CN113929445B - 一种永磁铁氧体预烧料的制备方法 - Google Patents

一种永磁铁氧体预烧料的制备方法 Download PDF

Info

Publication number
CN113929445B
CN113929445B CN202111123603.7A CN202111123603A CN113929445B CN 113929445 B CN113929445 B CN 113929445B CN 202111123603 A CN202111123603 A CN 202111123603A CN 113929445 B CN113929445 B CN 113929445B
Authority
CN
China
Prior art keywords
equal
presintering
sintering material
permanent magnetic
magnetic ferrite
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.)
Active
Application number
CN202111123603.7A
Other languages
English (en)
Other versions
CN113929445A (zh
Inventor
丁伯明
胡良权
叶华
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.)
Hengdian Group DMEGC Magnetics Co Ltd
Original Assignee
Hengdian Group DMEGC Magnetics 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 Hengdian Group DMEGC Magnetics Co Ltd filed Critical Hengdian Group DMEGC Magnetics Co Ltd
Priority to CN202111123603.7A priority Critical patent/CN113929445B/zh
Publication of CN113929445A publication Critical patent/CN113929445A/zh
Application granted granted Critical
Publication of CN113929445B publication Critical patent/CN113929445B/zh
Active legal-status Critical Current
Anticipated expiration legal-status Critical

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
    • C04B35/622—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
    • C04B35/62645—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
    • 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
    • C04B35/6268—Thermal treatment of powders or mixtures thereof other than sintering characterised by the applied pressure or type of atmosphere, e.g. in vacuum, hydrogen or a specific oxygen pressure
    • 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
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3213—Strontium oxides 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
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3227—Lanthanum oxide 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
    • C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3272—Iron oxides or oxide forming salts thereof, e.g. hematite, magnetite
    • 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
    • C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3275—Cobalt oxides, cobaltates or cobaltites or oxide forming salts thereof, e.g. bismuth cobaltate, zinc cobaltite
    • 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
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
    • 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
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
    • 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
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602—Making the green bodies or pre-forms by moulding
    • 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
    • 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
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658—Atmosphere during thermal treatment
    • C04B2235/6583—Oxygen containing atmosphere, e.g. with changing oxygen pressures
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding

Landscapes

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

Abstract

本发明涉及永磁铁氧体制造领域，为了克服现有预烧料的制备方法离子交换率低、对预烧料性能提升不足，提供一种永磁铁氧体预烧料的制备方法。通过预压增大混合原料间的接触面积，提升离子交换率，提高离子分散均匀性，再控制预烧的温度和氧气浓度，最优化条件下进行预烧，提升预烧料的性能，为后续制得性能优良的永磁铁氧体打下基础。

