CN103467106A - Sintering process of ferrite with high magnetic permeability - Google Patents
Sintering process of ferrite with high magnetic permeability Download PDFInfo
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- CN103467106A CN103467106A CN2013103948482A CN201310394848A CN103467106A CN 103467106 A CN103467106 A CN 103467106A CN 2013103948482 A CN2013103948482 A CN 2013103948482A CN 201310394848 A CN201310394848 A CN 201310394848A CN 103467106 A CN103467106 A CN 103467106A
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Abstract
The invention discloses a sintering process of ferrite with high magnetic permeability. The sintering process comprises a heating step, a densification step, a heat preservation step and a cooling step, wherein the heating step comprises the processes: sending the ferrite into a bell type sintering furnace, keeping the initial temperature at 50 DEG C, then heating at the rate of 2-3 DEG C/min, firstly performing glue discharge on the ferrite, and then adopting an air sintering method; the densification step comprises the processes: controlling the range of oxygen content between 3% and 4%, and continuously performing densification for 2-3h; the heat preservation step comprises the processes: controlling the oxygen content at 4%-5%, and continuously performing heat preservation for 4-5h; the cooling step comprises the processes: adopting a cooling way with relatively small cooling amplitude, controlling the cooling speed at 2-3 DEG C/min, and obtaining the oxygen content through an equilibrium atmosphere formula in the process. The sintering process disclosed by the invention has the beneficial effects that the equilibrium atmosphere formula for sintering the ferrite with high magnetic permeability can be flexibly adjusted against the ferrite with different formulas, different temperatures correspond to relative equilibrium atmospheres, and the sintering process has the advantages of strong practicality, flexibility and changeability.
Description
Technical field
The present invention relates to a kind of high magnetic conductivity ferrite sintering process.
Background technology
Electronic industry constantly develops, and make the volume of magnetic elements more and more be tending towards microminiaturized, thereby the research of high permeability MnZn ferrite day by day becomes an important directions of soft magnetic ferrite research.Because when initial permeability is higher, just can reach the inductance value needed with less coil turn, thereby can effectively reduce the direct current resistance of coil and the loss of introducing thereof, and can also reduce significantly device volume simultaneously, be conducive to miniaturization and the lightweight of device.
Sintering technology for high permeability MnZn ferrite has following several sintering processing on technique: the vacuum cool-down sintering, refer to after the Mn-Zn ferrite sintering cooling down in a vacuum, the method for balanced atmosphere when cooling with strict control prevents the redox of Mn-Zn ferrite; Nitrogen cooling sintering, refer at the nitrogen protection borehole cooling, and product in air after sintering, is protected coolingly immediately in nitrogen, until stop below 200 ℃, the purpose that passes into nitrogen is to reduce the oxygen partial pressure in stove, and the atmosphere in stove is maintained to equilibrium state; The quench hot sintering, refer to that Mn-Zn ferrite is after high temperature sintering, cooling rapidly, with high speed, by the temperature of easy oxygenolysis, reduces the degree of oxidation.But existing sintering technology does not obtain more optimal sintering process.
Therefore, for addressing the above problem, the spy provides a kind of new technical scheme to satisfy the demands.
Summary of the invention
The invention provides a kind of high magnetic conductivity ferrite sintering process.
The technical solution used in the present invention is:
The high magnetic conductivity ferrite sintering process comprises the following steps: heating step, fine and close step, incubation step and cooling step,
Heating step: ferrite is sent in bell jar type sintering furnace, and starting temperature is 50 ℃, and then the speed with 2 ~ 3 ℃/min heats up, at first ferrite is carried out to binder removal, and then adopt the air calcination method, and air content is between 20-22%, temperature is controlled at 1100 ℃;
Fine and close step: the scope control of oxygen level, between 3% ~ 4%, is continued to 2 ~ 3 hours densification time, and temperature is controlled at 1225 ~ 1350 ℃, in bell jar type sintering furnace, for maintaining malleation, guarantees at 1300Pa;
Incubation step: by Control for Oxygen Content, 4% ~ 5%, its oxygen level can be that the balanced atmosphere formula is LgPO by equilibrium relationship between temperature and oxygen level
2=-(14100 ~ 14150)/(t+273)+(7.0 ~ 7.2), obtain corresponding oxygen level, continues soaking time at 4 ~ 5 hours, and holding temperature is 1400 ℃, in bell jar type sintering furnace, for maintaining malleation, guarantees at 1300Pa;
Cooling step: adopt the less cooling method of cooling extent, cooling rate is controlled at 2 ~ 3 ℃/min, in bell jar type sintering furnace, for maintaining malleation, guarantees at 1300Pa, and its oxygen level can be balanced atmosphere formula: LgPO by equilibrium relationship between temperature and oxygen level
2=-(14100 ~ 14150)/(t+273)+(7.0 ~ 7.2), obtain corresponding oxygen level.
