CN101857427A - High-frequency low-loss MnZn ferrite material and manufacturing method thereof - Google Patents
High-frequency low-loss MnZn ferrite material and manufacturing method thereof Download PDFInfo
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Abstract
The invention provides a high-frequency low-loss MnZn ferrite material, which comprises main components and auxiliary components, wherein the main components are 53-56 mol percent of ferric oxide, 34-41 mol percent of manganese oxide and 6-10 mol percent of zinc oxide, the content of manganese oxide is measured by Mn; the auxiliary components are at least three selected from CaCO3, SiO2, Nb2O5, CoO, V2O5, SnO2 and TiO2, and based on the total weight of the main components, the auxiliary components comprise: 0.02-0.08 weight percent of CaCO3, 0.002-0.01 weight percent of SiO2, 0.02-0.06 weight percent of Nb2O5, 0.03-0.20 weight percent of CoO, 0.01-0.05 weight percent of V2O5, 0-0.20 weight percent of SnO2 and 0-0.10 weight percent of TiO2. The invention also provides a manufacturing method of the high-frequency low-loss MnZn ferrite material.
Description
Technical field
The present invention relates to a kind of MnZn Ferrite Material and manufacture method thereof, and relate in particular to a kind of high-frequency low-loss MnZn ferrite material and manufacture method thereof.
Background technology
High speed development along with TV, computer and various types of communication industry, requirement to various inducers, wave filter, magnetic core of transformer material trends towards high frequencyization, low-lossization, therefore each major company of the world is competitively studied, and power class material is brought up to the PC44 of more reduce power consumption and the PC50 of high frequency more from PC30, PC40 in the period of nearly 20.This class premium quality product is widely used in high definition digital television, high resolution computer indicating meter, pulse code modulation digital communication (PCM) and WDM and DWDM optical fiber communication equipment.
The MnZn power ferrite mainly as magnetic core of transformer, carries out the transmission and the conversion of energy.The watt level of one secondary magnetic core transmission can be expressed as:
As seen, operating frequency f is high more, the effective volume Ve of magnetic core is big more, and then Chuan Shu power is just big more.In other words, transmission nominal power, if operating frequency is high more, the effective volume of magnetic core just can be more little.Consider factors such as copper loss, waveform, the watt level of a transformer transmission is:
As seen, operating frequency f is high more, the loss P of magnetic core
vLow more, then the power of transformer transmission is just big more.Take all factors into consideration, transmission nominal power, if operating frequency is high more, the loss of magnetic core is low more, and then the volume of required magnetic core is just more little, and transformer just can be done forr a short time like this.The high-frequency low-consumption of MnZn Ferrite Material, device miniaturization, light-weighted basis just.
Ferritic loss mainly comprises magnetic hysteresis loss, eddy-current loss and residual loss three parts, when applying frequency is brought up to high frequency (500kHz) by low and medium frequency (100kHz), significant variation has taken place loss characteristic: eddy-current loss surpasses magnetic hysteresis loss and accounts for the over half of total loss, in total loss, occupy an leading position, become the main part of high-frequency loss.Domestic and international research shows that the method that the reduction high-frequency loss is mainly adopted is to add CaCO in main formula at present
3, SiO
2As ancillary component, because of it is enriched in crystal boundary, can form the high resistance grain boundary layer Deng the high resistance additive, can reach the purpose that reduces high-frequency loss, its sintering temperature is at 1300 ℃ to 1450 ℃ or a little less than 1450 ℃.But then, because SiO
2With the Fe in the principal constituent
2O
3Can react and generate Fe
2(SiO
3)
3, and its fusing point is 1150 ℃, and is lower than ferritic sintering temperature, therefore occurs the crystal grain phenomenon of growing up unusually easily when sintering, causes ferrite performance to worsen.
A lot of people have been arranged at the research high-frequency low-loss MnZn ferrite material, but these existing MnZn Ferrite Materials are respectively at 60 ℃, 100 ℃, 120 ℃, 500kHz, the loss under the 50mT condition is mostly at 100kW/m
3More than, and required sintering temperature is arranged on more than 1300 ℃ when making these materials, and the sintering top temperature is higher, is unfavorable for saving electric energy, reduces production costs.
Therefore, need provide a kind of and show the MnZn Ferrite Material of low loss characteristic at high frequency, and need a kind of improving one's methods of its of making, this method makes the highest holding temperature setting of agglomerating reduce significantly.
