CN105384435A - Manganese-zinc ferrite material with quaternary formula and ultrahigh Bs and preparation method - Google Patents
Manganese-zinc ferrite material with quaternary formula and ultrahigh Bs and preparation method Download PDFInfo
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Abstract
The invention discloses a manganese-zinc ferrite material with a quaternary formula and ultrahigh Bs and a preparation method. The manganese-zinc ferrite material comprises main components and auxiliary components, wherein the main components are mainly ferric oxide, manganese oxide, zinc oxide and nickel oxide; the auxiliary components are mainly calcium carbonate and zirconium dioxide and also include one or more of tungsten trioxide, molybdenum trioxide and niobium pentoxide. The preparation method comprises the following steps: mixing raw materials formed by Fe2O3, MnO, ZnO and NiO in a sand mill, pressing the mixture into a cake at a pressure of 10Mpa after drying the mixture and then presintering the cake; based on the mass of the powder obtained after presintering, adding a corresponding quantity of auxiliary components, carrying out secondary sand milling and drying the slurry obtained after secondary sand milling to particle size test; adding PVA (polyvinyl alcohol), then carrying out spray granulation, to form a standard toroidal core and sintering the standard toroidal core. The manganese-zinc ferrite material has the beneficial effects that the characteristic of high Bs of the manganese-zinc ferrite material can be fully utilized and temperature rise can be also satisfied; meanwhile, the cost of the material is far lower than the costs of magnetic powder core materials and the design performances and cost requirements of power transformers with high power and high power density can be better satisfied.
Description
Technical field
The present invention relates to soft magnetic ferrite correlative technology field, refer in particular to a kind of 4 yuan of formula superelevation Bs MnZn ferrite materials and preparation method.
Background technology
Along with the continuous miniaturization of electronic product, corresponding power supply must realize high power density design.Realize the high power density of power supply, the magnetic core miniaturization wherein in electronic devices and components, flattening are keys wherein.And the miniaturization of magnetic core will be realized, the high power density design of flattening and power supply just needs high Bs, low-loss magneticsubstance.
At some high-power transformer design fields such as new forms of energy photovoltaic DC-to-AC converter and charging pile, need to consider small volume design and temperature rise design simultaneously.The saturation magnetic flux density Bs of conventional power ferrite material high temperature 100 DEG C generally only has about 400mT, even the high Bs material PC90 of TDK company release now, under high temperature 100 DEG C of conditions, saturation magnetic flux density Bs is 450mT, and the loss at 100 DEG C is less than 320kw/m
3.Its Bs value still can not meet the application of the higher Bs of the needs such as photovoltaic industry and automotive field.Current more design adopts metal magnetic powder core, and widely used is iron silica-alumina material, and its high temperature Bs is about 900mT.But its magnetic core power loss is very high, be 4000kw/m
3, so high power loss also limit the application of itself high Bs characteristic.So the exploitation higher Bs of one and low-loss Ferrite Material just seems more important.
Summary of the invention
There is above-mentioned deficiency to overcome in prior art in the present invention, provides a kind of high Bs and low-loss MnZn ferrite material and preparation method.
To achieve these goals, the present invention is by the following technical solutions:
A kind of 4 yuan of formula superelevation Bs MnZn ferrite materials, comprise ferric oxide, manganese oxide, zinc oxide and nickel oxide, wherein each composition take molar fraction as metering, described Fe
2o
3content is 59.4 ~ 67.7mol%, and described MnO content is 12.1 ~ 20.2mol%, and described ZnO content is 12.2 ~ 20.6mol%, and described NiO content is 1.2 ~ 8.3mol%.
As preferably, also comprise ancillary component, be mainly calcium carbonate and titanium dioxide, wherein also have in tungstic oxide, molybdic oxide and Niobium Pentxoxide one or more, with the ppm of massfraction for metering, described calcium carbonate content is 400ppm ~ 1000ppm, and zirconium dioxide content is 100 ~ 300ppm, WO
3content is 100 ~ 500ppm, described MoO
3content is 100 ~ 600ppm, described Nb
2o
5content is 100 ~ 450ppm.Wherein: the usage quantity of calcium carbonate and zirconium dioxide is prepare the usage quantity of conventional MnZn ferrite material.
