CN107417269A - Two peak temperatures are less than 20 DEG C of the ferritic preparation method of wide-temperature high-permeability Mn-Zn - Google Patents

Two peak temperatures are less than 20 DEG C of the ferritic preparation method of wide-temperature high-permeability Mn-Zn Download PDF

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CN107417269A
CN107417269A CN201710496494.0A CN201710496494A CN107417269A CN 107417269 A CN107417269 A CN 107417269A CN 201710496494 A CN201710496494 A CN 201710496494A CN 107417269 A CN107417269 A CN 107417269A
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temperature
major ingredient
permeability
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刘�东
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Chongqing Zheng Feng Electronics Co Ltd
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Chongqing Zheng Feng Electronics Co Ltd
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Abstract

The present invention relates to a kind of preparation method of Ferrite, and in particular to a kind of two peak temperature is less than 20 DEG C of the ferritic preparation method of wide-temperature high-permeability Mn-Zn；Its component includes major ingredient and auxiliary material, and major ingredient includes Fe2O3, MnO and ZnO, auxiliary material include CaCO3、Nb2O5、Bi2O3And MoO3, preparation method includes, and (1), after major ingredient is pressed into proportion ingredient, coordinates to obtain major ingredient slurry using wet method；(2), major ingredient is starched and sieved after 120 DEG C of dryings in baking oven, is subsequently placed in high temperature furnace and carries out pre-burning, obtain Preburning material；(3) after, auxiliary ingredients are proportionally added in Preburning material, wet pulverizing is carried out, obtains crushed material；(4) addition using manual granulation, is sieved equivalent to the polyvinyl alcohol of crushed material dry weight 1.2%, drying, obtains particulate material in the crushed material after, being sieved to drying；(5), by particulate material it is compressing after be placed in atmosphere clock hood type furnace and sinter；The material prepared using a kind of wide-temperature high-permeability Mn-Zn ferrite of two peak temperature of this programme less than 20 DEG C has the advantages of high Curie temperature, strong applicability.

