CN105174931B - The preparation method of NiCuZn Ferrite Material - Google Patents

The preparation method of NiCuZn Ferrite Material Download PDF

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CN105174931B
CN105174931B CN201510543515.0A CN201510543515A CN105174931B CN 105174931 B CN105174931 B CN 105174931B CN 201510543515 A CN201510543515 A CN 201510543515A CN 105174931 B CN105174931 B CN 105174931B
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CN105174931A (en
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孙科
郑照阳
余忠
蒋晓娜
兰中文
燕周民
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University of Electronic Science and Technology of China
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Abstract

The preparation method of NiCuZn Ferrite Material belongs to technical field of electronic materials, and the present invention includes the following steps: 1) to be formulated: using Ni0.52‑xCoxCu0.1Zn0.4Fe1.98O3.99, x=0-0.40；2) ball milling；3) pre-burning: ball milling material is dried, and pre-burning 2-4 hours in 900 DEG C of furnaces；4) it adulterates: following dopant: 0.001-0.80wt%BaTiO is added3, 0.01-0.20wt%CaCO3, 0.01-0.20wt%V2O5, 0.001-0.20wt%Bi2O3；5) secondary ball milling: ball milling 4-8 hours, final powder particle size was 0.6-1.0 μm after ball milling；6) it forms；7) be sintered: blank obtained by step 6) be placed in sintering furnace, 960-1080 DEG C heat preservation sintering 2-6 hours.NiCuZn Ferrite Material prepared by the present invention has the excellent characteristics such as high saturated magnetic induction, high-curie temperature, low-dielectric loss and low ferromagnetic resonance line width.

Description

The preparation method of NiCuZn Ferrite Material
Technical field
The invention belongs to technical field of electronic materials, in particular to a kind of NiCuZn Ferrite Material and preparation method.
Background technique
Microwave Iron Oxide Elements are microwave/millimeter wave electronic information as a branch very important in microwave device Indispensable component in communication equipment and system, be widely used in for a long time radar, microwave communication, satellite communication, The fields such as navigation, electronic countermeasure and microwave measurement system (see document 1.J.D.Adam, L.E.Davis, G.F.Dionne, E.F.Schloemann,and S.N.Stitzer,“Ferrite devices and materials,”IEEE Trans.Microwave Theory Tech.,vol.50,pp.721-737,2002.).The bandwidth of Microwave Iron Oxide Elements is inserted The high power ability to bear for entering the performances such as loss, isolation, differential phase shift and device, depends greatly on microwave iron The basic performance of ferrite is (see full microwave ferrite material Latest Development commentary [J] the magnetic material of 2. Han Zhi of document and device Part .2010,41 (4): 5-13).
Basis of the microwave ferrite material as Microwave Iron Oxide Elements, main tensor characteristic using permeability and The precessional motion made by the H under the collective effect of steady magnetic field H and microwave magnetic field h of ferromagnetic resonance effect, i.e. magnetization M, So microwave ferrite material is also known as gyromagnetic material.Its major requirement to material are as follows: strong with required saturated magnetization Spend Ms, high Curie temperature Tc, low ferromagnetic resonance line width Δ H and microwave dielectric loss tg δεAnd high high-power ion beam hc(i.e. self-rotating wave linewidth Δ HkIt is high) etc. (see the full microwave ferrite material of 3. Han Zhi of document general situation of development [J] magnetic material and Device, 2000,31 (5): 32-35).In recent decades, under the development of material preparation and representation technology and the promotion of the market demand, The research of microwave ferrite material has been achieved for significantly being in progress, by the design of Ferrite Material new component structure and respectively The application of kind of new glass forming theory, promotes to meet novel microwave Ferrite Material that various frequency range demands use and device is sent out Exhibition.The advantages that NiZn microwave ferrite material is high, temperature stability is good, resistivity is high with saturation magnetization is (see 4. Song of document New, Xu Junming, Zheng Liang are opened, microwave ferrite material is waited and its applies [J] material Leader .2009,23 (6): 45-49), extensively Ground is applied in the Microwave Iron Oxide Elements such as isolator, phase shifter, circulator, modulator.But it easily occurs porous in sintering Structure causes density lower, and ferromagnetic resonance line width is also higher.Use Cu2+Ionic compartmentation part Ni2+The NiCuZn ferrite of ion There is density height, M compared with NiZn ferritesThe advantages that greatly, resistivity is high (see document 5. Zheng Yalin, Xu Guangliang, Lai Zhenyu, Influence [J] piezoelectricity and acousto-optic of the equal .Cu content to the ferrite sintered performance of NiCuZn, 2007,29 (6): 707-709).