Present invention also offers a kind of preparation method of 4 yuan of formula superelevation Bs MnZn ferrite materials, concrete operation step is as follows:
(1) by Fe
2o
3, MnO, ZnO, NiO composition starting material mix in sand mill, after oven dry, become cake at 10Mpa pressure, then carry out pre-burning;
(2) with the powder quality after pre-burning for benchmark, the ancillary component adding respective amount carries out secondary sand milling, secondary sand milling slip dry do testing graininess;
(3) carry out mist projection granulating after adding PVA, be shaped to standard toroidal magnetic core and sinter.
As preferably, in step (3), sintering process is as follows: holding temperature 1340 DEG C ~ 1380 DEG C; From the temperature of 600 DEG C ~ holding-zone, temperature rise rate 3 ~ 15 DEG C/min; The oxygen concentration 0 ~ 4.5% of holding-zone; During cooling, oxygen concentration carries out atmosphere protection cooling by balance oxygen concentration.Wherein: holding-zone time used is the conventional MnZn ferrite material of preparation time used, and the technique that cooling adopts is also for preparing the technique that conventional MnZn ferrite material adopts.
As preferably, prepare the MnZn ferrite material of gained under 50Hz, 1194A/m test condition, when 25 DEG C, saturation induction density Bs is greater than 600mT; When 100 DEG C, saturation induction density Bs is greater than 500mT.
As preferably, prepare the MnZn ferrite material of gained under 100kHz, 200mT test condition, when 25 DEG C, power loss is less than 1000kw/m
3; When 60 DEG C, power loss is less than 800kw/m
3; When 100 DEG C, power loss is less than 1250kw/m
3.
The invention has the beneficial effects as follows: there is high Bs, low-loss feature; Can make full use of its high Bs characteristic, and temperature rise also can be met; Material cost is also well below powder core material simultaneously, can better meet performance and the cost needs of the design of high-power high power density supply transformer.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1:
By the Fe by 65.5mol%
2o
3, the starting material of the NiO composition of the ZnO of the MnO of 19.3mol%, 14mol%, 1.2mol% mix 1 hour, after oven dry in sand mill, become external diameter to be the cake of 100mm at 10Mpa pressure, then pre-burning 2 ~ 4 hours at 800 DEG C.With the powder quality after pre-burning for benchmark, in above-mentioned Preburning material, add ancillary component, the ancillary component (ppm) of interpolation is: the CaCO of 600ppm
3, the ZrO of 200ppm
2, the WO of 120ppm
3, the MoO of 200ppm
3, the Nb of 400ppm
2o
5.Then carry out secondary sand milling 140min, secondary sand milling slip is dried and is done testing graininess, and SMD is 0.9 ~ 1.1 μm, and X50 is 1 ~ 1.15 μm, and X90, for being less than 3 μm, carries out mist projection granulating after adding PVA, and the standard toroidal magnetic core being shaped to Φ 25*15*8 sinters.600 DEG C ~ 1360 DEG C temperature rise rates, 5 DEG C/min, 1360 DEG C of insulations 6 hours, oxygen concentration 2.5%, carried out atmosphere protection cooling by balance oxygen concentration.
With SY-8258 type B-H tester at 50Hz, 1194A/m, test 25 DEG C with the Bs of 100 DEG C, under 100kHz, 200mT, test the power consumption of 25 DEG C, 60 DEG C, 100 DEG C.Formula and test result are in table 1, lower same.
Embodiment 2:
Formula is: the Fe of 63.5mol%
2o
3, the NiO of the ZnO of the MnO of 16.5mol%, 16mol%, 4mol%, manufacture craft, sintering process and test condition are identical with example 1.
Embodiment 3:
Formula is: the Fe of 61.5mol%
2o
3, the NiO of the ZnO of the MnO of 14.5mol%, 18mol%, 6mol%, manufacture craft, sintering process and test condition are identical with example 1.