Summary of the invention
An object of the present invention is to provide a kind of high-frequency low-loss MnZn ferrite material.
MnZn Ferrite Material of the present invention comprises principal constituent and ancillary component, and wherein said principal constituent is the ferric oxide of 53mol%-56mol%, the manganese oxide of 34mol%-41mol% and the zinc oxide of 6mol%-10mol%, and wherein the content of manganese oxide is in Mn; And described ancillary component is selected from CaCO
3, SiO
2, Nb
2O
5, CoO, V
2O
5, SnO
2, TiO
2In at least three kinds, based on the gross weight of described principal constituent, CaCO
3Be 0.02wt%-0.08wt%, SiO
2Be 0.002wt%-0.01wt%, Nb
2O
5Be that 0.02wt%-0.06wt%, CoO are 0.03wt%-0.20wt%, V
2O
5Be 0.01wt%-0.05wt%, SnO
2Be 0wt%-0.20wt%, TiO
2Be 0wt%-0.10wt%.
The present invention also provides a kind of MnZn method for manufacturing ferrite material, and the method comprising the steps of:
1) with Fe
2O
3, Mn
3O
4Mix and dry in described ratio wet-milling with ZnO;
2) with step 1) gained powder at 800 ℃ of-920 ℃ of following pre-burning 1-3 hours;
3) to step 2) add at least three kinds of described ancillary components in described ratio in the powder of gained, add the deionized water in the 60wt%-120wt% that accounts for described principal constituent gross weight, the dispersion agent of 0.5wt%-3wt%, the defoamer of 0.5wt%-3wt% again and carry out ball milling together, make the powder particle size behind the ball milling reach 1.0 ± 0.2 μ m;
4) based on the gross weight of the powder of described step 3) gained, in the powder of described step 3) gained, add the organic binder bond of 7wt%-12wt%, mix granulation and get particulate material;
5) pressure of employing 50MPa-200MPa is pressed into green compact sample with particulate material;
6) with green compact sample sintering under 1080 ℃-1260 ℃ sintering temperature of step 5) gained, and insulation 3-5 hour under described sintering temperature, be cooled to 180 ℃ then and come out of the stove, wherein the holding-zone oxygen partial pressure is 1%-15%, temperature-fall period adopts equilibrium oxygen partial pres-sure.
Described organic binder bond is a polyvinyl alcohol.
Dispersion agent that uses among the present invention and defoamer can be dispersion agent and defoamers commonly used in this area, can select n-caprylic acid, stearic acid etc. for use as defoamer, and dispersion agent can be selected poly-propionic acid, glyconic acid, citric acid etc. for use.
Equilibrium oxygen partial pres-sure in the inventive method is according to formula lg (P (O
2))=α-b/T calculates, a value 5-10 wherein, and b value 10000～15000, T is an absolute temperature.
High-frequency low-loss MnZn ferrite of the present invention, the uniform crystal particles densification, the about 5 μ m-12 μ m of average grain size, its magnetic property after tested, its magnetic property index is as follows:
1. high-frequency low-loss MnZn ferrite of the present invention has and is higher than 1500 initial permeability.
2. high-frequency low-loss MnZn ferrite of the present invention is made OR25 * 8-15mm standard rings, and at 5Ts, 50mT tests loss characteristic under the 500kHz condition, and at 25 ℃, 60 ℃, 100 ℃, 120 ℃ of losses are lower than 120kW/m respectively
3, 70kW/m
3, 70kW/m
3, 90kW/m
3
The present invention is by adding the ancillary component CaCO more than three kinds or three kinds
3, SiO
2, CoO, Nb
2O
5, V
2O
5, SnO
2, TiO
2, and addition is optimized combination, thus the loss problem when having solved high frequency effectively.
The present invention is optimized combination to additive and the addition thereof with fusing assistant effect, has reduced sintering temperature effectively, makes the highest holding temperature of agglomerating be reduced to 1080 ℃-1260 ℃.Under low relatively sintering temperature, grain growing is even, fine and close, the about 5 μ m-12 μ m of average grain size, size to fit, avoided growing up unusually of crystal grain, thereby produced a kind of MnZn ferrite of high frequency, especially shown the MnZn ferrite of low loss characteristic at high frequency.
In addition, sintering temperature of the present invention is lower than of the prior art, thereby energy efficient has reduced production cost.
