CN1200312A - 镍粉及其制备方法 - Google Patents
镍粉及其制备方法 Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 147
- 238000004519 manufacturing process Methods 0.000 title description 2
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 43
- 239000002131 composite material Substances 0.000 claims abstract description 36
- 239000004020 conductor Substances 0.000 claims abstract description 33
- 239000000919 ceramic Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 24
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 23
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims abstract description 23
- 150000002604 lanthanum compounds Chemical class 0.000 claims abstract description 10
- 150000002816 nickel compounds Chemical class 0.000 claims abstract description 10
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 150000001845 chromium compounds Chemical class 0.000 claims abstract description 6
- 239000011651 chromium Substances 0.000 claims description 15
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 12
- 229910052804 chromium Inorganic materials 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 10
- 239000000758 substrate Substances 0.000 claims description 8
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 238000005245 sintering Methods 0.000 abstract description 31
- 239000000843 powder Substances 0.000 abstract description 15
- 150000001875 compounds Chemical class 0.000 abstract description 12
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 abstract description 5
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 abstract description 2
- 229910000423 chromium oxide Inorganic materials 0.000 abstract description 2
- 230000000977 initiatory effect Effects 0.000 abstract 2
- 230000003111 delayed effect Effects 0.000 abstract 1
- 230000008602 contraction Effects 0.000 description 15
- 239000000243 solution Substances 0.000 description 13
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
- 238000010276 construction Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
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- 238000005118 spray pyrolysis Methods 0.000 description 5
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- 238000005979 thermal decomposition reaction Methods 0.000 description 4
- 238000012932 thermodynamic analysis Methods 0.000 description 4
- 241000877463 Lanio Species 0.000 description 3
