CN110467449A - 一种锰锌高导软磁铁氧体材料及其制备方法和应用 - Google Patents

一种锰锌高导软磁铁氧体材料及其制备方法和应用 Download PDF

Info

Publication number
CN110467449A
CN110467449A CN201910769219.0A CN201910769219A CN110467449A CN 110467449 A CN110467449 A CN 110467449A CN 201910769219 A CN201910769219 A CN 201910769219A CN 110467449 A CN110467449 A CN 110467449A
Authority
CN
China
Prior art keywords
soft magnetic
magnetic ferrite
mnzn
height
principal component
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201910769219.0A
Other languages
English (en)
Inventor
刘培元
傅膑
盘良三
张凯
李俊
孔令才
谢振华
万里云
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
RUYUAN DONG YANG GUANG MATERIALS CO Ltd
Original Assignee
RUYUAN DONG YANG GUANG MATERIALS CO Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by RUYUAN DONG YANG GUANG MATERIALS CO Ltd filed Critical RUYUAN DONG YANG GUANG MATERIALS CO Ltd
Priority to CN201910769219.0A priority Critical patent/CN110467449A/zh
Publication of CN110467449A publication Critical patent/CN110467449A/zh
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
    • C04B35/2608—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead
    • C04B35/2633—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead containing barium, strontium or calcium
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
    • C04B35/2658—Other ferrites containing manganese or zinc, e.g. Mn-Zn ferrites
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/6261—Milling
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
    • C04B35/62675—Thermal treatment of powders or mixtures thereof other than sintering characterised by the treatment temperature
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
    • H01F1/36—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites in the form of particles
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0206—Manufacturing of magnetic cores by mechanical means
    • H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3256—Molybdenum oxides, molybdates or oxide forming salts thereof, e.g. cadmium molybdate
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3298—Bismuth oxides, bismuthates or oxide forming salts thereof, e.g. zinc bismuthate
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6562—Heating rate
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
    • C04B2235/786—Micrometer sized grains, i.e. from 1 to 100 micron

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Organic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Materials Engineering (AREA)
  • Power Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Magnetic Ceramics (AREA)
  • Soft Magnetic Materials (AREA)

Abstract

本发明公开了一种锰锌高导软磁铁氧体材料及其制备方法和应用。软磁铁氧体材料包括主成分和副成分，主成分包括Fe2O3、MnO、ZnO，所述副成分组分为：Ca2CO3、Bi2O3、MoO3、SiO2。本发明的软磁铁氧体材料的居里温度可达190℃，10KHz 0.1V的磁导率可达9897，200KHz 0.1V的磁导率可达10663，通过优化预烧温度和二次球磨工艺，从而可以较好地控制产品晶粒大小和致密性，通过综合控制预烧温度、烧结温度和粉料粒径，从而提高起始磁导率，使产品具有较高的居里温度，尤其适用于工作在180℃以下的工作环境，可广泛应用于制备汽车电子器件。

