CN105174930A - Low-power-consumption soft magnetism Mn-Zn ferrite and preparing method thereof - Google Patents
Low-power-consumption soft magnetism Mn-Zn ferrite and preparing method thereof Download PDFInfo
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- CN105174930A CN105174930A CN201510605889.0A CN201510605889A CN105174930A CN 105174930 A CN105174930 A CN 105174930A CN 201510605889 A CN201510605889 A CN 201510605889A CN 105174930 A CN105174930 A CN 105174930A
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Abstract
The invention discloses low-power-consumption soft magnetism Mn-Zn ferrite. The low-power-consumption soft magnetism Mn-Zn ferrite is prepared from main ingredients and auxiliary ingredients. The main ingredients are prepared from, by oxide, 52.75% of Fe2O3, 10.45% of ZnO10 and 36.8% of MnO. The auxiliary ingredients are prepared from, by oxide, 0.06% of MnO3, 0.03% of Bi2O3 and 0.02% of CaO. The invention further discloses a preparing method of the ferrite. The preparing method includes the steps of primary ball milling, pre-burning, secondary ball milling, freezing prilling, low-temperature vacuum drying, forming and sintering. The lowest power consumption of the low-power-consumption soft magnetism Mn-Zn ferrite under the conditions of 100 KHz, 200 mT and 100 DEG C is 280 kW/m<3>.
Description
Technical field
The present invention relates to a kind of ferrite, be specifically related to a kind of reduce power consumption soft magnetism Mn-Zn ferrite and preparation method thereof.
Background technology
Soft magnetic ferrite is a kind of under more weak the action of a magnetic field, is easy to the Ferrite Material being magnetized and demagnetizing.As developing morning, many, the broad-spectrum materials of kind, soft magnetic ferrite has become one of product of outbalance in Economic development.In recent years, along with the development of the electronic information technologies such as computer networking technology, the communication technology and power technology, the demand of traditional field to the soft magnetic ferrite of excellent property constantly increases.The application of soft magnetic ferrite also constantly extends to other field, has already become indispensable a kind of base mateirals such as various signal equipment, computer, household electrical appliance, automotive electronics, supply unit, instrument, space industry.The Mn-Zn ferrite of spinel type applies maximum soft magnetic ferrites, and its output accounts for more than 80% of soft magnetic ferrite.
Because technique is simple, accurately, industry preparation Mn-Zn ferrite uses dry process to formula usually.So-called dry method and conventional ceramic technique, namely select the raw materials such as the ferric oxide of certain proportioning, zinc oxide and manganese oxide, is prepared from through techniques such as mixing, ball milling, drying, pre-burning, pulverizing, doping, secondary ball milling, granulation, shaping and sintering.There is inherent defect in dry process: adopt oxide compound as raw material, because the reactive behavior of each oxide components is not high, other mixes cannot to ensure microscopic level.At hot stage, although temperature of reaction is up to more than 1,000 degree, but still cannot avoid the difference of each composition speed when diffusion reaction, thus make the composition generation segregation of material, microtexture is even not.In addition, when ball milling, oxide compound is easily reunited, and the homogeneity of powder is declined.Long Ball-milling Time can generate excessive iron and bring impurity into.These all result in the instability of quality product, limit the further lifting of the performance of MnZn ferrite material.Current domestic many magneticsubstance companies and part university and scientific research institution are all at independent research Mn-Zn Ferrite Material, but be subject to the restriction of equipment, preparation and sintering process etc., domestic product performance are compared with foreign well-known company, and power consumption is higher (350kW/m still
3left and right, " development of super low-power consumption MnZn ferrite ", University of Electronic Science and Technology's Master's thesis, Xu Zhiyong; " development of high temperature height Bs low-consumption Mn-Zn ferrite ", University of Electronic Science and Technology's Master's thesis, Zhao Hui), mainly concentrate on mid and low-end products.
