CN105384435B - A kind of 4 yuan of formula superelevation Bs MnZn ferrite materials and preparation method - Google Patents
A kind of 4 yuan of formula superelevation Bs MnZn ferrite materials and preparation method Download PDFInfo
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Abstract
The invention discloses a kind of 4 yuan of formula superelevation Bs MnZn ferrite materials and preparation method.It is mainly di-iron trioxide, manganese oxide, zinc oxide and nickel oxide including principal component, and auxiliary element is mainly calcium carbonate and zirconium dioxide, and wherein auxiliary element also has the one or more in tungstic acid, molybdenum trioxide and niobium pentaoxide, by Fe2O3, MnO, ZnO, NiO composition raw material mixed in sand mill, after drying, depress to cake in 10Mpa pressure, then carry out pre-burning；On the basis of the powder quality after pre-burning, the auxiliary element for adding respective amount carries out secondary sand milling, and testing graininess is done in secondary sand milling slurry drying；Mist projection granulating is carried out after adding PVA, standard toroidal magnetic core is shaped to and is sintered.The beneficial effects of the invention are as follows：Its high Bs characteristic can be made full use of, and temperature rise can be also met；Material cost can better meet performance and cost needs that high-power high power density power transformer designs also well below magnetic core material simultaneously.
Description
Technical field
The present invention relates to soft magnetic ferrite correlative technology field, refers in particular to a kind of 4 yuan of formulas superelevation Bs MnZn iron
Ferrite and preparation method.
Background technology
With being increasingly miniaturized for electronic product, corresponding power supply has to realize that high power density designs.Realize electricity
Magnetic core miniaturization, flattening in the high power density in source, wherein electronic component are keys therein.And to realize magnetic core
The high power density design of miniaturization, flattening and power supply just needs high Bs, low-loss magnetic material.
In the high-power transformer design field such as some new energy photovoltaic DC-to-AC converters and charging pile, it is necessary to consider corpusculum simultaneously
Product design and temperature rise design.The saturation flux density Bs of 100 DEG C conventional of power ferrite material high temperature generally only has 400mT left
The right side, even the high Bs materials PC90 that TDK companies release now, saturation flux density Bs is under the conditions of 100 DEG C of high temperature
450mT, and the loss at 100 DEG C is less than 320kw/m3.Its Bs value still can not meet the need such as photovoltaic industry and automotive field
Will higher Bs application.More design uses metal magnetic powder core at present, and widely used is iron silica-alumina material, its high temperature Bs
For 900mT or so.It is 4000kw/m but its magnetic core power attenuation is very high3, so high power attenuation also limit itself
The application of high Bs characteristics.So developing a kind of higher Bs and low-loss Ferrite Material just seems more important.
The content of the invention
The present invention is above-mentioned in order to overcome the shortcomings of to exist in the prior art, there is provided a kind of high Bs and low-loss MnZn
Ferrite Material and preparation method.
To achieve these goals, the present invention uses following technical scheme：
A kind of 4 yuan of formulas superelevation Bs MnZn ferrite materials, including di-iron trioxide, manganese oxide, zinc oxide and nickel oxide,
Wherein each composition is using molar fraction as metering, the Fe2O3Content is 59.4~67.7mol%, the MnO contents are 12.1~
20.2mol%, the ZnO content are 12.2~20.6mol%, and the NiO contents are 1.2~8.3mol%.
Preferably, also include auxiliary element, predominantly calcium carbonate and titanium dioxide, wherein also tungstic acid, three oxygen
Change the one or more in molybdenum and niobium pentaoxide, using the ppm of mass fraction for metering, the calcium carbonate content for 400ppm~
1000ppm, zirconium dioxide content are 100~300ppm, WO3Content is 100~500ppm, the MoO3Content be 100~
600ppm, the Nb2O5Content is 100~450ppm.Wherein：The usage amount of calcium carbonate and zirconium dioxide is to prepare conventional MnZn
The usage amount of Ferrite Material.
