CN102010192B - Mangan zinc ferrite resintering process - Google Patents
Mangan zinc ferrite resintering process Download PDFInfo
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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
Technical field
The present invention relates to a kind of magnetic materials production technique, particularly a kind of Mangan zinc ferrite resintering process.
Background technology
Mn-Zn ferrite is by MnO-ZnO-Fe
2O
3Three kinds of complex ferrites that main component forms.MnZn ferrite material has the characteristics such as magnetic permeability height, saturation magnetic flux density is high, loss is low, is widely used in the 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, be the binder removal section from room temperature-600 ℃ (particularly 200-400 a ℃), 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 larger, 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 material character and product service requirements are different, as being 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 causes the blank cracking, or cause internal stress in blank inside, so that the degradation of product.
[0004]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, usually adopts the equilibrium oxygen partial pres-sure pattern to control.Through the formed Mn-Zn ferrite of high temperature sintering, if the oxygen partial pressure in the surrounding atmosphere is higher than the oxygen decomposition pressure of product, will be so that the oxygen in the surrounding atmosphere enters product, cause the product oxygen uptake, oxidizing reaction namely occurs, otherwise then put oxygen, reduction reaction namely occurs.Oxygen partial pressure (Po when surrounding atmosphere
2) suitably the time, oxide compound and ferrite neither oxidation do not reduce yet, the oxygen that absorbs in other words equates with the oxygen of emitting, and 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 clock hood type furnace, 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, and the oxygen level by the test sintering atmosphere in the production represents oxygen partial pressure.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, in the very not serious situation of the oxidation of system and iuvenescence, although 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, and meeting is so that 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 with the Fe metal, and sintering atmosphere is nitrogen and air mixed, generally can not form strongly reducing atmosphere, therefore, does not relate to the over reduction problem.
[0006]In the sintering process of Mn-Zn ferrite, a series of solid state reactions will occur.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 Mn ferrite of generation and Zn ferrite at high temperature mutual solid solution just obtain 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 so that the oxygen in the surrounding atmosphere enters product, cause the product oxygen uptake.When Mn-Zn ferrite cooled off in oxidizing atmosphere, the chemical transformation that can occur was as follows:
(1) temperature is more than 1100 ℃, when oxygen partial pressure is larger in the surrounding atmosphere, and MnFe
2O
4In some divalent manganesetion be oxidized to 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 is larger in the surrounding atmosphere, and MnFe
2O
4In divalent manganesetion continue to be oxidized to Manganic ion.In this temperature range, the γ-Mn with face-centred cubic structure of solid solution in ferrite
3O
4Isomeric transition occurs become the β-Mn with tetragonal
3O
4Because β-Mn
3O
4Different from the Spinel structure, β-Mn
3O
4Will from sosoloid, out exist mutually with other by precipitation.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 larger on the product performance impact.
(3) when temperature continues to drop to 950 ℃ of left and right sides, larger such as oxygen partial pressure in the surrounding atmosphere, MnFe
2O
4In divalent manganesetion continue to be oxidized to Manganic ion.In addition, β-Mn
3O
4Be oxidized to the α-Mn with body-centered cubic structure because of oxygen uptake
2O
3, namely
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, larger such as oxygen partial pressure in the surrounding atmosphere, MnFe
2O
4In divalent manganesetion also can be oxidized to 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 occurs become the α-Fe with rhombohedron structure
2O
3Because α-Fe
2O
3Structure different from the Spinel structure, understand precipitation equally and out 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
3With front precipitation α-Mn out
2O
3Form the in the form of sheets sosoloid α of tissue-(Fe
2O
3Mn
2O
3), be mixed in the crystal grain of Spinel, very large 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 in addition phase of needle-like, 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 the peroxidation degree is different, its surface color is also different, the blueing that has, and the general purple that has, what have is general red.
