CN101575206A - High-frequency high-power Ni-Zn base magnetic ferrite material and manufacturing method thereof - Google Patents
High-frequency high-power Ni-Zn base magnetic ferrite material and manufacturing method thereof Download PDFInfo
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- CN101575206A CN101575206A CNA2008100696370A CN200810069637A CN101575206A CN 101575206 A CN101575206 A CN 101575206A CN A2008100696370 A CNA2008100696370 A CN A2008100696370A CN 200810069637 A CN200810069637 A CN 200810069637A CN 101575206 A CN101575206 A CN 101575206A
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Abstract
The invention discloses a high-frequency high-power Ni-Zn base magnetic ferrite material and a manufacturing method thereof. The Ni-Zn base magnetic ferrite material comprises a main ingredient, an ionic substitute ingredient and a compound composite and doped ingredient, wherein the main ingredient comprises Fe2O3, ZnO and the balance of NiO; the ionic substitute ingredient comprises one or more kinds of Co3O4, MnCO3 and CuO containing Co3O4; and the compound composite and doped ingredient comprises 2-3 kinds of V2O5, Bi2O3, Ta2O5, ZrO2, CuO, Nb2O5 and Co3O4. The manufacturing method comprises the following steps: (a) preparing a Ni-Zn base ferrite main ingredient mixture; (b) preparing a main ingredient pre-sintered material; (c) preparing micro-fine ferrite powder; (d) preparing a raw blank of a magnetic core; and (e) sintering the magnetic core. The invention obtains the Ni-Zn base magnetic ferrite material with high electromagnetic performance, high strength, high frequency and low loss by optimizing the composite design of a formulation and adopting the manufacturing method of the high-frequency high-power Ni-Zn base magnetic ferrite material. The Ni-Zn base magnetic ferrite material is used for high-power equipment of 1-30MHz and used as the magnetic core for a transformer, an inductor, a filter, a tuner, and the like.
Description
Technical field
The present invention relates to a kind of Ni-Zn base magnetic ferrite material and manufacture method thereof, particularly a kind of high-frequency high-power Ni-Zn base magnetic ferrite material and manufacture method thereof.
Background technology
The NiZn soft magnetic ferrite is a class soft magnetic materials important in the magneticsubstance, Yin Qiyi forms little crystal grain, vesicular structure, electricalresistivity's height, high frequency characteristics that losstangenttan is low, good, so be widely used in the electronic product in high frequency fields such as aviation, navigation, communication, broadcast television, instrument, electric power, network digitalization, control automatically, computer, automobile, medicine equipment, high-frequency induction welder, household electrical appliance, Green Lighting Project, anti-electromagnetic interference, as inducer, transformer, wave filter, reactance coil, no line oscillator equimagnetic core.When making wide frequency band device, its lower frequency limit can arrive several kilohertzs, upper limiting frequency can reach several Gigahertzs, as radio-frequency transformer, impedance transformer, power division/synthesizer, frequency mixer, radio frequency amplifier, directional coupler, electrically controlled attenuator, phase detector etc.
Development along with electronic industry, information industry, digital technique and Fibre Optical Communication Technology etc., performance to soft magnetic ferrite has proposed new requirement, can not satisfy the service requirements of specific occasion (as the high-frequency high-power occasion) with the common NiZn soft magnetic ferrite of conventional dry conventional ceramic technique (low energy ball milling) preparation, therefore, adopt new chemical process to prepare Ferrite Material in recent years more and more, as chemical co-precipitation method, hydrothermal method, microemulsion method, sol-gel method, self propagating high temperature synthesis method, spray roasting, high-energy ball milling method etc.But to the different purposes and the performance requriements of material, these new chemical process all come with some shortcomings and shortcoming, need to improve and improve, to satisfy the material development new demand of using the preparation specific occasion.Simultaneously, high speed development along with electronics and information industry, also more and more to the soft magnetic materials demand that the high-frequency high-power state is used down, but in the prior art, common NiZn soft magnetic ferrite is lower in the over-all properties of physicals, mechanical property and magnetic property, and unstable product quality, the product performance preparation is repeatable poor, therefore influences its application in the high-frequency high-power occasion.Common NiZn soft magnetic ferrite is under high-power condition, because the electric current of order of amps intensity passes through magnetic core coil, the core loss height, heating is big, temperature rise is fast, temperature is high causes magnetic core " to burst " or magnetic core " inefficacys " and product cisco unity malfunction, or owing to electric current formed foreign field increase causes the magnetic core magneticsaturation to can't pass the transmission signal.Therefore, can bear NiZn base soft magnetic ferrite high-power and can the stable delivery signal under high frequency, must be a kind of improved extraordinary NiZn base soft magnetic ferrite with good over-all properties.NiZn base soft magnetic ferrite provided by the invention has superperformance at aspects such as physicals, mechanical property and magnetic properties, especially the over-all properties under the high-frequency high-power condition.
