CN110128129A - 一种低损耗石榴石铁氧体材料的制备方法 - Google Patents

一种低损耗石榴石铁氧体材料的制备方法 Download PDF

Info

Publication number
CN110128129A
CN110128129A CN201910592143.9A CN201910592143A CN110128129A CN 110128129 A CN110128129 A CN 110128129A CN 201910592143 A CN201910592143 A CN 201910592143A CN 110128129 A CN110128129 A CN 110128129A
Authority
CN
China
Prior art keywords
loss
preparation
low
ferrogarnet
ball milling
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
CN201910592143.9A
Other languages
English (en)
Other versions
CN110128129B (zh
Inventor
张虎
钟喜春
龙克文
刘仲武
余红雅
胡锦文
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.)
Sanqiaohui Foshan New Material Co ltd
Original Assignee
Sanqiaohui Foshan New Material 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 Sanqiaohui Foshan New Material Co ltd filed Critical Sanqiaohui Foshan New Material Co ltd
Priority to CN201910592143.9A priority Critical patent/CN110128129B/zh
Publication of CN110128129A publication Critical patent/CN110128129A/zh
Priority to JP2019168385A priority patent/JP2021011421A/ja
Application granted granted Critical
Publication of CN110128129B publication Critical patent/CN110128129B/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
    • C04B35/62625—Wet mixtures
    • C04B35/62635—Mixing details
    • 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
    • C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/6303—Inorganic additives
    • 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
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3225—Yttrium 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
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
    • 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
    • C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, 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
    • C04B2235/3284—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
    • C04B2235/3286—Gallium oxides, gallates, indium oxides, indates, thallium oxides, thallates or oxide forming salts thereof, e.g. zinc gallate
    • 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
    • C04B2235/3293—Tin oxides, stannates or oxide forming salts thereof, e.g. indium tin oxide [ITO]
    • 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
    • C04B2235/02—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
    • C04B2235/5454—Particle size related information expressed by the size of the particles or aggregates thereof nanometer sized, i.e. below 100 nm
    • 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
    • C04B2235/6562—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
    • C04B2235/6565—Cooling 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

Landscapes

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

Abstract

本发明公开了一种低损耗石榴石铁氧体材料的制备方法，包括下述步骤：(1)配料；(2)一次球磨；(3)预烧；(4)二次球磨；(5)造粒；(6)压制成型；(7)烧结。其中，造粒采用纳米TiO2、纳米SiO2和聚乙烯醇配制得到的纳米改性胶粘剂，造粒之前在真空加压条件下将二次球磨后的物料与纳米改性胶粘剂进行混匀处理。本发明的制备方法能使制备的石榴石铁氧体材料晶格缺陷少，气孔率低，微观结构规整且均匀、致密，有效降低材料的损耗。

