WO2019199732A1 - Textured planar m-type hexagonal ferrites and methods of use thereof - Google Patents

Textured planar m-type hexagonal ferrites and methods of use thereof Download PDF

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Publication number
WO2019199732A1
WO2019199732A1 PCT/US2019/026465 US2019026465W WO2019199732A1 WO 2019199732 A1 WO2019199732 A1 WO 2019199732A1 US 2019026465 W US2019026465 W US 2019026465W WO 2019199732 A1 WO2019199732 A1 WO 2019199732A1
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Prior art keywords
grain
oriented
type hexagonal
hexagonal ferrite
fei2
Prior art date
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Ceased
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PCT/US2019/026465
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English (en)
French (fr)
Inventor
Yajie Chen
Kevin Ring
Li Zhang
Michael S. White
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Rogers Corp
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Rogers Corp
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Filing date
Publication date
Application filed by Rogers Corp filed Critical Rogers Corp
Priority to GB2014487.9A priority Critical patent/GB2585601B/en
Priority to KR1020207025246A priority patent/KR20200142499A/ko
Priority to CN201980025094.9A priority patent/CN112005324A/zh
Priority to DE112019001920.1T priority patent/DE112019001920T5/de
Priority to JP2020545531A priority patent/JP7223020B2/ja
Publication of WO2019199732A1 publication Critical patent/WO2019199732A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • H01F1/342—Oxides
    • H01F1/344—Ferrites, e.g. having a cubic spinel structure (X2+O)(Y23+O3), e.g. magnetite Fe3O4
    • H01F1/348—Hexaferrites with decreased hardness or anisotropy, i.e. with increased permeability in the microwave (GHz) range, e.g. having a hexagonal crystallographic structure
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    • 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
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Definitions

  • This disclosure is directed to grain-oriented M-type hexagonal ferrites that have high permeability and low magnetic loss over a broad range of operating frequencies.
  • High permeability and low magnetic loss at microwave frequencies will provide materials for the creation of electrically small antennas for electronic communications.
  • the unique magnetodielectric nature of ferrite substrates allows for miniaturization of antenna elements without the subsequent loss of bandwidth that is often observed in high dielectric constant substrates. Magnetodielectric materials thus have great potential for application in the miniaturization of antennas with broad bandwidth, which are widely used in personal mobile phones, base stations, and the like.
  • both microwave antennas and inductors are vital components in advanced microwave communications.
  • a grain-oriented M-type hexagonal ferrite has the formula
  • a method of making a doped, grain-oriented M-type hexagonal ferrite comprises preparing a plurality of ferrite grains of the formula
  • a dopant effective to provide planar magnetic anisotropy and easy magnetization in a c- plane, or a cone anisotropy, wherein Me is Sr 2+ , Ba 2+ , or Pb 2+ ; aligning the plurality of ferrite grains such that greater than 30%, preferably greater than 80% of the c-axes of the ferrite grains are aligned perpendicular to the c- plane, to provide the doped, grain-oriented M-type hexagonal ferrite; and optionally sintering the doped, grain-oriented M-type hexagonal ferrite at a temperature of greater than 800°C, preferably 800-1350°C to provide a sintered material having a density of at least 85% of a theoretical density, preferably greater than 90% of a theoretical density.
  • novel grain-oriented M-type hexagonal ferrites which can be used to provide magnetodielectric materials having high permeability and low magnetic loss over a broad range of operating frequencies, such as at the VHF band of 30-1000 MHz and the UHF band at 300-1000 MHz.
  • the materials disclosed herein can have relative permeabilities of greater than or equal to about 80, 100, or even 150 MHz and above, which have not previously been observed for hexagonal ferrite materials.
  • a grain-oriented M-type hexagonal ferrite has the formula
  • Grain-oriented hexagonal ferrites are also referred to as textured hexagonal ferrites.
  • Hexagonal ferrites have a crystalline structure in which the planar axis is referred to as the“a” (ai, a2, a 3 ) axis.
  • the c-plane plane is also referred to as the basal plane.
  • the c-axis is the axis out of the c-plane.
  • a proper dopant or mixture of dopants in a pure MFei 2 0i 9 structure can readily tailor a magnetic anisotropy from uniaxial c-axis to c-plane or easy cone- plane. As a result, easy magnetization can be modified from c-axis to c-plane or easy cone.
  • the c-axis becomes a hard axis, while the c-plane or cone plane is easy magnetization.
  • the inventors have developed M-type hexagonal ferrites with unexpectedly high alignment along the c-axis of the crystal structure while retaining easy magnetization in c-plane or cone plane.
  • the grain-oriented ferrites greater than 30%, preferably greater than 80%, of grains of the ferrite are aligned along the c-axis of the crystal structure, perpendicular to the c- plane.
