CN103708815B - The high curie point High Initial Permeability MnZn Ferrite Materials at two 55 DEG C, peaks and preparation method thereof - Google Patents

The high curie point High Initial Permeability MnZn Ferrite Materials at two 55 DEG C, peaks and preparation method thereof Download PDF

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CN103708815B
CN103708815B CN201310673514.9A CN201310673514A CN103708815B CN 103708815 B CN103708815 B CN 103708815B CN 201310673514 A CN201310673514 A CN 201310673514A CN 103708815 B CN103708815 B CN 103708815B
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CN103708815A (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 present invention relates to the high curie point High Initial Permeability MnZn Ferrite Materials at a kind of 55 DEG C, two peak and preparation method thereof.MnZn ferrite material of the present invention is made up of major ingredient and additive, and major ingredient is by Fe 2o 3: 52.6-53.2mol%, MnO:30.1-31.3mol% and ZnO:16.1-17.5mol% form, and additive is respectively the CaCO of 0.025wt%, 0.020wt%, 0.020wt%, 0.020wt%, 0.050wt% and 0.030wt%-0.100wt% of major ingredient by consumption 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3composition.Preparation method of the present invention in turn includes the following steps: mixing, pre-burning, pulverizing, granulation, compacting and sintering.55 DEG C, two peak of MnZn ferrite material of the present invention, high curie point, high magnetic permeability.

Description

The high curie point High Initial Permeability MnZn Ferrite Materials at two 55 DEG C, 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 a kind of 55 DEG C, 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 current MnZn ferrite material is more and more extensive, some MnZn ferrite materials are disclosed at present, if publication date is on 03 14th, 2012, publication number is in the Chinese patent of CN102376408A, disclose a kind of wide-temperature manganese zinc ferrite, the material of this wide-temperature manganese zinc ferrite comprises major ingredient and auxiliary material, and wherein, major ingredient is the ZnO of Fe2O3,21.2-25.1mol% of 53.5-56.3mol% and the MnO of surplus; Auxiliary material is Nb 2o 5, CaO, TiO 2, SnO 2, MoO 3in 2 to 4 kinds; The magnetic permeability change in-40 DEG C of-150 DEG C of temperature ranges of this wide-temperature manganese zinc ferrite is very little, and when using in particular situations, specific aim is not strong, is difficult to really realistic.And for example publication date 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.Prepared by employing conventional ceramic technique, sinter under nitrogen kiln densified conditions, this Mn-Zn ferrite has the feature of wide temperature low distortion, and when using in particular situations, specific aim is not strong, is difficult to really realistic.
Also do not have a kind of stable performance now, 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 DEG C, peaks and preparation method thereof.
Summary of the invention
The object of the invention is to overcome above shortcomings in prior art, and a kind of stable performance is provided, magnetic permeability is high, eddy-current loss can be reduced, improve solid state reaction speed, there is the high curie point High Initial Permeability MnZn Ferrite Materials at 55 DEG C, two peak of high initial magnetic permeability and the low high band relative loss factor factor and preparation method thereof under low-temperature sintering condition.
The present invention's adopted technical scheme that solves the problem is: the feature of the high curie point High Initial Permeability MnZn Ferrite Materials at 55 DEG C, this two peak is: it is made up of 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 3composition, wherein, CaCO 3consumption be the 0.025wt% of major ingredient, V 2o 5consumption be the 0.020wt% of major ingredient, Nb 2o 5consumption be the 0.020wt% of major ingredient, ZrO 2consumption be the 0.020wt% of major ingredient, Co 3o 4consumption be the 0.050wt% of major ingredient, Li 2cO 3consumption be the 0.030wt%-0.100wt% of major ingredient.Make raw material type of the present invention simple thus, 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 control 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 DEG C, 0-200 DEG C 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 DEG C, 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, 30.7mol% MnO and 16.4mol% ZnO composition, Li 2cO 3consumption be the 0.030wt% of major ingredient.Make the proportioning science more of the additive in the present invention thus, CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3acting in conjunction, produce synergistic effect, the performance of obtained MnZn ferrite material is more stable, and two peaks are at 55 DEG C, and 0-200 DEG C of magnetic permeability temperature stability is good, and magnetic permeability reaches 4500, and Curie temperature is high, and Curie temperature is greater than 190 DEG C.