Embodiment 4:
Formula is: the Fe of 59.5mol%
2o
3, the NiO of the ZnO of the MnO of 12.2mol%, 20mol%, 8.3mol%, manufacture craft, sintering process and test condition are identical with example 1.
Comparative example 1:
Formula is: the Fe of 68mol%
2o
3, the NiO of the ZnO of the MnO of 16mol%, 12mol%, 4mol%, manufacture craft, sintering process and test condition are identical with example 1.
Comparative example 2:
Formula is: the Fe of 59mol%
2o
3, the NiO of the ZnO of the MnO of 16mol%, 21mol%, 4mol%, manufacture craft, sintering process and test condition are identical with example 1.
Comparative example 3:
Formula is: the Fe of 67.8mol%
2o
3, the NiO of the ZnO of the MnO of 15.2mol%, 16mol%, 1mol%, manufacture craft, sintering process and test condition are identical with example 1.
Comparative example 4:
Formula is: the Fe of 59.2mol%
2o
3, the NiO of the ZnO of the MnO of 16.3mol%, 16mol%, 8.5mol%, manufacture craft, sintering process and test condition are identical with example 1.
Comparative example 5:
Formula is: the Fe of 61.5mol%
2o
3, the NiO of the ZnO of the MnO of 16.4mol%, 21mol%, 1.1mol%, manufacture craft, sintering process and test condition are identical with example 1.
Comparative example 6:
Formula is: the Fe of 61.5mol%
2o
3, the NiO of the ZnO of the MnO of 18mol%, 12mol%, 8.5mol%, manufacture craft, sintering process and test condition are identical with example 1.
Table 1
Embodiment 5:
By the Fe by 63.5mol%
2o
3, the starting material of the NiO composition of the ZnO of the MnO of 16.5mol%, 16mol%, 4mol% mix 1 hour, after oven dry in sand mill, become cake, then pre-burning 2 ~ 4 hours at 800 DEG C at 10Mpa pressure.With the powder quality after pre-burning for benchmark, in above-mentioned Preburning material, add ancillary component, the ancillary component (ppm) of interpolation is: the CaCO of 600ppm
3, the ZrO of 200ppm
2, the WO of 120ppm
3, the MoO of 200ppm
3, the Nb of 400ppm
2o
5.Then carry out secondary sand milling 140min, secondary sand milling slip is dried and is done testing graininess, and SMD is 0.9 ~ 1.1 μm, and X50 is 1 ~ 1.15 μm, and X90, for being less than 3 μm, carries out mist projection granulating after adding PVA, and the standard toroidal magnetic core being shaped to Φ 25*15*8 sinters.600 DEG C ~ 1360 DEG C temperature rise rates, 5 DEG C/min, 1360 DEG C of insulations 6 hours, oxygen concentration 2.5%, carried out atmosphere protection cooling by balance oxygen concentration.Note: this embodiment is identical with embodiment 2.
With SY-8258 type B-H tester at 50Hz, 1194A/m, test 25 DEG C with the Bs of 100 DEG C, under 100kHz, 200mT, test the power consumption of 25 DEG C, 60 DEG C, 100 DEG C.Formula and test result are in table 2, lower same.
Embodiment 6:
Ancillary component changes the CaCO of 600ppm into
3, the ZrO of 200ppm
2, the WO of 250ppm
3, the MoO of 300ppm
3, the Nb of 350ppm
2o
5, manufacture craft, sintering process and test condition are identical with example 5.
Embodiment 7:
Ancillary component changes the CaCO of 600ppm into
3, the ZrO of 200ppm
2, the WO of 350ppm
3, the MoO of 200ppm
3, the Nb of 300ppm
2o
5, manufacture craft, sintering process and test condition are identical with example 5.
Embodiment 8:
Ancillary component changes the CaCO of 600ppm into
3, the ZrO of 200ppm
2, the WO of 450ppm
3, the MoO of 120ppm
3, the Nb of 150ppm
2o
5, manufacture craft, sintering process and test condition are identical with example 5.