Description

一种锰锌高导软磁铁氧体材料及其制备方法和应用
技术领域
本发明涉及电子材料技术领域，更具体地，涉及一种锰锌高导软磁铁氧体材料及其制备方法和应用。
背景技术
电子材料是现代电子工业和科学技术发展的物质基础，主要是一类应用于电子技术和微电子技术中的材料，包括介电材料、半导体材料、压电与铁电材料、导电金属及其合金材料、磁性材料、光电子材料以及其他相关材料，作为电子材料之一的铁氧体磁芯材料，广泛应用于通信设备和汽车电子等领域。软磁材料在工业中的应用始于十九世纪末，应用范围极其广泛，不仅应用于家电领域、信息化领域、汽车领域和其他配套领域，更是电子元器件生产的主要原材料。而随着电子行业的发展与应用领域的扩展，对磁性材料的要求也越来越高，且对材料特性的分类要求更加细化和专业化，而目前用于汽车电感的磁性材料的温度稳定性和磁导率水平亟待提高。汽车产品在工作过程中温度会急剧升高，尤其在发动机周边器件，最高温度可达180℃，要保证这些设备能够正常使用，就必须要求使用的磁芯材料在高温下有稳定的性能。现行技术中的很多铁氧体磁芯材料虽具有较高的起始磁导率，但居里温度偏低，超过居里温度后性能失效无法正常工作；有些产品虽具备较高的居里温度，但磁导率偏低。CN101106003A公开了一种超高磁导率、高居里温度的Mn-Zn铁氧体及其制备方法，其所能达到的具体温度仅在130℃作用，无法达到目前汽车发动机周边器件最高温度180℃的使用要求。
因此，本发明提供一种新型的磁芯材料，其居里温度和磁导率都得到了较大改善，适用于180℃下的工作环境，对于改善磁芯的适用性能具有非常重要的意义。
发明内容
本发明要解决的技术问题是克服现有磁芯材料的磁导率和温度特性上的缺陷和不足，提供一种锰锌高导软磁铁氧体材料，通过特定的配方和掺杂体系，从而达到很好的磁芯材料综合性能的提升。
本发明的另一目的在于提供一种锰锌高导软磁铁氧体材料的制备方法。
本发明的又一目的在于提供锰锌高导软磁铁氧体材料在制备汽车电子器件中的应用，比如车载电感器等。
本发明上述目的通过以下技术方案实现：
一种锰锌高导软磁铁氧体材料，包括主成分和副成分，其中主成分包括如下摩尔百分比的组分：Fe2O3 52～54mol％，MnO 30～31mol％、ZnO 14～17mol％，所述副成分组分的质量百分比为：Ca2CO3 0.05～0.1wt％，Bi2O30.01～0.03wt％，MoO30.01～0.03wt％，SiO20.01～0.3wt％，其副成分的质量百分比是相对于主成分总质量的百分比。
本发明的锰锌高导软磁铁氧体材料在采用特别的配方和掺杂体系，结合烧结工艺，在保证高居里温度的同时获得高的磁导率特性，并保证高的磁通密度。
本发明的高频材料居里温度Tc≥180℃，磁导率Ui＝1000±20％，同时25℃的饱和磁通密度Bs≥510mT，具有高的磁导率，以及较高的饱和磁通密度和较高的居里温度。
优选地，所述软磁铁氧体材料的密度为5.0～5.1g/cm3。
本发明控制密度为5.0～5.1g/cm3的原因为：提高材料的致密化，减少气孔率，可以获得高的磁导率。
优选地，所述软磁铁氧体材料的晶粒大小为30～40μm。例如可以为30μm，40μm，50μm。
本发明控制晶粒大小为30～50μm的原因为：控制晶粒的大小，获得致密均匀的晶粒尺寸，晶粒过小，磁导率偏低，晶粒过大容易生成异常晶粒长大，恶化磁导率。
优选地，所述软磁铁氧体材料的晶粒大小为40μm。
更优选地，所述软磁铁氧体材料的密度为5.05g/cm3，晶粒大小为40μm。
作为本发明的一种实现方案，上述锰锌高导软磁铁氧体材料可以通过如下方法制备得到：
S1：将主成分混合破碎，循环混合后加入聚乙烯醇溶液，烘干后预烧结；
S2：将S1中预烧结的主成分与副成分混合二次破碎，制得粒度为0.8～1.0μm的磨细粉料；
S3：将磨细粉料进行喷雾造粒，制得80～180μm的喷雾粉料，将喷雾粉料压制成型，制得密度为3.0～3.1g/cm3的生坯；
S4：将S3所述生坯在惰性气体保护下，在1350～1380℃下烧结定型，冷却后制得所述软磁铁氧体材料。
粉料制作上，本发明的料将的平均粒径控制比常规的小，0.8～1.0μm(通过透气法测试)，常规产品在1.0～1.2μm左右，便于控制产品最终晶粒不能太大，从而控制产品的低温烧结。
