CN102682946A - MnZn ferrite magnetic core with double characteristics and manufacture method - Google Patents
MnZn ferrite magnetic core with double characteristics and manufacture method Download PDFInfo
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Abstract
The invention discloses a MnZn ferrite magnetic core with double characteristics and a manufacture method. The magnetic core consists of main components and auxiliary components. The main components consist of Fe2O3 54-56 mol%, ZnO 5-10 mol% and the balance manganese oxide, wherein the sum of the Fe2O3, the ZnO and the manganese oxide is 100 mol%. The auxiliary components comprise a first auxiliary material, a second auxiliary material, a third auxiliary material and a selectable fourth auxiliary material, wherein the first auxiliary material is an oxide of Co, the second auxiliary material is one of Ni2O3, NiO or Li2CO3, the third auxiliary material is selected from CaCO3 and Nb2O5, and the fourth auxiliary material is selected from SiO2, V2O5 and ZrO2. The shortcoming that a common MnZn power ferrite material cannot integrate multiple characteristics is overcome, the MnZn ferrite magnetic core has the double characteristics of high temperature and Bs and wide temperature and low loss, the unit volume loss Pcv (100kHz, 200mT) of the magnetic core at the temperature of 25 DEG C to 120 DEG C is smaller than 350 kW/m<3>, the lowest loss at the temperature of about 90 DEG C is 300 kW/m<3>, and the saturation magnetic flux density can reach to 450 mT at the temperature of 100 DEG C.
Description
Technical field
The present invention relates to a kind of MnZn soft magnetic ferrite and manufacturing approach, particularly a kind of MnZn soft-magnetic ferrite core and manufacturing approach that has high Bs of high temperature and wide-temperature and low-consumption double grading concurrently.
Background technology
Soft magnetic ferrite be kind at most, use the widest, the maximum a kind of magnetic material of consumption, be the important foundation functional material of electronics and information industry.Prevailing in soft magnetic ferrite production and use is the MnZn ferrite, and the ferritic output of MnZn accounts for 70% of soft magnetic ferrite total output, is field of greatest concern and the most active in the present soft magnetic material.In recent years, the development of MnZn Ferrite Material improves the horizontal expansion that turns to many index to improve simultaneously by the depth of single performance.Such as power ferrite material, except the loss of further reduction material, also require more reducing the wastage in the wide temperature range, perhaps more reduce the wastage perhaps higher saturation flux density etc. under the broadband.
Existing multinomial technology can laterally be expanded the ferritic performance of MnZn, but only is the horizontal expansion of a few performance mostly.
In the CN1287985A disclosed method, by adding the cobalt oxide of accessory ingredient, the minimum of a value that makes the power attenuation of magnetic ferrites materials in 20～100 ℃ temperature province is at 400kW/m
3Below, and in the difference of the maximum of the power attenuation of 20～100 ℃ temperature province and minimum of a value at 150kW/m
3Below.Realized the horizontal expansion of low-loss, but and be unrealized and have the performance of high Bs concurrently at wide temperature range.
And for example in the disclosed technical scheme of CN1404076A; Through the NiO of a large amount of interpolations up to 3～6mol%; Make magnetic core more than 100 ℃ saturation flux density is up to 450mT, but the low loss characteristic sacrifice is too many, the loss under 100kHz, 200mT, the 100 ℃ of conditions is up to 550～900kW/m
3
In the disclosed technical scheme of CN1649039A, use powder through the shaping for preparing specific specific area for another example, reached and reduced the purpose of power loss, but also only realized low-loss and high Bs, its normal temperature loss is up to 600kW/m
3More than, and the performance of the wide-temperature and low-consumption of being unrealized.
In the existing MnZn ferrite core material manufacture process, in the temperature-fall period behind the sintering, generally adopt to keep the equilibrium oxygen partial pres-sure method to handle, to guarantee product quality and performances.According to the equilibrium oxygen partial pres-sure computing formula, the oxygen content in the time of 1100 ℃ can be 0.01～0.6%, and in order to keep the balanced atmosphere of temperature descending section, oxygen content needs slowly to reduce.Yet, in the scope below 0.6% oxygen content is accurately controlled, furnace equipment and technical staff all there are strict requirement, be unfavorable for the stable operation of producing in batches.
