氣壓由約1 〇托耳至約2 0 0 0托耳，以約 100托耳至約1000托耳為佳，約1〇〇托耳至約930粍耳最 佳。可以使用&和惰性氣體（如：Ar)之混合物。同樣地， 在化中的H2也可用以控制鈮氧化物中的n2含量。 熱處理期間内，整個熱處理程序可以使用固定的熱處理 溫度，或者可以變化溫度或利用溫度改變步驟。例如，可 以先使氫為1000 °c，之後將溫度提高至125〇°c達30分鐘， 之，降溫至1 00 0 °c並維持於此溫度直到移除氫氣為止。 除氫或他種氣體之後，可以降低爐溫。可以改變這些去 以適用於工業需求。之後可以利用，如：粉碎方式了1" 一步降低氧減少的鈮氧化物之尺寸。氧減少的鈮氧化= 以閥金屬可利用的任何方法凝聚和粉碎或加工。 氧減少的鈮氧化物亦可含有氮，如：約1〇〇 3 0, 0 0 0 ppm 的 N2。 —主約 氧減少的鈮氧化物是任何鈮氧化物中的 氧化物來得低的銳氧化物。典型氧減少 々：起 組合。通常，…之』還原的銳氧化的任何 比是約1 :低於2‘5，以丨：2為佳，！ ：1勿】之，與氧的原子 更佳。換S之，較佳情況中，經還原的鈮，1 . 〇. 7 NbxOy中，Nb是鈮，x是2或以下，y小於2 ’表示式 中，X是1，y小於2，如：i .丄、！ _ 〇 1…。更佳情况 460414 _______________. 五、發明說明（7) 起始鈮氧化物可以藉由於1000 °C鍛燒直到移除所有揮發 性Μ份而製得。此氧化物可以藉過篩而分粒。可以利用氧 化物的預熱處理來製造氧化物顆粒中之經控制的孔隙度。 本發明之經還原的鈮氧化物以具有微多孔表面為佳，具 有海棉狀結構更佳，其中，主要顆粒以約1微米或以下為 佳。SEM進一步說明本發明之較佳之經還原的鈮氧化物類 型°如可由這些照片得知者，本發明之經還原的鈮氧化物 具有高表面積和約50%孔隙度的多孔結構。此外，本發明 之經還原的錠氧化物之特徵在於具有較佳的比表面積，約 0. 5至約1 〇. 〇平方米/克，約〇 5至約2, 〇平方米/克更 佳，約1.0至約1.5平方米/克又更佳。鈮氧化物粉末的較 佳表觀密度是低於約2. 〇克/立方公分，低於丨.5克/立方 公$更佳，約0.5至約15克/立方公分又更佳。此外’此 鈮氧=物粉末的Scott密度由約5克/立方英吋至約35克〆 因為形成氧減少的銳氧化物及使用此物，所以本發明呈 有使得使用較少量的銳所得到之產物具有與有銳存在時類 二即使未能優於)的性質。因此，因為使用同量的銳可以 取付更夕的陽極或他種產物’所以’本發明擴展 (如：電容器陽極）中的鈮量。 、 物 本發明之各種氧減少的鈮氧化物的進—步 =i發=之氧減少的銳氧化物形成電容器陽極而得到的電 性貝。通吊’將本發明之氧減少的鈮氧化物粉末壓成陽 極，於適當溫度燒結此壓成的粉末，之後對此陽極進行陽
第11頁 460414 __ 五、發明說明（8) 極化處理以製得電解用電容器陽極，可於之後測試其電性 質，藉此測試本發明之氧減少的鈮氧化物。 據此’本發明的另一實施例係關於由本發明之氧減少的 鈮氧化物形成之用於電容器的陽極。類似於製造金屬陽極 所用的方法，即，擠壓有鈮埋於其中的多孔丸粒及之後加 以燒結及陽極化，可以由粉末形式之經還原的氧化物製得 陽極。由本發明之一些氧減少的銳氧化物製得的陽極之電 容量由約1，000 CV/克或少至約300, 000 CV/克或更多，且 其它電容量由約20, 000或以下CV/克至約300, 000 CV /克 或以上，電容量的其他範圍可由約62，000 CV/克至約 2 0 0,0 0 0 CV/克或以上，且以約60, 0 00至約1 5 0, 0 00 CV/ 克為佳 得電容 氧減少 是氧減 °c ，以 佳。氧 可以與 由本 至約3 5 的氧化 40伏特 化物之 後在氫 。