CN115490507A - 一种宽频高强度耐热冲击镍锌铁氧体磁芯及其制备方法 - Google Patents

一种宽频高强度耐热冲击镍锌铁氧体磁芯及其制备方法 Download PDF

Info

Publication number
CN115490507A
CN115490507A CN202211162347.7A CN202211162347A CN115490507A CN 115490507 A CN115490507 A CN 115490507A CN 202211162347 A CN202211162347 A CN 202211162347A CN 115490507 A CN115490507 A CN 115490507A
Authority
CN
China
Prior art keywords
sintering
zinc ferrite
ball milling
nickel
steps
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.)
Granted
Application number
CN202211162347.7A
Other languages
English (en)
Other versions
CN115490507B (zh
Inventor
陈诗煌
付泽春
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.)
Zhongshan Dongchen Magnetic Electronic Products Co ltd
Original Assignee
Zhongshan Dongchen Magnetic Electronic Products 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 Zhongshan Dongchen Magnetic Electronic Products Co ltd filed Critical Zhongshan Dongchen Magnetic Electronic Products Co ltd
Priority to CN202211162347.7A priority Critical patent/CN115490507B/zh
Publication of CN115490507A publication Critical patent/CN115490507A/zh
Application granted granted Critical
Publication of CN115490507B publication Critical patent/CN115490507B/zh
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/26Shaped 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
    • C04B35/2608Compositions 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
    • C04B35/2633Compositions 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
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/26Shaped 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
    • C04B35/265Compositions containing one or more ferrites of the group comprising manganese or zinc and one or more ferrites of the group comprising nickel, copper or cobalt
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F3/00Cores, Yokes, or armatures
    • H01F3/08Cores, Yokes, or armatures made from powder
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3208Calcium oxide or oxide-forming salts thereof, e.g. lime
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3258Tungsten oxides, tungstates, or oxide-forming salts thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/327Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3275Cobalt oxides, cobaltates or cobaltites or oxide forming salts thereof, e.g. bismuth cobaltate, zinc cobaltite
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/327Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3279Nickel oxides, nickalates, or oxide-forming salts thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3281Copper oxides, cuprates or oxide-forming salts thereof, e.g. CuO or Cu2O
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3284Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3298Bismuth oxides, bismuthates or oxide forming salts thereof, e.g. zinc bismuthate
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/608Green bodies or pre-forms with well-defined density
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Landscapes

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

Abstract

本发明公开了一种宽频高强度耐热冲击镍锌铁氧体磁芯及其制备方法。所述宽频高强度耐热冲击镍锌铁氧体磁芯包括主成分和添加剂,所述主成分为Fe2O3、NiO、ZnO和CuO,所述添加剂为Bi2O3、WO3、Co2O3、SiO2、CaO。所述宽频高强度耐热冲击镍锌铁氧体磁芯的制备方法,包括混合球磨、预烧、二次球磨、造粒、压制、烧结。本发明通过改良配方及制作工艺和烧结工艺,制得的镍锌铁氧体磁芯同时具有高强度和高耐热冲击性,本发明的制备过程简单、可工业化生产。

