CN1587192A - Anti-interference magnesium-zinc ferrite and producing method - Google Patents

Anti-interference magnesium-zinc ferrite and producing method Download PDF

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Publication number
CN1587192A
CN1587192A CN 200410053529 CN200410053529A CN1587192A CN 1587192 A CN1587192 A CN 1587192A CN 200410053529 CN200410053529 CN 200410053529 CN 200410053529 A CN200410053529 A CN 200410053529A CN 1587192 A CN1587192 A CN 1587192A
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magnetic core
ferrite
oxide
sample
interference magnetic
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CN100353468C (en
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秦会斌
周继军
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QNI HUIBIN
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QNI HUIBIN
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Abstract

The anti-interference magnesium-zinc ferrite is produced with MgO, ZnO and Fe2O3 in certain proportion as main material, and through mixing, calcining at 1000-1200 deg.c for 30-90 min, adding supplementary material, crushing, mixing, adding adhesive, spray pelletizing to obtain grains of 180 micron average size, pressing to form magnetic core, sintering at 1250-1350 deg.c for 2-5 hr and cooling. The present invention has simple production process, and the produced magnesium-zinc ferrite has high initial magnetic permeability, high resistivity, excellent magnetic curve characteristic, low cost, wide application range and good use effect.

Description

Anti-Interference Magnesium Zinc Ferrite and Manufacturing Approach
Technical field
The present invention relates to anti-interference magnetic core ferrite of a kind of magnesium zinc (MgZn) and manufacture method, have at its 5MHz～25MHz and be higher than 100 initial permeability, resistivity coefficient can be up to 10 7～10 8More than (ohmcm), and excellent magnetic spectrum character of curve is arranged, be mainly used in anti-interference magnetic core Ferrite Material.
Background technology
When traditional MnZn (MnZn) based ferrite was used as anti-interference magnetic core ferrite (anti-EMI) material, the ferritic electricalresistivity of MnZn was generally 10 1～10 3Between (ohmcm), because resistivity is lower, eddy-current loss was big when the MnZn ferrite used at high frequency, and magnetic permeability quickly falls to 1, makes the MnZn ferrite not have effect substantially when high frequency uses, and can only be used in the low frequency frequency range.In fact to can be used for the scope of anti-EMI device very little for the MnZn ferrite, and what use at present is the NiZn Ferrite Material basically.
Practicality substantially all is the anti-interference core material of Ni-Zn series ferrite in the present world wide, and its main component is NiO, Fe in this class ferrite 2O 3, ZnO.Used raw material NiO (content is 5～10mol%, by NiO) costs an arm and a leg, and is general more than 80,000 yuan/ton.
The anti-EMI Ferrite Material that uses relates to following problem at present:
1, anti-EMI ferrite material therefor performance mainly is the performance of the magnetic spectrum curve of material.Say for concrete should being used for, because the spectrum of the electromagnetic interference in electronics and the electrical equipment is wider, general magnitude from tens KHz to GHz, scope commonly used is 9KHz～30MHz.
When 2, anti-EMI ferrite used as anti-EMI magnetic core etc., the initial permeability of material did not also require too highly, and importantly magnetic permeability is along with the variation relation of frequency, i.e. the magnetic spectrum curvilinear characteristic.Require the magnetic spectrum curve along with the increase of frequency do not reduce too fast, remain on the needed scope of device.
3, for the MnZn Ferrite Material, because its resistivity is lower, generally at ρ=10～1000 (ohmcm), frequency of utilization is below 0.1MHz.When using as anti-EMI material, its range of application is too little, can't satisfy a large amount of needs to 30MHz.
4, for the NiZn Ferrite Material, because its resistivity height, generally in ρ=10 4～10 5(ohmcm), frequency of utilization can reach more than the 20MHz.When using as anti-EMI material, its range of application of NiZn Ferrite Material of some prescription can reach the needs of 30MHz.But its deadly defect is the cost height, has in the used raw material) and expensive NiO (3～6mol%), general more than 80,000 yuan/ton.
Summary of the invention
The objective of the invention is to overcome the deficiency of above-mentioned existence, and provide a kind of anti-interference magnetic core ferrite and manufacture method of cheapness, this MgZn based ferrite can replace the nickel Zinc material aspect anti-EMI on performance, and its result of use and quality product can reach the requirement of desired product to material property.On cost, the used raw-material price of MgO of MgZn ferrite material only is NiO 3 percent five below 0.25 ten thousand yuan/ton, makes material have good market outlook.
