CN109336581A - 铁氧体材料及其制备方法 - Google Patents
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Abstract
本发明提供一种铁氧体材料,包括主粉体和添加剂;主粉体包括:按主粉体摩尔百分比计,Fe2O3:45~49.2mol%,ZnO:10~35mol%,CuO:8~14mol%,余量为NiO;添加剂包括:按主粉体的重量计,V2O5:0~0.2wt%、Co2O3:0~1wt%。本发明还提供该铁氧体材料的制备方法。本发明铁氧体材料,不含Bi,纯度高,烧结性能良好,结构均匀,可用于制作具有高致密性、高强度和高可靠性的电感器件。本发明铁氧体材料的制备方法使得制作具有高致密性、高强度和高可靠性的电感器件成为可能。
Description
技术领域
本发明涉及一种铁氧体材料,尤其是一种具有高致密性、高强度和高可靠性的铁氧体材料。
背景技术
随着5G通讯、电动汽车、智能网的发展,电子元件的使用逐渐增多。应用环境的多样化,对元件可靠性提出了更高的要求,比如高温高湿、高温负载等,还有一些特殊场所要求防硫化。国内的叠层电感在高可靠性要求领域面临挑战,如车载、军工、工业等应用领域。
在导致电子元件可靠性失效的原因中,很多主要是由于产品致密性不够所致。传统的叠层铁氧体材料为了实现低温烧结,通常采取添加助烧剂的方法,如Bi2O3。而这会造成晶粒生长过大、晶粒不均匀、晶界较厚、气孔率增多等不利影响;另外,Bi2O3除了促进晶粒生长,也会促进Ag离子迁移,加快了产品的可靠性失效。
发明内容
本发明所要解决的一个技术问题是提供一种具有高致密性、高强度和高可靠性的铁氧体材料。
为解决上述技术问题,本发明提供一种铁氧体材料,包括主粉体和添加剂;主粉体包括:按主粉体摩尔百分比计,Fe2O3:45~49.2mol%,ZnO:10~35mol%,CuO:8~14mol%,余量为NiO;添加剂包括:按主粉体的重量计,V2O5:0~0.2wt%、Co2O3:0~1wt%。
本发明铁氧体材料中,适当含量的CuO在组分中起到促进烧结作用;当CuO含量较低时,会导致烧结致密性不足;当CuO含量较高时,会导致绝缘电阻下降,Q值降低。Fe2O3含量偏低时,材料相对磁导率及饱和磁通密度Bs都会降低,而Fe2O3含量过高会影响烧结活性。本发明铁氧体的添加剂中,微量添加V2O5在产品烧结时可起到细化晶粒、均匀生长的作用,当V2O5添加量过多会产生较多杂质相以及气孔。添加剂中的Co2O3在烧结时会形成尖晶石相,不会影响烧结致密性,主要用于调节材料的Q值及频谱特性。
本发明铁氧体材料的纯度越高越好,杂质含量越少越好,要求P含量小于50ppm、SiO2含量小于100ppm。
为保证材料的良好性能,本发明铁氧体材料的粒度D50<0.3μm,比表面积BET值为15~25m2/g。
现有技术中,固相法铁氧体粉料粒度是D50约1μm,BET值约5m2/g。当粒度较大时,材料烧结活性偏低,无法在900℃下烧结致密;而当BET值过大时,铁氧体粉料团聚严重,制浆难以分散。本发明的配方及粒度范围内所得到的铁氧体粉料,可满足制浆流延工艺,且在900℃下烧结致密。
本发明所要解决的另一个技术问题是提供一种不含Bi的具有高致密性、高强度和高可靠性的铁氧体材料的制备方法。
为解决上述技术问题,本发明提供一种铁氧体材料的制备方法,包括以下步骤:
a.选取原材料Fe2O3、ZnO、NiO、CuO,构成铁氧体材料的主粉体;主粉体中,按主粉体摩尔百分比,Fe2O3:45~49.2mol%,ZnO:10~35mol%,CuO:8~14mol%,余量为NiO;Fe2O3、ZnO、NiO、CuO的粒度满足D50<0.5μm;