Description

一种宽频高强度耐热冲击镍锌铁氧体磁芯及其制备方法
技术领域
本发明涉及软磁铁氧体技术领域,具体涉及一种宽频高强度耐热冲击镍锌铁氧体磁芯及其制备方法。
背景技术
软磁铁氧体主要包括锰锌、镍锌铁氧体材料两大系列,主要应用于计算机、通讯、电源及消费类电子产品等领域。相较于锰锌铁氧体,具有优良高频性能的镍锌铁氧体是电子器件中使用最广泛的软磁铁氧体之一。镍锌铁氧体具有化学性质稳定、制备工艺条件易控制且具有高电阻率、低电磁损耗、高机械硬度以及优异的宽频特性等优点。随着目前电子产品向轻薄化、高密度化方向发展,软磁元件尺寸越来越小,尤其是点焊工艺的出现,对磁芯强度和耐热冲击性能要求越来越高。
CN102432279A公开了一种高强度耐热冲击镍锌铁氧体及其制备方法,该镍锌铁氧体主成分以氧化物计算为:Fe2O3 45-52mol%、NiO2 0-29mol%、ZnO 20-30mol%、CuO 3-6.5mol%,辅助成分为:CaCO30.2-0.5wt%,Co2O30.01-0.09wt%,V2O50.05-0.19wt%,SiO20.8-1.5wt%。采用氧化物法制备,在一定条件下烧结,得到耐热冲击性能和机械强度良好的功率镍锌铁氧体磁芯,其磁导率和饱和磁感应强度分别在200和280附近。
CN104045333A公开了一种NiZn软磁铁氧体及其制备方法,主成分为三氧化二铁、氧化亚镍、氧化锌、氧化铜、碳酸锰、氧化镁;所述副成分包括氧化铋、碳酸钙、二氧化硅、氮化硼、硼化钛、氧化钇(稀土氧化物),得到的材料具有高磁导率、高BS、高强度和高耐热冲击性,满足SMD功率电感用软磁铁氧体材料性能要求,但是其添加剂氮化硼和硼化钛较贵,且工艺繁琐,制造成本高。
发明内容
基于背景技术存在的问题,本发明提供了一种宽频高强度耐热冲击镍锌铁氧体磁芯及其制备方法。本发明通过改良配方及制作工艺和烧结工艺,制得的镍锌铁氧体磁芯同时具有高强度和高耐热冲击性,本发明的制备过程简单、可工业化生产。
本发明通过以下技术方案实施:
一种宽频高强度耐热冲击镍锌铁氧体磁芯,所述镍锌铁氧体磁芯包括主成分和添加剂,所述主成分为Fe2O3、NiO、ZnO和CuO,所述添加剂为Bi2O3、WO3、Co2O3、SiO2、CaO;其中,主成分以各自标准物计的含量为:Fe2O345-55mol%、NiO 12-17mol%、ZnO 25-35mol%和CuO3-8mol%;所述添加剂成分相对于所述主成分总量以其各自标准物计的含量为:Bi2O30.01-0.4wt%、WO30.01-0.1wt%、Co2O30.01-0.1wt%、SiO20.01-0.5wt%、CaO 0.01-0.3wt%。
一种宽频高强度耐热冲击镍锌铁氧体磁芯的制备方法,包括以下步骤:
S1、混合球磨:将主成分Fe2O3、NiO、ZnO、CuO和添加剂中部分Bi2O3配料后进行湿法球磨混合,得到混合料A;
S2、预烧:将混合料A转入烧结炉中进行预烧,得到预烧料;
S3、二次球磨:在预烧料中加入添加剂WO3、Co2O3、SiO2、CaO和剩余部分Bi2O3,进行二次球磨,得到混合料B;
S4、造粒:在混合料B中加入粘合剂和消泡剂进行喷雾造粒,得到颗粒料;
S5、压制:将颗粒料通过专用模具在粉末成型机上压制成型得到坯件;
S6、烧结:将坯件转入烧结炉中进行烧结,烧结完成后,快速冷却,得到所述镍锌铁氧体磁芯。
进一步地,添加剂Bi2O3分两次加入,步骤S1中Bi2O3的加入量为0.01-0.2wt%,步骤S3中Bi2O3加入量为0.01-0.2wt%。
进一步地,步骤S1中球磨时间为2-3h。
进一步地,步骤S2中的预烧温度为850±20℃,预烧时间为3-4h。
