CN100404463C - 基于低氧化铌的烧结体 - Google Patents
基于低氧化铌的烧结体 Download PDFInfo
- Publication number
- CN100404463C CN100404463C CNB2004100900035A CN200410090003A CN100404463C CN 100404463 C CN100404463 C CN 100404463C CN B2004100900035 A CNB2004100900035 A CN B2004100900035A CN 200410090003 A CN200410090003 A CN 200410090003A CN 100404463 C CN100404463 C CN 100404463C
- Authority
- CN
- China
- Prior art keywords
- sintered compact
- moles
- niobium
- nbo
- niobium suboxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
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- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000010955 niobium Substances 0.000 title claims abstract description 45
- 229910052758 niobium Inorganic materials 0.000 title claims abstract description 44
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 239000007784 solid electrolyte Substances 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 14
- 239000002243 precursor Substances 0.000 claims description 2
- 238000007669 thermal treatment Methods 0.000 claims 1
- 239000003990 capacitor Substances 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 description 12
- 239000002184 metal Substances 0.000 description 12
- 239000000395 magnesium oxide Substances 0.000 description 10
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 10
- 239000007789 gas Substances 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- HFLAMWCKUFHSAZ-UHFFFAOYSA-N niobium dioxide Inorganic materials O=[Nb]=O HFLAMWCKUFHSAZ-UHFFFAOYSA-N 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 239000011733 molybdenum Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 229910052715 tantalum Inorganic materials 0.000 description 3
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 239000008246 gaseous mixture Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000006259 organic additive Substances 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 238000007569 slipcasting Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 241001329471 Mycobacterium phage Rich Species 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052728 basic metal Inorganic materials 0.000 description 1
- 150000003818 basic metals Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000005518 polymer electrolyte Substances 0.000 description 1
- 229910021426 porous silicon Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
- H01G9/052—Sintered electrodes
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- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
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- Power Engineering (AREA)
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- Microelectronics & Electronic Packaging (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Powder Metallurgy (AREA)
Abstract
具有高耐化学性的烧结体,含有30到100摩尔%的NbOx和70到0摩尔%的MgO,其中0.5<x<1.5,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
技术领域
本发明涉及一种基于低氧化铌的烧结体,特别是烧结成形体,由于他们耐化学性,因而用于化学仪器上,并优选用于生产固体电解质电容器的阳极,特别是由低氧化铌制成的烧结阳极。
背景技术
由烧结的低氧化铌细颗粒形成表面积极大的海绵状结构来生产这种类型的阳极。通过电解氧化在此表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二氧化锰或高分子电解质组成的电容器阴极。用于生产此类型的阳极或电容器的方法,以及电容器前体粉末的生产方法,包括在真空或反应气体和/或保护气体中进行一系列的机械和热处理步骤,这必然要承担被某些元素污染的风险,而这些元素对电容器性能有副作用。因此,根据WO02/086923A2,有人提出用于生产阳极的机械处理或热处理的全部设备由铌金属制成或至少用铌金属涂覆。
这种技术的一个缺点是铌金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温处理步骤中,其可能涉及高达1600℃的温度,特别是在此高温下如果低氧化铌和铌金属直接接触时,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,当重复使用时,由于摄入氧,铌金属变得愈加脆弱,因此具有较短的使用寿命。
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低氧化铌和,如果适当,氧化镁的烧结体形成。