Summary of the invention
Purpose of the present invention is exactly at the deficiencies in the prior art, adopt principal constituent optimum combination, ion substitution, combination doping vario-property and special preparation (fine ferrite powder, high quality green compact and low temperature high density material sintering) technology, strict control of material preparation process, a kind of high-frequency high-power Ni-Zn base magnetic ferrite material and manufacture method thereof with good physical behavior, mechanical property and magnetic property is provided, thereby realizes the special use under its high-frequency high-power condition.
For achieving the above object, the present invention adopts following technical matters scheme:
A kind of high-frequency high-power Ni-Zn base magnetic ferrite material is doping to by principal constituent, ion substitution composition and compound combination and is grouped into, and its principal constituent is: Fe
2O
347～50.25mol%, ZnO10～27.5mol%, surplus is NiO; The ion substitution composition that is used for alternative NiO is: Co
3O
40.05～4mol%, MnCO
3Contain Co among 0～5mol%, the CuO0～12.5mol%
3O
4One or more, principal constituent and ion substitution composition constitute major ingredient; The compound combination is doping to and is divided into: V
2O
5, Bi
2O
3, Ta
2O
5, ZrO
2, CuO, Nb
2O
5, Co
3O
4In 2～3 kinds; Compound combination doping composition incorporation is counted by the major ingredient weight percent behind ion substitution: V
2O
50～0.5wt%, Bi
2O
30～0.5wt%, Ta
2O
50～0.5wt%, ZrO
20～1.0wt%, CuO0～0.5wt%, Nb
2O
50～0.5wt%, Co
3O
40～1.0wt%.
Preferably, described ion substitution composition is: Co
3O
40.15～2mol%, MnCO
3Contain Co among 0～3mol%, the CuO0～8mol%
3O
4One or more.
Preferably, described compound combination doping composition incorporation is counted by the major ingredient weight percent behind ion substitution: V
2O
50～0.3wt%, Bi
2O
30～0.3wt%, Ta
2O
50～0.3wt%, ZrO
20～0.5wt%, CuO0～0.3wt%, Nb
2O
50～0.3wt%, Co
3O
4Among 0～0.5wt% 2～3 kinds.
Preferably, described compound combination doped forms is: a class doping V
2O
5, Bi
2O
3, Ta
2O
5In a kind of and two class doping ZrO
2, CuO, Nb
2O
5, Co
3O
4In one or both combinations mix.
Material composition unitized design of the present invention is with ingredient formula Ni
xZn
yCo
zMn
uCu
vFe
wO
4Be the main formula scope, wherein principal constituent is: 0.2≤x≤0.92,0.2≤y≤0.55,1.88≤w≤2.01; The composition that is used for the substitutional ion of alternative Ni is: 0.003≤z≤0.24,0≤u≤0.1,0≤v≤0.25; And satisfy x+y+z+u+v+w=1.Doping is with V
2O
5, Bi
2O
3, Ta
2O
5, ZrO
2, CuO, Nb
2O
5, Co
3O
4In 2～3 kinds of combinations mix.By composition is optimized combination, obtain initial permeability μ
i, magnetic property such as saturation induction density Bs, Curie temperature Tc and the electricalresistivity is high as far as possible and loss Pcv (tan δ/μ
i) alap optimum formula composition.