- 208000037656 Respiratory Sounds Diseases 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000032798 delamination Effects 0.000 description 3
- 239000000428 dust Substances 0.000 description 3
- 229910000765 intermetallic Inorganic materials 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 150000002815 nickel Chemical class 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
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- 150000007942 carboxylates Chemical class 0.000 description 2
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- 238000009616 inductively coupled plasma Methods 0.000 description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 2
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 2
- 238000009766 low-temperature sintering Methods 0.000 description 2
- 150000002736 metal compounds Chemical class 0.000 description 2
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- SWELZOZIOHGSPA-UHFFFAOYSA-N palladium silver Chemical compound [Pd].[Ag] SWELZOZIOHGSPA-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000011265 semifinished product Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910017563 LaCrO Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000004523 agglutinating effect Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910002064 alloy oxide Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Inorganic materials [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- CSSYLTMKCUORDA-UHFFFAOYSA-N barium(2+);oxygen(2-) Chemical compound [O-2].[Ba+2] CSSYLTMKCUORDA-UHFFFAOYSA-N 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
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- 238000007796 conventional method Methods 0.000 description 1
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- 239000013078 crystal Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
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- 238000004993 emission spectroscopy Methods 0.000 description 1
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- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000013528 metallic particle Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
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- 230000001105 regulatory effect Effects 0.000 description 1