A preparation method for the high curie point High Initial Permeability MnZn Ferrite Materials at two 55 DEG C, peaks, its feature is: in turn include the following steps:
(1) mix: after major ingredient is pressed proportion ingredient, adopt wet-mixed to obtain major ingredient slurry, the mixing time of wet-mixed is 50-90 minute;
(2) pre-burning: be added to after major ingredient being starched spraying dry in rotary kiln and carry out pre-burning, obtain Preburning material, the temperature of pre-burning is 850-950 DEG C, and the time of pre-burning is 60-90 minute;
(3) pulverize: be added to by additive after 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 μm;
(4) granulation: add in crushed material be equivalent to crushed material weight 1.5% PVA, adopt mist projection granulating, obtain particulate material;
(5) suppress: with powder former, particulate material is pressed into blank, the density of blank is 3.0 ± 0.2g/cm 3;
(6) sinter: blank is placed in nitrogen kiln and sinters, temperature rise rate is 1.25-3 DEG C/min, carry out densification at 1000 DEG C to sintering temperature to control, control oxygen level lower than 0.5%, sintering temperature controls at 1320-1340 DEG C, and holding-zone Control for Oxygen Content, at 4.5-5.5%, is incubated 3-5 hour, rate of temperature fall controls, at 1.5-2.5 DEG C/min, to obtain MnZn ferrite material.
Sintering temperature in the preparation method of the high curie point High Initial Permeability MnZn Ferrite Materials at 55 DEG C, the present invention two peak is at 1320-1340 DEG C, and the sintering temperature of 1370-1400 DEG C of the material of relatively conventional initial magnetic permeability 5000, reduces 50-60 DEG C.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: mixing of the additive of reasonably major ingredient proportioning and optimization, make the MnZn ferrite material stable performance obtained, two peaks are at 55 DEG C, and 0-200 DEG C of magnetic permeability temperature stability is good, magnetic permeability reaches 4500, Curie temperature is high, and Curie temperature is greater than 190 DEG C, environment for use with strong points, more professional, better reliability.
Process optimization in the present invention, tiny homogeneous, the cavernous Mn-Zn ferrite of microcosmic crystal grain has been obtained under the condition of low-temperature sintering temperature, this Mn-Zn ferrite has higher initial magnetic permeability, concretely, the initial permeability μ i of the MnZn ferrite material that the present invention obtains be 4500 ± 30%(10kHz, 0.25mT, 25 DEG C ± 3 DEG C), its Curie temperature is greater than 190 DEG C, and two peaks are positioned at 55 DEG C, temperature stability is good, and eddy-current loss is low.Particularly-40 DEG C have high magnetic permeability to 45 DEG C, can be good at improving signal transmission capabilities.The production method that the present invention adopts low temperature densification to sinter prepares MnZn ferrite material, stable processing technique, excellent property, and 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 DEG C, two peak is made up of major ingredient and additive, and wherein, major ingredient is by the Fe of 52.3mol% 2o 3, 30.2mol% MnO and 17.5mol% ZnO composition, additive is by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3composition, wherein, CaCO 3consumption be the 0.025wt% of major ingredient, V 2o 5consumption be the 0.020wt% of major ingredient, Nb 2o 5consumption be the 0.020wt% of major ingredient, ZrO 2consumption be the 0.020wt% of major ingredient, Co 3o 4consumption be the 0.050wt% of major ingredient, Li 2cO 3consumption be the 0.030wt% of major ingredient.
In the present embodiment, the preparation method of the high curie point High Initial Permeability MnZn Ferrite Materials at 55 DEG C, two peak in turn includes the following steps.
(1) mix: by the Fe of 52.3mol% 2o 3, 30.2mol% MnO and 17.5mol% ZnO mixing after, add in skin grinder and mix, in mixing process, add the pure water of the 35wt% being equivalent to major ingredient weight, adopt wet-mixed obtain major ingredient slurry, the mixing time of wet-mixed is 50 minutes.
(2) pre-burning: be added to after major ingredient being starched spraying dry in rotary kiln and carry out pre-burning, obtain Preburning material, the temperature of pre-burning is 850-950 DEG C, 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 3these additives are all added to after 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 μm, in crushing process, add the pure water of the 35wt% being equivalent to major ingredient weight, and dispersion agent and defoamer some (with obtain setting particle size range be as the criterion), this is common practise to those skilled in the art.
