CN1289435C - 磁性铁氧体组合物及其生产方法 - Google Patents

磁性铁氧体组合物及其生产方法 Download PDF

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CN1289435C
CN1289435C CNB001285939A CN00128593A CN1289435C CN 1289435 C CN1289435 C CN 1289435C CN B001285939 A CNB001285939 A CN B001285939A CN 00128593 A CN00128593 A CN 00128593A CN 1289435 C CN1289435 C CN 1289435C
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oxide
ferrite composition
ferrite
sintering
ppm
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CN1293169A (zh
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青木卓也
野村武史
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TDK Corp
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Abstract

一种磁性铁氧体组合物,包含Mg、Ni、Cu、Zn、Mn和Li的至少一种并具有在预定范围,例如大于9.7重量ppm至小于96重量ppm内的碳含量。该组合物可用作电感器、变压器、线圈等的磁芯,用于收音机、电视机、通信装置、办公自动装置、配电***电源和其它电子装置,或视频装置或磁盘驱动器或其它电子元件的磁头。

Description

磁性铁氧体组合物及其生产方法
本发明涉及铁氧体组合物及其生产方法。
Mn-Zn铁氧体组合物,Ni-Cu-Zn铁氧体组合物、Mn-Mg-Zn铁氧体组合物和其它磁性铁氧体组合物被广泛用于各种电子器件,例如线圈磁芯、变压器、磁头等。
随着目前电子器件大小和厚度的减小,希望磁性铁氧体组合物的大小和厚度相应的减小。为了同时保持产品的可靠性,要求更高的机械强度和更高的磁性能。
从改进机械强度的观点看,已知使用的方法有热压制造、减小原料粉末的颗粒直径和降低烧结温度以减小晶粒直径或添加各种添加剂以减小晶粒直径。另外,为改进磁性能,已知的方法有添加各种添加剂和最佳化烧结条件。
但是,由于使用热压改进机械强度的方法,生产时间变长,并需要昂贵的设备,这样有成本高的缺点。
另外,采用制造细小原料粉末以提高机械强度的方法,则为减小颗粒直径需要单独的工艺。还有,当生产磁性铁氧体组分时,处理细小原料粉末非常困难。
再者,采用添加各种添加剂改进机械性能的方法有成本高的缺点,在一些情况下平衡各种磁性能变得困难。
还有,采用最佳化烧结条件改进磁性能的方法,则控制烧结气氛、温度升高与降低速率等困难,在一些情况下需要采用新设备并增加其它问题。
应注意到日本未审专利说明书(公开)No.1994-132111公开了在铁氧体烧结体中所含的碳量,但是完全没有说明其控制的问题。另外,实际上所含的碳量通常约为在通过去除粘结剂,然后烧结获得的烧结体中所含的碳量相同的范围(约100ppm),且保证足够的机械强度困难。即,在上述说明书中,将原料粉末通过冷等静压压实,并当赤铁矿料变成尖晶石型铁氧体时在氧排出困难的情况下烧结。所以,烧结前添加到原料粉末中的碳或在加热下分解成碳的还原剂对烧结后相的磁性能有影响。还有,上述说明书完全没有说明剩余碳对强度与磁性能的影响。