The details of one or more embodiments of the present invention has been proposed in accompanying drawing below and the description.Require from specification sheets, accompanying drawing and Accessory Right, other features of the present invention, purpose and advantage will be tangible.
Description of drawings
Fig. 1 is for making the P of high-frequency low-loss MnZn ferrite material according to the present invention under different sintering temperatures of OR 25 * 8-15mm standard rings form
L/ f～f curve.
Fig. 2 is the SEM photo of the high-frequency low-loss MnZn ferrite material made according to an embodiment of the invention.
Fig. 3 is at the SEM of 1280 ℃ of following agglomerating comparative samples photo.
Embodiment
Below each material among each embodiment all be commercially available.
Embodiment 1:
With sand mill is the Fe of 54.6mol% with principal constituent
2O
3, in the Mn of Mn 37.9mol%
3O
4Mix with the ZnO wet-milling of 7.5mol% and to place loft drier to dry.Use chamber type electric resistance furnace, with the gained powder 820 ℃ of following pre-burnings 2 hours.Then the powder after the pre-burning is put into ball mill,, in the gained powder, add the CaCO of ancillary component: 0.04wt% based on the gross weight of described principal constituent
3, 0.006wt% SiO
2, 0.035wt% Nb
2O
5, the CoO of 0.10wt%, the V of 0.04wt%
2O
5, 0.06wt% SnO
2TiO with 0.03wt%
2Add the deionized water in the 66wt% that accounts for described principal constituent gross weight, the dispersion agent of 1wt%, the defoamer of 1wt% again and carry out ball milling together.With this powder ball milling to mean particle size is about 1.0 ± 0.2 μ m; Based on the gross weight of the powder behind the ball milling, in this powder, add the polyvinyl alcohol solution of 8wt%, mix granulation, adopt the pressure of 50-200MPa that particulate material is pressed into green compact sample; In the last programme controlled bell jar stove of active computer,, and under sintering temperature, be incubated 4.5 hours, under balanced atmosphere, be cooled to 180 ℃ and come out of the stove at 1180 ℃ sintering temperature, insulation oxygen partial pressure 1.8%, temperature-fall period adopts equilibrium oxygen partial pres-sure.
The material of aforementioned manufacturing is made the standard rings of OR 25 * 8-15mm, and at 5Ts, 50mT detects its magnetic property under the condition of 500kHz.Detected result is listed in the following table 2, that is: initial permeability: 1573; At 25 ℃, 60 ℃, 100 ℃, 120 ℃ of losses are respectively 107.4kW/m
3, 53.9kW/m
3, 58.0kW/m
3, 78.2kW/m
3
Embodiment 2-8:
Each component of embodiment 2-8 and sintering temperature are referring to following table 1, and implementation step is with above-mentioned embodiment 1.The magnetic property detected result of the material that embodiment 2-8 is prepared is listed in the following table 2.
Comparing embodiment 1:
Each component of comparing embodiment 1 and sintering temperature are referring to following table 1, and implementation step is with above-mentioned embodiment 1.The magnetic property detected result of the material that comparing embodiment 1 is prepared is listed in the following table 2.
Table 1
Annotate:
*The expression sintering temperature has exceeded the scope of 1080 ℃-1260 ℃ of preferred sintering temperatures of the present invention.
The magnetic property detected result data of embodiment 1-8 and comparing embodiment 1 see the following form 2.
Table 2
Annotate:
*The expression sintering temperature has exceeded the scope of 1080 ℃-1260 ℃ of preferred sintering temperatures of the present invention.
Under the sintering temperature of 1140 ℃ and 1280 ℃, the P of test sintered sample magnetic property
L/ f～f curve is as Fig. 1.As can be seen from the figure, sintering temperature is set under 1140 ℃ the situation, and significant variation has taken place the loss characteristic of high-frequency low-consumption material under high frequency: the proportion of eddy-current loss reduces significantly.And when sintering temperature was set to 1280 ℃, material was in the loss under the high frequency, and eddy-current loss has but accounted for most.Reduce eddy-current loss, will improve the resistivity of material, particularly crystal boundary, require material to have the microstructure that crystal grain is little, crystal boundary is thick, the additive that this has fusing assistant character by interpolation, thus reduced sintering temperature effectively.
Lower sintering temperature is set, in crystal boundary, mixes high-resistance ancillary component simultaneously, as SiO
2, CaCO
3, Nb
2O
5Deng having increased the grain boundary resistance rate effectively.
