CN103708815A - Manganese-zinc ferrite material with secondary peak temperature of 55DEG C, high Curie point and high magnetic conductivity, and preparation method thereof - Google Patents

Manganese-zinc ferrite material with secondary peak temperature of 55DEG C, high Curie point and high magnetic conductivity, and preparation method thereof Download PDF

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CN103708815A
CN103708815A CN201310673514.9A CN201310673514A CN103708815A CN 103708815 A CN103708815 A CN 103708815A CN 201310673514 A CN201310673514 A CN 201310673514A CN 103708815 A CN103708815 A CN 103708815A
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CN103708815B (en
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茅柳强
陆自强
刘九皋
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Tongxiang Yaorun Electronic Co ltd
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TONGXIANG YAORUN ELECTRIC CO Ltd
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Abstract

The invention relates to a manganese-zinc ferrite material with a secondary peak temperature of 55DEG C, a high Curie point and a high magnetic conductivity, and a preparation method thereof. The manganese-zinc ferrite material is prepared by using main materials and additives, the main materials are composed of 52.6-53.2mol% of Fe2O3, 30.1-31.3mol% of MnO and 16.1-17.5mol% of ZnO; and the additives are composed of CaCO3, V2O5, Nb2O5, ZrO2, Co3O4 and Li2CO3, the amount of CaCO3 accounts for 0.025wt% of the amount of the main materials, the amount of V2O5 accounts for 0.020wt% of the amount of the main materials, the amount of Nb2O5 accounts for 0.020wt% of the amount of the main materials, the amount of ZrO2 accounts for 0.020wt% of the amount of the main materials, the amount of Co3O4 accounts for 0.050wt% of the amount of the main materials, and the amount of Li2CO3 accounts for 0.030-0.100wt% of the amount of the main materials. The preparation method sequentially comprises the steps of mixing, pre-burning, crushing, granulating, compacting, and sintering to obtain the manganese-zinc ferrite material. The manganese-zinc ferrite material has a secondary peak temperature of 55DEG C, a high Curie point and a high magnetic conductivity.

Description

The high curie point High Initial Permeability MnZn Ferrite Materials at two 55 ℃, peaks and preparation method thereof
Technical field
The present invention relates to a kind of MnZn ferrite material and preparation method thereof, especially relate to the high curie point High Initial Permeability MnZn Ferrite Materials at 55 ℃, a kind of two peak and preparation method thereof, this MnZn ferrite material is mainly applicable in the electronic devices and components such as communication class, illumination class.
Background technology
The application of MnZn ferrite material is more and more extensive at present, some MnZn ferrite materials are disclosed at present, if open day is on 03 14th, 2012, publication number is in the Chinese patent of CN102376408A, a kind of wide-temperature manganese zinc ferrite is disclosed, the material of this wide-temperature manganese zinc ferrite comprises major ingredient and auxiliary material, wherein, and the MnO of the Fe2O3 that major ingredient is 53.5-56.3mol%, the ZnO of 21.2-25.1mol% and surplus; Auxiliary material is Nb 2o 5, CaO, TiO 2, SnO 2, MoO 3in 2 to 4 kinds; This wide-temperature manganese zinc ferrite magnetic permeability in-40 ℃ of-150 ℃ of temperature ranges changes very little, and while using under particular case, specific aim is not strong, is difficult to really realistic.And for example open day is on 06 09th, 2010, in the Chinese patent of publication number CN101728048A, discloses a kind of wide-temperature low-distortion mangan zinc ferrite and preparation method thereof, and this Mn-Zn ferrite principal constituent is with Fe 2o 3meter 52.0mol%～53.0mol% ferric oxide, in 21.0mol%～23.0mol% zinc oxide of ZnO, all the other are trimanganese tetroxides; Also comprise minor component: with its standard substance CaCO separately 3, SiO 2, V 2o 5, Co 2o 3the content of meter is respectively (wt%): CaCO 3: 0.03～0.04, SiO 2: 0.005～0.01, V 2o 5: 0.01～0.03, Co 2o 3: 0.03～0.1.The preparation of employing conventional ceramic technique, sintering under nitrogen kiln densification condition, this Mn-Zn ferrite has the feature of wide temperature low distortion, and while using under particular case, specific aim is not strong, is difficult to really realistic.
Also there is no now a kind of stable performance, magnetic permeability is high, can reduce eddy-current loss, improves solid state reaction speed, the high curie point High Initial Permeability MnZn Ferrite Materials at two 55 ℃, peaks and preparation method thereof.
Summary of the invention
The object of the invention is to overcome above shortcomings in prior art, and provide a kind of stable performance, magnetic permeability is high, can reduce eddy-current loss, improve solid state reaction speed, under low-temperature sintering condition, there is the high curie point High Initial Permeability MnZn Ferrite Materials and preparation method thereof at 55 ℃, two peak of high initial magnetic permeability and the low high band relative loss factor factor.
