CN102060518A - High-resistivity low-loss nanocrystal manganese-zinc (MnZn) ferrite material and preparation method thereof - Google Patents
High-resistivity low-loss nanocrystal manganese-zinc (MnZn) ferrite material and preparation method thereof Download PDFInfo
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- CN102060518A CN102060518A CN 201010563669 CN201010563669A CN102060518A CN 102060518 A CN102060518 A CN 102060518A CN 201010563669 CN201010563669 CN 201010563669 CN 201010563669 A CN201010563669 A CN 201010563669A CN 102060518 A CN102060518 A CN 102060518A
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Abstract
The invention relates to a high-resistivity low-loss nanocrystal manganese-zinc (MnZn) ferrite material, of which the chemical formula is Mn[x]Zn[1-x]La[y]Fe[2-y]O[4], wherein 0.2<=x<=0.8, and 0.1<=y<=0.4. The particle size of the nanocrystal MnZn ferrite material is 10-25nm, the resistivity at room temperature is up to 3.2*10<3> omega m, and the high-frequency loss is only 70 mW/cm<3> (100 DEG C; 50mT; 500kHz). In addition, the preparation technique in the invention is simple and controllable, has the advantage of low cost, and can be easily used for mass production; and the prepared nanocrystal MnZn ferrite can be widely used in the fields of communication, automatic control, electronic devices and the like.
Description
Technical field
The present invention relates to a kind of MnZn ferrite material, relate in particular to a kind of have high resistivity and low-loss nanocrystalline MnZn ferrite material, belong to the oxidate magnetic material technical field.The invention still further relates to a kind of preparation method with high resistivity and low-loss nanocrystalline MnZn ferrite material.
Background technology
The Mn-Zn ferrite of spinel structure has advantages such as high resistivity, high magnetic permeability, low-loss, low cost owing to it, thereby is widely used in the various power electronic devices, particularly in some high-frequency elements.The performance of Mn-Zn ferrite is inseparable with its microtexture, and microtexture depends on chemical ingredients and preparation technology thereof.In recent years, along with the fast development of nanotechnology, nano material has the very big concern that special surface effects, volume effect and quantum tunneling effect or the like have been subjected to people because of it, and some nano-crystalline MnZn ferrites are developed in succession.In the preparation method of nano-crystalline MnZn ferrite, high-energy ball milling method compare with methods such as coprecipitation method, sol-gel method, hydrothermal methods have that technology is simple, composition proportion is easy to control, output is big, with low cost advantage thereby be widely used, and realized industrialization.Yet power electronic devices high frequencyization, miniaturization, lightening development trend are had higher requirement to nano-crystalline MnZn ferrite, wish that it has high resistivity and high-frequency low-consumption characteristic.
Summary of the invention
Technical problem to be solved by this invention provides a kind of have high resistivity and low-loss nanocrystalline MnZn ferrite material and preparation method thereof.
For solving above-mentioned technical problem, technical scheme of the present invention is: a kind of have high resistivity and a low-loss nanocrystalline MnZn ferrite material, and the chemical formula of this nano-crystalline MnZn ferrite material can be expressed as: Mn
xZn
1-xLa
yFe
2-yO
4, 0.2≤x≤0.8,0.1≤y≤0.4 wherein.
Rare earth ion is to the ferritic electricity of MnZn, magnetic property important influence.Rare earth ion La
3+Bigger ionic radius is arranged, in the MnZn ferrite, mix La
3+The time, they can enter position, octahedral interstice position (B) and replace Fe
3+, therefore reduced the Fe of B position
3+Quantity, reduced generation Fe
3+And Fe
2+Between the electronics quantity of jumping, thereby improved the ferritic resistivity of MnZn.In addition, La
3+Replacement cause the generation of microstress, hinder electronic motion, improved the ferritic resistivity of MnZn equally.Work as La
3+When content was big, they can accumulate in the crystal boundary place of crystal grain, thereby have increased passing to the scattering of electronics, have improved resistivity.The MnZn ferrite is when high frequency uses, and its loss is mainly eddy-current loss, and the increase of resistivity can effectively reduce eddy-current loss.Simultaneously, special sintering process of the present invention can effectively be removed the internal stress that stays in the high-energy ball milling process, has reduced magnetic hysteresis loss.Thereby the nano-crystalline MnZn ferrite that adopts the present invention to prepare has high resistivity and low loss characteristic.