Switch power supply is a kind of time ratio opened and cut off using electric power and electronic technology to carry out trip switch, thus ME for maintenance stablizes the power supply of output.Along with the progress of electric power and electronic technology, switch power technology is impelled to be developed chronically.At present, switch power supply is due to the feature of the aspects such as its high efficiency, lightweight and miniaturization, being widely used in the electronics that industrial automatic control equipment, research equipment, instrument, military industry equipment, audio-visual products, communication equipment, power equipment etc. are nearly all, is the vital power supply mode of electronic information rapid industrial development.Along with electron device to high performance, lightweight, miniaturization development, as High Frequency Switching power supply core the ferritic power loss of Mn-Zn lower the requirement more and more higher.Domestic product performance are compared with foreign well-known company, and power consumption is higher (350kW/m still
3left and right).
Summary of the invention
The present invention is directed to the deficiencies in the prior art, provide a kind of reduce power consumption soft magnetism Mn-Zn ferrite.
Another object of the present invention is to provide the ferritic preparation method of this reduce power consumption soft magnetism Mn-Zn.
The object of the invention is to be achieved through the following technical solutions:
A kind of reduce power consumption soft magnetism Mn-Zn ferrite, this Ferrite Material is made up of principal constituent and ancillary component, and principal constituent content is calculated as with oxide compound: Fe
2o
352.75%, ZnO10.45%, MnO36.8%; Ancillary component content is calculated as with oxide compound: MoO
30.06%, Bi
2o
30.03% and CaO0.02%;
The ferritic preparation method of this reduce power consumption soft magnetism Mn-Zn, is prepared by following steps:
1) ball milling: according to molar percentage, each component is mixed: Fe
2o
352.75%, ZnO10.45%, MnO36.8%, mixed raw material and deionized water are mixed according to 10:1 mass ratio, steel ball ball milling, obtains powder;
The diameter 6mm of described steel ball, Ball-milling Time 2h, rotating speed 300r/min, the particle diameter of powder is 1 μm;
2) pre-burning: powder is placed in retort furnace pre-burning, before 600 DEG C, temperature rise rate is 200 DEG C/h, and 600 DEG C of-920 DEG C of temperature rise rates are 100 DEG C/h, and 920 DEG C of insulations 2h, then furnace cooling, obtain Preburning material;
3) secondary ball milling: add the MoO accounting for powder 0.06% by total weight percent
3, the Bi of 0.03%
2o
3with 0.02% CaO as additive, by steel ball ball milling, obtain ball milling material;
MoO
3, Bi
2o
3powder can be suppressed to reunite with CaO, improve particle uniformity, promote that each oxide compound mixes, improve reactive behavior, improve grain size, defect when reducing shaping and gap.
Because Preburning material solid state reaction is incomplete, its grain size distribution is uneven, needs to carry out secondary ball milling again.The Main Function of secondary ball milling has two: after pre-burning, only has the ferrite of part spinel type to generate.Can make mixture again by pulverizing evenly by secondary ball milling, the raw material simultaneously making part be wrapped in responding layer inside comes out, and is beneficial to ferritic generation in follow-up sintering process; By secondary ball milling, powder particles is attenuated, there is high sintering activity, facilitate the densification of material in sintering process and the growth of crystal grain.
The diameter 6mm of described steel ball, Ball-milling Time 2h, rotating speed 300r/min;
4) freezing granulation: mix according to the mass ratio of ball milling material and glue 9:1, granulation, 60 mesh sieves repeatedly sieve, and tail over and give up, and obtain pellet; Pellet is dropped into frozen water content in liquid nitrogen, obtain freezing material;
5) low-temperature vacuum drying: freezing material is placed in vacuum chamber rapidly, air pressure is lower than under 60Pa condition, and heating pellets is to 25-30 DEG C, and the moisture distilled in freezing material, obtains dried feed;
The conventional too fast easy generation capillary pressure of dry means moisture evaporation causes diffusion and the condensation of pellet, thus reduces the homogeneity of composition and form, increases magnetic hysteresis loss.The present invention adopts freezing granulation and low-temperature vacuum drying, the moisture glaciation in pellet, sublimation drying in low-temperature vacuum environment, and the pellet density obtained like this, form are homogeneous, and can not produce hole in inside.The more important thing is and adopt this technology, capillary pressure and pellet can be avoided to subside contraction, after compression moulding, form homogeneous closely knit microtexture.