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- 238000003980 solgel method Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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- H01G4/00—Fixed capacitors; Processes of their manufacture
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23D—ENAMELLING OF, OR APPLYING A VITREOUS LAYER TO, METALS
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Abstract
一种在至少其部分表面上具有含镧和镍,及视具体情况而定含铬的氧化物的复合氧化物层的镍粉。制造该镍粉的方法包括下列步骤:使含至少一种可热分解的镍化合物和至少一种可热分解的镧化合物及视具体情况而定含至少一种可热分解的铬化合物的溶液成为细液滴;然后在高于这些化合物的分解温度的温度下加热该液滴而制成镍粉,同时将含镧和镍及铬的氧化物(当存在时)的复合氧化物层沉积在该镍粉表面周围。该镍粉适用于与多层元件的未焙烧半成品板共焙烧的导体糊,因为该粉末的烧结开始温度被有效地推迟到陶瓷半成品板的烧结开始温度左右,由此避免了因过烧结而引起的问题。
Description
本发明涉及一种适用于厚膜导体糊的新型镍粉及其制备方法,还涉及采用此镍粉的导体糊、包含用此糊构成的导体的多层电子元件或多层基片。
在电子工业领域中,一直用厚膜糊,如导体糊和电阻糊来生产电子电路和元件,如电阻、电容及集成电路组件。这种厚膜糊是这样制成的:将导电粉末,如金属、合金或金属氧化物,视具体情况而定与玻璃质粘合剂或其它添加物一起在有机载体中均匀混合和分散而制成一种糊浆。在将其涂于基片上后,在高温下焙烧,以形成导体膜或电阻膜。
多层陶瓷电子元件,如多层电容器或多层电感器和多层陶瓷基片一般是这样制成的:将未焙烧的陶瓷半成品板(比如是用介电材料或磁性材料制成的板)和内导体糊层交替叠放而形成多层体,然后将此多层体共焙烧。迄今为止一直主要用贵金属,如钯、银-钯和铂作内导体。但近年来,由于节约资源的要求和解决起因于钯或银-钯的焙烧过程中的氧化膨胀的,诸如脱层、裂纹及其它不利现象之类的问题的需求,基底金属,如镍已引起了注意。
在这些多层元件和多层基片中,构成多层结构的层的数目呈增加的趋势。如,已制成有数百层的多层结构的多层电容器。这就产生了这样的需求:减少每个陶瓷层的厚度及进而减少每个内导体层的厚度。比如,当该陶瓷层的厚度为约3μm时,要求内导体厚度不大于1μm,更好是约0.5μm,因为该厚度大于上述值时,该层制品的中心部位厚,导致结构缺陷的产生及恶化可靠性。
但采用镍粉形成的常规导体糊存在的问题是在焙烧步骤中过度烧结导致形成了不连续膜的内导体,这使电阻值和裂纹增加,此外,镍粉的集聚导致该导体厚度增大,限制该膜厚度的减小。确切地说,镍粉,尤其是为防止其氧化而在惰性气氛或还原性气氛中焙烧时,在早期就开始烧结,即,甚至在只有相当低的活性的单晶粉末的情况在400℃或更低温度中开始烧结和收缩。另一方面,该陶瓷层开始烧结的温度一般远高于这个温度,比如,在钛酸钡的情况下为约1200℃。因此,镍和陶瓷层,即使在共焙烧时,也不同时收缩,而是将镍膜拉向表面。因此认为,于低温烧结过程中在镍膜中所产生的小孔隙,由于在高温区中进行烧结而趋于变大,而且镍粉的集聚使膜沿厚度方向生长。
为此,为使镍的内导体层厚度减小,需要考虑进一步减小镍粉的尺寸及改善其分散能力,从而将烧结过程中孔隙的形成量减至最小,另外,还使镍层的烧结—收缩行为与该陶瓷层的此行为相一致。
此外,导体层和陶瓷层之间的不一致的烧结一收缩行为,尤其在此膜厚度很大时,是产生结构缺陷,如脱层和裂纹的原因,并导致产率和可靠性下降。
因类似的过度烧结而引起的电阻值增大和形成结构缺陷还在外导体和上述层的共焙烧过程中产生问题。
为将导体的烧结推迟到直至温度达到陶瓷层的烧结开始温度,迄今已作了各种研究。
所推荐的方法的例子有:将金属氧化物颗粒,如氧化钛、氧化锆、氧化钡、或氧化铁的颗粒,或在焙烧时能产生上述氧化物的前体化合物添加到导体糊中,或用上述金属氧化物颗粒或其前体覆盖金属粉末。上述氧化物是绝缘体,而其大量添加导致导电性下降。
此外,大量添加与用于陶瓷层中的陶瓷粉末的组成相同的陶瓷粉末可明显地将导体膜的开始收缩推迟至约800℃。但在此情况下,由于金属粉末本身的烧结未受抑制,所以在约1300℃时的高温烧结导致导体膜的连续性和导电性的损失。
本发明的目在于有效地抑制镍粉在低温的烧结,即使在厚度小的情况下也是如此,以便提供有高导电性的导体膜。
尤其是在与用于多层元件等的未焙烧的陶瓷层共焙烧的导电糊的情况下,本发明的目的在于使镍粉的烧结开始温度尽可能地与陶瓷层的烧结开始温度一致,而又不损失导电性,由此使其收缩行为与陶瓷的收缩行为相近似,以便防止因过烧结引起的导体膜破裂或结构缺陷的产生并能使该膜厚度减小。
本发明的另一目的在于提供一种简单的和经改进的制备上述镍粉的方法。
因此,本发明的一个方面是提供一种具有复合氧化物层的镍粉,该氧化层位于镍粉的至少一部分表面上,并含有镧和镍,此外该镍粉还视具体情况而定含铬的氧化物。