  • the dopant provides planar magnetic anisotropy, that is, easy magnetization in the c- plane, or an easy cone anisotropy in the crystal.
  • the easy axis is defined as the preferred axis for the magnetization direction.
  • an easy cone anisotropy is an anisotropy for which the stable magnetic state(s) are at an angle around a particular, symmetry axis.
  • the dopant can be a single dopant, or a mixture of dopants.
  • the dopant comprises Co, Ti, Zr, Sn, Ir, Sc, In, Zn, Mg, Cu, Ni, Bi, Al, Ga, La, or a combination thereof.
  • the dopant comprises Co 2+ /Ti 4+ , Co 2+ /Zr 4+ , Co 2+ /Sn 4+ , Co 2+ /Ir 4+ , Bi 2+ /Co 2+ /Ti 4+ , Bi 2+ /Co 2+ /Zr 4+ , Bi 2+ /Co 2+ /Sn 4+ , or a combination thereof.
  • the dopant replaces at least a portion of the Fe in the grain-oriented M-type hexagonal ferrite.
  • a specific grain-oriented M-type hexagonal ferrite has the formula (Bi x Sr y Bai- x-y ) (CoTi) z Fei2-2 z Oi9, wherein x is 0.05-0.5, y is 0-1 and z is 0.5-2.0.
  • Sr substitutes for a portion of the Ba.
  • the grain- oriented M-type hexagonal ferrites can have one or more of a number of advantageous properties.
  • Relative permeability is a property indicative of the performance of a magnetic material in high frequency applications, and is a measure of the degree of magnetization of a material that responds linearly to an applied magnetic field relative to that of free species. Relative permeability can be measured by an impedance analyzer over 1-1000 MHz or a Vector network analyzer (VNA) with co-axial airline fixture over 0.5-10 GHz.
  • VNA Vector network analyzer
  • the grain-oriented M-type hexagonal ferrites can have an in-plane relative permeability of greater than 50, greater than 80, greater than 100, or greater than 150 over an operating frequency of 50 MHz-300 MHz.
  • the grain-oriented M-type hexagonal preferably can have an in-plane relative permeability of greater than 50, greater than 80, greater than 100, or greater than 150 at an operating frequency of 100 MHz.
  • the magnetic loss tangent, the dielectric loss tangent, and the dielectric constant are also measures of the magnetodielectric properties of a material.
  • the grain-oriented M-type hexagonal ferrites can have a magnetic loss tangent of less than 0.5, or even less than 0.2 at 100 MHz, preferably less than 0.1 at 100 MHz.
  • the magnetic loss tangent can be measured by impedance analyzer or VNA with coaxial airline fixture.
  • the grain-oriented M-type hexagonal ferrites can have a dielectric loss tangent of less than 0.02 over 0-300 MHz, preferably less than 0.03 at 30-300 MHz.
  • the dielectric loss tangent can be measured by impedance analyzer or VNA with coaxial airline fixture,
  • the grain-oriented M-type hexagonal ferrites can have a dielectric constant of 10- 30 over 30-300 MHz, or 6-30 over 300-1000 MHz.
  • the dielectric constant can be measured by an impedance analyzer or a VNA with a coaxial airline fixture.
  • the grain- oriented M-type hexagonal ferrites have an in-plane relative permeability of greater than 80 at an operating frequency over 50-300 MHz; and a magnetic loss tangent of less than 0.2 at 100 MHz, preferably less than 0.1 at 100 MHz.
  • the grain-oriented M-type hexagonal ferrites have a magnetic loss tangent of less than 0.5, or less than 0.2 over 30-300 MHz, preferably less than 0.1 over 30- 300 MHz; and a dielectric loss tangent of less than 0.05 over 30-300 MHz, preferably less than 0.02 over 30-300 MHz.
  • the grain-oriented M-type hexagonal ferrites have each of an in-plane permeability of greater than 50 over an operating frequency of 50 MHz-300 MHz or greater than 50 at an operating frequency of 100 MHz; a magnetic loss tangent of less than 0.5 at 100 MHz; a dielectric loss tangent of less than 0.02 over 0-300 MHz; and a dielectric constant of 10-30 over 30-300 MHz, or 6-30 over 300-1000 MHz.
  • the grain-oriented M-type hexagonal ferrite have each of an in-plane permeability of greater than 80 over an operating frequency of 50 MHz-300 MHz, or greater than 80 at an operating frequency of 100 MHz; a magnetic loss tangent of less 0.2 at 100 MHz; a dielectric loss tangent of less than 0.03 over 30-300 MHz; and a dielectric constant of 10-30 over 30-300 MHz, or 6-30 over 300-1000 MHz.
