CN112125655A - 高温高频低损耗的铁氧体材料的制备方法 - Google Patents
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Abstract
本发明涉及铁氧体材料的技术领域,公开了高温高频低损耗的铁氧体材料的制备方法,包括以下制备步骤:1)、采用配方为52~58mol%三氧化二铁、9~13mol%氧化锌、0.5~5mol%氧化镍,31~38mol%碳酸锰混合研磨形成研磨粉料;2)、将研磨粉料在950~1050℃温度下预烧形成烧制粉料;3)、将烧制粉料按质量比加入二氧化锡、二氧化钛以及五氧化二钒,并再次研磨粉料的粒径达到亚微米级的初级粉料;4)、在初级粉料中添加有机黏合剂,成型为粒状胚料;5)、将粒状胚料放置在烧结炉中高温烧结数小时,形成高温高频低损耗铁氧体材料;达到降低高温高频条件下功率损耗的目的。
Description
技术领域
本发明专利涉及铁氧体材料的技术领域,具体而言,涉及高温高频低损耗的铁氧体材料的制备方法。
背景技术
铁氧体材料,其主成分含有规定量的三氧化二铁、氧化锰、氧化锌以及氧化镍的MnNiZn系的铁氧体材料,另外,其含有规定量的氧化铋、氧化镁、氧化钴,以此构成铁氧体材料,因此,铁氧体材料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MnNiZn系铁氧体材料。
目前,铁氧体材料的制备工艺需要经过以下多个步骤,依序进行配方、一次球磨、预烧、掺杂、二次球磨、造粒成型、烧结等。这些工艺的目的都是增大铁氧体材料的晶界电阻率,降低高频下的涡流损耗,达到降低高频条件下损耗的目的。
现有技术中,上述公开的铁氧体材料的制备方法,均难以达到高温高频条件下,功率损耗低的目的。
发明内容
本发明的目的在于提供高温高频低损耗的铁氧体材料的制备方法,旨在解决现有技术中,铁氧体材料的制备方法,难以达到高温高频条件下,功率损耗低的问题。
本发明是这样实现的,高温高频低损耗的铁氧体材料的制备方法,包括以下制备步骤:
1)、采用配方为52~58mol%三氧化二铁、9~13mol%氧化锌、0.5~5mol%氧化镍,31~38mol%碳酸锰混合均匀研磨,形成研磨粉料;
2)、将步骤1)所得的研磨粉料在950~1050℃温度下预烧,形成烧制粉料;
3)、将步骤2)所得的烧制粉料按质量比加入以下添加剂:二氧化锡、二氧化钛以及五氧化二钒,并再次研磨,使研磨后的粉料的粒径达到亚微米级的初级粉料;
4)、在步骤3)所得的初级粉料中添加有机黏合剂,并将初级粉料造粒成型为粒状胚料;
5)、将步骤4)所得的粒状胚料放置在烧结炉中高温烧结数小时,粒状胚料形成高温高频低损耗铁氧体材料。
进一步的,所述步骤1)中,采用球磨方式制得所述研磨粉料。
进一步的,在所述步骤5)中,在烧结粒状胚料的过程中,所述烧结炉内部处于弱氧化状态。
进一步的,在所述步骤5)中,在烧结粒状胚料的过程中,所述烧结炉内部的氧分压为1.5%~5%的弱氧化状态。
进一步的,所述的步骤5)中,在烧结粒状胚料的过程中,所述烧结炉内部的烧结温度为1320℃。
进一步的,在所述步骤5)中,粒状胚料在烧结炉中的烧结时间为2~4h。
进一步的,在所述步骤2)中,所述研磨粉料的预烧时间为1.5h~2.5h。
进一步的,在所述步骤4)中,添加到所述初级粉料中的有机黏合剂的质量配比为7wt%-8wt%。
进一步的,在所述步骤3)中,将添加添加剂的烧制粉料进行球磨。
进一步的,在所述步骤3)中,添加到所述烧制粉料中的添加剂的质量配比是0.02~0.3wt%二氧化锡、0.02~0.3wt%二氧化钛、0.02~0.3wt%五氧化二钒。