Of the present invention have high resistivity and low-loss nano-crystalline MnZn ferrite material preparation method comprises the steps:
(1) batching: according to chemical formula Mn
xZn
1-xLa
yFe
2-yO
4The mol ratio of middle Mn, Zn, La, Fe takes by weighing MnO, ZnO, La
2O
3, Fe
3O
4Raw material, wherein 0.2≤x≤0.8,0.1≤y≤0.4;
(2) mixing, ball milling: each raw material is mixed in ball grinder, is the hardened steel ball of 6～10mm with diameter, and steel ball is 15～25: 1 with the ratio of raw materials quality.At room temperature carry out, rotational speed of ball-mill is 180～400r/min, and the ball milling time is 100～120h continuously;
(3) add tackiness agent and granulation: add the certain organic solution and the processing of sieving, powder is made circular fine particle;
(4) moulding: use the desktop electric tabletting machine powder to be pressed into the blank of specified shape size;
(5) sintering: the blank vacuum tube furnace is carried out sintering, and wherein the mean pressure of argon gas is 200～280mbar.Rate of heating with 5～8K/min is warmed up to 350 ℃～450 ℃, soaking time 30～50min.Rate of heating with 10～15K/min is warming up to 550 ℃～970 ℃ subsequently, soaking time 10～20min, and insulation cools to room temperature with the furnace after finishing.
The advantage of invention:
(1) the present invention has added rare-earth elements La, thereby has obtained having high resistivity, the MnZn Ferrite Material of low high-frequency loss.
(2) preparation method's technology of the present invention is simple, with low cost, is easy to realize industrialized mass production.
Embodiment
Below be the specific embodiment of the present invention, technical characterictic of the present invention is described further, but the present invention is not limited only to these embodiment.
Embodiment 1
(1) batching: according to chemical formula Mn
0.2Zn
0.8La
0.2Fe
1.8O
4The mol ratio of Mn, Zn, La, Fe takes by weighing MnO, ZnO, La in (wherein 0.2≤x≤0.8,0.1≤y≤0.4)
2O
3, Fe
3O
4Raw material;
(2) mixing, ball milling: each raw material is mixed in ball grinder, is the hardened steel ball of 6mm with diameter, and steel ball is 15: 1 with the ratio of raw materials quality.At room temperature carry out, rotational speed of ball-mill is 400r/min, and the ball milling time is 100h continuously;
(3) add tackiness agent and granulation: add the certain organic solution and the processing of sieving, powder is made circular fine particle;
(4) moulding: use the desktop electric tabletting machine powder to be pressed into the blank of specified shape size;
(5) sintering: the blank vacuum tube furnace is carried out sintering, and wherein the mean pressure of argon gas is 280mbar.Rate of heating with 5K/min is warmed up to 350 ℃, soaking time 50min.Rate of heating with 15K/min is warming up to 970 ℃ subsequently, soaking time 20min, and insulation cools to room temperature with the furnace after finishing.