Present invention also offers the preparation method of a kind of 4 yuan formula superelevation Bs MnZn ferrite materials, concrete operation step
It is as follows：
(1) by Fe2O3, MnO, ZnO, NiO composition raw material mixed in sand mill, after drying, under 10Mpa pressure
Cake is pressed into, then carries out pre-burning；
(2) on the basis of the powder quality after pre-burning, the auxiliary element for adding respective amount carries out secondary sand milling, secondary sand milling
Testing graininess is done in slurry drying；
(3) mist projection granulating is carried out after adding PVA, standard toroidal magnetic core is shaped to and is sintered.
Preferably, in step (3), sintering process is as follows：1340 DEG C~1380 DEG C of holding temperature；From 600 DEG C~guarantor
The temperature of temperature section, 3~15 DEG C/min of heating rate；The oxygen concentration 0~4.5% of soaking zone；During cooling, oxygen concentration is by balance
Oxygen concentration carries out atmosphere protection cooling.Wherein：Time used in soaking zone is to prepare used in conventional MnZn ferrite material
Time, and cool the technique that uses also to prepare conventional MnZn ferrite material used by technique.
Preferably, the MnZn ferrite material of gained is prepared under 50Hz, 1194A/m test conditions, and at 25 DEG C, saturation
Magnetic induction density B s is more than 600mT；At 100 DEG C, saturation induction density Bs is more than 500mT.
Preferably, the MnZn ferrite material of gained is prepared under 100kHz, 200mT test conditions, and at 25 DEG C, power
Loss is less than 1000kw/m3；At 60 DEG C, power attenuation is less than 800kw/m3；At 100 DEG C, power attenuation is less than 1250kw/m3。
The beneficial effects of the invention are as follows：With high Bs, low-loss feature；Its high Bs characteristic can be made full use of, and
Temperature rise can be also met；It is close to better meet high-power high power also well below magnetic core material for material cost simultaneously
Spend the performance and cost needs of power transformer design.
Embodiment
With reference to embodiment, the present invention will be further described.
Embodiment 1：
By by 65.5mol% Fe2O3, the original of 19.3mol% MnO, 14mol% ZnO, 1.2mol% NiO compositions
Material mixes 1 hour, after drying in sand mill, the cake that external diameter is 100mm is depressed in 10Mpa pressure, then at 800 DEG C
Lower pre-burning 2~4 hours.On the basis of the powder quality after pre-burning, auxiliary element, the auxiliary of addition are added in above-mentioned Preburning material
Composition (ppm) is：600ppm CaCO3, 200ppm ZrO2, 120ppm WO3, 200ppm MoO3, 400ppm Nb2O5。
Then secondary sand milling 140min is carried out, testing graininess is done in secondary sand milling slurry drying, and SMD is 0.9~1.1 μm, and X50 is 1~
1.15 μm, X90 is less than 3 μm, carries out mist projection granulating after adding PVA, the standard toroidal magnetic core for being shaped to Φ 25*15*8 is burnt
Knot.600 DEG C~1360 DEG C heating rates, 5 DEG C/min, 6 hours are incubated at 1360 DEG C, oxygen concentration 2.5% is dense by balance oxygen
Degree carries out atmosphere protection cooling.
With SY-8258 type B-H testers in 50Hz, 1194A/m, the Bs that 25 DEG C and 100 DEG C of test, in 100kHz, 200mT
Lower test 25 DEG C, 60 DEG C, 100 DEG C of power consumption.Formula is shown in Table 1 with test result, similarly hereinafter.
Embodiment 2：
It is formulated and is：63.5mol% Fe2O3, 16.5mol% MnO, 16mol% ZnO, 4mol% NiO, make work
Skill, sintering process and test condition are identical with example 1.
Embodiment 3：
It is formulated and is：61.5mol% Fe2O3, 14.5mol% MnO, 18mol% ZnO, 6mol% NiO, make work
Skill, sintering process and test condition are identical with example 1.