[0017] in long-term production process, sometimes because fault causes the kiln afterbody to enter air, or owing to reasons such as nitrogen gas purity reductions, cause product over oxidation in temperature-fall period, it is unusual to be embodied in surface color.Traditional treatment process is that these products are processed 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 Mangan zinc ferrite resintering process, excessive during with first sintering
The bad product of oxidation is reduced into qualified product again through returning burning.
The object of the present invention is achieved like this, and a kind of Mangan zinc ferrite resintering process places kiln to heat the ripe base product of Mn-Zn ferrite of over oxidation, average heating speed 200-300 ℃/h, do not produce cracking as prerequisite take product.Because redox reaction in the larger atmosphere of oxygen partial pressure, will occur 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 ion.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 be equilibrium oxygen partial pres-sure or weakly reducing atmosphere more than 900 ℃.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 technique.
For snperoxiaized Mn-Zn ferrite, owing to be in the low oxygen partial pressure atmosphere in the temperature-rise period, opposite chemical transformation when occuring with oxidation, its process is:
(1) when temperature is raised to 250 ℃ of left and right sides, the acicular α-Fe in the product
2O
3Become sheet.
(2) when temperature is raised to 600 ℃ of left and right sides, α-Fe
2O
3Isomeric transition occurs become γ-Fe
2O
3, its reaction is: α-Fe
2O
3→ 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 occurs 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 is until total overall reaction generates MnFe
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.
For reducing the volatile quantity of zinc and growing up of crystal grain, to select the lower soaking time of returning the burning temperature and lacking as good.
Owing to return in the burning process, the chemical reactions such as redox not only can occur in product, the physical reaction that is attended by simultaneously the further densification of product exists, and particularly returns and burns in the situation that temperature is higher, soaking time is long, returns the apparent size of product after burning 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, also can make low because of first sintering temperature or the short product that the size overlength occurs of soaking time after returning burning, become the normal product of size and surface color.
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 when being 900 ℃ divides
Press (0.01%) log (Po
2)
2Oxygen partial pressure when being 1000 ℃ (0.2%), T is 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 technique 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 ℃ for temperature (0.01%), log (Po
2)
2Oxygen partial pressure when being 1360 ℃ (7.5%), T is temperature, unit ℃.Temperature-fall period adopts conventional sintering technique 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 ℃ for temperature (0.01%), log (Po
2)
2Oxygen partial pressure when being 1100 ℃ (0.5%), T is temperature, unit ℃.Temperature-fall period adopts conventional sintering technique 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 ℃ for temperature (0.01%), log (Po
2)
2Oxygen partial pressure when being 1100 ℃ (0.5%), T is temperature, unit ℃.Temperature-fall period adopts conventional sintering technique 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. Mangan zinc ferrite resintering process, it is characterized in that: 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, the oxygen level that oxygen level≤0.02%, 900 is ℃-1000 ℃ 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 0.01% when being 900 ℃, log (Po
2)
2Oxygen partial pressure 0.2% when being 1000 ℃, T is temperature, unit ℃, and the first sintering temperature of this product is 1360 ℃, top temperature is 1000 ℃ when returning burning, reach 1000 ℃ and enter holding stage, soaking time is 0.5h, and the holding stage oxygen level is set to 0.2%, temperature-fall period adopts conventional sintering technique to control, 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.
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CN102376444B (en) * | 2011-08-25 | 2016-01-20 | 天长市中德电子有限公司 | A kind of sintering method of magnetic core |
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 |
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 |
CN103570363B (en) * | 2013-11-13 | 2015-04-22 | 宝钢磁业(江苏)有限公司 | High-performance power manganese zinc ferrite sintering process |
CN104310981B (en) * | 2014-10-10 | 2017-03-29 | 江苏省晶石磁性材料与器件工程技术研究有限公司 | A kind of manganese-zinc ferrite flashes 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 |
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 |
CN112794723B (en) * | 2021-01-12 | 2022-09-02 | 乳源东阳光磁性材料有限公司 | Return firing method of manganese-zinc power ferrite magnetic core |
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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