CN101620908B - Mn-Zn ferrite with broad temperature, broadband, high curie point and low loss and preparation method thereof - Google Patents
Mn-Zn ferrite with broad temperature, broadband, high curie point and low loss and preparation method thereof Download PDFInfo
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Abstract
The present invention discloses a Mn-Zn ferrite with broad temperature, broadband, high curie point and low loss and a preparation method thereof, the composition calculated by content of oxides is as follows: 52-57mol% of Fe2O3, 3-7mol% of ZnO and the balance of MnO; a first auxiliary component comprises 0.01wt%-0.1wt% of CaO and 0.005wt%-0.02wt% of SiO2; a second auxiliary component comprises one or more of V2O5, Nb2O5, Ta2O5, ZrO2, K2O and NiO, and the content is 0-0.2wt% by calculation, and a third auxiliary component comprises 0.04-0.075wt% of SnO2, 0.08-0.15wt% of TiO2 and 0.05-0.5wt% of Co2O3,wherein, the content of TiO2 is twice as much as that of SnO2. Pre-burning under the protection of nitrogen, sintering, the control of cooling atmosphere and the densification process are carried out, thereby leading the Mn-Zn ferrite with broad temperature, broadband and high curie point to not only meet the market demands of magnetic cores of electromagnetic couplers for electrodeless lamps, but also open up a vast world for new applications of a variety of high frequency power ferrite magnetic cores in communication and strong electric fields.
Description
Technical field
The present invention relates to a kind of broad temperature, broadband, high curie point and low loss MnZn ferrite material and preparation method thereof, belong to the ferrite magnetic material technical field.
Background technology
In recent years, the MnZn ferrite material technical performance competitively improves in each big ferrite company of the world, to adapt to the application of expanding day by day, at making excessive demands down of users such as IT industry, power electronics, illumination electronics, a kind of theory of looking for novelty, demanding perfection is being dominated the R﹠D direction of soft magnetic ferrites gradually.Here it is requires material to have higher saturation flux density Bs, better dc superposition characteristic, lower specific loss coefficient tg δ/μ
i(comprising the power consumption Pc under the high magnetic flux density) and total harmonic distortion coefficient (THD) and wideer frequency of utilization and wider serviceability temperature scope.Therefore, the research of MnZn ferrite material has marched low temperature, high temperature and wideer and high band field more.After analysing in depth each Company Material's performance index and various indicatrix, as can be seen, work as frequency of utilization:
During f＜250kHz, select the PC40, the PC44 material that are analogous to TDK company for use, power consumption is starkly lower than PC50, and particularly as B＜100mT, during f＜100kHz, PC40 occupies price and performance advantage, need not select PC50 for use;
During 250kHz＜f＜300kHz, PC44 is least in power-consuming, PC50 secondly, PC40 power consumption maximum, this is the market scope that PC44 monopolizes;
During 300kHz＜f＜1MHz, PC50 is least in power-consuming;
During 1MHz＜f＜10MHz, select for use to be analogous to the 3F4 of FERROXCUBE company, 3F45 section bar material;
During f＞10MHz, have only the Ni-Zn Ferrite Material could work as this important task at present, so select 4F1 for use.
Based on above thinking, each made producer is for a long time actively seeking the low remanent magnetism material of a kind of broad temperature, broadband, high curie point, in the hope of replacing the numerous high-frequency and low-consumption Ferrite Material of item.
The extensive use of environmental protection electromagnetic induction electrodeless lamp and performance improve, the exploitation and the volume production of this material have been promoted, owing to broken through traditional incandescent lamp, the luminescence mechanism of gaseous discharge lamp, electrodeless lamp has become internationally recognized the 4th generation energy-conserving and environment-protective new light sources.Characteristics such as high light efficiency, long-life, height develop the color, light is stable more make its rapid fashionable world.Thereby the also fast-selling thereupon market of core component high-performance magnetic core of its electromagnetic energy conversion.
HF lamp without electrodes is mostly used nickel-zinc-ferrite material with magnetic core, because design is at the built-in electromagnetic generator in luminous element centre position, the essential enough big electromagnetic energy of frequency generation that uses up to 2.65MHz apart from the fluorescent material that is activated very big distance arranged, so just can make it to activate luminous.But the electromagnetic radiation that the 2.65MHz higher-order of oscillation produces, the technical finesse that the radio frequency interference problem is carried out had both hindered the light transmission efficiency of lamp, and too high lamp body temperature has influenced the light decay and the useful life of this electrodeless lamp again, has also greatly increased manufacturing cost.