Description

Two peak temperatures are less than -20 DEG C of the ferritic preparation method of wide-temperature high-permeability Mn-Zn
Technical field
The present invention relates to a kind of preparation method of Ferrite, and in particular to a kind of width temperature of two peak temperature less than -20 DEG C The preparation method of high permeability MnZn ferrite.
Background technology
As the fast development of the digital communication technologies such as ADSL, Wireless Communication, communication apparatus are more next More it is widely used for open air.Moreover, with the expansion of mankind's activity scope, also more next is required to the temperature stability of communications service It is higher.It is TDK H5C4 materials that material commonly used in the prior art is a kind of, secondly peak temperature is at -10 DEG C or so, Curie temperature Tc For 110 DEG C, 25 DEG C of magnetic conductivity is 12000 ± 25%, -20 DEG C of magnetic conductivities 9000 or so, but the magnetic conductivity at -40 DEG C compared with Low, -60 DEG C do not provide.The shortcomings that this material is that 1, Applicable temperature scope is narrower, for less than -20 DEG C of low temperature electromagnetic property It is required that usually can not meet, winding turns can only be increased, increase is designed and manufactured as this；2nd, Curie temperature is relatively low, is 110 DEG C.
Another kind is Ceramic Magnetics, Inc. TC6000, and two peak temperatures are at -25 DEG C, 104 DEG C of Curie temperature. 25 DEG C of magnetic conductivity is 7500, and after coating Parylene (parylene), minimum magnetic conductivity is in the range of -40~85 DEG C 6000, -60 DEG C do not provide.The shortcomings that this material (1) Applicable temperature scope is narrower, the magnetic conductivity in the range of -40 DEG C~104 DEG C More than 7000；(2) Curie temperature is relatively low, only 104 DEG C, for -40~105 DEG C, -40~120 DEG C of such ultra-wide Temperature requires, often requires that Curie temperature more than 120 DEG C, or even 130 DEG C or so, the material does not reach design requirement.
The content of the invention
The invention is intended to provide the initial permeability having in the range of a kind of -60~120 DEG C higher than 6000, it is very suitable for The requirement such as ISDN pulse transformers, wireless communication base station transformer keeps the equipment of electromagnetic property in wide temperature range A kind of two peak temperature is less than -20 DEG C of the ferritic preparation method of wide-temperature high-permeability Mn-Zn.
A kind of two peak temperature in this programme is less than -20 DEG C of the ferritic preparation method of wide-temperature high-permeability Mn-Zn, group Dividing includes major ingredient and auxiliary material, and major ingredient includes 53.0~55.0mol% Fe2O3, 22.0~24.0mol% MnO, surplus is ZnO, auxiliary material include CaCO3、Nb2O5、Bi2O3And MoO3, preparation method comprises the following steps：
(1) after major ingredient, is pressed into proportion ingredient, coordinate to obtain major ingredient slurry using wet method, the incorporation time that wet method coordinates is 100-150 minutes；
(2), major ingredient is starched and sieved after 120 DEG C of dryings in baking oven, is subsequently placed in high temperature furnace and carries out pre-burning, obtain pre-burning Material, calcined temperature are 850~930 DEG C, and burn-in time is 150~180 minutes；
(3) after, auxiliary ingredients are proportionally added in Preburning material, wet pulverizing is carried out, obtains crushed material, wet method powder The broken time is 150~200 minutes, and the particle diameter of crushed material is 1.2~1.6 μm；
(4) polyvinyl alcohol equivalent to crushed material dry weight 1.2% is added in the crushed material after, being sieved to drying, using hand Work is granulated, and is crossed 60~120 mesh sieves, drying, is obtained particulate material；
(5), by particulate material it is compressing after be placed in atmosphere clock hood type furnace and sinter, heating rate is 3~5 DEG C/min, insulation For section temperature control at 1400~1430 DEG C, soaking zone Control for Oxygen Content is incubated 10~12 hours, rate of temperature fall control 12~15% System is at 2~5 DEG C/min；
It is an advantage of the invention that：MnZn ferrite material of the present invention due to still have at -60 DEG C more than 6000 magnetic Conductance, so in design and fabrication stage, equal escapable cost.And Curie's temperature of MnZn ferrite material of the present invention Degree is more than 120 DEG C, and measured value is between 125 DEG C to 130 DEG C, can be very therefore for requiring the device of 120 DEG C of Curie temperature Meet design requirement well.Fig. 1 shows the magnetic conductivity (μ i) of the present invention program product with temperature (T) change curve.
Further, in step (1), the incorporation time that wet method coordinates is 120 minutes.
Further, in step (2), calcined temperature is 890 DEG C, and burn-in time is 160 minutes.
Further, in step (3), the time of wet pulverizing is 180 minutes.
Further, in step (4), the sieve of selection is 80 mesh.
Further, in step (5), heating rate is 4 DEG C/min, and at 1420 DEG C, soaking zone oxygen contains soaking zone temperature control Amount control is incubated 11 hours 13%, and rate of temperature fall is controlled at 4 DEG C/min.
Brief description of the drawings
Fig. 1 is wide-temperature high-permeability Mn-Zn ferritic preparation method product of two peak temperatures less than -20 DEG C of the invention Magnetic conductivity varies with temperature curve.