本发明的目的是解决在相关技术中的上述问题并提供具有高机械强度和优越磁性能,甚至当尺寸和厚度减小时也如此的铁氧体组合物及其生产方法。
本发明注意到磁性铁氧体组合物中的碳含量并控制它,由此完成了本发明。应注意到在本发明中“磁性铁氧体组合物”包括铁氧体材料和铁氧体烧结体。
本发明磁性铁氧体组合物的特征在于包含Mg、Ni、Cu、Zn、Mn和Li的至少一种并具有小于96重量ppm,较好不大于91重量ppm,更好不大于77重量ppm,最好不大于70重量ppm的碳含量。
该铁氧体组合物除Mg外最好还包含,Cu、Zn、Mn、Ni和Li的至少一种。这种铁氧体组合物的典型例子是Mg-Cu-Zn铁氧体。在这样的铁氧体组合物中,碳含量较好超过9.7重量ppm(大于9.7重量ppm),更好至少10重量ppm,最好至少15重量ppm。另外,在这样的铁氧体组合物中,碳含量较好不大于91重量ppm。
该铁氧体组合物可以是至少含Mn和Zn的铁氧体组合物。这样的铁氧体组合物的典型例子是Mn-Zn铁氧体组合物。在这样一种铁氧体组合物中,碳含量小于52重量ppm,较好不大于50重量ppm,更好不大于45重量ppm。另外,在这样一种铁氧体组合物中,碳含量较好超过9.8重量ppm(大于9.8重量ppm),更好至少10重量ppm,最好至少15重量ppm。
该铁氧体组合物还可含有作为添加成分的选自氧化硅、氧化钙、氧化锡、氧化钛、氧化铌、氧化锆、氧化钒、氧化钼、氧化铋和氧化钽的至少一种氧化物。
还有,除Ni外,该铁氧体组合物可以是含Cu、Zn和Mn的至少一种的铁氧体组合物。这样一种铁氧体组合物的典型例子是Ni-Cu-Zn铁氧体组合物。在这样一种铁氧体组合物中,碳含量小于67重量ppm,较好不大于60重量ppm,更好不大于50重量ppm。最好不大于45重量ppm。另外,在这样一种铁氧体组合物中,碳含量较好超过9.7重量ppm(大于9.7重量ppm),更好至少10重量ppm,最好至少15重量ppm。
本发明磁性铁氧体组合物的生产方法控制吹入烧结炉的气体流量,以使控制该铁氧体组合物中包含的碳量。
另外,调节本发明磁性铁氧体组合物抗弯强度的方法控制磁性铁氧体组合物中包含的碳量。
本发明通过控制磁性铁氧体中的碳含量可改善该磁性铁氧体组合物的机械强度(例如,抗弯强度较好至少8kgf/mm2,更好至少10kgf/mm2),并可提供可靠性高的裂纹或碎屑少的铁氧体组合物。
本发明通过将磁性铁氧体组合物中的碳含量控制到预定范围内可改善抗弯强度并可保持预定组分的磁性铁氧体组合物的高磁导率μ。另外,对于另一组分的磁性铁氧体组合物可改善抗弯强度并保持低的铁芯损耗。
应注意到,烧结后铁氧体组合物中含的碳可认为是碳酸盐材料和/或有机粘合剂中含的碳组分。
本发明铁氧体组合物可用作电感器、变压器、线圈等的铁芯,可用于电子仪器,如收音机、电视机、通信装置、办公自动化装置和配电***电源或者用于电子仪器,如视频装置或磁盘驱动器或其它电子器件的磁头铁芯。
其中,本发明Mg-Cu-Zn铁氧体组合物和Ni-Cu-Zn铁氧体组合物可优选用于电感器,而Mn-Zn铁氧体组合物可优选用于变压器。
在本发明铁氧体组合物的生产方法中,当生产铁氧体绕结体时,可在烧结时按预定的流量将气体吹入烧结炉中并转移粒状材料中所含的碳组分,以使控制烧结后的碳量。所以,可很容易使所获得的铁氧体烧结体的机械强度与磁性能平衡。
本发明调节铁氧体烧结体的抗弯强度的方法可控制通过控制该组合物中的碳量获得的铁氧体烧结体的抗弯强度。这一新的发现由本发明人完成。
本公开涉及日本专利申请No.1999-264775(9月20日申请)包含的内容,特意将其公开全部引入本文供参考。
本发明的目的和特征可由下述优选的实施方案并参考附图清楚地说明。
图1是实施例1-7、参照例1和比较例1的铁氧体烧结体的碳量与磁导率之间的关系图。
图2是实施例1-7、参照例1和比较例1的铁氧体烧结体的碳量与抗弯强度之间的关系图。
