CN104591712B - Low-loss manganese zinc ferrite material for temperature of 20 DEG C below zero to 140 DEG C and manufacturing method thereof - Google Patents
Low-loss manganese zinc ferrite material for temperature of 20 DEG C below zero to 140 DEG C and manufacturing method thereof Download PDFInfo
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Abstract
The invention provides a low-loss manganese zinc ferrite material for temperature of 20 DEG C below zero to 140 DEG C and a manufacturing method thereof. The ferrite material comprises main components and auxiliary components, wherein the main components refer to x mol% of Fe2O3, y mol% of MnO and z mol% of ZnO; the auxiliary components comprise c wt% of Co2O3 and n wt% of NiO based on the total weight of main components; the ratios of the components are that x is equal to 54.5-55.5, z is equal to 7.5-9.5, y is equal to 100-x-z, c is equal to 0.25-0.45 and n is equal to 0.3-0.9; A being 2600-45x-9z is more than or equal to 30 and less than or equal to 80; and B being 150-3x-3y+371c-1.6n is more than or equal to -30 and less than or equal to 30. The manganese zinc ferrite material is prepared by the process steps of batching, mixing, pre-sintering, performing secondary grinding, granulating, molding and sintering.
Description
Technical field
The present invention relates to a kind of MnZn soft magnetic ferrite material and manufacture method, more particularly to a kind of to be used for -20～140 DEG C
Low-loss MnZn power ferrite material and its manufacture method, belong to electronic devices and components Metallic Functional Materials manufacturing technology
New material high-technology field.
Background technology
Soft magnetic ferrite is that kind is most, most widely used, a kind of magnetic material that consumption is maximum, is electronics and information industry
Important foundation functional material.Soft magnetic ferrite production and it is prevailing using in be MnZn ferrites, MnZn ferrites
Yield account for the 70% of soft magnetic ferrite total output, be of greatest concern in current soft magnetic materials and field the most active.Closely
The development of Nian Lai, MnZn Ferrite Material is improved by the depth of single performance and turns to the horizontal expansion that many index is improved simultaneously.
Such as power ferrite material, in addition to the loss for further reducing material, also requires the reduce loss in more wide temperature range,
Or the decline low-loss of more broadband, or higher saturation flux density etc..
Existing multinomial technology can laterally expand the ferritic performances of MnZn, but only be mostly the horizontal of a few performance
Expand.
In the method as disclosed in CN1287985A, by the cobalt oxide for adding accessory ingredient, magnetic ferrites materials are made 20
The minima of the power attenuation of～100 DEG C of temperature province Inner is in 400kW/m3Hereinafter, and in 20～100 DEG C of temperature province
Power attenuation maxima and minima difference in 150kW/m3Below.Realize low-loss laterally opening up in wide temperature range
Exhibition, but and the unrealized performance for having high Bs concurrently.
And for example in technical scheme disclosed in CN1404076A, the NiO of 3～6mol% is up to by a large amount of additions, makes magnetic core
More than 450mT is up in 100 DEG C of saturation flux densities, but low loss characteristic sacrifices too many, 100kHz, 200mT, 100 DEG C of bars
Loss under part is up to 550～900kW/m3。
For another example in technical scheme disclosed in CN1649039A, by the shaping powder for preparing specific specific surface area, reach
The purpose of power attenuation is reduced, but also only realizes low-loss and high Bs, its room temperature loss is up to 600kW/m3More than, and
The performance of unrealized wide-temperature and low-consumption.
Disclosed patent of invention CN102682946A of the present inventor and CN103496963A have taken into account the high Bs of high temperature and width
The technical scheme of temperature and low-consumption double grading, but its wide-temperature and low-consumption scope needs to be further expanded.
The content of the invention
It is an object of the invention to provide a kind of simple inexpensive low-loss manganese for -20～140 DEG C
Zinc ferrite material and its manufacture method.The Ferrite Material includes main constituent and auxiliary element, and main constituent is Fe2O3： x
Mol%, MnO：Y mol%, ZnO：Z mol%, auxiliary element is Co based on main constituent gross weight2O3：C wt% and NiO：n
Wt%, wherein the ratio of each composition is x=54.5-55.5, z=7.5-9.5, y=100-x-z, c=0.25-0.45, n=
0.3-0.9, defines A=2600-45x-9z, B=150-3x-3y+371c-1.6n, then A, B meet following condition：30≤A≤
80、-30≤B≤30.Made by processing steps such as dispensing, batch mixing, pre-burning, two mills, pelletize, molding, sintering, material sintering is close
Degree reaches the 97% of solid density, in -20～140 DEG C of wide temperature ranges, the work(of magnetic core 100kHz, 200mT made by the material
Rate loss is less than 380kW/m3, wherein 100 DEG C of loss is less than 300kW/m3, and saturation flux density Bs at 100 DEG C is high
In 450mT, initial permeability is more than 3300.