在产品烧结上，控制产品烧结温度在1350～1380℃，相对于常规10K料烧结温度1380℃～1420℃更低，使产品最终密度控制在5.01g/cm3左右。例如烧结温度可以为1350℃、1370℃或1380℃。
优选地，S1中所述预烧结升温速度为2～2.5℃/min。例如可以为2℃/min或2.5℃/min。
优选地，S3中所述烧结定型升温速度为1～2℃/min。例如可以为1℃/min或2℃/min。
优选地，S1中所述破碎时间为40～50min，循环混合时间为10～20min。
优选地，S1中所述预烧结温度为880～920℃，保温2～3h。相对于常规的预烧结温度850℃～880℃，本发明的预烧结温度更高，一方面有利于饱和磁铁密度的提高，另一方面有利于粉碎粒径的一致性控制。例如可以为880℃、900℃或920℃。
优选地，S3中所述二次破碎时间为90～120min。相对于常规的加入辅料混合破碎时间50～80min，本发明的二次破碎时间更长，可以获得细小均匀的二次粒径，提高粉体活性，降低烧结温度。
优选地，S3中采用成型油压机，压制H25-15-7.5样环。
一种锰锌高导软磁铁氧体材料在制备汽车电子器件中的应用也在本发明的保护范围内。本发明的高居里温度高磁导率软磁铁氧体材料尤其适用于工作温度会达到180℃的环境，可广泛应用于汽车电子等，比如车载电感器。
与现有技术相比，本发明的有益效果是：
(1)本发明提供了一种锰锌高导软磁铁氧体材料，采用特定的配方和掺杂体系，在保证高居里温度的同时获得高的磁导率特性，并保证高的磁通密度，材料的居里温度可达190℃，10KHz 0.1V的磁导率可达9897，200KHz 0.1V的磁导率可达10663。
(2)本发明提供了一种锰锌高导软磁铁氧体材料的制备方法，通过优化预烧温度和二次球磨工艺，从而可以较好地控制产品晶粒大小和致密性，通过综合控制预烧温度、烧结温度和粉料粒径，从而提高起始磁导率，使产品具有较高的居里温度，尤其适用于工作在180℃以下的工作环境，可广泛应用于制备汽车电子器件。
具体实施方式
下面结合具体实施方式对本发明作进一步的说明，但实施例并不对本发明做任何形式的限定。除非另有说明，本发明实施例采用的原料试剂为常规购买的原料试剂。
实施例1
一种锰锌高导软磁铁氧体材料，其原料包括主成分和副成分，其中主成分包括如下摩尔百分比的组分：Fe2O3 53％，MnO 31％、ZnO 16％，所述副成分组分的质量百分比为：Ca2CO3 0.1t％，Bi2O30.03％，MoO30.03％，SiO2 0.3％，其副成分的质量百分比是相对于主成分总质量的百分比，软磁铁氧体材料的密度为5.05g/cm3，软磁铁氧体材料的晶粒大小为40μm。
实施例2
一种锰锌高导软磁铁氧体材料，其原料包括主成分和副成分，其中主成分包括如下摩尔百分比的组分：Fe2O3 54％，MnO 31％、ZnO 15％，所述副成分组分的质量百分比为：Ca2CO3 0.1t％，Bi2O30.03％，MoO30.03％，SiO2 0.3％，其副成分的质量百分比是相对于主成分总质量的百分比，软磁铁氧体材料的密度为5.01g/cm3，软磁铁氧体材料的晶粒大小为40μm。
实施例3
一种锰锌高导软磁铁氧体材料，其原料包括主成分和副成分，其中主成分包括如下摩尔百分比的组分：Fe2O3 53％，MnO 30.5％、ZnO 16.5％，所述副成分组分的质量百分比为：Ca2CO3 0.1t％，Bi2O30.03％，MoO30.03％，SiO2 0.3％，其副成分的质量百分比是相对于主成分总质量的百分比，软磁铁氧体材料的密度为5.0g/cm3，软磁铁氧体材料的晶粒大小为30μm。
实施例4
一种锰锌高导软磁铁氧体材料，其原料包括主成分和副成分，其中主成分包括如下摩尔百分比的组分：Fe2O3 52％，MnO 30％、ZnO 14％，所述副成分组分的质量百分比为：Ca2CO3 0.1t％，Bi2O30.03％，MoO30.03％，SiO2 0.3％，其副成分的质量百分比是相对于主成分总质量的百分比，软磁铁氧体材料的密度为5.1g/cm3，软磁铁氧体材料的晶粒大小为40μm。
实施例5