进一步地,步骤S3中二次球磨时间为5-6h,二次球磨浆料粒径控制在1-5μm。
进一步地,步骤S4中的粘合剂为聚乙烯醇,聚乙烯醇的加入量为S3中混合料B固含量的0.1-0.3%;消泡剂为聚二甲基硅氧烷,聚二甲基硅氧烷的加入量为S3中混合料B固含量的0.01-0.15%。
进一步地,步骤S4中的喷雾造粒所得的颗粒料粒径为50-180μm,颗粒料的比重为1.25-1.45g/cm3,含水量≤0.4%。
进一步地,步骤S5中坯件的压制密度控制在3.0-3.5g/cm3
进一步地,步骤S6中烧结温度为950±20℃,烧结时间为5-6h;快速降温时间控制在10-15min内。
进一步地,步骤S5中坯件压制所需要的压力可通过如下公式计算:
Figure BDA0003860219590000031
其中,P为坯件压制所需要的压力,单位为Pa;
ρ为坯件压制需达到的密度,单位为g/cm3
e0为颗粒料无压力时的空隙率,单位为%;
σ为单个金属粒子的屈服应力,单位为N。
本发明的有益效果:
(1)本发明提供的宽频高强度耐热冲击镍锌铁氧体磁芯对配方进行调整,其中主成分中添加适量的CuO可以提高镍锌铁氧体的致密度和饱和磁感应强度,降低镍锌铁氧体的矫顽力;Bi2O3因其熔点低可以在烧结过程中引入液相起到助烧作用,促进镍锌铁氧体的致密度;WO3可以很好的控制晶粒的微观形貌,减小晶粒尺寸,改善镍锌铁氧体的电磁性能;Co2O3可以提高镍锌铁氧体的电阻率,降低介电损耗;SiO2和CaO可以增加晶界层厚度,提高晶界强度,同时降低材料的损耗。
(2)本发明将主成分和部分Bi2O3混合球磨进行预烧,二次球磨再加入包含剩余Bi2O3的所有添加剂部分,分两次添加Bi2O3可以明显优化高镍锌铁氧体的结构,使晶粒更加均匀,明显提高镍锌铁氧体的致密度,从而使镍锌铁氧体获得高强度。
(3)本发明镍锌铁氧体坯件烧结后采用快速降温的方法,能够阻止晶体进一步生长,控制晶体大小,提高镍锌铁氧体强度和表面硬度,提升镍锌铁氧体耐热冲击能力。
具体实施方式
下面结合具体实施例对本发明的技术方案做进一步的详述,但本发明的保护范围并不仅限于以下实施例。
本发明实施例1-6和对比例1-4制得的镍锌铁氧体磁芯的成分如表1所示:
表1
Figure BDA0003860219590000041
实施例1-6镍锌铁氧体磁芯的制备方法:
S1、混合球磨:按表1中主成分Fe2O3、NiO、ZnO和CuO的配比和添加剂中Bi2O3配料后进行湿法球磨混合,球磨时间为2.5h,得到混合料A;
S2、预烧:将混合料A转入烧结炉中进行预烧,预烧温度为850℃,预烧时间为4h,得到预烧料;
S3、二次球磨:按照表1中的配比,在预烧料中加入添加剂Bi2O3、WO3、Co2O3、SiO2、CaO,进行二次球磨,二次球磨时间为6h,二次球磨浆料粒径控制在3-5μm,得到混合料B;
S4、造粒:在混合料B中加入S3中混合料B固含量的0.2%聚乙烯醇和S3中混合料B固含量的0.1%聚二甲基硅氧烷进行喷雾造粒,得到颗粒料,颗粒料粒径为50-180μm,颗粒料的比重为1.35g/cm3左右,含水量≤0.4%;
S5、压制:将颗粒料通过专用模具在粉末成型机上压制成型得到坯件,坯件的压制密度控制在3.2g/cm3左右;
S6、烧结:将坯件转入烧结炉中进行烧结,烧结温度为950℃,烧结时间为6h,烧结完成后,快速冷却,12min内降温至室温,得到所述镍锌铁氧体磁芯。
对比例1
对比例1与实施例1的区别在于:主成分的配方不同,如表1所示,其余工艺完全相同。
对比例2
对比例2与实施例1的区别在于:混合球磨时未添加Bi2O3,全部在二次球磨时添加,其余工艺完全相同。