图3是实施例8-11、参照例2和参照例3的铁氧体烧结体的碳量与铁芯损耗之间的关系曲线图。
图4是实施例8-11、参照例2和参照例3的铁氧体烧结体的碳量与抗弯强度之间的关系图。
图5是实施例12-16、参照例4和参照例5的铁氧体烧结体的碳量与磁导率之间的关系图。
图6是实施例12-16、参照例4和参照例5的铁氧体烧结体的碳量与抗弯强度之间的关系图。
第一实施方案
第一实施方案的铁氧体烧结体例如可如下生产。
首先,将原料称重并混合,以使具有预定比例的组分并获得原料混合物。
称重通常以1/1000的精度进行。作为混合的方法,例如有使用球磨机的湿混和使用干混机的干混。应注意到,原料的平均颗粒直径最好为0.1-3μm。
除了氧化铁或烧结后成为氧化铁的材料外,本实施方案中的原料混合物还含有选自氧化镁、氧化镍、氧化铜、氧化锌、氧化锰、氧化锂的至少一种氧化物或烧结后成为这些金属氧化物的材料。应注意到,烧结后成为金属氧化物的材料包括金属、碳酸盐、氢氧化物、卤化物等。
本实施方案的铁氧体组合物的组分不特别限制。根据目的可选择各种组分,但最好组分含有作为主成分的Fe2O3和选自MgO、CuO、ZnO、MnO、NiO和Li2O的至少一种氧化物。本实施方案的铁氧体组合物的典型例子是Mg-Cu-Zn铁氧体组台物。
除上述主成分外,本实施方案的原料混合物还可具有添加其中的各种添加剂。
应注意到,本实施方案的原料混合物可含材料杂质元素。作为这些元素有B、Al、Si、P、Ca、Cr、Co、Na、K、S、Cl等。要减小能量损失或对磁性能的作用,最好这些元素的重量比,相对于组合物总量不大于200ppm,但P和B对能量损失或磁性能的影响大,因此,P的重量比,相对于组合物总量最好为0-30ppm,而B的重量比,相对于组合物总量最好为0-50ppm。
接着,将原料混合物预烧,以使获得预烧的材料。进行预烧,以使通过加热使材料分解,使组分均匀化,产生铁氧体,消除烧结引起超细颗粒并使颗粒直径生长到合适的颗粒尺寸,并将原料混合物转变成适合后处理的形式。该预烧最好在700-1000℃的温度下通常进行1-3小时。该预烧可在空气中或在具有比空气含更高氧分压的气氛中或纯氧气氛中进行。应注意到,当在铁氧体组合物中含有添加成分时,主成分与添加成分可在预烧以前或预烧以后混合。
接着,将预烧材料粉磨,以获得粉末材料。进行粉磨是将预烧材料的聚集体粉碎,以生产具有合适烧结性的粉末。当预烧材料形成大块时,将该材料粗磨,然后用球磨机或研磨机等湿磨。进行湿磨直到预烧材料的平均颗粒直径最好为1-2μm。
接着,将粉末材料制粒,以使获得颗粒材料。进行制粒是将粉末材料制成合适尺寸的集聚颗粒,以将其转变成适合成形的形式。作为制粒的方法,例如有压制制粒法或喷雾干燥法等。在本实施方案中,喷雾干燥法常将聚乙烯醇或其它通常使用的粘合剂添加到粉末材料中,然后用喷雾干燥机将其喷雾并在低温干燥。
接着,将颗粒材料成形成预定形状,以获得成形物。作为颗粒材料的成形,例如有干成形、湿成形、挤压成形等,但在本实施方案中,使用将颗粒材料填充到模中,然后压制的干成形法。成形物的形状没有特别的限制,例如可采用环形等。
接着,将成形物烧结,以获得本实施方案组分的铁氧体烧结体。进行烧结是使包含大量气孔的成形物的粉末颗粒在低于熔点的温度下粘合,以使获得致密的烧结体。作为烧结使用的炉子,可采用分批式、推送式、车运式等的一种。
在本实施方案中,在烧结期间例如将空气或其它气体吹入炉中,气体流量较好大于25ml/min到小于5000ml/min,更好为200-40ml/min。
如果吹入炉中的气体的流量太小,烧结后含的碳量趋于变大,而获得的铁氧体烧结体的机械强度变低。再者,如果吹入炉中的气体的流量太大,烧结后含的碳量趋于变得太小,而获得的铁氧体烧结体的磁导率变小。即,烧结同时以预定的流量将气体吹入炉中,可控制获得的铁氧体烧结体烧结后含的碳量并平衡机械强度(抗弯强度)与磁性能(磁导率)。