本发明的另一方面是提供一种制备在其至少部分表面上具有包含镧和镍的,复合氧化物层的镍粉的方法,而该镍粉还视具体情况而定含有铬的氧化物,该方法包括步骤:使含至少一种可热分解的镍化合物和至少一种可热分解的镧化合物的溶液,或含至少一种镍化合物,至少一种镧化合物,和至少一种可热分解的铬化合物的溶液形成细的液滴;在高于该镍化合物和镧化合物的分解温度的温度下,或在铬化合物存在时,在高于该镍化合物,镧化合物和铬化合物的分解温度的温度下加热此液滴,以制备镍粉末,同时,使含镧和镍的复合氧化物层,或该氧化物层和铬的氧化物沉积在该镍粉表面周围。
此外,本发明还提供含上述镍粉的导体糊、各含用上述导体糊构成的导体层的多层陶瓷电子元件和多层陶瓷基片。
该复合氧化物可覆盖镍粉的表面,或可以高浓度集聚在该镍粉的表面上和/或集聚在表面周围,而在复合化合物存在情况下所要求的是以一种能够有效地推迟镍粉烧结的形式集聚在该表面周围。为防止镍金属颗粒之间的接触,人们认为最有效的作法是用该复合氧化物覆盖其全部表面。但是,以按用途、焙烧气氛、所要求的性能等确定的有效量存在于该镍粉表面的复合氧化物,即使全部表面不总是被复合氧化物覆盖,也足以达到预期的效果。
该复合氧化物至少含镧和镍,其例子包括:具有LaNiO3、La2NiO4、La3Ni2O7等结构的化合物。
由于这些化合物是陶瓷质的,故其烧结行为与未烧结陶瓷板的行为类似。对于其表面上有此复合氧化物的镍粉而言,低温区的烧结被抑制,而且根据该氧化物的量,可将烧结开始推迟至该陶瓷的烧结开始温度附近,而防止过烧结。这就可防止导体电阻率的增加,破裂、膜厚度的增加、脱层及其它的,起因于共焙烧时,该导体层和陶瓷层之间不一致收缩的其它不利现象,而实现具有小厚度和良好的导电性和粘附性的镍导体的形成。这又能使多层元件等中的导体层厚度减小。
在上述复合氧化物中,尤其是具有钙钛矿结构的LaNio3是一种有良好导电性的导电陶瓷,且其它的复合氧化物也导电。因此,该复合氧化物在不使导体电阻率升高方面远优于常规的烧结阻止剂。
以氧化物的形式,如Cr2O3或LaCrO3,主要存在于该复合氧化物层中的铬被认为能增强延迟烧结开始的效果。
复合氧化物层可用任何方法形成。其例子包括其中用湿法,如溶胶一凝胶法将镧氧化物等沉积在镍粉表面上,再煅烧以便形成复合化合物层的方法;喷雾热解法;和将镍粉和复合氧化物机械地混在一起以便复合氧化物沉积的方法。
本发明的镍粉最好用喷雾热解法生产。如于日本专利公告31522/1988和日本专利公开279816/1994中所述,在喷雾热解法中,将含至少一种金属化合物的溶液雾化以形成细液滴,然后在高于该金属化合物的分解温度的温度下,更好是在该金属熔点左右或更高的温度下加热此液滴,以便该金属化合物热分解,由此沉积该金属或其合金的粉末。
此法可生产有良好结晶性、高密度和高分散性的镍粉,可方便地控制颗粒尺寸、能通过事先将镧化合物等添加于原料镍化合物溶液中以一个步骤制成具有本发明复合氧化物层的镍粉,从而有利地消除了另行提供覆盖步骤的需要。确切地说,因为所得的镍颗粒有良好的结晶性,所以由热分解而沉积的镧或镧的氧化物就被从颗粒的内部挤出,以便在表面附近形成复合氧化物。此外,复合氧化物相当均匀地沉积在表面上,因而,其很少量的使用就足以达到预期的效果。在喷雾热解法中,所形成颗粒的组成基本上与溶液中的金属化合物的组成相对应,从而便于调整该组成,这就使得该方法适于制备本发明的镍粉。
当将铬的化合物加入此原料溶液中时,铬主要以氧化物,或与镧的复合氧化物的形态存在于该复合氧化物层中。在此情况下,认为一部分铬以固溶体形态溶于镍中。
按照本发明的方法,镍的化合物至少是一种可热分解的化合物,它选自硝酸盐、硫酸盐、氯化物、铵合物、磷酸盐、羧酸盐、金属的醇化物、金属的树脂酸盐等。采用复盐或配盐也是可能的。镧和铬的化合物也可从诸如硝酸盐、硫酸盐、氯化物、铵合物、磷酸盐、羧酸盐、金属的醇化物和金属的树脂酸盐、配盐之类的化合物中选择。
将这些金属化合物溶于水、有机溶剂如醇、丙酮或醚,或其混合溶剂以制成溶液,然后通过雾化器,如超声波雾化器或双流体雾化器,使该溶液成为细液滴,然后在超过该金属化合物分解温度的温度下加热此液滴以便进行热分解。这种加热处理最好在镍熔点或更高的温度下进行。然而,低于此熔点约200℃的温度就足以有挤出的效果。尤其是在不要求高密度、均匀的形状等时,该加热温度可比熔点低得多。加热是在基本上不使镍粉氧化的气氛,如还原性的或惰性的气氛,而较好的是含氢或一氧化碳的弱还原性气氛中进行。
其量小到约0.01%(重量)(以镍为基准计,按La2O3折算)的复合氧化物可产生此效果。复合氧化物的量最好不少于0.1%(重量)(以镍为基准计,按La2O3折算)。使用大量的此复合氧化物不会产生问题,因为它是导电的。但是,在用喷雾热解法制备这种镍粉时,量过大的复合氧化物就不易集聚在此镍粉的表面上,从而在阻止烧结的效果方面未产生明显的改进。另外,降低镍的份额导致导电性变差。为此,从实施的观点看,该复合氧化物的量最好是,以镍为基准计,折合成La2O3,高达约50%(重量)。
即使是少量的铬的氧化物也会产生预期的效果。当铬的氧化物的量过大时,则损失可烧结性。因此,以不使镍的烧结性恶化的量添加铬的氧化物。按Cr2O3折算的铬的氧化物的用量最好至多与La2O3的用量相等。
含作为导电组分的本发明镍粉的导体糊可按常规方法将此镍粉在有机载体中均匀混合和分散而制成。若需要,可添加其它的导电粉末,无机粘合剂,如玻璃粉及其它的添加剂。
本发明的镍粉适于具体地说在制造多层元件和多层基片的内、外导体时与陶瓷一起焙烧。但是,它也可用于通常的厚膜导体糊。
参照以下的实施例和对比例,将更详细地描述本发明。实施例1-9
将硝酸镍六水合物溶于水,到镍浓度为50g/升,然后以表1中所规定的量加入硝酸镧,以该镍元素为基准计,折合成La2O3,使其浓度为0.01-20%(重量),以制成原料溶液。
