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CN1174443C - 制备甚高频片感器材料的方法 - Google Patents

制备甚高频片感器材料的方法 Download PDF

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Publication number
CN1174443C
CN1174443C CNB011205318A CN01120531A CN1174443C CN 1174443 C CN1174443 C CN 1174443C CN B011205318 A CNB011205318 A CN B011205318A CN 01120531 A CN01120531 A CN 01120531A CN 1174443 C CN1174443 C CN 1174443C
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China
Prior art keywords
low
oxide
ferrite
vhf
sintering
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Expired - Fee Related
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CNB011205318A
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English (en)
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CN1397961A (zh
Inventor
王晓慧
李龙土
周济
苏水源
桂治轮
岳振星
马振伟
张力
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Tsinghua University
Tongfang Co Ltd
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Tsinghua University
Qinghua Tongfang Co Ltd
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Priority to CNB011205318A priority Critical patent/CN1174443C/zh
Priority to US10/046,878 priority patent/US6695972B2/en
Priority to JP2002134811A priority patent/JP2003048773A/ja
Publication of CN1397961A publication Critical patent/CN1397961A/zh
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Abstract

本发明涉及一种甚高频片感材料的制备方法。现有技术中尚无高性能低烧铁氧体材料，只能用低介陶瓷作为介质制作低电感量的多层片式电感代替。该材料的主料为平面六角软磁铁氧体，配料为低温助烧剂。制备方法为固相反应合成法，助烧剂采用二次掺杂，通过球磨、烘干、预烧、球磨、烘干、造粒、成型、烧结等工艺获得性能优异的甚高频电感器材料，实现900℃以下低温烧结。本发明成本低、性能高、适用于300M～800MHz的甚高频段使用的片感器材料的要求。