对比例3
对比例3与实施例1的区别在于:混合球磨时添加所有Bi2O3,二次球磨时未添加,其余工艺完全相同。
对比例4
对比例4与实施例1的区别在于:烧结完成后通过自然降温至室温,其余主成分和添加剂配方完全相同。
性能测试
将实施例1-6以及对比例1-4得到的镍锌铁氧磁芯体进行如下性能测试:
(1)初始磁导率μi:在匝数N=20Ts条件下,用HP-4284A型LCR测试仪测试镍锌铁氧体磁芯的初始磁导率;
(2)饱和磁感应强度Bs:在匝数N=20Ts条件下,用SY-8258型B-H分析仪测试镍锌铁氧体磁芯的饱和磁感应强度Bs;
(3)居里温度Tc:匝数N=20Ts条件下,用HP-4284A型LCR测试仪配合PHH-101高温试验箱,测试镍锌铁氧体磁芯的居里温度;
(4)热冲击前强度:采用三点弯曲强度测试法,用美特斯工业系统(中国)有限公司微机控制电子万能试验机测试镍锌铁氧体磁芯的机械强度,通过如下公式计算:
Figure BDA0003860219590000061
其中,R为镍锌铁氧体磁芯的机械强度,单位为MPa;Rd为镍锌铁氧体磁芯的断裂载荷,单位为N;L为下支点间跨距,单位为mm;b为镍锌铁氧体磁芯的宽度,单位为mm;h为镍锌铁氧体磁芯的厚度,单位为mm;
(5)热冲击实验:将镍锌铁氧体磁芯1/2没入温度为400℃以上锡槽中浸泡3秒,测试50只样品,记录开裂数;
(6)热冲击后强度:实验步骤同(4)热冲击前强度。
具体测试结果见表2。
表2
Figure BDA0003860219590000062
从表2结果可以看出,实施例1-3中添加CuO的镍锌铁氧体的饱和磁感应强度和热冲击前强度明显优于对比例1中未添加CuO的镍锌铁氧体。
从实施例1、4-6可以看出,分两次加入Bi2O3,镍锌铁氧体的各项性能表现优异。通过对比例2和对比例3可以看出,混合球磨时添加所有Bi2O3制得的镍锌铁氧体的各项性能优于二次球磨时添加所有Bi2O3制得的镍锌铁氧体,而本发明中通过实验发现,混合球磨时添加部分Bi2O3,二次球磨时添加部分Bi2O3,所制得的镍锌铁氧体的饱和磁感应强度、热冲击前强度和耐热冲击性能明显提升。预烧是低于烧结温度下进行的焙烧过程,在预烧过程中主成分初步发生化学反应,理论上预烧温度越高材料耐热冲击性能和强度性能越好,但温度过高,预烧粉料的活性会降低,不利于晶粒的成长,晶粒生长速率不一致导致晶粒大小不均匀增加气孔率,材料的电磁性能会下降明显。本发明通过实验发现,主成分添加部分Bi2O3球磨后进行预烧,可以在较低的预烧温度(850℃)下,明显提高所制得的镍锌铁氧体的饱和磁感应强度、热冲击前强度和耐热冲击性。
从实施例1和对比例4可以看出,本发明中烧结完成后快速降温,快速降温的方法能够阻止晶体进一步生长,控制晶体大小,明显提高了镍锌铁氧体的耐热冲击性能和强度。
在一个实施例中,步骤S5中坯件压制所需要的压力可通过如下公式计算:
Figure BDA0003860219590000071
其中,P为坯件压制所需要的压力,单位为Pa;
ρ为坯件压制需达到的密度,单位为g/cm3
e0为颗粒料无压力时的空隙率,单位为%;
σ为单个金属粒子的屈服应力,单位为N。
通过该公式能够对粉末的密度和压制所需的压力之间的变化规律进行描述,从而对所需压力进行预估,提高压制效率和质量。
最后应说明的是:以上所述实施例仅表达了本发明的几种实施方式,并不用以限制本发明创造,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,所作的任何修改、等同替换、改进等,均应包含在本发明创造的保护范围之内。因此,本发明专利的保护范围应以所附权利要求为准。

