CN104129980A - Low-sintering-temperature soft magnetic ferrite material and preparation method thereof - Google Patents

Low-sintering-temperature soft magnetic ferrite material and preparation method thereof Download PDF

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Publication number
CN104129980A
CN104129980A CN201410320152.XA CN201410320152A CN104129980A CN 104129980 A CN104129980 A CN 104129980A CN 201410320152 A CN201410320152 A CN 201410320152A CN 104129980 A CN104129980 A CN 104129980A
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soft magnetic
magnetic ferrite
preparation
ferrite
major ingredient
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CN201410320152.XA
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张祖军
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NINGBO HAISHU OSTCORE ELECTRONICS Co Ltd
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NINGBO HAISHU OSTCORE ELECTRONICS Co Ltd
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Abstract

The invention discloses a low-sintering-temperature soft magnetic ferrite material. The formula of the soft magnetic ferrite material comprises main materials and an auxiliary material. The soft magnetic ferrite material is characterized in that the main materials comprise 51-63 mole percent of Fe2O3, 25-35 mole percent of ZnO, 6-9 mole percent of Li2CO3, 0-7 mole percent of TiO2 and 0-3.0 mole percent of MnCO3; and the auxiliary material is Bi2O3, and the adding amount of the auxiliary material is 0.4-1.2 percent based on the total weight of the main materials. The auxiliary material is pelletized, molded and sintered together with the main materials after the main materials are burdened, mixed and pre-sintered. The soft magnetic ferrite material disclosed by the invention has excellent high-frequency performance like nickel-zinc ferrite, and the performance of the soft magnetic ferrite material is approximate to that of a nickel-zinc material. The comprehensive costs of various compounds in main components are lower than the nickel-zinc material. The sintering temperature of the soft magnetic ferrite material is 100-200 DEG C lower than that of an ordinary nickel-zinc material, and the soft magnetic ferrite material has very high economical efficiency on the aspect of energy consumption.