此类装置的例子包括:容器、反应器、反应器衬里、磨机衬里、磨球、磨辊、压模、压力机滑块等。
因此,本发明的主题是提供一种低氧化铌基烧结体,这种烧结体包含30到100摩尔%NbOx和高达70摩尔%氧化镁,其中0.5<x<1.5。
该烧结体优选含有分子式为NbOx的低氧化铌,其中0.7<x<1.3。
除不可避免的外来元素杂质之外,低氧化铌和氧化镁的摩尔百分数总量特别优选为100%。特别是,该烧结体应该基本上不含铁、铬、镍、碱金属和卤素。铁、镍、铬、钠、钾、氯和氟杂质的各自量应优选小于10ppm,特别优选小于5ppm,且总计优选小于30ppm。另一方面,杂质或钒、钽、钼和钨的搀杂元素含量为最多几摩尔%,例如5摩尔%以下,是无害的。
本发明的烧结体优选由35到100摩尔%的NbOx和65到0摩尔%的MgO组成。本发明的烧结体更优选地由30到60摩尔%的NbOx和70到40摩尔%的MgO组成,特别优选由45到60摩尔%的NbOx和55到40摩尔%的MgO组成。
本发明优选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优选包括基本上包含均匀富低氧化铌区和富氧化镁区的微观结构,其在至少一个方向上延伸最多1.5μm,优选最多1.0μm。富低氧化铌区优选含有至少95%,特别优选至少99%的低氧化铌。富氧化镁区优选含有最多达99%的氧化镁。
可以利用普通的陶瓷工艺生产本发明的烧结体。例如,可以用轴压和/或等静压法、挤压法、常规无压法或加压粉浆浇铸法或通过注射模塑法进行成形。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合适的有机助剂,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(用于注射模塑法等),其在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处理而不会留下任何残渣,不会改变无机碱粉末的基本性能。在空气中,处理温度不应该超过250℃,优选150℃,以免低氧化铌发生氧化。
在压力成形的情况下,为了改善粉末的流动性,优选在粒化步骤中加入有机助剂。
在粉浆浇铸的情况下,在脱模之后和排出粘结剂之前,必须优选在空气中进行预干燥。而且,在成形步骤之后和排出粘结剂之前,可以利用切屑成形方法例如车削、研磨、钻屑等进行(仔细的)机械处理,以便把坯体制成尽可能接近烧结体要求的最终形状。为了固结成形体,在排出粘结剂和任何预烧结步骤之后,也可以进行此类的处理,而在这种情况下,也可以使用机械加工的方法例如干磨或湿磨。
在保护气氛例如氩气或氩气和通常3到10体积%氢气等的气体混合物下,在气密的炉子中进行烧结,以便平衡掉低氧化铌氧化态的变化。在烧结开始以前,用保护气体吹扫加热炉或抽空,并充满保护气体。为避免要烧结的成形体与炉衬之间的直接接触,将成形体固定在支架/垫片(“烧结辅助装置”)上,该支架/垫片是由在烧结温度下是热稳定和化学稳定的并且不与低氧化物起任何反应的材料制成。已经证明由致密的或多孔的碳化硅制成的烧结辅助装置是特别适合的材料。烧结优选在小于1700℃,特别优选在1550和1650℃之间的温度下进行,以小于10K/分钟的缓慢加热速度加热到烧结温度,在1100℃到烧结温度的较高温度范围优选1到3K/分钟的加热速度,同时在烧结温度下优选保温小于10小时的时间,烧结条件根据成形体要求的致密化和使用的低氧化铌和任选的氧化镁的颗粒大小来定。
用于生产本发明烧结体的原料优选是市场上可买到的比表面积为5到20m2/g的高纯度五氧化二铌。可将这样的五氧化二铌本身或者在流动的氢气中还原形成二氧化铌之后,借助镁蒸汽在950到1150℃温度下还原成低氧化物。这样形成了含有氧化镁杂质的团聚粉末。
将此种粉末研磨之后,可以用来生产本发明的烧结体。如果原料是二氧化铌,则获得含有大约50摩尔%MgO的烧结体。另一方面,如果原料是五氧化二铌,则获得含有大约67摩尔%氧化镁的烧结体。
生产不含有任何氧化镁的烧结体的原料同样优选为具有高比表面积的五氧化二铌细颗粒。五氧化二铌在流动的氢气中在1100到1400℃温度下还原形成二氧化铌。一些二氧化铌在镁蒸气中进一步还原形成铌金属。然后,用酸,例如硫酸,洗掉铌金属中形成的氧化镁。然后在含氢气的气氛中将铌金属与化学计量的二氧化铌一起加热到1100至1600℃,使其转化为低氧化铌NbO。通过相应地改变各个反应组分或混合物的量比可以获得本发明其它组成的烧结粉末。
为了获得比较高密度的烧结体,优选使用细颗粒的团聚粉末,特别优选筛分部分为38μm以下,更优选20μm以下的粉末。
而且,可以用于生产本发明烧结体的粉末非常适合于借助于高温或等离子喷涂来生产涂料,而在这种情况下可以在金属例如铌、钽、钼和/或钨上形成类似于烧结体结构的表面层。在这种情况下,如果合适,可以另外使用在20重量%以下,优选在10和18重量%之间的作为粘结剂的金属铌粉。根据本发明,由铌、钽、钼或钨制成的此类涂覆装置也适合于生产基于低氧化铌的固体电解质电容器。具有涂层的此类金属装置也列入本发明的术语“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
以下通过本发明烧结体的例子来说明用于固体电解质电容器阳极的烧结板的生产。
使用组成为NbO的低氧化铌粉末,其颗粒大小小于38μm,并且按照ASTMB822(Malvern Mastersizer)的粒度分布相当于D10值为2.8μm,D50值为11.4μm和D90值为25.2μm。通过筛选粒化和滚光处理可以改善粉末的流动性,而不需要其它的添加剂就能均匀装入压模中。使用边长为125毫米的正方形孔的硬金属压模。将粒化的粉末输入模具中并且在2kN/cm2下压实。在脱模之后,将外形尺寸大约为125×125×15mm3的压制体与塑料薄膜熔接并且进一步在200兆帕下等压压实。获得大约为122×122×13mm3的压制体。在常规的铣机上加工此压制体,将其加工成带有底部和边缘的盘状部件,其周边高度为13毫米,且壁厚为5毫米。
不需要在SiC容器内进一步预处理,将加工的坯体部件放入用石墨电阻加热的气密加热炉中,并烧结。在烧结开始时,抽空加热炉,并充满含有97体积%的氩气和3体积%的氢气的气体混合物。加热程序按照10K/分钟的加热速度加热到500℃,以5K/分钟的加热速度加热到1100℃,然后以2.5K/分钟的加热速度加热到1600℃,在1600℃下保温3小时,以5K/分钟的可控冷却速度降至800℃,接着自由冷却至低于150℃。这时从加热炉中移出的成形部件的密度为6.9克/厘米3,且维氏硬度HV10为14Gpa。可以任选地对内部和/或外部再加工,以便获得预定的几何尺寸和表面结构。
Claims (11)
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的烧结体,由35到100摩尔%的NbOx和65到0摩尔%的MgO组成,其中0.5<x<1.5。
4.根据权利要求1或2的烧结体,由45到60摩尔%的NbOx和55到40摩尔%的MgO组成,其中0.5<x<1.5。
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分子式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1.5μm。
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容器阳极的烧结板形式。
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1到7之一的烧结体制成的设备对电容器前体进行机械处理和热处理。
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之一的烧结体形式的由低氧化铌粉末制成的阳极压制体放置在烧结板上并烧结。
10.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。
11.根据权利要求1到7之一的烧结体的用途,作为生产电容器用的低氧化铌粉末的惰性设备。
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