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基于低氧化铌的烧结体

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CN100404463C
CN100404463C CN 200410090003 CN200410090003A CN100404463C CN 100404463 C CN100404463 C CN 100404463C CN 200410090003 CN200410090003 CN 200410090003 CN 200410090003 A CN200410090003 A CN 200410090003A CN 100404463 C CN100404463 C CN 100404463C
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sintered
bodies
based
niobium
suboxide
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CN 200410090003
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CN1607197A (zh )
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C·施尼特尔
G·维廷
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H.C.施塔克股份有限公司
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Abstract

具有高耐化学性的烧结体,含有30到100摩尔%的NbO<sub>x</sub>和70到0摩尔%的MgO,其中0.5<x<1.5,以及它们在生产固体电解质电容器中的用途,特别是在生产由低氧化铌制成的烧结阳极中的用途,在生产低氧化铌和在化学仪器中的用途。

Description

基于低氧化铌的烧结体

技术领域

本发明涉及一种基于低氧化铌的烧结体,特别魏结成形体,由于他们耐 化学性,因而用于化学仪器上,^K^于生产固体嫌质电織的阳极,特 别是由低氧化铌制成的烧结阳极。

背景技术

由烧结的〗旗化鄉颗粒形戯面积极大的海绵機构来生产这种鄉的 阳极。舰柳氧化在雌面上形成介电五氧化二铌层,并且在五氧化二铌层 上形成可由】化锰或高舒柳质,的电容辦月极。用于生产此鄉的阳

tM电容器的方法,以及电容器前体粉末的生产方法,包括在真空或te气体

禾0/或{,气体中进行一系列的«和热处理步骤,这必然要承担被某些元素污 染的风险,而这些元素对电容縱能有副作用。因此,根据WO02/086923A2, 有A^出用于生产阳极的^M或热处理的,设备由铌金属制成或至少用 铌金属涂覆。

这种技术的一错点是f^属是一种高温下会吸收氧的获氧材料。因此, 在生产低氧化铌阳极的高赚理步骤中,其可能涉及高达1600"的驗,特别 是舰高温下如果低氧化铌和Kg^属直^to时,带来的高风险是以无法控制 的方式从低氧化铌中取出氧。而且,当重复舰时,由于MA^t,链属变得 舶B脆弱,因此具有TO的^fflg。

发明内容

根据本发明,现建议用于生产此类阳极的装置应由基于^^化铌和,如果 适当,氧化镁的烧结体形成。

此类装置的例賴括:織、腿器、^^g^寸里、磨机衬里、磨球、磨 •、压模、压力机微等。

因此,本发明的iSJUIft—州氏氧化^S^结体,这f^结体包含30 到100摩尔。/。NbOx和高达70摩尔%氧化镁,其中0.5<x<1.5。

,结体tt^含有^F^J NbOx的《琉化铌,其中0.7<x<l .3 。除不可避免的外来元素杂质之外,低氧化^卩氧化镁的摩尔百分数总量特

另lj雌为100%。特别是,繊结体应该基本上不含铁、铬、镍、齢属和卤 素。铁、镍、铬、钠、钾、氯和,质的各自量应优选小于10ppm,特别« 小于5ppm,且总计雌小于30ppm。另一方面,杂质或钒、钽、钼和钩的搀 杂元素含量为最多几摩尔。/。,例如5摩尔%以下,是无害的。

本发明的烧结体tti^由35到100摩尔%的Nba和65到0摩尔%的MgO 组成。本发明的烧结体更,地由30到60摩尔%的N1A和70到40摩尔% 的MgO组成,特别优选由45到60摩尔%的NbOjn 55到40摩尔%的MgO 雖

本发明«的烧结体的孔隙率小于30体积%,特别优选小于20体积%。

根据本发明,含有氧化镁的烧结体ifc^包括基本上包含均匀富低氧化铌区

和富氧化镁区的微见结构,絲至少一个方向上延伸最多1.5 ii m,鶴最多1.0 txm。富低氧化铌区优选含有至少95%,特别,至少99%的低氧化铌。富氧 化镁区ttt^含有最多达99%的氧化镁。