(4) granulation: add in crushed material be equivalent to crushed material weight 1.5% PVA, adopt mist projection granulating, obtain particulate material.Under normal circumstances, PVA being mixed with concentration is that the aqueous solution of 10wt% adds, namely add be equivalent to crushed material weight 15% concentration be the PVA aqueous solution of 10wt%.
(5) suppress: with powder former, particulate material is pressed into blank, the shape of blank is annular, and the density of blank is 3.0 ± 0.2g/cm 3.
(6) sinter: blank is placed in nitrogen kiln and sinters, temperature rise rate is 1.25-3 DEG C/min, carry out densification at 1000 DEG C to sintering temperature to control, control oxygen level lower than 0.5%, sintering temperature controls at 1320-1340 DEG C, and holding-zone Control for Oxygen Content, at 4.5-5.5%, is incubated 3-5 hour, rate of temperature fall controls, at 1.5-2.5 DEG C/min, to obtain 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.Through magnetic core prepared by said process, test normal temperature initial permeability μ i respectively, Curie temperature, μ i-T curve with instruments such as HP4284ALCR tester, high/low temperature thermostat containers, obtaining μ i is that 5100,0 DEG C to 200 DEG C magnetic permeability temperature stability is better; Curie temperature is higher, is greater than 170 DEG C; Two peaks are positioned at 60 DEG C.
Embodiment 2.
In the present embodiment, the high curie point High Initial Permeability MnZn Ferrite Materials at 55 DEG C, two peak is made up of major ingredient and additive, and wherein, major ingredient is by the Fe of 52.8mol% 2o 3, 30.5mol% MnO and 16.7mol% ZnO composition, additive is by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3composition, wherein, CaCO 3consumption be the 0.025wt% of major ingredient, V 2o 5consumption be the 0.020wt% of major ingredient, Nb 2o 5consumption be the 0.020wt% of major ingredient, ZrO 2consumption be the 0.020wt% of major ingredient, Co 3o 4consumption be the 0.050wt% of major ingredient, Li 2cO 3consumption be the 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 DEG C, two peak in turn includes the following steps.
(1) mix: by the Fe of 52.8mol% 2o 3, 30.5mol% MnO and 16.7mol% ZnO mixing after, add in skin grinder and mix, in mixing process, add the pure water of the 35wt% being equivalent to major ingredient weight, adopt wet-mixed obtain major ingredient slurry, the mixing time of wet-mixed is 50 minutes.
(2) pre-burning: be added to after major ingredient being starched spraying dry in rotary kiln and carry out pre-burning, obtain Preburning material, the temperature of pre-burning is 850-950 DEG C, 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 3these additives are all added to after 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 μm, in crushing process, add the pure water of the 35wt% being equivalent to major ingredient weight, and dispersion agent and defoamer some (with obtain setting particle size range be as the criterion), this is common practise to those skilled in the art.
(4) granulation: add in crushed material be equivalent to crushed material weight 1.5% PVA, adopt mist projection granulating, obtain particulate material.Under normal circumstances, PVA being mixed with concentration is that the aqueous solution of 10wt% adds, namely add be equivalent to crushed material weight 15% concentration be the PVA aqueous solution of 10wt%.
(5) suppress: with powder former, particulate material is pressed into blank, the shape of blank is annular, and the density of blank is 3.0 ± 0.2g/cm 3.
(6) sinter: blank is placed in nitrogen kiln and sinters, temperature rise rate is 1.25-3 DEG C/min, carry out densification at 1000 DEG C to sintering temperature to control, control oxygen level lower than 0.5%, sintering temperature controls at 1320-1340 DEG C, and holding-zone Control for Oxygen Content, at 4.5-5.5%, is incubated 3-5 hour, rate of temperature fall controls, at 1.5-2.5 DEG C/min, to obtain 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.Through magnetic core prepared by said process, test normal temperature initial permeability μ i respectively, Curie temperature, μ i-T curve with instruments such as HP4284ALCR tester, high/low temperature thermostat containers, obtaining μ i is that 4600,0 DEG C to 200 DEG C magnetic permeability temperature stability is better; Curie temperature is higher, is greater than 180 DEG C; Two peaks are positioned at 40 DEG C.
Embodiment 3.