Embodiment 2
(1) batching: according to chemical formula Mn
0.6Zn
0.4La
0.1Fe
1.9O
4The mol ratio of Mn, Zn, La, Fe takes by weighing MnO, ZnO, La in (wherein 0.2≤x≤0.8,0.1≤y≤0.4)
2O
3, Fe
3O
4Raw material;
(2) mixing, ball milling: each raw material is mixed in ball grinder, is the hardened steel ball of 10mm with diameter, and steel ball is 25: 1 with the ratio of raw materials quality.At room temperature carry out, rotational speed of ball-mill is 180r/min, and the ball milling time is 120h continuously;
(3) add tackiness agent and granulation: add the certain organic solution and the processing of sieving, powder is made circular fine particle;
(4) moulding: use the desktop electric tabletting machine powder to be pressed into the blank of specified shape size;
(5) sintering: the blank vacuum tube furnace is carried out sintering, and wherein the mean pressure of argon gas is 200mbar.Rate of heating with 8K/min is warmed up to 450 ℃, soaking time 30min.Rate of heating with 10K/min is warming up to 550 ℃ subsequently, soaking time 15min, and insulation cools to room temperature with the furnace after finishing.
Embodiment 3
(1) batching: according to chemical formula Mn
0.8Zn
0.2La
0.3Fe
1.7O
4The mol ratio of Mn, Zn, La, Fe takes by weighing MnO, ZnO, La in (wherein 0.2≤x≤0.8,0.1≤y≤0.4)
2O
3, Fe
3O
4Raw material;
(2) mixing, ball milling: each raw material is mixed in ball grinder, is the hardened steel ball of 8mm with diameter, and steel ball is 20: 1 with the ratio of raw materials quality.At room temperature carry out, rotational speed of ball-mill is 300r/min, and the ball milling time is 110h continuously;
(3) add tackiness agent and granulation: add the certain organic solution and the processing of sieving, powder is made circular fine particle;
(4) moulding: use the desktop electric tabletting machine powder to be pressed into the blank of specified shape size;
(5) sintering: the blank vacuum tube furnace is carried out sintering, and wherein the mean pressure of argon gas is 250mbar.Rate of heating with 8K/min is warmed up to 400 ℃, soaking time 40min.Rate of heating with 15K/min is warming up to 970 ℃ subsequently, soaking time 10min, and insulation cools to room temperature with the furnace after finishing.
Embodiment 4
(1) batching: according to chemical formula Mn
0.8Zn
0.2La
0.4Fe
1.6O
4The mol ratio of Mn, Zn, La, Fe takes by weighing MnO, ZnO, La in (wherein 0.2≤x≤0.8,0.1≤y≤0.4)
2O
3, Fe
3O
4Raw material;
(2) mixing, ball milling: each raw material is mixed in ball grinder, is the hardened steel ball of 10mm with diameter, and steel ball is 20: 1 with the ratio of raw materials quality.At room temperature carry out, rotational speed of ball-mill is 400r/min, and the ball milling time is 110h continuously;
(3) add tackiness agent and granulation: add the certain organic solution and the processing of sieving, powder is made circular fine particle;
(4) moulding: use the desktop electric tabletting machine powder to be pressed into the blank of specified shape size;
(5) sintering: the blank vacuum tube furnace is carried out sintering, and wherein the mean pressure of argon gas is 250mbar.Rate of heating with 6K/min is warmed up to 400 ℃, soaking time 40min.Rate of heating with 15K/min is warming up to 900 ℃ subsequently, soaking time 15min, and insulation cools to room temperature with the furnace after finishing.
With the phase structure of sample among the XRD detection embodiment 1,2,3, calculate average grain size with Scherrer formula D=0.94 λ/β cos θ (D is that crystal grain diameter, λ are X ray wavelength 0.1542nm); Measuring magnetic core with the power loss instrument is loss P under the 500kHz 100 ℃ of 50mT frequencies
CvResistivity with four point probe resistivity tester measure sample.Measuring result is listed in table 1.
By listed result as can be known, nano-crystal soft-magnetic Ferrite Material of the present invention have that magnetic core that the excellent properties of high resistivity, low high-frequency loss makes with it can be widely used in communicating by letter, in the devices such as the various types of inducers in broadcasting, TV, control automatically, spationautics, computer technology and other IT industry, transformer, reactance coil, suppressor.
Table 1
Claims (2)
1. one kind has high resistivity and low-loss nanocrystalline MnZn ferrite material, and it is characterized in that: the chemical formulation of this nanocrystalline MnZn ferrite material is: Mn
xZn
1-xLa
yFe
2-yO
4, 0.2≤x≤0.8,0.1≤y≤0.4 wherein.