形成 器陽極 的鈮氧 少的氧 約 1 2 0 〇 減少的 用於銳 發明之 伏特， 銳時， 更佳。 陽極可 氣氛或 本發明的電各IS陽極時 具有所欲性質的溫度。此燒結溫度視所用之 化物而定。較佳情況中，氧減少的鈮氧化物 化銳時’此燒結溫度是由約12〇〇 t至約丨750 C至約1 4 0 0 C為佳，約1 2 5 0。(：至約1 3 5 0 °c更 ，氧化物是氧減少的氧化鈕時，此燒結溫度 氧化物時相同。 銳氧化物形忐& 以約6至約AW極存的形成電壓是約^伏特 形成電壓以約6:= D此外’使用氧減少 也可以使用更古伏特為佳，約Μ至約 製自：製成有：的形成電壓。經還原的鈮氧 他種適用的氣或他種連接線的丸粒，之 们孔汛中於有吸氣材料存在的情況 460414
五 '發明說明（9) 下處理，所用條件如同本發明 視情況地加以鍛燒及陽極化。 粒可直接製得’如：同時形成 勤連接器可於陽極化處理之前 較於鈕氧化物的鈮氧化物，預 電壓類似或大約相同，甚至於 明之乳減少的銳乳化物形成的 微安培/CV。舉例言之，在本 的一些氧減少的鈮氧化物形成 微安培/CV至約〇· 50毫微安培 的粉狀鈮氧化物一般，之後 此實施例中，製得的陽極顆 氧減少的鈮氧化物和陽極。 的任何時間埋藏或接上。相 期使用他種鈮氧化物的形成 可能高些。同樣地，由本發 陽極之DC漏失低於約5.0毫 發明的實施例中，由本發明 的陽極之DC漏失為約5.0毫 /CV。 本發明亦係關於根據本發明之表面上具有鈮氧化物膜的 電容器γ較佳情況中，此膜是五氧化鈮膜a將金屬粉末製 成電容器陽極的方法是嫻於此技藝之人士熟知者，這樣的 方法述於美國專利案第4,805,074、5,412,533、 5,211，741和5,245,514號及歐洲專利案第〇 634 76 2 A1和
0 634 761 A1，茲將其中所述者列入參考B 本發明的電容器可用於多種最終用途，如：汽車電子零 件、行動電話、電腦（如：顯示器、主機板之類）、消耗性 電子零件’包括TV和CRT、印表機/影印機、電力供應 物、調變解調器、筆記型電腦、光碟驅動器之類。 以下列實例進一步說明本發明’這些實例僅作為本發明 的例子。 測試方法 陽極製造：
第13頁 460414 五、發明說明（ίο) 尺寸-直徑0.197英吋 3.5 Dp 粉末重量= 341毫克 陽極燒結： 1 3 0 0 °C 1 0 分鐘 1 4 5 0 °C 1 0 分鐘 1 6 0 0 °C 1 0 分鐘 1 7 5 (TC 1 0 分鐘 30伏特Ef 陽極化處理： 30 伏特Ef，60°C/0.1% Η3Ρ04電解質 20毫安培/克穩定電流 D C漏失/電容量_ E S R測試 : DC漏失測試- 70% Ef (21 VDC)試驗電壓 充電時間6 0秒鐘 1 0% Η3Ρ04 > 21 °C 電容量-DF試驗： 18% H2S04 > 21 °C 120 Hz 50伏特Ef再次陽極化處理： 50 伏特Ef，60°C/0,1% Η3Ρ04 電解質 2 0毫安培/克穩定電流 DC漏失/電容量-ESR測試： D C漏失測試-
第14頁 _^46041 4 五'發明說明（11) 70% Ef (35 VDC)試驗電壓 充電時間6 0秒鐘 !〇% Η3Ρ04 > 21 °C 電容量-DF試驗： 18% H2S04 > 21 °C 120 Hz 特Ef再攻陽極化處理： 75 伏特 Ef，60°C/0.1% Η3Ρ04 電解質 20毫安培/克穩定電流 DCjj失/雷宄晉-ESR測試： DC漏失測試_ 70% Ef ( 52. 5 VDC)試驗電壓 充電時間6 0秒鐘 10¾ H3P04 > 21 °C 電容量-DF試驗： 18% H2S04 > 21 °C 120 Hz 根據前面所提到的美國專利案第5, 011，742、4, 960, 471 和4, 964, 906號所述程序（茲將其中所述者列入參考），測 定Scott密度、氧分析、磷分析和BET分析。 實例 貫例1 大於10網目的Ta氫化物粒（99. 2克）和約50 ppm氧與22克 Nbd5混合並置於Ta盤中。將盤置於真空熱處理爐中並加熱