The MgZn that the present invention relates to is anti-EMI ferrite, has 300～3000 initial permeability, high resistivity coefficient, and resistivity coefficient can reach 10 7～10 8More than (ohmcm), frequency of utilization reaches more than the 30MHz, reaches the requirement of the anti-EMI conduction test of present electronics and electric installation standard fully.
Ferrite Material of the present invention mainly includes by magnesia, zinc oxide, three kinds of main components of iron oxide, wherein also can add one or more accessory ingredients that have in silica, calcium oxide, the nickel oxide, the magnesia that in main component, contains respectively 8～27mol% (pressing MgO calculates), the zinc oxide of 7～27mol% (pressing ZnO calculates), 30～36.7mol% (presses Fe 2O 3Calculating) iron oxide; And the compositing range in accessory ingredient comprises: 0～4mol% (presses MnCO 3Calculating) nickel oxide, the 0～4mol% of manganese carbonate, 0～4mol% (pressing NiO calculates) (press CuCO 3Calculating) copper carbonate.
In the above-mentioned Ferrite Material, also add one or more following adding ingredient: CaCO with specific scope 3, CoO, Al 2O 3, TiO 2, SiO 2, B 2O 3, P 2O 5, As 2O 5, Pb 3O 4, the amount of each composition all is not higher than 2.0mol%, and other is limited in below the 1000ppm such as P, S, Cl impurity.
In the above-mentioned Ferrite Material, can also specific scope add one or more following added ingredientss:
Nb2O 5: below the 0.2mol%; Ta 2O 5: below the 0.2mol%; V 2O 5: below the 0.2mol%; ZrO 2: below the 0.2mol%; Bi 2O 3: below the 0.2mol%; MoO 3: below the 0.2mol%.
In the above-mentioned ferrite, the median size of its sintered compact is 1～25 μ m.
Above-mentioned ferrite, wherein saturated magnetic is 300mT or bigger with density Bs (25 ℃); Saturated magnetic is 80m/A or littler with density Hc (25 ℃); Initial susceptibility (25 ℃) is 200 or bigger; Curie temperature is 120 ℃ or bigger; Resistivity coefficient can reach 10 7～10 8(ohmcm), perhaps higher.
The ferritic manufacture method of a kind of anti-interference magnetic core, it is that magnesium oxide, zinc oxide, three kinds of main components of ferric oxide are prepared burden, and is mixed in proportion, and the mixture that mixes was calcined 30-90 minute down at 1000～1200 ℃.Add secondary component materials and additive then in proportion, after pulverize mixing, adding that tackiness agent mixes and adopt the mist projection granulating method to obtain average particulate diameter is 180 microns particle, with the particle compression moulding that granulation obtains, obtains needed magnetic core sample; Progressively be warmed up to 1250～1350 ℃, and under the temperature that sets heat preservation sintering 2～5 hours, obtain the sample of being fired after the cooling.
The optimum calcinating temperature of mixture of the present invention is 1320 ℃, and calcination time is 2.5 hours.
The present invention obtains anti-EMI magnetic core sample or anti-EMI wire sample or anti-EMI magnetosphere sample with the particle compression moulding that granulation obtains.
The present invention adopts ferrite sintering process to prepare material or element, control coercivity, saturated magnetization, magnetic conductivity and the magnetic spectrum characteristic thereof etc. of material by the control of main component, be controlled in the sintering process grain morphology and the influential attachment component of structure such as SiO 2, CaO etc. within the limits prescribed, and realize the scope that average crystal grain is being set by the control sintering.
Characteristics such as the present invention compared with prior art has the anti-interference magnetic core ferrite of preparation technology simple, prepared (MgZn) initial permeability, resistivity coefficient height, and excellent magnetic spectrum character of curve is arranged, and cheap, applied widely, and result of use is good.
Embodiment
Embodiment 1
Earlier to MgO, ZnO, Fe 2O 3Prepare burden for main component, get the magnesia of 27mol% (pressing MgO calculates), the zinc oxide of 13mol% (pressing ZnO calculates), 30mol% (presses Fe 2O 3Calculating) iron oxide mixes, and the mixture that mixes was calcined 90 minutes under 1000 ℃.And then adding additive: 50ppm (presses SiO 2Calculating) silica, 50ppm (pressing CaO calculates) is calcium oxide.After pulverizing mixing, adding that tackiness agent mixes and obtaining average grain with the mist projection granulating method directly is 180 microns particle, the particle compression moulding that granulation is obtained, obtain needed anti-EMI magnetic core sample, progressively be warmed up to 1350 ℃ again, and, obtain the sample of being fired after the cooling 1350 ℃ of following heat preservation sinterings 2 hours.The permeability measurement result of sample is (adopting ring-type sample, the employing Agilent4291 test of external diameter * internal diameter * height=14 * 7.8 * 10mm3):
The magnetic conductivity test result of table 1 embodiment 1
F (MHz) 5 10 25 50 100
μ ' 221 134 83 52 26
μ " 91 101 74 63 50
μ 239 168 111 82 56
Embodiment 2
