CN102010192A - Mangan zinc ferrite resintering process - Google Patents

Mangan zinc ferrite resintering process Download PDF

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CN102010192A
CN102010192A CN 201010527186 CN201010527186A CN102010192A CN 102010192 A CN102010192 A CN 102010192A CN 201010527186 CN201010527186 CN 201010527186 CN 201010527186 A CN201010527186 A CN 201010527186A CN 102010192 A CN102010192 A CN 102010192A
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temperature
product
atmosphere
ferrite
sintering
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CN102010192B (en
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黄伟
李良俊
石庆辉
段树彬
胡健
李文庆
徐晓利
陈兴贵
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YIBIN JINCHUAN ELECTRONICS CO Ltd
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Abstract

The invention relates to a mangan zinc ferrite resintering process. A superoxidized mangan zinc ferrite ripe blank product is put into a kiln for heating, wherein the atmosphere is air or nitrogen atmosphere at the temperature of between room temperature and 500 DEG C, is nitrogen atmosphere at the temperature of between 500 and 900 DEG C, and is balanced oxygen partial pressure or weakly reducing atmosphere at the temperature of above 900 DEG C on the premise that the product is not cracked; and the lowest keeping temperature for resintering is 1,000 DEG C, and the highest temperature is the temperature at which a raw blank of the product is sintered and is kept for 0.5 to 3 hours, and a heat preservation period atmosphere and a temperature reduction process can be controlled according to the conventional sintering process. By the implementation of the process, a mangan zinc ferrite waste product of which the surface color is abnormal due to oxidation is converted into a product of which the surface color is normal. Meanwhile, a product with ultralong size due to low primary sintering temperature or short temperature keeping time can be changed into a product of the normal size and surface color after being resintered.

Description

A kind of Mn-Zn ferrite returns firing technique
Affiliated technical field
The present invention relates to a kind of magnetic materials production technology, particularly a kind of Mn-Zn ferrite returns firing technique.
Background technology
Mn-Zn ferrite is by MnO-ZnO-Fe 2O 3Three kinds of complex ferrites that main component is formed.MnZn ferrite material has characteristics such as magnetic permeability height, saturation magnetic flux density height, loss be low, is widely used in fields such as household electrical appliance, network communication, automotive electronics, aerospace.
In traditional sintering process process, the Mn-Zn ferrite green compact are placed the kiln high temperature sintering, be broadly divided into temperature rise period, holding stage and temperature-fall period.In the temperature rise period, from room temperature-600 ℃ (particularly 200-400 a ℃) is the binder removal section, heat-up rate is slower, V-bar is not higher than 100 ℃/h, and 600-900 ℃ heat-up rate is very fast, and average heating speed is 150-250 ℃/h, 900-1100 ℃ of blank shrinks bigger, heat-up rate is unsuitable too fast, and average heating speed is 100-200 ℃/h, and the average heating speed of 1100 ℃-sintering temperature is 200-300 ℃/h.Sintering temperature is 1100-1400 ℃, there are differences because of material character and product service requirements are different, as be used for 300kHz and following power ferrite, sintering temperature is generally 1300-1400 ℃, be used for the above power ferrite of 300kHz, sintering temperature is generally 1200-1300 ℃, and the sintering temperature of high magnetic conductivity ferrite is generally about 1400 ℃.Holding stage, the time is generally 3-6h, and it is 10-15h's that the soaking time of report sintering superhigh magnetic conductivity Mn-Zn ferrite is also arranged.At temperature-fall period, average cooling rate is generally 100-200 ℃/h.If speed of cooling is too fast, can cause blank cracking, or cause internal stress in blank inside, make the degradation of product.
