CN108314440B - 一种宽频宽温低温度因数高强度镍锌铁氧体及其制备方法 - Google Patents
一种宽频宽温低温度因数高强度镍锌铁氧体及其制备方法 Download PDFInfo
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- 229910001053 Nickel-zinc ferrite Inorganic materials 0.000 title description 15
- 239000000463 material Substances 0.000 claims abstract description 49
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 11
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 11
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 9
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- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 4
- 239000000314 lubricant Substances 0.000 claims description 4
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 4
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 4
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- 238000001238 wet grinding Methods 0.000 claims description 3
- 229910052681 coesite Inorganic materials 0.000 claims description 2
- 229910052906 cristobalite Inorganic materials 0.000 claims description 2
- 229910000484 niobium oxide Inorganic materials 0.000 claims description 2
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- 229910052682 stishovite Inorganic materials 0.000 claims description 2
- 229910052905 tridymite Inorganic materials 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims 1
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
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- 239000000395 magnesium oxide Substances 0.000 description 2
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- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical group [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
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- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 description 2
- GPKIXZRJUHCCKX-UHFFFAOYSA-N 2-[(5-methyl-2-propan-2-ylphenoxy)methyl]oxirane Chemical compound CC(C)C1=CC=C(C)C=C1OCC1OC1 GPKIXZRJUHCCKX-UHFFFAOYSA-N 0.000 description 1
