CN116813323A - Wide-temperature low-loss soft magnetic manganese zinc ferrite material suitable for 25-140 ℃ and preparation method and application thereof - Google Patents
Wide-temperature low-loss soft magnetic manganese zinc ferrite material suitable for 25-140 ℃ and preparation method and application thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 77
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 title claims description 40
- JIYIUPFAJUGHNL-UHFFFAOYSA-N [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] JIYIUPFAJUGHNL-UHFFFAOYSA-N 0.000 title claims description 40
- 238000002360 preparation method Methods 0.000 title abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 69
- 230000008569 process Effects 0.000 claims abstract description 61
- 238000005245 sintering Methods 0.000 claims abstract description 45
- 239000000654 additive Substances 0.000 claims abstract description 25
- 230000000996 additive effect Effects 0.000 claims abstract description 18
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 9
- 238000000465 moulding Methods 0.000 claims description 36
- 238000004321 preservation Methods 0.000 claims description 29
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 16
- 239000001301 oxygen Substances 0.000 claims description 16
- 229910052760 oxygen Inorganic materials 0.000 claims description 16
- 239000011230 binding agent Substances 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 14
- 229940110728 nitrogen / oxygen Drugs 0.000 claims description 14
- 238000005453 pelletization Methods 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 12
- 239000004576 sand Substances 0.000 claims description 9
- 238000005507 spraying Methods 0.000 claims description 9
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 230000000630 rising effect Effects 0.000 claims description 7
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 7
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- 239000000314 lubricant Substances 0.000 claims description 2
- 239000008188 pellet Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 229910000859 α-Fe Inorganic materials 0.000 abstract description 19
- 229910020599 Co 3 O 4 Inorganic materials 0.000 abstract description 11
- 230000006698 induction Effects 0.000 abstract description 8
- 238000005457 optimization Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 24
- 239000011701 zinc Substances 0.000 description 23
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- 238000007580 dry-mixing Methods 0.000 description 11
- 229910000831 Steel Inorganic materials 0.000 description 10
- 239000010959 steel Substances 0.000 description 10
- 238000009472 formulation Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 230000007423 decrease Effects 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 238000005461 lubrication Methods 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 238000010298 pulverizing process Methods 0.000 description 5
- 238000001694 spray drying Methods 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 3
- 239000011787 zinc oxide Substances 0.000 description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
- AXWLFOKLQGDQFR-UHFFFAOYSA-N zinc iron(2+) manganese(2+) oxygen(2-) Chemical compound [O-2].[Fe+2].[Zn+2].[Mn+2].[O-2].[O-2] AXWLFOKLQGDQFR-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T10/00—Road transport of goods or passengers
- Y02T10/60—Other road transportation technologies with climate change mitigation effect
- Y02T10/70—Energy storage systems for electromobility, e.g. batteries
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- Magnetic Ceramics (AREA)
- Soft Magnetic Materials (AREA)
Abstract
The invention discloses a wide-temperature low-loss soft magnetic Mn-Zn ferrite material suitable for 25-140 ℃ and a preparation method and application thereof, wherein the material comprises a main component and an additive, and the main component comprises Fe in mole percent 2 O 3 53 to 53.5mol percent, 9 to 10mol percent of ZnO and the balance of MnO; the additive comprises CaCO 3 、SiO 2 、Co 3 O 4 And NiO, co based on the total weight of the main component 3 O 4 ：0.33～0.4wt％，NiO：0～0.08wt％，CaCO 3 ：0.03～0.05wt％，SiO 2 :0.003 to 0.006 weight percent, obviously reduces the power consumption within the temperature range of 25 to 140 ℃ through the optimization of a formula and a sintering process, simultaneously the material has high saturation magnetic induction intensity within the temperature range of 25 to 100 ℃, and is charged on a new energy automobile in a vehicleThe machine and DC/DC converter fields have good application prospects.
Description
Technical Field
The invention belongs to the technical field of soft magnetic materials, and particularly relates to a wide-temperature low-loss soft magnetic manganese zinc ferrite material suitable for 25-140 ℃ and a preparation method and application thereof.