The general air atmosphere environment that adopts of temperature rise period is perhaps controlled oxygen level less than 0.2% volume at 900-1100 ℃, and the sintering atmosphere of holding stage and temperature-fall period needs control, adopts the equilibrium oxygen partial pres-sure pattern to control usually.Through the formed Mn-Zn ferrite of high temperature sintering,, will make that the oxygen in the surrounding atmosphere enters product if the oxygen partial pressure in the surrounding atmosphere is higher than the oxygen decomposition pressure of product, cause the product oxygen uptake, oxidizing reaction promptly takes place, otherwise then put oxygen, reduction reaction promptly takes place.Oxygen partial pressure (Po when surrounding atmosphere 2) suitably the time, oxide compound and ferrite neither oxidation do not reduce yet, the oxygen of Xi Shouing equates with the oxygen of emitting in other words, is in chemistry balance state, oxygen partial pressure at this moment just is called equilibrium oxygen partial pres-sure.The equilibrium oxygen partial pres-sure of Mn-Zn ferrite and the relation of temperature can be represented by the formula:
log(Po 2)＝-A/T+B
In the formula, Po 2It is the pressure component of oxygen under 1 atmospheric pressure.Because Mn-Zn ferrite is generally produced in tunnel furnace or bell jar stove, the product ambient pressure is a little more than ambient atmosphere pressure, and therefore, oxygen content is similar to oxygen partial pressure value in the atmosphere, represents oxygen partial pressure by the oxygen level of test sintering atmosphere in the production.A, B are constant, and be relevant with material prescription and product performance requirement, and generally speaking, the span of A is 13000-15000, and the span of B is 7-10.T is the absolute temperature of product, unit K.
Usually, in the sintering process of Mn-Zn ferrite, when the oxidation of system and iuvenescence not very under the serious situation, though appraising at the current rate or the room occurring of metal ion can appear, their can solid solution in original mutually in, still keep single-phase.If but serious oxidation and iuvenescence appear in system, Mn-Zn ferrite is oxidized with reduction and precipitation is separated out other mutually, can make the degradation of Mn-Zn ferrite.Owing to only under the strongly reducing atmosphere condition, just have Mn in the Mn-Zn ferrite 2+And Fe 2+Be reduced into Mn and exist with other form mutually, and sintering atmosphere is nitrogen and air mixed, generally can not form strongly reducing atmosphere, therefore, does not relate to the over reduction problem with the Fe metal.
In the sintering process of Mn-Zn ferrite, a series of solid state reactions will take place.The solid state reaction of Mn-Zn ferrite can be divided into Mn ferrite and two the solid state reaction processes of Zn ferrite of generating, and the at high temperature mutual solid solution of the Mn ferrite of generation and Zn ferrite just obtains Mn-Zn ferrite.Through the formed Mn-Zn ferrite of high temperature sintering, along with the reduction of temperature, the oxygen decomposition pressure in the product descends, if the oxygen partial pressure in the surrounding atmosphere is higher than the oxygen decomposition pressure of product, will make that the oxygen in the surrounding atmosphere enters product, causes the product oxygen uptake.When Mn-Zn ferrite cooled off in oxidizing atmosphere, the chemical transformation that can take place was as follows:
(1) temperature is more than 1100 ℃, when oxygen partial pressure in the surrounding atmosphere is big, and MnFe 2O 4In some divalent manganesetion be oxidized to the manganic ion.γ-Mn appears in the result 3O 4, γ-Fe also appears simultaneously 2O 3Its reaction is:
4MnFe 2O 4+[O]→MnFe 2O 4·γ-Mn 3O 4·3γ-Fe 2O 3
Because the γ-Mn that generates 3O 4And γ-Fe 2O 3All be face-centred cubic structure, they can solid solution form sosoloid in ferrite, still be single-phase, and are little to the performance impact of material.
(2) temperature drops in the 1100-1000 ℃ of scope, when oxygen partial pressure in the surrounding atmosphere is big, and MnFe 2O 4In divalent manganesetion continue to be oxidized to the manganic ion.In this temperature range, the γ-Mn with face-centred cubic structure of solid solution in ferrite 3O 4Isomeric transition takes place become the β-Mn with tetragonal 3O 4Because β-Mn 3O 4Different with the spinel phase structure, β-Mn 3O 4Will from sosoloid, come out to exist mutually by precipitation with other.Its reaction is:
MnFe 2O 4·γ-Mn 3O 4·γ-Fe 2O 3→MnFe 2O 4·γ-Fe 2O 3+β-Mn 3O 4
Owing to β-Mn occurred 3O 4Phase can cause lattice distortion in addition, and is bigger to the product performance influence.