Comparative example 7:
Ancillary component changes the CaCO of 600ppm into
3, the ZrO of 200ppm
2, the WO of 600ppm
3, the MoO of 0ppm
3, the Nb of 300ppm
2o
5, manufacture craft, sintering process and test condition are identical with example 5.
Comparative example 8:
Ancillary component changes the CaCO of 600ppm into
3, the ZrO of 200ppm
2, the WO of 0ppm
3, the MoO of 700ppm
3, the Nb of 300ppm
2o
5, manufacture craft, sintering process and test condition are identical with example 5.
Comparative example 9:
Ancillary component changes the CaCO of 600ppm into
3, the ZrO of 200ppm
2, the WO of 600ppm
3, the MoO of 300ppm
3, the Nb of 0ppm
2o
5, manufacture craft, sintering process and test condition are identical with example 5.
Comparative example 10:
Ancillary component changes the CaCO of 600ppm into
3, the ZrO of 200ppm
2, the WO of 0ppm
3, the MoO of 300ppm
3, the Nb of 500ppm
2o
5, manufacture craft, sintering process and test condition are identical with example 5.
Comparative example 11:
Ancillary component changes the CaCO of 600ppm into
3, the ZrO of 200ppm
2, the WO of 300ppm
3, the MoO of 700ppm
3, the Nb of 0ppm
2o
5, manufacture craft, sintering process and test condition are identical with example 5.
Comparative example 12:
Ancillary component changes the CaCO of 600ppm into
3, the ZrO of 200ppm
2, the WO of 300ppm
3, the MoO of 0ppm
3, the Nb of 500ppm
2o
5, manufacture craft, sintering process and test condition are identical with example 5.
Table 2
Embodiment 9:
The main compositing formula of material, ancillary component compositing formula, manufacture craft are identical with example 5.Sintering curre is changed into 600 ~ 1340 DEG C of temperature rise rates and change 3 DEG C/min into, holding-zone oxygen concentration is set to 0%, and holding temperature is 1340 DEG C.Pre-burning and sintering process and test result in table 2, lower with.
Embodiment 10:
The main compositing formula of material, ancillary component compositing formula, manufacture craft are identical with example 5.Sintering curre is changed into 600 ~ 1360 DEG C of temperature rise rates and change 9 DEG C/min into, holding-zone oxygen concentration is set to 2%, and holding temperature is 1360 DEG C.
Embodiment 11:
The main compositing formula of material, ancillary component compositing formula, manufacture craft are identical with example 5.Sintering curre is changed into 600 ~ 1380 DEG C of temperature rise rates and change 15 DEG C/min into, holding-zone oxygen concentration is set to 4.5%, and holding temperature is 1380 DEG C.
Comparative example 13:
The main compositing formula of material, ancillary component compositing formula are identical with example 5.Starting material mix in sand mill 1 hour dry after, directly divide pre-burning in saggar, subsequent manufacturing processes and sintering process identical with example 5.
Comparative example 14:
The main compositing formula of material, ancillary component compositing formula, manufacture craft are identical with example 5.Sintering curre is become 600 DEG C ~ 1330 DEG C temperature rise rates and become 16 DEG C/min, holding temperature is 1330 DEG C.
Comparative example 15:
The main compositing formula of material, ancillary component compositing formula, manufacture craft are identical with example 5.Sintering curre is become 600 DEG C ~ 1390 DEG C temperature rise rates and become 2 DEG C/min, holding temperature is 1390 DEG C.
Comparative example 16:
The main compositing formula of material, ancillary component compositing formula, manufacture craft are identical with example 5.Holding-zone oxygen concentration is set to 5%, and holding temperature is set to 1330 DEG C.
Comparative example 17:
The main compositing formula of material, ancillary component compositing formula, manufacture craft are identical with example 5.Holding-zone oxygen concentration is set to 5%, and holding temperature is set to 1390 DEG C.
Comparative example 18:
The main compositing formula of material, ancillary component compositing formula, manufacture craft are identical with example 5.Sintering curre is become 600 ~ 1360 DEG C of temperature rise rates and be set to 16 DEG C/min, holding-zone oxygen concentration is set to 5%.