Summary of the invention
The technical problem to be solved by the invention is to provide one kind to have low-dielectric loss, low ferromagnetic resonance line width and height The high performance NiCuZn Ferrite Material of the microwave device of the excellent characteristics such as saturation induction density.
Core of the invention thought is: use suitable NiCuZn ferrite iron deficiency formula, then its conductive mechanism is p-type, Material has high resistivity, can significantly reduce high-frequency dielectric loss；NiO is substituted using suitable CoO, on the one hand to material Theoretical molecular magnetic moment slightly improves, and achievees the effect that promotion to saturation induction density；On the other hand, the CoFe that CoO is formed2O4 Ferritic magnetocrystalline anisotropy constant is positive, can be with the NiFe that is formed by NiO2O4Ferritic magnetocrystalline anisotropy constant shape At compensation, the magnetocrystalline anisotropy constant of material is significantly reduced, anisotropy line width is reduced, finally reduces ferromagnetic resonance line width； Meanwhile reducing ZnO content as far as possible in formula, and then guarantee that material has high Curie temperature.On dopant, use BaTiO3、CaCO3、V2O5、Bi2O3Equal dopants, on the one hand, reduce sintering temperature, improve density, it is strong to increase saturation induction Degree；On the other hand, control crystallite dimension should not be too large, and improves the microstructural uniformity of material, improves the resistivity of material, drop Low-dielectric loss.Based on the control of above-mentioned two aspects micro-structure, stomata broadening is significantly reduced.
The present invention solve the technical problem the technical solution adopted is that, the preparation method of NiCuZn Ferrite Material, packet Include following steps:
1) it is formulated
Using Ni0.52-xCoxCu0.1Zn0.4Fe1.98O3.99, x=0-0.40；
2) ball milling
The powder being formulated above is uniformly mixed in ball mill, the time is 1-3 hours, and ball-milling medium is steel ball；
3) pre-burning
By the drying of ball milling material obtained by step 2), and pre-burning 2-4 hours in 900 DEG C of furnaces；
4) it adulterates
Following dopant: 0.001-0.80wt%BaTiO is added in powder obtained by step 3) by weight3、0.01- 0.20wt%CaCO3, 0.01-0.20wt%V2O5, 0.001-0.20wt%Bi2O3；
5) secondary ball milling
By powder obtained in step 4) ball milling 4-8 hours in the ball mill, ball-milling medium was zirconium ball, final powder particle size It is 0.6-1.0 μm；
6) it forms
By feed powder obtained by step 5) by weight 10-16wt% organic bond is added, mix, after granulation, on press Granular powder is pressed into blank；
7) it is sintered
By blank obtained by step 6) be placed in sintering furnace 960-1080 DEG C heat preservation sintering 2-6 hours.
It is using feed powder weight as calculation basis, for example, adding in 100g feed powder that dopant is added in step 4) by weight Enter 0.80wt%BaTiO3, refer to the BaTiO that 0.8g is added3.Organic bond is also similarly.
Prepare NiCuZn Ferrite Material by process above, saturation induction density, residual magnetic flux density and The coercivity rugged SY-8232B-H analyzer test of Japanese rock, density are tested with drainage, and ferromagnetic resonance line width is according to GB/ T9633-200 ×/IEC60556:2005 standard tests Φ 0.8mm bead sample at 9.25GHz, and dielectric loss angle tangent is pressed Circle rod-like samples are measured at 9.25GHz according to IEC standard.