The present invention addresses the above problem adopted technical scheme: the feature of the high curie point High Initial Permeability MnZn Ferrite Materials that this two peak is 55 ℃ is: it is made by major ingredient and additive, and described major ingredient is by Fe 2o 3: 52.6-53.2mol%, MnO:30.1-31.3mol% and ZnO:16.1-17.5mol% form, and described additive is by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3form, wherein, CaCO 3consumption be major ingredient 0.025wt%, V 2o 5consumption be major ingredient 0.020wt%, Nb 2o 5consumption be major ingredient 0.020wt%, ZrO 2consumption be major ingredient 0.020wt%, Co 3o 4consumption be major ingredient 0.050wt%, Li 2cO 3the consumption 0.030wt%-0.100wt% that is major ingredient.Make thus raw material type of the present invention simple, proportioning science, calcium carbonate can increase resistivity, reduces eddy-current loss; Vanadium Pentoxide in FLAKES has katalysis, improves solid state reaction speed; Niobium Pentxoxide changes magnetic properties, improves initial permeability; Zirconium dioxide can be controlled grain-size, improves magnetic permeability; Cobalt oxide can regulate the temperature stability of magnetic permeability; Quilonum Retard improves ferrite performance, changes temperature profile.CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3acting in conjunction, produces synergistic effect, makes MnZn ferrite material have two peaks at 55 ℃, 0-200 ℃ of magnetic permeability temperature stability is good, the performance that Curie temperature is high, and the Curie temperature of this MnZn ferrite material is greater than 190 ℃, environment for use with strong points, performance is more reliable.
As preferably, major ingredient of the present invention is by the Fe of 52.9mol% 2o 3, the MnO of 30.7mol% and the ZnO of 16.4mol% form, Li 2cO 3the consumption 0.030wt% that is major ingredient.The proportioning that makes thus the additive in the present invention is science more, CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3acting in conjunction, produces synergistic effect, and the performance of the MnZn ferrite material making is more stable, and two peaks are at 55 ℃, and 0-200 ℃ of magnetic permeability temperature stability is good, and magnetic permeability reaches 4500, and Curie temperature is high, and Curie temperature is greater than 190 ℃.
A preparation method for the high curie point High Initial Permeability MnZn Ferrite Materials at two 55 ℃, peaks, its feature is: in turn include the following steps:
(1) mix: major ingredient is pressed after proportion ingredient, adopted wet-mixed to obtain major ingredient slurry, the mixing time of wet-mixed is 50-90 minute;
(2) pre-burning: be added in rotary kiln and carry out pre-burning after the spraying of major ingredient slurry is dry, obtain Preburning material, the temperature of pre-burning is 850-950 ℃, and the time of pre-burning is 60-90 minute;
(3) pulverize: after additive is added in Preburning material, carry out wet pulverization, obtain crushed material, the grinding time of wet pulverization is 90-150 minute, and the particle diameter of crushed material is 1-1.5 μ m;
(4) granulation: to adding 1.5% the PVA that is equivalent to crushed material weight in crushed material, adopt mist projection granulating, obtain particulate material;
(5) compacting: with powder former, particulate material is pressed into blank, the density of blank is 3.0 ± 0.2g/cm 3;
(6) sintering: blank is placed in to nitrogen kiln sintering, temperature rise rate is 1.25-3 ℃/min, at 1000 ℃, to sintering temperature, carrying out densification controls, control oxygen level lower than 0.5%, sintering temperature is controlled at 1320-1340 ℃, and holding-zone Control for Oxygen Content, at 4.5-5.5%, is incubated 3-5 hour, rate of temperature fall is controlled at 1.5-2.5 ℃/min, obtains MnZn ferrite material.
Sintering temperature in the preparation method of the high curie point High Initial Permeability MnZn Ferrite Materials that the present invention two peak is 55 ℃ is at 1320-1340 ℃, and the sintering temperature of the 1370-1400 of the material of relatively conventional initial magnetic permeability 5000 ℃, has reduced 50-60 ℃.Production technique of the present invention has low pre-burning and sintering temperature, effectively reduces the production energy consumption of product.
The present invention compared with prior art, have the following advantages and effect: reasonably the additive of major ingredient proportioning and optimization mixes, make the MnZn ferrite material stable performance making, two peaks are at 55 ℃, and 0-200 ℃ of magnetic permeability temperature stability is good, magnetic permeability reaches 4500, Curie temperature is high, and Curie temperature is greater than 190 ℃, environment for use with strong points, more professional, better reliability.
Process optimization in the present invention, the tiny homogeneous of microcosmic crystal grain, cavernous Mn-Zn ferrite under the condition of low-temperature sintering temperature, have been made, this Mn-Zn ferrite has higher initial magnetic permeability, concretely, the initial permeability μ i of the MnZn ferrite material that the present invention makes be 4500 ± 30%(10kHz, 0.25mT, 25 ℃ ± 3 ℃), its Curie temperature is greater than 190 ℃, two peak positions are in 55 ℃, temperature stability is good, and eddy-current loss is low.Particularly-40 ℃ to 45 ℃ have high magnetic permeability, can be good at improving signal transmission capabilities.The present invention adopts the production method of low temperature densification sintering to prepare MnZn ferrite material, stable processing technique, and excellent property, MnZn ferrite material can meet the service requirements of the electronic devices and components such as communication class, illumination class.
Embodiment
Below by embodiment, the present invention is described in further detail, and following examples are explanation of the invention and the present invention is not limited to following examples.
Embodiment 1.
In the present embodiment, the high curie point High Initial Permeability MnZn Ferrite Materials at 55 ℃, two peak is made by major ingredient and additive, and wherein, major ingredient is by the Fe of 52.3mol% 2o 3, the MnO of 30.2mol% and the ZnO of 17.5mol% form, additive is by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3form, wherein, CaCO 3consumption be major ingredient 0.025wt%, V 2o 5consumption be major ingredient 0.020wt%, Nb 2o 5consumption be major ingredient 0.020wt%, ZrO 2consumption be major ingredient 0.020wt%, Co 3o 4consumption be major ingredient 0.050wt%, Li 2cO 3the consumption 0.030wt% that is major ingredient.
