CN103588472A - Wide-temperature MnZn power ferrite material and preparation method thereof - Google Patents
Wide-temperature MnZn power ferrite material and preparation method thereof Download PDFInfo
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- CN103588472A CN103588472A CN201310272252.5A CN201310272252A CN103588472A CN 103588472 A CN103588472 A CN 103588472A CN 201310272252 A CN201310272252 A CN 201310272252A CN 103588472 A CN103588472 A CN 103588472A
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Abstract
The invention relates to the technical field of production of MnZn power ferrite materials and particularly relates to a wide-temperature MnZn power ferrite material and a preparation method thereof. The wide-temperature MnZn power ferrite material consists of main components and auxiliary components, wherein the main components include 52.45-52.6 mol% of Fe2O3, 9.2-9.7mol% of ZnO and the balance of MnO; according to the total weight of the main components, the auxiliary components include 0.05-0.06% of CaCO3, 0.02-0.03% of ZrO2, 0.03-0.04% of Nb2O5 and 0.35-0.4% of Co2O3. The wide-temperature MnZn power ferrite material has low loss characteristic at the temperature ranges of 25 DEG C and 140 DEG C and also gives consideration to high Bs characteristic.
Description
Technical field
The present invention relates to MnZn power ferrite material production technical field, particularly a kind of wide temperature MnZn power ferrite material and preparation method thereof.
Background technology
The MnZn power ferrite material of at present external main flow is all focused on the loss of a certain temperature spot aspect loss, as PC44, PC47, the material such as PC45, PC46 of Japanese TDK company, abroad TDK company has developed PC95 material, and Philips company has developed 3C97 material.Although Japanese TDK company has announced PC95 material, and the loss of 25 ℃-100 ℃ is pressed lowlyer, the application of this material mainly still reduces idling consumption, is not suitable for for a long time working under 100 ℃ or higher temperature.Although Philips company has announced 3C97 material, this material is lower at the scope internal loss of wide temperature, but the Bs of this material is lower, the Bs of 100 ℃ particularly, being about 410mT(1200A/m 10kHz) this has limited the transmission efficiency under the efficiency of the power delivery of this material, particularly high temperature on the one hand.On be also unfavorable on the other hand the miniaturization of device.3C97 mainly focuses on the loss of 60 ℃-120 ℃, does not consider 25 ℃ of idling consumptions.
Domestic some company has also developed the material of similar PC95, as got over the P47 at peak.
In general, domestic and international company is aspect wide adiabator, or Bs is on the low side, or wide temperature range is inadequate, does not take into account the loss of 140 ℃ of 25 ℃ of normal temperature and high temperature.
The disclosure of the invention of CN102693802A a kind of wide temperature MnZn power ferrite material and preparation method thereof, by principal constituent and ancillary component, formed, wherein, principal constituent and content are calculated as with oxide compound: Fe
2o
3be that 52.1~52.6mol%, ZnO are 9~11.5mol%, MnO surplus; Ancillary component by principal constituent raw material gross weight is calculated as with oxide compound: CaCO
3, ZrO
2, Nb
2o
5, SnO
2and Co
2o
3, and Co
2o
3raw material must be greater than 0.35wt%.This material temperature is lower 25 ℃ to 140 ℃ scope loss ratios, but Bs is on the low side.
Summary of the invention
The object of the invention is to overcome the deficiency that above-mentioned materials exists, a kind of wide temperature MnZn power ferrite material is provided, make it in the temperature range of 25 ℃ and 140 ℃, have low loss characteristic, take into account the characteristic of high Bs simultaneously.
The present invention also provides the preparation method of above-mentioned wide temperature MnZn power ferrite material, simple for process, is applicable to suitability for industrialized production.