b.将满足步骤a要求的主粉体在600~800℃进行预烧;
c.以步骤b得到的主粉体的重量计,掺入0~0.2wt%的V2O5以及0~1.0wt%的Co2O3作为添加剂,经过磨细烘干后得到铁氧体材料,磨细的粒度要求D50<0.3μm,BET值为15~25m2/g。
本发明制备方法的铁氧体材料中,P含量小于50ppm、SiO2含量小于100ppm。
本发明制备方法的铁氧体材料的粒度D50<0.3μm,比表面积BET值为15~25m2/g。
作为本发明方法的一个具体实施,步骤a中,按主粉体摩尔百分比,Fe2O3:48mol%,ZnO:20mol%,CuO:8mol%,NiO:24mol%;步骤c中,V2O5以及Co2O3均为0,经过磨细烘干后得到铁氧体材料,磨细的粒度要求D50值为0.18μm,BET值为25m2/g;制得的铁氧体材料的烧结密度为5.15g/cm3,相对磁导率为125,抗弯强度为150MPa,平均晶粒尺寸为1.2μm,硫化实验△R/R为1.4%。
作为本发明方法的一个具体实施,步骤a中,按主粉体摩尔百分比,Fe2O3:48mol%,ZnO:20mol%,CuO:14mol%,NiO:18mol%;步骤c中,V2O5以及Co2O3均为0,经过磨细烘干后得到铁氧体材料,磨细的粒度要求D50值为0.25μm,BET值为18m2/g;制得的铁氧体材料的烧结密度为5.2g/cm3,相对磁导率为140,抗弯强度为155MPa,平均晶粒尺寸为1.3μm,硫化实验△R/R为-1.5%。
作为本发明方法的一个具体实施,步骤a中,按主粉体摩尔百分比,Fe2O3:48mol%,ZnO:10mol%,CuO:12mol%,NiO:30mol%;步骤c中,以步骤b得到的主粉体的重量计,掺入0.1wt%的V2O5作为添加剂,Co2O3为0,经过磨细烘干后得到铁氧体材料,磨细的粒度要求D50值为0.22μm,BET值为20m2/g;制得的铁氧体材料的烧结密度为5.25g/cm3,相对磁导率为80,抗弯强度为160MPa,平均晶粒尺寸为1.5μm,硫化实验△R/R为-0.5%。
作为本发明方法的一个具体实施,步骤a中,按主粉体摩尔百分比,Fe2O3:48mol%,ZnO:35mol%,CuO:12mol%,NiO:5mol%;步骤c中,以步骤b得到的主粉体的重量计,掺入0.5wt%的Co2O3作为添加剂,V2O5为0,经过磨细烘干后得到铁氧体材料,磨细的粒度要求D50值为0.22μm,BET值为20m2/g;制得的铁氧体材料的烧结密度为5.2g/cm3,相对磁导率为355,抗弯强度为150MPa,平均晶粒尺寸为1.5μm,硫化实验△R/R为1.6%。
本发明铁氧体材料,不含Bi,纯度高,烧结性能良好,结构均匀,可用于制作具有高致密性、高强度和高可靠性的电感器件。本发明铁氧体材料的制备方法使得制作具有高致密性、高强度和高可靠性的电感器件成为可能。
附图说明
下面通过具体实施方式并结合附图,对本发明作进一步的详细说明:
图1是本发明实施例S1中的铁氧体材料的扫描电镜照片;
图2是本发明实施例S2中的铁氧体材料的扫描电镜照片;
图3是对比例D1中的铁氧体材料的扫描电镜照片;
图4是对比例D3中的铁氧体材料的扫描电镜照片。
具体实施方式
下面结合实施例S1-S8和对比例D1-D8对本发明进行说明。
表一列出了实施例S1-S8和对比例D1-D8中的铁氧体材料的成分配比和相关参数。
表一实施例与对比例的成分配比及相关参数
成分 | Fe<sub>2</sub>O<sub>3</sub> | ZnO | NiO | CuO | Co<sub>2</sub>O<sub>3</sub> | V<sub>2</sub>O<sub>5</sub> | Bi<sub>2</sub>O<sub>3</sub> | D50 | BET |