Background
The Mn-Zn ferrite is one kind of important soft magnetic material and is used mainly in various kinds of magnetic elements, such as transformer core, inductor, etc. In the field of automotive electronics, with the development of semiconductor and electronic packaging technologies, in order to reduce the number of wiring harnesses, the installation of an engine electronic control unit close to an engine or directly in an engine compartment has become a future technical trend, which has led to automotive electronics to operate at higher ambient temperatures, and needs to meet low power consumption requirements in a wider temperature range.
In the prior art, patent document CN115650718A discloses a manganese zinc ferrite material with ultra-wide temperature, low power consumption and magnetic permeability temperature stability and a preparation method thereof, wherein the material has small power consumption along with temperature change in an ultra-wide temperature range of 0-150 ℃, but has higher overall power consumption, 100kHz,200mT and power consumption of 374-460 kw/m at 100 DEG C 3 The power consumption at 150 ℃ is 419-466 kw/m 3 The power consumption in the normal temperature range is 400kw/m 3 Left and right. Patent document CN110078488A discloses a high-Bs wide-temperature low-loss soft magnetic ferrite material and a preparation method thereof, and the power consumption of the material at 25 ℃ and 120 ℃ is 330kw/m 3 About, the formula uses oxides of hafnium and cerium noble metals, and the low-temperature sintering is adopted, so that the sintering universality is poor, the cost is high, and the performance at 140 ℃ is avoided.
In order to solve the technical problems, the invention provides a wide-temperature low-loss soft magnetic manganese zinc ferrite material suitable for 25-140 ℃.
Disclosure of Invention
The invention aims to provide a wide-temperature low-loss soft magnetic manganese zinc ferrite material suitable for 25-140 ℃, and the material is suitable for wide-temperature application occasions of 25-140 ℃ through the compounding optimization of main components of iron, manganese and zinc and additives.
The second purpose of the invention is to provide the preparation method of the wide-temperature low-loss soft magnetic manganese zinc ferrite material suitable for 25-140 ℃, and the low-loss characteristic in the range of 25-140 ℃ is realized by compounding, optimizing and combining a sintering process of the main components of iron, manganese and zinc and additives, and meanwhile, the preparation method has high saturation induction intensity in the range of 25-100 ℃.
The third object of the invention is to provide the application of the wide-temperature low-loss soft magnetic manganese zinc ferrite material suitable for 25-140 ℃ in OBC and DC/DC converters of electric vehicles.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the invention provides a wide-temperature low-loss soft magnetic manganese zinc ferrite material suitable for 25-140 ℃, which comprises a main component and an additive; wherein:
the main component comprises the following components in mole percent: fe (Fe) 2 O 3 :53 to 53.5mol percent, znO: 9-10 mol% and the balance of MnO;
the additive comprises the following main components in percentage by mass: co (Co) 3 O 4 ：0.33～0.4wt％，NiO：0～0.08wt％，CaCO 3 ：0.03～0.05wt％，SiO 2 ：0.003～0.006wt％。
The invention optimizes Fe 2 O 3 、Co 3 O 4 The proportion of NiO, and strictly control Fe 2 O 3 、Co 3 O 4 The content of NiO realizes the low-loss characteristic of the Mn-Zn ferrite material in a wide temperature range, and simultaneously has higher saturation induction intensity. Wherein: fe (Fe) 2 O 3 Too high a content leads to a decrease in resistivity, especially a significant increase in high temperature section losses; fe (Fe) 2 O 3 If the content is too low, on one hand, the ferrous ion content is reduced, the magnetocrystalline anisotropy cannot be balanced, the overall power consumption can be increased, the saturation magnetic induction intensity is reduced, and on the other hand, the room temperature loss is particularly increased remarkably, so that the standby power consumption of automobile electronics is not facilitated. Co (Co) 3 O 4 The magnetic crystal anisotropy value is increased due to the excessively high content, and the overall power consumption of a temperature zone is increased; co (Co) 3 O 4 If the content is too low, the loss at room temperature and high temperature is too high, which is unfavorable for low loss in a wide temperature range. Too high a NiO content increases magnetocrystalline anisotropy, resulting in an increase in overall power consumption, especially in room temperature power consumption.