Description

一种低损耗石榴石铁氧体材料的制备方法
技术领域
本发明涉及铁氧体材料技术领域，尤其涉及一种低损耗石榴石铁氧体材料的制备方法。
背景技术
微波铁氧体是电子信息产业的重要材料，作为微波器件的基础材料在雷达、通信系统以及民用电子系统等领域有着广泛的应用。近年来，随着科技的进步，对微波器件的性能提出更高的要求，主要朝高功率、低损耗、小型化、高稳定性等方面发展。其中，低损耗铁氧体材料有利于降低微波器件在工作中的损耗，正在受到越来越多研究者的关注。
钇铁石榴石铁氧体是一种典型的石榴石铁氧体材料，因其优良的性能而被广泛应用和研究，其特点是低介电损耗、磁损耗，具有制作低损耗微波器件的开发潜力。但是，纯的钇铁石榴石铁氧体各方面性能均不足以满足微波器件的性能要求。为了开发低损耗、且能满足微波器件工作要求的铁氧体材料，有必要对钇铁石榴石铁氧体的配方以及制备工艺作出改进。
发明内容
本发明目的就是为了弥补已有技术的缺陷，提供一种低损耗石榴石铁氧体材料的制备方法，该方法通过合理的配方以及工艺改进，能有效抑制材料中多气孔粗晶粒的结构的形成，降低材料的磁损耗。
本发明是通过以下技术方案实现的：
一种低损耗石榴石铁氧体材料的制备方法，包括下述步骤：
(1)配料：按以下重量份称取原料：Y203 44～46份、Fe203 50～52份、CaCO3 2～3份、ZrO2 1～1.2份、ZnO 0.4～0.5份、SnO2 0.1～0.2份、In2O3 0.1～0.2份；
(2)一次球磨：将步骤(1)称取的原料加入行星式球磨机中进行湿法球磨，原料、球和水的质量比为(1～1.5)：(3～4)：1，球磨完成后烘干、过筛；
(3)预烧：将一次球磨后的物料于1150～1250℃预烧3～4h，然后冷却至常温；
(4)二次球磨：将预烧后的物料加入行星式球磨机中进行湿法球磨，原料、球和水的质量比为(0.5～0.8)：(3～4)：1，球磨完成后烘干、过筛；
(5)造粒：按重量份计，将0.5～1份纳米TiO2、0.3～0.5份纳米SiO2和0.5～1份聚乙烯醇加入10～15份水中配制得到纳米改性胶粘剂，然后在真空加压条件下与二次球磨后的物料混匀处理，然后造粒，形成30～40目的颗粒料；
(6)压制成型：将颗粒料放入成型模具内压制成坯件；
(7)烧结：将坯件放入炉中进行烧结，冷却后即得低损耗石榴石铁氧体材料。
优选地，所述步骤(2)中，一次球磨的转速为250～350r/min，时间为6～8h。
优选地，所述步骤(3)中，冷却的具体步骤如下：先以3～5℃/min的降温速率将温度降至900～950℃，保温0.5～1h，再以20～30℃/min的降温速率冷却至常温。
优选地，所述步骤(4)中，二次球磨的转速为400～450r/min，时间为3～4h。
优选地，所述步骤(5)中，纳米TiO2的平均粒径为50-60nm，纳米SiO2的平均粒径为20-30nm。
优选地，所述步骤(5)中，纳米改性胶粘剂的具体配制方法为：先称取0.05～0.1份聚乙烯醇加入水中，在80～90℃溶解完全，然后加入纳米TiO2、纳米SiO2超声分散均匀，最后加入剩余的聚乙烯醇，在90～95℃继续溶解完全，即得。
优选地，所述步骤(5)中，真空加压混匀处理的具体步骤为：先将二次球磨后的物料加入真空加压罐中抽真空到-0.095～-0.085MPa保持1-2h，然后将纳米改性胶粘剂注入罐中，加压至1-1.5MPa后保压2-4h，取出后再于200-300r/min搅拌1-2h。
优选地，所述步骤(6)中，压制成型的压力为60～80MPa。
优选地，所述步骤(7)中，烧结的具体步骤为：先以10～15℃/min的升温速率加热至700～800℃，保温20～30min，然后以30～40℃/min的升温速率加热至1300～1450℃，保温烧结2～3h后，再以40～50℃的降温速率冷却至400～500℃，保温1～1.5h，然后随炉冷却至常温。
本发明的优点是：
(1)本发明的配方中，ZrO2能降低材料的磁晶各向异性，从而降低磁损耗；In2O3能促进晶化，SnO2能在烧结过程中形成液相烧结，促进晶粒增大，两者共同作用能提高材料的致密性；ZnO能与Y203和Fe203发生反应生成另相，提高材料致密性；SiO2、TiO2起到抑制晶粒的异常长大的作用，使材料更为均匀、致密，这些原料协同配合，通过提高致密度降低磁损耗；且SiO2能与CaCO3形成CaSiO3，TiO2能与CaCO3形成CaTiO3，这两者共同在晶界形成高电阻层，有利于提高材料的电阻率，降低涡流损耗。