烧结温度最好为900-1300℃。如果烧结温度太低,不仅烧结趋于不完全,而且烧结后含的碳量趋于变大。烧结时间通常约为1-3小时。烧结可在空气或在氧分压高于空气的气氛中进行。
按照上述方法可获得将碳量控制到合适值的铁氧体烧结体。
铁氧体烧结体的平均晶粒直径最好为1-30μm。如果平均晶粒直径太小,磁滞损失趋于变大,而如果平均晶粒直径太大,涡流电流损失趋于变大。
本实施方案组分的铁氧体烧结体通过将碳含量控制到预定的范围(9.7-96重量ppm)内可改善机械强度并保持高的磁导率。另外,按照本实施方案的方法,通过烧结,同时以预定流量将气体吹入炉中控制碳含量,这样可简单并便宜地生产将烧结后的碳量控制到合适量的铁氧体烧结体。因此,使用该铁氧体烧结体构成电感器磁芯,可获得磁导率优越的、即使很薄也避免了裂纹或碎屑、以及可靠性优越的产品。而且促进产品尺寸的减小和成本的降低。
第二实施方案
第二实施方案的铁氧体烧结体例如可按如下方法生产。
首先,按照与第一实施方案相同的方法。将原料称重并混合成预定的组分比例,以获得原料混合物。应注意到,原料的平均颗粒直径最好为0.1-3μm。
该铁氧体组合物的组分不特别限制。各组分可按照目的来选择。最好,除Fe2O3外,该铁氧体组合物还含有MnO和ZnO。本实施方案的铁氧体组合物的典型例子是Mn-Zn铁氧体组合物。
在这种情况下,该原料混合物含有作为主要成分的氧化铁、氧化锰和氧化锌或烧结后变成这些金属氧化物的材料。应注意到,烧结后变成金属氧化物的材料包括金属、碳酸盐、氢氧化物、卤化物等。
本实施方案的原料混合物最好除上述主成分外,还具有如下添加到其中的添加成分。
添加成分包括至少一种选自氧化硅、氧化钙、氧化锡、氧化钛、氧化铌、氧化锆、氧化钒、氧化钼、氧化铋和氧化钽的氧化物。
最好,添加成分包括至少一种选自如下氧化物的氧化物:转变成50-2000ppm的SiO2的添加量的氧化硅、转变成100-3100ppm的CaO的添加量的氧化钙、转变成不大于8500ppm(不包括0)的SnO2添加量的氧化锡、转变成不大于12000ppm(不包括0)的TiO2的添加量的氧化钛、转变成50-300ppm的Nb2O5的添加量的氧化铌、转变成200-1200ppm的ZrO2的添加量的氧化锆、转变成100-1100ppm的V2O5的添加量的氧化钒、转变成50-310ppm的MoO3的添加量的氧化钼、转变成350-800ppm的Bi2O3的添加量的氧化铋、转变成400-1400ppm的Ta2O5的添加量的氧化钽。通过以这样范围添加这些添加成分,Br(剩磁通密度)减小,ΔB(=Bm-Br)增加,能量损失降低,且磁性能改善。
应注意到,本实施方案的原料混合物可包括在材料中的杂质元素。作为这些元素可有B、Al、P、Cr、Co、Na、K、S、Cl等。要减小能量损失和对磁性能的作用,每种元素的重量比,相对于组合物总量最好不大于200ppm,但P和B对能量损失或磁性能的影响大,因此P的重量比,相对于组合物总量最好为0-30ppm或B的重量比,相对于组合物总量最好为0-50ppm。
接着,按照与第一实施方案相同的方法,将原料混合物预烧,磨粉、制粒并成形,然后烧结,以使获得铁氧体成形物。进而,在本实施方案中,在烧结期间较好以大于10ml/min和小于5000ml/min,更好以300-4000ml/min的流量将最好基本上与烧结气氛相同的气氛气体吹入炉中。如果吹入炉中的气氛气体的流量太小,烧结后含的碳量趋于变大,获得的铁氧体烧结体的机械强度趋于变低,而铁芯损耗趋于增加。另外,如果吹入炉中的气氛气体的流量太大,烧结后含的碳量趋于变得过小,而获得的铁氧体烧结体的铁芯损耗趋于变大。即,烧结同时按预定流量将气氛气体吹入炉中,可控制烧结后的碳含量,并可平衡获得的铁氧体烧结体的机械强度(抗弯强度)和磁性能(铁芯损耗)。
烧结温度最好为1200-1400℃。如果烧结温度太低,不仅烧结趋于不充分,而且烧结后含的碳量趋于变大。烧结时间通常为约3-7小时。