The technical solution adopted for the present invention to solve the technical problems is: a kind of wide temperature MnZn power ferrite material, by principal constituent and ancillary component, formed, and the molar percentage of each component of wherein said principal constituent is: Fe
2o
3for 52.45-52.6mol%, ZnO is 9.2-9.7mol%, MnO surplus; By accounting for principal constituent gross weight, each component concentration of ancillary component is: CaCO
30.05-0.06%, ZrO
20.02-0.03%, Nb
2o
50.03-0.04%, Co
2o
30.35-0.4%.
Contriver studies discovery, CaCO
3, Nb
2o
5and ZrO
2add, can improve the resistivity of crystal boundary, reduce the power consumption of material, Co
2o
3add the crystal anisotropy constant K that can reduce material
1, the magnetic hysteresis loss of reduction material.So what ancillary component adopted is the resistivity that improves material, controls the K of grain-size and reduction material
1realize the object reducing the wastage.Co
2o
3content 0.35-0.4%, can effectively reduce the K of material
1, reduce the loss of material.
For principal constituent Fe
2o
3, ZnO and MnO will be controlled, and need to drop on Fe
2o
3for 52.45-52.6mol%, ZnO are in the scope of 9.2-9.7mol%, MnO surplus.If Fe
2o
3content has surpassed the scope of the invention, can reduce the resistivity of material, improves the K of material
1value, thereby eddy-current loss and the magnetic hysteresis loss of increase material; If Fe
2o
3content, lower than this scope, can not effectively reduce the K of vectolite
2, be unfavorable for the reduction of material magnetic hysteresis loss.If ZnO content has surpassed the scope of the invention, be unfavorable for the raising of material B s, affect Fe in material simultaneously
3o
4generation, improve the magnetic hysteresis loss of material; If ZnO content, lower than the scope of the invention, is not only unfavorable for material K
1reduction, but also can affect the Bs of 25 ℃ of materials.
As preferably, described wide temperature MnZn power ferrite material is in 25 ℃ of-140 ℃ of temperature ranges, and the loss Pcv under the condition of 100kHz, 200mT is:
25 ℃ of power consumption≤330kW/m
3,
60 ℃ of power consumption≤310kW/m
3,
120 ℃ of power consumption≤330kW/m
3,
140 ℃ of power consumption≤380kW/m
3;
Bs under 1194A/m 50Hz condition is:
Bs >=the 540mT of 25 ℃
Bs >=the 420mT of 100 ℃.
A kind of preparation method of wide temperature MnZn power ferrite material, take each component of principal constituent, a sand milling post-drying is also sieved, pre-burning adds each component of ancillary component, secondary sand milling post-drying granulation in the mixture after pre-burning, then compression moulding, formed body is obtained to finished product after sintering under nitrogen atmosphere, and described sintering process comprises heat up section and temperature descending section, and oxygen level when control temperature descending section is cooled to 1200 ℃ is at 1-1.5%.
A bright spot of the present invention is, generally, obtain the characteristic of wide adiabator, normally SnO
2or TiO
2and Co
2o
3combine to add to realize and reduce K
1, reach wide temperature characteristics.But the oxygen level that the present invention passes through to reduce by 1200 ℃ of temperature descending sections, at 1-1.5%, makes material produce a certain amount of Fe in generating ferritic process
2+, generate iron ferrite, reach and add SnO
2or TiO
2with Co
2o
3the effect of associating interpolation.Method of the present invention is to improve targetedly for the above-mentioned special formulation of the present invention.
Except good formula, also need the sintering process having had to guarantee.In sintering process, be mainly by controlling temperature descending section, to be cooled to the oxygen level of 1200 ℃ to realize excellent ferrite phase, thereby obtain there is low loss characteristic in the temperature range of 25 ℃ and 140 ℃, take into account the wide temperature MnZn power ferrite material of the characteristic of high Bs simultaneously.
The invention has the beneficial effects as follows: in the temperature range of 25 ℃ and 140 ℃, have low loss characteristic, take into account the characteristic of high Bs simultaneously, can be widely used in the electronic devices and components fields such as switching mode power supply transformer, LCD illumination.
Embodiment
Below by specific embodiment, technical scheme of the present invention is described in further detail.