(2)本发明在造粒之前，在真空加压条件下将二次球磨后的物料与纳米改性胶粘剂进行混匀处理，一方面，通过真空加压提高聚乙烯醇与物料的渗透性，使聚乙烯醇与物料均匀、牢固地结合，有利于在烧结时限制聚乙烯醇的分解、排出速度，避免过快排胶，从而减少气孔的形成，使材料更为致密；另一方面，使纳米TiO2、纳米SiO2紧密且均匀地分布在物料表面，在烧结时能形成更均匀的绝缘层，更有利于提高材料的电阻率，降低涡流损耗。
综上所述，本发明通过对配方和工艺的改进，使制备的石榴石铁氧体材料电阻率大，晶格缺陷少，气孔率低，微观结构规整且均匀、致密，从而有效降低材料的损耗。
具体实施方式
实施例1
一种低损耗石榴石铁氧体材料的制备方法，包括下述步骤：
(1)配料：按以下重量份称取原料：Y203 44份、Fe203 50份、CaCO3 2份、ZrO2 1份、ZnO0.4份、SnO2 0.1份、In2O3 0.1份；
(2)一次球磨：将步骤(1)称取的原料加入行星式球磨机中，在转速为250r/min下进行湿法球磨，时间为6h，原料、球和水的质量比为1：3：1，球磨完成后烘干、过筛；
(3)预烧：将一次球磨后的物料于1150℃预烧3h，然后先以3℃/min的降温速率将温度降至900℃，保温0.5h，再以20℃/min的降温速率冷却至常温；
(4)二次球磨：将预烧后的物料加入行星式球磨机中，在转速为400r/min下进行湿法球磨，时间为3h，原料、球和水的质量比为0.5：3：1，球磨完成后烘干、过筛；
(5)造粒：按重量份计，将0.5份平均粒径为50nm的纳米TiO2、0.3份平均粒径为20nm的纳米SiO2和0.5份聚乙烯醇加入10份水中配制得到纳米改性胶粘剂，先将二次球磨后的物料加入真空加压罐中抽真空到-0.095MPa保持1h，然后将纳米改性胶粘剂注入罐中，加压至1MPa后保压2h，取出后再于200r/min搅拌1h，然后造粒，形成30目的颗粒料，纳米改性胶粘剂的具体配制方法为：先称取0.05份聚乙烯醇加入水中，在80℃溶解完全，然后加入纳米TiO2、纳米SiO2超声分散均匀，最后加入剩余的聚乙烯醇，在90℃继续溶解完全。
(6)压制成型：将颗粒料放入成型模具内在60MPa的压力下压制成坯件；
(7)烧结：将坯件放入炉中，先以10℃/min的升温速率加热至700℃，保温20min，然后以30℃/min的升温速率加热至1300℃，保温烧结2h后，再以40℃的降温速率冷却至400℃，保温1h，然后随炉冷却至常温冷却后即得低损耗石榴石铁氧体材料。
实施例2
一种低损耗石榴石铁氧体材料的制备方法，包括下述步骤：
(1)配料：按以下重量份称取原料：Y203 45份、Fe203 51份、CaCO3 2.5份、ZrO2 1.15份、ZnO 0.44份、SnO2 0.12份、In2O3 0.15份；
(2)一次球磨：将步骤(1)称取的原料加入行星式球磨机中，在转速为300r/min下进行湿法球磨，时间为7h，原料、球和水的质量比为1.2：3.5：1，球磨完成后烘干、过筛；
(3)预烧：将一次球磨后的物料于1200℃预烧3.5h，然后先以4℃/min的降温速率将温度降至920℃，保温0.6h，再以25℃/min的降温速率冷却至常温；
(4)二次球磨：将预烧后的物料加入行星式球磨机中，在转速为440r/min下进行湿法球磨，时间为3.5h，原料、球和水的质量比为0.6：3.6：1，球磨完成后烘干、过筛；
(5)造粒：按重量份计，将0.8份平均粒径为55nm的纳米TiO2、0.4份平均粒径为25nm的纳米SiO2和0.8份聚乙烯醇加入12份水中配制得到纳米改性胶粘剂，先将二次球磨后的物料加入真空加压罐中抽真空到-0.09MPa保持1.5h，然后将纳米改性胶粘剂注入罐中，加压至1.2MPa后保压3h，取出后再于250r/min搅拌1.5h，然后造粒，形成35目的颗粒料，纳米改性胶粘剂的具体配制方法为：先称取0.08份聚乙烯醇加入水中，在85℃溶解完全，然后加入纳米TiO2、纳米SiO2超声分散均匀，最后加入剩余的聚乙烯醇，在92℃继续溶解完全。