一种锰锌高导软磁铁氧体材料，其原料包括主成分和副成分，其中主成分包括如下摩尔百分比的组分：Fe2O3 53％，MnO 31％、ZnO 16％，所述副成分组分的质量百分比为：Ca2CO3 0.05％，Bi2O30.01％，MoO30.03％，SiO2 0.02％，其副成分的质量百分比是相对于主成分总质量的百分比，软磁铁氧体材料的密度为5.01g/cm3，软磁铁氧体材料的晶粒大小为35μm。
实施例6
一种锰锌高导软磁铁氧体材料的制备方法，包括如下步骤：
S1：对主成分按摩尔百分比含量进行配比，混合破碎，破碎时间为50min循环混合20min后加入聚乙烯醇溶液，烘干后预烧结，预烧结温度为920℃，升温速度为2℃/min，保温3h；
S2：将S1中预烧结的主成分与副成分组合二次破碎，二次破碎时间为120min，制得粒度为0.8μm的磨细粉料；
S3：将磨细粉料进行喷雾造粒，制得150μm的喷雾粉料；然后将喷雾粉料压制成型，制得密度为3.05g/cm3的生坯；
S4：将S3所述生坯在惰性气体保护下，在1370℃下烧结定型，冷却后制得所述高居里温度、高饱和磁通密度锰锌高磁导率软磁铁氧体材料，铁氧体材料的密度为5.05g/cm3，铁氧体材料的晶粒大小为35μm。
实施例7
一种锰锌高导软磁铁氧体材料的制备方法，包括如下步骤：
S1：对主成分按摩尔百分比含量进行配比，混合破碎，破碎时间为50min循环混合20min后加入聚乙烯醇溶液，烘干后预烧结，预烧结温度为880℃，升温速度为2℃/min，保温3h；
S2：将S1中预烧结的主成分与副成分组合二次破碎，二次破碎时间为90min，制得粒度为0.9μm的磨细粉料；
S3：将磨细粉料进行喷雾造粒，制得80μm的喷雾粉料；然后将喷雾粉料压制成型，制得密度为3.05g/cm3的生坯；
S4：将S3所述生坯在惰性气体保护下，在1380℃下烧结定型，冷却后制得所述高居里温度、高磁导率软磁铁氧体材料，铁氧体材料的密度为5.0g/cm3，铁氧体材料的晶粒大小为45μm。
实施例8
一种锰锌高导软磁铁氧体材料的制备方法，包括如下步骤：
S1：对主成分按摩尔百分比含量进行配比，混合破碎，破碎时间为50min循环混合20min后加入聚乙烯醇溶液，烘干后预烧结，预烧结温度为880℃，升温速度为2℃/min，保温3h；
S2：将S1中预烧结的主成分与副成分组合二次破碎，二次破碎时间为90min，制得粒度为0.9μm的磨细粉料；
S3：将磨细粉料进行喷雾造粒，制得80μm的喷雾粉料；然后将喷雾粉料压制成型，制得密度为3.05g/cm3的生坯；
S4：将S3所述生坯在惰性气体保护下，在1350℃下烧结定型，冷却后制得所述高居里温度、高磁导率软磁铁氧体材料，铁氧体材料的密度为5.0g/cm3，铁氧体材料的晶粒大小为35μm。
对比例1
一种锰锌高导软磁铁氧体材料的制备方法，包括如下步骤：
S1：对主成分按摩尔百分比含量进行配比，混合破碎，破碎时间为50min循环混合20min后加入聚乙烯醇溶液，烘干后预烧结，预烧结温度为850℃，保温3h；
S2：将S1中预烧结的主成分与副成分组合二次破碎，二次破碎时间为90min，制得粒度为0.9μm的磨细粉料；
S3：将磨细粉料进行喷雾造粒，制得80μm的喷雾粉料；然后将喷雾粉料压制成型，制得密度为3.05g/cm3的生坯；
S4：将S3所述生坯在惰性气体保护下，在1420℃下烧结定型，冷却后制得所述高居里温度、高磁导率软磁铁氧体材料，铁氧体材料的密度为5.1g/cm3，铁氧体材料的晶粒大小为45μm。
结果检测
对实施例1的高居里温度、高磁导率软磁铁氧体材料的性能进行检测，检测结果如表1所示。其中μi为起始磁导率，Bs为饱和磁通密度，Tc为居里温度。
μi和Tc数据监测方法为：HP4284电感仪。
Bs数据检测方法为：使用岩崎SY8218仪器测试。
检测结果见表1。
表1
从上述实施例数据可以看出，本发明的保护范围内的软磁铁氧体材料的居里温度Tc可以达到185～190℃，10KHz 0.1V的起始磁导率可达1000±20％，具有高居里温度和高磁导率。
显然，本发明的上述实施例仅仅是为清楚地说明本发明所作的举例，而并非是对本发明的实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。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，均应包含在本发明权利要求的保护范围之内。