单位 | mol% | mol% | mol% | mol% | wt% | wt% | wt% | μm | m<sup>2</sup>/g |
实施例S1 | 48 | 20 | 24 | 8 | 0 | 0 | 0 | 0.18 | 25 |
实施例S2 | 48 | 20 | 22 | 10 | 0 | 0 | 0 | 0.2 | 20 |
实施例S3 | 48 | 20 | 18 | 14 | 0 | 0 | 0 | 0.25 | 18 |
实施例S4 | 45 | 23 | 22 | 10 | 0 | 0.05 | 0 | 0.25 | 18 |
实施例S5 | 49.2 | 23 | 18 | 10 | 0.5 | 0 | 0 | 0.25 | 18 |
实施例S6 | 48 | 10 | 30 | 12 | 0 | 0.2 | 0 | 0.22 | 20 |
实施例S7 | 48 | 35 | 5 | 12 | 0.5 | 0 | 0 | 0.22 | 20 |
实施例S8 | 48 | 20 | 20 | 12 | 0 | 0.05 | 0 | 0.3 | 15 |
对比例D1 | 48 | 20 | 28 | 6 | 0 | 0 | 0 | 0.3 | 15 |
对比例D2 | 48 | 20 | 22 | 10 | 0 | 0.05 | 0 | 0.6 | 8 |
对比例D3 | 48 | 20 | 22 | 10 | 0 | 0.05 | 1 | 0.6 | 8 |
对比例D4 | 48 | 20 | 18 | 14 | 0 | 0.05 | 0 | 1.0 | 4 |
对比例D5 | 48 | 20 | 22 | 10 | 0 | 0.1 | 0.5 | 0.3 | 15 |
对比例D6 | 48 | 20 | 22 | 10 | 0.1 | 0.5 | 0 | 0.8 | 5 |
对比例D7 | 48 | 30 | 16 | 6 | 0.5 | 0.1 | 0.5 | 0.5 | 10 |
对比例D8 | 48 | 30 | 16 | 6 | 0.5 | 0 | 1 | 0.5 | 10 |
根据表一中的成分配比,按照以下步骤分别制备实施例S1-S8和对比例D1-D8的各铁氧体粉体材料和铁氧体生带、叠层片式电感,叠层片式电感都按同一规格型号PZ1005U121进行制作。
A.选取高纯度高活性的原材料Fe2O3、ZnO、NiO、CuO,并将原材料进行磨细处理;
B.按照表1的成分配比进行配料;
C.将粉体在600~800℃进行预烧;
D.以预烧后铁氧体粉料为基础,掺入表1对应重量百分比为的添加剂,经过砂磨烘干后得到铁氧体材料,砂磨后的粒度如表一;
E.制得的铁氧体粉料,经过添加溶剂、分散剂、粘合剂及增塑剂等制成流延浆料,再进行干法流延得到铁氧体生带;
F.铁氧体生带经过开孔、印刷、叠层、等静压、切割,得到生坯产品;
G.产品在900℃进行烧结,再经过端电极、电镀工序得到叠层片式电感器件。
步骤E中,相对于铁氧体粉体重量,溶剂添加量:60~70wt%、粘合剂量:10~15wt%、分散剂量:2~5wt%、增塑剂量:4~8wt%。
溶剂选取乙醇、乙酸乙酯、异丙醇、异丁醇、异丙醇、丙酮、***、二甲基乙酰胺中的一种或多种。
粘合剂选取聚乙烯醇缩丁醛、聚甲基丙烯酸甲酯、乙基纤维素、丙烯酸树脂中的一种或多种,优选聚乙烯醇缩丁醛。
分散剂选用高分子型分散剂,可选用脂肪酸酰胺类、有机磷酸酯类或者羧酸类。
采用各实施例和对比例的铁氧体粉体制作磁环以及长条样品,样品在900℃/2h下烧结,分别测试烧结密度、抗弯强度及1MHz下的相对磁导率。测试结果如表二所示。