Notice that the dispersion of pellet appropriateness is beneficial to the distillation of moisture.
6) shaping: with 6 × 10
7dried feed is pressed into annular blank by the pressure of Pa;
Forming method technique of the present invention is simple, prepared blank size is accurate, water content is low, sintering time low, the compactness of shrinking percentage and physical strength better.
7) sinter: sintered under certain condition by annular blank, before 300 DEG C, temperature rise rate is 100 DEG C/h, 300 DEG C of insulation 0.5h; 300 DEG C of-900 DEG C of temperature rise rates are 100 DEG C/h; 900 DEG C of-1100 DEG C of temperature rise rates are 80 DEG C/scope of h, 960-1050 DEG C in oxygen partial pressure be that within the scope of 0.1-0.2%O2,1050-1100 DEG C, oxygen partial pressure is 0.3%O2; 1100 DEG C of-1360 DEG C of temperature rise rates are 100 DEG C/h; 1360 DEG C of insulation 4h, oxygen partial pressure is 4%O2; 1360 DEG C of-1100 DEG C of rate of temperature fall are 100 DEG C/h; 1100 DEG C of-800 DEG C of rate of temperature fall are 120 DEG C/h; After 800 DEG C, rate of temperature fall is 80 DEG C/h, is cooled to room temperature, can obtain reduce power consumption soft magnetism Mn-Zn ferrite of the present invention.
The sintering of Mn-Zn power ferrite is divided into intensification, is incubated and this three phases of lowering the temperature.Each stage is as follows for the requirement of temperature and atmosphere:
Temperature rise period: the temperature rise period of Mn-Zn power ferrite can be subdivided into the volatilization of blank residual moisture, binder removal and be heated to top temperature three phases.Wherein, the volatilization of blank residual moisture generally completes within the scope of 100-200 DEG C.The binder removal of blank carries out within the scope of 250-600 DEG C, and about 300 DEG C time, binder removal speed reaches maximum greatly.Therefore, the present invention locates insulations 30 minutes, in case section temperature rise rate causes too greatly blank to ftracture here at 300 DEG C.Meanwhile, it should be noted that the binder removal stage should ensure that there is good air circulation in volatilization district, the glue that blank is evaporated all is discharged.After the binder removal stage terminates, blank will enter heating zone.Due to temperature rise rate on the ion diffuse of blank inside, grain formation with to grow up and the discharge of pore has important impact.
It should be noted that and heat up appropriate to the occasion employing at a slow speed within the scope of 900-1100 DEG C, to ensure that the crystal grain of blank can homoepitaxial, reach the object of densification.
Holding stage: will experience the growth of crystal grain, the contraction of size, the discharge of pore and final solid state reaction due to blank at holding stage and generate ferrite, therefore the selection of sintering temperature and soaking time is most important.Too low sintering temperature will cause blank solid state reaction insufficient, and grain-size is little, void content is high, thus magnetic property is worsened; And too high sintering temperature can make the grain growing of blank abnormal, cause microtexture to become uneven, contriver studies and finds that optimal sintering temperature is 1360 DEG C.
Temperature-fall period: also adopt segmentation different rates cooling method at temperature-fall period.
Oxygen partial pressure controls: Mn-Zn power ferrite strictly will control the change of oxygen level at temperature-fall period, makes it reach the atmosphere of balance, in case oxidation is decomposed.In temperature-fall period, need to regulate oxygen partial pressure in real time by size stream gauge.The oxygen level of temperature-fall period defers to Morineau calculating formula:
Wherein log
p o2oxygen partial pressure value,
tabsolute temperature.Mode can calculate the oxygen partial pressure value that in temperature-fall period, each temperature is corresponding thus.In enterprise practical operation, generally temperature interval is set to 10 DEG C, makes in body of heater all corresponding upper every the oxygen partial pressure value of 10 DEG C.
This Ferrite Material performance characteristic is, under 100KHz, 200mT, 100 DEG C of conditions, the least in power-consuming of material is 280kW/m
3.
Described, annular blank is of a size of Ф 29mm × Ф 17mm × h11mm.
Described, glue is that polyethylene alcohol and water is obtained according to the mass ratio mixing of 9:1.