Low frequency electrodeless lamp is operated under 200～300KHz low and medium frequency state, usually use the manganese-zinc ferrite magnetic core, its outlet structure is beneficial to realization to the development of high-power, super high power (200W-1000W) light fixture, thus be applicable to tall and big broad field of illumination, and also efficient is very high.With respect to the frequency of oscillation about 200KHz, on EMC, EMI technical finesse means, just be easy to up to standardly, the manufacturing process relative difficulty is also little a lot.The benevolent see benevolence and the wise see wisdom, and built-in and external these two kinds of structures have his own strong points, and at present and be stored in electrodeless lamp industry each show his special prowess, but how to produce the two all high-performance magnetic core of dual-purpose, then become the difficult problem of magnetic material producer.
These two kinds of operating states are all harsh especially to the soft magnetic ferrite performance demands, should have enough magnetic permeabilitys by extremely low temperature [below 40 ℃], start the higher-order of oscillation, quite high again Curie temperature [more than+280 ℃] is to keep not failure of oscillation, also will be in so wide temperature range maintenance higher flux density and lower power consumption, this is a very large contradiction.The nickel Zinc material has high frequency, high-Curie-point feature, but the ultralow temperature magnetic permeability is low, make coil sensibility reciprocal deficiency be difficult to start, and the material power consumption is bigger, and the light fixture heating is too high; Though the MnZn material has high-magnetodensity low-power consumption advantage, Curie point and frequency difficulty get on, the easy failure of oscillation of high temperature, and the light fixture volume is bigger.
Chinese patent application (CN101183582A) discloses a kind of high saturation magnetic flux density low loss NiMnZn power ferrite material, it is by optimization formula and doping, particularly add 2～4mol%NiO, obtained saturation flux density Bs1194A/m, under 100 ℃ greater than 460mT, under 100 ℃ of the high frequency power consumption 500kHz 50mT less than 150kw/m
3, but do not mention broad temperature, broadband characteristic and Curie point height at all, thereby it is of limited application, and cost is higher.
And for example Chinese patent application (CN1749209A) discloses a kind of high saturation magnetic flux density, low loss manganese-zinc ferrite material and preparation method thereof, and it is by mixing and technology controlling and process, has obtained 100kHz, 200mT, has been lower than 245kw/m 45 ℃ the time
3Power consumption and 1194A/m, 50mT, saturation flux density is higher than the result of 535mT 25 ℃ the time, but does not have the introduction of high and low temperature and high frequency characteristics equally, obviously its scope of application is quite limited.
Chinese patent application (CN101004961A) discloses the preparation method of high frequency high power ferrite material for another example, by the doping of effective change crystal boundary and microstructure, has obtained magnetic permeability about 1000,100 ℃ of following power consumption 250kw/m of 1MHz, 30mT
3, 3MHz, 10mT, 100 ℃ of following power consumption 350kw/m
3, but lack data and the wide temperature characteristics and the Curie point introduction of low frequency power consumption, particularly avoided saturation flux density Bs value, with high-frequency high-power as if a reality be contrary to.
The essentially identical Chinese patent application of content (CN101004962A) discloses the high frequency low-loss manganese zine ferrite material preparation method therewith, obtains initial permeability μ i900 ± 20%, 1MHz, 30mT, between 25～100 ℃ power consumption less than 200kw/m
3, 3MHz, 10mT, between 25～100 ℃ power consumption less than 350kw/m
3, Curie temperature is more than or equal to 220 ℃, and 25 ℃ of saturation flux density Bs do not have the characteristic introduction of low temperature and low frequency equally more than or equal to 350mT, and Curie point and saturation flux density Bs value are also too on the low side.