Essence of the invention is to obtain the high-performance NiCuZn iron that microwave device uses using conventional solid-state method process flow Ferrite.NiCuZn Ferrite Material prepared by the present invention has high saturated magnetic induction, high-curie temperature, low dielectric damage The excellent characteristics such as consumption and low ferromagnetic resonance line width.
The technology of preparing of NiCuZn Ferrite Material of the invention, technical indicator are as follows:
Saturation induction density BBs: >=450mT (25 DEG C)
Ferromagnetic resonance line width Δ H :≤85Oe
Dielectric loss tan δε:≤2.0 × 10-4
Curie temperature Tc: >=320 DEG C
Electricalresistivityρ: >=106Ω·m
Density db: >=5.2g/cm3
Specific embodiment
A kind of embodiment 1: NiCuZn Ferrite Material and preparation method thereof, comprising the following steps:
1) it is formulated
Using Ni0.37Co0.15Cu0.1Zn0.4Fe1.98O3.99；
2) ball milling
The powder being formulated above is uniformly mixed in ball mill, the time is 2 hours, and ball-milling medium is steel ball；
3) pre-burning
By the drying of ball milling material obtained by step 2), and pre-burning 2.5 hours in 900 DEG C of furnaces；
4) it adulterates
Following dopant: 0.10wt%BaTiO is added in powder obtained by step 3) by weight3, 0.12wt%CaCO3、 0.08wt%V2O5, 0.12wt%Bi2O3；
5) secondary ball milling
By powder obtained in step 4), ball milling 6 hours, ball-milling medium are zirconium ball in the ball mill, and final powder particle size is 0.6-1.0μm；
6) it forms
By feed powder obtained by step 5) by weight 15wt% organic bond is added, mix, after granulation, by grain on press Shape powder pressing is at blank；
7) it is sintered
Blank obtained by step 6) is placed in sintering in sintering furnace, keeps the temperature 3 hours at 1040 DEG C.
A kind of embodiment 2: NiCuZn Ferrite Material and preparation method thereof, comprising the following steps:
1) it is formulated
Using Ni0.37Co0.15Cu0.1Zn0.4Fe1.98O3.99；
2) ball milling
The powder being formulated above is uniformly mixed in ball mill, the time is 2 hours, and ball-milling medium is steel ball；
3) pre-burning
By the drying of ball milling material obtained by step 2), and pre-burning 2.5 hours in 900 DEG C of furnaces；
4) it adulterates
Following dopant: 0.20wt%BaTiO is added in powder obtained by step 3) by weight3, 0.06wt%CaCO3、 0.12wt%Bi2O3；
5) secondary ball milling
By powder obtained in step 4), ball milling 6 hours, ball-milling medium are zirconium ball in the ball mill, and final powder particle size is 0.6-1.0μm；
6) it forms
By feed powder obtained by step 5) by weight 15wt% organic bond is added, mix, after granulation, by grain on press Shape powder pressing is at blank；
7) it is sintered
Blank obtained by step 6) is placed in sintering in sintering furnace, keeps the temperature 3 hours at 1040 DEG C.
A kind of embodiment 3: NiCuZn Ferrite Material and preparation method thereof, comprising the following steps:
1) it is formulated
Using Ni0.32Co0.2Cu0.1Zn0.4Fe1.98O3.99；
2) ball milling
The powder being formulated above is uniformly mixed in ball mill, the time is 2 hours, and ball-milling medium is steel ball；
3) pre-burning
By the drying of ball milling material obtained by step 2), and pre-burning 2.5 hours in 900 DEG C of furnaces；
4) it adulterates
Following dopant: 0.10wt%BaTiO is added in powder obtained by step 3) by weight3, 0.12wt%CaCO3、 0.08wt%V2O5, 0.12wt%Bi2O3；
5) secondary ball milling
By powder obtained in step 4), ball milling 6 hours, ball-milling medium are zirconium ball in the ball mill, and final powder particle size is 0.6-1.0μm；
6) it forms
By feed powder obtained by step 5) by weight 15wt% organic bond is added, mix, after granulation, by grain on press Shape powder pressing is at blank；
7) it is sintered
Blank obtained by step 6) is placed in sintering in sintering furnace, keeps the temperature 3 hours at 1040 DEG C.