通过上述方法可获得将碳量控制到一个合适值的铁氧体烧结体。
该铁氧气体烧结体的平均晶粒直径最好为1-30μm。如果平均晶粒直径太小,磁滞损失趋于变大,而如果平均晶粒直径太大,涡流损失趋于变大。
本实施方案组分的铁氧体烧结体可改善机械强度,同时通过将碳含量控制到一个预定范围(大于9.8重量ppm至小于52重量ppm)中以降低铁芯损耗。另外,按照本实施方案的方法,烧结同时按预定流量将气体吹入炉中控制碳含量,这样可简单与便宜地生产将烧结后碳含控制到合适量的铁氧体烧结体。因此,使用这种铁氧体烧结体构成变压器磁芯,可获得铁芯损耗小、即使很薄也避免了裂纹或碎屑、以及可靠性优越的产品。而且,可促进产品尺寸的减小和成本的降低。
第三实施方案
第三实施方案的铁氧体烧结体例如可按如下方法生产。
按照与第一和第二实施方案相同的方法,首先,将原料称重并混合成预定的组分比例,以获得原料混合物。应注意到,原料的平均颗粒直径最好为0.1-3μm。
除了氧化铁和氧化镍或烧结后变成这些氧化物的材料外,本实施方案原料混合物还含有至少一种选自氧化铜、氧化锌和氧化锰的氧化物或烧结后变成这些金属氧化物的材料。应注意到,烧结后变成金属氧化物的材料包括金属、碳酸盐、氢氧化物、卤化物等。
该铁氧体组合物的组分不特别限制。按照目的可选择各种组分。最好该组分包含作为主成分的Fe2O3、NiO和至少一种选自CuO、ZnO和MnO的氧化物。本实施方案的铁氧体组合物的典型例子是Ni-Cu-Zn铁氧体组合物。
除上述主成分外,本实施方案原料混合物可具有添加到其中的各种添加剂。
应注意到,本实施方案原料混合物可包含材料中的杂质元素。作为这些元素有B、Al、Si、P、Ca、Cr、Co、Na、K、S、Cl等。要降低能量损失和对磁性能的作用,每种元素的重量比例,相对于组合物总量最好不大于200ppm,但P和B对能量损失或磁性能的影响大,因此,P的重量比例,相对于组合物总量最好为0-30ppm,或B的重量比例,相对于组合物总量最好为0-50ppm。
接着,将原料混台物预烧、磨粉、制粒和成形,然后烧结,以使获得与第一实施方案相同方法中的铁氧体成形物。
在本实施方案中,例如在烧结期间按照较好大于100ml/min,小于5000ml/min的流速,更好200-4000ml/min的流量将空气或其它气体吹入炉中。如果吹入炉中的气体流量太小,烧结后的碳含量变大,且获得的铁氧体烧结体的机械强度趋于变小。另外,如果吹入炉中的气体的流量太大,烧结后的碳含量趋于变得太小,且获得的铁氧体烧结体的磁导率趋于变小。即,通过烧结材料,同时按预定的流量将气体吹入炉中可控制烧结后的碳量,且可平衡获得的铁氧体烧结体的机械强度(抗弯强度)和磁性能(磁导率)。应注意到,烧结温度、烧结时间和烧结气氛可与第一实施方案相同。
通过上述方法可获得将碳量控制到合适值的铁氧体烧结体。
铁氧体烧结体的平均晶粒直径最好为1-30μm。如果平均晶粒直径太小,磁滞损失趋于变大,而如果平均晶粒直径太大,涡流损失趋于变大。
本实施方案组分的铁氧体烧结体可改善机械强度,同时通过将碳量控制到一个预定的范围(大于9.7重量ppm至小于60重量ppm)以保持高磁导率。另外,按照本实施方案的方法,烧结同时按预定的流量将气体吹入炉中控制碳量,这样可简单并便宜地生产将烧结后的碳量控制到合适量的铁氧体烧结体。所以,使用这种铁氧体烧结体构成电感器磁芯可获得磁导率优越的,即使很薄也避免裂纹或碎屑、且可靠性优越的产品。另外可促使产品尺寸的减小和成本的降低。
下面将通过更具体的实施例来更详细地说明本发明,但是本发明不限于这些实施例。
实施例1-7、参照例1、比较例1
称重作为材料的48.0%摩尔的Fe2O3,19.3摩尔%的MgO,7.1摩尔%的CuO和25.6摩尔%的ZnO,然后用球磨机湿混16小时,以使获得原料混合物。
接着,将原料混合物在900℃预烧2小时,以使获得预烧材料,然后用球磨机湿磨16小时,以使获得粉末材料。