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- VSAISIQCTGDGPU-UHFFFAOYSA-N tetraphosphorus hexaoxide Chemical compound O1P(O2)OP3OP1OP2O3 VSAISIQCTGDGPU-UHFFFAOYSA-N 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
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Abstract
本发明公开了一种宽频宽温低温度系数高强度镍锌软磁铁氧体及其制备方法，所述镍锌铁氧体由主成分和副成分组成，Fe2O3 44.8~48.9mol%、NiO 16.5~21.8mol%、ZnO 29.1~32.2mol%、CuO 5.2~7.2mol%；副成分为：SiO2 0.60~0.90wt%、CaCO3 0.33~0.55wt%、Co3O4 0.02~0.06wt%、ZrO2 0.60~0.98wt%、Nb2O5 0.06~0.12wt%。采用氧化物法制备，在一定条件下烧结。烧结后制品的结晶晶粒平均尺寸为15～25μm，有明显晶界，制品具有在10MHz以下、‑40℃～125℃范围内磁导率变化较小及强度高的特点，适应小薄化绕线型功率电感对铁氧体材料频率、温度稳定性及强度的要求。
Description
技术领域
本发明属于软磁铁氧体技术领域，具体涉及一种宽频宽温低温度因数高强度镍锌铁氧体及其制备方法。
背景技术
市场的全球化要求各种电子元器件及构成各种器件的材料在很宽的温度范围内都具有良好的温度特性，而且铁氧体工作时由于损耗等导致的自身发热现象也将引起磁性能的变化，为保证器件工作的稳定性，要求材料的性能有较好的温度稳定性。
随着电子移动终端高频化、小型化、薄型化发展趋势，所使用的镍锌铁氧体功率电感需适应更宽的频率范围，同时需要更小、更薄，这就要求镍锌铁氧体具有高使用频率的同时需具备很高的机械强度。
本发明材料是一款宽温宽频低磁导率温度因数与高强度相结合的产品，制成的磁心作为绕线型功率电感的核心，其性能适应频率范围宽、随温度的变化小、强度高，特别适用作用薄型3D绕线型功率电感，广泛用于汽车电子、自动控制、家用电器、计算机、船舶、通信电子、绿色能源等领域，前景较好。
在国内已有一些相关镍锌铁氧体材料的制造方法的专利，具体如下：
（1）公开号为CN 104529423B，公开日为2016.07.20，发明名称为“一种低温度因数抗应力镍锌铁氧体及其制备方法”的中国专利公开了一种功率电感适用的起始磁导率为500的低温度因数抗应力镍锌铁氧体及其制备方法。采用氧化物法制备，在一定条件下烧结，烧结后制品的结晶晶粒尺寸为25～35μm，有明显晶界，制品具有在应力作用下-40~125℃范围内磁导率变化较小的特点，适应需要树脂封装的功率电感对铁氧体材料抗应力的要求。
（2）公开号为CN 1211049A，公开日为1999.03.17，发明名称为“铁氧体和电感器”的中国专利公开了提供一种铁氧体，具有高的初始导磁率、优异的抗应力特性和优异的温度特性，避免使用铅、价廉。该铁氧体可以实现树脂模制型电感器的小公差和高可靠性，不会引起环境污染。该铁氧体包括：主成分，至少包含氧化铁和氧化镍；添加物，包含氧化铋、氧化钒、氧化磷和氧化硼中的至少一种；第一辅助成分，包含氧化硅；第二辅助成分，包含氧化镁、氧化钙、氧化钡和氧化锶中的至少一种，基于主成分的添加物含量是0.5～15wt%，基于主成分的各辅助成分含量是0.1～10.0wt%。并提供一种使用上述铁氧体的树脂模制型电感器。
（3）公开号为CN101891456A，公开日为2010.11.24，发明名称为“一种高抗折强度镍锌软磁铁氧体材料及其制造方法”的中国专利公开了一种高抗折强度镍锌软磁铁氧体材
料。按摩尔份计的主配方：氧化铁Fe2O3 35～50mol%、氧化锌ZnO 8～15mol%、氧化亚镍NiO 30～40mol%、氧化铜CuO 5～11mol%。该发明提供了一种具有较高的抗折强度的镍锌软磁铁氧体材料。
（4）公开号为CN 1749211A，公开日为2006.03.22，发明名称为“铁氧体材料”的中国专利公开了一种铁氧体材料，它是作为主成分含有规定量的氧化铁、氧化铜、氧化锌以及氧化镍的NiCuZn系的铁氧体材料，作为辅助成分，含有规定量的氧化铋、氧化硅、氧化镁、四氧化三钴，以此构成铁氧体材料，因此能够提供温度特性极其良好(相对于温度变化的磁导率的变化率小)、品质因数Q高、高强度的NiCuZn系铁氧体材料。
发明内容
针对温度变化大、高频化、小薄化对于镍锌铁氧体材料宽频宽温低温度因数和机械强度的多重要求，本发明的目的是提供一种宽频宽温低温度因数、高强度的镍锌铁氧体。
为了达到上述目的，本发明采取以下的技术方案：一种宽频宽温低温度因数、高强度镍锌铁氧体，其特征包括主成分和副成分，主成分为：氧化铁、氧化镍、氧化锌、氧化铜，所述主成分以各自标准物计的含量如下：
Fe2O3 44.8~48.9mol%