Description

一种永磁铁氧体预烧料的制备方法
技术领域
本发明涉及永磁铁氧体制造领域，尤其是一种永磁铁氧体预烧料的制备方法。
背景技术
预烧是氧化物法生产永磁铁氧体的重要工序之一，对产品的质量起到重要的作用，预烧的目的是将混合料在一定温度下保温数小时，使混合料颗粒间产生初步的固相反应，生成部分铁氧体。其作用主要体现在降低化学活性的不均匀性、降低烧结产品的收缩率、提高产品的烧结密度和易于成型等方面。气氛以及气氛和温度的相互匹配是预烧的关键，总的来说，需要氧化气氛，在烘干、排出水分初步氧化分解、预烧、以及无机盐的分解和亚铁的氧化阶段都需要在氧化气氛中完成。
中国专利公开号CN 106747390B，公开了一种锶铁氧体预烧料及其制备方法，其特征在于，包括以下步骤：a、按摩尔比Fe2O3﹕SrO＝6.2～6.3﹕1进行计算，称取原料铁鳞和碳酸锶，加入高岭土，混合均匀后加水球磨2.5～3.5h，得到混合浆料，高岭土的添加量为铁鳞和碳酸锶总量的0.25～0.3％；b、将步骤a中的混合浆料烘干，于电炉中进行预烧；c、预烧结束后，将预烧产物破碎至60目筛以下，加入碳酸钙和硼酸，球磨14～18h，过滤，碳酸钙和硼酸加入量分别预烧产物总量的0.5～0.7％和0.15～0.25％；d、将步骤c中过滤得到的固体物质进行烧结，制得锶铁氧体预烧料。其不足之处在于，混合浆料未经处理直接预烧，固相-固相之间接触面积有限，离子交换率低，且该方法对预烧料的性能提升效果有限，后续制得的永磁铁氧体磁学性能较差。
发明内容
本发明是为了克服现有预烧料的制备方法离子交换率低、对预烧料性能提升不足，制得永磁铁氧体磁学性能较差的不足，公开一种离子交换率高、预烧料性能提升大，制得的永磁铁氧体磁学性能优良的一种永磁铁氧体预烧料的制备方法。
为了实现上述发明目的，本发明采用的技术方案如下：
一种永磁铁氧体预烧料的制备方法，永磁铁氧体预烧料具有CayLaxSr1-x-yFe2n- zCozO19主相，其中0.3≤x≤0.6、0.1≤y≤0.5、0.2≤z≤0.4、5.1≤n≤5.6，永磁铁氧体预烧料的制备方法包括以下步骤：
A.按配比称取Fe2O3、CaCO3、La2O3、CoCO3、SrCO3，混合后加入助熔剂进行球磨，烘干得混合粉料；
B.对步骤A所得混合粉料进行预压、有氧预烧得预烧料。
原料中各氧化物和碳酸盐经球磨混合均匀后烘干，在经预压后，减少了原料颗粒间空隙，增大原料间的接触面积，有利于固相反应的发生，有利于离子的交换，在得到的预烧料体系中，离子分布也就更均匀，再经有氧预烧，控制预烧过程中的升温和含氧量，最大化提升预烧料的性能。
进一步的，步骤A中，助熔剂为SiO2。
进一步的，步骤A中，助熔剂的添加量为Fe2O3、CaCO3、La2O3、CoCO3、SrCO3总质量的0.1％～0.2％。
进一步的，步骤A中，球磨方法为湿法球磨，球磨时间为4～8小时，球磨后的平均粒度为0.5～1μm。
进一步的，步骤B中，预压压力为5～10MPa。
进一步的，步骤B中，有氧预烧温度为1180～1230℃。
进一步的，步骤B中，有氧预烧的氧气浓度为22％～25％。
进一步的，步骤B中，有氧预烧的时间为2～4小时。
由于采用以上的技术方案，本发明具有这样的有益效果：通过预压和控制有氧预烧的条件，提升了原料间的离子交换，均匀了预烧料中的离子分布，并提升了预烧料的性能，为后续制备性能优良的永磁铁氧体提供基础。
具体实施方式
下面结合具体实施方式对本发明做进一步的描述。
总实施例
一种永磁铁氧体预烧料的制备方法，永磁铁氧体预烧料具有CayLaxSr1-x-yFe2n- zCozO19主相，其中0.3≤x≤0.6、0.1≤y≤0.5、0.2≤z≤0.4、5.1≤n≤5.6，永磁铁氧体预烧料的制备方法包括以下步骤：
A.按配比称取Fe2O3、CaCO3、La2O3、CoCO3、SrCO3，混合后加入混合物重量0.1％～0.2％的SiO2进行湿法球磨，球磨4～8小时后，球磨后的平均粒度为0.5～1μm，烘干得混合粉料；
B.对步骤A所得粉料在5～10MPa下进行预压，于管式炉中1180～1230℃预烧2～4小时，控制管式炉中氧气含量在22～25％之间，得预烧料。
实施例中使用的原料规格如下：Fe2O3纯度≥99.3wt％，Cl-≤0.1wt％，颗粒的原始平均粒度≤1.5μm；CaCO3纯度≥98.5wt％，颗粒的原始平均粒度≤1.0μm；La2O3纯度≥99.2wt％，颗粒的原始平均粒度≤5μm；氧化钴Co含量≥72.2％，颗粒的原始平均粒度≤3μm；SrCO3纯度≥97.2wt％，颗粒的原始平均粒度≤1.5μm。
实施例1
A.按配比称取Fe2O3、CaCO3、La2O3、CoCO3、SrCO3混合，混合后加入混合物中质量0.1％的SiO2进行湿法球磨，球磨6小时后，烘干得平均粒度0.8μm的混合粉料；