制作得到的PZ1005U121叠层片式电感的结构中包括铁氧体材料、Ag内电极、Ag引出端和Ag-Ni-Sn端头镀层。
对各实施例和对比例的叠层片式电感,采用SEM扫描电镜观察铁氧体材料的显微结构,测量铁氧体材料表面晶粒尺寸,得到每一种铁氧体材料表面晶粒尺寸的多个测量值求取每一种铁氧体材料的表面晶粒尺寸平均值;电感产品进行硫化实验,实验条件:将产品放置于H2S浓度为10ppm的试验箱中,时间500hrs,测试实验前后的直流电阻DCR值,求取直流电阻平均变化率△R/R,结果如表二所示。对于各实施例和对比例的叠层片式电感,如果测试所得直流电阻平均变化率△R/R小于或等于5%,则判定为合格(OK);如果测试所得直流电阻平均变化率△R/R大于5%,则判定为不合格(NG)。
表二实施例与对比例的性能对比
从表二可以看出,本发明的实施例与对比例相比较,本发明各实施例中铁氧体材料具有比个对比例中铁氧体材料更高的烧结密度及抗弯强度;图1、图2为实施例S1与S2的显微形貌结构,其晶粒尺寸细小均匀且致密,晶粒尺寸在1~2μm之间,无明显孔隙;图3为对比例D1的显微形貌结构,其晶粒生长不够致密,空隙率较多,而图4为对比例D3的显微形貌,其晶粒生长不均匀,晶粒与晶粒之间的间隙明显;从硫化实验对比来看,实施例产品的DCR值基本没有太明显的变化,而对比例中有部分产品的DCR值上升明显,这是由于Ag与H2S发生了反应,根本原因是产品的致密性不够,H2S气体进入到产品内部中,使得Ag烧损进而导致DCR值上升。
在没有添加Bi2O3的对比例中,与实施例S1相比,对比例D1中的CuO含量低,所得铁氧体材料的烧结密度较低,相对磁导率和抗弯强度也都较小,DCR值变化率大;与实施例S2相比,对比例D2中的材料粒度D50较大、比表面积BET值小,烧结活性降低,虽然添加了V2O5以起到细化晶粒、均匀生长的作用,所得铁氧体材料的烧结密度仍然较低,相对磁导率、抗弯强度也较低,DCR值变化大;与实施例S4相比,对比例D4中的材料粒度D50较大、比表面积BET值小,烧结活性降低,所得铁氧体材料的烧结密度较低,抗弯强度也较低,DCR值变化大;与实施例S6相比,对比例D6中的材料粒度D50较大、比表面积BET值小,烧结活性降低,虽然添加了V2O5以起到细化晶粒、均匀生长的作用,使得烧结密度、相对磁导率、抗弯强度数值较大,但V2O5添加量太大,导致产生较多杂质相以及气孔,所得铁氧体材料的DCR值变化大。
本发明各实施例中的铁氧体粉料,采取固相法制备方法,通过原材料磨细处理提升原料活性。
相比于传统叠层片式电感器件,采用本发明铁氧体粉料的高可靠性叠层片式电感器件的优势在于烧结后晶粒细小均匀,晶粒尺寸在1~2μm,晶界较薄,气孔率较低,具有高致密性、高强度等特点,具备更高的可靠性。
采用本发明铁氧体粉料的的高可靠性叠层片式电感器件,H2S硫化实验结果表明,产品的DCR值未出现明显变化;而传统叠层片式电感器件由于瓷体的致密性偏低,H2S气体进入到瓷体中与Ag发生反应,导致DCR值发生明显上升。
本发明铁氧体材料除了采用固相法的工艺实现外,也可以采用其它化学法制备,如溶胶-凝胶法、水热法等。
以上内容是结合具体的优选实施方式对本发明所作的进一步详细说明,不能认定本发明的具体实施只局限于这些说明。对于本发明所属技术领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干简单推演或替换,都应当视为属于本发明的保护范围。
Claims (10)
1.一种铁氧体材料,包括主粉体和添加剂;其特征在于:所述主粉体包括:按所述主粉体摩尔百分比计,Fe2O3:45~49.2mol%,ZnO:10~35mol%,CuO:8~14mol%,余量为NiO;所述添加剂包括:按主粉体的重量计,V2O5:0~0.2wt%、Co2O3:0~1wt%。