可以利用普通的陶紅艺生产本发明的烧结体。例如,可以用轴压禾D/或等 静压法、挤压法、常规班法鄉压麟練法^131細莫塑法进行成形。

根据使用的方法,可以利用烧结技术中本来已知的方式向粉末中加入^ii的有

机助剂,例如PVA、 PEG等(用于压制法),市场上可买到的用于此目的的 蜡或塑化剂(用于糊模塑法等),^E模制之后可以被排出(粘结剂排出), 在空气、保护气体下或在真空中进行热M而不会留下ft^残渣,不会改变无

机^T分末的基本性能。在空气中,处理ffi不应iMi!25(TC, «150°C, 以免《P^化铌发生氧化。

鄉力成形的情况下,为了改善粉末的流动性,雌在粒化步骤中加入有 ,剂。

在«,的情况下,在脱模之后和排出粘结剂之前,必须,在空气中

进itf页干燥。而且,在成形步mt后和排出粘结齐y^前,可以利用切屑成形方 法例如车削、研磨、钻屑等进行(仔细的)ww,以便把坯体制^可能

^fi^体要求的最终形沃。为了固结^体,在排出粘结剂和任何预烧结步

mt后,也可以进行此类的处理,而在这种瞎况下,也可以iMIW加工的方 、,咖干磨或湿磨。胶150 g,己烷:醋酸乙酯=2: 1),得到呈褐色粉末的5-氟-2-巯基苯并咪唑(5.93 g,収率79 %)。 制造例61-叔丁氧基羰基-4-[2-(5-氟苯并咪哇-2-基硫代)乙基]哌嗪的制造: 在THF(36 mL)中溶解l-叔丁氧基羰基-4-(2-羟乙基)哌嗪(6.00 g, 26.05 mmol),加入三乙胺(3.43g, 33. 90 mmol) 、 4-二甲基氨基吡啶(159 mg, 1. 30 mmol) 后,在冰冷却下滴入甲磺酰氯(3.58 g, 31.25 ramol)的THF (9mL)溶液。搅拌1 小时后过滤反应液,减压浓縮滤液,在DMF(90 mL)中溶解所得残渣。在室温一边 搅拌, 一边依次加入5-氟-2-巯基苯并咪唑(4.82g, 28.66画o1)、碳酸钾(5.40g, 39. 07咖ol)以及18-冠醚-6(688 mg, 2. 60 mmol),在8(TC搅拌2小时。减压浓縮 反应液,在所得残渣中加入水,再用醋酸乙酯萃取,用水、饱和食盐水洗浄有机层。 用无水硫酸钠干燥后,用硅胶柱色谱法(硅胶150 g,己烷:醋酸乙酯=2: 1~1:1〜1: 2)精制减压浓缩所得残渣,得到1-叔丁氧基羰基-4-[2-(5-氟苯并咪唑-2-基硫代)乙基]哌嗪(7.28 g,収率73 %)。'H-纖(400MHz, CDC13) S: 1.49 (9H, s), 2.63 (4H, t, J = 4. 9Hz), 2.94 (2H, t, J = 5.9 Hz), 3.29 (2H, t, J = 5. 9 Hz), 3.58 (4H, t, J = 4. 9 Hz), 6.93 (1H, td, J=9.2, 2.5Hz), 7.19 (1H, dd, J = 9.2, 2.5Hz), 7.40 (1H, dd, J = 9. 2, 4. 9 Hz). 实施例61-[2-(5-氟苯并咪唑-2-基硫代)乙基]哌嗪'3三氟醋酸盐的制造: 在冰冷却并搅拌下,于30分钟之内,在三氟醋酸(17mL)中加入、溶解1-叔丁 氧基羰基-4-[2-(5-氟苯并咪唑-2-基硫代)乙基]哌嗪(6.50 g, 17.08mrno1)。返回 至室温搅拌30分钟后,加入乙醚以及己烷,过滤分离所生成的固形物。用乙醚将 其洗浄,得到呈褐色粉末1-[2-(5-氟苯并咪唑-2-基硫代)乙基]哌嗪'3三氟醋酸 盐(10.50 g,収率99 %)。 mp 127. 7 - 129. 3 。CIR(KBr): 3143, 3032, 2731, 1789, 1747, 1660 (cnf1).'H-NMR(400MHz, DMSO-d6) S : 3.29-3.47 (8H, m)' 3.48 (2H, t, J = 6.6Hz), 3.62 (2H, t, J = 6. 6 Hz), 7.03 (1H, t, J = 9. 0 Hz), 7.32 (1H, d, J = 9. 0 Hz), 7.48 (1H, dd, J=9.0, 4.4 Hz), 9.36 (2H, br), 13.76 (3H, br). 制造例7以下,iM在io和i8重ly。之间的作为粘结剂的金属铌粉。根据本发明,由 铌、钽、钼或钩制成的此麟覆驢舰舒生产基于低氧化铌的固体电解质 电容器。具有涂层的此,属装置也列x^发明的术语"烧结体"之内,所述 涂层的结构与烧结体的结构类似。具体实施方式生产实施例以下aa本发明烧结体的例子来说明用于固体^质电,阳极的烧结板的生产。使用组成为NbO的低氧化fg^末,其颗粒大小小于38 u m,并且按照ASTM B822 (MalvemMasterei2效)的粒度分布相当于D10值为2.8iim, D50值为11.4 y m和D90值为25.2 n m。 ilil筛选粒化,光M可以改善粉末的流动性, 而不需要其它的添加剂就能均匀駄压模中。4顿边长为125毫米的正方形孔 的石脸属压模。将粒化的粉末输入模具中并且在2kN/cm2下压实。在脱模之后, »卜形尺寸大约为125xl25xl5mm3的压制^塑料薄^)^并M—步在200 兆帕下等压压实。获得大约为122xmxl3mirf的压制体。在常规的铣tLh力口 工雌制体,将其加工成带有底部和纖的盘状部件,其周边高度为13毫米, 5W为5毫米。不需要在Sf容器内进一步预鹏,将加工的坯体部件^A用石墨电鹏1J 热附密加热炉中,并麟。^^开始时,,•,并充满含有97條% 的氩气和3 #|只%的氢气的气体混^1。加热HJ^照10K/5H中的加热iM加 热到5(KTC,以5K/併中的加热棘加热到110(TC,然后以2.5K/射中的加热速 戯B热到16(XTC ,在16(KTC下保温3小时,以5K/併中的可控糊敏降至800 °C,接着自由斛瞎低于15(TC。这时抛B热炉中移出的鹏部件的密度为6.9 穷棘3,且维氏S艘HV10为14Gpa。可以任iiiW内部柳或外部再加工, 以便获得?页定的几何尺寸和表面结构。