Embodiment
Embodiment 1
The present invention provides the ferritic preparation method of wide-temperature high-permeability Mn-Zn that a kind of two peak temperature is less than -20 DEG C, group Dividing includes major ingredient and auxiliary material, and major ingredient includes 53.0mol% Fe2O3, 22.0mol% MnO, surplus ZnO, auxiliary material includes 200ppmCaCO3、50ppmNb2O5、300ppmBi2O3And 300ppmMoO3, preparation method comprises the following steps：
(1) after major ingredient, is pressed into proportion ingredient, coordinate to obtain major ingredient slurry using wet method, the incorporation time that wet method coordinates is 100 Minute；
(2), major ingredient is starched and sieved after 120 DEG C of dryings in baking oven, is subsequently placed in high temperature furnace and carries out pre-burning, obtain pre-burning Material, calcined temperature are 850 DEG C, and burn-in time is 150 minutes；
(3) after, auxiliary ingredients are proportionally added in Preburning material, wet pulverizing is carried out, obtains crushed material, wet method powder The broken time is 150 minutes, and the particle diameter of crushed material is 1.2 μm；
(4) polyvinyl alcohol equivalent to crushed material dry weight 1.2% is added in the crushed material after, being sieved to drying, using hand Work is granulated, and is crossed 60 mesh sieves, drying, is obtained particulate material；
(5), by particulate material it is compressing after be placed in atmosphere clock hood type furnace and sinter, heating rate is 3 DEG C/min, soaking zone For temperature control at 1400 DEG C, soaking zone Control for Oxygen Content is incubated 12 hours, rate of temperature fall is controlled at 2 DEG C/min 12%.
Embodiment 2
The present invention provides the ferritic preparation method of wide-temperature high-permeability Mn-Zn that a kind of two peak temperature is less than -20 DEG C, group Dividing includes major ingredient and auxiliary material, and major ingredient includes 55.0mol% Fe2O3, 24.0mol% MnO, surplus ZnO, auxiliary material includes 500ppmCaCO3、100ppmNb2O5、500ppmBi2O3And 500ppmMoO3, preparation method comprises the following steps：
(1) after major ingredient, is pressed into proportion ingredient, coordinate to obtain major ingredient slurry using wet method, the incorporation time that wet method coordinates is 150 Minute；
(2), major ingredient is starched and sieved after 120 DEG C of dryings in baking oven, is subsequently placed in high temperature furnace and carries out pre-burning, obtain pre-burning Material, calcined temperature are 930 DEG C, and burn-in time is 180 minutes；
(3) after, auxiliary ingredients are proportionally added in Preburning material, wet pulverizing is carried out, obtains crushed material, wet method powder The broken time is 200 minutes, and the particle diameter of crushed material is 1.6 μm；
(4) polyvinyl alcohol equivalent to crushed material dry weight 1.2% is added in the crushed material after, being sieved to drying, using hand Work is granulated, and is crossed 120 mesh sieves, drying, is obtained particulate material；
(5), by particulate material it is compressing after be placed in atmosphere clock hood type furnace and sinter, heating rate is 5 DEG C/min, soaking zone For temperature control at 1430 DEG C, soaking zone Control for Oxygen Content is incubated 10 hours, rate of temperature fall is controlled at 5 DEG C/min 15%.
Embodiment 3
The present invention provides the ferritic preparation method of wide-temperature high-permeability Mn-Zn that a kind of two peak temperature is less than 20 DEG C, component Including major ingredient and auxiliary material, major ingredient includes 54.0mol% Fe2O3, 23.0mol% MnO, surplus ZnO, auxiliary material includes 450ppmCaCO3、80ppmNb2O5、400ppmBi2O3And 400ppmMoO3, preparation method comprises the following steps：
(1) after major ingredient, is pressed into proportion ingredient, coordinate to obtain major ingredient slurry using wet method, the incorporation time that wet method coordinates is 120 Minute；
(2), major ingredient is starched and sieved after 120 DEG C of dryings in baking oven, is subsequently placed in high temperature furnace and carries out pre-burning, obtain pre-burning Material, calcined temperature are 890 DEG C, and burn-in time is 160 minutes；
(3) after, auxiliary ingredients are proportionally added in Preburning material, wet pulverizing is carried out, obtains crushed material, wet method powder The broken time is 180 minutes, and the particle diameter of crushed material is 1.4 μm；
(4) polyvinyl alcohol equivalent to crushed material dry weight 1.2% is added in the crushed material after, being sieved to drying, using hand Work is granulated, and is crossed 80 mesh sieves, drying, is obtained particulate material；
(5), by particulate material it is compressing after be placed in atmosphere clock hood type furnace and sinter, heating rate is 4 DEG C/min, soaking zone For temperature control at 1420 DEG C, soaking zone Control for Oxygen Content is incubated 11 hours, rate of temperature fall is controlled at 4 DEG C/min 13%.
Above-described is only embodiments of the invention, and the general knowledge such as known concrete structure and characteristic is not made herein in scheme Excessive description., without departing from the structure of the invention, can be with it should be pointed out that for those skilled in the art Several modifications and improvements are made, these should also be considered as protection scope of the present invention, and these are implemented all without the influence present invention Effect and practical applicability.