In the present embodiment, the preparation method of the high curie point High Initial Permeability MnZn Ferrite Materials at 55 ℃, two peak in turn includes the following steps.
(1) mix: by the Fe of 52.3mol% 2o 3, after the MnO of 30.2mol% and the ZnO of 17.5mol% mix, add in skin grinder and mix, in mixing process, add the pure water of the 35wt% that is equivalent to major ingredient weight, adopt wet-mixed to obtain major ingredient slurry, the mixing time of wet-mixed is 50 minutes.
(2) pre-burning: be added in rotary kiln and carry out pre-burning after the spraying of major ingredient slurry is dry, obtain Preburning material, the temperature of pre-burning is 850-950 ℃, and the time of pre-burning is 60 minutes.
(3) pulverize: by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3after these additives are all added in Preburning material, carry out wet pulverization, obtain crushed material, the grinding time of wet pulverization is 120 minutes, the particle diameter of crushed material is 1-1.5 μ m, the pure water that adds the 35wt% that is equivalent to major ingredient weight in crushing process, and dispersion agent and defoamer some (being as the criterion to obtain setting particle size range), this is common practise to those skilled in the art.
(4) granulation: to adding 1.5% the PVA that is equivalent to crushed material weight in crushed material, adopt mist projection granulating, obtain particulate material.Generally, it is that the aqueous solution of 10wt% adds that PVA is mixed with to concentration, adds and is equivalent to the PVA aqueous solution that 15% concentration of crushed material weight is 10wt%.
(5) compacting: with powder former, particulate material is pressed into blank, blank be shaped as annular, the density of blank is 3.0 ± 0.2g/cm 3.
(6) sintering: blank is placed in to nitrogen kiln sintering, temperature rise rate is 1.25-3 ℃/min, at 1000 ℃, to sintering temperature, carrying out densification controls, control oxygen level lower than 0.5%, sintering temperature is controlled at 1320-1340 ℃, and holding-zone Control for Oxygen Content, at 4.5-5.5%, is incubated 3-5 hour, rate of temperature fall is controlled at 1.5-2.5 ℃/min, obtains MnZn ferrite material.
MnZn ferrite material in the present embodiment is toroidal cores goods, and these toroidal cores goods are of a size of Φ 22mm * Φ 14mm * h7mm.The magnetic core of preparing through said process, tests respectively normal temperature initial permeability μ i with instruments such as HP4284ALCR tester, high cryostats, Curie temperature, and μ i-T curve, obtaining μ i is that 5100,0 ℃ to 200 ℃ magnetic permeability temperature stabilities are better; Curie temperature is higher, is greater than 170 ℃; Two peak positions are in 60 ℃.
Embodiment 2.
In the present embodiment, the high curie point High Initial Permeability MnZn Ferrite Materials at 55 ℃, two peak is made by major ingredient and additive, and wherein, major ingredient is by the Fe of 52.8mol% 2o 3, the MnO of 30.5mol% and the ZnO of 16.7mol% form, additive is by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3form, wherein, CaCO 3consumption be major ingredient 0.025wt%, V 2o 5consumption be major ingredient 0.020wt%, Nb 2o 5consumption be major ingredient 0.020wt%, ZrO 2consumption be major ingredient 0.020wt%, Co 3o 4consumption be major ingredient 0.050wt%, Li 2cO 3the consumption 0.100wt% that is major ingredient.
In the present embodiment, the preparation method of the high curie point High Initial Permeability MnZn Ferrite Materials at 55 ℃, two peak in turn includes the following steps.
(1) mix: by the Fe of 52.8mol% 2o 3, after the MnO of 30.5mol% and the ZnO of 16.7mol% mix, add in skin grinder and mix, in mixing process, add the pure water of the 35wt% that is equivalent to major ingredient weight, adopt wet-mixed to obtain major ingredient slurry, the mixing time of wet-mixed is 50 minutes.
(2) pre-burning: be added in rotary kiln and carry out pre-burning after the spraying of major ingredient slurry is dry, obtain Preburning material, the temperature of pre-burning is 850-950 ℃, and the time of pre-burning is 60 minutes.
(3) pulverize: by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3after these additives are all added in Preburning material, carry out wet pulverization, obtain crushed material, the grinding time of wet pulverization is 120 minutes, the particle diameter of crushed material is 1-1.5 μ m, the pure water that adds the 35wt% that is equivalent to major ingredient weight in crushing process, and dispersion agent and defoamer some (being as the criterion to obtain setting particle size range), this is common practise to those skilled in the art.
(4) granulation: to adding 1.5% the PVA that is equivalent to crushed material weight in crushed material, adopt mist projection granulating, obtain particulate material.Generally, it is that the aqueous solution of 10wt% adds that PVA is mixed with to concentration, adds and is equivalent to the PVA aqueous solution that 15% concentration of crushed material weight is 10wt%.
(5) compacting: with powder former, particulate material is pressed into blank, blank be shaped as annular, the density of blank is 3.0 ± 0.2g/cm 3.
(6) sintering: blank is placed in to nitrogen kiln sintering, temperature rise rate is 1.25-3 ℃/min, at 1000 ℃, to sintering temperature, carrying out densification controls, control oxygen level lower than 0.5%, sintering temperature is controlled at 1320-1340 ℃, and holding-zone Control for Oxygen Content, at 4.5-5.5%, is incubated 3-5 hour, rate of temperature fall is controlled at 1.5-2.5 ℃/min, obtains MnZn ferrite material.