接着,将10重量%的6%的聚乙烯醇水溶液作为粘合剂添加到100重量%的粉末材料中并制粒,以使获得颗粒材料。在1吨/cm2的压力下将其压制成环形,以使获得成形物。另外,为了抗弯强度试验,在1吨/cm2的压力下将该材料压制成5×5×500mm的棒形,以使获得成形物。
接着,将这些成形物放入烧结炉中。通过将空气吹入炉内,同时如表1所示改变吹入的流量(单位:ml/min),在空气中,在1020℃的烧结温度下进行烧结2小时,以使获得铁氧体烧结体。
测量以这种方法获得的每个铁氧体烧结体的碳量(单位:ppm)。测量碳量使用由Horiba Seisakusho制造的碳-硫分析仪(EMIA520),在氧气流中通过高频加热烧结试样,并用红外线吸收法测量。结果示于表1。
另外,测量每个获得的铁氧体烧结体的磁导率μ。求磁导率μ是将铜丝(丝径:0.35mm)绕试样缠20匝,在测量频率100KHz和测量电流0.25mA下用LCR仪(Hewlett-Packard制造)测量电感,并用下式(1)计算。结果示于表1。与碳量的关系示于图1。
磁导率μ=(le×L)(μ0×Ae×N2)        (1)
其中:le是磁路的长度,L是试样的电感,μ0是在真空中的磁导率=4Π×10-7(H/m),Ae是试样的截面积,而N是线圈的匝数。
另外,按照JIS-R1601使用棒形铁氧体烧结体试验抗弯强度。结果示于表1。与碳量的关系示于图2。
表1
    气体流量(ml/min)     碳量(ppm)     抗弯强度(kgf/mm2)     磁导率μ
    比较例1     25     96     7.8     852
    实施例1     50     91     8     845
    实施例2     100     77     10     833
    实施例3     200     67     10.4     821
    实施例4     300     55     12.3     812
    实施例5     500     48     13.4     802
    实施例6     1000     41     14.5     782
    实施例7     3000     33     14.6     772
    参照例1     5000     9.7     16.5     734
由上述结果可证明,如果烧结后碳量为96ppm(比较例1),则抗弯强度低,为7.8/kgf/mm2,且铁氧体成形物缺少可靠性。
与此相反,当烧结后的碳量不大于91ppm(实施例1-7和参照例1)时,抗弯强度足够大,为8-16.5kgf/mm2,且磁导率μ足够大,为734-845。其中,实施例2-7很好平衡了抗弯强度和磁导率。应注意到,这证明当烧结后的碳量为9.7ppm(参照例1)时,磁导率稍趋于下降,但实际上没有大问题。
实施例8-11,参照例2和参照例3
称重53.6摩尔%的Fe2O3,36.2摩尔%的MnO和10.2摩尔%的ZnO,然后用球磨机湿混16小时,以获得原料混合物。
接着,在850℃预烧原料混合物,以获得预烧的材料,然后将110重量ppm的SiO2粉末,500重量ppm的CaO粉末,3300重量ppm的SnO2粉末,320重量ppm的Nb2O5粉末和100重量ppm的MOO3粉末添加到100重量%的这样一种预烧材料中,然后将所得物用球磨机粉磨3小时,以获得粉末材料。
接着,将10重量%的聚乙烯醇的8%水溶液作为粘合剂添加到100重量%的粉末材料中,并将所得物制粒,以使获得颗粒的材料。以与实施例1-7相同的方法压制,以使获得环形物和棒形物。
接着,将这些成形物放入烧结炉中。进行烧结,将控制氧分压的烧结气氛气体吹入炉内,同时如表2所示改变吹入的流量(单位:ml/min),在控制氧分压的气氛中,在1300℃的烧结温度下烧结5小时,以使获得铁氧体烧结体。