(3) when temperature continues to drop to 950 ℃ of left and right sides, bigger as oxygen partial pressure in the surrounding atmosphere, MnFe 2O 4In divalent manganesetion continue to be oxidized to the manganic ion.In addition, β-Mn 3O 4Be oxidized to α-Mn with body-centered cubic structure because of oxygen uptake 2O 3, promptly
2β-Mn 3O 4+[O]→3α-Mn 2O 3
Because α-Mn 2O 3Have body-centered cubic structure, also will exist mutually with other, this will exert an influence to the performance of Mn-Zn ferrite.
(4) when temperature continues to drop to 600 ℃ of left and right sides, bigger as oxygen partial pressure in the surrounding atmosphere, MnFe 2O 4In divalent manganesetion also can be oxidized to the manganic ion, but since temperature lower, oxidation rate slows down.Solid solution is in MnFe 2O 4In the γ-Fe with face-centred cubic structure 2O 3Isomeric transition takes place become the α-Fe with rhombohedron structure 2O 3Because α-Fe 2O 3Structure different with the spinel phase structure, understand precipitation equally and come out to exist mutually with other.Its reaction is:
MnFe 2O 4·γ-Fe 2O 3→MnFe 2O 4+α-Fe 2O 3
These α-Fe 2O 3α-the Mn that comes out with the front precipitation 2O 3Form the sosoloid α-(Fe of tissue in the form of sheets 2O 3Mn 2O 3), be mixed in the crystal grain of spinel phase, very big to the performance impact of material.
(5) in the time of in system temperature drops to 300-250 ℃ of scope, a large amount of α-Fe 2O 3To form needle-like phase in addition, have a strong impact on the Mn-Zn ferrite product performance.
As known from the above, in the Mn-Zn ferrite of in peroxidation atmosphere, lowering the temperature, produce α-Mn 2O 3And α-Fe 2O 3The phase precipitation is to cause that the unusual major cause of surface color appears in product in addition.Because peroxidation degree difference, its surface color is also different, the blueing that has, and the general purple that has, what have is general red.
In the long-term production process, sometimes because fault causes the kiln afterbody to enter air, or, cause product over oxidation in temperature-fall period owing to reasons such as nitrogen gas purity reductions, it is unusual to be embodied in surface color.Traditional treatment process is that these products are handled as bad product or scrap products, brings financial loss to enterprise, causes the wasting of resources to society.
Summary of the invention
The purpose of this invention is to provide a kind of Mn-Zn ferrite and return firing technique, the bad product of over oxidation is reduced into qualified product again through returning burning during with first sintering.
The object of the present invention is achieved like this, and a kind of Mn-Zn ferrite returns firing technique, places kiln to heat the ripe base product of Mn-Zn ferrite of over oxidation, and average heating speed 200-300 ℃/h, not producing cracking with product is prerequisite.Because redox reaction in the bigger atmosphere of oxygen partial pressure, will take place about 600 ℃ in Mn-Zn ferrite, therefore need controlled atmosphere, product is in the lower oxygen partial pressure atmosphere, thereby suppresses the oxidizing reaction in the product, promote the reduction of manganic ionic.Concrete operations are exactly to be air or nitrogen atmosphere from room temperature to 500 ℃, rise to from 500 ℃ to be nitrogen atmosphere 900 ℃ of processes, and more than 900 ℃ equilibrium oxygen partial pres-sure or weakly reducing atmosphere.Return minimum 1000 ℃ of the holding temperature of burning, be up to the temperature of product green sintering, soaking time is 0.5-3h, and holding stage atmosphere and temperature reduction technology can be controlled by conventional sintering technology.