Embodiment 4：
It is formulated and is：59.5mol% Fe2O3, 12.2mol% MnO, 20mol% ZnO, 8.3mol% NiO, make
Technique, sintering process and test condition are identical with example 1.
Comparative example 1：
It is formulated and is：68mol% Fe2O3, 16mol% MnO, 12mol% ZnO, 4mol% NiO, manufacture craft,
Sintering process and test condition are identical with example 1.
Comparative example 2：
It is formulated and is：59mol% Fe2O3, 16mol% MnO, 21mol% ZnO, 4mol% NiO, manufacture craft,
Sintering process and test condition are identical with example 1.
Comparative example 3：
It is formulated and is：67.8mol% Fe2O3, 15.2mol% MnO, 16mol% ZnO, 1mol% NiO, make work
Skill, sintering process and test condition are identical with example 1.
Comparative example 4：
It is formulated and is：59.2mol% Fe2O3, 16.3mol% MnO, 16mol% ZnO, 8.5mol% NiO, make
Technique, sintering process and test condition are identical with example 1.
Comparative example 5：
It is formulated and is：61.5mol% Fe2O3, 16.4mol% MnO, 21mol% ZnO, 1.1mol% NiO, make
Technique, sintering process and test condition are identical with example 1.
Comparative example 6：
It is formulated and is：61.5mol% Fe2O3, 18mol% MnO, 12mol% ZnO, 8.5mol% NiO, make work
Skill, sintering process and test condition are identical with example 1.
Table 1
Embodiment 5：
By by 63.5mol% Fe2O3, the former material of 16.5mol% MnO, 16mol% ZnO, 4mol% NiO compositions
Material mixes 1 hour in sand mill, after drying, cake is depressed in 10Mpa pressure, then pre-burning 2~4 hours at 800 DEG C.
On the basis of the powder quality after pre-burning, auxiliary element is added in above-mentioned Preburning material, the auxiliary element (ppm) of addition is：
600ppm CaCO3, 200ppm ZrO2, 120ppm WO3, 200ppm MoO3, 400ppm Nb2O5.Then carry out secondary
140min is sanded, testing graininess is done in secondary sand milling slurry drying, and SMD is 0.9~1.1 μm, and X50 is 1~1.15 μm, and X90 is small
In 3 μm, mist projection granulating is carried out after adding PVA, the standard toroidal magnetic core for being shaped to Φ 25*15*8 is sintered.600 DEG C~1360
DEG C 5 DEG C/min of heating rate, 6 hours are incubated at 1360 DEG C, oxygen concentration 2.5%, atmosphere protection are carried out by balance oxygen concentration
Cooling.Note：The embodiment is same as Example 2.
With SY-8258 type B-H testers in 50Hz, 1194A/m, the Bs that 25 DEG C and 100 DEG C of test, in 100kHz, 200mT
Lower test 25 DEG C, 60 DEG C, 100 DEG C of power consumption.Formula is shown in Table 2 with test result, similarly hereinafter.
Embodiment 6：
Auxiliary element is changed to 600ppm CaCO3, 200ppm ZrO2, 250ppm WO3, 300ppm MoO3, 350ppm
Nb2O5, manufacture craft, sintering process and test condition are identical with example 5.
Embodiment 7：
Auxiliary element is changed to 600ppm CaCO3, 200ppm ZrO2, 350ppm WO3, 200ppm MoO3, 300ppm
Nb2O5, manufacture craft, sintering process and test condition are identical with example 5.
Embodiment 8：
Auxiliary element is changed to 600ppm CaCO3, 200ppm ZrO2, 450ppm WO3, 120ppm MoO3, 150ppm
Nb2O5, manufacture craft, sintering process and test condition are identical with example 5.
Comparative example 7：
Auxiliary element is changed to 600ppm CaCO3, 200ppm ZrO2, 600ppm WO3, 0ppm MoO3, 300ppm's
Nb2O5, manufacture craft, sintering process and test condition are identical with example 5.