The present invention, by the optimization to the selection of preparation process Raw, material proportion, processing parameter, as the control of freezing granulation, low-temperature vacuum drying, sintering temperature etc., makes the ferritic total power consumption of reduce power consumption soft magnetism Mn-Zn of the present invention be low to moderate 315kW/m
3.
Accompanying drawing explanation
Fig. 1 is the power loss figure of embodiment 1.
Embodiment
embodiment 1
A kind of reduce power consumption soft magnetism Mn-Zn ferrite, be made up of principal constituent and ancillary component, principal constituent content is calculated as with oxide compound: Fe
2o
352.75%, ZnO10.45%, MnO36.8%; Ancillary component content is calculated as with oxide compound: MoO
30.06%, Bi
2o
30.03% and CaO0.02%;
The ferritic preparation method of a kind of reduce power consumption soft magnetism Mn-Zn is prepared by following steps:
1) ball milling: according to molar percentage, each component is mixed: Fe
2o
352.75%, ZnO10.45%, MnO36.8%, mixed raw material and deionized water are mixed according to 10:1 mass ratio, steel ball ball milling, obtains powder;
The diameter 6mm of described steel ball, Ball-milling Time 2h, rotating speed 300r/min, the particle diameter of powder is 1 μm;
2) pre-burning: powder is placed in retort furnace pre-burning, before 600 DEG C, temperature rise rate is 200 DEG C/h, and 600 DEG C of-920 DEG C of temperature rise rates are 100 DEG C/h, and 920 DEG C of insulations 2h, then furnace cooling, obtain Preburning material;
3) secondary ball milling: add the MoO accounting for powder 0.06% by total weight percent
3, the Bi of 0.03%
2o
3with 0.02% CaO as additive, by steel ball ball milling, obtain ball milling material;
The diameter 6mm of described steel ball, Ball-milling Time 2h, rotating speed 300r/min;
4) freezing granulation: mix according to the mass ratio of ball milling material and glue 9:1, granulation, 60 mesh sieves repeatedly sieve, and tail over and give up, and obtain pellet; Pellet is dropped into frozen water content in liquid nitrogen, obtain freezing material;
5) low-temperature vacuum drying: freezing material is placed in vacuum chamber rapidly, air pressure is lower than under 60Pa condition, and heating pellets is to 25-30 DEG C, and the moisture distilled in freezing material, obtains dried feed;
6) shaping: with 6 × 10
7dried feed is pressed into annular blank by the pressure of Pa;
7) sinter: sintered under certain condition by annular blank, before 300 DEG C, temperature rise rate is 100 DEG C/h, 300 DEG C of insulation 0.5h; 300 DEG C of-900 DEG C of temperature rise rates are 100 DEG C/h; 900 DEG C of-1100 DEG C of temperature rise rates are 80 DEG C/scope of h, 960-1050 DEG C in oxygen partial pressure be that within the scope of 0.1-0.2%O2,1050-1100 DEG C, oxygen partial pressure is 0.3%O2; 1100 DEG C of-1360 DEG C of temperature rise rates are 100 DEG C/h; 1360 DEG C of insulation 4h, oxygen partial pressure is 4%O2; 1360 DEG C of-1100 DEG C of rate of temperature fall are 100 DEG C/h; 1100 DEG C of-800 DEG C of rate of temperature fall are 120 DEG C/h; After 800 DEG C, rate of temperature fall is 80 DEG C/h, is cooled to room temperature, can obtain reduce power consumption soft magnetism Mn-Zn ferrite of the present invention;
This Ferrite Material performance characteristic is, under 100KHz, 200mT, 100 DEG C of conditions, the least in power-consuming of material is 280kW/m
3.
Described, annular blank is of a size of Ф 29mm × Ф 17mm × h11mm.
Described, glue is that polyethylene alcohol and water is obtained according to the mass ratio mixing of 9:1.
Adopt WL3866B broadband power signal generator determine sample under the test environment of 100kHz, 200mT power loss as shown in Figure 1, least in power-consuming when temperature is 100 DEG C is 280kW/m
3.