The preparation method of above-mentioned high-frequency high-power Ni-Zn base magnetic ferrite material may further comprise the steps:
A), the wet method mix grinding prepares NiZn based ferrite major ingredient compound
Take by weighing the deionized water of major ingredient, 1.1 times of weight parts of major ingredient, the steel ball of 2 times of weight parts of major ingredient in proportion, place and carry out the wet method mix grinding in the ball mill cylinder of steel, the mix grinding linear velocity is not less than 300m/min, and the mix grinding time is not less than 2h, obtain the compound of good uniformity, oven dry was pulverized behind 40 mesh sieves standby;
B), the low-temperature sintering chilling prepares the pre-imitation frosted glass of NiZn based ferrite major ingredient
With the NiZn based ferrite compound of step a preparation in air with more than 800～950 ℃ of pre-burning 2h, adopt emergency cooling process to obtain the preburning powdered material of the particle diameter of single spinel phase less than 1 μ m;
C), high energy mechanical wet ball-milling method prepares fine NiZn based ferrite powder
The NiZn based ferrite major ingredient preburning powdered material of step b preparation is mixed compound combination doping composition in proportion, add 1.1 times of parts by weight of deionized water of major ingredient, 2 times of weight part steel balls of major ingredient, place and carry out ball milling in the ball mill cylinder of steel, the ball milling linear velocity is not less than 350m/min, the ball milling time is not less than 12h, makes the ball milling powder particles be distributed as 0.1～0.2 μ m, and volumetric concentration is greater than 80%, become single spinel phase pollution-free, no dephasign, oven dry was pulverized behind 40 mesh sieves standby;
D), preparation magnetic core green compact
Ferrite powder with step c preparation mixes binding agent in 10～20% ratios and carries out granulation, and binding agent is the polyvinyl alcohol water solution of 6～15% concentration; The pressure that adopts 300～600MPa is pressed into the magnetic core green compact of desired shape with the granulation material, and the density that makes described magnetic core green compact is 3.2～3.7g/cm
3
E), low temperature high density sintering magnetic core
With the magnetic core green compact of steps d preparation, with more than 850～1050 ℃ of sintering 4h, the relative density of sintered blank is greater than 93% in nitrogen/oxygen gas mixture atmosphere, and actual density is not less than 5.0g/cm
3, promptly get high-frequency high-power Ni-Zn base magnetic ferrite material.
Material of the present invention adopts high energy mechanical ball milling wet powder-making electronic ceramic process, and its main technique route and node are as follows:
The present invention adopts special alloy abrading-ball and high energy mechanical wet ball-milling legal system to be equipped with the high fine NiZn based ferrite powder of uniformity consistency, and powder particles is distributed as 0.1～0.2 μ m, and volumetric concentration is greater than 80%.
The present invention adopt mix 6～15% cause particulate material through adding dispersion agent, antifoams, lubricant modified low ash content binding agent (polyvinyl alcohol) aqueous solution
The present invention adopts novel high-strength high rigidity special alloy mould, big pressure 300～600MPa (being generally less than 200MPa) pressure compacting uniform high strength degree magnetic core green compact to NiZn based ferrite particulate material, and its green density is 3.2～3.7g/cm
3
The present invention adopts the processing method of the pre-sinter process of 800 ℃～950 ℃ of sintering chillings of atmosphere and nitrogen/850～1050 ℃ of low temperature high density double sinterings of oxygen gas mixture atmosphere that flow to NiZn based ferrite material, and strict control air pressure and sintering process are to obtain homogeneous microstructure, crystal grain is tiny, defective is few and density is high microstructure tissue, realize high electromagnetic performance, high strength and the high-frequency low-consumption performance of material, the relative density of its sintered blank is greater than 93%, and actual density is not less than 5.0g/cm
3, ultimate compression strength＞400N/mm
2
High-power Ni-Zn base magnetic ferrite material of the present invention have high saturated magnetic induction Bs (＞380mT), high-curie temperature Tc (＞280 ℃), good than temperature factor α
μ/ μ
i(5～+ 30 * 10
-6/ ℃), high resistivity ρ (＞10
8Ω cm), high-density d (＞5.0g/cm
3), high compressive strength (＞400N/mm
2), low-loss tan δ/μ
i(＜20/2MHz) or reduce power consumption Pcv (＜450KW/m
3/ 2MHz, 25mT/5MHz, 10mT), higher initial permeability μ
i(100～500) and same magnetic permeability have higher limiting frequency fr (15～90MHz) relatively.