与现有技术相比,本发明提供的高温高频低损耗的铁氧体材料的制备方法,采用适当的配方研磨为研磨粉料,在预烧形成的烧制粉料中加入添加剂并研磨形成初级粉料,在初级粉料中添加有机黏合剂形成粒状胚料,并将粒状胚料进行烧结,增大材料的晶界电阻率,降低高频条件下的涡流损耗,调整其特性曲线二峰温度点,从而达到降低高温高频条件下功率损耗的目的。在超过120~180℃的较高工作温度下功率损耗最低,各项技术指标良好。在100~1000K Hz频率范围下有着较低的功率损耗。
附图说明
图1是本发明提供的高温高频低损耗的铁氧体材料的P~T测试曲线;
图2是本发明提供的高温高频低损耗的铁氧体材料(曲线a)与常规铁氧体材料(曲线b和c)的Q~F测试曲线。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合附图及实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。
以下结合具体实施例对本发明的实现进行详细的描述。
本实施例的附图中相同或相似的标号对应相同或相似的部件;在本发明的描述中,需要理解的是,若有术语“上”、“下”、“左”、“右”等指示的方位或位置关系为基于附图所示的方位或位置关系,仅是为了便于描述本发明和简化描述,而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作,因此附图中描述位置关系的用语仅用于示例性说明,不能理解为对本专利的限制,对于本领域的普通技术人员而言,可以根据具体情况理解上述术语的具体含义。
参照图1-2所示,为本发明提供的较佳实施例。
高温高频低损耗的铁氧体材料的制备方法,包括以下制备步骤:
1)、采用配方为52~58mol%三氧化二铁、9~13mol%氧化锌、0.5~5mol%氧化镍,31~38mol%碳酸锰混合均匀研磨,形成研磨粉料;
2)、将步骤1)所得的研磨粉料在950~1050℃温度下预烧,形成烧制粉料;
3)、将步骤2)所得的烧制粉料按质量比加入以下添加剂:二氧化锡、二氧化钛以及五氧化二钒,并再次研磨,使研磨后的粉料的粒径达到亚微米级的初级粉料;
4)、在步骤3)所得的初级粉料中添加有机黏合剂,并将初级粉料造粒成型为粒状胚料;
5)、将步骤4)所得的粒状胚料放置在烧结炉中高温烧结数小时,粒状胚料形成高温高频低损耗铁氧体材料。
上述提供的高温高频低损耗的铁氧体材料的制备方法,采用适当的配方研磨为研磨粉料,在预烧形成的烧制粉料中加入添加剂并研磨形成初级粉料,在初级粉料中添加有机黏合剂形成粒状胚料,并将粒状胚料进行烧结,增大材料的晶界电阻率,降低高频条件下的涡流损耗,调整其特性曲线二峰温度点,从而达到降低高温高频条件下功率损耗的目的。
通过微调配方和烧结工艺,可以制作出系列铁氧体材料,根据不同的使用条件,对应选用合适性能特点的铁氧体材料
在超过120~180℃的较高工作温度下功率损耗最低,各项技术指标良好。在100~1000K Hz频率范围下有着较低的功率损耗。
在步骤1)中,采用球磨方式制得研磨粉料。
在步骤5)中,在烧结粒状胚料的过程中,烧结炉内部处于弱氧化状态。
在步骤5)中,在烧结粒状胚料的过程中,烧结炉内部的氧分压为1.5%~5%的弱氧化状态。
在步骤5)中,在烧结粒状胚料的过程中,烧结炉内部的烧结温度为1320℃。
在步骤5)中,粒状胚料在烧结炉中的烧结时间为2~4h。
在步骤2)中,研磨粉料的预烧时间为1.5h~2.5h。
在步骤4)中,添加到所述初级粉料中的有机黏合剂的质量配比为7wt%-8wt%。
在步骤3)中,将添加添加剂的烧制粉料进行球磨。