NiO 16.5~21.8mol%
ZnO 29.1~32.2mol%
CuO 5.2~7.2mol%；
所述副成分包括二氧化硅、碳酸钙、四氧化三钴、氧化镐、氧化铌，相对所述主成分总量，所述副成分以各自标准物计的含量如下：
SiO2 0.60~0.90wt%
CaCO3 0.33~0.55wt%
Co3O4 0.02~0.06wt%
ZrO2 0.60~0.98wt%
Nb2O5 0.06~0.12wt%。
作为一种优选，相对所述主成分总量，所述副成分优选SiO2 0.80wt%，CaCO30.46wt%，Co3O4 0.03wt%，ZrO2 0.60wt%，Nb2O5 0.08wt%。
本发明的一种宽频宽温低温度因数高强度镍锌铁氧体材料采用氧化物法制造，具体步骤依次如下：
（1）一次造粒：按主成分配比配料后置于一次造粒设备中进行混合造粒，造粒时间为30~45分钟；
（2）预烧：将混合造球好的材料在一体式结构的回转窑中进行预烧，预烧温度控制在910±20℃，预烧量控制在(80±10)kg/h；
（3）粉碎：将上步得到的主成分预烧料中加入副成分后采用立式砂磨机进行湿法粉碎，粉碎时间为100~130分钟，粉碎后料浆中位粒径控制在0.9~1.3μm；
（4）造粒：在上步的料浆加入相当于料浆重量的10~18%的PVA溶液，采用高速离心造粒，得到颗粒料；
（5）增润：将上步的颗粒料加入相当于颗粒重量0.1~0.5%的润滑剂、0.1~0.5%软化剂进行整粒，整粒时间为20~30分钟；
（6）压制：将上步增润后颗粒料采用粉末成型机压制得到坯件，坯件的压制密度控制在(3.25±0.10)g/cm3；
（7）烧结：在电阻炉中进行烧结，烧结温度控制在1050℃~1150℃，保温150~240分钟，烧结气氛为空气，烧结结束后随炉冷却至室温。
通过以上工序制得所述镍锌铁氧体磁环样品(Φ12.7mm×Φ7.9mm×6.5mm)、磁条样品(I 25mm×5mm×5mm)。
本发明采用合理的主配方，通过对Fe2O3、ZnO含量的调整来优化材料的饱和磁通密度、起始磁导率、磁导率温度因数以及居里温度；通过NiO含量的调整来调整材料的使用频率；通过CuO含量的调整来调整材料的烧结温度。在副成分中加入SiO2、CaCO3、Nb2O5、ZrO2来改善材料强度；Co3O4改善材料的频率特性与磁导率特性；通过副成分的组合添加增加晶界的厚度，降低高频段相对损耗因子和磁导率的温度因数；再通过生产工艺进一步调整材料晶体结构和晶界分布，从而得到较宽的频率范围、较低的磁导率温度因数和良好的强度。该材料除了具有在宽温宽频范围磁导率变化较小的特点外，还特别适用于目前电子产品小薄化后对产品强度提出的要求，可以保证产品在小型化、薄型化、高组装密度后具有更好的耐摔打、抗碰撞、防震、抗机械破坏能力，达到保证产品性能的稳定和使用寿命的延长，符合电子设备小型化发展方向，其市场前景广阔。
材料的性能指标如下：
（1）起始磁导率 μi：480(1±20%),( f=100kHz,10mV,25℃)
≥240, ( f=10MHz,10mV,25℃)
（2）磁导率温度因数αF：(-2～2)×10-6, (f=100kHz,Bm＜0.25mT, -25℃～20℃)
(-2～2)×10-6, (f=100kHz,Bm＜0.25mT, 20℃～80℃)
（3）饱和磁通密度 Bs：≥370mT,( f=1kHz,Hm=4000A/m,25℃)
（4）居里温度 Tc：≥160 ℃, (f=100kHz,B＜0.25mT)
（5）机械强度 S：≥500 N。
附图说明
图1是磁条机械强度测试示意图；
图2是不同频率下磁环磁导率随温度的变化；
图3是断面SEM照片：(a) 对比例1；(b) 实施例1。
具体实施例
以下按照具体实施例说明本发明，但本发明不限定于这些实施例。
实施例和对比例的成分配比如表1所示：
表1
本发明的镍锌铁氧体采用传统氧化物法制造，具体步骤依次如下：
（1）一次造粒：按表1(实施例和对比例)主成分配比配料后置于一次造粒设备中进行混合造粒，造粒时间为30~45分钟；
（2）预烧：将混合好的材料在回转窑中进行预烧，预烧温度控制在910±20℃，预烧量控制在(80±10)kg/h；
（3）粉碎：将上步得到的主成分预烧料中按表1加入副成分后采用立式砂磨机进行湿法粉碎，粉碎时间为100~130分钟，粉碎后料浆中位粒径控制在0.9~1.3μm；
（4）造粒：在上步的料浆加入相当于料浆重量的10~18%的PVA溶液，采用高速离心造粒，得到颗粒料；
（5）增润：将上步的颗粒料加入相当于颗粒重量0.1~0.5%的润滑剂、0.1~0.5%软化剂进行整粒，整粒时间为20~30分钟；
（6）压制：将上步的颗粒料采用粉末成型机压制得到坯件，坯件的压制密度控制在(3.25±0.10)g/cm3；