(6)压制成型：将颗粒料放入成型模具内在70MPa的压力下压制成坯件；
(7)烧结：将坯件放入炉中，先以14℃/min的升温速率加热至750℃，保温25min，然后以35℃/min的升温速率加热至1400℃，保温烧结2.5h后，再以45℃的降温速率冷却至450℃，保温1.2h，然后随炉冷却至常温冷却后即得低损耗石榴石铁氧体材料。
实施例3
一种低损耗石榴石铁氧体材料的制备方法，包括下述步骤：
(1)配料：按以下重量份称取原料：Y203 46份、Fe203 52份、CaCO3 3份、ZrO2 1.2份、ZnO 0.5份、SnO2 0.2份、In2O3 0.2份；
(2)一次球磨：将步骤(1)称取的原料加入行星式球磨机中，在转速为350r/min下进行湿法球磨，时间为8h，原料、球和水的质量比为1.5：4：1，球磨完成后烘干、过筛；
(3)预烧：将一次球磨后的物料于1250℃预烧4h，然后先以5℃/min的降温速率将温度降至950℃，保温1h，再以30℃/min的降温速率冷却至常温；
(4)二次球磨：将预烧后的物料加入行星式球磨机中，在转速为450r/min下进行湿法球磨，时间为4h，原料、球和水的质量比为0.8：4：1，球磨完成后烘干、过筛；
(5)造粒：按重量份计，将1份平均粒径为60nm的纳米TiO2、0.5份平均粒径为30nm的纳米SiO2和1份聚乙烯醇加入15份水中配制得到纳米改性胶粘剂，先将二次球磨后的物料加入真空加压罐中抽真空到-0.085MPa保持2h，然后将纳米改性胶粘剂注入罐中，加压至1.5MPa后保压4h，取出后再于300r/min搅拌2h，然后造粒，形成40目的颗粒料，纳米改性胶粘剂的具体配制方法为：先称取0.1份聚乙烯醇加入水中，在90℃溶解完全，然后加入纳米TiO2、纳米SiO2超声分散均匀，最后加入剩余的聚乙烯醇，在95℃继续溶解完全。
(6)压制成型：将颗粒料放入成型模具内在80MPa的压力下压制成坯件；
(7)烧结：将坯件放入炉中，先以15℃/min的升温速率加热至800℃，保温30min，然后以40℃/min的升温速率加热至1450℃，保温烧结3h后，再以50℃的降温速率冷却至500℃，保温1.5h，然后随炉冷却至常温冷却后即得低损耗石榴石铁氧体材料。
对比例1
按化学式Y3Fe5O12，通过常规方法制备铁氧体材料。具体制备方法如下：
按化学式称取Y203和Fe203原料，加入行星式球磨机中进行湿法球磨，原料、球和水的质量比为1：3：1，球磨完成后烘干、过筛，于1150℃预烧3h，冷却至常温后加入行星式球磨机中进行湿法球磨，原料、球和水的质量比为0.5：3：1，球磨完成后烘干、过筛得到粉料，再加入相当于粉料重量10％的质量分数为5％的聚乙烯醇胶粘剂混匀后造粒，形成30目的颗粒料，在60MPa下压制成坯件，放入炉中，在烧结温度为1300℃的条件下烧结5h，冷却后即得铁氧体材料。
对比例2
按以下重量份称取原料：Y203 44份、Fe203 50份、CaCO3 2份、ZrO2 1份、ZnO 0.4份、SnO2 0.1份、In2O3 0.1份、平均粒径为50nm的纳米TiO2 0.5份、平均粒径为20nm的纳米SiO20.3份、通过常规方法制备铁氧体材料。具体制备方法如下：
称取原料，加入行星式球磨机中进行湿法球磨，原料、球和水的质量比为1：3：1，球磨完成后烘干、过筛，于1150℃预烧3h，冷却至常温后加入行星式球磨机中进行湿法球磨，原料、球和水的质量比为0.5：3：1，球磨完成后烘干、过筛得到粉料，再加入10重量份质量分数为5％的聚乙烯醇水溶液胶粘剂混匀后造粒，形成30目的颗粒料，在60MPa下压制成坯件，放入炉中，在烧结温度为1300℃的条件下烧结5h，冷却后即得铁氧体材料。
将实施例1-3以及对比例1-2制得的铁氧体材料进行介电损耗(tanδε)和铁磁共振线宽(ΔH)的测试，其中介电损耗的测试按IEC60556的标准，测试频率为10.7GHz；铁磁共振线宽的测试按IEC60556的标准，测试频率为9.3GHz。测试结果如下表所示：
由此可见，本发明制备的铁氧体具有较低的磁损耗和介电损耗，说明本发明的制备方法能有效降低石榴石铁氧体材料的损耗。