Summary of the invention
The object of the present invention is to provide a kind of novel MnZn ferrite core material.
Another object of the present invention is to provide the manufacturing approach of above-mentioned material.
The technical scheme that the present invention taked is:
A kind of MnZn ferrite core is become to be grouped into assisting by principal component, principal component consist of Fe
2O
3: 54～56 mol%, ZnO:5～10 mol%, surplus is a manganese oxide, three's sum is counted 100 mol%; Auxilliary composition comprises first auxiliary material, second auxiliary material, the 3rd auxiliary material and the 4th auxiliary material, and wherein, first auxiliary material is the oxide of Co, and it is 2500～4500ppm at ferrite magnetic content in the heart; Second auxiliary material is that addition is the Ni of 4300～8500 ppm
2O
3, addition is that NiO or the addition of 4000～8000 ppm is 1000～2500 ppm Li
2CO
3In a kind of; The 3rd auxiliary material is that addition is the CaCO of 100～500 ppm
3With addition be the Nb of 100～500 ppm
2O
5The 4th auxiliary material is selected from SiO
2, V
2O
5, ZrO
2, its addition is 0～500 ppm.
The composition of principal component is preferably Fe
2O
3: 54.5～55.5 mol%, ZnO:6～9 mol%, surplus is a manganese oxide, three's sum is counted 100 mol%.
First auxiliary material is that addition is the Co of 3000～4500 ppm
2O
3, the CoO of 2500～4000 ppm or the Co of 2500～4500 ppm
3O
4
The manufacturing approach of above-mentioned MnZn ferrite core comprises the steps:,
1) based on the composition of MnZn ferrite core, take by weighing principal component, or at least a in principal component and first auxiliary material and second auxiliary material; Adding water stirs; Grind mixing, spray-drying obtains powder, and the gained powder is warming up to 900 ℃～1050 ℃ with the programming rate of 150～200 ℃/h; Be incubated 1～3 hour, the cooling come out of the stove the pre-burning material;
2) with pre-burning material, the auxiliary material, water, dispersant, the antifoaming agent mixing that do not add or do not add fully as yet, regrind to powder particle size is 0.8～1.2 μ m, adds organic bond, mixing, and spray drying obtains the particulate material that is used to be shaped;
3) aqueous solution with particulate material and organic bond carries out batch mixing, and the moisture content of control particulate material is 0.2～0.4%, is pressed into green compact;
4) with green sintering, grinding obtains the MnZn ferrite core.
Preferably, the sintering temperature of green compact is 1200 ℃～1350 ℃.
Preferably, adopt the secondary reduction sintering process during green sintering, temperature-fall period keeps equilibrium oxygen partial pres-sure.
Preferably, the computing formula of equilibrium oxygen partial pres-sure is lg (P (O
2))=a-b/T, wherein, a value 4～15, b value 10000～19000, T is an absolute temperature.
Preferably, comprise respectively in the temperature-rise period of secondary reduction sintering and the temperature-fall period and at least once be incubated platform, and be cooled to 1100 ℃ and directly charge into nitrogen later on.
Preferably, the MnZn ferrite that sinters adopts the through type grinding machine, and cleans with ultrasonic cleaning apparatus.
Preferably, the through type grinding machine is selected the above emery wheel of 300 orders for use.
The invention has the beneficial effects as follows:
MnZn ferrite core material of the present invention; Overcome conventional MnZn power ferrite material and can't take into account the deficiency of multiple characteristic; Have high Bs of high temperature and wide-temperature and low-consumption double grading concurrently, (100kHz is 200mT) less than 350kW/m from 25 ℃～120 ℃ unit volume loss Pcv for this magnetic core
3, lowest loss is lower than 300kW/m near 90 ℃
3, and in the time of 100 ℃, also have saturation flux density up to 450mT.This magnetic core has the double grading of high Bs of high temperature and wide-temperature and low-consumption concurrently with respect to conventional power ferrite magnetic core, is the most all-round in the heart a kind of of existing ferrite magnetic, and properties of product are superior to the import hit product, can be widely used in various occasions.