以与实施例1-7相同的方法测量获得的铁氧体烧结体的碳量。结果示于表2。
另外,按照JIS-C2561-1992将一个100KH2和200mT的正弦波交流磁场施加到获得的铁氧体烧结体上,并在100℃测量铁芯损耗(单位:kw/m3)。结果示于表2。与碳量的关系示于图3。
另外,接着进行与实施例1-7相同的步骤,以使使用棒形铁氧体烧结体试验抗弯强度。结果示于表2。与碳量的关系示于图4。
表2
    气体流量(ml/min)     碳量(ppm)    抗弯强度(kgf/mm2)   铁芯损耗(kw/m3)
    参照例2     100     52     5.7     530
    实施例8     300     42     9.7     407
    实施例9     500     35     10.4     368
    实施例10     1000     30     14.4     374
    实施例11     3000     18.6     16.6     433
    参照例3     5000     9.8     20.2     506
由上述结果可证明,当烧结后的碳量为52ppm(参照例2)时,抗弯强度相对低,为5.7kgf/mm2
与此相反,当烧结后的碳量不大于42ppm(实施例8-11和参照例3)时,抗弯强度足够大,为9.7-20.2kgf/mm2,且铁芯损耗也足够低,为368-433kw/m3。其中,实施例8-11很好平衡了抗弯强度和铁芯损耗。应注意到,这证明当烧结后碳量为9.8ppm(参照例3)时,铁心损耗稍趋于变大,但实际上这不是大问题。
实施例12-16、参照例4和参照例5
按照实施例1-7相同的步骤,以使获得环成形物和棒成形物,除了使用49.5摩尔%的Fe2O3,9摩尔%的NiO,10摩尔%的CuO和31.5摩尔%的ZnO作为材料外。
接着,将成形物放入烧结炉中。进行烧结时将空气吹入炉中,同时如表3所示改变吹入的气体的流量(单位:ml/min),在空气中,在1100℃的烧结温度下烧结2小时,以使获得铁氧体烧结体。
按照与实施例1-7相同的方法测量这样得到的每个铁氧体烧结体的碳量。结果示于表3。
另外,按照与实施例1-7相同的方法测量每个获得的铁氧体烧结体的磁导率μ。结果示于表3。与碳量的关系示于图5。
另外,按照与实施例1-7相同的方法,使用棒形铁氧体烧结体试验抗弯强度。结果示于表3。与碳量的关系示于图6。
表3
    气体流量(ml/min)     碳量(ppm)     抗弯强度(kgf/mm2)     磁导率μ
  参照例4     100     67     7.1     872
  实施例12     200     58     8.3     864
  实施例13     300     52     9     834
  实施例14     500     36     9.9     804
  实施例15     1000     30     10.6     798
  实施例16     3000     18.6     1.6     778
  参照例5     5000     9.7     13.4     755
从上述结果可证明,如果烧结后的碳量为67ppm(参照例4),抗弯强度相对低,为7.1kgf/mm2
与此相反,当烧结后碳量不大于58ppm(实施例12-16和参照例5)时,抗弯强度足够大,为8.3-13.4kgf/mm2,而且磁导率μ足够大,为755-864。其中,实施例14-16很好地平衡了抗弯强度和磁导率。应注意到,当烧结后的碳量为9.7ppm(参照例5)时,可证明虽然磁导率稍趋于降低,但实际上没有大问题。