Claims (10)

1. 烧结体,含有30到100摩尔%的NbOx和70到0摩尔%的MgO,其中0.5<x<1.5,其特征在于孔隙率小于30体积%。
2. 根据权利要求1的烧结体其特征在于孔隙率小于15体积%。
3. 根据权利要求1或2的鹏体由35至IJ100摩尔。/。的NbOx和65到0 摩尔y。的MgO组成,其中0.5^<1.5。
4. 根据权利要求1或2的麟体,由45到60摩尔o/o的Nba和55到40 摩尔%的MgO组成,其中0.5<x<l .5 。
5. 根据权利要求1到4之一的烧结体,其特征在于它含有的低氧化铌具 有肝式NbOx,其中0,7〈x〈1.3。
6. 根据权利要求1到5之一的烧结体,其特征在于含有均匀的富NbOx 区和富MgO区的微观结构,其在至少一个方向上延伸最多1.5 ii m。
7. 根据权利要求1到6之一的烧结体,其为用于固体电解质电織阳 极的烧结板形式。
8. 生产具有低氧化铌阳极的固体电解质电容器的方法,其特征在于至少部分使用由权利要求i到7之一的烧结体制成的设备对电鄉前体进行m^处理和热处理。
9. 根据权利要求8的方法,其特征在于将以权利要求1到7之一的烧根据权利要求1到7之一的烧结体的用途,用作化学仪器中的耐化学的元件。
10.根据权利要求1到7之一的烧结体的用途,作为生产电WII用的低 氧化铌粉末盼隋性设备。
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