In the present embodiment, the high curie point High Initial Permeability MnZn Ferrite Materials at 55 DEG C, two peak is made up of major ingredient and additive, and wherein, major ingredient is by the Fe of 53.5mol% 2o 3, 31.2mol% MnO and 15.3mol% ZnO composition, additive is by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3composition, wherein, CaCO 3consumption be the 0.025wt% of major ingredient, V 2o 5consumption be the 0.020wt% of major ingredient, Nb 2o 5consumption be the 0.020wt% of major ingredient, ZrO 2consumption be the 0.020wt% of major ingredient, Co 3o 4consumption be the 0.050wt% of major ingredient, Li 2cO 3consumption be the 0.030wt% of major ingredient.
In the present embodiment, the preparation method of the high curie point High Initial Permeability MnZn Ferrite Materials at 55 DEG C, two peak in turn includes the following steps.
(1) mix: by the Fe of 53.5mol% 2o 3, 31.2mol% MnO and 15.3mol% ZnO mixing after, add in skin grinder and mix, in mixing process, add the pure water of the 35wt% being equivalent to major ingredient weight, adopt wet-mixed obtain major ingredient slurry, the mixing time of wet-mixed is 50 minutes.
(2) pre-burning: be added to after major ingredient being starched spraying dry in rotary kiln and carry out pre-burning, obtain Preburning material, the temperature of pre-burning is 850-950 DEG C, 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 3these additives are all added to after 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 μm, in crushing process, add the pure water of the 35wt% being equivalent to major ingredient weight, and dispersion agent and defoamer some (with obtain setting particle size range be as the criterion), this is common practise to those skilled in the art.
(4) granulation: add in crushed material be equivalent to crushed material weight 1.5% PVA, adopt mist projection granulating, obtain particulate material.Under normal circumstances, PVA being mixed with concentration is that the aqueous solution of 10wt% adds, namely add be equivalent to crushed material weight 15% concentration be the PVA aqueous solution of 10wt%.
(5) suppress: with powder former, particulate material is pressed into blank, the shape of blank is annular, and the density of blank is 3.0 ± 0.2g/cm 3.
(6) sinter: blank is placed in nitrogen kiln and sinters, temperature rise rate is 1.25-3 DEG C/min, carry out densification at 1000 DEG C to sintering temperature to control, control oxygen level lower than 0.5%, sintering temperature controls at 1320-1340 DEG C, and holding-zone Control for Oxygen Content, at 4.5-5.5%, is incubated 3-5 hour, rate of temperature fall controls, at 1.5-2.5 DEG C/min, to obtain 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.Through magnetic core prepared by said process, test normal temperature initial permeability μ i respectively, Curie temperature, μ i-T curve with instruments such as HP4284ALCR tester, high/low temperature thermostat containers, obtaining μ i is that 4000,0 DEG C to 200 DEG C magnetic permeability temperature stability is better; Curie temperature is higher, is greater than 200 DEG C; Two peaks are positioned at 25 DEG C.
Embodiment 4.
In the present embodiment, the high curie point High Initial Permeability MnZn Ferrite Materials at 55 DEG C, two peak is made up of major ingredient and additive, and wherein, major ingredient is by the Fe of 52.9mol% 2o 3, 30.7mol% MnO and 16.4mol% ZnO composition, additive is by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3composition, wherein, CaCO 3consumption be the 0.025wt% of major ingredient, V 2o 5consumption be the 0.020wt% of major ingredient, Nb 2o 5consumption be the 0.020wt% of major ingredient, ZrO 2consumption be the 0.020wt% of major ingredient, Co 3o 4consumption be the 0.050wt% of major ingredient, Li 2cO 3consumption be the 0.030wt% of major ingredient.
In the present embodiment, the preparation method of the high curie point High Initial Permeability MnZn Ferrite Materials at 55 DEG C, two peak in turn includes the following steps.
(1) mix: by the Fe of 52.9mol% 2o 3, 30.7mol% MnO and 16.4mol% ZnO mixing after, add in skin grinder and mix, in mixing process, add the pure water of the 35wt% being equivalent to major ingredient weight, adopt wet-mixed obtain major ingredient slurry, the mixing time of wet-mixed is 50 minutes.