第15頁 4 6041 4 五、發明說明（12) °在爐中通以氫氣至μ力大於3 PSi。溫度進— 二=至1 24 0 c並維持3〇分鐘。溫度降低至丨〇5〇 t達6分 J , f所有的氫氣由爐中散出。仍維持1 050 °C時，抽出 爐中的氬氣直到壓力迠jn_4私瓦lL ± 町抽出 m £λΐοη ^ ^ 成為5x10托耳。此時，再於容器中 〇〇毫米氬氣，此爐冷卻至60 π β :爐中移出之前，以數次循環暴於越來 而鈍化此材料，其方法&丁 .诚士 士杜> ^ ^ 繼而古/Γ 如下.爐中充填氬氣至7〇〇毫米， :充填空氣至-大氣壓。4分鐘之後，容器抽真空至ι〇2 托，器再以氬氣充填至60 0毫米’之後以空 一大氣壓並維持4分鐘。容器抽真空至10_ 、 氣氣充填遍毫•，之後以空氣充填至—大耳氣壓'= 器托耳。容器再以氣氣充填至_ 晕未，之後以空氣充填至一大氣壓並維持4分鐘。 j空至…托耳。容器再以空氣充填至一大氣；
:。容器抽真空至1〇-2托耳。容器再以氩氣充填至一：刀 壓並開啟取出樣品。 K 藉由篩過40網目篩網而自组粒吸氣材料中分離 物。此產物的試驗結果如下。 &不產 丸粒於1 3 0 0 °C燒結1 0分鐘並於3 5伏粒士 0 297 巩特成形之CV/克=81， 毫微安培/ CV (DC漏失）= 5. 0 丸粒的燒結密度= 2.7克/立方公分 Scot t密度=0. 9克/立方公分 化學分析（p p m ) ‘460414 五、發明說明（13) 070 H2 = 56 Ti=25 F e = 25 Μη = 1 0 S i = 2 5 Sn= 5 N i = 5 Cr- 1 0 A 1=5 Mo = 25 Mg = 5 Cu = 50 B = 2 Pb = 2 所有其 所有其他者〈測定限度 實例2 樣品1至20是舟滕 示於附表。大部份的實似：：”的樣品’但粉狀_5量 寸列於附表中，如_ 60/U始時輸入的材料的網目尺 目。類似地，—此小於60網目但大於100網 "Ta翁彳卜物#二 材料的尺寸為14/4〇。被標示為 者。' 的吸氣材料大於40網目且顆粒尺寸無上限 樣品丨8使用Nb作為吸氣材料（CPM以N2 00 flaked Nb P:W:L名私銷售的商品）。樣品1 8所用的吸氣材料是經細 _ 分末，其未自最終產物中分離出來。X射線繞射顯 不些吸氣材料仍為Nb形式，但大部份被處理步驟轉變成 Nbt^」和仳0，此處的鈮氧化物材料是心办。 ，品1 5是被壓成接近固體密度並與&在有Ta吸氣材料存 在時反應的Nb2〇5粒。此程序將密實的氧化物粒轉變成Nb〇 低氧化物的多孔小塊狀物。此小塊狀物被燒結成Nb金屬
# 17頁 46041 4 五、發明說明（14) U成陽極錯連接物並使用用於粉末小塊狀物之類似的 ，力成形程序將其陽極化至35伏特。此樣 步驟由Nb2〇5材料便利地將小塊狀物予 ^ 出來自本發明之經壓出和燒結的粉末/丸狀物製 传之％極所具有的高電容量和低Dc漏失情況。取得各樣品 的顯微照月（SEM)。這些照片顯示本發明之氧減少的氧化 鈮的多孔結構。特別地，附圖丸粒外表面的5,〇〇〇倍照 片（樣品15)。附圖2是相同丸粒之丸粒内部的5, 〇〇〇倍照 片。附圖3和4是相同丸粒外表面的！，〇 〇 〇倍照片。附圖5是 樣11的2，0 0 0倍照片，而附圖6和7是樣品4的5 , 0 0 0倍照 片。附圖8是樣品3的2，〇 〇 〇倍照片，而附圖9是樣品6的 2, 0 00倍照片。