A kind of embodiment 4: NiCuZn Ferrite Material and preparation method thereof, comprising the following steps:
1) it is formulated
Using Ni0.32Co0.20Cu0.1Zn0.4Fe1.98O3.99；
2) ball milling
The powder being formulated above is uniformly mixed in ball mill, the time is 2 hours, and ball-milling medium is steel ball；
3) pre-burning
By the drying of ball milling material obtained by step 2), and pre-burning 2.5 hours in 900 DEG C of furnaces；
4) it adulterates
Following dopant: 0.20wt%BaTiO is added in powder obtained by step 3) by weight3, 0.06wt%CaCO3、 0.12wt%Bi2O3；
5) secondary ball milling
By powder obtained in step 4), ball milling 6 hours, ball-milling medium are zirconium ball in the ball mill, and final powder particle size is 0.6-1.0μm；
6) it forms
By feed powder obtained by step 5) by weight 15wt% organic bond is added, mix, after granulation, by grain on press Shape powder pressing is at blank；
7) it is sintered
Blank obtained by step 6) is placed in sintering in sintering furnace, 1040 DEG C heat preservation sintering 3 hours.
Test result is as follows by embodiment 1-4:

Claims (5)

  1. The preparation method of 1.NiCuZn Ferrite Material, which is characterized in that include the following steps:
    1) it is formulated
    Using Ni0.52-xCoxCu0.1Zn0.4Fe1.98O3.99, x=0.15~0.20；
    2) ball milling
    The powder being formulated above is uniformly mixed in ball mill, the time is 1-3 hours, and ball-milling medium is steel ball；
    3) pre-burning
    By the drying of ball milling material obtained by step 2), and pre-burning 2-4 hours in 900 DEG C of furnaces；
    4) it adulterates
    Following dopant: 0.001-0.80wt%BaTiO is added in powder obtained by step 3) by weight3, 0.01-0.20wt% CaCO3, 0.01-0.20wt%V2O5, 0.001-0.20wt%Bi2O3；
    5) secondary ball milling
    By powder obtained in step 4) ball milling 4-8 hours in the ball mill, final powder particle size was 0.6-1.0 μm after ball milling；
    6) it forms
    By feed powder obtained by step 5) by weight 10-16wt% organic bond is added, mix, after granulation, by grain on press Shape powder pressing is at blank；
    7) it is sintered
    Blank obtained by step 6) is placed in sintering furnace, 960-1080 DEG C heat preservation sintering 2-6 hours；
    Preparation gained NiCuZn Ferrite Material has following performances:
    Saturation induction density Bs: >=450mT (25 DEG C)
    Ferromagnetic resonance line width Δ H :≤85Oe
    Dielectric loss tan δε:≤2.0 × 10-4
    Curie temperature Tc: >=320 DEG C.
  2. 2. the preparation method of NiCuZn Ferrite Material as described in claim 1, which is characterized in that
    In step 1), using Ni0.37Co0.15Cu0.1Zn0.4Fe1.98O3.99；
    In step 2), Ball-milling Time 2 hours；
    In step 3), burn-in time 2.5 hours；
    In step 4), dopant 0.10wt%BaTiO3, 0.12wt%CaCO3, 0.08wt%V2O5, 0.12wt%Bi2O3；
    In step 5), ball-milling medium is zirconium ball, and final powder particle size is 0.6-1.0 μm；
    In step 6), by weight addition 15wt% organic bond；
    In step 7), 1040 DEG C heat preservation sintering 3 hours.