The invention has the beneficial effects as follows: the balanced atmosphere formula of sintering high magnetic conductivity ferrite can be adjusted flexibly for the ferrite of different ingredients, by theoretical balanced atmosphere formula, grope to find the sintering atmosphere that is applicable to high permeability MnZn ferrite and the relational expression of temperature through great many of experiments, can be better the sintering of the high permeability MnZn ferrite of different ingredients be done flexibly and adjusted, the balanced atmosphere that different temperature is corresponding relative, its advantage is exactly practical, flexible and changeable.
Embodiment
In order to deepen the understanding of the present invention, below in conjunction with embodiment, the invention will be further described, and this embodiment only, for explaining the present invention, does not form limiting the scope of the present invention.
Embodiment 1
The high magnetic conductivity ferrite sintering process comprises the following steps: heating step, fine and close step, incubation step and cooling step,
Heating step: ferrite is sent in bell jar type sintering furnace, and starting temperature is 50 ℃, and then the speed with 2 ℃/min heats up, and at first ferrite is carried out to binder removal, and then adopts the air calcination method, and air content is 20%, and temperature is controlled at 1100 ℃;
Fine and close step: oxygen level is 3%, continues the densification time 2 h, and temperature is controlled at 1225 ℃, in bell jar type sintering furnace, for maintaining malleation, guarantees at 1300Pa;
Incubation step: oxygen level is 4%, and its oxygen level can be that the balanced atmosphere formula is LgPO by equilibrium relationship between temperature and oxygen level
2=-(14100 ~ 14150)/(t+273)+(7.0 ~ 7.2), obtain corresponding oxygen level, continues soaking time at 4 hours, and holding temperature is 1400 ℃, in bell jar type sintering furnace, for maintaining malleation, guarantees at 1300Pa;
Cooling step: adopt the less cooling method of cooling extent, cooling rate is controlled at 2 ℃/min, in bell jar type sintering furnace, for maintaining malleation, guarantees at 1300Pa, and its oxygen level can be balanced atmosphere formula: LgPO by equilibrium relationship between temperature and oxygen level
2=-(14100 ~ 14150)/(t+273)+(7.0 ~ 7.2), obtain corresponding oxygen level, gets the A value and be 14120, the B value is 7.083, O in the time of t=1400 ℃
2%=4.39.
Embodiment 2
The high magnetic conductivity ferrite sintering process comprises the following steps: heating step, fine and close step, incubation step and cooling step,
Heating step: ferrite is sent in bell jar type sintering furnace, and starting temperature is 50 ℃, and then the speed with 3 ℃/min heats up, and at first ferrite is carried out to binder removal, and then adopts the air calcination method, and air content is 21%, and temperature is controlled at 1100 ℃;
Fine and close step: oxygen level is 3.5%, continues 2.5 hours densification time, and temperature is controlled at 1300 ℃, in bell jar type sintering furnace, for maintaining malleation, guarantees at 1300Pa;
Incubation step: oxygen level is 4.3%, and its oxygen level can be that the balanced atmosphere formula is LgPO by equilibrium relationship between temperature and oxygen level
2=-(14100 ~ 14150)/(t+273)+(7.0 ~ 7.2), obtain corresponding oxygen level, continues soaking time at 4.5 hours, and holding temperature is 1400 ℃, in bell jar type sintering furnace, for maintaining malleation, guarantees at 1300Pa;
Cooling step: adopt the less cooling method of cooling extent, cooling rate is controlled at 3 ℃/min, in bell jar type sintering furnace, for maintaining malleation, guarantees at 1300Pa, and its oxygen level can be balanced atmosphere formula: LgPO by equilibrium relationship between temperature and oxygen level
2=-(14100 ~ 14150)/(t+273)+(7.0 ~ 7.2), obtain corresponding oxygen level; Get the A value and be 14130, the B value is 7.094, O in the time of t=1100 ℃
2%=0.066.