The beneficial effect of high-power Ni-Zn base magnetic ferrite material of the present invention and manufacture method thereof is, by extraordinary formulation optimization unitized design, obtain initial permeability, saturation induction density, Curie temperature, resistivity four height and the low NiZn Ferrite Material of loss.Use The addition of C o
2+, Mn
2+And Cu
2+Substitute Ni
2+Can guarantee material have on the basis of high initial permeability, high saturated magnetic induction, high-curie temperature characteristic improve resistivity, the factor and increase limiting frequency of reducing the wastage, thereby improve the electromagnetic property of material.An amount of compound that mixes can improve the electromagnetic property of material, comprises physical and mechanical property.Prescription is after improving, and prepare fine ferrite powder, big pressure forming high quality green compact and low-temperature sintering ferrite of high density material through the high energy mechanical wet ball-milling, the over-all properties of Ferrite Material obviously improves, and material has high saturated magnetic induction, high-curie temperature, good ratio temperature factor, high resistivity, high-density, high compressive strength, low-loss (reduce power consumption), higher initial permeability and same magnetic permeability higher limiting frequency is arranged relatively.Material of the present invention is used for 1～30MHz high-power, and (200～3000kW) equipment especially are as magnetic cores such as transformer, inductor block, wave filter and tuners.
Embodiment
The present invention is further illustrated below in conjunction with embodiment, but therefore do not limit the present invention among the described scope of embodiments.
The specific embodiment composition proportion that the specific embodiment high-frequency high-power Ni-Zn base magnetic ferrite material becomes to be grouped into sees Table 1:
Table 1 becomes to be grouped into
The high-frequency high-power Ni-Zn base magnetic ferrite material preparation method may further comprise the steps:
A), the wet method mix grinding prepares NiZn based ferrite major ingredient compound
Take by weighing the deionized water of major ingredient, 1.1 times of weight parts of major ingredient, the steel ball of 2 times of weight parts of major ingredient in proportion, place and carry out the wet method mix grinding in the ball mill cylinder of steel, the mix grinding linear velocity is not less than 300m/min, and the mix grinding time is not less than 2h, obtain the compound of good uniformity, oven dry was pulverized behind 40 mesh sieves standby;
B), the low-temperature sintering chilling prepares the pre-imitation frosted glass of NiZn based ferrite major ingredient
With the NiZn based ferrite compound of step a preparation in air with more than 800～950 ℃ of pre-burning 2h, adopt emergency cooling process to obtain the preburning powdered material of the little 1 μ m of particle diameter of single spinel phase;
C), high energy mechanical wet ball-milling method prepares fine NiZn based ferrite powder
The NiZn based ferrite major ingredient preburning powdered material of step b preparation is mixed compound combination doping composition in proportion, add 1.1 times of parts by weight of deionized water of major ingredient, 2 times of weight part steel balls of major ingredient, place and carry out ball milling in the ball mill cylinder of steel, the ball milling linear velocity is not less than 350m/min, the ball milling time is not less than 12h, makes the ball milling powder particles be distributed as 0.1～0.2 μ m, and volumetric concentration is greater than 80%, become single spinel phase pollution-free, no dephasign, it is standby that the back is pulverized in taking-up;
D), preparation magnetic core green compact
Ferrite powder with step c preparation mixes binding agent in 10～20% ratios and carries out granulation, and binding agent is the polyvinyl alcohol water solution of 6～15% concentration.The granulation material adopts the pressure of 300～600MPa to be pressed into the magnetic core green compact of desired shape, and the density that makes described magnetic core green compact is 3.2～3.7g/cm
3
E), low temperature high density sintering magnetic core
With the magnetic core green compact of steps d preparation, with more than 850～1050 ℃ of sintering 4h, the relative density of sintered blank is greater than 93% in nitrogen/oxygen gas mixture atmosphere, and actual density is not less than 5.0g/cm
3, promptly get high-frequency high-power Ni-Zn base magnetic ferrite material.