The technical solution used in the present invention is：
For -20～140 DEG C of low loss manganese-zinc ferrite material, it is characterised in that：The Ferrite Material includes master
Composition and auxiliary element, main constituent is Fe2O3：X mol%, MnO：Y mol%, ZnO：Z mol%, auxiliary element based on it is main into
Gross weight is divided to be Co2O3：C wt% and NiO：N wt%, wherein the ratio of each composition is x=54.5-55.5, z=7.5-
9.5th, y=100-x-z, c=0.25-0.45, n=0.3-0.9, define A=2600-45x-9z, B=150-3x-3y+
371c-1.6n, then A, B meet following condition：30≤A≤80、-30≤B≤30.
Preferably, auxiliary element also includes M1, M2 and M3 component, wherein, based on the gross weight of the main constituent, M1 is
SiO2, its content is 40ppm-100ppm；
M2 is CaCO3, its content is 100ppm-500ppm；
M3 is V2O5、Nb2O5、ZrO2、Ta2O5、In2O3In one or more, the wherein total addition level of M3 is less than
1000ppm。
The Ferrite Material sintered density reaches the 97% of solid density, in -20～140 DEG C of special wide temperature range,
The power attenuation of ferrite core 100kHz, 200mT is less than 380kW/m3, wherein 100 DEG C of loss is less than 300kW/m3, and
Saturation flux density Bs at 100 DEG C is higher than 450mT, and initial permeability is more than 3300.
The invention has the beneficial effects as follows：
On the basis of the present inventor previous work CN102682946A, ground by the main formula doping test of a large amount of systems
Study carefully, each main constituent and Co in the high Bs low waste that induction and conclusion has gone out in -20～140 DEG C of wide temperature ranges and main formula2O3、
The relational expression of NiO additions, so that it is determined that material realizes the essential condition of high Bs low waste in -20～140 DEG C of wide temperature ranges
For 30≤A≤80, -30≤B≤30.In order to reach higher Bs and lower power attenuation, main formula is limited at Fe2O3：x
=54.5-55.5, ZnO：Z=7.5-9.5, balance of MnO.Relative to solid density 97% sintered density ensure that it is higher
Bs.
Compared with prior art, the present invention have it is preferably creative, the MnZn power ferrite material low cost of preparation,
Excellent performance.
Description of the drawings
Fig. 1 is the loss temperature curve comparison diagram of comparative example 5*, 6* and embodiment 7.
Specific embodiment
For -20～140 DEG C of low loss manganese-zinc ferrite material, comprise the following steps：
1) dispensing：Main constituent is weighed according to design component；
2) batch mixing：Alleged main constituent mixing is put into into sand mill or ball mill, uniform powder is sufficiently mixed；
3) pre-burning：Gained powder is carried out into pre-burning, calcined temperature is 800 DEG C -1000 DEG C, temperature retention time 1-3 hour, from
Right Preburning material of coming out of the stove to obtain of lowering the temperature；
4) two mill：Add auxiliary element in above-mentioned Preburning material, carry out two and be milled to 0.8 μm or so of particle mean size and dry
Powder, two thinner abrasive particle degree are the bases that sintered density reaches solid density more than 97%；
5) pelletize：Based on step 4) gained powder gross weight, be added to 8-10wt% concentration be 8-10wt%
Polyvinyl alcohol water solution, mix homogeneously pelletize obtains the particulate material for molding；
6) molding：To step 5) gained particulate material in add concentration for 0.1-0.5wt% polyvinyl alcohol water solution, make powder
Material moisture content reaches 0.15-0.35wt%, with the gross weight meter of the aqueous powder of gained, adds the zinc stearate of 0.1-1.0wt%
Batch mixing is carried out, it is compressing for green product；
7) sinter：Sintering temperature is 1300 DEG C -1360 DEG C, and temperature retention time 3-8 hour, cooling is come out of the stove and obtains manganese-zinc ferrite
Body material.Specially：From room temperature to 600 DEG C, 100 DEG C/h of programming rate, air；From 600 DEG C to 900 DEG C -1100 DEG C, heat up
300 DEG C/h of speed, air；From 900 DEG C -1100 DEG C to 1300 DEG C -1400 DEG C, 60 DEG C/h-300 DEG C/h of programming rate, nitrogen
Gas；In 1300 DEG C of -1400 DEG C of insulation 6-10 hours, soaking zone partial pressure of oxygen is controlled for 1-10%；Temperature-fall period is using balance oxygen
Less than 0.01%, 60 DEG C/h-300 DEG C/h of cooling rate are depressed into, 180 DEG C are cooled to and are come out of the stove and obtain MnZn ferrite material.