Described as embodiment 1-8, suitable main formula has added the optimum combination of three kinds or three kinds of above-described ancillary components and ancillary component addition, the loss problem when having solved high frequency effectively.Ancillary component with fusing assistant effect reduces sintering temperature effectively.Under low relatively sintering temperature, grain growing is even, and size to fit has been avoided growing up unusually of crystal grain.Fig. 2 is the SEM figure of embodiment 3, by this figure as can be seen, and uniform crystal particles densification, the about 5 μ m-12 μ m of average grain size.
As shown in Figure 3, among the comparative example 1,1280 ℃ of sintering temperatures are set, crystal grain is grown up unusually, and pore is many, lack of homogeneity, and the magnetic permeability of material improves, but the serious variation of high-frequency loss.
From The above results as can be seen, the MnZn Ferrite Material of Zhi Zaoing compared to existing technology, high-frequency low-loss MnZn ferrite material of the present invention shows and is higher than 1500 initial permeability; At 50mT, under the 500kHz condition, different temperature spots has all shown low loss characteristic.
Though explained and described the preferred embodiments of the invention, not showing each embodiment explaination and described institute of the present invention might form.Or rather, using the vocabulary in specification sheets is descriptive vocabulary, rather than restrictive vocabulary, and should be appreciated that, can carry out various variations and does not depart from the spirit and scope of the invention that is defined by following claim.
Claims (5)
1. high-frequency low-loss MnZn ferrite material, it is characterized in that: described MnZn Ferrite Material comprises principal constituent and ancillary component, wherein said principal constituent is the ferric oxide of 53mol%-56mol%, the manganese oxide of 34mol%-41mol% and the zinc oxide of 6mol%-10mol%, and wherein the content of manganese oxide is in Mn; And
Described ancillary component is selected from CaCO
3, SiO
2, Nb
2O
5, CoO, V
2O
5, SnO
2, TiO
2In at least three kinds, based on the gross weight of described principal constituent, CaCO
3Be 0.02wt%-0.08wt%, SiO
2Be 0.002wt%-0.01wt%, Nb
2O
5Be that 0.02wt%-0.06wt%, CoO are 0.03wt%-0.20wt%, V
2O
5Be 0.01wt%-0.05wt%, SnO
2Be 0wt%-0.20wt%, TiO
2Be 0wt%-0.10wt%.
2. MnZn Ferrite Material as claimed in claim 1 is characterized in that: described Ferrite Material has and is higher than 1500 initial permeability.
3. MnZn Ferrite Material as claimed in claim 1 is characterized in that: described material is at 5Ts, 50mT, and under the condition of 500kHz, 25 ℃, 60 ℃, 100 ℃, 120 ℃ loss is lower than 120kW/m respectively
3, 70kW/m
3, 70kW/m
3, 90kW/m
3
4. the manufacture method of a high-frequency low-loss MnZn ferrite material as claimed in claim 1 is characterized in that: may further comprise the steps:
1) with Fe
2O
3, Mn
3O
4Mix and dry in described ratio wet-milling with ZnO;
2) with step 1) gained powder at 800 ℃ of-920 ℃ of following pre-burning 1-3 hours;
3) to step 2) add at least three kinds of described ancillary components in described ratio in the powder of gained, add the deionized water in the 60wt%-120wt% that accounts for described principal constituent gross weight, the dispersion agent of 0.5wt%-3wt%, the defoamer of 0.5wt%-3wt% again and carry out ball milling together, make the powder particle size behind the ball milling reach 1.0 ± 0.2 μ m;
4) based on the gross weight of the powder of described step 3) gained, in the powder of described step 3) gained, add the organic binder bond of 7wt%-12wt%, mix granulation and get particulate material;
5) pressure of employing 50MPa-200MPa is pressed into green compact sample with particulate material;
6) with green compact sample sintering under 1080 ℃-1260 ℃ sintering temperature of step 5) gained, and insulation 3-5 hour under described sintering temperature, be cooled to 180 ℃ then and come out of the stove, wherein the holding-zone oxygen partial pressure is 1%-15%, temperature-fall period adopts equilibrium oxygen partial pres-sure.
5. manufacture method as claimed in claim 4 is characterized in that: the described organic binder bond in the described step 4) is a polyvinyl alcohol.
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