Claims (10)

1.一种锰锌高导软磁铁氧体材料，其特征在于，包括主成分和副成分，其中主成分包括如下摩尔百分比的组分：Fe2O3 52～54％，MnO 30～31％、ZnO 14～17％，所述副成分组分的质量百分比为：Ca2CO3 0.05～0.1％，Bi2O3 0.01～0.03％，MoO3 0.01～0.03％，SiO2 0.01～0.3％，其副成分的质量百分比是相对于主成分总质量的百分比。
2.如权利要求1所述锰锌高导软磁铁氧体材料，其特征在于，所述软磁铁氧体材料的密度为5.0～5.1g/cm3。
3.如权利要求1所述锰锌高导软磁铁氧体材料，其特征在于，所述软磁铁氧体材料的晶粒大小为30～50μm。
4.如权利要求3所述锰锌高导软磁铁氧体材料，其特征在于，所述软磁铁氧体材料的晶粒大小为40μm。
5.如权利要求3所述锰锌高导软磁铁氧体材料，其特征在于，所述软磁铁氧体材料的密度为5.05g/cm3，晶粒大小为40μm。
6.权利要求1～5任意一项所述锰锌高导软磁铁氧体材料的制备方法，其特征在于，包括如下步骤：
S1：将主成分混合破碎，循环混合后加入聚乙烯醇溶液，烘干后预烧结；
S2：将S1中预烧结的主成分与副成分混合二次破碎，制得粒度为0.8～1.0μm的磨细粉料；
S3：将磨细粉料进行喷雾造粒，制得80～180μm的喷雾粉料，将喷雾粉料压制成型，制得密度为3.0～3.1g/cm3的生坯；
S4：将S3所述生坯在惰性气体保护下，在1350～1380℃下烧结定型，冷却后制得所述软磁铁氧体材料。
7.根据权利要求6所述制备方法，其特征在于，S1中所述破碎时间为40～50min，循环混合时间为10～20min。
8.根据权利要求6所述制备方法，其特征在于，S1中所述预烧结温度为880～920℃，保温2～3h。
9.根据权利要求6所述制备方法，其特征在于，S3中所述二次破碎时间为90～120min。
10.权利要求1～5任意一项所述锰锌高导软磁铁氧体材料在制备汽车电子器件中的应用。
CN201910769219.0A 2019-08-20 2019-08-20 一种锰锌高导软磁铁氧体材料及其制备方法和应用 Pending CN110467449A (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910769219.0A CN110467449A (zh) 2019-08-20 2019-08-20 一种锰锌高导软磁铁氧体材料及其制备方法和应用