In the present invention, if not refer in particular to, the raw material adopting and equipment etc. all can be buied from market or this area is conventional.Method in following embodiment, if no special instructions, is the ordinary method of this area.
embodiment 1
By following principal constituent content, take principal constituent raw material: Fe
2o
3content is that 52.45mol%, ZnO content are that 9.7mol%, MnO content are 37.85mol%, and a sand milling post-drying is also crossed 45 orders/cun sieve; Powder after a sand milling is carried out to pre-burning, and calcined temperature is 880 ℃, and the time is 2 hours; (the ancillary component content by principal constituent gross weight is: CaCO in Preburning material, to add the ancillary component raw material taking in proportion
3: 0.05wt%, ZrO
2: 0.02wt%, Nb
2o
5: 0.03wt% and Co
2o
3: 0.35wt%), while carrying out secondary sand milling sand milling, the ratio of pellet water is 1:6:2, and the sand milling time is 220 minutes, and the granularity of sand milling gained is 1.05 μ m; Above-mentioned secondary sand milling material is dried and granulation, and then under 5MPa pressure, being pressed into density is 3.0g/cm
3mark ring.
comparative example 1
By following principal constituent content, take principal constituent raw material: Fe
2o
3content is that 52.35mol%, ZnO content are that 9.7mol%, MnO content are 37.95mol%, and a sand milling post-drying is also crossed 45 orders/cun sieve; Powder after a sand milling is carried out to pre-burning, and calcined temperature is 880 ℃, and the time is 2 hours; (the ancillary component content by principal constituent gross weight is: CaCO in Preburning material, to add the ancillary component raw material taking in proportion
3: 0.04wt%, ZrO
2: 0.02wt%, Nb
2o
5: 0.03wt% and Co
2o
3: 0.35wt%), carry out secondary sand milling, during sand milling, the ratio of pellet water is 1:6:2, and the sand milling time is 220 minutes, and the granularity of sand milling gained is 1.06 μ m; Above-mentioned secondary sand milling material is dried and granulation, and then under 5MPa pressure, being pressed into density is 3.0g/cm
3mark ring.
Sintering process of the present invention is: sintering under nitrogen atmosphere, sintering process comprises heat up section, holding-zone and temperature descending section, first be warming up to 1310-1330 ℃ of sintering 5-6 hour (now controlling oxygen level is 3-5vol%), then cooling, Control for Oxygen Content while being cooled to 1200 ℃ is at 1-1.5 vol %, be cooled to 900 ℃ following control oxygen levels below 20ppm until room temperature.
Mark in embodiment 1 and comparative example 1 is encircled to sintering under the same conditions, sintering temperature is controlled at 1320 ℃, sintering 5 hours, oxygen level is 3vol%, then cooling, Control for Oxygen Content while being cooled to 1200 ℃ is at 1-1.5 vol %, be cooled to 900 ℃ following control oxygen levels below 20ppm until room temperature.Obtain desired power ferrite material.Concrete outcome is in Table 1.
As can be seen from Table 1, because iron level in comparative example 1 is on the low side, make magnetic hysteresis loss increase, Bs reduces.
embodiment 2
By following principal constituent content, take principal constituent raw material: Fe
2o
3content is that 52.6mol%, ZnO content are that 9.5mol%, MnO content are 37.9mol%, and a sand milling post-drying is also crossed 45 orders/cun sieve; Powder after a sand milling is carried out to pre-burning, and calcined temperature is 880 ℃, and the time is 2 hours; (the ancillary component content by principal constituent gross weight is: CaCO in Preburning material, to add the ancillary component raw material taking in proportion
3: 0.06wt%, ZrO
2: 0.03wt%, Nb
2o
5: 0.04wt% and Co
2o
3: 0.4wt%), while carrying out secondary sand milling sand milling, the ratio of pellet water is 1:6:2, and the sand milling time is 220 minutes, and the granularity of sand milling gained is 1.05 μ m; Above-mentioned secondary sand milling material is dried and granulation, and then under 5MPa pressure, being pressed into density is 3.0g/cm
3mark ring.