应注意到,本发明实施方案和实施例构成了上述说明,但本发明不以任何方式限于这些实施方案或实施例。当然在本发明要点范围内可以各种方式实行本发明。

Claims (21)

1.一种磁性铁氧体组合物,包含Mg、Ni、Cu、Zn、Mn和Li的至少一种并在烧结之后具有小于96重量ppm的碳含量,并且其中烧结之后的碳含量大于9.7重量ppm。
2.按照权利要求1所述的铁氧体组合物,其中,除了Mg外,所述铁氧体组合物还包含Cu、Zn、Mn、Ni和Li的至少一种。
3.按照权利要求1所述的铁氧体组合物,其中,碳含量不大于70重量ppm。
4.按照权利要求2所述的铁氧体组合物,其中,碳含量不大于70重量ppm。
5.按照权利要求1所述的铁氧体组合物,其中,铁氧体组合物至少包含Mn和Zn,且碳含量小于52重量ppm。
6.按照权利要求5所述的铁氧体组合物,其中,碳含量大于9.8重量ppm。
7.按照权利要求5所述的铁氧体组合物,其中,碳含量不大于45重量ppm
8.按照权利要求6所述的铁氧体组合物,其中,碳含量不大于45重量ppm
9.按照权利要求5所述的铁氧体组合物,其中,铁氧体组合物还包含作为添加的组分,它选自氧化硅、氧化钙、氧化锡、氧化钛、氧化铌、氧化锆、氧化钒、氧化钼、氧化铋和氧化钽的至少一种氧化物。
10.按照权利要求6所述的铁氧体组合物,其中,铁氧体组合物还包含作为添加的组分,它选自氧化硅、氧化钙、氧化锡、氧化钛、氧化铌、氧化锆、氧化钒、氧化钼、氧化铋和氧化钽的至少一种氧化物。
11.按照权利要求7所述的铁氧体组合物,其中,铁氧体组合物还包含作为添加的组分,它选自氧化硅、氧化钙、氧化锡、氧化钛、氧化铌、氧化锆、氧化钒、氧化钼、氧化铋和氧化钽的至少一种氧化物。
12.按照权利要求8所述的铁氧体组合物,其中,铁氧体组合物还包含作为添加的组分,它选自氧化硅、氧化钙、氧化锡、氧化钛、氧化铌、氧化锆、氧化钒、氧化钼、氧化铋和氧化钽的至少一种氧化物。
13.按照权利要求1所述的铁氧体组合物,其中,除了Ni外,所述铁氧体组合物包含Cu、Zn和Mn的至少一种,并且碳含量小于67重量ppm。
14.按照权利要求13所述的铁氧体组合物,其中,碳含量不大于60重量ppm。
15.一种电子元件,它包含一种磁性铁氧体组合物,该组合物含Mg、Ni、Cu、Zn、Mn和Li的至少一种并在烧结之后含小于96重量ppm的碳含量,并且其中烧结之后的碳含量大于9.7重量ppm。
16.一种生产如权利要求2所述的磁性铁氧体组合物的方法,其特征在于烧结铁氧体材料的同时向烧结炉中以超过25ml/min并小于5000ml/min的流量吹入气体。
17.一种生产如权利要求5或6所述的磁性铁氧体组合物的方法,其特征在于烧结铁氧体材料的同时向烧结炉中以超过100ml/min并小于5000ml/min的流量吹入一种氧分压受控的气体。
18.一种生产如权利要求13所述的磁性铁氧体组合物的方法,其特征在于烧结铁氧体材料的同时向烧结炉中以超过100ml/min并小于5000ml/min的流量吹入气体。
19.一种调整如权利要求2所述的磁性铁氧体组合物抗弯强度的方法,其特征在于在制造该磁性铁氧体组合物时,在烧结铁氧体材料的同时向烧结炉中以超过25ml/min并小于5000ml/min的流量吹入气体。
20.一种调整如权利要求5或6所述的磁性铁氧体组合物抗弯强度的方法,其特征在于在制造该磁性铁氧体组合物时,在烧结铁氧体材料的同时向烧结炉中以超过100ml/min并小于5000ml/min的流量吹入气体。
21.一种调整如权利要求13所述的磁性铁氧体组合物抗弯强度的方法,该组合物除了Ni之外还包括Cu、Zn、和Mn中的至少一种,其特征在于在制造该磁性铁氧体组合物时,在烧结铁氧体材料的同时向烧结炉中以超过100ml/min并小于5000ml/min的流量吹入气体。
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