2. the preparation method with high resistivity and low-loss nanocrystalline MnZn ferrite material is characterized in that this preparation method comprises the steps:
(1) batching: according to chemical formula Mn
xZn
1-xLa
yFe
2-yO
4The mol ratio of middle Mn, Zn, La, Fe takes by weighing MnO, ZnO, La
2O
3, Fe
3O
4Raw material, wherein 0.2≤x≤0.8,0.1≤y≤0.4;
(2) mixing, ball milling: each raw material is mixed in ball grinder, with diameter is the hardened steel ball of 6～10mm, and steel ball is 15～25: 1 with the ratio of raw materials quality, at room temperature carries out, rotational speed of ball-mill is 180～400r/min, and the ball milling time is 100～120h continuously;
(3) add tackiness agent and granulation: add the certain organic solution and the processing of sieving, powder is made circular fine particle;
(4) moulding: use the desktop electric tabletting machine powder to be pressed into the blank of specified shape size;
(5) sintering: the blank vacuum tube furnace is carried out sintering, wherein the mean pressure of argon gas is 200～280mbar, rate of heating with 5～8K/min is warmed up to 350 ℃～450 ℃, soaking time 30～50min, rate of heating with 10～15K/min is warming up to 550 ℃～970 ℃ subsequently, soaking time 10～20min, insulation cools to room temperature with the furnace after finishing.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502856A (en) * | 2011-09-23 | 2012-06-20 | 常州大学 | Multiferroic rare earth doped ferrate materials and preparation method thereof |
| CN103011790A (en) * | 2012-12-11 | 2013-04-03 | 海宁联丰磁业股份有限公司 | Preparation method of high-permeability manganese zinc ferrite |
| CN104900362A (en) * | 2014-03-07 | 2015-09-09 | Tdk株式会社 | Sintered ferrite magnet and motor provided therewith |
| CN107555981A (en) * | 2017-08-24 | 2018-01-09 | 成都圻坊生物科技有限公司 | A kind of low-temperature sintering MnZn Ferrite Materials and its prepare sintering method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811861A (en) * | 2010-03-31 | 2010-08-25 | 苏州天铭磁业有限公司 | Nano-crystalline MnZn ferrite material with high saturation induction density and high resistivity and preparation method thereof |
-
2010
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811861A (en) * | 2010-03-31 | 2010-08-25 | 苏州天铭磁业有限公司 | Nano-crystalline MnZn ferrite material with high saturation induction density and high resistivity and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 《Phys.stat.sol.(a)》 20021230 A.A.SATTAR et al. Effect of Rare Earth Substitution on Magnetic and Electrical Properties of Mn-Zn Ferrites 第86页2.Experimental至87页表1 1-2 第193卷, 第1期 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502856A (en) * | 2011-09-23 | 2012-06-20 | 常州大学 | Multiferroic rare earth doped ferrate materials and preparation method thereof |
| CN103011790A (en) * | 2012-12-11 | 2013-04-03 | 海宁联丰磁业股份有限公司 | Preparation method of high-permeability manganese zinc ferrite |
| CN103011790B (en) * | 2012-12-11 | 2014-01-08 | 海宁联丰磁业股份有限公司 | Preparation method of high-permeability manganese zinc ferrite |
| CN104900362A (en) * | 2014-03-07 | 2015-09-09 | Tdk株式会社 | Sintered ferrite magnet and motor provided therewith |
| CN104900362B (en) * | 2014-03-07 | 2017-09-01 | Tdk株式会社 | Ferrite sintered magnet and the motor for possessing it |
| CN107555981A (en) * | 2017-08-24 | 2018-01-09 | 成都圻坊生物科技有限公司 | A kind of low-temperature sintering MnZn Ferrite Materials and its prepare sintering method |
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Application publication date: 20110518 |