Claims (10)

1.一种宽频高强度耐热冲击镍锌铁氧体磁芯,其特征在于,所述镍锌铁氧体磁芯包括主成分和添加剂,所述主成分为Fe2O3、NiO、ZnO和CuO,所述添加剂为Bi2O3、WO3、Co2O3、SiO2、CaO;其中,主成分以各自标准物计的含量为:Fe2O345-55mol%、NiO 12-17mol%、ZnO 25-35mol%和CuO 3-8mol%;所述添加剂成分相对于所述主成分总量以其各自标准物计的含量为:Bi2O30.01-0.4wt%、WO30.01-0.1wt%、Co2O30.01-0.1wt%、SiO20.01-0.5wt%、CaO0.01-0.3wt%。
2.一种宽频高强度耐热冲击镍锌铁氧体磁芯的制备方法,其特征在于,包括以下步骤:
S1、混合球磨:将主成分Fe2O3、NiO、ZnO、CuO和添加剂中部分Bi2O3配料后进行湿法球磨混合,得到混合料A;
S2、预烧:将混合料A转入烧结炉中进行预烧,得到预烧料;
S3、二次球磨:在预烧料中加入添加剂WO3、Co2O3、SiO2、CaO和剩余部分Bi2O3,进行二次球磨,得到混合料B;
S4、造粒:在混合料B中加入粘合剂和消泡剂进行喷雾造粒,得到颗粒料;
S5、压制:将颗粒料通过模具在粉末成型机上压制成型得到坯件;
S6、烧结:将坯件转入烧结炉中进行烧结,烧结完成后,快速冷却,得到所述镍锌铁氧体磁芯。
3.根据权利要求2所述的宽频高强度耐热冲击镍锌铁氧体磁芯的制备方法,其特征在于:添加剂Bi2O3分两次加入,步骤S1中Bi2O3的加入量为0.01-0.2wt%,步骤S3中Bi2O3加入量为0.01-0.2wt%。
4.根据权利要求2所述的宽频高强度耐热冲击镍锌铁氧体磁芯的制备方法,其特征在于:步骤S1中球磨时间为2-3h。
5.根据权利要求2所述的宽频高强度耐热冲击镍锌铁氧体磁芯的制备方法,其特征在于:步骤S2中的预烧温度为850±20℃,预烧时间为3-4h。
6.根据权利要求2所述的宽频高强度耐热冲击镍锌铁氧体磁芯的制备方法,其特征在于:步骤S3中二次球磨时间为5-6h,二次球磨浆料粒径控制在1-5μm。
7.根据权利要求2所述的宽频高强度耐热冲击镍锌铁氧体磁芯的制备方法,其特征在于:步骤S4中的粘合剂为聚乙烯醇,聚乙烯醇的加入量为S3中混合料B固含量的0.1-0.3%;消泡剂为聚二甲基硅氧烷,聚二甲基硅氧烷的加入量为S3中混合料B固含量的0.01-0.15%。
8.根据权利要求2所述的宽频高强度耐热冲击镍锌铁氧体磁芯的制备方法,其特征在于:步骤S4中的喷雾造粒所得的颗粒料粒径为50-180μm,颗粒料的比重为1.25-1.45g/cm3,含水量≤0.4%。
9.根据权利要求2所述的宽频高强度耐热冲击镍锌铁氧体磁芯的制备方法,其特征在于:步骤S5中坯件的压制密度控制在3.0-3.5g/cm3
10.根据权利要求2所述的宽频高强度耐热冲击镍锌铁氧体磁芯的制备方法,其特征在于:步骤S6中烧结温度为950±20℃,烧结时间为5-6h;快速降温时间控制在10-15min内。
CN202211162347.7A 2022-09-23 2022-09-23 一种宽频高强度耐热冲击镍锌铁氧体磁芯及其制备方法 Active CN115490507B (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202211162347.7A CN115490507B (zh) 2022-09-23 2022-09-23 一种宽频高强度耐热冲击镍锌铁氧体磁芯及其制备方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202211162347.7A CN115490507B (zh) 2022-09-23 2022-09-23 一种宽频高强度耐热冲击镍锌铁氧体磁芯及其制备方法

Publications (2)

Publication Number Publication Date
CN115490507A true CN115490507A (zh) 2022-12-20
CN115490507B CN115490507B (zh) 2023-05-12

Family

ID=84469857

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202211162347.7A Active CN115490507B (zh) 2022-09-23 2022-09-23 一种宽频高强度耐热冲击镍锌铁氧体磁芯及其制备方法

Country Status (1)

Country Link
CN (1) CN115490507B (zh)

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH1050514A (ja) * 1996-04-03 1998-02-20 Tdk Corp フェライト磁性材料およびフェライトコア
JP2003321273A (ja) * 2002-04-26 2003-11-11 Tdk Corp スピネル型フェライトコアの製造方法とスピネル型フェライトコア
CN101412622A (zh) * 2008-10-31 2009-04-22 天通控股股份有限公司 高频镍铜锌铁氧体及其制备方法
CN101668719A (zh) * 2007-02-07 2010-03-10 日立金属株式会社 低损耗铁氧体及使用其的电子零件
CN101889319A (zh) * 2007-12-25 2010-11-17 日立金属株式会社 叠层电感器以及使用该叠层电感器的功率转换装置
JP2013079163A (ja) * 2011-10-03 2013-05-02 Tdk Corp フェライト組成物、フェライトコアおよび電子部品
CN104045333A (zh) * 2014-05-21 2014-09-17 肇庆冠磁科技有限公司 一种NiZn软磁铁氧体及其制备方法
CN105198395A (zh) * 2015-09-02 2015-12-30 电子科技大学 一种耐热冲击功率镍锌铁氧体及其制备方法
CN110785892A (zh) * 2017-06-13 2020-02-11 日立金属株式会社 线圈装置及天线

