CN109065346A - A kind of technique improving the control of manganese-zinc ferrite sintering atmosphere - Google Patents

A kind of technique improving the control of manganese-zinc ferrite sintering atmosphere Download PDF

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CN109065346A
CN109065346A CN201811035259.4A CN201811035259A CN109065346A CN 109065346 A CN109065346 A CN 109065346A CN 201811035259 A CN201811035259 A CN 201811035259A CN 109065346 A CN109065346 A CN 109065346A
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air
air inlet
flow
nitrogen
oxygen content
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张金龙
沈琪平
徐青青
井威
赵林风
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Baosteel Magnetics (jiangsu) Co Ltd
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    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
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    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
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    • C01G49/0072—Mixed oxides or hydroxides containing manganese
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    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
    • C04B35/2658—Other ferrites containing manganese or zinc, e.g. Mn-Zn ferrites
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    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6565—Cooling rate
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658—Atmosphere during thermal treatment
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658—Atmosphere during thermal treatment
    • C04B2235/6583—Oxygen containing atmosphere, e.g. with changing oxygen pressures
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658—Atmosphere during thermal treatment
    • C04B2235/6586—Processes characterised by the flow of gas

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  • Soft Magnetic Materials (AREA)

Abstract

The technique that the present invention discloses a kind of raising manganese-zinc ferrite sintering atmosphere control, which comprises the following steps: air mass flow air inlet section: ferrite is sent in bell jar type sintering furnace, is sintered heating, then dumping, then heat up, air calcination；Nitrogen big flow air inlet densification section: being sintered heating densification, and total air inflow is arranged in oxygen content 0%, controls temperature, nitrogen air inlet, interior bell jar type sintering furnace is to maintain positive pressure；Air mass flow and nitrogen big flow match air inlet section: sintered heat insulating, control oxygen content, total air inflow is arranged, and keep the temperature, and manganese-zinc ferrite carries out sufficient solid phase reaction in the section；Air mass flow and nitrogen big flow match air inlet, are to maintain positive pressure in bell jar type sintering furnace；The small flow of air and nitrogen big flow match air inlet section: sintering cools down.Control climate precision is promoted, flexibly adjustment air inlet proportion is carried out for the manganese-zinc ferrite of different performance, avoids because of the final ferrite sintered result of the influences such as air pressure, flow.