For snperoxiaized Mn-Zn ferrite, owing to be in the low oxygen partial pressure atmosphere in the temperature-rise period, opposite chemical transformation when taking place with oxidation, its process is:
(1) when temperature is raised to 250 ℃ of left and right sides, the acicular-Fe in the product 2O 3Become sheet.
(2) when temperature is raised to 600 ℃ of left and right sides, α-Fe 2O 3Isomeric transition takes place become γ-Fe 2O 3, its reaction is: α-Fe2O3 → γ-Fe 2O 3
(3) when temperature is raised to 950 ℃ of left and right sides, α-Mn 2O 3Put oxygen and be reduced to β-Mn 3O 4, i.e. 3 α-Mn 2O 3→ 2 β-Mn 3O 4+ [O]
(4) when temperature is raised to 1000 ℃ of left and right sides, β-Mn 3O 4Isomeric transition takes place become γ-Mn 3O 4, i.e. β-Mn 3O 4→ γ-Mn 3O 4
And γ-Mn 3O 4Be face-centred cubic structure, can with γ-Fe 2O 3Form sosoloid.Mn 3O 4Can regard Mn as again 2O 3MnO facilitates and Fe like this 2O 3Reaction generates MnFe 2O 4Concrete reaction is: Mn 3O 4+ Fe 2O 3→ MnFe 2O 4+ Mn 2O 3The Mn that reaction is remaining 2O 3Again can deoxidation changes Mn into because being in 1000 ℃ high temperature 3O 4Newly-generated Mn 3O 4Again with Fe 2O 3React and generate MnFe 2O 4, so circulation generates MnFe up to total overall reaction 2O 4Temperature-fall period adopts traditional technology, and atmosphere is controlled by equilibrium oxygen partial pres-sure basically, has prevented the generation of peroxidation phenomenon.
Owing to produce α-Mn in the Mn-Zn ferrite of over oxidation 2O 3And α-Fe 2O 3Again formed MnFe 2O 4, so its surface color improves, simultaneously, because other is eliminated mutually, so product performance have also obtained improvement to a certain degree.
Be to reduce the volatile quantity of zinc and growing up of crystal grain, to select lower returning to burn temperature and short soaking time is good.
Owing to return in the burning process, chemical reactions such as redox not only can take place in product, the physical reaction that is attended by the further densification of product simultaneously exists, and particularly returns and burns under the situation that temperature is higher, soaking time is long, returns the apparent size that burns the back product and has reducing to a certain degree.
By implementing the present invention, can will change the normal product of surface color into because of the unusual Mn-Zn ferrite waste product of oxidation surface color.Simultaneously, can make also that the low or short product that the size overlength occurs of soaking time becomes the normal product of size and surface color after returning burning because of first sintering temperature.
Embodiment
Below in conjunction with example, the present invention is described further:
Embodiment one:
Place kiln to heat the unusual Mn-Zn ferrite product of first sintering over oxidation surface color, average heating speed is 200 ℃/h, rise to 500 ℃ from room temperature and be air atmosphere, 500-900 ℃ is nitrogen atmosphere (oxygen level≤0.02%), and 900 ℃-1000 ℃ oxygen level is controlled by following formula:
log(Po 2) T＝log(Po 2) 1+[log(Po 2) 1-log(Po 2) 2](T-900)/100
In the formula, log (Po 2) TOxygen partial pressure during for temperature T, log (Po 2) 1Oxygen partial pressure when being 900 ℃ (0.01%), log (Po 2) 2Oxygen partial pressure when being 1000 ℃ (0.2%), T is a temperature, unit ℃.The first sintering temperature of this product is 1360 ℃, and top temperature is 1000 ℃ when returning burning, reaches 1000 ℃ and enters holding stage, and soaking time is 0.5h, and the holding stage oxygen level is set to 0.2%.Temperature-fall period adopts conventional sintering technology to control, and the product surface color was normal after cooling was finished, and obtained qualified Mn-Zn ferrite product, and the product design size through returning burning does not change substantially.