Summary of the invention
As everyone knows, soft magnetic ferrite loss and frequency are generally linear, when being lower than 200kHz, and magnetic hysteresis part (P
Hv) greater than eddy current part (P
Ev), and when being higher than 200kHz, then opposite.200kHz is a transition point, under this frequency, and P
Hv=P
Ev, as f＞200kHz, eddy current loss rises to main influence, and frequency is high more, and eddy current loss is big more, is contained eddy current so must increase grain boundary resistance.Usually add SiO
2, CaCO
3, Ta
2O
5, SnO
2And TiO
2Have good effect.Calcium ion forms the calcium silicates barrier layer in the place's segregation of Mn-Zn ferrite crystal boundary with silicon, can improve the grain boundary resistance rate and significantly reduce eddy current loss.Add TiO
2, also can form calcium titanium type resistive formation, in order to keep electric neutrality, Ti at crystal boundary
4+Ion increases, Fe
3+Ion can reduce, and Fe
2+Content increase.The high price titanium ion is owing to follow closely at Fe
2+The position can become an electrostatic trap, improves the reactivity of particle.Control Fe
2+Content can also be regulated two peaks (SMP) temperature, adds Co
2+Ion is got involved, and ferritic wide temperature characteristics just can obtain.
The lowest power consumption of valley point and main formula Fe on the Pcv-T curve
2O
3Content is closely related.Particularly when frequency of utilization when 1MHz is above, desire reduces magnetic core power consumption Pcv, improves performance factor Bmf, then general the employing reduced initial permeability μ
iWay, with close Bs of the magnetic that obtains better high frequency performance and Geng Gao and Curie point Tc, at this moment in the main formula ZnO content to have reduced to 6mol% following so that about 3mol%, and Fe
2O
3Content then increases to more than the 56mol%.Along with Fe
2O
3The increase of content, coercivity H reduces, and the magnetic hysteresis loss that is directly proportional with area of hysteresis loop also reduces thereupon; And Fe
2O
3Content increases, and power consumption valley point temperature reduces, but the increase of the resistivity under this temperature, thereby also make eddy current loss descend; On the other hand, along with Fe
2O
3The increase of/ZnO ratio, magnetic permeability μ
iReduction, Curie temperature Tc rises, and maximum results are that high temperature Bs improves, and make the material dc superposition characteristic improve, and while domain wall resonance frequency is shifted to high-end, can cause residual loss to reduce.
As previously mentioned, the characteristics of new material are to widen suitable frequency, reduce the power loss under the wide temperature range corresponding frequencies again, for reaching this purpose, except that preferred main formula with mixing, also must cool off atmosphere by meticulous adjustment sintering, strict control solid phase reaction process.
In order to reach above purpose, the invention provides a kind of preparation method of broad temperature, broadband, high curie point and low loss MnZn ferrite material.
By adjusting prescription and mixing and optimization technology, the broad temperature, broadband MnZn ferrite material of preparing is-40
-Ratio temperature coefficient in+25 ℃ the temperature range is less than 3.0 * 10
-6Curie point reaches+and 280 ℃; Density is 4.85 * 10
3Kg/m
3Initial permeability μ
i+ 25 ℃ is 1500 ± 25%; At 200kHz, 100mT, under 100 ℃ of test conditions than power consumption less than 200kw/m
3At 500kHz, 50mT, under 100 ℃ of test conditions than power consumption less than 120kw/m
3At 1MHz, 30mT, under 100 ℃ of test conditions than power consumption less than 250kw/m
3At 3MHz, 10mT, under 100 ℃ of test conditions than power consumption less than 350kw/m
3At 1194A/m, saturation flux density Bs is 450mT under 100 ℃ of test conditions.
The technical scheme that a kind of broad temperature, broadband, high curie point and low loss MnZn ferrite material of the present invention is adopted is as follows:
It is characterized in that principal component content is calculated as with oxide: Fe
2O
3Be 52～57mol%; ZnO is 3～7mol%; All the other are MnO, wherein Fe
2O
3Preferably ratio is 53～55mol%, and the ratio of ZnO is 4～6mol%;
The first auxiliary element content that adds is calculated as with oxide: CaO is 0.01wt%～0.1wt%; SiO
2Be 0.005wt%～0.02wt%;
Second auxiliary element that adds comprises one or more in the following impurity of representing with oxide form: V
2O
5, Nb
2O
5, Ta
2O
5, ZrO
2, K
2O, NiO, each impurity content calculates greater than 0～0.2wt% with oxide in second auxiliary element of interpolation, and the total amount of described second auxiliary element adds up to and is less than or equal to 0.3wt%;
The 3rd auxiliary element content that adds is calculated as with oxide: SnO
2Be 0.04～0.075wt%; TiO
2Be 0.08～0.15wt%; , Co
2O
3Be 0.05～0.5wt%, wherein TiO
2Content be SnO
2Twice, and TiO
2With SnO
2The content sum greater than 0.1wt%.