The effect of first auxiliary material according to the invention is and Fe
2+Ion is united the magnetocrystalline constant K that compensates conventional manganese-zinc ferrite
1, realize K
1Value levels off to 0 in wider temperature range, thereby realizes the performance of wide-temperature and low-consumption.When the first auxiliary material addition is lower than limited range of the present invention, can't realize performance index of the present invention, particularly enlarge markedly with loss meeting more than 100 ℃ below 60 ℃; When the first auxiliary material addition surpasses limited range of the present invention, will make loss～temperature curve too smooth, and cause the overall losses level to increase, near the loss 90 ℃ can't reach and be lower than 300kW/m
3Level.
The effect of second auxiliary material according to the invention is to improve the magnetic core sintered density, and can improve two peak temperatures, so that can increase Fe in the principal component
2O
3Content, thereby the saturation flux density Bs of raising magnetic core.When the second auxiliary material addition is lower than limited range of the present invention, can't make two peak temperatures be increased to enough scopes, high temperature consumption is difficult to reduce, and this moment is if reduce Fe
2O
3Content is realized the reduction of high temperature consumption to improve two peak temperatures, will cause the synchronous reduction of saturation flux density Bs; When the second auxiliary material addition exceeds limited range of the present invention,, core loss is enlarged markedly with forming a large amount of Ni ferrite solid solutions in magnetic core.Of CN1404076A, wherein NiO content is 3-6 mol%, is scaled part by weight and is about 19000～37000 ppm, and its nickel oxide addition ultra limited range of the present invention far away is so core loss enlarges markedly.
The present invention has realized that through the interpolation scope of control first auxiliary material and second auxiliary material MnZn ferrite core has the double grading of high Bs and wide-temperature and low-consumption concurrently.
The effect of the 3rd, the 4th auxiliary material according to the invention is to reduce the power loss of magnetic core.
The inventive method is provided with on the basis of insulation platform at temperature descending section, is cooled to 1100 ℃ and can directly charges into nitrogen later, reduces kiln and regulates difficulty, and the product quality that obtains ensures that more the properties of product between batch are more stable.
The through type grinding machine is selected the above emery wheel of 300 orders for use, can make the magnetic core abradant surface level and smooth, and it is remaining to reduce stress, avoids leakage inductance increase, core loss to increase.
Description of drawings
Fig. 1 is the loss temperature curve of different core materials.
Embodiment
A kind of MnZn ferrite core is become to be grouped into assisting by principal component, principal component consist of Fe
2O
3: 54～56 mol%, ZnO:5～10 mol%, surplus is a manganese oxide, three's sum is counted 100 mol%; Auxilliary composition comprises first auxiliary material, second auxiliary material, the 3rd auxiliary material and the 4th auxiliary material, and wherein, first auxiliary material is the oxide of Co, and it is 2500～4500ppm at ferrite magnetic content in the heart; Second auxiliary material is that addition is the Ni of 4300～8500 ppm
2O
3, addition is that NiO or the addition of 4000～8000 ppm is 1000～2500 ppm Li
2CO
3In a kind of; The 3rd auxiliary material is that addition is the CaCO of 100～500 ppm
3With addition be the Nb of 100～500 ppm
2O
5The 4th auxiliary material is selected from SiO
2, V
2O
5, ZrO
2, its addition is 0～500 ppm.
The composition of principal component is preferably Fe
2O
3: 54.5～55.5 mol%, ZnO:6～9 mol%, surplus is a manganese oxide, three's sum is counted 100 mol%.
First auxiliary material is that addition is the Co of 3000～4500 ppm
2O
3, the CoO of 2500～4000 ppm or the Co of 2500～4500 ppm
3O
4
The manufacturing approach of above-mentioned MnZn ferrite core comprises the steps:,
5) based on the composition of MnZn ferrite core, take by weighing principal component, or at least a in principal component and first auxiliary material and second auxiliary material; Adding water stirs; Grind mixing, spray-drying obtains powder, and the gained powder is warming up to 900 ℃～1050 ℃ with the programming rate of 150～200 ℃/h; Be incubated 1～3 hour, the cooling come out of the stove the pre-burning material;
6) with pre-burning material, the auxiliary material, water, dispersant, the antifoaming agent mixing that do not add or do not add fully as yet, regrind to powder particle size is 0.8～1.2 μ m, adds organic bond, mixing, and spray drying obtains the particulate material that is used to be shaped;
7) aqueous solution with particulate material and organic bond carries out batch mixing, and the moisture content of control particulate material is 0.2～0.4%, is pressed into green compact;
8) with green sintering, grinding obtains the MnZn ferrite core.