With reference to embodiment, the present invention is further illustrated.
Example 1-25
1) using commercially available Fe2O3(purity >=99.3%), MnO (Mn content >=76.6%), ZnO (purity >=99.7%)
As main constituent, according to the amount shown in table 1 by Fe2O3, MnO, ZnO be placed in sand mill, stirring and ground and mixed is uniform is dried
The pre-burning 2h at 890 DEG C afterwards；
2) gross weight based on the powder after pre-burning, adds additive：Co shown in table 12O3With the SiO of NiO, 50ppm2、
The CaCO of 300ppm3, 300ppm Nb2O5, 300ppm ZrO2And deionized water, dispersant, defoamer carry out together it is secondary
Grinding, is ground to powder particle mean size for 0.8 μm；
3) gross weight based on the powder after ball milling, the polyethylene of the concentration for 9wt% of 9.0wt% is added in the powder
Polyvinyl alcohol water solution of the concentration for 0.2wt% is added in alcoholic solution, mix homogeneously pelletize in particulate material, makes powder moisture content
0.25wt% is reached, with the gross weight meter of the aqueous powder of gained, adding the zinc stearate of 0.4wt% carries out batch mixing, using 40 tons
Particulate material is pressed into green density for 2.9 ± 0.2g/cm by dry powder press3Green compact sample；
4) it is last to sinter under 1360 DEG C of sintering temperature, and it is incubated 4 hours at a sintering temperature.Specially：From room temperature
To 600 DEG C, 100 DEG C/h of programming rate, air；From 600 DEG C to 900 DEG C -1100 DEG C, 300 DEG C/h of programming rate, air；From
900 DEG C -1100 DEG C to 1360 DEG C, 60 DEG C/h-300 DEG C/h of programming rate, nitrogen；4 hours are incubated at 1360 DEG C, control insulation
Section partial pressure of oxygen is 4.8%；Temperature-fall period adopts equilibrium oxygen partial pres-sure to less than 0.01%, 60 DEG C/h-300 DEG C/h of cooling rate, cold
But come out of the stove to 180 DEG C and obtain MnZn ferrite material.
Using HP4294A electric impedance analyzers (Agilent Technology 4294A) and special fixture (Agilent
Technology 16047E) room temperature inductance L under measuring samples magnet ring 10kHz feeble fields, calculate the initial permeability of material；
With Bs of the SY-8258 types B-H tester at 100 DEG C of 50Hz, 1200A/m test sample magnet ring；Use Model 2335Watt
Power attenuation of the Meter test samples magnet ring at 100kHz, 200mT, -20 DEG C, 40 DEG C, 100 DEG C, 140 DEG C, as a result lists table in
In 2.
Table 1
Note：Numbering band the scheme of No. * be comparative example, A=A=2600-45x-9z, B=150-3x-3y+371c-1.6n.
Table 2
Note：Numbering is comparative example with the scheme of No. *.
Data display in table 1,2：
1) comparative example 1～2 is that ZnO content limits scope beyond the present invention, and wherein the ZnO content of comparative example 1 is beyond this
The bright restriction upper limit, causes Bs low；The ZnO content of comparative example 2 limits lower limit beyond the present invention, and Bs is sufficiently high, but is lost higher.
2) comparative example 3～4 is Fe2O3Content limits scope, the wherein Fe of comparative example 3 beyond the present invention2O3Content is beyond this
Invention limits lower limit, and high Bs cannot be guaranteed, K1Value complement repays deficiency, while parameter A causes low temp power to damage beyond the upper limit is limited
Consumption is higher；The Fe of comparative example 42O3Content limits the upper limit, K beyond the present invention1Value complement is repaid excessively, while parameter A is under limiting
Limit, causes high temperature consumption higher.
3) comparative example 5～6 is Co2O3Addition limits scope, the wherein Co of comparative example 5 beyond the present invention2O3Addition surpasses
Go out the present invention and limit lower limit, K1Value does not obtain effective compensation, and parameter B substantially beyond lower limit is limited, causes high and low temperature power attenuation
It is all higher；The Co of comparative example 62O3Addition limits the upper limit, K beyond the present invention1Value complement is repaid excessively, and parameter B is substantially on limiting
Limit, causes loss comprehensively higher.