Description

制备甚高频片感器材料的方法
(一)技术领域
本发明涉及一种高性能低烧甚高频叠层片式电感器材料的制备方法，属材料
技术领域。
(二)背景技术
叠层片式电感器(Multilayer Chip Inductors or Multilayer FerriteInductor，简称MLCI或MLFI)是铁氧体材料与内部螺旋式串联电极共烧的独石结构。其工艺技术的关键是磁介质材料(软磁铁氧体)和内导体材料(从导电性能及成本方面考虑，银为最佳选择)共烧。这要求其中的软磁铁氧体具有较低的烧结温度，同时具有高磁导率和高品质因数。目前国内外片式电感材料主要是NiZnCu低烧铁氧体和低介陶瓷。NiZnCu低烧铁氧体材料及器件的工作频率一般在200MHz以下，当组分中不含Zn时，工作频率最高达到300MHz；低介陶瓷由于磁导率一般为1，因此只能被用于对电感量要求不高的超高频段(800MHz)以上。而在移动通讯、IT技术、电视及国防领域常用的300M-800MHz的甚高频段，迄今为止尚无高性能低烧铁氧体材料，只能用低介陶瓷作为介质制作低电感量的多层片式电感代替。
平面六角晶系各向异性Z型铁氧体Ba3Co2Fe24O41(Co2Z)，由荷兰菲利普实验室发现于50年代末，其自然共振频率在1.3-3.4GHz，具有优良的电磁性能，因此在甚高频、微波波段具有广泛的应用。但由于Z型铁氧体复杂的晶体结构，其成相和烧结温度高达1300℃左右。要用其作为片感器材料必须使其烧结温度降低到900℃左右才能与银内电极共烧。现有技术已经可通过化学法制备Co2Z系平面六角铁氧体低烧片感器材料，可实现900℃以下低温烧结，磁导率为4-8。但该种化学法制备粉体工艺较复杂、成本相对较高，并材料性能差。
(三)发明内容
本发明是提出一种甚高频片感器材料的配方及其制备方法，采取固相合成方法，实现900℃以下低温烧结，获得低介高磁导率的甚高频电感器材料，以满足工艺简单、低成本、高性能、适用于300M-800MHz的甚高频段使用的片感器材料的要求。
本发明采用固相反应合成方法制备，其步骤是：
(1)平面六角软磁铁氧体主料的合成：根据分子式在初始原料Fe2O3，SrCO3或SrO，BaCO3或BaO，Co3O4或CoO，ZnO，CuO，Mn2O3或MnO2或MnCO3选择材料，按分子式化学计量比称取，混合后球磨2~48小时，以水为介质；
(2)将步骤(1)中获得的球磨浆料烘干，经1000-1300℃预烧，获得主料Z型平面六角软磁铁氧体；
(3)按配方将二次掺杂的助烧剂与主料混合，球磨2~48小时，以水为介质；
(4)将步骤(3)获得的球磨浆料烘干，过100-200目筛，造粒，成型；
(5)在860-920℃烧结1-10小时。
该方法中所用的甚高频片感器材料的组成成分为：主料为平面六角软磁铁氧体，其分子式为Ba3-XSrXCo2-Y-ZZnYCuZMnWFe24-W-VO41，其中0≤X≤2，0≤Y≤2，0≤Z≤2.0，0≤W≤1.0；0≤V≤1.0；配料为低温助烧剂，由氧化铋、氧化钒、氧化镉、氧化钙、氧化硅、氧化铅、氧化硼、氟化铅、氟化锂、氟化钙、硼铅玻璃、碳酸锂或硼酸锂中的一种或一种以上组成；配方中主料占总料的重量百分比为99-88％，配料二次掺杂物占总料的重量百分比为1-12％。
通过本发明的配方和制备工艺，可制备出平面六角系列纯Co2Z及掺杂改性的Z型软磁铁氧体材料，实现900℃低温烧结，调节配方和工艺得到高性能甚高频应用的片式电感器材料。与现有技术相比较其优点在于：配方可调，烧成温度低，烧成温区宽；工艺简单、成本低，获得的低烧铁氧体材料性能稳定、可靠性好、电磁性能优异，900℃以下烧结磁导率可达到10。
(四)附图说明
图1是应用本发明的一组样品的磁频谱特性曲线图。
图2是与图1对应的品质因数曲线图。
图3是应用本发明的另一组样品的磁频谱特性曲线图。
图4是与图3对应的品质因数曲线图。
图5是应用本发明的一组样品的磁频谱特性曲线图。
图6是与图5对应的品质因数曲线图。
图7是应用本发明的另一组样品的磁频谱特性曲线图。
图8是与图7对应的品质因数曲线图。
(五)具体实施方式
实施例1
固相法合成平面六角Z型软磁铁氧体Ba3Co1.0Zn0.8Cu0.2Fe23MnO41，助烧剂为氧化铋和氧化硅。初始原料BaCO3，Co3O4，ZnO，CuO，Mn2O3，Fe2O3，按化学计量比分别称取59.20g，8.03g，6.511g，1.591g，7.89g，183.6g。混合球磨24小时，烘干后，在1000-1300℃预烧形成Z型软磁铁氧体。取20克铁氧体粉，加入助烧剂，含量为占总料重量百分比的3％，经球磨24小时混合，干燥后，过100~200目筛，成型，在870℃，890℃，920℃烧结6小时，分别记为样品1-1，1-2，1-3。圆环样品，外径20mm，内径10mm，厚度3mm，成型压力7MPa；圆片样品，直径为10mm，厚度为1mm，成型压力为2MPa。烧成的瓷片上下被银后测量其电阻率。烧成的圆环样品用HP4291B(1M-1.8GHz)射频阻抗分析仪测量磁频谱和温度特性(测试温度区间-55-120℃)。图1给出样品的磁频谱特性曲线，初始磁导率可达到10左右，截止频率在1.5GHz以上。图2为相应的品质因数曲线。所获得样品性能参数见表1。表1中各参数代表的意义如下：
μi材料的初始磁导率；Q材料的品质因数；
(αμ)rel材料的相对(比)温度系数；ρ材料的电阻率。
                                   表1
  样品  烧结条件  μi   Q(300MHz)   (αμ)rel(/℃)  ρ(Ω·cm)
  1-1  870℃/6h  9.0   60   1.2×10-6  8.4×108
  1-2  890℃/6h  9.4   42   9.8×10-7  9.1×108