Description

A kind of sintering temperature and low soft magnetic ferrite and preparation method thereof
Technical field
The present invention relates to a kind of soft magnetic ferrite and preparation method thereof.
Background technology
At present conventional soft magnetic ferrite mainly contains that these are several: Mn-Zn ferrite, nickel-zinc ferrite and MgZn ferrite.The magnetic permeability scope of MnZn ferrite material is μ i=1000-15000, electricalresistivityρ is lower, only has 1-1000 Ω cm, and the limiting frequency of magnetic permeability only has hundreds of kilohertz, and the sintering temperature of material is between 1300 DEG C-1450 DEG C.This material is mainly used in making the electron devices such as inducer, transformer, wave filter and reactance coil.
The magnetic permeability μ of nickel Zinc material inot high, conventionally between 10-1000, but its resistivity is very high, more than can reaching 10M Ω cm, is an isolator substantially, and the limiting frequency of magnetic permeability is more than the megahertz order of magnitude.The sintering temperature of material is 1000 DEG C-1200 DEG C, and this material is mainly used in the occasion that frequency ratio is higher, such as absorbing high-frequency electromagnetic interference signal, to reach anti-electromagnetic interference object.
The magnetic permeability of MgZn ferrite material is close with nickel Zinc material, and frequency of utilization and resistivity are all lower than nickel Zinc material, but because the magnesium in its principal constituent is more much lower than nickel cost, can partly replace nickel-zinc ferrite to use in less demanding occasion.
Li ferrite is typically used as microwave material, if Chinese Patent Application No. is 200910106919.8 disclosed " a kind of lithium ferrite materials that are applied to C-band phase shifter and preparation method thereof ", C-band is the one section frequency band of frequency from 4.0GHz-8.0GHz, as the frequency range of the capable transmission signal of telstar, this material is for Phased Array Radar Antenna.Also just like Chinese Patent Application No. 200810015096.3 disclosed " a kind of Li ferrite electric wave absorbing materials and preparation method thereof ", effective absorption ripple frequency span of this material is 1.3GHz, but lithium-zinc-ferrite as soft magnetic ferrite but few people mention.
Also there is a kind of nickel-copper-zinc ferrite (NiCuZn) material of sintering temperature and low, sometimes be called for short nickel zinc (NiZn) material, as disclosed in Chinese Patent Application No. 200610052525.5 " nickel zinc ferrite low temperature high density production method and finished product thereof ", its disclosed sintering temperature is 880 DEG C-980 DEG C, but this material has added outside the CuO of 3-3.5wt% in main material, also needing to add six kinds of subsidiary material realizes, material mixture ratio is more complex by contrast, and the comprehensive cost of material is also higher.
Summary of the invention
Technical problem to be solved by this invention is to provide soft magnetic ferrite that a kind of sintering temperature is lower, cost is lower and easy to make and preparation method thereof.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of sintering temperature and low soft magnetic ferrite, its formula comprises major ingredient and auxiliary material, it is characterized in that: described major ingredient comprises Fe 2o 3for 51-63mol%, ZnO is 25-35mol%, Li 2cO 3for 6-9mol%, TiO 2for 0-7mol%, MnCO 3for 0-3.0mol%; Described auxiliary material is Bi 2o 3, its add-on accounts for the 0.4%-1.2% of major ingredient gross weight.
Preferably, described auxiliary material accounts for the 0.6%-1.0% of major ingredient gross weight.
The preparation method of above-mentioned soft magnetic ferrite, after evenly being mixed, major ingredient carries out presintering, cooling after the insulation of calcined temperature point, then auxiliary material is added and is ground into together powder, add a certain proportion of binding agent, by powder granulation magnetic, then particle magnetic is pressed into magnetic core with mould by flouring technology, magnetic core after moulding sintering in stove, cooling after the insulation of sintering temperature point.
Preferably, the calcined temperature of described major ingredient is 650 DEG C-750 DEG C, is incubated cool to room temperature after 2-4 hour.
Preferably, described calcined temperature is 700 DEG C.
Preferably, to be pressed into the required pressure of magnetic core be 1.5-2.0 ton/cm to described mould 2.
Preferably, the sintering temperature of described magnetic core is 900 DEG C-1000 DEG C.
Preferably, described magnetic core is at sintering temperature point insulation 2-4 hour.
Compared with prior art, the invention has the advantages that soft magnetic ferrite of the present invention, the same with nickel-zinc ferrite have a good high frequency performance, properties approaches with nickel Zinc material, and the comprehensive cost of various compounds is lower than nickel Zinc material in principal constituent, sintering temperature, more than the common low 100-200 DEG C of nickel Zinc material, has good economy aspect energy consumption.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Sintering temperature and low soft magnetic ferrite of the present invention, using lithium ferrite material as essentially consist, the good high frequency performance that lithium-zinc-ferrite material has itself, more than operating frequency can reach 300MHz, this material is the same with nickel-zinc ferrite has good high frequency performance, properties also approaches with nickel-zinc-ferrite material, but sintering temperature is lower 100 DEG C-200 DEG C than common nickel-zinc-ferrite material, and comprehensive cost is also lower.