The invention also provides a preparation method of the wide-temperature low-loss soft magnetic manganese zinc ferrite material suitable for 25-140 ℃, which comprises the following steps:
(1) Weighing Fe according to the proportion of the main component 2 O 3 Mixing MnO and ZnO raw materials, pelletizing and presintering to obtain a presintering material;
(2) The presintered material is coarsely crushed, then an additive is added for sanding, a binder is added for spray granulation and molding sintering, and the wide-temperature low-loss soft magnetic manganese zinc ferrite material suitable for 25-140 ℃ is obtained.
The invention adopts dry pelletizing and presintering, ensures the uniform mixing of the main component and the additive through one-time dry mixing and one-time wet grinding, adopts sintering at higher temperature and balanced oxygen partial pressure, ensures the density of the finished product, has low cost and good presintering and sintering stability, and is beneficial to industrial production.
Preferably, in the step (1), the size of the pelletizing is 3-8 mm, so that the uniformity of the strength of the pellets and the presintering is ensured.
Preferably, in the step (1), the presintering temperature is 950-1000 ℃ and the presintering time is 5-7 h.
Preferably, in the step (2), the sand grain diameter used in the sand grinding is 1.5-2.4 μm.
Preferably, in step (2), the weight of the binder added by the spray granulation is from 0.5 to 2% of the dry weight of the sanding slurry.
Preferably, in step (2), the binder comprises polyvinyl alcohol.
Preferably, in step (2), the binder is added in an amount of 0.75 to 1.5% by weight of the dry weight of the sanding slurry.
Preferably, in the step (2), the spraying flow rate after the binder is added in the spraying granulation process is 1.5-2.4L/h.
Preferably, in the step (2), zinc stearate of 0.1wt% in terms of molding weight percentage is added as a lubricant during the molding and sintering.
Preferably, in the step (2), the molding pressure is applied in the process of molding and sintering and is 3.5-5 MPa.
Preferably, in the step (2), the temperature rising process of the molding sintering adopts a nitrogen/oxygen mixed atmosphere, and the oxygen partial pressure is 0-0.2% at 900-1250 ℃.
Preferably, in the step (2), the heat preservation temperature is 1330-1360 ℃ and the heat preservation time is 4-6 hours in the molding and sintering process; the heat preservation process adopts a nitrogen/oxygen mixed atmosphere, and the equilibrium oxygen partial pressure in the heat preservation process is 4-6%.
Preferably, in the step (2), the cooling rate in the cooling process of the molding sintering is 1-3 ℃/min.
The invention also provides application of the wide-temperature low-loss soft magnetic manganese zinc ferrite material suitable for 25-140 ℃ in an electric vehicle-mounted charger (OBC) and a DC/DC converter.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention provides a wide-temperature low-loss soft magnetic Mn-Zn ferrite material suitable for 25-140 ℃, which is prepared from Fe 2 O 3 、Co 3 O 4 The proportion of NiO is optimized and strictly controlled, so that the wide-temperature low-loss performance and high saturation magnetic induction intensity of the Mn-Zn ferrite in the range of 25-140 ℃ are realized, and the power consumption at 25 ℃ is only 310-360 kw/m 3 The power consumption at 140 ℃ is only 350-370 kw/m 3 The saturation magnetic induction intensity at 25 ℃ and 100 ℃ is respectively above 530 mT and 420 mT.
(2) The invention adopts high-temperature sintering and balanced oxygen partial pressure sintering, ensures the sintering compactness, thereby improving the mechanical strength and saturation magnetic induction strength of the material, has good sintering stability, is beneficial to mass production and manufacture, and has wide market prospect when used for OBC and DC/DC converters of electric automobiles.
Drawings
Fig. 1 is a graph showing comparison of power consumption temperature curves of example 2 and comparative example 2.
Detailed Description
The invention is further illustrated in the following figures and specific examples, which are included to illustrate the invention and are not intended to limit the scope of the invention.
Example 1
The embodiment provides a manganese-zinc ferrite material comprising a main component of iron-manganese-zinc oxide and an additive, wherein the main component comprises Fe in mole percent 2 O 3 :53.25mol%, znO:9.3mol% with the balance MnO; the additive comprises CaCO based on the total weight of the main component 3 ：0.035wt％，SiO 2 ：0.006wt％，Co 3 O 4 :0.35wt%, niO:0wt%. The preparation method of the manganese zinc ferrite material comprises the following steps:
(1) Dry mixing the raw materials according to the proportion of the main components, adding a small amount of water for pelletizing, presintering at 1000 ℃ to obtain the presintering material, wherein the dry mixing time is 10min, the pelletizing size distribution is 3-8 mm, and the presintering time is 5h.