The preparation method of a kind of broad temperature, broadband, high curie point and low loss MnZn ferrite material of the present invention, its technology comprises the steps:
1), raw-material mixing:
With prepare by 52～57mol%Fe
2O
3, 3～7mol%ZnO, principal component that all the other are formed for MnO and by 0.01wt%～0.1wt%CaCO
3, 0.005wt%～0.02wt%SiO
2First auxiliary element of forming is put into ball mill, the deionized water of weight such as adding, ball milling 1～3 hour;
2), pre-burning:
Pre-burning in the pre-firing is sent in the raw material oven dry that above-mentioned mix grinding is good again, and the calcined temperature scope is 900～1050 ℃, temperature retention time is 2～4 hours, and atmosphere is air, and pre-firing cooling area feeds nitrogen, cooling atmosphere control oxygen content makes pre-imitation frosted glass powder magnetization degree less than 1% below 5%;
3), impurity adds:
Select for use by 0～0.2wt%V
2O
5, 0～0.2wt%Nb
2O
5, 0～0.2wt%Ta
2O
5, 0～0.2wt%ZrO
2, 0～0.2wt%K
2Second auxiliary element of one or more compositions among O, the 0～0.2wt%NiO and by 0.04～0.075wt%SnO
2, 0.08～0.15wt%TiO
2, 0.05～0.5wt%Co
2O
3The 3rd auxiliary element of forming is as the associating additive, and wherein the total content of second auxiliary element is less than or equal to 0.3wt%, TiO
2Content is SnO
2The twice of content, and TiO
2With SnO
2The content sum is greater than 0.1wt%;
4) secondary ball milling:
Pre-imitation frosted glass and additive are put into ball mill, the deionized water of weight such as adding, ball milling 8 hours, the particle mean size that makes slip is less than 1.2 μ m;
5) forming and sintering:
With the slurry oven dry, add the 10wt% ingredients by weight, concentration is 9% polyvinyl alcohol solution, evenly mixes, and uses 45 order sub-sieve granulations, and compression moulding, puts into bell jar stove sintering, the control of sintering process temperature is as follows:
Temperature rise period: programming rate per hour about 150 ℃, to 800 ℃, carries out in the air atmosphere, takes the air blast discharging, the about 100m of flow velocity
3/ h;
Per hour about 250 ℃, partial pressure of oxygen is 0.005% to programming rate between 800 ℃ to 1100 ℃;
1100 ℃ to 1200 ℃ heating-up times are 1 hour, and pre-incubation is 1 hour again, and partial pressure of oxygen is 0.5～1%;
Heating up between 1200 ℃ to 1350 ℃ is 1 hour, and partial pressure of oxygen is 1～3%;
Holding stage: be incubated 2～6 hours about 1350 ℃, partial pressure of oxygen is 2～8%;
Temperature-fall period: per hour about 150 ℃, partial pressure of oxygen switches to 0.5～2% to cooling rate between 1350 ℃ to 1100 ℃;
1100 ℃ down cooling rate drop to about 150 ℃ and come out of the stove per hour about 250 ℃, whole process is kept equilibrium oxygen partial pres-sure about 0.2～0.01%.
In the technology of the present invention, pre-firing cooling area feeds nitrogen, regulates oxygen content below 5%, make material slowly cooling under nitrogen protection, control powder magnetization degree prevents that less than 1% peroxidating and quenching phenomenon from taking place, in order to avoid the magnetic core properties of product are inferior, embrittlement, cracking; The finished product sintering process adopts precise dose and atmosphere segmentation control, takes the air blast discharging during intensification, in case adhesive residue causes pore, can both guarantee effectively that product magnetic and density improve.
The broad temperature, broadband, high curie point MnZn ferrite material that the present invention prepares can be used for electrodeless lamp electromagnetic coupler, and in energy-conserving and environment-protective green illumination electronic material, its special performance is:
1, the numerous high-frequency and low-consumption Mn-Zn ferrite material Curie point overwhelming majority of item is about 250 ℃, can reach 280 ℃ of persons individually, not that the high temperature power consumption is excessive, be exactly that the ultralow temperature magnetic permeability is too low, therefore as electrodeless lamp coupler magnetic core, be not temperature overheating loss of excitation failure of oscillation, being exactly that the ultralow temperature inductance is too low can't start, and the wide temperature high-Curie-point of the present invention feature has been stopped these two kinds of phenomenons and taken place;
2, high-frequency and low-consumption Mn-Zn ferrite material high and low frequency power consumption differs greatly, and can't take into account, and wideband low-power consumption feature of the present invention makes 200kHz and two operating frequencies of 2.65MHz can both satisfy customer requirements;
3, low zinc prescription of the preferred high ferro of the present invention and effectively doping, both guaranteed the wide temperature characteristics of magnetic permeability and power consumption and temperature, taken into account the broadband properties of power consumption and frequency again, also guaranteed the raising of high temperature saturation flux density Bs, specific sintering cooling atmosphere control and densification process improve product density, thereby further reduced power consumption and increased saturation flux density Bs, guaranteed the stable of operating state.