Equally earlier to MgO, ZnO, Fe 2O 3Prepare burden for main component, get the magnesia of 18mol% (pressing MgO calculates), the zinc oxide of 16.7mol% (pressing ZnO calculates), 32.7mol% (presses Fe 2O 3Calculating) iron oxide mixes, and the mixture that mixes was calcined 60 minutes under 1050 ℃.And then the adding minor component, wherein minor component has nickel oxide, the 2.7mol% of 1mol% (pressing NiO calculates) (to press CuCO 3Calculating) copper carbonate, 2.7mol% (press MnCO 3Calculating) manganous carbonate.Wherein additive has 1mol% (to press SiO 2Calculating) silica, the calcium oxide of 0.6mol% (pressing CaO calculates), 0.3mol% (presses Al 2O 3Calculating) aluminium oxide.After pulverize mixing, adding that tackiness agent mixes and adopt the mist projection granulating method to obtain average grain directly is 180 microns particle, with the particle compression moulding that granulation obtains, obtains the needed ring specimen of parameter testing; Progressively be warmed up to 1320 ℃, and, obtain the sample of being fired after the cooling 1320 ℃ of following heat preservation sinterings 3 hours.The permeability measurement result of sample (adopts external diameter * internal diameter * height=16.3 * 12 * 8mm 3The ring-type sample, adopt the Agilent4291 test):
The magnetic conductivity test result of table 2 embodiment 2
F (MHz) 5 10 25 50 100
μ ' 269 155 92 58 28
μ " 192 153 100 79 58
μ 330 218 136 98 64
Embodiment 3
Sample is earlier to MgO, ZnO, Fe 2O 3Prepare burden for main component, get the magnesia of 8.3mol% (pressing MgO calculates), the zinc oxide of 13.3mol% (pressing ZnO calculates), 36.7mol% (presses Fe 2O 3Calculating) iron oxide mixes.And then the adding accessory ingredient, wherein accessory ingredient has nickel oxide, the 0.9mol% of 0.77mol% (pressing NiO calculates) (to press CuCO 3Calculating) copper carbonate, 3.3mol% (press MnCO 3Calculating) manganese carbonate mixes.The mixture that mixes was calcined 60 minutes down at 1100 ℃.After pulverize mixing, adding that tackiness agent mixes and adopt the mist projection granulating method to obtain average grain directly is 180 microns particle, with the particle compression moulding that granulation obtains, obtains the needed ring specimen of parameter testing; Progressively be warmed up to 1320 ℃, and, obtain the sample of being fired after the cooling 1320 ℃ of following heat preservation sinterings 2.5 hours.The permeability measurement result of sample (adopts external diameter * internal diameter * height=8.4 * 5 * 5mm 3The ring-type sample, adopt the Agilent4291 test):
The magnetic conductivity test result of table 3 embodiment 3
F (MHz) 5 10 25 50 100
μ ' 328 192 106 63 30
μ " 151 166 115 89 64
μ 361 254 156 109 71
Embodiment 4
Earlier to MgO, ZnO, Fe 2O 3Prepare burden for main component, get the magnesia of 19.3mol% (pressing MgO calculates), the zinc oxide of 7.0mol% (pressing ZnO calculates), 33.3mol% (presses Fe 2O 3Calculating) iron oxide mixes.And then the adding accessory ingredient, wherein accessory ingredient has 1mol% (to press CuCO 3Calculating) copper carbonate, 2.7mol% (press MnCO 3Calculating) manganese carbonate; Add again 1.7mol% and (press MnCO 3Calculating) SiO 2, CaO1.7mol% (presses MnCO 3Calculate), mix again.The mixture that mixes was calcined 60 minutes down at 1150 ℃.After pulverize mixing, adding that tackiness agent mixes and adopt the mist projection granulating method to obtain average grain directly is 180 microns particle, with the particle compression moulding that granulation obtains, obtains the needed ring specimen of parameter testing; Progressively be warmed up to 1300 ℃, and, obtain the sample of being fired after the cooling 1300 ℃ of following heat preservation sinterings 3.5 hours.The permeability measurement result of sample (adopts external diameter * internal diameter * height=20 * 10 * 10mm 3The ring-type sample, adopt the Agilent4291 test):
The magnetic conductivity test result of table 4 embodiment 4
F (MHz) 5 10 25 50 100
μ ' 278 159 87 51 23
μ " 129 140 96 75 54
μ 306 212 130 91 59
Embodiment 5
Equally earlier to MgO, ZnO, Fe 2O 3Prepare burden for main component, get the magnesia of 7.3mol% (pressing MgO calculates), the zinc oxide of 27mol% (pressing ZnO calculates), 32.8mol% (presses Fe 2O 3Calculating) iron oxide mixes, and the mixture that mixes was calcined 30 minutes under 1200 ℃.And then the adding minor component, wherein minor component has nickel oxide, the 4mol% of 4mol% (pressing NiO calculates) (to press CuCO 3Calculating) copper carbonate, 4mol% (press MnCO 3Calculating) manganous carbonate.Wherein additive has 0.3mol% (to press P 3O 4Calculating) lead oxide, the calcium oxide of 1mol% (pressing CaO calculates).After pulverize mixing, adding that tackiness agent mixes and adopt the mist projection granulating method to obtain average grain directly is 180 microns particle, with the particle compression moulding that granulation obtains, obtains the needed ring specimen of parameter testing; Progressively be warmed up to 1250 ℃, and, obtain the sample of being fired after the cooling 1250 ℃ of following heat preservation sinterings 5 hours.The permeability measurement result of sample (adopts external diameter * internal diameter * height=18 * 10 * 10mm 3The ring-type sample, adopt the Agilent4291 test):
The magnetic conductivity test result of table 5 embodiment 5
F (MHz) 5 10 25 50 100
μ ' 281 155 88 53 24
μ " 145 142 96 75 54
μ 316 210 130 92 59