MnZn ferrite material in the present embodiment is toroidal cores goods, and these toroidal cores goods are of a size of Φ 22mm * Φ 14mm * h7mm.The magnetic core of preparing through said process, tests respectively normal temperature initial permeability μ i with instruments such as HP4284ALCR tester, high cryostats, Curie temperature, and μ i-T curve, obtaining μ i is that 4600,0 ℃ to 200 ℃ magnetic permeability temperature stabilities are better; Curie temperature is higher, is greater than 180 ℃; Two peak positions are in 40 ℃.
Embodiment 3.
In the present embodiment, the high curie point High Initial Permeability MnZn Ferrite Materials at 55 ℃, two peak is made by major ingredient and additive, and wherein, major ingredient is by the Fe of 53.5mol% 2o 3, the MnO of 31.2mol% and the ZnO of 15.3mol% form, additive is by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3form, wherein, CaCO 3consumption be major ingredient 0.025wt%, V 2o 5consumption be major ingredient 0.020wt%, Nb 2o 5consumption be major ingredient 0.020wt%, ZrO 2consumption be major ingredient 0.020wt%, Co 3o 4consumption be major ingredient 0.050wt%, Li 2cO 3the consumption 0.030wt% that is major ingredient.
In the present embodiment, the preparation method of the high curie point High Initial Permeability MnZn Ferrite Materials at 55 ℃, two peak in turn includes the following steps.
(1) mix: by the Fe of 53.5mol% 2o 3, after the MnO of 31.2mol% and the ZnO of 15.3mol% mix, add in skin grinder and mix, in mixing process, add the pure water of the 35wt% that is equivalent to major ingredient weight, adopt wet-mixed to obtain major ingredient slurry, the mixing time of wet-mixed is 50 minutes.
(2) pre-burning: be added in rotary kiln and carry out pre-burning after the spraying of major ingredient slurry is dry, obtain Preburning material, the temperature of pre-burning is 850-950 ℃, and the time of pre-burning is 60 minutes.
(3) pulverize: by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3after these additives are all added in Preburning material, carry out wet pulverization, obtain crushed material, the grinding time of wet pulverization is 120 minutes, the particle diameter of crushed material is 1-1.5 μ m, the pure water that adds the 35wt% that is equivalent to major ingredient weight in crushing process, and dispersion agent and defoamer some (being as the criterion to obtain setting particle size range), this is common practise to those skilled in the art.
(4) granulation: to adding 1.5% the PVA that is equivalent to crushed material weight in crushed material, adopt mist projection granulating, obtain particulate material.Generally, it is that the aqueous solution of 10wt% adds that PVA is mixed with to concentration, adds and is equivalent to the PVA aqueous solution that 15% concentration of crushed material weight is 10wt%.
(5) compacting: with powder former, particulate material is pressed into blank, blank be shaped as annular, the density of blank is 3.0 ± 0.2g/cm 3.
(6) sintering: blank is placed in to nitrogen kiln sintering, temperature rise rate is 1.25-3 ℃/min, at 1000 ℃, to sintering temperature, carrying out densification controls, control oxygen level lower than 0.5%, sintering temperature is controlled at 1320-1340 ℃, and holding-zone Control for Oxygen Content, at 4.5-5.5%, is incubated 3-5 hour, rate of temperature fall is controlled at 1.5-2.5 ℃/min, obtains MnZn ferrite material.
MnZn ferrite material in the present embodiment is toroidal cores goods, and these toroidal cores goods are of a size of Φ 22mm * Φ 14mm * h7mm.The magnetic core of preparing through said process, tests respectively normal temperature initial permeability μ i with instruments such as HP4284ALCR tester, high cryostats, Curie temperature, and μ i-T curve, obtaining μ i is that 4000,0 ℃ to 200 ℃ magnetic permeability temperature stabilities are better; Curie temperature is higher, is greater than 200 ℃; Two peak positions are in 25 ℃.
Embodiment 4.
In the present embodiment, the high curie point High Initial Permeability MnZn Ferrite Materials at 55 ℃, two peak is made by major ingredient and additive, and wherein, major ingredient is by the Fe of 52.9mol% 2o 3, the MnO of 30.7mol% and the ZnO of 16.4mol% form, additive is by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3form, wherein, CaCO 3consumption be major ingredient 0.025wt%, V 2o 5consumption be major ingredient 0.020wt%, Nb 2o 5consumption be major ingredient 0.020wt%, ZrO 2consumption be major ingredient 0.020wt%, Co 3o 4consumption be major ingredient 0.050wt%, Li 2cO 3the consumption 0.030wt% that is major ingredient.
In the present embodiment, the preparation method of the high curie point High Initial Permeability MnZn Ferrite Materials at 55 ℃, two peak in turn includes the following steps.
(1) mix: by the Fe of 52.9mol% 2o 3, after the MnO of 30.7mol% and the ZnO of 16.4mol% mix, add in skin grinder and mix, in mixing process, add the pure water of the 35wt% that is equivalent to major ingredient weight, adopt wet-mixed to obtain major ingredient slurry, the mixing time of wet-mixed is 50 minutes.
(2) pre-burning: be added in rotary kiln and carry out pre-burning after the spraying of major ingredient slurry is dry, obtain Preburning material, the temperature of pre-burning is 850-950 ℃, and the time of pre-burning is 60 minutes.
(3) pulverize: by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3after these additives are all added in Preburning material, carry out wet pulverization, obtain crushed material, the grinding time of wet pulverization is 120 minutes, the particle diameter of crushed material is 1-1.5 μ m, the pure water that adds the 35wt% that is equivalent to major ingredient weight in crushing process, and dispersion agent and defoamer some (being as the criterion to obtain setting particle size range), this is common practise to those skilled in the art.