Preferably, the sintering temperature of green compact is 1200 ℃～1350 ℃.
Preferably, adopt the secondary reduction sintering process during green sintering, temperature-fall period keeps equilibrium oxygen partial pres-sure.
Preferably, the computing formula of equilibrium oxygen partial pres-sure is lg (P (O
2))=a-b/T, wherein, a value 4～15, b value 10000～19000, T is an absolute temperature.
Preferably, comprise respectively in the temperature-rise period of secondary reduction sintering and the temperature-fall period and at least once be incubated platform, and be cooled to 1100 ℃ and directly charge into nitrogen later on.
Preferably, the MnZn ferrite that sinters adopts the through type grinding machine, and cleans with ultrasonic cleaning apparatus.
Preferably, the through type grinding machine is selected the above emery wheel of 300 orders for use.
Below in conjunction with embodiment, further specify the present invention.
Example 1～8
1) adopts commercially available Fe
2O
3, Mn
3O
4, ZnO is as principal component, according to the amount shown in the table 1 with Fe
2O
3, (raw material is Mn to MnO
3O
4), ZnO and based on a certain proportion of Ni of principal component
2O
3Place sand mill, in the aforementioned powder that takes by weighing, add the water of the 90wt% of said powder total weight, stirring and ground and mixed are even; Speed with 180 ℃/h after the spray drying is warming up to 950 ℃ of following pre-burning 2h;
2), add the Co of additive: 3500ppm based on the total weight of the powder after the pre-burning
2O
3, 30ppm SiO
2, 300ppm CaCO
3, 300ppm Nb
2O
5And the deionized water of 65wt%, the dispersant of 1.2wt%, the antifoaming agent of 0.8wt% carry out regrind together, and being ground to particle mean size is 1.0 ± 0.2mm;
3) based on the total weight of the powder behind the ball milling, in this powder, add the poly-vinyl alcohol solution of 7.7wt%, mix granulation, adopt 20 tons of dry powder press that particulate material is pressed into green compact sample;
4) last at sintering under 1300 ℃ sintering temperature, and under sintering temperature, be incubated 8 hours, under balanced atmosphere, be cooled to 180 ℃ and come out of the stove, soaking zone partial pressure of oxygen 5%, temperature-fall period adopts equilibrium oxygen partial pres-sure.
Adopt the normal temperature inductance L under HP4294A electric impedance analyzer (Agilent Technology 4294A) and special fixture (Agilent Technology 16047E) the measuring samples magnet ring 10kHz feeble field, calculate the initial permeability of material; With the Bs of SY-8258 type B-H tester at 50Hz, 1200A/m, 100 ℃ of following specimen magnet rings; With the power loss of Model 2335 Watt Meter specimen magnet rings under 100kHz, 200mT, condition of different temperatures, the result lists in the table 1.
In table 1 example illustrated, 1～4 is the embodiment of the invention, and 5～8 is comparative example.
Can know by the data in the table 1:
1) all within limited range of the present invention, the magnetic core performance index are up to standard fully for embodiment 1～4 principal component.
2) comparative example 5～6 for ZnO content exceeds limited range of the present invention, wherein the ZnO content of comparative example 5 exceeds the present invention and limits lower limit, power loss is higher; The ZnO content of comparative example 6 exceeds the present invention and limits the upper limit, and the temperature stability of Bs worsens, and causes 100 ℃ Bs obviously on the low side.
3) comparative example 7～8 is Fe
2O
3Content exceeds limited range of the present invention, wherein the Fe of comparative example 7
2O
3Content exceeds the present invention and limits the upper limit, the power loss severe exacerbation; The Fe of comparative example 8
2O
3Content exceeds the present invention and limits lower limit, causes 100 ℃ Bs on the low side.
The product of example 3 and the product of TDK company are carried out performance comparison, record its loss temperature curve.Result of the test is as shown in Figure 1.Can know that by figure properties of product of the present invention obviously are superior to the product of TDK company.