  1-3  920℃/6h  9.7   40   2.0×10-6  2.3×109
实施例2
固相法合成平面六角Z型软磁铁氧体Ba1.5Sr1.5Co2Fe23MnO41，助烧剂为氧化硼和氧化铅。初始原料BaCO3，SrCO3，Co3O4，Mn2O3，Fe2O3，按化学计量比分别称取29.60g，22.14g，16.05g，7.89g，183.6g。混合球磨24小时，烘干后，在1000-1300℃预烧形成Z型软磁铁氧体。分别取20克铁氧体粉，加入助烧剂，含量分别为占总料的重量百分比3，6，9％，经球磨混合12小时，干燥后，过100~200目筛，成型，在890℃烧结6小时，分别记为样品2-1，2-2，2-3。圆环样品，外径20mm，内径10mm，厚度3mm，成型压力7MPa；圆片样品，直径为10mm，厚度为1mm，成型压力为2MPa。烧成的瓷片上下被银后测量其电阻率。烧成的圆环样品用HP4291B(1M-1.8GHz)射频阻抗分析仪测量磁频谱和温度特性(测试温度区间-55-120℃)。图3给出样品的磁频谱特性曲线，初始磁导率2-4，截止频率在1.8GHz以上。图4为相应的品质因数曲线。所获得样品性能参数见表2。表2中各参数代表的意义如下：
μi材料的初始磁导率；Q材料的品质因数；
(αμ)rel材料的相对(比)温度系数；ρ材料的电阻率。
                                         表2
  样品   烧结条件   μi   Q(300MHz)     (αμ)rel(/℃)  ρ(Ω·cm)
  2-1   890℃/6h   3.7   85     2.4×10-6  3.9×108
  2-2   890℃/6h   2.7   80     1.2×10-6  5.3×108
  2-3   890℃/6h   2.0   50     1.7×10-6  4.7×108
实施例3
固相法合成平面六角Z型软磁铁氧体Ba3Co2Fe24O41，助烧剂为氟化铅。初始原料BaO，Co3O4，Fe2O3，按化学计量比分别称取45.96g，16.05g，191.6g。混合球磨24小时，烘干后，在1000-1300℃预烧形成Z型软磁铁氧体。分别取20克铁氧体粉，加入助烧剂，含量分别为占总料的重量百分比6％，经球磨混合24小时，干燥后，过100~200目筛，成型，在890℃分别烧结4、8小时，分别记为样品3-1，3-2。圆环样品，外径20mm，内径10mm，厚度3mm，成型压力7MPa；圆片样品，直径为10mm，厚度为1mm，成型压力为2MPa。烧成的瓷片上下被银后测量其电阻率。烧成的圆环样品用HP4291B(1M-1.8GHz)射频阻抗分析仪测量磁频谱和温度特性(测试温度区间-55-120℃)。所获得样品性能参数见表3。图5给出样品的磁频谱特性曲线，初始磁导率4-5，截止频率在1.8GHz以上。图6为相应的品质因数曲线。表3中各参数代表的意义如下：
μi材料的初始磁导率；Q材料的品质因数；
(αμ)rel材料的相对(比)温度系数；ρ材料的电阻率。
                                  表3
  样品   烧结条件   μi   Q(300MHz)     (αμ)rel(/℃) ρ(Ω·cm)
  3-1   890℃/4h   4.5   45     1.7×10-6 2.9×109
  3-2   890℃/8h   4.8   40     3.2×10-6 1.4×109
实施例4
固相法合成平面六角Z型软磁铁氧体Ba2.9Sr0.1Co1.4Cu0.6Fe23Mn0.2O39.8，助烧剂为氟化锂、氟化钙和氧化铋。初始原料BaO，SrO，CoO，CuO，MnCO3，Fe2O3，按化学计量比分别称取44.43g，1.04g，10.49g，4.77g，2.30g，183.6g。混合球磨24小时，烘干后，在1000-1300℃预烧形成Z型软磁铁氧体。分别取20克铁氧体粉，加入助烧剂，含量分别为占总料的重量百分比5％，经球磨混合24小时，干燥后，过100~200目筛，成型，在860，890和920℃烧结6小时，分别记为样品4-1，4-2，4-3。圆环样品，外径20mm，内径10mm，厚度3mm，成型压力7MPa；圆片样品，直径为10mm，厚度为1mm，成型压力为2MPa。烧成的瓷片上下被银后测量其电阻率。烧成的圆环样品用HP4291B(1M-1.8GHz)射频阻抗分析仪测量磁频谱和温度特性(测试温度区间-55-120℃)。所获得样品性能参数见表4。图7给出样品的磁频谱特性曲线，初始磁导率5-6，截止频率在1.8GHz以上。图8为相应的品质因数曲线。表4中各参数代表的意义如下：
μi材料的初始磁导率；Q材料的品质因数；
(αμ)rel材料的相对(比)温度系数；ρ材料的电阻率。
                                    表4
    样品     烧结条件     μi   Q(300MHz)   (αμ)rel(/℃) ρ(Ω·cm)
    4-1     860℃/6h     5.1   55   8.9×10-7 8.2×108
    4-2     890℃/6h     5.8   40   7.3×10-7 2.7×109
    4-3     920℃/6h     6.1   40   5.9×10-7 4.4×109
以上实施例说明，通过本发明能够获得高性能甚高频片式电感器材料。助烧剂的加入，可实现900℃低温烧结，瓷体密度高，粒度均匀，平均粒径为1-2微米。通过配方和工艺的调整，材料的初始磁导率覆盖从2到10一个系列，截止频率大于1.5GHz，比温度变化率不大于10-6/℃，品质因数大于40，电阻率大于108Ω·cm。本发明的材料是一种具有巨大应用前景的甚高频片感器材料，用这种材料可制备出高性能甚高频片感元件。