Description

A kind of technique improving the control of manganese-zinc ferrite sintering atmosphere
Technical field
The present invention relates to a kind of techniques of raising manganese-zinc ferrite sintering atmosphere control.
Background technique
As world manganese-zinc ferrite industry center is shifted to the Asian-Pacific area, China's manganese-zinc ferrite industry has been obtained quickly Development, after semicentennial research and application, people already are familiar with manganese-zinc ferrite with spinel structure, closely packed oxygen Tetrahedron and octahedral interstice are formed in ion cubic lattice, due to cation distribution situation and interionic interaction situation Diversity and complexity, make manganese-zinc ferrite have electromagnetic property abundant, and system is varied and controlled in adjustment component proportion appropriate Its structural behaviour can be then transformed in Preparation Method and condition, but same under when preparation condition again, how to mention to greatest extent The electromagnetic performance of manganese-zinc ferrite is risen, therefore, sintering condition control is that have the technique ring for determining to influence to manganese-zinc ferrite performance Section.
Still there is certain gap since the performance of domestic ferrite sintered equipment is relatively external, and manganese-zinc ferrite is to sintering furnace Temperature and atmosphere control require it is again very high, therefore, to use the agglomerating plant of domestic manganese-zinc ferrite go research and development with The quite even more good material of external manganese-zinc ferrite performance, it is necessary to which our R&D workers open up thinking, seek more to have The development approach of effect and better method of production, there are many burning factor for influencing manganese-zinc ferrite performance, this patent mainly for The problem of sintering atmosphere controls.
Therefore, to solve this problem, a kind of technique of raising manganese-zinc ferrite sintering atmosphere control is provided.
Summary of the invention
To solve the above-mentioned problems, the invention discloses a kind of techniques of raising manganese-zinc ferrite sintering atmosphere control.
The technical solution of the present invention is as follows: a kind of technique for improving the control of manganese-zinc ferrite sintering atmosphere, comprising the following steps: Air mass flow air inlet section, nitrogen big flow air inlet densification section, air mass flow and nitrogen big flow match air inlet section, air Small flow and nitrogen big flow match air inlet section；
Air mass flow air inlet section: ferrite is sent in bell jar type sintering furnace, and the locating sintering temperature rise period, oxygen content is Between 20-21%, total air inflow 100-300Nl/min is set；50 DEG C of warming temperature of starting carries out dumping to ferrite；Temperature liter To 800 ~ 1000 DEG C, carry out air calcination, air inlet control air mass flow 100-300Nl/min(nitrogen flow be 0), air into Atmospheric pressure 0.4-0.55Mpa；
Nitrogen big flow air inlet densifies section: total air inflow 100- is arranged in locating sintering heating densification stage, oxygen content 0% 200Nl/min, temperature, which controls, squeezes away the oxygen absorbed by nitrogen, so that crystal grain increases cause rapidly Close, nitrogen big flow 100-200Nl/min(air/oxygen flow is that 0), nitrogen admission pressure 0.4-0.55Mpa, bell-jar is burnt To maintain positive pressure in freezing of a furnace, guarantee in 1100Pa-1300Pa；
Air mass flow and nitrogen big flow match air inlet section: locating sintered heat insulating stage, for the manganese-zinc ferrite of different performance Total air inflow 100-200Nl/min is arranged by its Control for Oxygen Content in 4-8% in body, and holding temperature is 1250 DEG C ~ 1380 DEG C, Manganese-zinc ferrite carries out sufficient solid phase reaction in the section；Air mass flow and nitrogen big flow match air inlet, the i.e. big stream of air Measure the oxygen content 21% in Nl/min=(oxygen content % × total air inflow Nl/min)/air, nitrogen big flow Nl/min=always into Tolerance Nl/min- air mass flow Nl/min；Nitrogen is consistent with air inlet pressure, and control is burnt in 0.4-0.55Mpa, bell-jar To maintain positive pressure in freezing of a furnace, guarantee in 1100Pa-1300Pa；
The small flow of air and nitrogen big flow match air inlet section: locating sintering temperature-fall period, oxygen content are contained by temperature and oxygen Equilibrium relation between amount, i.e. balanced atmosphere formula are LgPO2=-(13400 ~ 14200)/(T+273)+(7.0 ~ 7.2), obtain phase The oxygen content answered, is arranged total air inflow 100-200Nl/min, cools down 1300-1380 DEG C of initial temperature, cooling rate control 2 ~ 3 DEG C/min, the small flow of air and nitrogen big flow match air inlet, this section of demand oxygen content is reduced with the reduction of temperature, use The small flow air inlet of air is to guarantee the accuracy of Control for Oxygen Content；That is the small flow Nl/min of air=(oxygen content % × total air inflow Nl/min the oxygen content 21% in)/air, the nitrogen big flow Nl/min=small flow Nl/min of total air inflow Nl/min- air； Nitrogen is consistent with air inlet pressure, and control, to maintain positive pressure, guarantees in 0.4-0.55Mpa, bell jar type sintering furnace 1100Pa-1300Pa。