最後’附圖10是樣品6的3, 〇〇〇倍照片，而 附圖1 1是樣品9的2，〇 〇 〇倍照片。 由此處所揭示的本發明之說明和實施，嫻於此技藝者明 白本發明的其他實施例。申請專利說明書和實例僅作為例 子，本發明的真正目標和精神述於下面的申請專利範圍 中。
第18頁 ’ 460414 五、發明說明（15) 附表 樣品 輸入材料 克 輸入吸氣材料 克 溫度 (°C) 時間 (分鐘） 氩氣壓 1 -40網目經鍛 燒的Nb205 20 (估計） Ta氫化物片 40 (估計） 1250 30 3 psi 2 60/100 m2o5 23.4 Ta氫化物片 65.4 1250 30 3 psi 3 60/100 Nb205 23.4 Ta氫化物片 65.4 1250 30 3 psi 4 100/325 Nb205 32.3 Ta氫化物片 92.8 1250 30 3 psi 5 100/325 Nb205 32.3 Ta氫化物片 92.8 1250 30 3 psi 6 60/100 Nb205 26.124 Ta氫化物片 72.349 1250 90 3 psi 7 60/100 Nb205 26.124 Ta氫化物片 72.349 1250 90 3 psi 8 200/325 Nb205 29.496 Ta氫化物片 83.415 1250 90 3 psi 9 60/100 Nb205 20.888 Ta氫化物片 60.767 1200 90 3 psi 10 60/100 Nb205 20.888 Ta氫化物片 60.767 1200 90 3 psi 11 200/325 Nb205 23.936 Ta氫化物片 69.266 1200 90 3 psi 12 200/325 Nb205 23.936 Ta氫化物片 69.266 1200 90 3 psi 13 200/325 Nb205 15.5 14/40Ta氫化物 41.56 1250 30 3 psi 14 200/325 Nb20; 10.25 14/40Ta氫化物 68.96 1250 30 3 psi 15 Nb205 粒 3.49 14/40Ta氫化物 25.7 1250 30 3 psi 16 200/325 Nb205 13.2 14/40Ta氫化物 85.7 1200 30 3 psi 17 200/325 Nb205 14.94 14/40Ta氮化物 41.37 1200 30 3 psi 18 200/325 Nb2〇5 11.92 N200 Nb粉末 21.07 1200 30 3 psi 19 200/325 Nb205 10 14/40Ta氫化物 69 1250 30 100托耳 20 200/325 Nb205 16 14/40Ta氫化物 41 1250 30 100托耳
第19頁 460414 五、發明說明（16) 樣品 XRX)* 主要1** XRD* 主要2** XRD* 次要l * 0 XRD* 次要2*** 1300°C，35伏特 cv/克 13CKTC，35伏特 毫微安培/cv 1 81297 5 2 NbO,, NbO TaO 115379 1.28 3 NbO】.， NbO TaO 121293 2.19 4 113067 1.02 5 145589 1.42 6 17793 12.86 7 41525 5.63 8 17790 16.77 9 Nb〇!., NbO Ta2〇5 63257 5,17 10 NbOj.! NbO T&2〇5 69881 5.5 11 NbOLI NbO Ta2Oj 61716 6.65 12 NbO,., NbO Ta205 68245 6.84 13 NbO〇.v NbO TaO NbO, 76294 4.03 14 NbO〇.7 NbO TaO Nb02 29281 21.03 15 70840 0.97 16 Nb02 NbO„.7 TaO NbO 5520 34.33 17 6719 38.44 18 Nb NbO,., NbO 25716 4.71 19 108478 1.95 20 10604& 1.66 * X射線繞射分析結果。 * * 主要1和2代表主要组份，此以重量表示。 *木* 次要1和2代表第二種組份，此以重量表示。 樣品11和1 2的輸入材料相同。樣品2和3的輸入材料相 同。 樣品6和7的輸入材料相同。樣品9和1 0的輸入材料相 同。
O:\60\60466.PTD 第20頁

Claims (1)

  1. 88116(^860 41 4^- 月 曰 _Α·請鼻利蔌1 1. 一種至 吸氣材料存 吸氣材料的 度，以形成 2. 根據申 五氧化鈮。 3. 根據申 氧化物是銳 4 .根據申 氧化物的銳 5. 根據申 氧化物之氧 6. 根據申 氧化物具有 7. 根據申 氣化物的孔 _騎·根據中 # 1 0托耳 _.根據中 年 #正1 WE\ h 3. -9 少部分還原鈮氧化物的方法，其中，包含在有 在時，於能夠使得鈮氧化物中的氧原子轉移至 環境中，熱處理此鈮氧化物達足夠的時間和溫 氧減少的銳氧化物。 請專利範圍第1項之方法，其中，鈮氧化物是 其中 請專利範圍第1項之方法 低氧化物。 請專利範圍第1項之方法 和氧之原子比是1 :低於2 請專利範圍第1項之方法 含量低於使銳完全氧化的化學量 請專利範圍第1項之方法，其中 微多孔結構。 請專利範圍第1項之方法，其中 隙體積50%。 請專利範圍第1項之方法，其中 至2 0 0 0托耳。 請專利範圍第1項之方法，其中 其中 其中 氧減少的鈮 氧減少的鈮 氧減少的鈮 氧減少的銀 氧減少的鈮 存在的氫氣 吸氣材料是 ::灌製成陽極時的電容量至少7 5，0 0 0 CV /克的鈮 材 _〇.根據申請專利範圍第1項之方法，其中，丨是氫氣
    1.根據申請專利範圍第1項之方法，其中，吸氣材料是
    I O:\60\60466.ptc 第1頁 2001.03. 08. 022 460414 _案號88116008_年月 六、申請專利範圍 在製成陽極時的電容量由100, 〇〇〇 W/\ 至200,000 CV / 克的鈮吸氣材料。 12. 根據申請專利範圍第1項之方法，其中，該熱處理是 於1000 °C至1500 °C進行10至90分鐘。 13. 根據申請專利範圍第1項之方法，其中，該吸氣材料 在熱處理步驟之前與鈮氧化物均質化。 14. 根據申請專利範圍第1項之方法，其中，吸氣材料是 片狀的鈮吸氣材料。 15. 根據申請專利範圍第1項之方法，其中，熱處理之 後，吸氣材料形成氧減少的鈮氧化物。 1 6.根據申請專利範圍第1項之方法，其中，吸氣材料是 含鎂的吸氣材料。 17.根據申請專利範圍第1項之方法，其中，吸氣材料包 含氫化钽顆粒。 1 8.根據申請專利範圍第1項之方法，其中，吸氣材料包 含组、說或二者。 1 9.根據申請專利範圍第1項之方法，其中，吸氣材料是 1 4 / 4 0網目氩化组顆粒。 20. 根據申請專利範圍第1項之方法，其中，該吸氣材料 是電容器級材料。 21. —種鈮氧化物，其鈮與氧之原子比為1 :低於2. 5的 親氧化物。 2 2 .根據申請專利範圍第2 1項之鈮氧化物，其中，比例 是1 :低於2 . 0。