Embodiment
Following specific embodiment only is that the present invention's spirit is described in further detail, but the present invention is not limited to given example.The technical staff of the technical field of the invention can make various modification or replenishes or adopt similar fashion to substitute described instantiation, but can't depart from spirit of the present invention or surmount the scope of appended claims definition.
Embodiment 1
Raw-material selection:
Commercially pure Fe
2O
3, the above CaCO of ZnO, MnO and chemical pure
3, SiO
2, V
2O
5, Nb
2O
5, Ta
2O
5, ZrO
2, K
2CO
3, SnO
2, TiO
2, Co
2O
3Deng;
The design of components of broad temperature, broadband, high curie point and low loss MnZn ferrite material of the present invention:
The main component content of Ferrite Material is calculated as with oxide: Fe
2O
3For 54.2mol%, ZnO are 4.5mol%, all the other are MnO; First adds auxiliary calculating with oxide comprises: SiO
2Be 100ppm (0.01wt%); CaO is 700ppm (0.07wt%); Second auxiliary element that adds calculates with oxide and comprises: V
2O
5Be 300ppm (0.03wt%), Nb
2O
5Be 200ppm (0.02wt%); The 3rd auxiliary element content that adds is calculated as with oxide: TiO
2Be 1000ppm (0.1wt%); SnO
2Be 500ppm (0.05wt%); Co
2O
3Be 500ppm (0.05wt%).
The preparation method of broad temperature, broadband, high curie point and low loss MnZn ferrite material of the present invention, its technology comprises the steps:
1), raw-material mixing:
With aforementioned prepare by Fe
2O
3, the principal component formed of ZnO, MnO and by CaCO
3, SiO
2First auxiliary element of forming is put into ball mill, the deionized water of weight such as adding, ball milling 2 hours;
2), pre-burning:
Pre-burning in the stove is sent in the raw material oven dry that above-mentioned mix grinding is good, and calcined temperature is 980 ℃, and temperature retention time is 2 hours, and atmosphere is air, and pre-firing cooling area feeds nitrogen, and cooling atmosphere control oxygen content makes the powder magnetization degree less than 1% below 5%;
3), impurity adds:
With the aforesaid second auxiliary element (V
2O
5Be 300ppm, Nb
2O
5Be 200ppm), the 3rd auxiliary element (TiO
2Be 1000ppm, SnO
2Be 500ppm, Co
2O
3Be 500ppm) unite interpolation for additive;
4) secondary ball milling:
Material is put into ball mill, the deionized water of weight such as adding, ball milling 8 hours, the particle mean size that makes pre-imitation frosted glass is less than 1.2 μ m;
5) forming and sintering:
With the slurry oven dry, add the 10wt% ingredients by weight, concentration is 9% poly-vinyl alcohol solution, evenly mixes, and uses 45 order sub-sieve granulations, and is pressed into product and standard magnet ring, puts into bell jar stove sintering, the control of sintering process temperature atmosphere is as follows:
Temperature rise period: programming rate per hour about 150 ℃, to 800 ℃, carries out in the air atmosphere, takes the air blast discharging, the about 100m of flow velocity
3/ h fully volatilizees bonding agent;
Per hour about 250 ℃, partial pressure of oxygen is 0.005% to programming rate between 800 ℃ to 1100 ℃;
1100 ℃ to 1200 ℃ heating-up times are 1 hour, and pre-incubation is 1 hour again, and partial pressure of oxygen is 0.5～1%;
Heating up between 1200 ℃ to 1350 ℃ is 1 hour, and partial pressure of oxygen is 1～3%;
Holding stage: be incubated 2～6 hours about 1350 ℃, partial pressure of oxygen is 2～8%;
Temperature-fall period: per hour about 150 ℃, partial pressure of oxygen switches to 0.5～2% to cooling rate between 1350 ℃ to 1100 ℃;
1100 ℃ down cooling rate drop to about 150 ℃ and come out of the stove per hour about 250 ℃, whole process is kept equilibrium oxygen partial pres-sure about 0.2～0.01%.