Usefulness of the present invention: large and small in the air that accurate control atmosphere is added in each stage of original sintering process Flow air inlet control, the control of nitrogen big flow promote the control climate precision in each stage, and can be directed to the manganese of different performance Zn ferrite carries out flexibly adjustment air inlet proportion, avoids because the factors such as air pressure, flow influence final ferrite sintered result. For this patent compared with original sintering process, the Control for Oxygen Content in sintering atmosphere is more accurate, the air inlet control of large and small air mass flow System, guarantees more acurrate in high and low Control for Oxygen Content, avoids because of partial pressure of oxygen PO2Excessively high, ferrous ion is reduced, and is unfavorable for manganese Zn ferrite anisotropy (K1) reduction, magnetic conductivity reduce；Partial pressure of oxygen PO2Too low, ferrous ion increases, and leads to ferrous iron Ion is unfavorable for manganese-zinc ferrite anisotropy (K to ferric ion electron transfer1) reduction, reduce magnetic conductivity, material electricity The problem of resistance rate decline, high-frequency loss steeply rises.
Specific embodiment
In order to deepen the understanding of the present invention, the present invention will be described in further detail with reference to the examples below, the embodiment For explaining only the invention, it is not intended to limit the scope of the present invention..
Embodiment 1
A kind of technique improving the control of manganese-zinc ferrite sintering atmosphere, including with the next stage: air mass flow air inlet section, nitrogen are big Flow air inlet densifies section, air mass flow and nitrogen big flow proportion air inlet section, the small flow of air and nitrogen big flow and matches Air inlet section；
Air mass flow air inlet section: ferrite is sent in bell jar type sintering furnace, and the locating sintering temperature rise period, oxygen content is Between 20%, total air inflow 100Nl/min is set；50 DEG C of warming temperature of starting carries out dumping to ferrite；Temperature rises to 800 DEG C, air calcination is carried out, it is 0) air inlet pressure 0.4Mpa that air inlet, which controls air mass flow 100Nl/min(nitrogen flow,；
Nitrogen big flow air inlet densifies section: total air inflow is arranged in locating sintering heating densification stage, oxygen content 0% 100Nl/min, temperature, which controls, squeezes away the oxygen absorbed by nitrogen, so that crystal grain increases densification, nitrogen rapidly Big flow 100Nl/min(air/oxygen flow is 0) nitrogen admission pressure 0.4Mpa, is to maintain just in bell jar type sintering furnace Pressure, guarantees in 1100Pa；
Air mass flow and nitrogen big flow match air inlet section: locating sintered heat insulating stage, for the manganese-zinc ferrite of different performance Total air inflow 100Nl/min is arranged by its Control for Oxygen Content 4% in body, and holding temperature is 1250 DEG C, and manganese-zinc ferrite is at this The sufficient solid phase reaction of Duan Jinhang；Air mass flow and nitrogen big flow match air inlet, i.e. air mass flow Nl/min=19Nl/ Min, nitrogen big flow Nl/min=81Nl/min；Nitrogen is consistent with air inlet pressure, and control is in 0.4Mpa, bell-jar sintering To maintain positive pressure in furnace, guarantee in 1100Pa；
The small flow of air and nitrogen big flow match air inlet section: locating sintering temperature-fall period, oxygen content are contained by temperature and oxygen Equilibrium relation between amount, i.e. balanced atmosphere formula are LgPO2=-(13400)/(T+273)+(7.0), obtain corresponding oxygen content 1.6%, total air inflow 100Nl/min is set, is cooled down 1300 DEG C of initial temperature, cooling rate is controlled in 2 DEG C/min, the small stream of air Amount matches air inlet with nitrogen big flow, this section of demand oxygen content reduce with the reduction of temperature, using the small flow air inlet of air with Guarantee the accuracy of Control for Oxygen Content；That is the small flow Nl/min=7.6Nl/min of air, nitrogen big flow Nl/min=92.4Nl/ min；Nitrogen is consistent with air inlet pressure, and control, to maintain positive pressure, guarantees in 0.4Mpa, bell jar type sintering furnace 1100PaPa。
Embodiment 2
A kind of technique improving the control of manganese-zinc ferrite sintering atmosphere, including with the next stage: air mass flow air inlet section, nitrogen are big Flow air inlet densifies section, air mass flow and nitrogen big flow proportion air inlet section, the small flow of air and nitrogen big flow and matches Air inlet section；
Air mass flow air inlet section: ferrite is sent in bell jar type sintering furnace, and the locating sintering temperature rise period, oxygen content is Between 20.5%, total air inflow 200Nl/min is set；50 DEG C of warming temperature of starting carries out dumping to ferrite；Temperature rises to 900 DEG C, air calcination is carried out, it is 0) air inlet pressure 0.5Mpa that air inlet, which controls air mass flow 200Nl/min(nitrogen flow,；
Nitrogen big flow air inlet densifies section: total air inflow is arranged in locating sintering heating densification stage, oxygen content 0% 150Nl/min, temperature, which controls, squeezes away the oxygen absorbed by nitrogen, so that crystal grain increases densification, nitrogen rapidly Big flow 150Nl/min(air/oxygen flow is 0) nitrogen admission pressure 0.5Mpa, is to maintain just in bell jar type sintering furnace Pressure, guarantees in 1200Pa；
Air mass flow and nitrogen big flow match air inlet section: locating sintered heat insulating stage, for the manganese-zinc ferrite of different performance Total air inflow 150Nl/min is arranged by its Control for Oxygen Content 6% in body, and holding temperature is 1300 DEG C, and manganese-zinc ferrite is at this The sufficient solid phase reaction of Duan Jinhang；Air mass flow and the proportion air inlet of nitrogen big flow, i.e. air mass flow Nl/min= 42.8Nl/min, nitrogen big flow Nl/min=107.2Nl/min；Nitrogen is consistent with air inlet pressure, controls in 0.5Mpa, To maintain positive pressure in bell jar type sintering furnace, guarantee in 1200Pa；