B.对步骤A所得混合粉料在8MPa下进行预压成圆饼状，于管式炉中升温预烧，在温度达到1200℃后停止升温，开始持续充氧气，检测氧气分压，使管式炉中氧气含量保持稳定在23％，煅烧3小时后，停止充氧，停止加热，冷却得预烧料。
实施例2
A.按配比称取Fe2O3、CaCO3、La2O3、CoCO3、SrCO3混合，混合后加入混合物中质量0.2％的SiO2进行湿法球磨，球磨8小时后，烘干得平均粒度0.5μm的混合粉料；
B.对步骤A所得混合粉料在5MPa下进行预压成圆饼状，于管式炉中升温预烧，在温度达到1180℃后停止升温，开始持续充氧气，检测氧气分压，使管式炉中氧气含量保持稳定在22％，煅烧4小时后，停止充氧，停止加热，冷却得预烧料。
实施例3
A.按配比称取Fe2O3、CaCO3、La2O3、CoCO3、SrCO3混合，混合后加入混合物中质量0.1％的SiO2进行湿法球磨，球磨4小时后，烘干得平均粒度1μm的混合粉料；
B.对步骤A所得混合粉料在10MPa下进行预压成圆饼状，于管式炉中升温预烧，在温度达到1230℃后停止升温，开始持续充氧气，检测氧气分压，使管式炉中氧气含量保持稳定在25％，煅烧2小时后，停止充氧，停止加热，冷却得预烧料。
对比例1
对比例1相较于实施例1，未对混合粉料进行预压；
A.按配比称取Fe2O3、CaCO3、La2O3、CoCO3、SrCO3混合，混合后加入混合物中质量0.1％的SiO2进行湿法球磨，球磨6小时后，烘干得平均粒度0.8μm的混合粉料；
B.对步骤A所得混合粉料于管式炉中升温预烧，在温度达到1200℃后停止升温，开始持续充氧气，检测氧气分压，使管式炉中氧气含量保持稳定在23％，煅烧3小时后，停止充氧，停止加热，冷却得预烧料。
对比例2
对比例2相较于实施例1，在温度达到1200℃后持续充空气煅烧；
A.按配比称取Fe2O3、CaCO3、La2O3、CoCO3、SrCO3混合，混合后加入混合物中质量0.1％的SiO2进行湿法球磨，球磨6小时后，烘干得平均粒度0.8μm的混合粉料；
B.对步骤A所得混合粉料于管式炉中升温预烧，在温度达到1200℃后停止升温，开始持续充空气煅烧3小时后，停止充空气，停止加热，冷却得预烧料。
对比例3
对比例3相较于实施例1，有氧预烧过程中氧气含量稳定在30％；
A.按配比称取Fe2O3、CaCO3、La2O3、CoCO3、SrCO3混合，混合后加入混合物中质量0.1％的SiO2进行湿法球磨，球磨6小时后，烘干得平均粒度0.8μm的混合粉料；
B.对步骤A所得混合粉料于管式炉中升温预烧，在温度达到1200℃后停止升温，持续充氧气，检测氧气分压，使管式炉中氧气含量保持稳定在30％，煅烧3小时后，停止充氧，停止加热，冷却得预烧料。
对比例4
对比例4相较于实施例1，在1250℃进行有氧预烧；
A.按配比称取Fe2O3、CaCO3、La2O3、CoCO3、SrCO3混合，混合后加入混合物中质量0.1％的SiO2进行湿法球磨，球磨6小时后，烘干得平均粒度0.8μm的混合粉料；
B.对步骤A所得混合粉料于管式炉中升温预烧，在温度达到1250℃后停止升温，开始充氧气，检测氧气分压，使管式炉中氧气含量保持在23％，煅烧3小时后停止加热，停止充氧气，冷却得预烧料。
称取实施例1～3及对比例1～4的预烧料各500g，分别添加2.5gSiO2、7.2gCaCO3，5g葡萄糖酸钙混合物投入到球磨机，再添加750mL去离子水作为球磨介质研磨30小时至料浆平均粒度为0.60μm。
湿法粉碎之后，对成型用料浆进行离心脱水，各个料浆的浓度调整为68％，然后在5MPa下成型，在压制的同时，在压制方向施加15000Oe的成型磁场。得到成型体直径为45mm、高度为10mm的圆柱体。
在400℃下对成型体进行热处理，彻底去除水分，然后在空气中进行烧结，升温速度为150℃/小时，在1190℃保温60分钟，获得烧结体。对各个烧结体的上下表面研磨，测量其剩余磁感应强度(Br)、矫顽力(Hcb)、内禀矫顽力(Hcj)、最大磁能积(BH)max，结果如下表所示。
编号 Br(Gs) Hcb(Oe) Hcj(Oe) (BH)max(MGOe) 矫顽力温度系数
实施例1 4560 4230 5440 4.997 0.12
实施例2 4573 4238 5560 5.001 0.12
实施例3 4523 5128 5249 4.687 0.13
对比例1 4490 4029 4850 4.654 0.26
对比例2 4520 4060 4960 4.885 0.2
对比例3 4450 4145 5021 4.747 0.18
对比例4 4390 4179 4941 4.702 0.16
可见，由实施例1～3的预烧料制得的永磁铁氧体，具有明显优于对比例1～4的磁学特性，由对比例1可见，预压过程对提高预烧料性能有着极大提升，且矫顽力系数有明显下降；由对比例2、对比例3可见，过低及过高的氧浓度预烧，都不利于固相反应的进行，对最终烧结体的磁学特性也会产生影响；由对比例4可见，有氧预烧的温度过高，也会导致最终烧结体性能下降。