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH1050514A (ja) * 1996-04-03 1998-02-20 Tdk Corp フェライト磁性材料およびフェライトコア
JP2003321273A (ja) * 2002-04-26 2003-11-11 Tdk Corp スピネル型フェライトコアの製造方法とスピネル型フェライトコア
CN101668719A (zh) * 2007-02-07 2010-03-10 日立金属株式会社 低损耗铁氧体及使用其的电子零件
CN101889319A (zh) * 2007-12-25 2010-11-17 日立金属株式会社 叠层电感器以及使用该叠层电感器的功率转换装置
CN101412622A (zh) * 2008-10-31 2009-04-22 天通控股股份有限公司 高频镍铜锌铁氧体及其制备方法
JP2013079163A (ja) * 2011-10-03 2013-05-02 Tdk Corp フェライト組成物、フェライトコアおよび電子部品
CN104045333A (zh) * 2014-05-21 2014-09-17 肇庆冠磁科技有限公司 一种NiZn软磁铁氧体及其制备方法
CN105198395A (zh) * 2015-09-02 2015-12-30 电子科技大学 一种耐热冲击功率镍锌铁氧体及其制备方法
CN110785892A (zh) * 2017-06-13 2020-02-11 日立金属株式会社 线圈装置及天线

Also Published As

Publication number Publication date
CN115490507B (zh) 2023-05-12

Similar Documents

Publication Publication Date Title
CN107473727B (zh) 一种宽频宽温高功率密度低损耗锰锌软磁铁氧体材料及其制备方法
CN105565790B (zh) Yr950宽温高直流叠加低功耗锰锌铁氧体材料及其制备方法
CN111116191B (zh) 一种高磁导率低损耗锰锌软磁铁氧体材料及其制备方法
CN101552074A (zh) 一种NiZnCu铁氧体材料及其制备方法
CN110204325B (zh) 铁氧体材料及其制备方法
CN108706968B (zh) 一种低温烧结抗直流偏置NiCuZn铁氧体及制备方法
CN113185276A (zh) 常温高标软磁铁氧体材料及材料的制备方法
CN108987062A (zh) 一种铁氧体-软磁合金复合磁芯及其制备方法
CN110922179A (zh) 一种高磁导率低损耗铁氧体材料及其制备方法
CN114436636A (zh) 一种差共模电感用高磁导率锰锌铁氧体材料及其制备方法
JP2005132715A (ja) Ni−Cu−Zn系フェライト材料及びその製造方法
CN110981460B (zh) 一种高磁导率铁氧体磁性材料的制备方法
US9434622B2 (en) Sintered ferrite material, wire wound component, and producing method of sintered ferrite material
CN115490507B (zh) 一种宽频高强度耐热冲击镍锌铁氧体磁芯及其制备方法
JP2004296865A (ja) 巻き線チップインダクタ用フェライトコアとその製造方法及び巻き線チップインダクタ
CN114853461A (zh) 一种宽温低损耗NiZn软磁铁氧体材料及其制备方法
JP2007297232A (ja) 酸化物磁性材料の製造方法
CN113636838A (zh) 一种镍锌铁氧体材料及制备方法和应用
CN114133231A (zh) 镍锌铁氧体材料及其制造方法
CN112562958A (zh) 一种低温烧结锰锌软磁铁氧体材料的制备方法
CN112479697B (zh) 一种高频时兼具低温度系数和低损耗的MnZn铁氧体材料及制备方法
JP4761187B2 (ja) 酸化物磁性材料
JP2004262710A (ja) Mn−Zn系フェライトおよびその製造方法
CN110838399A (zh) 一种软磁铁氧体粉末制备方法及叠层片式电感器制备方法
JPH08310856A (ja) Ni−Cu−Znフェライト焼結体

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
GR01 Patent grant
GR01 Patent grant