(2) pre-burning: be added to after major ingredient being starched spraying dry in rotary kiln and carry out pre-burning, obtain Preburning material, the temperature of pre-burning is 850-950 DEG C, 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 3these additives are all added to after 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 μm, in crushing process, add the pure water of the 35wt% being equivalent to major ingredient weight, and dispersion agent and defoamer some (with obtain setting particle size range be as the criterion), this is common practise to those skilled in the art.
(4) granulation: add in crushed material be equivalent to crushed material weight 1.5% PVA, adopt mist projection granulating, obtain particulate material.Under normal circumstances, PVA being mixed with concentration is that the aqueous solution of 10wt% adds, namely add be equivalent to crushed material weight 15% concentration be the PVA aqueous solution of 10wt%.
(5) suppress: with powder former, particulate material is pressed into blank, the shape of blank is annular, and the density of blank is 3.0 ± 0.2g/cm 3.
(6) sinter: blank is placed in nitrogen kiln and sinters, temperature rise rate is 1.25-3 DEG C/min, carry out densification at 1000 DEG C to sintering temperature to control, control oxygen level lower than 0.5%, sintering temperature controls at 1320-1340 DEG C, and holding-zone Control for Oxygen Content, at 4.5-5.5%, is incubated 3-5 hour, rate of temperature fall controls, at 1.5-2.5 DEG C/min, to obtain 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.Through magnetic core prepared by said process, test normal temperature initial permeability μ i respectively, Curie temperature, μ i-T curve with instruments such as HP4284ALCR tester, high/low temperature thermostat containers, obtaining μ i is that 4500,0 DEG C to 200 DEG C magnetic permeability temperature stability is better; Curie temperature is higher, is greater than 190 DEG C; Two peaks are positioned at 55 DEG C.
Embodiment 5.
In the present embodiment, the high curie point High Initial Permeability MnZn Ferrite Materials at 55 DEG C, two peak is made up of major ingredient and additive, and wherein, major ingredient is by the Fe of 52.9mol% 2o 3, 30.7mol% MnO and 16.4mol% ZnO composition, additive is by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3composition, wherein, CaCO 3consumption be the 0.025wt% of major ingredient, V 2o 5consumption be the 0.020wt% of major ingredient, Nb 2o 5consumption be the 0.020wt% of major ingredient, ZrO 2consumption be the 0.020wt% of major ingredient, Co 3o 4consumption be the 0.050wt% of major ingredient, Li 2cO 3consumption be the 0.050wt% of major ingredient.
In the present embodiment, the preparation method of the high curie point High Initial Permeability MnZn Ferrite Materials at 55 DEG C, two peak in turn includes the following steps.
(1) mix: by the Fe of 52.9mol% 2o 3, 30.7mol% MnO and 16.4mol% ZnO mixing after, add in skin grinder and mix, in mixing process, add the pure water of the 35wt% being equivalent to major ingredient weight, adopt wet-mixed obtain major ingredient slurry, the mixing time of wet-mixed is 50 minutes.
(2) pre-burning: be added to after major ingredient being starched spraying dry in rotary kiln and carry out pre-burning, obtain Preburning material, the temperature of pre-burning is 850-950 DEG C, 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 3these additives are all added to after 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 μm, in crushing process, add the pure water of the 35wt% being equivalent to major ingredient weight, and dispersion agent and defoamer some (with obtain setting particle size range be as the criterion), this is common practise to those skilled in the art.
(4) granulation: add in crushed material be equivalent to crushed material weight 1.5% PVA, adopt mist projection granulating, obtain particulate material.Under normal circumstances, PVA being mixed with concentration is that the aqueous solution of 10wt% adds, namely add be equivalent to crushed material weight 15% concentration be the PVA aqueous solution of 10wt%.
(5) suppress: with powder former, particulate material is pressed into blank, the shape of blank is annular, and the density of blank is 3.0 ± 0.2g/cm 3.
(6) sinter: blank is placed in nitrogen kiln and sinters, temperature rise rate is 1.25-3 DEG C/min, carry out densification at 1000 DEG C to sintering temperature to control, control oxygen level lower than 0.5%, sintering temperature controls at 1320-1340 DEG C, and holding-zone Control for Oxygen Content, at 4.5-5.5%, is incubated 3-5 hour, rate of temperature fall controls, at 1.5-2.5 DEG C/min, to obtain 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.Through magnetic core prepared by said process, test normal temperature initial permeability μ i respectively, Curie temperature, μ i-T curve with instruments such as HP4284ALCR tester, high/low temperature thermostat containers, obtaining μ i is that 4500,0 DEG C to 200 DEG C magnetic permeability temperature stability is better; Curie temperature is higher, is greater than 180 DEG C; Two peaks are positioned at 70 DEG C.