Comparative example 8：
Auxiliary element is changed to 600ppm CaCO3, 200ppm ZrO2, 0ppm WO3, 700ppm MoO3, 300ppm's
Nb2O5, manufacture craft, sintering process and test condition are identical with example 5.
Comparative example 9：
Auxiliary element is changed to 600ppm CaCO3, 200ppm ZrO2, 600ppm WO3, 300ppm MoO3, 0ppm's
Nb2O5, manufacture craft, sintering process and test condition are identical with example 5.
Comparative example 10：
Auxiliary element is changed to 600ppm CaCO3, 200ppm ZrO2, 0ppm WO3, 300ppm MoO3, 500ppm's
Nb2O5, manufacture craft, sintering process and test condition are identical with example 5.
Comparative example 11：
Auxiliary element is changed to 600ppm CaCO3, 200ppm ZrO2, 300ppm WO3, 700ppm MoO3, 0ppm's
Nb2O5, manufacture craft, sintering process and test condition are identical with example 5.
Comparative example 12：
Auxiliary element is changed to 600ppm CaCO3, 200ppm ZrO2, 300ppm WO3, 0ppm MoO3, 500ppm's
Nb2O5, manufacture craft, sintering process and test condition are identical with example 5.
Table 2
Embodiment 9：
The main compositing formula of material, auxiliary element compositing formula, manufacture craft are identical with example 5.Sintering curre is changed to 600
~1340 DEG C of heating rates are changed to 3 DEG C/min, and soaking zone oxygen concentration is set to 0%, and holding temperature is 1340 DEG C.Pre-burning and sintering
Technique is shown in Table 2 with test result, similarly hereinafter.
Embodiment 10：
The main compositing formula of material, auxiliary element compositing formula, manufacture craft are identical with example 5.Sintering curre is changed to 600
~1360 DEG C of heating rates are changed to 9 DEG C/min, and soaking zone oxygen concentration is set to 2%, and holding temperature is 1360 DEG C.
Embodiment 11：
The main compositing formula of material, auxiliary element compositing formula, manufacture craft are identical with example 5.Sintering curre is changed to 600
~1380 DEG C of heating rates are changed to 15 DEG C/min, and soaking zone oxygen concentration is set to 4.5%, and holding temperature is 1380 DEG C.
Comparative example 13：
The main compositing formula of material, auxiliary element compositing formula are identical with example 5.Raw material mix 1 hour in sand mill
After drying, it is identical with example 5 directly to divide the pre-burning in saggar, subsequent manufacturing processes and sintering process.
Comparative example 14：
The main compositing formula of material, auxiliary element compositing formula, manufacture craft are identical with example 5.Sintering curre is changed into 600
DEG C~1330 DEG C of heating rates are changed into 16 DEG C/min, holding temperature is 1330 DEG C.
Comparative example 15：
The main compositing formula of material, auxiliary element compositing formula, manufacture craft are identical with example 5.Sintering curre is changed into 600
DEG C~1390 DEG C of heating rates are changed into 2 DEG C/min, holding temperature is 1390 DEG C.
Comparative example 16：
The main compositing formula of material, auxiliary element compositing formula, manufacture craft are identical with example 5.By soaking zone oxygen concentration
5% is set to, holding temperature is set to 1330 DEG C.
Comparative example 17：
The main compositing formula of material, auxiliary element compositing formula, manufacture craft are identical with example 5.By soaking zone oxygen concentration
5% is set to, holding temperature is set to 1390 DEG C.
Comparative example 18：
The main compositing formula of material, auxiliary element compositing formula, manufacture craft are identical with example 5.Sintering curre is changed into 600
~1360 DEG C of heating rates are set to 16 DEG C/min, and soaking zone oxygen concentration is set into 5%.
Comparative example 19：
The main compositing formula of material, auxiliary element compositing formula, manufacture craft are identical with example 5.Sintering curre is changed into 600
~1360 DEG C of heating rates are set to 2 DEG C/min, and soaking zone oxygen concentration is set into 5%.