Embodiment 3
The high magnetic conductivity ferrite sintering process comprises the following steps: heating step, fine and close step, incubation step and cooling step,
Heating step: ferrite is sent in bell jar type sintering furnace, and starting temperature is 50 ℃, and then the speed with 3 ℃/min heats up, and at first ferrite is carried out to binder removal, and then adopts the air calcination method, and air content is 22%, and temperature is controlled at 1100 ℃;
Fine and close step: the scope control of oxygen level, between 4%, is continued to 3 hours densification time, and temperature is controlled at 1350 ℃, in bell jar type sintering furnace, for maintaining malleation, guarantees at 1300Pa;
Incubation step: by Control for Oxygen Content, 5%, its oxygen level can be that the balanced atmosphere formula is LgPO by equilibrium relationship between temperature and oxygen level
2=-(14100 ~ 14150)/(t+273)+(7.0 ~ 7.2), obtain corresponding oxygen level, continues soaking time at 5 hours, and holding temperature is 1400 ℃, in bell jar type sintering furnace, for maintaining malleation, guarantees at 1300Pa;
Cooling step: adopt the less cooling method of cooling extent, cooling rate is controlled at 3 ℃/min, in bell jar type sintering furnace, for maintaining malleation, guarantees at 1300Pa, and its oxygen level can be balanced atmosphere formula: LgPO by equilibrium relationship between temperature and oxygen level
2=-(14100 ~ 14150)/(t+273)+(7.0 ~ 7.2), obtain corresponding oxygen level, gets the A value and be 14130, the B value is 7.078, O in the time of t=900 ℃
2%=0.0011.
Solid from the solid) ≒ S(of thermodynamics viewpoint S()+G(gas), during biphase-equilibrium, the pass of the pressure and temperature of gas phase is, LgP=-A/T+B, (14100 ~ 14150) in above-mentioned are the A values in balanced relationship, and because the T in balanced relationship is degree Fahrenheit, the transformational relation of itself and centigradetemperature t is (t+273), and (7.0 ~ 7.2) are the B values in relational expression, the amounts of pressurized gaseous in relational expression just refers to oxygen partial pressure PO in this technique
2.
The invention has the beneficial effects as follows: the balanced atmosphere formula of sintering high magnetic conductivity ferrite can be adjusted flexibly for the ferrite of different ingredients, by theoretical balanced atmosphere formula, grope to find the sintering atmosphere that is applicable to high permeability MnZn ferrite and the relational expression of temperature through great many of experiments, can be better the sintering of the high permeability MnZn ferrite of different ingredients be done flexibly and adjusted, the balanced atmosphere that different temperature is corresponding relative, its advantage is exactly practical, flexible and changeable.
Experimental data of the present invention:
Sintering high magnetic conductivity ferrite 10K, 12K product, tested the sample ring of sintering, wideband high magnetic conductivity ferrite 10K
Under the condition of 10 kHz, 0.08mA, 25 ℃ of test magnetic permeabilities of normal temperature are 11017;
Under the condition of 100 kHz, 0.08mA, 25 ℃ of test magnetic permeabilities of normal temperature are 11369;
Under the condition of 150kHz, 0.08mA, 25 ℃ of test magnetic permeabilities of normal temperature are 10845;
Under the condition of 200 kHz, 0.08mA, 25 ℃ of test magnetic permeabilities of normal temperature are 9994;
High magnetic conductivity ferrite 10K 25 ℃ of test magnetic permeabilities of normal temperature under the condition of 10 kHz, 0.08mA are 12720;
High magnetic conductivity ferrite 12K 25 ℃ of test magnetic permeabilities of normal temperature under the condition of 10 kHz, 0.08mA are 13606.