4) example 7～20 is Fe2O3Content, ZnO content, Co2O3Addition is limiting scope, and parameter A, B is limiting model
Embodiment and comparative example inside and outside enclosing, wherein embodiment of parameter A, B in the range of restriction, excellent material performance；Comparative example 10
All it is that parameter A goes out the present invention and limit the upper limit beyond present invention restriction lower limit, parameter B ultrasonic with 15, causes high/low temperature loss higher.
Example 26～30
1) with Fe2O3Component prescription weighs Fe based on 55.0mol%, MnO 36.5mol%, ZnO 8.5mol%2O3It is (pure
Degree >=99.3%), MnO (Mn content >=76.6%), ZnO (purity >=99.7%) raw materials and based on main constituent gross weight
The Co of 0.34wt%2O3It is placed in sand mill with the NiO of 0.7wt%, simultaneously ground and mixed is uniform for stirring, is dried pre- at 920 DEG C
Burn 1.5h；
2) gross weight based on the powder after pre-burning, according to shown in table 3 addition add auxiliary element, add from
Sub- water, dispersant, defoamer carry out together two mills, are ground to powder particle mean size for 0.8 μm；
3) gross weight based on the powder after ball milling, the polyethylene of the concentration for 9wt% of 9.0wt% is added in the powder
Polyvinyl alcohol water solution of the concentration for 0.2wt% is added in alcoholic solution, mix homogeneously pelletize in particulate material, makes powder moisture content
0.25wt% is reached, with the gross weight meter of the aqueous powder of gained, adding the zinc stearate of 0.4wt% carries out batch mixing, using 40 tons
Particulate material is pressed into green density for 2.9 ± 0.2g/cm by dry powder press3Green compact sample；
4) it is last to sinter under 1320 DEG C of sintering temperature, and it is incubated 7 hours at a sintering temperature.Specially：From room temperature
To 600 DEG C, 100 DEG C/h of programming rate, air；From 600 DEG C to 900 DEG C -1100 DEG C, 300 DEG C/h of programming rate, air；From
900 DEG C -1100 DEG C to 1320 DEG C, 60 DEG C/h-300 DEG C/h of programming rate, nitrogen；7 hours are incubated at 1320 DEG C, control insulation
Section partial pressure of oxygen is 3.1%；Temperature-fall period adopts equilibrium oxygen partial pres-sure to less than 0.01%, 60 DEG C/h-300 DEG C/h of cooling rate, cold
But come out of the stove to 180 DEG C and obtain MnZn ferrite material.
Using HP4294A electric impedance analyzers (Agilent Technology 4294A) and special fixture (Agilent
Technology 16047E) room temperature inductance L under measuring samples magnet ring 10kHz feeble fields, calculate the initial permeability of material；
With Bs of the SY-8258 types B-H tester at 100 DEG C of 50Hz, 1200A/m test sample magnet ring；Use Model 2335Watt
Power attenuation of the Meter test samples magnet ring at 100kHz, 200mT, -20 DEG C, 40 DEG C, 100 DEG C, 140 DEG C, as a result lists table in
In 4.
Table 3
Table 4
Note：Numbering is comparative example with the scheme of No. *.
Data display in table 3,4：
1) doping of embodiment 21～22 the present invention limit within the scope of, excellent material performance；
2) comparative example 23～24 is SiO2Restriction scope of the doping beyond the present invention：The wherein SiO of comparative example 232Addition
Amount is less than the lower limit that the present invention is limited, it is impossible to form CaSiO3Resistive formation is distributed in crystal boundary, causes eddy-current loss to increase, total to damage
Consumption deteriorates；The SiO of comparative example 242Addition causes abnormal crystallization higher than the upper limit that the present invention is limited, and causes loss to deteriorate；
3) comparative example 25～26 is CaCO3Restriction scope of the doping beyond the present invention：The CaCO of comparative example 303Addition
Less than the lower limit that the present invention is limited, it is impossible to form CaSiO3Resistive formation is distributed in crystal boundary, causes eddy-current loss to increase, total to damage
Consumption deteriorates；The CaCO of comparative example 313Addition causes abnormal crystallization higher than the upper limit that the present invention is limited, and causes loss to deteriorate.
4) embodiment, comparative example 27～35 respectively show V2O5、Nb2O5、ZrO2、Ta2O5、In2O3Additive effect.Its
Middle addition Nb2O5、ZrO2、Ta2O5Effect with crystal grain thinning, with the effect for reducing power attenuation；Addition V2O5、In2O3Promote
Enter grain growth, use cooperatively with crystal grain thinning impurity, improve performance.The doping of embodiment 27～33 limits scope in the present invention
Within, excellent material performance；The total amount of adding of comparative example 34～35 is more than 1000ppm, penalty.