Embodiment two:
Place kiln to heat the unusual Mn-Zn ferrite product of first sintering over oxidation surface color, average heating speed is 300 ℃/h, rise to 500 ℃ from room temperature and be air atmosphere, 500-900 ℃ is nitrogen atmosphere (oxygen level≤0.02%), the first sintering temperature of this product is 1360 ℃, and top temperature is similarly 1360 ℃ when returning burning, and is identical with this product green sintering temperature, soaking time is 3h, and the holding stage oxygen level is 7.5%.900-1360 ℃ oxygen level is controlled by following formula:
log(Po 2) T＝log(Po 2) 1+[log(Po 2) 1-log(Po 2) 2](T-900)/460
In the formula, log (Po 2) TOxygen partial pressure when being T for temperature, log (Po 2) 1Oxygen partial pressure when being 900 ℃ (0.01%) for temperature, log (Po 2) 2Oxygen partial pressure when being 1360 ℃ (7.5%), T is a temperature, unit ℃.Temperature-fall period adopts conventional sintering technology to control, the product surface color was normal after cooling was finished, obtain qualified Mn-Zn ferrite product, product design size foreign minister through returning burning becomes 28.30mm by 28.54mm, width becomes 11.94mm by 12.04mm, center pillar becomes 7.44mm by 7.50mm, has dwindled about 0.8%.
Embodiment three:
Place kiln to heat the unusual Mn-Zn ferrite product of first sintering over oxidation surface color, average heating speed is 200 ℃/h, rise to 500 ℃ from room temperature and be air atmosphere, 500-900 ℃ is nitrogen atmosphere (oxygen level≤0.02%), the first sintering temperature of this product is 1360 ℃, top temperature is 1100 ℃ when returning burning, and soaking time is 0.5h, and the holding stage oxygen level is 0.5%.900-1100 ℃ oxygen level is controlled by following formula:
log(Po 2) T＝log(Po 2) 1+[log(Po 2) 1-log(Po 2) 2](T-900)/200
In the formula, log (Po 2) TOxygen partial pressure when being T for temperature, log (Po 2) 1Oxygen partial pressure when being 900 ℃ (0.01%) for temperature, log (Po 2) 2Oxygen partial pressure when being 1100 ℃ (0.5%), T is a temperature, unit ℃.Temperature-fall period adopts conventional sintering technology to control, the product surface color was normal after cooling was finished, obtain qualified Mn-Zn ferrite product, product design size foreign minister through returning burning becomes 28.54mm by 28.56mm, width becomes 12.04mm by 12.04mm, center pillar becomes 7.50mm by 7.50mm, and product size changes very little.
Embodiment four:
Place kiln to heat the unusual Mn-Zn ferrite product of first sintering over oxidation surface color, average heating speed is 320 ℃/h, rise to 900 ℃ from room temperature and be nitrogen atmosphere (oxygen level≤0.02%), the first sintering temperature of this product is 1360 ℃, top temperature is 1100 ℃ when returning burning, soaking time is 1h, and the holding stage oxygen level is 0.5%.900-1100 ℃ oxygen level is controlled by following formula:
log(Po 2) T＝log(Po 2) 1+[log(Po 2) 1-log(Po 2) 2](T-900)/200
In the formula, log (Po 2) TOxygen partial pressure when being T for temperature, log (Po 2) 1Oxygen partial pressure when being 900 ℃ (0.01%) for temperature, log (Po 2) 2Oxygen partial pressure when being 1100 ℃ (0.5%), T is a temperature, unit ℃.Temperature-fall period adopts conventional sintering technology to control, the product surface color was normal after cooling was finished, obtain qualified Mn-Zn ferrite product, product design size foreign minister through returning burning becomes 28.52mm by 28.54mm, width becomes 12.02mm by 12.04mm, center pillar becomes 7.50mm by 7.50mm, and product size changes less.