Claims (9)

1.一种低损耗石榴石铁氧体材料的制备方法，其特征在于，包括下述步骤：
(1)配料：按以下重量份称取原料：Y203 44～46份、Fe203 50～52份、CaCO3 2～3份、ZrO2 1～1.2份、ZnO 0.4～0.5份、SnO2 0.1～0.2份、In2O3 0.1～0.2份；
(2)一次球磨：将步骤(1)称取的原料加入行星式球磨机中进行湿法球磨，原料、球和水的质量比为(1～1.5)：(3～4)：1，球磨完成后烘干、过筛；
(3)预烧：将一次球磨后的物料于1150～1250℃预烧3～4h，然后冷却至常温；
(4)二次球磨：将预烧后的物料加入行星式球磨机中进行湿法球磨，原料、球和水的质量比为(0.5～0.8)：(3～4)：1，球磨完成后烘干、过筛；
(5)造粒：按重量份计，将0.5～1份纳米TiO2、0.3～0.5份纳米SiO2和0.5～1份聚乙烯醇加入10～15份水中配制得到纳米改性胶粘剂，然后在真空加压条件下与二次球磨后的物料混匀处理，然后造粒，形成30～40目的颗粒料；
(6)压制成型：将颗粒料放入成型模具内压制成坯件；
(7)烧结：将坯件放入炉中进行烧结，冷却后即得低损耗石榴石铁氧体材料。
2.根据权利要求1所述的一种低损耗石榴石铁氧体材料的制备方法，其特征在于，所述步骤(2)中，一次球磨的转速为250～350r/min，时间为6～8h。
3.根据权利要求1所述的一种低损耗石榴石铁氧体材料的制备方法，其特征在于，所述步骤(3)中，冷却的具体步骤如下：先以3～5℃/min的降温速率将温度降至900～950℃，保温0.5～1h，再以20～30℃/min的降温速率冷却至常温。
4.根据权利要求1所述的一种低损耗石榴石铁氧体材料的制备方法，其特征在于，所述步骤(4)中，二次球磨的转速为400～450r/min，时间为3～4h。
5.根据权利要求1所述的一种低损耗石榴石铁氧体材料的制备方法，其特征在于，所述步骤(5)中，纳米TiO2的平均粒径为50-60nm，纳米SiO2的平均粒径为20-30nm。
6.根据权利要求1所述的一种低损耗石榴石铁氧体材料的制备方法，其特征在于，所述步骤(5)中，纳米改性胶粘剂的具体配制方法为：先称取0.05～0.1份聚乙烯醇加入水中，在80～90℃溶解完全，然后加入纳米TiO2、纳米SiO2超声分散均匀，最后加入剩余的聚乙烯醇，在90～95℃继续溶解完全，即得。
7.根据权利要求1所述的一种低损耗石榴石铁氧体材料的制备方法，其特征在于，所述步骤(5)中，真空加压混匀处理的具体步骤为：先将二次球磨后的物料加入真空加压罐中抽真空到-0.095～-0.085MPa保持1-2h，然后将纳米改性胶粘剂注入罐中，加压至1-1.5MPa后保压2-4h，取出后再于200-300r/min搅拌1-2h。
8.根据权利要求1所述的一种低损耗石榴石铁氧体材料的制备方法，其特征在于，所述步骤(6)中，压制成型的压力为60～80MPa。
9.根据权利要求1所述的一种低损耗石榴石铁氧体材料的制备方法，其特征在于，所述步骤(7)中，烧结的具体步骤为：先以10～15℃/min的升温速率加热至700～800℃，保温20～30min，然后以30～40℃/min的升温速率加热至1300～1450℃，保温烧结2～3h后，再以40～50℃的降温速率冷却至400～500℃，保温1～1.5h，然后随炉冷却至常温。
CN201910592143.9A 2019-07-03 2019-07-03 一种低损耗石榴石铁氧体材料的制备方法 Active CN110128129B (zh)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN201910592143.9A CN110128129B (zh) 2019-07-03 2019-07-03 一种低损耗石榴石铁氧体材料的制备方法
JP2019168385A JP2021011421A (ja) 2019-07-03 2019-09-17 低損失ガーネットフェライト材料の調製方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910592143.9A CN110128129B (zh) 2019-07-03 2019-07-03 一种低损耗石榴石铁氧体材料的制备方法