  • the grain-oriented M-type hexagonal ferrite has an in-plane permeability of greater than 150 over an operating frequency of 50 MHz-300 MHz, or greater than 150 at an operating frequency of 100 MHz; a magnetic loss tangent of less than 0.1 at 100 MHz; a dielectric loss tangent of preferably less than 0.03 at 30-300 MHz; and a dielectric constant of 6-30 over 300-1000 MHz.
  • the grain sizes of the grain-oriented M-type hexagonal ferrites in the c-plane can be 0.5-2 micrometer (pm), 2-6 pm, 6-20 pm, 20-100 pm, 100-200 pm, or up to 300 pm.
  • the grain-oriented M-type hexagonal ferrites are sintered. Sintering can be performed at a temperature of greater than 800°C, preferably 800-l350°C.
  • the sintered grain-oriented M-type hexagonal ferrites can have a sintered density of at least 85% of a theoretical density, preferably at least 90% of a theoretical density. The theoretical density is calculated by crystal structure and chemical formulation or x-ray diffraction measurement.
  • articles comprising the grain-oriented M-type hexagonal ferrites described herein.
  • Exemplary articles include an inductor, a perpendicular magnetic record, an antenna, a microwave absorber, an electromagnetic interference suppressor, or a shielding material, such as shielding materials in wireless power devices and near-field communication.
  • the doped, grain-oriented M-type hexagonal ferrites are expected to provide improved performance in the presence of the user’s hand or head, better absorbed radiation properties, and the like.
  • Also included herein is a method of making a doped, grain-oriented M-type hexagonal ferrite comprising preparing a plurality of ferrite grains of the formula
  • a dopant effective to provide planar magnetic anisotropy and easy magnetization in the c- plane, or an easy cone anisotropy, wherein Me is Sr 2+ , Ba 2+ or Pb 2+ ; aligning the plurality of ferrite grains such that greater than 30%, preferably greater than 80% of the c-axes of the ferrite grains are aligned perpendicular to the c- plane, to provide the doped, grain-oriented M- type hexagonal ferrite; and optionally sintering the doped, grain-oriented M-type hexagonal ferrite at a temperature of greater than 800°C, preferably 800-l350°C to provide a sintered material having a density of at least 85% of a theoretical density, preferably greater than 90% of a theoretical density.
  • the dopant is provided by substituting a portion of the Fe with CoTi, CoZr or CoSn.
  • preparing single grains comprises calcining and sintering dry powders, a sol-gel process, a molten salt process, a co-precipitation process, a sol-gel hydrothermal process, a hydrothermal process, or another chemical process.
  • Calcining/sintering dry powders is a conventional ceramic process.
  • BaFei 2 0i 9 powder is prepared by ball milling BaCo 3 and Fe 2 0 3 powders followed by calcining at 900-l200°C. The powder is doped with B12O3, for example, followed by additional ball milling to incorporate the dopant.
  • Ba(or Sr)Fei 2 0i 9 is prepared by dissolving Ba (or Sr) (N0 3 ) 2 and Fe(N0 3 ) 3 9H 2 0 in a solvent such as ethylene glycol, followed by dehydration to produce a gel, and calcining to provide the BaFei20i9 or SrFei20i9 powder.
  • a molten salt such as a chloride or a sulfate salt is used.
  • a mixture of reactants and salt is heated above the melting temperature of the salt, and product particles form.
  • the salt is removed using a solvent for the salt, typically water.
  • a BaFei 2 0i 9 powder is prepared by mixing iron nitrate and barium acetate powders at a selected Fe 3+ /Ba 2+ molar ratio and co- precipitating using NaOH at room temperature. The co-precipitated products are then calcined to provide the hexagonal ferrite.
  • an aqueous suspension containing barium hydroxide and FeOOH is heated slowly to a temperature of 250°C-325°C in an autoclave for example, and then cooled to room temperature to provide the hexagonal ferrite.
  • any of the hexagonal ferrite powders produced by the foregoing methods can be doped by adding a dopant such as B12O3, for example, followed by ball milling to incorporate the dopant.
  • the dopant can be added during synthesis of the hexagonal ferrite.
  • aligning the plurality of grains comprises applying a rotating in plane magnetic field to the grains while applying vertical mechanical pressure to the grains, applying a mechanical shearing force to the grains with or without applying a magnetic field, or a combination thereof. Applying a rotating magnetic field while applying mechanical pressure to the grains provides ferrite powder compaction during the alignment.
  • aligning the plurality of grains comprises applying a rotating in-plane magnetic field having a magnetic field has a strength of greater than 2000 Oersted (Oe), preferably greater than 8000 Oe.
  • the method optionally includes shaping the grain-oriented M-type hexagonal ferrite. That is, magnetic field alignment and mechanical pressing can be applied simultaneously to provide a powder compact, typically referred to as a green body.
  • Formation of the green body can be followed by sintering, for example at a temperature of 900- l300°C for 2-10 hours. Prior to sintering, the green compact can be cut to a specified
  • the green compact can be sintered in a mold to provide the shape of a component comprising the grain-oriented M-type hexagonal ferrite.