The formula of sintering temperature and low soft magnetic ferrite of the present invention, comprises major ingredient and auxiliary material, and wherein major ingredient and per-cent composition thereof are: Fe 2o 3for 51-63mol%, ZnO is 25-35mol%, Li 2cO 3for 6-9mol%, TiO 2for 0-7mol%, MnCO 3for 0-3.0mol%, auxiliary material is Bi 2o 3, its add-on accounts for the 0.4%-1.2% of major ingredient total weight percent, i.e. 0.4-1.2wt%.
Its preparation method is as described below: above-mentioned major ingredient carries out presintering after evenly mixing, and calcined temperature is 650-750 DEG C, and best calcined temperature is 700 DEG C, and cool to room temperature after calcined temperature point is incubated 2-4 hour, completes pre-burning operation.
In major ingredient after pre-burning completes, add in proportion auxiliary material, with disintegrating apparatus as ball mill or sand mill etc., major ingredient and auxiliary material are pulverized to formation powder, the diameter of powder is approximately 1 μ m-10 μ m, then in the powder after pulverizing, add for example PVA solution of a certain amount of caking agent, the concentration of PVA solution is approximately 10%, the weight that the add-on of PVA solution is converted to PVA solid accounts for the 1%-1.5% of powder weight, powder evenly mixes after adding PVA solution, with powder manufacturing apparatus granulation magnetic, particle magnetic is pressed into various required magnetic cores with mould, the required pressure of form forming magnetic core is 1500-2000kg/cm 2, i.e. 1.5-2.0 ton/cm 2, the magnetic core after moulding is used air atmosphere sintering in stove, and sintering temperature is 900 DEG C-1000 DEG C, and at sintering temperature point insulation 2-4 hour, then cool to room temperature, takes out magnetic core, so just can test every magnetic property of magnetic core.Be that auxiliary material adds after batching, batch mixing, pre-burning at major ingredient, then with major ingredient pulverizing together, granulation, moulding and sintering.The effect of auxiliary material is as fusing assistant, reduces the sintering temperature of material and the body resistivity of increase material.
For the present invention, mainly test magnetic permeability μ i, body resistivity ρ, Curie temperature Tc, the saturation magnetic flux density Bs of magnetic core, these parameters are basic parameters of soft magnetic ferrite.As shown in table 1 below, in table, the sintering temperature of soft magnetic ferrite is Ts=975 DEG C, Bi 2o 3content is 0.8wt%.
Table 1
The embodiment that table 1 is principal constituent of the present invention, by seeing in table 1, according to the difference of principal constituent, can obtain magnetic permeability scope is that μ i=200-1000, Curie temperature scope are Tc=100-350 DEG C of soft magnetic ferrite, in actually operating, difference that can be according to requirements, such as the occasion having needs low magnetic permeability, some demand high magnetic permeabilities, thereby select different material prescriptions to achieve the goal, in general, the material that magnetic permeability is high, Curie temperature is relatively lower.
Auxiliary material B i 2o 3there is the effect of two aspects, the effect of the first fusing assistant, it makes ferrite complete solid state reaction at lower temperature, accelerates densification process, and sintering temperature and low also helps and suppresses the lower Li of high temperature (approximately 1100 DEG C) 2the volatilization of O, stops Fe 2+formation, thereby increase resistivity.The second, bismuth (Bi) element forms resistive formation at the intergranule of Li ferrite, and this is Bi 2o 3the Another reason that resistivity is increased.Table 2 is Bi in Li ferrite 2o 3add-on with the relation of resistivity and magnetic permeability, wherein sintering temperature be=950 DEG C, and removes Bi 2o 3outward, other compositions keep fixing.
Table 2
Although the increase of bismuth is favourable to improving resistivity, too much bismuth makes material become more crisp, affects practical effect, therefore, preferably, Bi 2o 3add-on be controlled between 0.6-1.0wt% and be advisable.
In the case of the composition of major ingredient and auxiliary material is fixing, sintering temperature Ts is higher, and magnetic permeability is also higher, as shown in table 3.
Table 3
But high sintering temperature can make resistivity decline, table 4 is the relation that sintering temperature Ts follows magnetic permeability μ i, electricalresistivityρ, has selected the changing conditions of several formulas magnetic permeability and resistivity under different sintering temperatures in this table.Although it is favourable to improving magnetic permeability to improve sintering temperature, resistivity declines, and considers the practicality of magnetic core and the economy of real cost of production, and optimal sintering temperature is 900-1000 DEG C.
Table 4
The present invention has made a kind of soft magnetism lithium titanium Zinc ferrite material, operating frequency is the highest can reach 300MHz, this material is the same with nickel-zinc ferrite has good high frequency performance, properties approaches with nickel Zinc material, and the comprehensive cost of various compounds is lower than nickel Zinc material in principal constituent, sintering temperature, than the common low 100-200 DEG C of nickel Zinc material, has good economy aspect energy consumption.
Although more than described the preferred embodiments of the present invention in detail, should be expressly understood that, for a person skilled in the art, the present invention can have various modifications and variations.All any amendments of doing within the spirit and principles in the present invention, be equal to replacement, improvement etc., within protection scope of the present invention all should be included in.