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910769219.0A CN110467449A (zh) 2019-08-20 2019-08-20 一种锰锌高导软磁铁氧体材料及其制备方法和应用

Publications (1)

Publication Number Publication Date
CN110467449A true CN110467449A (zh) 2019-11-19

Family

ID=68512307

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910769219.0A Pending CN110467449A (zh) 2019-08-20 2019-08-20 一种锰锌高导软磁铁氧体材料及其制备方法和应用

Country Status (1)

Country Link
CN (1) CN110467449A (zh)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111170731A (zh) * 2019-12-30 2020-05-19 江门安磁电子有限公司 一种锰锌高磁导率高居里温度高频材料及其制备方法
CN112707724A (zh) * 2020-12-29 2021-04-27 日照亿鑫电子材料有限公司 一种高磁导率锰锌铁氧体磁性材料及其制备方法
CN115010480A (zh) * 2022-07-04 2022-09-06 娄底市玖鑫电子科技有限公司 一种锰锌铁氧体kah100材料制备方法
CN115368125A (zh) * 2022-06-18 2022-11-22 信丰天科磁业有限公司 一种高抗折强度锰锌软磁铁氧体材料及其制造方法

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005289667A (ja) * 2004-03-31 2005-10-20 Tdk Corp ＭｎＺｎ系フェライト及びその製造方法
CN1810710A (zh) * 2006-02-27 2006-08-02 乳源瑶族自治县东阳光实业发展有限公司 一种宽温较高磁导率锰锌系铁氧体及其制备方法
CN101475366A (zh) * 2008-12-30 2009-07-08 横店集团东磁股份有限公司 具有高磁导率的宽频锰锌铁氧体材料及其制备方法
CN101696107A (zh) * 2009-10-26 2010-04-21 横店集团东磁股份有限公司 高初始磁导率高居里温度的Mn-Zn铁氧体材料及其制备方法
CN102231312A (zh) * 2011-04-16 2011-11-02 江门安磁电子有限公司 一种低THD宽频高磁导率MnZn铁氧体材料及其制造方法
CN102360917A (zh) * 2011-08-12 2012-02-22 临沂春光磁业有限公司 一种宽频高导锰锌铁氧体磁芯的制造方法
CN104402424B (zh) * 2014-11-07 2017-10-24 乳源东阳光磁性材料有限公司 高饱和磁通密度、高直流叠加、高居里温度的镍锌铁氧体材料及其制备方法

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005289667A (ja) * 2004-03-31 2005-10-20 Tdk Corp ＭｎＺｎ系フェライト及びその製造方法
CN1810710A (zh) * 2006-02-27 2006-08-02 乳源瑶族自治县东阳光实业发展有限公司 一种宽温较高磁导率锰锌系铁氧体及其制备方法
CN101475366A (zh) * 2008-12-30 2009-07-08 横店集团东磁股份有限公司 具有高磁导率的宽频锰锌铁氧体材料及其制备方法
CN101696107A (zh) * 2009-10-26 2010-04-21 横店集团东磁股份有限公司 高初始磁导率高居里温度的Mn-Zn铁氧体材料及其制备方法
CN102231312A (zh) * 2011-04-16 2011-11-02 江门安磁电子有限公司 一种低THD宽频高磁导率MnZn铁氧体材料及其制造方法
CN102360917A (zh) * 2011-08-12 2012-02-22 临沂春光磁业有限公司 一种宽频高导锰锌铁氧体磁芯的制造方法
CN104402424B (zh) * 2014-11-07 2017-10-24 乳源东阳光磁性材料有限公司 高饱和磁通密度、高直流叠加、高居里温度的镍锌铁氧体材料及其制备方法