Comparative example 19:
The main compositing formula of material, ancillary component compositing formula, manufacture craft are identical with example 5.Sintering curre is become 600 ~ 1360 DEG C of temperature rise rates and be set to 2 DEG C/min, holding-zone oxygen concentration is set to 5%.
Table 3
Claims (6)
1. 4 yuan of formula superelevation Bs MnZn ferrite materials, it is characterized in that, comprise ferric oxide, manganese oxide, zinc oxide and nickel oxide, wherein each composition take molar fraction as metering, described Fe
2o
3content is 59.4 ~ 67.7mol%, and described MnO content is 12.1 ~ 20.2mol%, and described ZnO content is 12.2 ~ 20.6mol%, and described NiO content is 1.2 ~ 8.3mol%.
2. a kind of 4 yuan of formula superelevation Bs MnZn ferrite materials according to claim 1, it is characterized in that, also comprise ancillary component, be mainly calcium carbonate and zirconium dioxide, wherein also have in tungstic oxide, molybdic oxide and Niobium Pentxoxide one or more, with the ppm of massfraction for metering, described calcium carbonate content is 400ppm ~ 1000ppm, zirconium dioxide content is 100 ~ 300ppm, WO
3content is 100 ~ 500ppm, described MoO
3content is 100 ~ 600ppm, described Nb
2o
5content is 100 ~ 450ppm.
3. one kind 4 yuan formula superelevation B
sthe preparation method of MnZn ferrite material, is characterized in that, concrete operation step is as follows:
(1) by Fe
2o
3, MnO, ZnO, NiO composition starting material mix in sand mill, after oven dry, become cake at 10Mpa pressure, then carry out pre-burning;
(2) with the powder quality after pre-burning for benchmark, the ancillary component adding respective amount carries out secondary sand milling, secondary sand milling slip dry do testing graininess;
(3) carry out mist projection granulating after adding PVA, be shaped to standard toroidal magnetic core and sinter.
4. the preparation method of a kind of 4 yuan of formula superelevation Bs MnZn ferrite materials according to claim 3, it is characterized in that, in step (3), sintering process is as follows: holding temperature 1340 DEG C ~ 1380 DEG C; From the temperature of 600 DEG C ~ holding-zone, temperature rise rate 3 ~ 15 DEG C/min; The oxygen concentration 0 ~ 4.5% of holding-zone; During cooling, oxygen concentration carries out atmosphere protection cooling by balance oxygen concentration.
5. the preparation method of a kind of 4 yuan of formula superelevation Bs MnZn ferrite materials according to claim 3 or 4, it is characterized in that, prepare the MnZn ferrite material of gained under 50Hz, 1194A/m test condition, when 25 DEG C, saturation induction density Bs is greater than 600mT; When 100 DEG C, saturation induction density Bs is greater than 500mT.
6. the preparation method of a kind of 4 yuan of formula superelevation Bs MnZn ferrite materials according to claim 3 or 4, it is characterized in that, prepare the MnZn ferrite material of gained under 100kHz, 200mT test condition, when 25 DEG C, power loss is less than 1000kw/m
3; When 60 DEG C, power loss is less than 800kw/m
3; When 100 DEG C, power loss is less than 1250kw/m
3.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107540360A (en) * | 2016-06-25 | 2018-01-05 | 临沂春光磁业有限公司 | It is a kind of that there is high saturated magnetic induction, high DC stacked Ferrite Material |
| CN108911732A (en) * | 2018-07-06 | 2018-11-30 | 横店集团东磁股份有限公司 | A kind of wireless charging high Bs ferrite sheet 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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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107540360A (en) * | 2016-06-25 | 2018-01-05 | 临沂春光磁业有限公司 | It is a kind of that there is high saturated magnetic induction, high DC stacked Ferrite Material |
| 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 |
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| CN108911732A (en) * | 2018-07-06 | 2018-11-30 | 横店集团东磁股份有限公司 | A kind of wireless charging high Bs ferrite sheet and preparation method thereof |
| 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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|---|---|
| CN105384435B (en) | 2018-03-09 |
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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 |
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