Embodiment 2:
Raw-material selection:
Commercially pure Fe
2O
3, the above CaCO of ZnO, MnO and chemical pure
3, SiO
2, V
2O
5, Nb
2O
5, Ta
2O
5, ZrO
2, K
2CO
3, SnO
2, TiO
2, Co
2O
3Deng;
The design of components of Ferrite Material:
Main component content is calculated as with oxide: Fe
2O
3For 55mol%, ZnO are 4.2mol%, all the other are MnO; First adds auxiliary calculating with oxide comprises: SiO
2Be 50ppm (0.005wt%); CaO is 500ppm (0.05wt%); Second auxiliary element that adds calculates with oxide and comprises: Ta
2O
5Be 150ppm (0.015wt%), Nb
2O
5Be 200ppm (0.02wt%), ZrO
2Be 300ppm (0.03wt%), K
2O is 1000ppm (0.1wt%); The 3rd auxiliary element content that adds is calculated as with oxide: TiO
2Be 800ppm (0.08wt%); SnO
2Be 400ppm (0.04wt%); Co
2O
3Be 1000ppm (0.1wt%).
The preparation method of the broad temperature, broadband, high curie point and low loss MnZn ferrite material of present embodiment, its processing step and process conditions and embodiment 1 are identical, and reinforced kind and content are referring to this routine design of components.
Embodiment 3:
Raw-material selection:
Commercially pure Fe
2O
3, the above CaCO of ZnO, MnO and chemical pure
3, SiO
2, V
2O
5, Nb
2O
5, Ta
2O
5, ZrO
2, K
2CO
3, SnO
2, TiO
2, Co
2O
3Deng;
The design of components of Ferrite Material:
Main component content is calculated as with oxide: Fe
2O
3For 55.7mol%, ZnO are 4mol%, all the other are MnO; First adds auxiliary calculating with oxide comprises: SiO
2Be 200ppm (0.02wt%); CaO is 500ppm (0.05wt%); Second auxiliary element that adds calculates with oxide and comprises: Ni
2O
3Be 1000ppm (0.1wt%), Nb
2O
5Be 200ppm (0.02wt%); The 3rd auxiliary element content that adds is calculated as with oxide: TiO
2Be 1500ppm (0.15wt%); SnO
2Be 750ppm (0.075wt%); Co
2O
3Be 4000ppm (0.4wt%).
The preparation method of the broad temperature, broadband, high curie point and low loss MnZn ferrite material of present embodiment, its processing step and process conditions and embodiment 1 are identical, and reinforced kind and content are referring to this routine design of components.
The magnetic property of above-mentioned three example sintered samples and density test the results are shown in following table (table 1):
Table 1
| Electromagnetic performance | Test condition | Example 1 | Example 2 | Example 3 |
| Initial permeability μ i | Frequency: 10kHz | 1920 | 1800 | 1540 |
| Than temperature coefficient α F×10 -6 | -40～+ 25 ℃, with surveying μ i | 2.6 | 2.8 | 2 |
| Curie temperature Tc (℃) | Frequency: 10kHz | 275 | 283 | 288 |
| Saturation flux density Bs (mT) | 1194A/m，50Hz，100℃ | 455 | 462 | 465 |
| Low frequency characteristic (Pcv kw/m 3) | 200kHz，100mT，100℃ | 195 | 210 | 180 |
| High frequency characteristics (Pcv kw/m 3) | 500kHz，50mT，100℃ | 125 | 100 | 115 |
| High frequency characteristics (Pcv kw/m 3) | 1MHz，30mT，100℃ | 225 | 195 | 210 |
| High frequency characteristics (Pcv kw/m 3) | 3MHz，10mT，100℃ | 320 | 305 | 315 |
| Density (10 3kg/m 3) | 25℃ | 4.8 | 4.9 | 4.85 |
Comparison example can be found out from table: with Fe
2O
3The minimizing of content increase and ZnO content, saturation flux density Bs and Curie temperature Tc rise, but initial permeability μ i descends; With TiO
2And Co
2O
3Unite the reinforcement of mending the reward effect, reduce than temperature coefficient, wide temperature characteristics improves; Doping system has been guaranteed the balance and the reduction of low-and high-frequency power consumption; The effect that technologies such as atmosphere control and pre-incubation improve density of material is obvious.