The above; be only the present invention's preferably embodiment, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (6)
1. a reduce power consumption soft magnetism Mn-Zn ferrite, is characterized in that, this Ferrite Material is made up of principal constituent and ancillary component, and principal constituent content is calculated as with oxide compound: Fe
2o
352.75%, ZnO10.45%, MnO36.8%; Ancillary component content is calculated as with oxide compound: MoO
30.06%, Bi
2o
30.03% and CaO0.02%;
A kind of reduce power consumption soft magnetism Mn-Zn ferrite is prepared by following steps:
1) ball milling: according to molar percentage, each component is mixed: Fe
2o
352.75%, ZnO10.45%, MnO36.8%, mixed raw material and deionized water are mixed according to 10:1 mass ratio, steel ball ball milling, obtains powder;
The diameter 6mm of described steel ball, Ball-milling Time 2h, rotating speed 300r/min, the particle diameter of powder is 1 μm;
2) pre-burning: powder is placed in retort furnace pre-burning, before 600 DEG C, temperature rise rate is 200 DEG C/h, and 600 DEG C of-920 DEG C of temperature rise rates are 100 DEG C/h, and 920 DEG C of insulations 2h, then furnace cooling, obtain Preburning material;
3) secondary ball milling: add the MoO accounting for powder 0.06% by total weight percent
3, the Bi of 0.03%
2o
3with 0.02% CaO as additive, by steel ball ball milling, obtain ball milling material;
The diameter 6mm of described steel ball, Ball-milling Time 2h, rotating speed 300r/min;
4) freezing granulation: mix according to the mass ratio of ball milling material and glue 9:1, granulation, 60 mesh sieves repeatedly sieve, and tail over and give up, and obtain pellet; Pellet is dropped into frozen water content in liquid nitrogen, obtain freezing material;
5) low-temperature vacuum drying: freezing material is placed in vacuum chamber rapidly, air pressure is lower than under 60Pa condition, and heating pellets is to 25-30 DEG C, and the moisture distilled in freezing material, obtains dried feed;
6) shaping: with 6 × 10
7dried feed is pressed into annular blank by the pressure of Pa;
7) sinter: sintered under certain condition by annular blank, before 300 DEG C, temperature rise rate is 100 DEG C/h, 300 DEG C of insulation 0.5h; 300 DEG C of-900 DEG C of temperature rise rates are 100 DEG C/h; 900 DEG C of-1100 DEG C of temperature rise rates are 80 DEG C/scope of h, 960-1050 DEG C in oxygen partial pressure be that within the scope of 0.1-0.2%O2,1050-1100 DEG C, oxygen partial pressure is 0.3%O2; 1100 DEG C of-1360 DEG C of temperature rise rates are 100 DEG C/h; 1360 DEG C of insulation 4h, oxygen partial pressure is 4%O2; 1360 DEG C of-1100 DEG C of rate of temperature fall are 100 DEG C/h; 1100 DEG C of-800 DEG C of rate of temperature fall are 120 DEG C/h; After 800 DEG C, rate of temperature fall is 80 DEG C/h, is cooled to room temperature, can obtain reduce power consumption soft magnetism Mn-Zn ferrite of the present invention;
This Ferrite Material performance characteristic is, under 100KHz, 200mT, 100 DEG C of conditions, the least in power-consuming of material is 280kW/m
3.
2. reduce power consumption soft magnetism Mn-Zn ferrite according to claim 1, it is characterized in that, described annular blank is of a size of Ф 29mm × Ф 17mm × h11mm.
3. reduce power consumption soft magnetism Mn-Zn ferrite according to claim 1, is characterized in that, described glue is that polyethylene alcohol and water is obtained according to the mass ratio mixing of 9:1.