(2) Coarse pulverizing the presintered material, adding additives in proportion, sanding for 60min, adding 0.95wt% of polyvinyl alcohol binder, granulating by a spray drying tower, and molding and sintering to obtain the manganese zinc ferrite material.
Wherein, steel balls and pure water are used as grinding media in the sanding process, and the mass ratio of the steel balls to the water to the dry powder is 8:1:1.6; the average grain diameter of sand grinding is 1.5-2.4 mu m; the spraying flow rate is 1.5L/h; zinc stearate accounting for 0.1 weight percent of the molding weight percentage is added in the molding process to be used as lubrication, and the molding pressure is 4MPa; the temperature rising process of the sintering process adopts a nitrogen/oxygen mixed atmosphere, and the oxygen partial pressure is 0.1% at 900-1250 ℃; the heat preservation temperature in the sintering process is 1340 ℃ and the heat preservation time is 5 hours; the heat preservation process adopts a nitrogen/oxygen mixed atmosphere, and the equilibrium oxygen partial pressure in the heat preservation process is 4%; the cooling rate in the cooling process in the sintering process is 3 ℃/min.
Comparative example 1
This comparative example provides a Mn-Zn ferrite material differing from example 1 in that the main component of the Mn-Zn ferrite material is heavy, fe 2 O 3 The content of ZnO is 53.76mol percentThe content was unchanged, the balance of MnO was adjusted to 36.94mol%, and the other formulation and preparation method were the same as in example 1.
Example 2
The embodiment provides a Mn-Zn ferrite material comprising a main component of Fe-Mn-Zn oxide and an additive, the main component comprising Fe in mole percent 2 O 3 :53.2mol%, znO:9.5mol% with the balance MnO; the additive comprises CaCO based on the total weight of the main component 3 ：0.035wt％，SiO 2 ：0.006wt％，Co 3 O 4 :0.4wt%, niO:0.045wt%. The preparation method of the manganese zinc ferrite material comprises the following steps:
(1) Dry mixing the raw materials according to the proportion of the main components, adding a small amount of water for pelletizing, presintering at 980 ℃ to obtain a presintering material, wherein the dry mixing time is 10min; the size distribution of the pelletizing is 3-8 mm; the burn-in time was 5.5 hours.
(2) Coarse pulverizing the presintered material, adding additives in proportion, sanding for 60min, adding 0.95wt% of polyvinyl alcohol binder, granulating by a spray drying tower, and molding and sintering to obtain the manganese zinc ferrite material.
Wherein, steel balls and pure water are used as grinding media in the sanding process, and the mass ratio of the steel balls to the water to the dry powder is 8:1:1.6; the average grain diameter of sand grinding is 1.5-2.4 mu m; the spraying flow rate is 1.5L/h; zinc stearate accounting for 0.1 weight percent of the molding weight percentage is added in the molding process to be used as lubrication, and the molding pressure is 4.5MPa; the temperature rising process of the sintering process adopts a nitrogen/oxygen mixed atmosphere, and the oxygen partial pressure is 0.1% at 900-1250 ℃; the heat preservation temperature in the sintering process is 1350 ℃, and the heat preservation time is 4.5 hours; the heat preservation process adopts a nitrogen/oxygen mixed atmosphere, and the equilibrium oxygen partial pressure in the heat preservation process is 5%; the cooling rate in the cooling process in the sintering process is 2.5 ℃/min.
Comparative example 2
This comparative example provides a Mn-Zn ferrite material differing from example 2 in that the main component of the Mn-Zn ferrite material is heavy, fe 2 O 3 The content was 52.5mol%, the ZnO content was unchanged, the balance of MnO was adjusted to 38.00mol%, and the other formulation and preparation method were the same as in example 2.