Example 9～21
1) with Fe
2O
354.9mol%, MnO 37.1mol%, ZnO 8.0mol% takes by weighing Fe for the principal component prescription
2O
3, Mn
3O
4, the ZnO raw material place sand mill, in the above-mentioned powder that takes by weighing, add first auxiliary material or second auxiliary material or first auxiliary material and second auxiliary material and based on the water of the 90wt% of said powder total weight, stir and ground and mixed even, the auxiliary material addition is as shown in table 2; Speed with 200 ℃/h after the spray drying is warming up to 1000 ℃ of following pre-burning 1.5h;
2) based on the total weight of the powder after the pre-burning; Add remaining auxiliary material according to the addition shown in the table 2; Add the deionized water of 67wt%, the dispersant of 1.1wt%, the antifoaming agent of 0.9wt% again and carry out regrind together, being ground to particle mean size is 1.0 ± 0.2mm;
3) based on the total weight of the powder behind the ball milling, in this powder, add the poly-vinyl alcohol solution of 8.2wt%, mix granulation, adopt 40 tons of dry powder press that particulate material is pressed into green compact sample;
4) last under 1330 ℃ sintering temperature sintering, and insulation 6 hours under sintering temperature, soaking zone partial pressure of oxygen 7.5% is cooled under balanced atmosphere after 1100 ℃, directly charges into nitrogen protection, to be cooledly comes out of the stove to 180 ℃.
Adopt the normal temperature inductance L under HP4294A electric impedance analyzer (Agilent Technology 4294A) and special fixture (Agilent Technology 16047E) the measuring samples magnet ring 10kHz feeble field, calculate the initial permeability of material; With the Bs of SY-8258 type B-H tester at 50Hz, 1200A/m, 100 ℃ of following specimen magnet rings; With the power loss of Model 2335 Watt Meter specimen magnet rings under 100kHz, 200mT, condition of different temperatures, the result lists in the table 2.
In table 2 example illustrated, 9～17 is the embodiment of the invention, and 18～21 is comparative example.
Can know by the data in the table 2:
1) all within limited range of the present invention, the magnetic core performance index are up to standard fully for embodiment 11～17 dopings.
2) comparative example 18-21 doping exceeds limited range of the present invention: the first auxiliary material Co of comparative example 18 wherein
2O
3Addition is lower than the lower limit that the present invention limits, K
1The value undercompensation fails to realize the wide-temperature and low-consumption characteristic; The second auxiliary material NiO addition of comparative example 19 is lower than the lower limit that the present invention limits, and two peak temperatures are significantly on the low side, and high temperature consumption worsens; The second auxiliary material Li of comparative example 20
2CO
3Addition exceeds the upper limit that the present invention limits, and two peak temperatures are significantly higher, and the normal temperature loss worsens; The 3rd auxiliary material CaCO of comparative example 20
3, Nb
2O
5Addition is lower than the lower limit that the present invention limits, and overall losses is higher.
Described the present invention above, still, should be appreciated that these preferred embodiments are not to be used to limit protection scope of the present invention through preferred embodiment.On the contrary, any modification of within purport of the present invention and principle, being done, be equal to replacement, improvement etc., all should be included within the protection scope of the present invention that is defined by the following claims.
Claims (10)
1. a MnZn ferrite core is become to be grouped into assisting by principal component, principal component consist of Fe
2O
3: 54～56 mol%, ZnO:5～10 mol%, surplus is a manganese oxide, three's sum is counted 100 mol%; Auxilliary composition comprises first auxiliary material, second auxiliary material, the 3rd auxiliary material and the 4th auxiliary material, and wherein, first auxiliary material is the oxide of Co, and it is 2500～4500ppm at ferrite magnetic content in the heart; Second auxiliary material is that addition is the Ni of 4300～8500 ppm
2O
3, addition is that NiO or the addition of 4000～8000 ppm is 1000～2500 ppm Li
2CO
3In a kind of; The 3rd auxiliary material is that addition is the CaCO of 100～500 ppm
3With addition be the Nb of 100～500 ppm
2O
5The 4th auxiliary material is selected from SiO
2, V
2O
5, ZrO
2, its addition is 0～500 ppm.
2. a kind of MnZn ferrite core according to claim 1 is characterized in that: principal component consist of Fe
2O
3: 54.5～55.5 mol%, ZnO:6～9 mol%, surplus is a manganese oxide, three's sum is counted 100 mol%.