Claims (9)

1, a kind of anti-interference magnetic core ferrite, it mainly includes by magnesia, zinc oxide, three kinds of main components of iron oxide, wherein also can add one or more accessory ingredients that have in silica, calcium oxide, the nickel oxide, the magnesia that in main component, contains respectively 8～27mol% (pressing MgO calculates), the zinc oxide of 7～27mol% (pressing ZnO calculates), 30～36.7mol% (presses Fe 2O 3Calculating) iron oxide; And the compositing range in accessory ingredient comprises: 0～4mol% (presses MnCO 3Calculating) nickel oxide, the 0～4mol% of manganese carbonate, 0～4mol% (pressing NiO calculates) (press CuCO 3Calculating) copper carbonate.
2, anti-interference magnetic core ferrite according to claim 1 is characterized in that in the above-mentioned Ferrite Material, also adds one or more following adding ingredient: CaCO with specific scope 3, CoO, Al 2O 3, TiO 2, SiO 2, B 2O 3, P 2O 5, As 2O 5, Pb 3O 4, the amount of each composition all is not higher than 2.0mol%, and other is limited in below the 1000ppm such as P, S, Cl impurity.
3, anti-interference magnetic core ferrite according to claim 1 and 2 is characterized in that in the above-mentioned Ferrite Material, also adds one or more following added ingredientss with specific scope:
Nb2O 5: below the 0.2mol%; Ta 2O 5: below the 0.2mol%; V 2O 5Below the 0.2mol%; ZrO 2: below the 0.2mol%; Bi 2O 3: below the 0.2mol%; MoO 3: below the 0.2mol%.
4, anti-interference magnetic core ferrite according to claim 1 and 2 is characterized in that in the above-mentioned ferrite, and the median size of its sintered compact is 1～25 μ m.
5, anti-interference magnetic core ferrite according to claim 3 is characterized in that in the above-mentioned ferrite, and the median size of its sintered compact is 1～25 μ m.
6, according to claim 4 or 5 described anti-interference magnetic core ferrites, it is characterized in that above-mentioned ferrite, wherein saturated magnetic is 300mT or bigger with density Bs (25 ℃); Saturated magnetic is 80m/A or littler with density Hc (25 ℃); Initial susceptibility (25 ℃) is 200 or bigger; Curie temperature is 120 ℃ or bigger; Resistivity coefficient can reach 10 7～10 8(ohmcm), perhaps higher.
7, a kind of as the ferritic manufacture method of anti-interference magnetic core as described in the claim 1～6, it is that magnesium oxide, zinc oxide, three kinds of main components of ferric oxide are prepared burden, be mixed in proportion, the mixture that mixes was calcined 30-90 minute down at 1000～1200 ℃.Add secondary component materials and additive then in proportion, after pulverize mixing, adding that tackiness agent mixes and adopt the mist projection granulating method to obtain average particulate diameter is 180 microns particle, with the particle compression moulding that granulation obtains, obtains needed magnetic core sample; Progressively be warmed up to 1250～1350 ℃, and under the temperature that sets heat preservation sintering 2～5 hours, obtain the sample of being fired after the cooling.
8, according to the ferritic manufacture method of the described anti-interference magnetic core of claim 7, the optimum calcinating temperature that it is characterized in that mixture is 1320 ℃, and calcination time is 2.5 hours.
9,, it is characterized in that particle compression moulding that granulation is obtained obtaining anti-EMI magnetic core sample or anti-EMI wire sample or anti-EMI magnetosphere sample according to right 7 or the ferritic manufacture method of 8 described anti-interference magnetic cores.
CNB2004100535296A 2004-08-05 2004-08-05 Anti-interference magnesium-zinc ferrite and producing method Expired - Fee Related CN100353468C (en)

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