Claims (6)

1.一种永磁铁氧体预烧料的制备方法，所述永磁铁氧体预烧料具有CayLaxSr1-x-yFe2n- zCozO19主相，其中0.3≤x≤0.6、0.1≤y≤0.5、0.2≤z≤0.4、5.1≤n≤5.6，其特征在于，所述永磁铁氧体预烧料的制备方法包括以下步骤：
A.按配比称取Fe2O3、CaCO3、La2O3、CoCO3、SrCO3，混合后加入助熔剂进行球磨，烘干得混合粉料；
B.对步骤A所得混合粉料进行预压、有氧预烧得预烧料；
所述步骤B中，有氧预烧的氧气浓度为22%~25%；
所述步骤B中，有氧预烧温度为1180~1230℃。
2.根据权利要求1所述的一种永磁铁氧体预烧料的制备方法，其特征在于，所述步骤A中，助熔剂为SiO2。
3.根据权利要求1或2所述的一种永磁铁氧体预烧料的制备方法，其特征在于，所述步骤A中，助熔剂的添加量为Fe2O3、CaCO3、La2O3、CoCO3、SrCO3总质量的0.1%~0.2%。
4.根据权利要求1所述的一种永磁铁氧体预烧料的制备方法，其特征在于，所述步骤A中，球磨方法为湿法球磨，球磨时间为4~8小时，球磨后的平均粒度为0.5~1μm。
5.根据权利要求1所述的一种永磁铁氧体预烧料的制备方法，其特征在于，所述步骤B中，预压压力为5~10MPa。
6.根据权利要求1所述的一种永磁铁氧体预烧料的制备方法，其特征在于，所述步骤B中，有氧预烧的时间为2~4小时。
CN202111123603.7A 2021-09-24 2021-09-24 一种永磁铁氧体预烧料的制备方法 Active CN113929445B (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111123603.7A CN113929445B (zh) 2021-09-24 2021-09-24 一种永磁铁氧体预烧料的制备方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111123603.7A CN113929445B (zh) 2021-09-24 2021-09-24 一种永磁铁氧体预烧料的制备方法

Publications (2)

Publication Number Publication Date
CN113929445A CN113929445A (zh) 2022-01-14
CN113929445B true CN113929445B (zh) 2023-07-21

Family

ID=79276773

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111123603.7A Active CN113929445B (zh) 2021-09-24 2021-09-24 一种永磁铁氧体预烧料的制备方法

Country Status (1)

Country Link
CN (1) CN113929445B (zh)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06151153A (ja) * 1992-11-06 1994-05-31 Nippon Steel Corp マンガン−亜鉛フェライト用仮焼粉およびその製造方法
CN102190501A (zh) * 2010-03-08 2011-09-21 无锡斯贝尔磁性材料有限公司 一种MnZn铁氧体粉料的预烧工艺
CN111004027A (zh) * 2019-12-09 2020-04-14 天长市华磁磁电有限公司 一种高磁导率软磁铁氧体及其制备方法
CN111362687A (zh) * 2019-12-17 2020-07-03 横店集团东磁股份有限公司 一种永磁铁氧体及其制备方法
WO2021057051A1 (zh) * 2019-09-25 2021-04-01 横店集团东磁股份有限公司 一种永磁材料及其制备方法
CN113185275A (zh) * 2021-04-23 2021-07-30 麦格磁电科技（珠海）有限公司 云计算用超高Bs低损耗锰锌铁氧体材料的制备方法