通过超声雾化器使这样制得的原料溶液成为细液滴,然后借助于调节后呈弱还原性的气体作载气将此液滴送入已在电炉中加热至1500℃的陶瓷管中。使液滴在通过加热区的过程中热分解,以制成含镧的氧化物的镍粉末。
此外,将这样制成的粉末分别溶于硝酸中,然后由ICP(感应耦合等离子体)发射光谱测量法确定此粉末中的镧浓度。结果是镧浓度与原料溶液组成中的镧浓度一致。
该粉末的X-射线衍射、在高分辨率FE-SEM(场发射-描扫电镜)下的观察、及电子衍射的结果表明:在该镍颗粒表面上存在LaNiO3、La2NiO4和La3Ni2O7中的至少一种晶体相。对比例1
以与实施例1中相同的方法制备纯镍粉,但不同的是不加镧。
对于实施例1-9中制成的镍粉和不含镧的对比例1的镍粉进行热力学分析(TMA),以评价这些粉末的烧结行为,而后将烧结时的收缩开始温度和烧结时的收缩终止温度归纳于表1中。如从表1中可知,当未加镧时,烧结过程中的收缩于300℃时逐渐开始,而加了镧则使收缩开始温度提高约200-600℃。此外,很明显,收缩的终止被推迟了不小于300℃。实施例10-14
向50g镍/升的硝酸镍六水合物中加硝酸镧,以镍元素为基准计,折成La2O3,其量为0.8%(重量),加硝酸铬,以镍元素为基准计,折成Cr2O3,其量为0.01-0.8%(重量),这些用量被列于表1中,由此制备原料溶液。
以与实施例1中的同样方法制备在其表面上有包含镧、铬和镍的复合氧化物层的镍粉,但不同的是采用上面制备的原料溶液。
用TMA分析法测量收缩开始温度和收缩终止温度,其结果也列于表1中。
表1
加镧量 加铬量 烧结时的收 烧结时的收
缩开始温度 缩终止温度
(重量%) (重量%) (℃) (℃)实施例1 0.01 - 535 880实施例2 0.1 - 600 1000实施例3 0.2 - 635 1000实施例4 0.5 - 640 1000实施例5 0.7 - 640 1000实施例6 0.8 - 810 1000实施例7 4.0 - 810 1100实施例8 7.0 - 850 1250实施例9 20.0 - 900 ≥1300实施例10 0.8 0.01 845 ≥1300实施例11 0.8 0.05 900 ≥1300实施例12 0.8 0.1 920 ≥1300实施例13 0.8 0.5 925 ≥1300实施例14 0.8 0.8 945 ≥1300对比例1 - - 330 600实施例15-17
以与实施例11中的相同方法制备在其表面上具有复合氧化物层的镍粉,但不同的是电炉的温度为1400℃,1300℃或1600℃。
该镍粉的收缩开始温度的TMA分析结果表明分别为900℃、890℃和910℃,所有镍粉的收缩终止温度为1300℃或更高。实施例18
将于实施例3、6、9和11及对比例1中制得的镍粉与有机载体研磨以制备糊浆。将每种糊涂在以BaTiO3为主要组分的陶瓷半成品板上,以便形成镍覆盖量为0.5mg/cm2的导体图形,接着干燥及在1300℃共焙烧。
该导体膜的厚度及电阻率列于表2。
对于采用对比例1中所制成的粉末的导体而言,由于过烧结而出现了破裂,虽然在镍存在的部位处的膜厚为2.0μm,但结构不连续。另一方面,对于实施例3、6、9和11中制成的无过烧结的粉末进行观察,如表2所示,其膜厚度和电阻率都小。尤其是对于其中加了铬的实施例11而言,尽管事实上其膜厚小到0.5μm,但其电阻率值低到20μΩ·cm。
表2
镍粉 焙烧膜厚度 电阻率
(μm) (μΩ·cm)
实施例3 0.8 50
实施例6 0.6 35
实施例9 0.6 55
实施例11 0.5 20
对比例1 2.0 ∞
本发明镍粉的低温烧结可受到抑制,而该镍糊焙烧时的开始收缩可被推迟到大致是陶瓷开始收缩的温度。
因此,尤其是在多层元件和多层基片中,可使镍导体层的收缩行为与陶瓷层的该行为近似,而又不损失导电性。这可防止导体膜破裂和出现结构缺陷,并制成高度可靠的,有高性能的产物,此外,能使内导体层厚度减小,进一步实现减少尺寸,及使构成多层结构的层数增加。
Claims (7)
1、一种在其至少部分表面上具有含镧和镍的复合氧化物层的镍粉。
2、一种在其至少部分表面上具有含镧和镍并含铬的氧化物的复合氧化物层的镍粉。
3、一种制备权利要求1的镍粉的方法,它包括下列步骤:使含至少一种可热分解的镍化合物和至少一种可热分解的镧化合物的溶液成为细液滴;在高于该镍化合物和镧化合物的分解温度的温度下加热此液滴,以制备镍粉,同时在该镍粉的表面周围沉积含镧和镍的复合氧化物层。
4、一种制备权利要求2的镍粉的方法,它包括下列步骤:使含至少一种可热分解的镍化合物,至少一种可热分解的镧化合物和至少一种可热分解的铬化合物的溶液成为细液滴;然后在高于该镍化合物,镧化合物及铬化合物的分解温度的温度下加热此液滴,以制备镍粉,同时在该镍粉表面周围沉积含镧和镍及铬的氧化物的复合氧化物层。
5、一种含有镍粉的导体糊,该镍粉选自在其至少部分表面上具有含镧和镍的复合氧化物层的镍粉及在其至少部分表面上具有含镧和镍及铬的氧化物的复合氧化物层的镍粉。
6、一种包含用权利要求5的导体糊构成的导体层的多层陶瓷电子元件。
7、一种包含用权利要求5的导体糊构成的导体层的多层陶瓷基片。
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JP3772967B2 (ja) | 2001-05-30 | 2006-05-10 | Tdk株式会社 | 磁性金属粉末の製造方法 |