The small flow of air and nitrogen big flow match air inlet section: locating sintering temperature-fall period, oxygen content are contained by temperature and oxygen Equilibrium relation between amount, i.e. balanced atmosphere formula are LgPO2=-(13900)/(T+273)+(7.1), obtain corresponding oxygen content 0.8%, total air inflow 150Nl/min is set, is cooled down 1350 DEG C of initial temperature, cooling rate is controlled in 2.5 DEG C/min, and air is small Flow and nitrogen big flow match air inlet, this section of demand oxygen content is reduced with the reduction of temperature, use the small flow air inlet of air To guarantee the accuracy of Control for Oxygen Content；That is the small flow Nl/min=5.7Nl/min of air, nitrogen big flow Nl/min= 144.3Nl/min；Nitrogen is consistent with air inlet pressure, and control maintains positive pressure in 0.5Mpa, bell jar type sintering furnace, guarantees In 1200Pa.
Embodiment 3
A kind of technique improving the control of manganese-zinc ferrite sintering atmosphere, including with the next stage: air mass flow air inlet section, nitrogen are big Flow air inlet densifies section, air mass flow and nitrogen big flow proportion air inlet section, the small flow of air and nitrogen big flow and matches Air inlet section；
Air mass flow air inlet section: ferrite is sent in bell jar type sintering furnace, and the locating sintering temperature rise period, oxygen content is Between 21%, total air inflow 300Nl/min is set；50 DEG C of warming temperature of starting carries out dumping to ferrite；Temperature rises 1000 DEG C, Air calcination is carried out, it is 0) air inlet pressure 0.55Mpa that air inlet, which controls air mass flow 300Nl/min(nitrogen flow,；
Nitrogen big flow air inlet densifies section: total air inflow is arranged in locating sintering heating densification stage, oxygen content 0% 200Nl/min, temperature, which controls, squeezes away the oxygen absorbed by nitrogen, so that crystal grain increases densification, nitrogen rapidly Big flow 200Nl/min(air/oxygen flow is 0) nitrogen admission pressure 0.55Mpa, is to maintain just in bell jar type sintering furnace Pressure, guarantees in 1300Pa；
Air mass flow and nitrogen big flow match air inlet section: locating sintered heat insulating stage, for the manganese-zinc ferrite of different performance Total air inflow 200Nl/min is arranged by its Control for Oxygen Content 8% in body, and holding temperature is 1380 DEG C, and manganese-zinc ferrite is at this The sufficient solid phase reaction of Duan Jinhang；Air mass flow and the proportion air inlet of nitrogen big flow, i.e. air mass flow Nl/min= 76.2Nl/min, nitrogen big flow Nl/min=123.8Nl/min；Nitrogen is consistent with air inlet pressure, controls in 0.55Mpa, To maintain positive pressure in bell jar type sintering furnace, guarantee in 1300Pa；
The small flow of air and nitrogen big flow match air inlet section: locating sintering temperature-fall period, oxygen content are contained by temperature and oxygen Equilibrium relation between amount, i.e. balanced atmosphere formula are LgPO2=-(14200)/(T+273)+(7.2), obtain corresponding oxygen content 0.1%, total air inflow 200Nl/min is set, is cooled down 1380 DEG C of initial temperature, cooling rate is controlled in 3 DEG C/min, the small stream of air Amount matches air inlet with nitrogen big flow, this section of demand oxygen content reduce with the reduction of temperature, using the small flow air inlet of air with Guarantee the accuracy of Control for Oxygen Content；That is the small flow Nl/min=1Nl/min of air, nitrogen big flow Nl/min=199Nl/min； Nitrogen is consistent with air inlet pressure, and control, to maintain positive pressure, guarantees in 1300Pa in 0.55Mpa, bell jar type sintering furnace.
Air mass flow air inlet section: enhancing is evaded because charge flow rate fluctuates to air flow control, dumping is caused not fill The problems such as dividing, cracking；Nitrogen big flow air inlet densifies section: control of the enhancing to oxygen content guarantees that nitrogen charge flow rate is full of In furnace, Control for Oxygen Content is 0%；Air mass flow and nitrogen big flow match air inlet section: control of the enhancing to oxygen content guarantees Nitrogen air inlet and the control accurate in scale of air inlet amount guarantee control oxygen content in required controlling value；The small flow of air and nitrogen Big flow match air inlet section: temperature descending section is more sensitive to the control of oxygen content, using the small discharge matching nitrogen big flow of air into Gas, it is ensured that Control for Oxygen Content keeps oxygen content to stablize in lesser value.
In conclusion this patent, compared with original sintering process, the Control for Oxygen Content in sintering atmosphere is more accurate, big, The air inlet of small air mass flow controls, and guarantees more acurrate in high and low Control for Oxygen Content, avoids because of partial pressure of oxygen PO2It is excessively high, ferrous iron Ion is reduced, and is unfavorable for manganese-zinc ferrite anisotropy (K1) reduction, magnetic conductivity reduce；Partial pressure of oxygen PO2It is too low, ferrous iron from Son increases, and causes ferrous ion to ferric ion electron transfer, is unfavorable for manganese-zinc ferrite anisotropy (K1) reduction, The problem of reduction magnetic conductivity, resistivity of material decline, high-frequency loss steeply rises.