(4) granulation: to adding 1.5% the PVA that is equivalent to crushed material weight in crushed material, adopt mist projection granulating, obtain particulate material.Generally, it is that the aqueous solution of 10wt% adds that PVA is mixed with to concentration, adds and is equivalent to the PVA aqueous solution that 15% concentration of crushed material weight is 10wt%.
(5) compacting: with powder former, particulate material is pressed into blank, blank be shaped as annular, the density of blank is 3.0 ± 0.2g/cm 3.
(6) sintering: blank is placed in to nitrogen kiln sintering, temperature rise rate is 1.25-3 ℃/min, at 1000 ℃, to sintering temperature, carrying out densification controls, control oxygen level lower than 0.5%, sintering temperature is controlled at 1320-1340 ℃, and holding-zone Control for Oxygen Content, at 4.5-5.5%, is incubated 3-5 hour, rate of temperature fall is controlled at 1.5-2.5 ℃/min, obtains MnZn ferrite material.
MnZn ferrite material in the present embodiment is toroidal cores goods, and these toroidal cores goods are of a size of Φ 22mm * Φ 14mm * h7mm.The magnetic core of preparing through said process, tests respectively normal temperature initial permeability μ i with instruments such as HP4284ALCR tester, high cryostats, Curie temperature, and μ i-T curve, obtaining μ i is that 4500,0 ℃ to 200 ℃ magnetic permeability temperature stabilities are better; Curie temperature is higher, is greater than 190 ℃; Two peak positions are in 55 ℃.
Embodiment 5.
In the present embodiment, the high curie point High Initial Permeability MnZn Ferrite Materials at 55 ℃, two peak is made by major ingredient and additive, and wherein, major ingredient is by the Fe of 52.9mol% 2o 3, the MnO of 30.7mol% and the ZnO of 16.4mol% form, additive is by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3form, wherein, CaCO 3consumption be major ingredient 0.025wt%, V 2o 5consumption be major ingredient 0.020wt%, Nb 2o 5consumption be major ingredient 0.020wt%, ZrO 2consumption be major ingredient 0.020wt%, Co 3o 4consumption be major ingredient 0.050wt%, Li 2cO 3the consumption 0.050wt% that is major ingredient.
In the present embodiment, the preparation method of the high curie point High Initial Permeability MnZn Ferrite Materials at 55 ℃, two peak in turn includes the following steps.
(1) mix: by the Fe of 52.9mol% 2o 3, after the MnO of 30.7mol% and the ZnO of 16.4mol% mix, add in skin grinder and mix, in mixing process, add the pure water of the 35wt% that is equivalent to major ingredient weight, adopt wet-mixed to obtain major ingredient slurry, the mixing time of wet-mixed is 50 minutes.
(2) pre-burning: be added in rotary kiln and carry out pre-burning after the spraying of major ingredient slurry is dry, obtain Preburning material, the temperature of pre-burning is 850-950 ℃, and the time of pre-burning is 60 minutes.
(3) pulverize: by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3after these additives are all added in Preburning material, carry out wet pulverization, obtain crushed material, the grinding time of wet pulverization is 120 minutes, the particle diameter of crushed material is 1-1.5 μ m, the pure water that adds the 35wt% that is equivalent to major ingredient weight in crushing process, and dispersion agent and defoamer some (being as the criterion to obtain setting particle size range), this is common practise to those skilled in the art.
(4) granulation: to adding 1.5% the PVA that is equivalent to crushed material weight in crushed material, adopt mist projection granulating, obtain particulate material.Generally, it is that the aqueous solution of 10wt% adds that PVA is mixed with to concentration, adds and is equivalent to the PVA aqueous solution that 15% concentration of crushed material weight is 10wt%.
(5) compacting: with powder former, particulate material is pressed into blank, blank be shaped as annular, the density of blank is 3.0 ± 0.2g/cm 3.
(6) sintering: blank is placed in to nitrogen kiln sintering, temperature rise rate is 1.25-3 ℃/min, at 1000 ℃, to sintering temperature, carrying out densification controls, control oxygen level lower than 0.5%, sintering temperature is controlled at 1320-1340 ℃, and holding-zone Control for Oxygen Content, at 4.5-5.5%, is incubated 3-5 hour, rate of temperature fall is controlled at 1.5-2.5 ℃/min, obtains MnZn ferrite material.
MnZn ferrite material in the present embodiment is toroidal cores goods, and these toroidal cores goods are of a size of Φ 22mm * Φ 14mm * h7mm.The magnetic core of preparing through said process, tests respectively normal temperature initial permeability μ i with instruments such as HP4284ALCR tester, high cryostats, Curie temperature, and μ i-T curve, obtaining μ i is that 4500,0 ℃ to 200 ℃ magnetic permeability temperature stabilities are better; Curie temperature is higher, is greater than 180 ℃; Two peak positions are in 70 ℃.
Embodiment 6.