  • Aspect 2 The grain-oriented M-type hexagonal ferrite of aspect 1, wherein the dopant comprises Co, Ti, Zr, Sn, Sc, In, Zn, Mg, Cu, Ni, Bi, Al, Ga, La, or a combination thereof.
  • Aspect 3 The grain-oriented M-type hexagonal ferrite of aspect 1, wherein the dopant comprises Co 2+ /Ti 4+ , Co 2+ /Zr 4+ , Co 2+ /Sn 4+ , Bi 2+ /Co 2+ /Ti 4+ , Bi 2+ /Co 2+ /Zr 4+ , Bi 2+ /Co 2+ /Sn 4+ , or a combination thereof.
  • Aspect 7 The grain-oriented M-type hexagonal ferrite of any one or more of aspects 1-6, wherein the grain-oriented M-type hexagonal ferrite has at least one of
  • Aspect 8 The grain-oriented M-type hexagonal ferrite of aspect 7, wherein the grain-oriented M-type hexagonal ferrite has
  • Aspect 9 The grain-oriented M-type hexagonal ferrite of aspect 7, wherein the grain-oriented M-type hexagonal ferrite has
  • Aspect 10 The grain-oriented M-type hexagonal ferrite of any one or more of aspects 1-9, wherein the hexagonal ferrite has a sintered density of at least 85% of a theoretical density, preferably at least 90% of a theoretical density.
  • Aspect 11 The grain-oriented M-type hexagonal ferrite of any one or more of aspects 1-10, wherein the grain size in the c- plane is 0.5-2 pm, 2-6 pm, 6-20 pm, 20-100 pm, 100-200 pm, or up to 300 pm.
  • Aspect 12 An article comprising the grain-oriented M-type hexagonal ferrite of any one or more of aspects 1-11.
  • Aspect 13 The article of aspect 12, wherein the article is an inductor, a perpendicular magnetic record, an antenna, a microwave absorber, an electromagnetic interference suppressor, or a shielding material.
  • Aspect 14 A wireless power device or near-field communication device comprising the shielding material of aspect 13.
  • Aspect 15 A method of making a doped, grain-oriented M-type hexagonal ferrite of any one or more of aspects 1-11, the method comprising
  • MeFei20i9 comprising a dopant effective to provide planar magnetic anisotropy in the c- plane and easy magnetization in the c-plane, or an easy cone anisotropy, wherein Me is Sr 2+ , Ba 2+ or Pb 2+ ; aligning the plurality of ferrite grains such that greater than 30%, preferably greater than 80% of the ferrite grains are aligned along the c-axis of the crystal structure perpendicular to the c-plane, to provide the doped, grain-oriented M-type hexagonal ferrite; and
  • the doped, grain-oriented M-type hexagonal ferrite at a temperature of greater than 800°C, preferably 800-l350°C to provide a sintered material having a density of at least 85% of a theoretical density, preferably greater than 90% of a theoretical density.
  • Aspect 16 The method of aspect 15, wherein the dopant is provided by substituting a portion of the Fe with CoTi, CoZr, or CoSn.
  • Aspect 17 The method of any one of more of aspects 15 and 16, wherein preparing single grains comprises calcining and sintering dry powders, a sol-gel process, a molten salt process, a co-precipitation process, a hydrothermal process, or a chemical synthesis process.
  • Aspect 18 The method of any one or more of aspects 15-17, wherein aligning the plurality of grains comprises applying a rotating in-plane magnetic field to the grains while applying vertical mechanical pressure to the grains, applying a mechanical shearing force to the grains with or without applying a rotating magnetic field, or a combination thereof.
  • Aspect 19 The method of aspect 18, wherein aligning the plurality of grains comprises applying a rotating in-plane magnetic field having a magnetic field has a strength of greater than 2000 Oe, preferably greater than 8000 Oe.
  • Aspect 20 The method of any one or more of aspects 15-19, comprising, during aligning the plurality of ferrite grains, shaping the grain-oriented M-type hexagonal ferrite.
  • Aspect 21 The method of any one or more of aspects 15-20, comprising, prior to sintering, cutting the grain-oriented M-type hexagonal ferrite to a specified dimension.
  • compositions, methods, and articles can alternatively comprise, consist of, or consist essentially of, any ingredients, steps, or components herein disclosed.
  • the compositions, methods, and articles can additionally, or alternatively, be formulated, conducted, or manufactured so as to be devoid, or substantially free, of any ingredients, steps, or components not necessary to the achievement of the function or objectives of the claims.

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DE112019001920.1T DE112019001920T5 (de) 2018-04-12 2019-04-09 Texturierte planare hexagonale ferrite vom m-typ und verfahren zu deren verwendung
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