Example 3
The embodiment provides a Mn-Zn ferrite material comprising a main component of Fe-Mn-Zn oxide and an additive, the main component comprising Fe in mole percent 2 O 3 :53.25mol%, znO:9.4mol% with the balance MnO; the additive comprises CaCO based on the total weight of the main component 3 ：0.035wt％，SiO 2 ：0.006wt％，Co 3 O 4 :0.4wt%, niO:0.06wt%. The preparation method of the manganese zinc ferrite material comprises the following steps:
(1) Dry mixing the raw materials according to the proportion of the main components, adding a small amount of water for pelletizing, and presintering at 950 ℃ to obtain a presintered material, wherein the dry mixing time is 10min; the size distribution of the pelletizing is 3-8 mm; the burn-in time was 6.5h.
(2) Coarse pulverizing the presintered material, adding additives in proportion, sanding for 60min, adding 0.95wt% of polyvinyl alcohol binder, granulating by a spray drying tower, and molding and sintering to obtain the manganese zinc ferrite material.
Wherein, steel balls and pure water are used as grinding media in the sanding process, and the mass ratio of the steel balls to the water to the dry powder is 8:1:1.6; the average grain diameter of sand grinding is 1.5-2.4 mu m; the spraying flow rate is 1.5L/h; zinc stearate accounting for 0.1 weight percent of the molding weight percentage is added in the molding process to be used as lubrication, and the molding pressure is 4.5MPa; the temperature rising process of the sintering process adopts a nitrogen/oxygen mixed atmosphere, and the oxygen partial pressure is 0.1% at 900-1250 ℃; the heat preservation temperature in the sintering process is 1350 ℃, and the heat preservation time is 4.5 hours; the heat preservation process adopts a nitrogen/oxygen mixed atmosphere, and the equilibrium oxygen partial pressure in the heat preservation process is 5%; the cooling rate in the cooling process in the sintering process is 2.5 ℃/min.
Comparative example 3
This comparative example provides a Mn-Zn ferrite material differing from example 3 in that the main component of Mn-Zn ferrite material is heavy, co 3 O 4 The content was 0.34wt%, and the other formulation and preparation method were the same as in example 3.
Example 4
The embodiment provides a Mn-Zn ferrite material comprising a main component of Fe-Mn-Zn oxideThe main component comprises Fe in mole percent 2 O 3 :53.28mol%, znO:9.3mol% with the balance MnO; the additive comprises CaCO based on the total weight of the main component 3 ：0.035wt％，SiO 2 ：0.006wt％，Co 3 O 4 :0.36wt%, niO:0.045wt%. The preparation method of the manganese zinc ferrite material comprises the following steps:
(1) Dry mixing the raw materials according to the proportion of the main components, adding a small amount of water for pelletizing, and presintering at 950 ℃ to obtain the presintered material. The dry mixing time is 10min; the size distribution of the pelletizing is 3-8 mm; the burn-in time was 6 hours.
(2) Coarse pulverizing the presintered material, adding additives in proportion, sanding for 60min, adding 0.95wt% of polyvinyl alcohol binder, granulating by a spray drying tower, and molding and sintering to obtain the manganese zinc ferrite material.
Wherein, steel balls and pure water are used as grinding media in the sanding process, and the mass ratio of the steel balls to the water to the dry powder is 8:1:1.6; the average grain diameter of sand grinding is 1.5-2.4 mu m; the spraying flow rate is 1.5L/h; zinc stearate accounting for 0.1 weight percent of the molding weight percentage is added in the molding process to be used as lubrication, and the molding pressure is 4MPa; the temperature rising process of the sintering process adopts a nitrogen/oxygen mixed atmosphere, and the oxygen partial pressure is 0.1% at 900-1250 ℃; the heat preservation temperature in the sintering process is 1355 ℃ and the heat preservation time is 4 hours; the heat preservation process adopts a nitrogen/oxygen mixed atmosphere, and the equilibrium oxygen partial pressure in the heat preservation process is 5.2%; the cooling rate in the cooling process in the sintering process is 3 ℃/min.
Comparative example 4
This comparative example provides a Mn-Zn ferrite material differing from example 4 in that the main component of Mn-Zn ferrite material is heavy, co 3 O 4 The content was 0.45% by weight, and the other formulation and preparation method were the same as in example 4.