Claims (8)

1. a sintering temperature and low soft magnetic ferrite, its formula comprises major ingredient and auxiliary material, it is characterized in that: described major ingredient comprises Fe 2o 3for 51-63mol%, ZnO is 25-35mol%, Li 2cO 3for 6-9mol%, TiO 2for 0-7mol%, MnCO 3for 0-3.0mol%; Described auxiliary material is Bi 2o 3, its add-on accounts for the 0.4%-1.2% of major ingredient gross weight.
2. soft magnetic ferrite as claimed in claim 1, is characterized in that: described auxiliary material accounts for the 0.6%-1.0% of major ingredient gross weight.
3. the preparation method of the soft magnetic ferrite as described in claim 1-2, it is characterized in that: after major ingredient is evenly mixed, carry out presintering, cooling after the insulation of calcined temperature point, then auxiliary material is added and is ground into together powder, add a certain proportion of binding agent, by powder granulation magnetic, then particle magnetic is pressed into magnetic core with mould by flouring technology, magnetic core after moulding sintering in stove, cooling after the insulation of sintering temperature point.
4. the preparation method of soft magnetic ferrite as claimed in claim 3, is characterized in that: the calcined temperature of described major ingredient is 650 DEG C-750 DEG C, is incubated cool to room temperature after 2-4 hour.
5. the preparation method of soft magnetic ferrite as claimed in claim 4, is characterized in that: described calcined temperature is 700 DEG C.
6. the preparation method of soft magnetic ferrite as claimed in claim 3, is characterized in that: it is 1.5-2.0 ton/cm that described mould is pressed into the required pressure of magnetic core 2.
7. the preparation method of soft magnetic ferrite as claimed in claim 3, is characterized in that: the sintering temperature of described magnetic core is 900 DEG C-1000 DEG C.
8. the preparation method of soft magnetic ferrite as claimed in claim 3, is characterized in that: described magnetic core is at sintering temperature point insulation 2-4 hour.
CN201410320152.XA 2014-07-07 2014-07-07 Low-sintering-temperature soft magnetic ferrite material and preparation method thereof Pending CN104129980A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104891975A (en) * 2015-04-24 2015-09-09 马鞍山科信咨询有限公司 High flexural strength nickel-zinc soft magnetic ferrite material and preparation method thereof
CN104891979A (en) * 2015-04-24 2015-09-09 马鞍山科信咨询有限公司 Wide temperature magnesium copper zinc soft magnetic ferrite magnetic core and preparation method thereof
CN104891982A (en) * 2015-04-24 2015-09-09 马鞍山科信咨询有限公司 Rare earth high-magnetic-permeability soft magnetic ferrite and preparation method thereof
CN106747481A (en) * 2016-12-15 2017-05-31 上海宝钢磁业有限公司 A kind of large scale magnetic core feed powder and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101355188A (en) * 2008-07-04 2009-01-28 深圳市华扬通信技术有限公司 Three centimeter frequency band rapid switch and technique of preparing the same
CN101549993A (en) * 2009-04-30 2009-10-07 深圳市华扬通信技术有限公司 Lithium ferrite material applied to C waveband phase shifter
CN103664154A (en) * 2012-09-21 2014-03-26 绵阳市维奇电子技术有限公司 Formula and process of Li-Ti-Zn soft magnetic ferrite material with high frequency and high resistivity
CN103880408A (en) * 2014-02-26 2014-06-25 南京国睿微波器件有限公司 High-performance high-compaction lithium ferrite material for phase shifter, and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101355188A (en) * 2008-07-04 2009-01-28 深圳市华扬通信技术有限公司 Three centimeter frequency band rapid switch and technique of preparing the same
CN101549993A (en) * 2009-04-30 2009-10-07 深圳市华扬通信技术有限公司 Lithium ferrite material applied to C waveband phase shifter
CN103664154A (en) * 2012-09-21 2014-03-26 绵阳市维奇电子技术有限公司 Formula and process of Li-Ti-Zn soft magnetic ferrite material with high frequency and high resistivity
CN103880408A (en) * 2014-02-26 2014-06-25 南京国睿微波器件有限公司 High-performance high-compaction lithium ferrite material for phase shifter, and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104891975A (en) * 2015-04-24 2015-09-09 马鞍山科信咨询有限公司 High flexural strength nickel-zinc soft magnetic ferrite material and preparation method thereof
CN104891979A (en) * 2015-04-24 2015-09-09 马鞍山科信咨询有限公司 Wide temperature magnesium copper zinc soft magnetic ferrite magnetic core and preparation method thereof
CN104891982A (en) * 2015-04-24 2015-09-09 马鞍山科信咨询有限公司 Rare earth high-magnetic-permeability soft magnetic ferrite and preparation method thereof
CN106747481A (en) * 2016-12-15 2017-05-31 上海宝钢磁业有限公司 A kind of large scale magnetic core feed powder and preparation method thereof

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