（7）烧结：在电阻炉中进行烧结，烧结温度控制在1050℃~1150℃，保温150~240分钟，烧结气氛为空气，烧结结束后随炉冷却至室温。
通过以上工序制得所述镍锌铁氧体磁环样品(Φ12.7mm×Φ7.9mm×6.5mm) 、磁条样品(I 25mm×5mm×5mm)。
将烧结后的磁环分别进行测试和评价。用HP-4284A型 LCR测试仪测量样品在f=100kHz，25℃时电感，按公式（1）计算起始磁导率μi；用E4991B测试仪测量样品在5MHz下的起始磁导率；配合MC-711小型超低温试验箱和PHH-101高温试验箱测试样品的磁导率温度因数αF和居里温度Tc；用SY-8218型B-H分析仪测试样品的饱和磁通密度Bs；按照图1所示方法用CMT 6203微机控制电子万能试验机对磁条施加压力；按公式（2）磁导率温度因数αF来表示铁氧体材料的温度稳定性：
其中：μref为参考温度20℃的磁导率；μT为测试温度T下的磁导率；L为制品电感（H）；N为绕组匝数；D为样品外径（mm）；d为样品内径（mm）；h为样品厚度（mm）。
表2列出了实施例和对比例的磁性能及评价，从表2中可以看出，本发明的实施例和对比例相比较，本发明有效地拓宽了材料的频率范围、降低了材料的磁导率温度因数的同时，提高了材料的机械强度，并能保持相应的起始磁导率，较高的饱和磁感应强度，并具有较高的居里温度。对比实施例和对比例的微观结构(图3)，对比例材料结晶粗大，晶界薄，主要晶粒尺寸为30～50μm，气孔率较高；实施例的结晶较小，晶界明显，主要晶粒尺寸为10～25μm，气孔率低。晶粒细化、晶界增厚、气孔率低以及穿晶断裂应该是实施例的材料的强度水平相对于对比例大幅度提升的重要原因。本发明的材料应该能够满足小薄化功率电感对镍锌材料的性能要求。
表2
注意:
（1）超过规格上限的附加“﹢”，超过规格下限的附加“－”；
（2）在Tc一栏中，≥160表示Tc至少不小于160℃。
本发明所描述的具体实施例仅仅是对本发明作举例说明，相关技术领域的专家或技术人员可以对所描述的具体实施例做不同程度的修改，补充或者用类似的方式替代，但并不会偏离本发明的精神或者超越所附权利要求书所定义的范围。
Claims (4)
1.一种宽频宽温低温度系数高强度镍锌软磁铁氧体材料，具有在10MHz以下、-40℃～125℃范围内磁导率变化较小及强度高的特点，适应小薄化绕线型功率电感对铁氧体材料宽频高温度稳定性及高强度的要求，其包括主成分和副成分组成，所述主成分为：氧化铁、氧化镍、氧化锌、氧化铜，所述主成分以各自标准物计的含量如下：
Fe2O3 44.8~48.9mol%、NiO 16.5~21.8mol%、ZnO 29.1~32.2mol%、CuO 5.2~7.2mol%；
所述副成分包括二氧化硅、碳酸钙、四氧化三钴、氧化锆、氧化铌，相对所述主成分总量，所述副成分以各自标准物计的含量如下：
SiO2 0.60~0.90wt%、CaCO3 0.33~0.55wt%、Co3O4 0.02~0.06wt%、ZrO2 0.60~0.98wt%、Nb2O5 0.06~0.12wt%。
2.根据权利要求1所述的一种宽频宽温低温度系数高强度镍锌软磁铁氧体材料，其特征在于：相对所述主成分总量，所述副成分为优选SiO2 0.80wt%，CaCO3 0.46wt%，Co3O40.03wt%，ZrO2 0.60wt%，Nb2O5 0.08wt%。
3.一种如权利要求 1 所述的宽频宽温低温度系数高强度镍锌软磁铁氧体材料的制备方法，其特征在于，包括如下步骤：
（1）一次造粒：按主成分配比配料后置于一次造粒设备中进行混合造粒，造粒时间为30~45分钟；
（2）预烧：将混合造球好的材料在一体式结构的回转窑中进行预烧，预烧温度控制在910±20℃，预烧量控制在(80±10)kg/h；
（3）粉碎：将上步得到的主成分预烧料中加入副成分后采用立式砂磨机进行湿法粉碎，粉碎时间为100~130分钟，粉碎后料浆中位粒径控制在0.9~1.3μm；
（4）造粒：在上步的料浆加入相当于料浆重量的10~18%的PVA溶液，采用高速离心造粒，得到颗粒料；
（5）增润：将上步的颗粒料加入相当于颗粒重量0.1~0.5%的润滑剂、0.1~0.5%软化剂进行增润，增润时间为20~30分钟；
（6）压制：将上步增润后颗粒料采用粉末成型机压制得到坯件，坯件的压制密度控制在(3.25±0.10)g/cm3；
（7）烧结：在电阻炉中进行烧结，烧结温度控制在1050℃~1150℃，保温150~240分钟，烧结气氛为空气，烧结结束后随炉冷却至室温。
4.根据权利要求3所述的一种宽频宽温低温度系数高强度镍锌软磁铁氧体材料的制备方法，其特征在于，在增润步骤中：加入相当于颗粒重量0.1~0.5wt%的润滑剂、0.1~0.5wt%软化剂进行增润，增润时间为20~30分钟。
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