Claims (1)

1. a kind of technique for improving the control of manganese-zinc ferrite sintering atmosphere, which comprises the following steps: air mass flow Air inlet section, nitrogen big flow air inlet densification section, air mass flow and nitrogen big flow proportion air inlet section, the small flow of air and nitrogen Gas big flow matches air inlet section；
The air mass flow air inlet section: ferrite is sent in bell jar type sintering furnace, the locating sintering temperature rise period, oxygen content For 20-21%, total air inflow 100-300Nl/min is set；50 DEG C of warming temperature of starting carries out dumping to ferrite；Temperature rises to 800 ~ 1000 DEG C, air calcination is carried out, it is 0) air inlet that air inlet, which controls air mass flow 100-300Nl/min(nitrogen flow, Pressure 0.4-0.55Mpa；
The nitrogen big flow air inlet densifies section: total air inflow is arranged in locating sintering heating densification stage, oxygen content 0% 100-200Nl/min, temperature control are in 1100 ~ 1250 DEG C, nitrogen big flow 100-200Nl/min(air/oxygen flow 0), nitrogen admission pressure 0.4-0.55Mpa, bell jar type sintering furnace is interior to maintain positive pressure, guarantees in 1100Pa-1300Pa；
The air mass flow and nitrogen big flow match air inlet section: locating sintered heat insulating stage, by its Control for Oxygen Content in 4- 8%, total air inflow 100-200Nl/min is set, and holding temperature is 1250 DEG C ~ 1380 DEG C, and manganese-zinc ferrite is filled in the section The solid phase reaction divided；Air mass flow and nitrogen big flow match air inlet, i.e. air mass flow Nl/min=(oxygen content % × always into Tolerance Nl/min) oxygen content 21% in/air, nitrogen big flow Nl/min=total air inflow Nl/min- air mass flow Nl/ min；Nitrogen is consistent with air inlet pressure, and control, to maintain positive pressure, guarantees in 0.4-0.55Mpa, bell jar type sintering furnace 1100Pa-1300Pa；
The small flow of air and nitrogen big flow match air inlet section: locating sintering temperature-fall period, oxygen content by temperature with Equilibrium relation between oxygen content, i.e. balanced atmosphere formula are LgPO2=-(13400 ~ 14200)/(T+273)+(7.0 ~ 7.2), it obtains Corresponding oxygen content is obtained, total air inflow 100-200Nl/min is set, is cooled down 1300-1380 DEG C of initial temperature, cooling rate control In 2 ~ 3 DEG C/min；That is the oxygen content 21% in the small flow Nl/min of air=(oxygen content % × total air inflow Nl/min)/air, The nitrogen big flow Nl/min=small flow Nl/min of total air inflow Nl/min- air；Nitrogen is consistent with air inlet pressure, control To maintain positive pressure in 0.4-0.55Mpa, bell jar type sintering furnace, guarantee in 1100Pa-1300Pa.
CN201811035259.4A 2018-09-06 2018-09-06 A kind of technique improving the control of manganese-zinc ferrite sintering atmosphere Pending CN109065346A (en)

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Cited By (2)

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Publication number Priority date Publication date Assignee Title
CN110256089A (en) * 2019-06-12 2019-09-20 湖南艾迪奥电子科技有限公司 A kind of magnetic ferrite magnetic core and its sintering method
CN112679217A (en) * 2021-01-14 2021-04-20 临沂银凤新材料技术服务有限公司 Novel power type sintering process for soft magnetic ferrite

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Application publication date: 20181221