In the present embodiment, the high curie point High Initial Permeability MnZn Ferrite Materials at 55 ℃, two peak is made by major ingredient and additive, and wherein, major ingredient is by the Fe of 52.9mol% 2o 3, the MnO of 30.7mol% and the ZnO of 16.4mol% form, additive is by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3form, wherein, CaCO 3consumption be major ingredient 0.025wt%, V 2o 5consumption be major ingredient 0.020wt%, Nb 2o 5consumption be major ingredient 0.020wt%, ZrO 2consumption be major ingredient 0.020wt%, Co 3o 4consumption be major ingredient 0.050wt%, Li 2cO 3the consumption 0.100wt% that is major ingredient.Major ingredient in the present invention can be by Fe 2o 3: 52.6-53.2mol%, MnO:30.1-31.3mol% and ZnO:16.1-17.5mol% form, Li 2cO 3consumption can be the 0.030wt%-0.100wt% of major ingredient.
In the present embodiment, the preparation method of the high curie point High Initial Permeability MnZn Ferrite Materials at 55 ℃, two peak in turn includes the following steps.
(1) mix: by the Fe of 52.9mol% 2o 3, after the MnO of 30.7mol% and the ZnO of 16.4mol% mix, add in skin grinder and mix, in mixing process, add the pure water of the 35wt% that is equivalent to major ingredient weight, adopt wet-mixed to obtain major ingredient slurry, the mixing time of wet-mixed is 50 minutes.
(2) pre-burning: be added in rotary kiln and carry out pre-burning after the spraying of major ingredient slurry is dry, obtain Preburning material, the temperature of pre-burning is 850-950 ℃, and the time of pre-burning is 60 minutes.
(3) pulverize: by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3after these additives are all added in Preburning material, carry out wet pulverization, obtain crushed material, the grinding time of wet pulverization is 120 minutes, the particle diameter of crushed material is 1-1.5 μ m, the pure water that adds the 35wt% that is equivalent to major ingredient weight in crushing process, and dispersion agent and defoamer some (being as the criterion to obtain setting particle size range), this is common practise to those skilled in the art.
(4) granulation: to adding 1.5% the PVA that is equivalent to crushed material weight in crushed material, adopt mist projection granulating, obtain particulate material.Generally, it is that the aqueous solution of 10wt% adds that PVA is mixed with to concentration, adds and is equivalent to the PVA aqueous solution that 15% concentration of crushed material weight is 10wt%.
(5) compacting: with powder former, particulate material is pressed into blank, blank be shaped as annular, the density of blank is 3.0 ± 0.2g/cm 3.
(6) sintering: blank is placed in to nitrogen kiln sintering, temperature rise rate is 1.25-3 ℃/min, at 1000 ℃, to sintering temperature, carrying out densification controls, control oxygen level lower than 0.5%, sintering temperature is controlled at 1320-1340 ℃, and holding-zone Control for Oxygen Content, at 4.5-5.5%, is incubated 3-5 hour, rate of temperature fall is controlled at 1.5-2.5 ℃/min, obtains MnZn ferrite material.
MnZn ferrite material in the present embodiment is toroidal cores goods, and these toroidal cores goods are of a size of Φ 22mm * Φ 14mm * h7mm.The magnetic core of preparing through said process, tests respectively normal temperature initial permeability μ i with instruments such as HP4284ALCR tester, high cryostats, Curie temperature, and μ i-T curve, obtaining μ i is that 4400,0 ℃ to 200 ℃ magnetic permeability temperature stabilities are better; Curie temperature is higher, is greater than 170 ℃; Two peak positions are in 100 ℃.
Embodiment 7.
The high curie point High Initial Permeability MnZn Ferrite Materials that two peak in the present embodiment is 55 ℃ is made by major ingredient and additive, and major ingredient is by the Fe of 52.6mol% 2o 3, the MnO of 30.1mol% and the ZnO of 17.3mol% form, additive is by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3form, wherein, CaCO 3consumption be major ingredient 0.025wt%, V 2o 5consumption be major ingredient 0.020wt%, Nb 2o 5consumption be major ingredient 0.020wt%, ZrO 2consumption be major ingredient 0.020wt%, Co 3o 4consumption be major ingredient 0.050wt%, Li 2cO 3the consumption 0.070wt% that is major ingredient.
In the present embodiment, the preparation method of the high curie point High Initial Permeability MnZn Ferrite Materials at 55 ℃, two peak in turn includes the following steps.
(1) mix: major ingredient is pressed after proportion ingredient, adopted wet-mixed to obtain major ingredient slurry, the mixing time of wet-mixed is 50-90 minute.
(2) pre-burning: be added in rotary kiln and carry out pre-burning after the spraying of major ingredient slurry is dry, obtain Preburning material, the temperature of pre-burning is 850-950 ℃, and the time of pre-burning is 60-90 minute.
(3) pulverize: after additive is added in Preburning material, carry out wet pulverization, obtain crushed material, the grinding time of wet pulverization is 90-150 minute, and the particle diameter of crushed material is 1-1.5 μ m.
(4) granulation: to adding 1.5% the PVA that is equivalent to crushed material weight in crushed material, adopt mist projection granulating, obtain particulate material.
(5) compacting: with powder former, particulate material is pressed into blank, the density of blank is 3.0 ± 0.2g/cm 3.
(6) sintering: blank is placed in to nitrogen kiln sintering, temperature rise rate is 1.25-3 ℃/min, at 1000 ℃, to sintering temperature, carrying out densification controls, control oxygen level lower than 0.5%, sintering temperature is controlled at 1320-1340 ℃, and holding-zone Control for Oxygen Content, at 4.5-5.5%, is incubated 3-5 hour, rate of temperature fall is controlled at 1.5-2.5 ℃/min, obtains MnZn ferrite material.
Embodiment 8.