Embodiment 6.
In the present embodiment, the high curie point High Initial Permeability MnZn Ferrite Materials at 55 DEG C, two peak is made up of major ingredient and additive, and wherein, major ingredient is by the Fe of 52.9mol% 2o 3, 30.7mol% MnO and 16.4mol% ZnO composition, additive is by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3composition, wherein, CaCO 3consumption be the 0.025wt% of major ingredient, V 2o 5consumption be the 0.020wt% of major ingredient, Nb 2o 5consumption be the 0.020wt% of major ingredient, ZrO 2consumption be the 0.020wt% of major ingredient, Co 3o 4consumption be the 0.050wt% of major ingredient, Li 2cO 3consumption be the 0.100wt% of major ingredient.Major ingredient in the present invention can 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 DEG C, two peak in turn includes the following steps.
(1) mix: by the Fe of 52.9mol% 2o 3, 30.7mol% MnO and 16.4mol% ZnO mixing after, add in skin grinder and mix, in mixing process, add the pure water of the 35wt% being equivalent to major ingredient weight, adopt wet-mixed obtain major ingredient slurry, the mixing time of wet-mixed is 50 minutes.
(2) pre-burning: be added to after major ingredient being starched spraying dry in rotary kiln and carry out pre-burning, obtain Preburning material, the temperature of pre-burning is 850-950 DEG C, 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 3these additives are all added to after 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 μm, in crushing process, add the pure water of the 35wt% being equivalent to major ingredient weight, and dispersion agent and defoamer some (with obtain setting particle size range be as the criterion), this is common practise to those skilled in the art.
(4) granulation: add in crushed material be equivalent to crushed material weight 1.5% PVA, adopt mist projection granulating, obtain particulate material.Under normal circumstances, PVA being mixed with concentration is that the aqueous solution of 10wt% adds, namely add be equivalent to crushed material weight 15% concentration be the PVA aqueous solution of 10wt%.
(5) suppress: with powder former, particulate material is pressed into blank, the shape of blank is annular, and the density of blank is 3.0 ± 0.2g/cm 3.
(6) sinter: blank is placed in nitrogen kiln and sinters, temperature rise rate is 1.25-3 DEG C/min, carry out densification at 1000 DEG C to sintering temperature to control, control oxygen level lower than 0.5%, sintering temperature controls at 1320-1340 DEG C, and holding-zone Control for Oxygen Content, at 4.5-5.5%, is incubated 3-5 hour, rate of temperature fall controls, at 1.5-2.5 DEG C/min, to obtain 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.Through magnetic core prepared by said process, test normal temperature initial permeability μ i respectively, Curie temperature, μ i-T curve with instruments such as HP4284ALCR tester, high/low temperature thermostat containers, obtaining μ i is that 4400,0 DEG C to 200 DEG C magnetic permeability temperature stability is better; Curie temperature is higher, is greater than 170 DEG C; Two peaks are positioned at 100 DEG C.
Embodiment 7.
The high curie point High Initial Permeability MnZn Ferrite Materials at 55 DEG C, two peak in the present embodiment is made up of major ingredient and additive, and major ingredient is by the Fe of 52.6mol% 2o 3, 30.1mol% MnO and 17.3mol% ZnO composition, additive is by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3composition, wherein, CaCO 3consumption be the 0.025wt% of major ingredient, V 2o 5consumption be the 0.020wt% of major ingredient, Nb 2o 5consumption be the 0.020wt% of major ingredient, ZrO 2consumption be the 0.020wt% of major ingredient, Co 3o 4consumption be the 0.050wt% of major ingredient, Li 2cO 3consumption be the 0.070wt% of major ingredient.
In the present embodiment, the preparation method of the high curie point High Initial Permeability MnZn Ferrite Materials at 55 DEG C, two peak in turn includes the following steps.
(1) mix: after major ingredient is pressed proportion ingredient, adopt wet-mixed to obtain major ingredient slurry, the mixing time of wet-mixed is 50-90 minute.