comparative example 2
By following principal constituent content, take principal constituent raw material: Fe
2o
3content is that 52.8mol%, ZnO content are that 9.2mol%, MnO content are 38mol%, and a sand milling post-drying is also crossed 45 orders/cun sieve; Powder after a sand milling is carried out to pre-burning, and calcined temperature is 880 ℃, and the time is 2 hours; (the ancillary component content by principal constituent gross weight is: CaCO in Preburning material, to add the ancillary component raw material taking in proportion
3: 0.06wt%, ZrO
2: 0.03wt%, Nb
2o
5: 0.04wt% and Co
2o3:0.2wt%), carry out secondary sand milling, during sand milling, the ratio of pellet water is 1:6:2, and the sand milling time is 220 minutes, and the granularity of sand milling gained is 1.06 μ m; Above-mentioned secondary sand milling material is dried and granulation, and then under 5MPa pressure, being pressed into density is 3.0g/cm
3mark ring.
Mark in embodiment 2 and comparative example 2 is encircled to sintering (with embodiment 1) under the same conditions, sintering temperature is controlled at 1320 ℃, sintering 5 hours, then cooling, Control for Oxygen Content while being cooled to 1200 ℃ is at 1-1.5 vol %, be cooled to 900 ℃ following control oxygen levels below 20ppm until room temperature.Obtain desired power ferrite material.Concrete outcome is in Table 2.
As can be seen from Table 2, owing to there is no the Co of q.s in comparative example 2
2o
3add, cause overall losses higher.
embodiment 3
By following principal constituent content, take principal constituent raw material: Fe
2o
3content is that 52.45mol%, ZnO content are that 9.7mol%, MnO content are 37.85mol%, and a sand milling post-drying is also crossed 45 orders/cun sieve; Powder after a sand milling is carried out to pre-burning, and calcined temperature is 880 ℃, and the time is 2 hours; (the ancillary component content by principal constituent gross weight is: CaCO in Preburning material, to add the ancillary component raw material taking in proportion
3: 0.05wt%, ZrO
2: 0.02wt%, Nb
2o
5: 0.04wt% and Co
2o
3: 0.35wt%), while carrying out secondary sand milling sand milling, the ratio of pellet water is 1:6:2, and the sand milling time is 220 minutes, and the granularity of sand milling gained is 1.05 μ m; Above-mentioned secondary sand milling material is dried and granulation, and then under 5MPa pressure, being pressed into density is 3.0g/cm
3mark ring.
Embodiment 3 mark ring sintering temperatures are controlled to 1320 ℃, sintering 5 hours (now controlling oxygen level is 5vol%), in the process of sintering, control the oxygen level of 1200 ℃ of temperature descending sections at 1-1.5%, be cooled to 900 ℃ following control oxygen levels below 20ppm until room temperature obtains performance as table 3.
comparative example 3
By following principal constituent content, take principal constituent raw material: Fe
2o
3content is that 52.45mol%, ZnO content are that 9.7mol%, MnO content are 37.85mol%, and a sand milling post-drying is also crossed 45 orders/cun sieve; Powder after a sand milling is carried out to pre-burning, and calcined temperature is 880 ℃, and the time is 2 hours; (the ancillary component content by principal constituent gross weight is: CaCO in Preburning material, to add the ancillary component raw material taking in proportion
3: 0.05wt%, ZrO
2: 0.02wt%, Nb
2o
5: 0.04wt% and Co
2o
3: 0.35wt%), while carrying out secondary sand milling sand milling, the ratio of pellet water is 1:6:2, and the sand milling time is 220 minutes, and the granularity of sand milling gained is 1.05 μ m; Above-mentioned secondary sand milling material is dried and granulation, and then under 5MPa pressure, being pressed into density is 3.0g/cm
3mark ring.