4. the ferritic preparation method of reduce power consumption soft magnetism Mn-Zn according to claim 1, is characterized in that, comprise the following steps:
1) ball milling: according to molar percentage, each component is mixed: Fe
2o
352.75%, ZnO10.45%, MnO36.8%, mixed raw material and deionized water are mixed according to 10:1 mass ratio, steel ball ball milling, obtains powder;
The diameter 6mm of described steel ball, Ball-milling Time 2h, rotating speed 300r/min, the particle diameter of powder is 1 μm;
2) pre-burning: powder is placed in retort furnace pre-burning, before 600 DEG C, temperature rise rate is 200 DEG C/h, and 600 DEG C of-920 DEG C of temperature rise rates are 100 DEG C/h, and 920 DEG C of insulations 2h, then furnace cooling, obtain Preburning material;
3) secondary ball milling: add the MoO accounting for powder 0.06% by total weight percent
3, the Bi of 0.03%
2o
3with 0.02% CaO as additive, by steel ball ball milling, obtain ball milling material;
The diameter 6mm of described steel ball, Ball-milling Time 2h, rotating speed 300r/min;
4) freezing granulation: mix according to the mass ratio of ball milling material and glue 9:1, granulation, 60 mesh sieves repeatedly sieve, and tail over and give up, and obtain pellet; Pellet is dropped into frozen water content in liquid nitrogen, obtain freezing material;
5) low-temperature vacuum drying: freezing material is placed in vacuum chamber rapidly, air pressure is lower than under 60Pa condition, and heating pellets is to 25-30 DEG C, and the moisture distilled in freezing material, obtains dried feed;
6) shaping: with 6 × 10
7dried feed is pressed into annular blank by the pressure of Pa;
7) sinter: sintered under certain condition by annular blank, before 300 DEG C, temperature rise rate is 100 DEG C/h, 300 DEG C of insulation 0.5h; 300 DEG C of-900 DEG C of temperature rise rates are 100 DEG C/h; 900 DEG C of-1100 DEG C of temperature rise rates are 80 DEG C/scope of h, 960-1050 DEG C in oxygen partial pressure be that within the scope of 0.1-0.2%O2,1050-1100 DEG C, oxygen partial pressure is 0.3%O2; 1100 DEG C of-1360 DEG C of temperature rise rates are 100 DEG C/h; 1360 DEG C of insulation 4h, oxygen partial pressure is 4%O2; 1360 DEG C of-1100 DEG C of rate of temperature fall are 100 DEG C/h; 1100 DEG C of-800 DEG C of rate of temperature fall are 120 DEG C/h; After 800 DEG C, rate of temperature fall is 80 DEG C/h, is cooled to room temperature, can obtain reduce power consumption soft magnetism Mn-Zn ferrite of the present invention.
5. preparation method according to claim 4, is characterized in that, described annular blank is of a size of Ф 29mm × Ф 17mm × h11mm.
6. preparation method according to claim 4, is characterized in that, described glue is that polyethylene alcohol and water is obtained according to the mass ratio mixing of 9:1.
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|---|---|---|---|---|
| CN101004963A (en) * | 2006-12-14 | 2007-07-25 | 程步峰 | Process for preparing MnZn soft magnetic ferrite particles |
| CN102161585A (en) * | 2011-01-20 | 2011-08-24 | 绵阳开磁科技有限公司 | High-frequency wide-temperature low-power-consumption soft magnetic Mn-Zn ferrite and preparation method thereof |
| CN103274676A (en) * | 2013-03-21 | 2013-09-04 | 电子科技大学 | Wide-temperature high-Bs MnZn soft magnetic ferrite material and preparation method thereof |
| CN104351171A (en) * | 2014-11-05 | 2015-02-18 | 朱忠良 | Plant leaf flour-milling freezing-drying process |
-
2015
- 2015-09-22 CN CN201510605889.0A patent/CN105174930A/en active Pending
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|---|---|---|---|---|
| CN101004963A (en) * | 2006-12-14 | 2007-07-25 | 程步峰 | Process for preparing MnZn soft magnetic ferrite particles |
| CN102161585A (en) * | 2011-01-20 | 2011-08-24 | 绵阳开磁科技有限公司 | High-frequency wide-temperature low-power-consumption soft magnetic Mn-Zn ferrite and preparation method thereof |
| CN103274676A (en) * | 2013-03-21 | 2013-09-04 | 电子科技大学 | Wide-temperature high-Bs MnZn soft magnetic ferrite material and preparation method thereof |
| CN104351171A (en) * | 2014-11-05 | 2015-02-18 | 朱忠良 | Plant leaf flour-milling freezing-drying process |
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Application publication date: 20151223 |