(2) pre-burning: be added to after major ingredient being starched spraying dry in rotary kiln and carry out pre-burning, obtain Preburning material, the temperature of pre-burning is 850-950 DEG C, and the time of pre-burning is 60-90 minute.
(3) pulverize: be added to by additive after 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 μm.
(4) granulation: add in crushed material be equivalent to crushed material weight 1.5% PVA, adopt mist projection granulating, obtain particulate material.
(5) suppress: with powder former, particulate material is pressed into blank, the density of blank is 3.0 ± 0.2g/cm 3.
(6) sinter: blank is placed in nitrogen kiln and sinters, temperature rise rate is 1.25-3 DEG C/min, carry out densification at 1000 DEG C to sintering temperature to control, control oxygen level lower than 0.5%, sintering temperature controls at 1320-1340 DEG C, and holding-zone Control for Oxygen Content, at 4.5-5.5%, is incubated 3-5 hour, rate of temperature fall controls, at 1.5-2.5 DEG C/min, to obtain MnZn ferrite material.
Embodiment 8.
The high curie point High Initial Permeability MnZn Ferrite Materials at 55 DEG C, two peak in the present embodiment is made up of major ingredient and additive, and major ingredient is by the Fe of 53.2mol% 2o 3, 30.7mol% MnO and 16.1mol% ZnO composition, additive is by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3composition, wherein, CaCO 3consumption be the 0.025wt% of major ingredient, V 2o 5consumption be the 0.020wt% of major ingredient, Nb 2o 5consumption be the 0.020wt% of major ingredient, ZrO 2consumption be the 0.020wt% of major ingredient, Co 3o 4consumption be the 0.050wt% of major ingredient, Li 2cO 3consumption be the 0.055wt% of major ingredient.
In the present embodiment, the preparation method of the high curie point High Initial Permeability MnZn Ferrite Materials at 55 DEG C, two peak in turn includes the following steps.
(1) mix: after major ingredient is pressed proportion ingredient, adopt wet-mixed to obtain major ingredient slurry, the mixing time of wet-mixed is 50-90 minute.
(2) pre-burning: be added to after major ingredient being starched spraying dry in rotary kiln and carry out pre-burning, obtain Preburning material, the temperature of pre-burning is 850-950 DEG C, and the time of pre-burning is 60-90 minute.
(3) pulverize: be added to by additive after 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 μm.
(4) granulation: add in crushed material be equivalent to crushed material weight 1.5% PVA, adopt mist projection granulating, obtain particulate material.
(5) suppress: with powder former, particulate material is pressed into blank, the density of blank is 3.0 ± 0.2g/cm 3.
(6) sinter: blank is placed in nitrogen kiln and sinters, temperature rise rate is 1.25-3 DEG C/min, carry out densification at 1000 DEG C to sintering temperature to control, control oxygen level lower than 0.5%, sintering temperature controls at 1320-1340 DEG C, and holding-zone Control for Oxygen Content, at 4.5-5.5%, is incubated 3-5 hour, rate of temperature fall controls, at 1.5-2.5 DEG C/min, to obtain MnZn ferrite material.
Embodiment 9.
The high curie point High Initial Permeability MnZn Ferrite Materials at 55 DEG C, two peak in the present embodiment is made up of major ingredient and additive, and major ingredient is by the Fe of 52.6mol% 2o 3, 31.3mol% MnO and 16.1mol% ZnO composition, additive is by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3composition, wherein, CaCO 3consumption be the 0.025wt% of major ingredient, V 2o 5consumption be the 0.020wt% of major ingredient, Nb 2o 5consumption be the 0.020wt% of major ingredient, ZrO 2consumption be the 0.020wt% of major ingredient, Co 3o 4consumption be the 0.050wt% of major ingredient, Li 2cO 3consumption be the 0.090wt% of major ingredient.
In the present embodiment, the preparation method of the high curie point High Initial Permeability MnZn Ferrite Materials at 55 DEG C, two peak in turn includes the following steps.
(1) mix: after major ingredient is pressed proportion ingredient, adopt wet-mixed to obtain major ingredient slurry, the mixing time of wet-mixed is 50-90 minute.
(2) pre-burning: be added to after major ingredient being starched spraying dry in rotary kiln and carry out pre-burning, obtain Preburning material, the temperature of pre-burning is 850-950 DEG C, and the time of pre-burning is 60-90 minute.