Example 5
The embodiment provides a Mn-Zn ferrite material comprising a main component of Fe-Mn-Zn oxide and an additive, wherein the main component comprises Fe in mole percent 2 O 3 :53.5mol%, znO:9.3mol% with the balance MnO; the additive is based on the total of the main componentsWeight, including CaCO 3 ：0.035wt％，SiO 2 ：0.006wt％，Co 3 O 4 :0.4wt%, niO:0.08wt%. The preparation method of the manganese zinc ferrite material comprises the following steps:
(1) Dry mixing the raw materials according to the proportion of the main components, adding a small amount of water for pelletizing, and presintering at 950 ℃ to obtain the presintered material. The dry mixing time is 10min; the size distribution of the pelletizing is 3-8 mm; the burn-in time was 6 hours.
(2) Coarse pulverizing the presintered material, adding additives in proportion, sanding for 60min, adding 0.95wt% of polyvinyl alcohol binder, granulating by a spray drying tower, and molding and sintering to obtain the manganese zinc ferrite material.
Wherein, steel balls and pure water are used as grinding media in the sanding process, and the mass ratio of the steel balls to the water to the dry powder is 8:1:1.6; the average grain diameter of sand grinding is 1.5-2.4 mu m; the spraying flow rate is 1.5L/h; zinc stearate accounting for 0.1 weight percent of the molding weight percentage is added in the molding process to be used as lubrication, and the molding pressure is 4MPa; the temperature rising process of the sintering process adopts a nitrogen/oxygen mixed atmosphere, and the oxygen partial pressure is 0.1% at 900-1250 ℃; the heat preservation temperature in the sintering process is 1360 ℃ and the heat preservation time is 4 hours; the heat preservation process adopts a nitrogen/oxygen mixed atmosphere, and the equilibrium oxygen partial pressure in the heat preservation process is 5.8%; the cooling rate in the cooling process in the sintering process is 3 ℃/min.
Comparative example 5
This comparative example provides a manganese-zinc-ferrite material differing from example 5 in that the manganese-zinc-ferrite material has a major component weight, a NiO content of 0.1wt%, and the remaining formulation and preparation method are the same as example 5.
Comparative example 6
This comparative example provides a manganese-zinc-ferrite material, which differs from example 5 in that the sintering temperature of the manganese-zinc-ferrite material is 1370 ℃, and the other formulation and preparation method are the same as example 5.
Comparative example 7
This comparative example provides a manganese-zinc-ferrite material, which differs from example 5 in that the sintering temperature of the manganese-zinc-ferrite material is 1300 ℃, and the other formulation and preparation method are the same as example 5.
The Mn-Zn ferrite materials provided in examples 1 to 5 and comparative examples 1 to 7 were tested by SY8218 under 100kHz,200mT, and 1200A/m saturation induction Bs, and the test results are shown in Table 1.
TABLE 1
As can be seen from the test results of example 1 and comparative example 1, the excessive amount of Fe 2 O 3 The magnetocrystalline anisotropy is excessively compensated, the resistivity is reduced, and the power consumption of a high-temperature section is increased, particularly the power consumption of 140 ℃ is greatly increased although the power consumption of the room temperature is reduced.
The power consumption temperature curves of example 2 and comparative example 2 are compared with those of example 2 and comparative example 2 as shown in FIG. 1, and it can be seen that Fe is excessively small 2 O 3 The anisotropic compensation of magnetocrystalline is insufficient, hysteresis loss is increased, high-temperature power consumption is not improved, and room-temperature power consumption is greatly increased.
Example 3 and comparative example 3 test results it can be seen that too little Co 3 O 4 The magnetic crystal anisotropy compensation is insufficient, the hysteresis loss is increased, the overall power consumption is increased, and the magnetic crystal anisotropy compensation is realized by Co 2+ Under-occupying A position of lattice tetrahedron, resulting in Fe of A and octahedral B position 3+ The superswitch between them decreases and Bs decreases.
Example 4 and comparative example 4 test results it can be seen that too much Co 3 O 4 The magnetocrystalline anisotropy is excessively compensated, the K2 value is increased, the hysteresis loss is increased, and the overall power consumption is increased.
As can be seen from the test results of example 5 and comparative example 5, too much NiO resulted in an increase in magnetocrystalline anisotropy, which was insufficient to offset the improvement effect of the increase in resistivity, and overall power consumption was increased.