The high curie point High Initial Permeability MnZn Ferrite Materials that two peak in the present embodiment is 55 ℃ is made by major ingredient and additive, and major ingredient is by the Fe of 53.2mol% 2o 3, the MnO of 30.7mol% and the ZnO of 16.1mol% form, additive is by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3form, wherein, CaCO 3consumption be major ingredient 0.025wt%, V 2o 5consumption be major ingredient 0.020wt%, Nb 2o 5consumption be major ingredient 0.020wt%, ZrO 2consumption be major ingredient 0.020wt%, Co 3o 4consumption be major ingredient 0.050wt%, Li 2cO 3the consumption 0.055wt% that is major ingredient.
In the present embodiment, the preparation method of the high curie point High Initial Permeability MnZn Ferrite Materials at 55 ℃, two peak in turn includes the following steps.
(1) mix: major ingredient is pressed after proportion ingredient, adopted wet-mixed to obtain major ingredient slurry, the mixing time of wet-mixed is 50-90 minute.
(2) pre-burning: be added in rotary kiln and carry out pre-burning after the spraying of major ingredient slurry is dry, obtain Preburning material, the temperature of pre-burning is 850-950 ℃, and the time of pre-burning is 60-90 minute.
(3) pulverize: after additive is added in Preburning material, carry out wet pulverization, obtain crushed material, the grinding time of wet pulverization is 90-150 minute, and the particle diameter of crushed material is 1-1.5 μ m.
(4) granulation: to adding 1.5% the PVA that is equivalent to crushed material weight in crushed material, adopt mist projection granulating, obtain particulate material.
(5) compacting: with powder former, particulate material is pressed into blank, the density of blank is 3.0 ± 0.2g/cm 3.
(6) sintering: blank is placed in to nitrogen kiln sintering, temperature rise rate is 1.25-3 ℃/min, at 1000 ℃, to sintering temperature, carrying out densification controls, control oxygen level lower than 0.5%, sintering temperature is controlled at 1320-1340 ℃, and holding-zone Control for Oxygen Content, at 4.5-5.5%, is incubated 3-5 hour, rate of temperature fall is controlled at 1.5-2.5 ℃/min, obtains MnZn ferrite material.
Embodiment 9.
The high curie point High Initial Permeability MnZn Ferrite Materials that two peak in the present embodiment is 55 ℃ is made by major ingredient and additive, and major ingredient is by the Fe of 52.6mol% 2o 3, the MnO of 31.3mol% and the ZnO of 16.1mol% form, additive is by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3form, wherein, CaCO 3consumption be major ingredient 0.025wt%, V 2o 5consumption be major ingredient 0.020wt%, Nb 2o 5consumption be major ingredient 0.020wt%, ZrO 2consumption be major ingredient 0.020wt%, Co 3o 4consumption be major ingredient 0.050wt%, Li 2cO 3the consumption 0.090wt% that is major ingredient.
In the present embodiment, the preparation method of the high curie point High Initial Permeability MnZn Ferrite Materials at 55 ℃, two peak in turn includes the following steps.
(1) mix: major ingredient is pressed after proportion ingredient, adopted wet-mixed to obtain major ingredient slurry, the mixing time of wet-mixed is 50-90 minute.
(2) pre-burning: be added in rotary kiln and carry out pre-burning after the spraying of major ingredient slurry is dry, obtain Preburning material, the temperature of pre-burning is 850-950 ℃, and the time of pre-burning is 60-90 minute.
(3) pulverize: after additive is added in Preburning material, carry out wet pulverization, obtain crushed material, the grinding time of wet pulverization is 90-150 minute, and the particle diameter of crushed material is 1-1.5 μ m.
(4) granulation: to adding 1.5% the PVA that is equivalent to crushed material weight in crushed material, adopt mist projection granulating, obtain particulate material.
(5) compacting: with powder former, particulate material is pressed into blank, the density of blank is 3.0 ± 0.2g/cm 3.
(6) sintering: blank is placed in to nitrogen kiln sintering, temperature rise rate is 1.25-3 ℃/min, at 1000 ℃, to sintering temperature, carrying out densification controls, control oxygen level lower than 0.5%, sintering temperature is controlled at 1320-1340 ℃, and holding-zone Control for Oxygen Content, at 4.5-5.5%, is incubated 3-5 hour, rate of temperature fall is controlled at 1.5-2.5 ℃/min, obtains MnZn ferrite material.
Although the present invention with embodiment openly as above; but it is not in order to limit protection scope of the present invention; any technician who is familiar with this technology, not departing from change and the retouching of doing in the spirit and scope of the present invention, all should belong to protection scope of the present invention.