2.根据权利要求1所述的铁氧体材料,其特征在于:所述铁氧体材料中,P含量小于50ppm、SiO2含量小于100ppm。
3.根据权利要求1或2所述的铁氧体材料,其特征在于:所述铁氧体材料的粒度D50<0.3μm,比表面积BET值为15~25m2/g。
4.一种铁氧体材料的制备方法,其特征在于:包括以下步骤:
a.选取原材料Fe2O3、ZnO、NiO、CuO,构成铁氧体材料的主粉体;主粉体中,按主粉体摩尔百分比,Fe2O3:45~49.2mol%,ZnO:10~35mol%,CuO:8~14mol%,余量为NiO;Fe2O3、ZnO、NiO、CuO的粒度满足D50<0.5μm;
b.将满足步骤a要求的主粉体在600~800℃进行预烧;
c.以步骤b得到的主粉体的重量计,掺入0~0.2wt%的V2O5以及0~1.0wt%的Co2O3作为添加剂,经过磨细烘干后得到铁氧体材料,磨细的粒度要求D50<0.3μm,BET值为15~25m2/g。
5.根据权利要求4所述的铁氧体材料的制备方法,其特征在于:所述铁氧体材料中,P含量小于50ppm、SiO2含量小于100ppm。
6.根据权利要求4或5所述的铁氧体材料的制备方法,其特征在于:所述铁氧体材料的粒度D50<0.3μm,比表面积BET值为15~25m2/g。
7.根据权利要求6所述的铁氧体材料的制备方法,其特征在于:步骤a中,按主粉体摩尔百分比,Fe2O3:48mol%,ZnO:20mol%,CuO:8mol%,NiO:24mol%;步骤c中,V2O5以及Co2O3均为0,经过磨细烘干后得到铁氧体材料,磨细的粒度要求D50值为0.18μm,BET值为25m2/g;制得的铁氧体材料的烧结密度为5.15g/cm3,相对磁导率为125,抗弯强度为150MPa,平均晶粒尺寸为1.2μm,硫化实验△R/R为1.4%。
8.根据权利要求6所述的铁氧体材料的制备方法,其特征在于:步骤a中,按主粉体摩尔百分比,Fe2O3:48mol%,ZnO:20mol%,CuO:14mol%,NiO:18mol%;步骤c中,V2O5以及Co2O3均为0,经过磨细烘干后得到铁氧体材料,磨细的粒度要求D50值为0.25μm,BET值为18m2/g;制得的铁氧体材料的烧结密度为5.2g/cm3,相对磁导率为140,抗弯强度为155MPa,平均晶粒尺寸为1.3μm,硫化实验△R/R为-1.5%。
9.根据权利要求6所述的铁氧体材料的制备方法,其特征在于:步骤a中,按主粉体摩尔百分比,Fe2O3:48mol%,ZnO:10mol%,CuO:12mol%,NiO:30mol%;步骤c中,以步骤b得到的主粉体的重量计,掺入0.1wt%的V2O5作为添加剂,Co2O3为0,经过磨细烘干后得到铁氧体材料,磨细的粒度要求D50值为0.22μm,BET值为20m2/g;制得的铁氧体材料的烧结密度为5.25g/cm3,相对磁导率为80,抗弯强度为160MPa,平均晶粒尺寸为1.5μm,硫化实验△R/R为-0.5%。
10.根据权利要求6所述的铁氧体材料的制备方法,其特征在于:步骤a中,按主粉体摩尔百分比,Fe2O3:48mol%,ZnO:35mol%,CuO:12mol%,NiO:5mol%;步骤c中,以步骤b得到的主粉体的重量计,掺入0.5wt%的Co2O3作为添加剂,V2O5为0,经过磨细烘干后得到铁氧体材料,磨细的粒度要求D50值为0.22μm,BET值为20m2/g;制得的铁氧体材料的烧结密度为5.2g/cm3,相对磁导率为355,抗弯强度为150MPa,平均晶粒尺寸为1.5μm,硫化实验△R/R为1.6%。
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