Publications (2)

Publication Number Publication Date
CN110128129A true CN110128129A (zh) 2019-08-16
CN110128129B CN110128129B (zh) 2021-06-15

Family

ID=67566598

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910592143.9A Active CN110128129B (zh) 2019-07-03 2019-07-03 一种低损耗石榴石铁氧体材料的制备方法

Country Status (2)

Country Link
JP (1) JP2021011421A (zh)
CN (1) CN110128129B (zh)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111004028A (zh) * 2019-12-25 2020-04-14 横店集团东磁股份有限公司 一种微波铁氧体磁片及其制备方法和用途
CN111187067A (zh) * 2020-01-15 2020-05-22 横店集团东磁股份有限公司 一种低损耗石榴石微波铁氧体磁片及其制备方法
CN112430080A (zh) * 2020-10-27 2021-03-02 北京无线电测量研究所 一种高功率和高剩磁比的石榴石铁氧体材料及其制备方法
CN112898008A (zh) * 2021-04-01 2021-06-04 电子科技大学 一种低损耗yig铁氧体及其制备方法
CN113045303A (zh) * 2021-03-22 2021-06-29 江苏启诚磁业有限公司 一种永磁铁氧体预烧料的生产方法
CN114031389A (zh) * 2021-11-02 2022-02-11 横店集团东磁股份有限公司 一种三阶互调环形器用微波铁氧体材料及其制备方法
CN115121353A (zh) * 2022-07-01 2022-09-30 广州天极电子科技股份有限公司 一种混合方法

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114644516A (zh) * 2022-03-22 2022-06-21 电子科技大学 一种低损耗yig材料及其制备方法
CN116496080A (zh) * 2023-05-11 2023-07-28 深圳市华扬通信技术有限公司 一种低温烧结高介旋磁铁氧体材料及其制备方法

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU1168332A1 (ru) * 1983-06-10 1985-07-23 Предприятие П/Я А-1067 Способ изготовлени поликристаллического иттриевого феррограната
US5902514A (en) * 1996-10-31 1999-05-11 Electronics And Telecommunications Research Institute Magnetic ceramic composition for use in microwave devices, magnetic ceramics for use in microwave devices, and preparation method therefor
CN101235557A (zh) * 2008-03-12 2008-08-06 长春理工大学 一种制备稀土石榴石型化合物纳米纤维的方法
CN101549994A (zh) * 2009-04-30 2009-10-07 深圳市华扬通信技术有限公司 适用于通讯频段的钇铁石榴石材料及其制备方法
CN102936131A (zh) * 2012-11-07 2013-02-20 天通控股股份有限公司 一种电涡流式接近开关用锰锌铁氧体材料、镀膜磁心及其制备方法
CN109608184A (zh) * 2018-12-29 2019-04-12 天长市中德电子有限公司 一种高磁性低损耗软磁铁氧体材料的制备方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU1168332A1 (ru) * 1983-06-10 1985-07-23 Предприятие П/Я А-1067 Способ изготовлени поликристаллического иттриевого феррограната
US5902514A (en) * 1996-10-31 1999-05-11 Electronics And Telecommunications Research Institute Magnetic ceramic composition for use in microwave devices, magnetic ceramics for use in microwave devices, and preparation method therefor
CN101235557A (zh) * 2008-03-12 2008-08-06 长春理工大学 一种制备稀土石榴石型化合物纳米纤维的方法
CN101549994A (zh) * 2009-04-30 2009-10-07 深圳市华扬通信技术有限公司 适用于通讯频段的钇铁石榴石材料及其制备方法
CN102936131A (zh) * 2012-11-07 2013-02-20 天通控股股份有限公司 一种电涡流式接近开关用锰锌铁氧体材料、镀膜磁心及其制备方法
CN109608184A (zh) * 2018-12-29 2019-04-12 天长市中德电子有限公司 一种高磁性低损耗软磁铁氧体材料的制备方法