The present invention is illustratively described by preferred embodiment above, it should be understood, however, that these embodiments
Not limiting the scope of the present invention.Conversely, any modification made within the purport and principle of the present invention, equivalent are replaced
Change, improve, should be included within protection scope of the present invention for being defined by the following claims.
Claims (1)
1. a kind of low loss manganese-zinc ferrite material for -20～140 DEG C, it is characterised in that：The Ferrite Material includes
Main constituent and auxiliary element；Main constituent is Fe2O3：55.0mol%, MnO：36.5mol%, ZnO：8.5mol%, auxiliary element base
In main constituent gross weight be Co2O3：0.34wt%, NiO：0.7wt%, SiO2：60ppm, CaCO3：300ppm, V2O5：100ppm,
Nb2O5：200ppm, ZrO2：100ppm, Ta2O5：100ppm, In2O3：100ppm；Prepare according to following steps：
(1) Fe is weighed2O3, MnO, ZnO raw material and Co2O3It is placed in sand mill with NiO, simultaneously ground and mixed is uniform for stirring, does
The dry pre-burning 1.5h at 920 DEG C；Fe2O3Purity >=99.3%, Mn content >=76.6% of MnO, ZnO purity >=99.7%；
(2) auxiliary element is added, adding deionized water, dispersant, defoamer carries out together two mills, is ground to the average grain of powder
Spend for 0.8 μm；
(3) gross weight based on the powder after ball milling, the polyvinyl alcohol of the concentration for 9wt% of 9.0wt% is added in the powder
Polyvinyl alcohol water solution of the concentration for 0.2wt% is added in solution, mix homogeneously pelletize in particulate material, reaches powder moisture content
To 0.25wt%, with the gross weight meter of the aqueous powder of gained, adding the zinc stearate of 0.4wt% carries out batch mixing, dry using 40 tons
Particulate material is pressed into green density for 2.9 ± 0.2g/cm by powder press3Green compact sample；
(4) it is last to sinter under 1320 DEG C of sintering temperature, and at a sintering temperature 7 hours are incubated, specially：From room temperature to
600 DEG C, 100 DEG C/h of programming rate, air；From 600 DEG C to 900 DEG C -1100 DEG C, 300 DEG C/h of programming rate, air；From 900
DEG C -1100 DEG C to 1320 DEG C, 60 DEG C/h-300 DEG C/h of programming rate, nitrogen；7 hours are incubated at 1320 DEG C, soaking zone oxygen is controlled
Partial pressure is 3.1%；Temperature-fall period, to less than 0.01%, 60 DEG C/h-300 DEG C/h of cooling rate, is cooled to using equilibrium oxygen partial pres-sure
Come out of the stove for 180 DEG C and obtain MnZn ferrite material.
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| CN106396657A (en) * | 2016-08-25 | 2017-02-15 | 天长市中德电子有限公司 | Broadband low loss soft magnetic ferrite material and preparation method thereof |
| CN106365624A (en) * | 2016-08-29 | 2017-02-01 | 天长市中德电子有限公司 | Low-loss manganese-zinc soft ferrite magnet core material |
| CN108727010A (en) * | 2018-06-21 | 2018-11-02 | 苏州天源磁业股份有限公司 | A kind of MnZnNiCo Ferrite Materials and preparation method thereof |
| CN113024235A (en) * | 2021-02-02 | 2021-06-25 | 浙江国石磁业有限公司 | Variable-frequency wide-temperature low-loss high-magnetic-flux-density MnZn power ferrite and preparation method thereof |
| CN113998999B (en) * | 2022-01-04 | 2022-04-01 | 天通控股股份有限公司 | Manufacturing method of wide-temperature low-loss high-Bs manganese-zinc ferrite material |
| CN115745588B (en) * | 2022-09-23 | 2023-11-03 | 西南应用磁学研究所(中国电子科技集团公司第九研究所) | High-performance factor manganese zinc ferrite material and preparation method thereof |
| CN116813323A (en) * | 2023-07-07 | 2023-09-29 | 上海宝钢磁业有限公司 | Wide-temperature low-loss soft magnetic manganese zinc ferrite material suitable for 25-140 ℃ and preparation method and application thereof |
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| CN104072118A (en) * | 2014-06-12 | 2014-10-01 | 天长市中德电子有限公司 | Manganese zinc ferrite material and preparation process thereof |
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