Claims (1)

1.一种制备高性能甚高频叠层片式电感器材料的方法，其特征在于：采用的固相反应合成法，该方法包括如下步骤：
(1)平面六角软磁铁氧体主料的合成：根据分子式在初始原料Fe2O3，SrCO3或SrO，BaCO3或BaO，Co3O4或CoO，ZnO，CuO，Mn2O3或MnO2或MnCO3选择材料，按分子式化学计量比称取，混合后球磨2～48小时，以水为介质；
(2)将步骤(1)获得的球磨浆料烘干，经1000～1300℃预烧，获得主料Z型平面六角软磁铁氧体；
(3)按配方将二次掺杂的助烧剂与主料混合，球磨2～48小时，以水为介质；
(4)将步骤(3)球磨浆料烘干，过100～200目筛，造粒，成型；
(5)在860～920℃烧结1～10小时；
该方法中所用材料的配方为：(1)材料组成成分：①主料为平面六角软磁铁氧体，其分子式为Ba3-XSrXCo2-Y-ZZnYCuZMnWFe24-W-VO41，其中0≤X≤2，0≤Y≤2，0≤Z≤2.0，0≤W≤1.0；0≤V≤1.0；②配料为二次掺杂的低温助烧剂，由氧化铋、氧化钒、氧化镉、氧化钙、氧化硅、氧化铅、氧化硼、氟化铅、氟化锂、氟化钙、硼铅玻璃、碳酸锂或硼酸锂中的一种或一种以上组成；(2)配方中主料所占总料的重量百分比为99～88％，配料二次掺杂物占总料的重量百分比为1～12％。
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