Claims (1)

1. a Mn-Zn ferrite returns firing technique, place kiln to heat the ripe base product of Mn-Zn ferrite of over oxidation, comprise temperature rise period, holding stage and temperature-fall period, holding stage atmosphere and temperature reduction technology can be controlled by conventional sintering technology, it is characterized in that: it is prerequisite that heat-up rate does not produce cracking with product, intensification ℃ is air or nitrogen atmosphere from room temperature to 500, rises to from 500 ℃ to be nitrogen atmosphere 900 ℃ of processes, and more than 900 ℃ equilibrium oxygen partial pres-sure atmosphere.Return minimum 1000 ℃ of the holding temperature of burning, be up to the temperature of product green sintering, soaking time is 0.5-3h.
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Cited By (9)

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CN102376444A (en) * 2011-08-25 2012-03-14 天长市中德电子有限公司 Magnetic core sintering method and device
CN102690122A (en) * 2012-06-05 2012-09-26 宜宾盈泰光电有限公司 Method for remedying rejected manganese-zinc ferrites by using atmosphere heat treatment
CN103467106A (en) * 2013-09-03 2013-12-25 宝钢磁业（江苏）有限公司 Sintering process of ferrite with high magnetic permeability
CN103570363A (en) * 2013-11-13 2014-02-12 宝钢磁业（江苏）有限公司 High-performance power manganese zinc ferrite sintering process
CN104310981A (en) * 2014-10-10 2015-01-28 江苏省晶石磁性材料与器件工程技术研究有限公司 Manganese zinc ferrite burn-back method
CN106007736A (en) * 2016-05-13 2016-10-12 泰州茂翔电子器材有限公司 Sintering method for high-performance manganese zinc ferrite material
CN107098693A (en) * 2017-04-28 2017-08-29 苏州冠达磁业有限公司 A kind of anti-interference manganese-zinc ferrite of high frequency and preparation method thereof
CN112794723A (en) * 2021-01-12 2021-05-14 乳源东阳光磁性材料有限公司 Return firing method of manganese-zinc power ferrite magnetic core
CN113284731A (en) * 2021-05-17 2021-08-20 湖北微硕电子科技有限公司 High-frequency large-magnetic-field soft magnetic ferrite material and preparation method thereof

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102376444A (en) * 2011-08-25 2012-03-14 天长市中德电子有限公司 Magnetic core sintering method and device
CN102690122A (en) * 2012-06-05 2012-09-26 宜宾盈泰光电有限公司 Method for remedying rejected manganese-zinc ferrites by using atmosphere heat treatment
CN103467106A (en) * 2013-09-03 2013-12-25 宝钢磁业（江苏）有限公司 Sintering process of ferrite with high magnetic permeability
CN103467106B (en) * 2013-09-03 2014-12-24 宝钢磁业（江苏）有限公司 Sintering process of ferrite with high magnetic permeability
CN103570363A (en) * 2013-11-13 2014-02-12 宝钢磁业（江苏）有限公司 High-performance power manganese zinc ferrite sintering process
CN104310981A (en) * 2014-10-10 2015-01-28 江苏省晶石磁性材料与器件工程技术研究有限公司 Manganese zinc ferrite burn-back method
CN106007736A (en) * 2016-05-13 2016-10-12 泰州茂翔电子器材有限公司 Sintering method for high-performance manganese zinc ferrite material
CN107098693A (en) * 2017-04-28 2017-08-29 苏州冠达磁业有限公司 A kind of anti-interference manganese-zinc ferrite of high frequency and preparation method thereof
CN107098693B (en) * 2017-04-28 2021-01-19 苏州冠达磁业有限公司 High-frequency anti-interference manganese-zinc ferrite and preparation method thereof
CN112794723A (en) * 2021-01-12 2021-05-14 乳源东阳光磁性材料有限公司 Return firing method of manganese-zinc power ferrite magnetic core
CN113284731A (en) * 2021-05-17 2021-08-20 湖北微硕电子科技有限公司 High-frequency large-magnetic-field soft magnetic ferrite material and preparation method thereof
CN113284731B (en) * 2021-05-17 2022-08-02 湖北微硕电子科技有限公司 High-frequency large-magnetic-field soft magnetic ferrite material and preparation method thereof

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