(3) pulverize: be added to by additive after 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 μm.
(4) granulation: add in crushed material be equivalent to crushed material weight 1.5% PVA, adopt mist projection granulating, obtain particulate material.
(5) suppress: with powder former, particulate material is pressed into blank, the density of blank is 3.0 ± 0.2g/cm 3.
(6) sinter: blank is placed in nitrogen kiln and sinters, temperature rise rate is 1.25-3 DEG C/min, carry out densification at 1000 DEG C to sintering temperature to control, control oxygen level lower than 0.5%, sintering temperature controls at 1320-1340 DEG C, and holding-zone Control for Oxygen Content, at 4.5-5.5%, is incubated 3-5 hour, rate of temperature fall controls, at 1.5-2.5 DEG C/min, to obtain MnZn ferrite material.
Although the present invention with embodiment openly as above; but it is also not used to limit protection scope of the present invention; any technician being familiar with this technology, not departing from the change and retouching done in the spirit and scope of the present invention, all should belong to protection scope of the present invention.

Claims (3)

1. the high curie point High Initial Permeability MnZn Ferrite Materials at 55 DEG C, two peak, it is characterized in that: it is made up of major ingredient and additive, described major ingredient is by Fe 2o 3: 52.6-53.2mol%, MnO:30.1-31.3mol% and ZnO:16.1-17.3mol% form, and described additive is by CaCO 3, V 2o 5, Nb 2o 5, ZrO 2, Co 3o 4and Li 2cO 3composition, wherein, CaCO 3consumption be the 0.025wt% of major ingredient, V 2o 5consumption be the 0.020wt% of major ingredient, Nb 2o 5consumption be the 0.020wt% of major ingredient, ZrO 2consumption be the 0.020wt% of major ingredient, Co 3o 4consumption be the 0.050wt% of major ingredient, Li 2cO 3consumption be the 0.030wt%-0.100wt% of major ingredient, calcium carbonate for increasing resistivity, reduce eddy-current loss; Vanadium Pentoxide in FLAKES has katalysis, improves solid state reaction speed; Niobium Pentxoxide changes magnetic properties, improves initial permeability; Zirconium dioxide, for controlling grain-size, improves magnetic permeability; Co 3o 4for regulating the temperature stability of magnetic permeability; Quilonum Retard improves ferrite performance, and change temperature profile, two peaks of MnZn ferrite material are at 55 DEG C, and 0-200 DEG C of magnetic permeability temperature stability is good, and Curie temperature is greater than 190 DEG C.
2. the high curie point High Initial Permeability MnZn Ferrite Materials at 55 DEG C, two peak according to claim 1, is characterized in that: described major ingredient is by the Fe of 52.9mol% 2o 3, 30.7mol% MnO and 16.4mol% ZnO composition, Li 2cO 3consumption be the 0.030wt% of major ingredient.
3. a preparation method for the high curie point High Initial Permeability MnZn Ferrite Materials at 55 DEG C, two peak as claimed in claim 1 or 2, is characterized in that: in turn include the following steps:
(1) mix: after major ingredient is pressed proportion ingredient, adopt wet-mixed to obtain major ingredient slurry, the mixing time of wet-mixed is 50-90 minute;
(2) pre-burning: be added to after major ingredient being starched spraying dry in rotary kiln and carry out pre-burning, obtain Preburning material, the temperature of pre-burning is 850-950 DEG C, and the time of pre-burning is 60-90 minute;
(3) pulverize: be added to by additive after 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 μm;
(4) granulation: add in crushed material be equivalent to crushed material weight 1.5% PVA, adopt mist projection granulating, obtain particulate material;
(5) suppress: with powder former, particulate material is pressed into blank, the density of blank is 3.0 ± 0.2g/cm 3;
(6) sinter: blank is placed in nitrogen kiln and sinters, temperature rise rate is 1.25-3 DEG C/min, carry out densification at 1000 DEG C to sintering temperature to control, control oxygen level lower than 0.5%, sintering temperature controls at 1320-1340 DEG C, and holding-zone Control for Oxygen Content, at 4.5-5.5%, is incubated 3-5 hour, rate of temperature fall controls, at 1.5-2.5 DEG C/min, to obtain MnZn ferrite material.
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