Table 3
Claims (3)
1. a kind of 4 yuan of formulas superelevation Bs manganese-zinc ferrites, it is characterized in that, including di-iron trioxide, manganese oxide, zinc oxide and oxidation
Nickel, wherein each composition is using molar fraction as metering, Fe2O3Content is 59.4~67.7mol%, MnO contents are 12.1~
20.2mol%, ZnO content are 12.2~20.6mol%, and NiO contents are 1.2~8.3mol%, in addition to auxiliary element, predominantly
Calcium carbonate and zirconium dioxide, wherein also tungstic acid, molybdenum trioxide and niobium pentaoxide, using the ppm of mass fraction as metering,
Calcium carbonate content is 400~1000ppm, and zirconium dioxide content is 100~300ppm, WO3Content is 100~500ppm, MoO3Contain
Measure as 100~600ppm, Nb2O5Content is 100~450ppm；Wherein 4 yuan formula superelevation Bs manganese-zinc ferrites are through procedure below system
It is standby to form：
（1）By Fe2O3, MnO, ZnO, NiO composition raw material mixed in sand mill, after drying, depressed in 10MPa pressure
Cake, then carry out pre-burning；
（2）On the basis of the powder quality after pre-burning, the auxiliary element for adding respective amount carries out secondary sand milling, secondary sand milling slurry
Testing graininess is done in drying；
（3）Mist projection granulating is carried out after adding PVA, standard toroidal magnetic core is shaped to and is sintered；Sintering process is as follows：Holding temperature
1340 DEG C~1380 DEG C；From the temperature of 600 DEG C~soaking zone, 3~15 DEG C/min of heating rate；The oxygen concentration 0 of soaking zone~
4.5%；During cooling, oxygen concentration carries out atmosphere protection cooling by balance oxygen concentration.
2. it is according to claim 1 it is a kind of 4 yuan formula superelevation Bs manganese-zinc ferrites, it is characterized in that, prepare gained MnZn
Ferrite Material is under 50Hz, 1194A/m test condition, and at 25 DEG C, saturation induction density Bs is more than 600mT；At 100 DEG C,
Saturation induction density Bs is more than 500mT.
3. it is according to claim 1 it is a kind of 4 yuan formula superelevation Bs manganese-zinc ferrites, it is characterized in that, prepare gained MnZn
Ferrite Material is under 100kHz, 200mT test conditions, and at 25 DEG C, power attenuation is less than 1000kW/m3；At 60 DEG C, power damage
Consumption is less than 800kW/m3；At 100 DEG C, power attenuation is less than 1250kW/m3。
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| CN107540360B (en) * | 2016-06-25 | 2020-12-04 | 临沂春光磁业有限公司 | Ferrite material with high saturation magnetic induction intensity and high direct current superposition |
| CN106336212A (en) * | 2016-08-28 | 2017-01-18 | 安徽华林磁电科技有限公司 | Ni-Zn soft magnetic ferrite used for transformer U-type part |
| CN108911732B (en) * | 2018-07-06 | 2020-10-23 | 横店集团东磁股份有限公司 | High Bs ferrite sheet for wireless charging and preparation method thereof |
| CN113735574A (en) * | 2021-09-30 | 2021-12-03 | 海宁辉恒磁业有限公司 | Ultrahigh BsLow-loss manganese-zinc ferrite material and preparation method thereof |
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| JP4523430B2 (en) * | 2005-01-18 | 2010-08-11 | Ｊｆｅフェライト株式会社 | High saturation magnetic flux density Mn-Zn-Ni ferrite |
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| CN101429017A (en) * | 2008-12-06 | 2009-05-13 | 广东风华高新科技股份有限公司 | Ferrite magnetic core for network communication and method for producing the same |
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Denomination of invention: A 4-element formula ultra-high Bs manganese zinc ferrite material and its preparation method Effective date of registration: 20230522 Granted publication date: 20180309 Pledgee: Dongyang Branch of China Construction Bank Co.,Ltd. Pledgor: HENGDIAN GROUP DMEGC MAGNETICS Co.,Ltd. Registration number: Y2023330000949 |