Claims (1)
1. high magnetic conductivity ferrite sintering process is characterized in that: comprise the following steps: heating step, fine and close step, incubation step and cooling step,
Described heating step: ferrite is sent in bell jar type sintering furnace, and starting temperature is 50 ℃, and then the speed with 2 ~ 3 ℃/min heats up, at first ferrite is carried out to binder removal, and then adopt the air calcination method, and air content is between 20-22%, temperature is controlled at 1100 ℃;
Described fine and close step: the scope control of oxygen level, between 3% ~ 4%, is continued to 2 ~ 3 hours densification time, and temperature is controlled at 1225 ~ 1350 ℃, in bell jar type sintering furnace, for maintaining malleation, guarantees at 1300Pa;
Described incubation step: by Control for Oxygen Content, 4% ~ 5%, its oxygen level can be that the balanced atmosphere formula is LgPO by equilibrium relationship between temperature and oxygen level
2=-(14100 ~ 14150)/(t+273)+(7.0 ~ 7.2), obtain corresponding oxygen level, continues soaking time at 4 ~ 5 hours, and holding temperature is 1400 ℃, in bell jar type sintering furnace, for maintaining malleation, guarantees at 1300Pa;
Described cooling step: adopt the less cooling method of cooling extent, cooling rate is controlled at 2 ~ 3 ℃/min, in bell jar type sintering furnace, for maintaining malleation, guarantees at 1300Pa, and its oxygen level can be balanced atmosphere formula: LgPO by equilibrium relationship between temperature and oxygen level
2=-(14100 ~ 14150)/(t+273)+(7.0 ~ 7.2), obtain corresponding oxygen level.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106747393A (en) * | 2016-11-15 | 2017-05-31 | 宝钢磁业（江苏）有限公司 | A kind of high-frequency and low-consumption Mn-Zn ferrite sintering process |
| CN107749345A (en) * | 2017-09-14 | 2018-03-02 | 重庆正峰电子有限公司 | The preparation method of SMD inductance core |
| CN109065346A (en) * | 2018-09-06 | 2018-12-21 | 宝钢磁业（江苏）有限公司 | A kind of technique improving the control of manganese-zinc ferrite sintering atmosphere |
| CN114085086A (en) * | 2021-11-02 | 2022-02-25 | 宝钢磁业（江苏）有限公司 | Sintering process of iron-rich ultrahigh Bs material |
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| CN101481243A (en) * | 2009-02-24 | 2009-07-15 | 上海大学 | Method for directly preparing MnZn ferrite material from nanocrystalline MnZn powder |
| JP2009173474A (en) * | 2008-01-22 | 2009-08-06 | Nec Tokin Corp | MANUFACTURING METHOD OF MnZn FERRITE HAVING HIGH MAGNETIC PERMEABILITY |
| CN102010192A (en) * | 2010-10-29 | 2011-04-13 | 宜宾金川电子有限责任公司 | Mangan zinc ferrite resintering process |
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Patent Citations (3)
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| JP2009173474A (en) * | 2008-01-22 | 2009-08-06 | Nec Tokin Corp | MANUFACTURING METHOD OF MnZn FERRITE HAVING HIGH MAGNETIC PERMEABILITY |
| CN101481243A (en) * | 2009-02-24 | 2009-07-15 | 上海大学 | Method for directly preparing MnZn ferrite material from nanocrystalline MnZn powder |
| CN102010192A (en) * | 2010-10-29 | 2011-04-13 | 宜宾金川电子有限责任公司 | Mangan zinc ferrite resintering process |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106747393A (en) * | 2016-11-15 | 2017-05-31 | 宝钢磁业（江苏）有限公司 | A kind of high-frequency and low-consumption Mn-Zn ferrite sintering process |
| CN107749345A (en) * | 2017-09-14 | 2018-03-02 | 重庆正峰电子有限公司 | The preparation method of SMD inductance core |
| CN109065346A (en) * | 2018-09-06 | 2018-12-21 | 宝钢磁业（江苏）有限公司 | A kind of technique improving the control of manganese-zinc ferrite sintering atmosphere |
| CN114085086A (en) * | 2021-11-02 | 2022-02-25 | 宝钢磁业（江苏）有限公司 | Sintering process of iron-rich ultrahigh Bs material |
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