  3. 3. the preparation method of NiCuZn Ferrite Material as described in claim 1, which is characterized in that
    In step 1), using Ni0.37Co0.15Cu0.1Zn0.4Fe1.98O3.99；
    In step 2), Ball-milling Time is 2 hours, and ball-milling medium is steel ball；
    In step 3), the pre-burning 2.5 hours in 900 DEG C of furnaces；
    In step 4), following dopant: 0.20wt%BaTiO is added3, 0.06wt%CaCO3, 0.12wt%Bi2O3；
    In step 5), ball milling 6 hours, ball-milling medium was zirconium ball, and final powder particle size is 0.6-1.0 μm；
    In step 6), by weight addition 15wt% organic bond；
    In step 7), 1040 DEG C heat preservation sintering 3 hours.
  4. 4. the preparation method of NiCuZn Ferrite Material as described in claim 1, which is characterized in that
    In step 1), using Ni0.32Co0.2Cu0.1Zn0.4Fe1.98O3.99；
    In step 2), Ball-milling Time is 2 hours, and ball-milling medium is steel ball；
    In step 3), the pre-burning 2.5 hours in 900 DEG C of furnaces；
    In step 4), following dopant: 0.10wt%BaTiO is added by weight3, 0.12wt%CaCO3, 0.08wt%V2O5、 0.12wt%Bi2O3；
    In step 5), ball milling 6 hours, ball-milling medium was zirconium ball, and final powder particle size is 0.6-1.0 μm；
    In step 6), 15wt% organic bond is added；
    In step 7), 1040 DEG C heat preservation sintering 3 hours.
  5. 5. the preparation method of NiCuZn Ferrite Material as described in claim 1, which is characterized in that
    In step 1), using Ni0.32Co0.20Cu0.1Zn0.4Fe1.98O3.99；
    In step 2), Ball-milling Time is 2 hours, and ball-milling medium is steel ball；
    In step 3), the pre-burning 2.5 hours in 900 DEG C of furnaces；
    In step 4), following dopant: 0.20wt%BaTiO is added by weight3, 0.06wt%CaCO3, 0.12wt%Bi2O3；
    In step 5), ball milling 6 hours, ball-milling medium was zirconium ball, and final powder particle size is 0.6-1.0 μm；
    In step 6), by weight addition 15wt% organic bond；
    In step 7), 1040 DEG C heat preservation sintering 3 hours.
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CN105924146B (en) * 2016-04-25 2018-04-20 西南应用磁学研究所 High-power multilayer sheet type ferrite device wide warm nickel zinc LTCF materials and preparation method
CN106747397B (en) * 2017-03-09 2021-02-12 电子科技大学 YIG ferrite material and preparation method thereof
CN107619271A (en) * 2017-08-10 2018-01-23 中国振华(集团)新云电子元器件有限责任公司(国营第四三二六厂) NiCuZn Ferrite Materials and preparation method thereof, application
CN108558383B (en) * 2018-04-04 2021-10-15 全球能源互联网研究院有限公司 NiZn ferrite material and preparation method thereof
CN108773858A (en) * 2018-07-10 2018-11-09 电子科技大学 A kind of pattern-band Surface Wave Absorbing Material and preparation method thereof
CN112321291A (en) * 2020-10-09 2021-02-05 北京无线电测量研究所 High-saturation low-temperature sintered gyromagnetic Ni-series spinel ferrite material and preparation method thereof
CN113461414A (en) * 2021-07-06 2021-10-01 深圳市华扬通信技术有限公司 Ferrite suitable for millimeter wave microstrip circulator and preparation method and application thereof
CN114890779B (en) * 2022-03-23 2023-05-05 电子科技大学 Garnet ferrite with high mechanical strength, high power and low resonance linewidth and preparation method thereof
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CN116283265A (en) * 2023-04-14 2023-06-23 电子科技大学 Low-temperature sintered NiCuZn power ferrite and preparation method thereof

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