US7767753B2 (en) * | 2004-06-21 | 2010-08-03 | Sekisui Chemical Co., Ltd. | Binder resin composition, paste and green sheet |
US20060169389A1 (en) * | 2005-01-31 | 2006-08-03 | Barber Daniel E | Electrode paste for thin nickel electrodes in multilayer ceramic capacitors and finished capacitor containing same |
JP5246338B2 (ja) | 2009-08-27 | 2013-07-24 | 株式会社村田製作所 | Esd保護デバイスおよびその製造方法 |
KR20140024584A (ko) * | 2012-08-20 | 2014-03-03 | 삼성전기주식회사 | 내부전극용 도전성 페이스트 조성물 및 이를 포함하는 적층 세라믹 전자부품 |
JP7245418B2 (ja) * | 2019-07-09 | 2023-03-24 | 住友金属鉱山株式会社 | 厚膜抵抗体用組成物、厚膜抵抗体用ペースト、および厚膜抵抗体 |
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US3883346A (en) * | 1973-03-28 | 1975-05-13 | Gen Electric | Nickel-lanthanum alloy produced by a reduction-diffusion process |
JPS58171502A (ja) * | 1982-04-02 | 1983-10-08 | Toyota Motor Corp | セラミック―金属複合微粉末体の製造方法 |
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JPH09129028A (ja) * | 1995-11-01 | 1997-05-16 | Daiken Kagaku Kogyo Kk | 無機皮膜を有する金属粉の製造法及び金属粉 |
-
1997
- 1997-05-26 JP JP09149949A patent/JP3137035B2/ja not_active Expired - Fee Related
- 1997-09-23 SG SG1997003504A patent/SG66396A1/en unknown
- 1997-09-23 US US08/933,921 patent/US5871840A/en not_active Expired - Lifetime
- 1997-09-23 TW TW086113816A patent/TW429180B/zh active
- 1997-09-24 CA CA002216457A patent/CA2216457C/en not_active Expired - Lifetime
- 1997-09-24 MY MYPI97004434A patent/MY121682A/en unknown
- 1997-09-25 CN CN97121400A patent/CN1093020C/zh not_active Expired - Lifetime
- 1997-09-25 KR KR1019970048652A patent/KR100259562B1/ko not_active IP Right Cessation
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN100478102C (zh) * | 2000-02-18 | 2009-04-15 | 加拿大电子学粉末公司 | 用作贱金属电极多层陶瓷电容器电极的镍粉 |
CN101062524B (zh) * | 2006-04-27 | 2012-06-27 | 昭荣化学工业株式会社 | 镍粉的制造方法 |
CN101264523B (zh) * | 2007-03-12 | 2011-04-13 | 昭荣化学工业株式会社 | 镍粉及其制法、含有该镍粉的导体糊及使用该导体糊的多层陶瓷电子元件 |
Also Published As
Publication number | Publication date |
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CA2216457A1 (en) | 1998-11-26 |
MY121682A (en) | 2006-02-28 |
CN1093020C (zh) | 2002-10-23 |
JPH10324906A (ja) | 1998-12-08 |
US5871840A (en) | 1999-02-16 |
JP3137035B2 (ja) | 2001-02-19 |
CA2216457C (en) | 2000-09-12 |
KR100259562B1 (ko) | 2000-06-15 |
KR19980086381A (ko) | 1998-12-05 |
TW429180B (en) | 2001-04-11 |
SG66396A1 (en) | 1999-07-20 |
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