    O:\60\60466.ptc 第2頁 2001.03. 08. 023 46041 4 _MM 88116008 —分- 修正丨 六、申請專利範圍 2 3 .根據申請專利範圍第2 1項之鈮氧化物 是1 :低於1. 5。 Μ 其中，比例 2 4 .根據申請專利範圍第2 1項之鈮氧化物，其中，比例 是1 : 1. 1。 2 5 .根據申請專利範圍第2 1項之鈮氧化物，其中，比例 是1 : 0. 7。 2 6 .根據申請專利範圍第2 1項之鈮氧化物，其中，比例 是1 : 0· 5。 2 7.根據申請專利範圍第2 1項之鈮氧化物，其中，該鈮 氧化物具有多孔結構。 2 8.根據申請專利範圍第2 1項之鈮氧化物，其中，該鈮 氧化物具有由0. 1至1 0微米孔洞的多孔結構。 2 9 .根據申請專利範圍第2 1項之鈮氧化物，其中，該鈮 氧化物包含NbO、NbO0 7、NbOu或它們的組合。 30.根據申請專利範圍第21項之鈮氧化物，其中，該鈮 氧化物形成電容量高至300, 000 CV/克的電解用電容器陽 極。 3 1.根據申請專利範圍第2 1項之鈮氧化物，其中，另包 含氮。 3 2 .根據申請專利範圍第3 1項之鈮氧化物，其中，該氮 的存在量由100 ppm至30，000 ppm 。 3 3 .根據申請專利範圍第2 1項之鈮氧化物，其中，該鈮 氧化物被製成電解用電容器陽極，該陽極的電容量由 1，0 0 0 至3 0 0, 0 0 0 CV / 克。
    0:\60\60466：ptc 第3頁 2001.03. 08.024 460414 _案號 88116008 年
    六'申請專利範圍 3 4 .根據申請專利範圍第3 3項之鈮氧化物，其中，該電 容量由60, 000至200, 000 CV /克的電解用電容器陽極。 35.根據申請專利範圍第33項之鈮氧化物，其中，該陽 極的DC漏失由0.5至5毫微安培/CV。 3 6 .根據申請專利範圍第2 1項之鈮氧化物，其中，該鈮 氧化物包含結節狀、片狀、角形或它們的組合。 37. —種電容器，其中包含根據申請專利範圍第21項之 說氧化物。 38. —種電容器，其中包含根據申請專利範圍第33項之 說氧化物。 3 9 .根據申請專利範圍第2 1項之鈮氧化物，其中 氧化物的燒結溫度是1 2 0 0 °C至1 7 5 0 °C。 4 0 .根據申請專利範圍第2 1項之鈮氧化物，其中 氧化物的燒結溫度是1 2 0 0 °C至1 4 5 0 °C。 4 1 .根據申請專利範圍第3 7項之電容器 由 1,0 0 0 CV / 克至 3 0 0, 0 0 0 CV / 克。 4 2 .根據申請專利範圍第3 7項之電容器 由 6 0,0 0 0 CV/克至 2 0 0,0 0 0 CV/ 克。 4 3 .根據申請專利範圍第3 7項之電容器 由0. 5至5毫微安培/CV。 44. 一種製造電容器陽極的方法，包含a)製造鈮氧化物 丸粒及在在有吸氣材料存在時，於能夠使得鈮氧化物中的 氧原子轉移至吸氣材料的環境中，熱處理此丸粒達足夠的 時間和溫度，以形成包含此丸粒的電極體，其中，此丸粒 該鈮 該鈮 其中，電容量 其中，電容量 其中，DC漏失
    O:\6O\60466.ptc 第4頁 2001.03. 08.025 460414 年 月，曰 _ 案號 88116008 六、申請專利範圍 ____ 包含氧減少的鈮氧化物，和b)對•猛9體施以陽極1¾ 理，形成該電容器陽極。 __ 4 據申請專利範圍第44項之方法，其中，該氣_是 i 。 響丨 據申請專利範圍第44項之方法，其中，該吸氣材 料ϋ、鈮或二者。 47.根據申請專利範圍第44項之方法，其中，該吸氣材 料是鈮。 4 8.根據申請專利範圍第4 4項之方法，其中，該氧減少 的銳氧化物之銳和氧的原子比是1 :小於2 . 5。
    O:\6O\60466.ptc 第5頁 2001.03.08.026
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