Claims (6)

1. two peak temperatures are less than -20 DEG C of the ferritic preparation method of wide-temperature high-permeability Mn-Zn, it is characterised in that：Its component bag Major ingredient and auxiliary material are included, major ingredient includes 53.0~55.0mol% Fe2O3, 22.0~24.0mol% MnO, surplus ZnO are auxiliary Material includes 200~500ppmCaCO3, 50~100ppmNb2O5, 300~500ppmBi2O3With 300~500ppmMoO3, preparation side Method comprises the following steps,
(1) after major ingredient, is pressed into proportion ingredient, coordinate to obtain major ingredient slurry using wet method, the incorporation time that wet method coordinates for 100~ 150 minutes；
(2), major ingredient is starched and sieved after 120 DEG C of dryings in baking oven, is subsequently placed in high temperature furnace and carries out pre-burning, obtain Preburning material, Calcined temperature is 850~930 DEG C, and burn-in time is 150~180 minutes；
(3) after, auxiliary ingredients are proportionally added in Preburning material, wet pulverizing is carried out, obtains crushed material, wet pulverizing Time is 150~200 minutes, and the particle diameter of crushed material is 1.2~1.6 μm；
(4) addition is made equivalent to the polyvinyl alcohol of crushed material dry weight 1.2% using manual in the crushed material after, being sieved to drying Grain, 60~120 mesh sieves are crossed, drying, obtain particulate material；
(5), by particulate material it is compressing after be placed in atmosphere clock hood type furnace and sinter, heating rate is 3~5 DEG C/min, soaking zone temperature At 1400~1430 DEG C, soaking zone Control for Oxygen Content is incubated 10~12 hours, rate of temperature fall control exists 12~15% for degree control 2~5 DEG C/min.
2. two peak temperature according to claim 1 is less than -20 DEG C of the ferritic preparation method of wide-temperature high-permeability Mn-Zn, It is characterized in that：In step (1), the incorporation time that wet method coordinates is 120 minutes.
3. two peak temperature according to claim 1 is less than -20 DEG C of the ferritic preparation method of wide-temperature high-permeability Mn-Zn, It is characterized in that：In step (2), calcined temperature is 890 DEG C, and burn-in time is 160 minutes.
4. two peak temperature according to claim 2 is less than -20 DEG C of the ferritic preparation method of wide-temperature high-permeability Mn-Zn, It is characterized in that：In step (3), the time of wet pulverizing is 180 minutes.
5. two peak temperature according to claim 1 is less than -20 DEG C of the ferritic preparation method of wide-temperature high-permeability Mn-Zn, It is characterized in that：In step (4), the sieve of selection is 80 mesh.
6. two peak temperature according to claim 1 is less than -20 DEG C of the ferritic preparation method of wide-temperature high-permeability Mn-Zn, It is characterized in that：In step (5), heating rate is 4 DEG C/min, and soaking zone temperature control is at 1420 DEG C, soaking zone oxygen content control System is incubated 11 hours 13%, and rate of temperature fall is controlled at 4 DEG C/min.
CN201710496494.0A 2017-06-26 2017-06-26 Two peak temperatures are less than 20 DEG C of the ferritic preparation method of wide-temperature high-permeability Mn-Zn Pending CN107417269A (en)

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EP4049987A4 (en) * 2020-02-19 2023-12-20 Hengdian Group DMEGC Magnetics Co., Ltd. Manganese zinc ferrite with high negative-temperature magnetic permeability and low high-temperature loss, and preparation method therefor

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CN101863657A (en) * 2010-06-23 2010-10-20 横店集团东磁股份有限公司 Mn-Zn ferrite material with wide temperature and high initial magnetoconductivity and preparation method thereof
CN103708818A (en) * 2013-12-12 2014-04-09 桐乡市耀润电子有限公司 Manganese-zinc ferrite material with secondary peak temperature of -20DEG C, high Curie point and high magnetic conductivity, and preparation method thereof

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CN103708818A (en) * 2013-12-12 2014-04-09 桐乡市耀润电子有限公司 Manganese-zinc ferrite material with secondary peak temperature of -20DEG C, high Curie point and high magnetic conductivity, and preparation method thereof

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EP4049987A4 (en) * 2020-02-19 2023-12-20 Hengdian Group DMEGC Magnetics Co., Ltd. Manganese zinc ferrite with high negative-temperature magnetic permeability and low high-temperature loss, and preparation method therefor

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