Claims (3)

1.一种二峰55℃的高居里点高磁导率锰锌铁氧体材料，其特征在于：它由主料和添加剂制成，所述主料由Fe2O3：52.6-53.2mol%、MnO：30.1-31.3mol%和ZnO：16.1-17.5mol%组成，所述添加剂由CaCO3、V2O5、Nb2O5、ZrO2、Co3O4和Li2CO3组成，其中，CaCO3的用量为主料的0.025wt%，V2O5的用量为主料的0.020wt%，Nb2O5的用量为主料的0.020wt%，ZrO2的用量为主料的0.020wt%，Co3O4的用量为主料的0.050wt%，Li2CO3的用量为主料的0.030wt%-0.100wt%。 1. A manganese-zinc ferrite material with a high Curie point and high magnetic permeability with two peaks of 55°C, characterized in that it is made of main ingredients and additives, and the main ingredients are Fe 2 O 3 : 52.6-53.2mol %, MnO: 30.1-31.3mol% and ZnO: 16.1-17.5mol%, the additive is composed of CaCO 3 , V 2 O 5 , Nb 2 O 5 , ZrO 2 , Co 3 O 4 and Li 2 CO 3 , Wherein, the consumption of CaCO3 is 0.025wt% of the main material, the consumption of V2O5 is 0.020wt% of the main material, the consumption of Nb2O5 is 0.020wt% of the main material, and the consumption of ZrO2 is 0.020wt% of the main material. 0.020wt%, the amount of Co 3 O 4 is 0.050wt% of the main material, and the amount of Li 2 CO 3 is 0.030wt%-0.100wt% of the main material. 2.根据权利要求1所述的二峰55℃的高居里点高磁导率锰锌铁氧体材料，其特征在于：所述主料由52.9mol%的Fe2O3、30.7mol%的MnO和16.4mol%的ZnO组成，Li2CO3的用量为主料的0.030wt%。 2. The manganese-zinc ferrite material with high Curie point and high magnetic permeability with two peaks at 55°C according to claim 1, characterized in that: the main material is composed of 52.9mol% Fe 2 O 3 , 30.7mol% Fe 2 O 3 Composed of MnO and 16.4mol% ZnO, the amount of Li 2 CO 3 is 0.030wt% of the main material. 3.一种如权利要求1或2所述的二峰55℃的高居里点高磁导率锰锌铁氧体材料的制备方法，其特征在于：依次包括如下步骤： 3. A method for preparing a high Curie point high permeability MnZn ferrite material with two peaks of 55°C as claimed in claim 1 or 2, characterized in that: comprising the steps in turn: （1）混合：将主料按配比配料后，采用湿法混合得到主料浆，湿法混合的混合时间为50-90分钟； (1) Mixing: After the main ingredients are mixed according to the proportion, the main slurry is obtained by wet mixing, and the mixing time of wet mixing is 50-90 minutes; （2）预烧：将主料浆喷雾干燥后投加到回转窑中进行预烧，得到预烧料，预烧的温度为850-950℃，预烧的时间为60-90分钟； (2) Pre-burning: The main slurry is spray-dried and put into the rotary kiln for pre-burning to obtain pre-fired material. The pre-fired temperature is 850-950°C, and the pre-fired time is 60-90 minutes; （3）粉碎：将添加剂投加到预烧料中后，进行湿法粉碎，得到粉碎料，湿法粉碎的粉碎时间为90-150分钟，粉碎料的粒径为1-1.5μm； (3) Grinding: after adding the additives to the calcined material, wet grinding is carried out to obtain ground material. The grinding time of wet grinding is 90-150 minutes, and the particle size of the ground material is 1-1.5 μm; （4）造粒：向粉碎料中投加相当于粉碎料重量的1.5%的PVA，采用喷雾造粒，得到颗粒料； (4) Granulation: Add PVA equivalent to 1.5% of the weight of the crushed material to the crushed material, and use spray granulation to obtain granules; （5）压制：用粉末成型机将颗粒料压制成坯件，坯件的密度为3.0±0.2g/cm3； (5) Compression: use a powder molding machine to press the granular material into a blank, and the density of the blank is 3.0±0.2g/cm 3 ; （6）烧结：将坯件置于氮窑中烧结，升温速率为1.25-3℃/分钟，在1000℃到烧结温度实行致密化控制，控制氧含量低于0.5%，烧结温度控制在1320-1340℃，保温段氧含量控制在4.5-5.5%，保温3-5小时，降温速率控制在1.5-2.5℃/分钟，得到锰锌铁氧体材料。 (6) Sintering: The blank is sintered in a nitrogen kiln, the heating rate is 1.25-3°C/min, the densification control is carried out at 1000°C to the sintering temperature, the oxygen content is controlled below 0.5%, and the sintering temperature is controlled at 1320- 1340°C, the oxygen content in the heat preservation section is controlled at 4.5-5.5%, the heat preservation period is 3-5 hours, and the cooling rate is controlled at 1.5-2.5°C/min to obtain manganese-zinc ferrite materials.
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CN107089828A (en) * 2017-03-21 2017-08-25 横店集团东磁股份有限公司 A kind of broad temperature, broadband is low than manganese zinc material with high magnetic permeability of magnetic conductivity temperature coefficient and preparation method thereof
CN107324793A (en) * 2017-06-26 2017-11-07 重庆正峰电子有限公司 The preparation method of the high excellent DC superposition characteristic manganese-zinc ferrites of μ i in wide temperature
CN111138182A (en) * 2019-12-31 2020-05-12 天长市中德电子有限公司 Method for preparing manganese-zinc ferrite with high magnetic conductivity

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CN102682946A (en) * 2012-05-30 2012-09-19 江门安磁电子有限公司 MnZn ferrite magnetic core with double characteristics and manufacture method

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CN102682946A (en) * 2012-05-30 2012-09-19 江门安磁电子有限公司 MnZn ferrite magnetic core with double characteristics and manufacture method

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CN107089828A (en) * 2017-03-21 2017-08-25 横店集团东磁股份有限公司 A kind of broad temperature, broadband is low than manganese zinc material with high magnetic permeability of magnetic conductivity temperature coefficient and preparation method thereof
CN107089828B (en) * 2017-03-21 2019-12-17 横店集团东磁股份有限公司 Manganese-zinc high-permeability material with wide temperature, wide frequency, low specific permeability and temperature coefficient and preparation method thereof
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CN111138182A (en) * 2019-12-31 2020-05-12 天长市中德电子有限公司 Method for preparing manganese-zinc ferrite with high magnetic conductivity

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