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
夏德贵等编著: "《软磁铁氧体制造原理与技术》", 31 December 2010, 陕西科学技术出版社 *
焦宝祥著: "《功能与信息材料》", 31 May 2011, 华东理工大学出版社 *
韩志全编著: "《铁氧体及其磁性物理》", 31 May 2010, 航空工业出版社 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111170731A (zh) * 2019-12-30 2020-05-19 江门安磁电子有限公司 一种锰锌高磁导率高居里温度高频材料及其制备方法
CN112707724A (zh) * 2020-12-29 2021-04-27 日照亿鑫电子材料有限公司 一种高磁导率锰锌铁氧体磁性材料及其制备方法
CN115368125A (zh) * 2022-06-18 2022-11-22 信丰天科磁业有限公司 一种高抗折强度锰锌软磁铁氧体材料及其制造方法
CN115010480A (zh) * 2022-07-04 2022-09-06 娄底市玖鑫电子科技有限公司 一种锰锌铁氧体kah100材料制备方法

Similar Documents

Publication Publication Date Title
CN110467449A (zh) 一种锰锌高导软磁铁氧体材料及其制备方法和应用
CN110156451B (zh) 一种高阻抗的贫铁锰锌铁氧体材料及其制备方法
CN104529425B (zh) 一种宽温高磁导率MnZn铁氧体材料及其制造方法
CN109851346A (zh) 一种高频锰锌软磁铁氧体材料及其制备方法和应用
CN102603279A (zh) 一种高强度高Bs镍锌铁氧体及其制备方法
CN107352993A (zh) 一种高频锰锌软磁铁氧体材料及其制备方法
CN105993053B (zh) 复合软磁材料及其制备方法
CN108640670B (zh) 高Bs值、低功率损耗软磁铁氧体材料及磁芯的制备方法
CN108706968B (zh) 一种低温烧结抗直流偏置NiCuZn铁氧体及制备方法
CN101337810A (zh) 一种(MgZnCa)TiO3微波陶瓷介质材料及其制备方法
CN108863333A (zh) 一种制备高性能NiZn铁氧体的Cu、V、Bi、Co离子联合替代方法
CN111233452A (zh) 一种高频高阻抗的贫铁锰锌铁氧体及其制备方法
CN108314440A (zh) 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
CN106542818A (zh) 一种高频低损耗锰锌铁氧体材料及制备工艺
CN113185276A (zh) 常温高标软磁铁氧体材料及材料的制备方法
CN106518052B (zh) 一种制备细晶钛酸钡热敏陶瓷的方法及其产品
CN104513059B (zh) 一种超宽温高磁导率MnZn铁氧体材料及其制造方法
JP3907642B2 (ja) フェライト材料及びフェライト材料の製造方法
CN109608185A (zh) 一种高性能锰锌铁氧体材料及其制备方法
CN110467450A (zh) 一种高频锰锌软磁铁氧体材料及其制备方法和应用
CN109553407A (zh) 一种高频低频兼容的锰锌功率材料及其制备方法和应用
CN108046791B (zh) 一种以纳米MnZn铁氧体粉体制备铁氧体的方法
CN103664168B (zh) 一种BCTZ-xLa体系多功能电子陶瓷的制备方法
Yan et al. Effects of V2O5 addition on the microstructure and microwave dielectric properties of ZnNb2O6 ceramics
CN114773047A (zh) 一种宽频高阻抗的锰锌铁氧体材料及其制备方法和应用

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20191119

RJ01 Rejection of invention patent application after publication