In addition to the implementation, the present invention can also have other execution modes.All employings are equal to the technical scheme of replacement or equivalent transformation form, all drop on the protection range of requirement of the present invention.
Claims (3)
1. the preparation method of a broad temperature, broadband, high curie point and low loss MnZn ferrite material, its technology comprises the steps:
1), raw-material mixing:
With prepare by 52～57mol%Fe
2O
3, 3～7mol%ZnO, principal component that all the other are formed for MnO and by 0.01wt%～0.1wt%CaCO
3, 0.005wt%～0.02wt%SiO
2First auxiliary element of forming is put into ball mill, the deionized water of weight such as adding, ball milling 1～3 hour;
2), pre-burning:
Pre-firing pre-burning is sent in the raw material oven dry that above-mentioned mix grinding is good again, and the calcined temperature scope is 900～1050 ℃, temperature retention time is 2～4 hours, and pre-burning atmosphere is air, and pre-firing cooling area feeds nitrogen, cooling atmosphere control oxygen content makes pre-imitation frosted glass powder magnetization degree less than 1% below 5%;
3), impurity adds:
Select for use by 0～0.2wt%V
2O
5, 0～0.2wt%Nb
2O
5, 0～0.2wt%Ta
2O
5, 0～0.2wt%ZrO
2, 0～0.2wt%K
2Second auxiliary element of one or more compositions among O, the 0～0.2wt%NiO and by 0.04～0.075wt%SnO
2, 0.08～0.15wt%TiO
2, 0.05～0.5wt%Co
2O
3The 3rd auxiliary element of forming is as additive, and wherein the total content of second auxiliary element is less than or equal to 0.3wt%, TiO
2Content is SnO
2The twice of content, and TiO
2With SnO
2The content sum is greater than 0.1wt%;
4) secondary ball milling:
Pre-imitation frosted glass powder and additive are put into ball mill, the deionized water of weight such as adding, ball milling 8 hours, the particle mean size that makes slurry is less than 1.2 μ m;
5) forming and sintering:
With the slurry oven dry, the concentration that adds the 10wt% ingredients by weight is 9% poly-vinyl alcohol solution, evenly mixes, and uses 45 order sub-sieve granulations, and compression moulding, puts into bell jar stove sintering, and the control of sintering process temperature is as follows:
Temperature rise period: programming rate per hour about 150 ℃, to 800 ℃, carries out in the air atmosphere, takes the air blast discharging, the about 100m of flow velocity
3/ h;
Per hour about 250 ℃, partial pressure of oxygen is 0.005% to programming rate between 800 ℃ to 1100 ℃;
1100 ℃ to 1200 ℃ heating-up times are 1 hour, and pre-incubation is 1 hour again, and partial pressure of oxygen is 0.5～1%;
Heating up between 1200 ℃ to 1350 ℃ is 1 hour, and partial pressure of oxygen is 1～3%;
Holding stage: be incubated 2～6 hours about 1350 ℃, partial pressure of oxygen is 2～8%;
Temperature-fall period: per hour about 150 ℃, partial pressure of oxygen switches to 0.5～2% to cooling rate between 1350 ℃ to 1100 ℃;
1100 ℃ down cooling rate drop to about 150 ℃ and come out of the stove per hour about 250 ℃, whole process is kept equilibrium oxygen partial pres-sure 0.2～0.01%.
2. the preparation method of broad temperature, broadband, high curie point and low loss MnZn ferrite material according to claim 1, it is characterized in that, meticulous adjustment pre-burning, sintering, cooling atmosphere, control densification process, product density is improved, thereby further reduce power consumption and increase saturation flux density Bs, the density of MnZn ferrite material is 4.85 * 10
3Kg/m
3At 1194 A/m, 50Hz, saturation flux density Bs reaches 455mT-465mT under 100 ℃ of test conditions.
3. the preparation method of broad temperature, broadband, high curie point and low loss MnZn ferrite material according to claim 1 is characterized in that, the ratio temperature coefficient of described MnZn ferrite material in-40-25 ℃ temperature range reaches 2.0 * 10
-6～2.8 * 10
-6, Curie temperature reaches 283 ℃～288 ℃.
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