3. a kind of MnZn ferrite core according to claim 1 and 2 is characterized in that: first auxiliary material is that addition is the Co of 3000～4500 ppm
2O
3, the CoO of 2500～4000 ppm or the Co of 2500～4500 ppm
3O
4
4. the manufacturing approach of any said MnZn ferrite core of claim 1～3 comprises the steps:
1) based on the composition of MnZn ferrite core, take by weighing principal component, or at least a in principal component and first auxiliary material and second auxiliary material; Adding water stirs; Grind mixing, spray-drying obtains powder, and the gained powder is warming up to 900 ℃～1050 ℃ with the programming rate of 150～200 ℃/h; Be incubated 1～3 hour, the cooling come out of the stove the pre-burning material;
2) with pre-burning material, the auxiliary material, water, dispersant, the antifoaming agent mixing that do not add or do not add fully as yet, regrind to powder particle size is 0.8～1.2 μ m, adds organic bond, mixing, and spray drying obtains the particulate material that is used to be shaped;
3) aqueous solution with particulate material and organic bond carries out batch mixing, and the moisture content of control particulate material is 0.2～0.4%, is pressed into green compact;
4) with green sintering, grinding obtains the MnZn ferrite core.
5. method according to claim 4 is characterized in that: the sintering temperature of green compact is 1200 ℃～1350 ℃.
6. method according to claim 5 is characterized in that: adopt the secondary reduction sintering process during green sintering, temperature-fall period keeps equilibrium oxygen partial pres-sure.
7. method according to claim 6 is characterized in that: the computing formula of equilibrium oxygen partial pres-sure is lg (P (O
2))=a-b/T, wherein, a value 4～15, b value 10000～19000, T is an absolute temperature.
8. method according to claim 7 is characterized in that: comprise respectively in the temperature-rise period of secondary reduction sintering and the temperature-fall period and at least once be incubated platform, and be cooled to 1100 ℃ and directly charge into nitrogen later on.
9. according to any described method of claim 4～8, it is characterized in that: the MnZn ferrite that sinters adopts the through type grinding machine, and cleans with ultrasonic cleaning apparatus.
10. according to any described method of claim 9, it is characterized in that: the through type grinding machine is selected the above emery wheel of 300 orders for use.
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| CN103708815A (en) * | 2013-12-12 | 2014-04-09 | 桐乡市耀润电子有限公司 | Manganese-zinc ferrite material with secondary peak temperature of 55DEG C, high Curie point and high magnetic conductivity, and preparation method thereof |
| CN103708816A (en) * | 2013-12-12 | 2014-04-09 | 桐乡市耀润电子有限公司 | Manganese-zinc ferrite material with secondary peak temperature of 25DEG C, high Curie point and high magnetic conductivity, and preparation method thereof |
| CN103803964A (en) * | 2013-12-19 | 2014-05-21 | 上海宝钢磁业有限公司 | Manganese-zinc soft magnetic ferrite material and preparation method thereof |
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| CN104556994A (en) * | 2014-12-19 | 2015-04-29 | 江门安磁电子有限公司 | Ni-free manganese zinc ferrite material applied to (-20)-140 DEG C and manufacturing method thereof |
| CN104591712A (en) * | 2014-12-19 | 2015-05-06 | 江门安磁电子有限公司 | Low-loss manganese zinc ferrite material for temperature of 20 DEG C below zero to 140 DEG C and manufacturing method thereof |
| CN105645943A (en) * | 2015-05-25 | 2016-06-08 | 泰州茂翔电子器材有限公司 | High Bs soft magnetic ferrite material |
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| CN111233451A (en) * | 2018-11-28 | 2020-06-05 | 泰州茂翔电子器材有限公司 | High Bs, high frequency and low loss magnetic material |
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| CN112552037A (en) * | 2020-12-11 | 2021-03-26 | 江门安磁电子有限公司 | Low-loss ferrite material and preparation method thereof |
| CN115650718A (en) * | 2022-11-18 | 2023-01-31 | 浙江工业大学 | Manganese-zinc ferrite material with ultra-wide temperature, low power consumption and magnetic conductivity and temperature stability and preparation method thereof |
| CN115745588A (en) * | 2022-09-23 | 2023-03-07 | 西南应用磁学研究所(中国电子科技集团公司第九研究所) | Manganese-zinc ferrite material with high performance factor and preparation method thereof |
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