Comparative example 3 mark ring sintering temperatures are controlled to 1320 ℃, sintering 5 hours (now controlling oxygen level is 5vol%), the oxygen level of 1200 ℃ of controlling temperature descending section in sintering process is 3-3.5%, be cooled to 900 ℃ following control oxygen levels below 20ppm until room temperature obtains performance as table 3.
Because the oxygen level of 1200 ℃ of temperature descending sections in comparative example 3 is higher, cause loss to uprise as can be seen from Table 3.
Above-described embodiment is a kind of preferably scheme of the present invention, not the present invention is done to any pro forma restriction, also has other variant and remodeling under the prerequisite that does not exceed the technical scheme that claim records.
Claims (3)
1. a wide temperature MnZn power ferrite material, is characterized in that: principal constituent and ancillary component, consist of, the molar percentage of each component of wherein said principal constituent is: Fe
2o
3for 52.45-52.6mol%, ZnO is 9.2-9.7mol%, MnO surplus; By accounting for principal constituent gross weight, each component concentration of ancillary component is: CaCO
30.05-0.06%, ZrO
20.02-0.03%, Nb
2o
50.03-0.04%, Co
2o
30.35-0.4%.
2. a kind of wide temperature MnZn power ferrite material according to claim 1, is characterized in that: described wide temperature MnZn power ferrite material is in 25 ℃ of-140 ℃ of temperature ranges, and the loss Pcv under the condition of 100kHz, 200mT is:
25 ℃ of power consumption≤330kW/m
3,
60 ℃ of power consumption≤310kW/m
3,
120 ℃ of power consumption≤330kW/m
3,
140 ℃ of power consumption≤380kW/m
3;
Bs under 1194A/m 50Hz condition is:
Bs >=the 540mT of 25 ℃
Bs >=the 420mT of 100 ℃.
3. the preparation method of a wide temperature MnZn power ferrite material as claimed in claim 1 or 2, it is characterized in that: take each component of principal constituent, a sand milling post-drying is also sieved, pre-burning adds each component of ancillary component, secondary sand milling post-drying granulation in the mixture after pre-burning, then compression moulding, formed body is obtained to finished product after sintering under nitrogen atmosphere, and described sintering process comprises heat up section and temperature descending section, and oxygen level when control temperature descending section is cooled to 1200 ℃ is at 1-1.5%.
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Cited By (6)
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CN104496446A (en) * | 2014-10-24 | 2015-04-08 | 横店集团东磁股份有限公司 | Wide-temperature power ferrite and manufacturing method thereof |
CN104803669A (en) * | 2015-03-17 | 2015-07-29 | 江苏新旭磁电科技有限公司 | Wide-temperature low-distortion Mn-Zn soft magnetic ferrite material and preparation method thereof |
CN112573912A (en) * | 2020-11-27 | 2021-03-30 | 天通控股股份有限公司 | Preparation method of medium-wide-band wide-temperature low-loss MnZn ferrite material |
CN112851328A (en) * | 2021-03-30 | 2021-05-28 | 横店集团东磁股份有限公司 | Manganese-zinc ferrite, preparation method and application thereof |
WO2021164191A1 (en) * | 2020-02-19 | 2021-08-26 | 横店集团东磁股份有限公司 | Manganese zinc ferrite with high negative-temperature magnetic permeability and low high-temperature loss, and preparation method therefor |
CN113956028A (en) * | 2021-11-25 | 2022-01-21 | 横店集团东磁股份有限公司 | High-temperature low-loss MnZn power ferrite and preparation method thereof |
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CN112573912A (en) * | 2020-11-27 | 2021-03-30 | 天通控股股份有限公司 | Preparation method of medium-wide-band wide-temperature low-loss MnZn ferrite material |
CN112851328A (en) * | 2021-03-30 | 2021-05-28 | 横店集团东磁股份有限公司 | Manganese-zinc ferrite, preparation method and application thereof |
CN113956028A (en) * | 2021-11-25 | 2022-01-21 | 横店集团东磁股份有限公司 | High-temperature low-loss MnZn power ferrite and preparation method thereof |
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