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111004028A (zh) * 2019-12-25 2020-04-14 横店集团东磁股份有限公司 一种微波铁氧体磁片及其制备方法和用途
CN111187067A (zh) * 2020-01-15 2020-05-22 横店集团东磁股份有限公司 一种低损耗石榴石微波铁氧体磁片及其制备方法
CN112430080A (zh) * 2020-10-27 2021-03-02 北京无线电测量研究所 一种高功率和高剩磁比的石榴石铁氧体材料及其制备方法
CN113045303A (zh) * 2021-03-22 2021-06-29 江苏启诚磁业有限公司 一种永磁铁氧体预烧料的生产方法
CN112898008A (zh) * 2021-04-01 2021-06-04 电子科技大学 一种低损耗yig铁氧体及其制备方法
CN114031389A (zh) * 2021-11-02 2022-02-11 横店集团东磁股份有限公司 一种三阶互调环形器用微波铁氧体材料及其制备方法
CN115121353A (zh) * 2022-07-01 2022-09-30 广州天极电子科技股份有限公司 一种混合方法
CN115121353B (zh) * 2022-07-01 2024-03-08 广州天极电子科技股份有限公司 一种混合方法

Also Published As

Publication number Publication date
JP2021011421A (ja) 2021-02-04
CN110128129B (zh) 2021-06-15

Similar Documents

Publication Publication Date Title
CN110128129A (zh) 一种低损耗石榴石铁氧体材料的制备方法
WO2021248813A1 (zh) 氧化铝陶瓷及其制备方法
Sadhana et al. Effect of Sm 3+ on dielectric and magnetic properties of Y 3 Fe 5 O 12 nanoparticles
CN102531559B (zh) 一种高性能锰锌铁氧体料粉的制造方法
CN107382301B (zh) 一种锰锌铁氧体料粉的制备方法
CN103951412B (zh) 一种软磁锰锌铁氧体材料的制法
CN110156453A (zh) 一种高功率稀土钇铁石榴石复合铁氧体材料的制备方法
WO2019113973A1 (zh) 一种介质陶瓷材料及其制备方法
CN104230325A (zh) 制备永磁铁氧体预烧料的方法及永磁铁氧体的制备方法
CN108774005A (zh) 玻璃体式添加剂和制备方法及在铁氧体永磁材料制备中的应用
CN111925201B (zh) Sc掺杂六角晶系Zn2W铁氧体材料及制备方法
CN106747435B (zh) 一种温度稳定的芯-壳结构微波介质陶瓷的制备方法
Wang et al. Effects of Bi2O3-V2O5 mixture on microstructure and magnetic properties for Li0. 42Zn0. 27Ti0. 11Mn0. 1Fe2. 1O4 ferrites sintered at low temperatures
CN115745573A (zh) 一种细晶izo靶材制备方法
CN103833351B (zh) 微波介质陶瓷及其制备方法
CN105565793A (zh) 一种熔融盐辅助烧结锶铁氧体的方法
CN112390637A (zh) 无钇配方的高介电常数微波铁氧体材料及其制备方法和器件
Shangguan et al. Production of Ba0. 991Bi0. 006TiO3@ ZnO–B2O3–SiO2 ceramics with a high dielectric constant, a core–shell structure, and a fine-grained microstructure by means of a sol-precipitation method
CN104788094B (zh) 一种钛酸铋陶瓷材料的制备方法
US3751366A (en) Process for preparing ferrite and garnet raw materials for microwave applications
CN113582694A (zh) 一种采用Isobam体系凝胶注模成型钇铝石榴石型微波介质陶瓷的方法
CN115259853A (zh) 一种高熵萤石氧化物靶材及其制备方法
CN113387710A (zh) 一种无粘结剂的粉体造粒压片方法
CN114409392A (zh) 一种高剩磁比低损耗复合六角铁氧体材料及其制备方法
CN111960815A (zh) 一种微波旋磁铁氧体材料及其制备工艺和用途

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