在步骤3)中,添加到烧制粉料中的添加剂的质量配比是0.02~0.3wt%二氧化锡、0.02~0.3wt%二氧化钛、0.02~0.3wt%五氧化二钒。
以下提供一较佳的具体实施例。
高温高频低损耗的铁氧体材料的制备方法,包括以下制备步骤:
步骤1)、采用配方为54.2mol%三氧化二铁、11.5mol%氧化锌、1.5mol%氧化镍、32.8mol%碳酸锰球磨混合均匀,形成研磨粉料;
步骤2)、将步骤1)所制得的形成研磨粉料在980℃温度下预烧2小时,形成烧制粉料;
步骤3)、将步骤2)所得的烧制粉料按质量比加入以下添加剂:0.05wt%二氧化锡、0.05wt%二氧化钛,0.05wt%五氧化二钒,并再次球磨,使球磨后的粉料粒径达到亚微米级的初级粉料;
步骤4)、造粒成型,将步骤3所得的初级粉料中加入7wt%的有机黏合剂,混匀造粒按需要的形状尺寸成型;
步骤5)、烧结,将步骤4所得的粒状胚料放置在烧结炉中,在氧分压为2%的弱氧化气氛,1320℃温度下烧结3小时。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.高温高频低损耗的铁氧体材料的制备方法,其特征在于,包括以下制备步骤:
1)、采用配方为52~58mol%三氧化二铁、9~13mol%氧化锌、0.5~5mol%氧化镍,31~38mol%碳酸锰混合均匀研磨,形成研磨粉料;
2)、将步骤1)所得的研磨粉料在950~1050℃温度下预烧,形成烧制粉料;
3)、将步骤2)所得的烧制粉料按质量比加入以下添加剂:二氧化锡、二氧化钛以及五氧化二钒,并再次研磨,使研磨后的粉料的粒径达到亚微米级的初级粉料;
4)、在步骤3)所得的初级粉料中添加有机黏合剂,并将初级粉料造粒成型为粒状胚料;
5)、将步骤4)所得的粒状胚料放置在烧结炉中高温烧结数小时,粒状胚料形成高温高频低损耗铁氧体材料。
2.根据权利要求1所述的高温高频低损耗的铁氧体材料的制备方法,其特征在于,所述步骤1)中,采用球磨方式制得所述研磨粉料。
3.根据权利要求1或2所述的高温高频低损耗的铁氧体材料的制备方法,其特征在于,在所述步骤5)中,在烧结粒状胚料的过程中,所述烧结炉内部处于弱氧化状态。
4.根据权利要求1或2所述的高温高频低损耗的铁氧体材料的制备方法,其特征在于,在所述步骤5)中,在烧结粒状胚料的过程中,所述烧结炉内部的氧分压为1.5%~5%的弱氧化状态。
5.根据权利要求1或2所述的高温高频低损耗的铁氧体材料的制备方法,其特征在于,所述的步骤5)中,在烧结粒状胚料的过程中,所述烧结炉内部的烧结温度为1320℃。
6.根据权利要求1或2所述的高温高频低损耗的铁氧体材料的制备方法,其特征在于,在所述步骤5)中,粒状胚料在烧结炉中的烧结时间为2~4h。
7.根据权利要求1或2所述的高温高频低损耗的铁氧体材料的制备方法,其特征在于,在所述步骤2)中,所述研磨粉料的预烧时间为1.5h~2.5h。
8.根据权利要求1或2所述的高温高频低损耗的铁氧体材料的制备方法,其特征在于,在所述步骤4)中,添加到所述初级粉料中的有机黏合剂的质量配比为7wt%-8wt%。
9.根据权利要求1或2所述的高温高频低损耗的铁氧体材料的制备方法,其特征在于,在所述步骤3)中,将添加添加剂的烧制粉料进行球磨。
10.根据权利要求1或2所述的高温高频低损耗的铁氧体材料的制备方法,其特征在于,在所述步骤3)中,添加到所述烧制粉料中的添加剂的质量配比是0.02~0.3wt%二氧化锡、0.02~0.3wt%二氧化钛、0.02~0.3wt%五氧化二钒。
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