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101377409B1 (ko) * 2009-07-08 2014-04-01 티디케이가부시기가이샤 페라이트 자성 재료
CN103030388A (zh) * 2013-01-17 2013-04-10 北矿磁材科技股份有限公司 一种高性能永磁铁氧体材料及制造方法
CN105399411B (zh) * 2015-12-01 2019-01-25 横店集团东磁股份有限公司 一种锰锌铁氧体低温烧结工艺
CN110372365A (zh) * 2019-07-16 2019-10-25 横店集团东磁股份有限公司 一种永磁铁氧体材料的制备方法
CN111943658B (zh) * 2020-06-30 2022-06-03 天通控股股份有限公司 一种宽温低损耗MnZn铁氧体材料及其制备方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06151153A (ja) * 1992-11-06 1994-05-31 Nippon Steel Corp マンガン−亜鉛フェライト用仮焼粉およびその製造方法
CN102190501A (zh) * 2010-03-08 2011-09-21 无锡斯贝尔磁性材料有限公司 一种MnZn铁氧体粉料的预烧工艺
WO2021057051A1 (zh) * 2019-09-25 2021-04-01 横店集团东磁股份有限公司 一种永磁材料及其制备方法
CN111004027A (zh) * 2019-12-09 2020-04-14 天长市华磁磁电有限公司 一种高磁导率软磁铁氧体及其制备方法
CN111362687A (zh) * 2019-12-17 2020-07-03 横店集团东磁股份有限公司 一种永磁铁氧体及其制备方法
CN113185275A (zh) * 2021-04-23 2021-07-30 麦格磁电科技（珠海）有限公司 云计算用超高Bs低损耗锰锌铁氧体材料的制备方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
永磁铁氧体元件机械强度分析;王自敏;《机械强度》;第38卷(第04期);第729-733页 *

Also Published As

Publication number Publication date
CN113929445A (zh) 2022-01-14

Similar Documents

Publication Publication Date Title
CN112919896B (zh) 一种高致密度永磁铁氧体材料的制备方法
CN109400139B (zh) 一种低成本永磁铁氧体材料的制备工艺
CN112159218A (zh) 一种低成本高性能永磁铁氧体材料的制备方法
CN107337447B (zh) 一种低成本永磁铁氧体及其制备方法
CN111099889A (zh) 一种提高永磁铁氧体磁性能的方法
CN115340373B (zh) 基于低纯度铁精矿原料体系的六角铁氧体材料制备方法
CN111362687A (zh) 一种永磁铁氧体及其制备方法
CN111704452A (zh) 一种永磁铁氧体材料及其制备方法
CN113698192A (zh) 一种以超纯磁铁精矿为原料制备永磁铁氧体的方法
CN111960816B (zh) 一种永磁铁氧体的制备工艺
CN111116192A (zh) 一种微波铁氧体材料、制备方法及微波通信器件
CN112908676A (zh) 一种干压成型用永磁铁氧体磁粉及其制备方法
CN109836147B (zh) 一种永磁铁氧体及其制备方法
CN1252743C (zh) 锰－锌功率软磁铁氧体料粉及其制备方法
CN105418062A (zh) 一种永磁铁氧体及其制造方法
CN113929445B (zh) 一种永磁铁氧体预烧料的制备方法
CN114014644A (zh) 一种钙系永磁铁氧体材料及其制备方法
CN106554197A (zh) 通过复合法制备高性能永磁铁氧体的方法
CN108585821B (zh) 固溶体结构添加剂和制备方法及在铁氧体永磁材料制备中的应用
CN111646791A (zh) 一种基于正交试验的干压永磁铁氧体的制备方法
CN110342923A (zh) 一种提高取向度和性能的干压异性铁氧体细粉制备方法及干压异性永磁铁氧体
CN112645704B (zh) 一种高性能铁氧体的制备方法
CN111196720A (zh) 一种改进的磁环用高性能锶铁氧体及其制备方法
CN115010478B (zh) 一种异性干压铁氧体及其制备方法
CN118063223A (zh) 一种永磁铁氧体预烧料的制备方法

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