The processing parameter of specific embodiment sees Table 2
Table 2 processing parameter
High-frequency high-power Ni-Zn base magnetic ferrite material sample over-all properties sees Table 3:
Table 3 sample over-all properties
In the table 3: Bs: saturation induction density mT; Tc: Curie temperature ℃; α
μ/ μ
i: than temperature factor ℃
-1ρ: resistivity Ω cm; D: density g/cm
3Tan δ/μ
i: specific loss 2MHz; Pcv: power consumption KW/m
3(2MHz, 25mT; 5MHz, 10mT); μ
i: initial permeability; Fr: limiting frequency MHz; σ
p: ultimate compression strength N/mm
2
Claims (5)
1, a kind of high-frequency high-power Ni-Zn base magnetic ferrite material is characterized in that: be doping to by principal constituent, ion substitution composition and compound combination and be grouped into, its principal constituent is: Fe
2O
347～50.25mol%, ZnO10～27.5mol%, surplus is NiO; The ion substitution composition that is used for alternative NiO is: Co
3O
40.05～4mol%, MnCO
3Contain Co among 0～5mol%, the CuO0～12.5mol%
3O
4One or more, principal constituent and ion substitution composition constitute major ingredient; The compound combination is doping to and is divided into: V
2O
5, Bi
2O
3, Ta
2O
5, ZrO
2, CuO, Nb
2O
5, Co
3O
4In 2～3 kinds; Compound combination doping composition incorporation is counted by the major ingredient weight percent behind ion substitution: V
2O
50～0.5wt%, Bi
2O
30～0.5wt%, Ta
2O
50～0.5wt%, ZrO
20～1.0wt%, CuO0～0.5wt%, Nb
2O
50～0.5wt%, Co
3O
40～1.0wt%.
2, high-frequency high-power Ni-Zn base magnetic ferrite material according to claim 1 is characterized in that: described ion substitution composition is: Co
3O
40.15～2mol%, MnCO
3Contain Co among 0～3mol%, the CuO0～8mol%
3O
4One or more.
3, high-frequency high-power Ni-Zn base magnetic ferrite material according to claim 1 is characterized in that: described compound combination doping composition incorporation is counted by the major ingredient weight percent behind ion substitution: V
2O
50～0.3wt%, Bi
2O
30～0.3wt%, Ta
2O
50～0.3wt%, ZrO
20～0.5wt%, CuO0～0.3wt%, Nb
2O
50～0.3wt%, Co
3O
4Among 0～0.5wt% 2～3 kinds.
4, high-frequency high-power Ni-Zn base magnetic ferrite material according to claim 1 is characterized in that: described compound combination doped forms is: a class doping V
2O
5, Bi
2O
3, Ta
2O
5In a kind of and two class doping ZrO
2, CuO, Nb
2O
5, Co
3O
4In one or both combinations mix.
5, the preparation method of the described high-frequency high-power Ni-Zn base magnetic ferrite material of claim 1 is characterized in that may further comprise the steps:
A), the wet method mix grinding prepares NiZn based ferrite major ingredient compound
Take by weighing the deionized water of major ingredient, 1.1 times of weight parts of major ingredient, the steel ball of 2 times of weight parts of major ingredient in proportion, place and carry out the wet method mix grinding in the ball mill cylinder of steel, the mix grinding linear velocity is not less than 300m/min, and the mix grinding time is not less than 2h, obtain the compound of good uniformity, oven dry was pulverized behind 40 mesh sieves standby;
B), the low-temperature sintering chilling prepares the pre-imitation frosted glass of NiZn based ferrite major ingredient
With the NiZn based ferrite compound of step a preparation in air with more than 800～950 ℃ of pre-burning 2h, adopt emergency cooling process to obtain the preburning powdered material of the particle diameter of single spinel phase less than 1 μ m;
C), high energy mechanical wet ball-milling method prepares fine NiZn based ferrite powder
The NiZn based ferrite major ingredient preburning powdered material of step b preparation is mixed compound combination doping composition in proportion, add 1.1 times of parts by weight of deionized water of major ingredient, 2 times of weight part steel balls of major ingredient, place and carry out ball milling in the ball mill cylinder of steel, the ball milling linear velocity is not less than 350m/min, the ball milling time is not less than 12h, makes the ball milling powder particles be distributed as 0.1～0.2 μ m, and volumetric concentration is greater than 80%, become single spinel phase pollution-free, no dephasign, oven dry was pulverized behind 40 mesh sieves standby;
D), preparation magnetic core green compact
Ferrite powder with step c preparation mixes binding agent in 10～20% ratios and carries out granulation, and binding agent is the polyvinyl alcohol water solution of 6～15% concentration; The pressure that adopts 300～600MPa is pressed into the magnetic core green compact of desired shape with the granulation material, and the density that makes described magnetic core green compact is 3.2～3.7g/cm
3
E), low temperature high density sintering magnetic core
With the magnetic core green compact of steps d preparation, with more than 850～1050 ℃ of sintering 4h, the relative density of sintered blank is greater than 93% in nitrogen/oxygen gas mixture atmosphere, and actual density is not less than 5.0g/cm
3, promptly get high-frequency high-power Ni-Zn base magnetic ferrite material.
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