As can be seen from the test results of example 5 and comparative example 6, not only does an excessively high sintering temperature not significantly raise Bs, but also the eddy current loss increases due to a decrease in resistivity caused by excessive grain growth, thereby increasing the overall power consumption.
As can be seen from the test results of example 5 and comparative example 7, too low a sintering temperature results in a decrease in density and thus in Bs. Although smaller grain growth reduces eddy current loss, at the same time uneven grain growth causes increased hysteresis loss and the resulting power consumption improvement is not significant.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments, and those skilled in the art, based on the principle of the present invention, should make improvements and modifications without departing from the scope of the present invention.
Claims (10)
1. A wide-temperature low-loss soft magnetic manganese zinc ferrite material suitable for 25-140 ℃ is characterized by comprising a main component and an additive; wherein:
the main component comprises the following components in mole percent: fe (Fe) 2 O 3 :53 to 53.5mol percent, znO: 9-10 mol% and the balance of MnO;
the additive comprises the following main components in percentage by mass: co (Co) 3 O 4 ：0.33～0.4wt％，NiO：0～0.08wt％，CaCO 3 ：0.03～0.05wt％，SiO 2 ：0.003～0.006wt％。
2. The method for preparing the wide-temperature low-loss soft magnetic manganese zinc ferrite material suitable for 25-140 ℃ as claimed in claim 1, which is characterized by comprising the following steps:
(1) Weighing Fe according to the proportion of the main component 2 O 3 Mixing, pelletizing and presintering MnO and ZnO raw materials to obtain presintering material；
(2) The presintered material is coarsely crushed, and then the additive is sequentially added for sanding, the binder is added for spray granulation and molding sintering, so that the wide-temperature low-loss soft magnetic manganese zinc ferrite material suitable for 25-140 ℃ is obtained.
3. The method for preparing a wide temperature range low loss soft magnetic manganese zinc ferrite material according to claim 2, wherein in step (1), the pellet size is 3-8 mm; and/or the presintering temperature is 950-1000 ℃ and the presintering time is 5-7 h.
4. The method for preparing a wide temperature range low loss soft magnetic manganese zinc ferrite material according to claim 2, wherein in step (2), the sand grain diameter used for the sand grinding is 1.5-2.4 μm.
5. The method for preparing a wide temperature range low loss soft magnetic manganese zinc ferrite material according to claim 2, wherein in step (2), the weight of the added binder is 0.5-2% of the dry weight of the sanding slurry; and/or the binder comprises polyvinyl alcohol.
6. The method of preparing a wide temperature range low loss soft magnetic manganese zinc ferrite material according to claim 5, wherein in step (2) said binder is added in an amount of 0.75 to 1.5% by weight based on the dry weight of the sanding slurry.
7. The method for preparing the wide-temperature low-loss soft magnetic manganese zinc ferrite material suitable for 25-140 ℃ according to claim 2, wherein in the step (2), the spraying flow rate of spraying granulation after adding the binder is 1.5-2.4L/h.
8. The method for preparing a wide temperature range low loss soft magnetic manganese zinc ferrite material according to claim 2, wherein in step (2), zinc stearate of 0.1wt% in terms of molding weight percentage is added as lubricant during the molding and sintering process; and/or the molding pressure is 3.5-5 MPa in the molding and sintering process.
9. The method for preparing the wide-temperature low-loss soft magnetic manganese zinc ferrite material suitable for 25-140 ℃ according to claim 2, wherein in the step (2), the temperature rising process of the molding sintering adopts a nitrogen/oxygen mixed atmosphere, and the oxygen partial pressure is 0-0.2% at 900-1250 ℃;
and/or the heat preservation temperature in the heat preservation process of the molding and sintering is 1330-1360 ℃ and the heat preservation time is 4-6 hours; the heat preservation process adopts a nitrogen/oxygen mixed atmosphere, and the equilibrium oxygen partial pressure in the heat preservation process is 4-6%;
and/or the cooling rate of the cooling process of the molding sintering is 1-3 ℃/min.
10. The application of the wide-temperature low-loss soft magnetic manganese zinc ferrite material suitable for 25-140 ℃ in an electric vehicle-mounted charger and a DC/DC converter in claim 1.
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