CN101979360A - Nanocrystalline Mn-Zn ferrite for high-speed switcher and preparation method thereof - Google Patents
Nanocrystalline Mn-Zn ferrite for high-speed switcher and preparation method thereof Download PDFInfo
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- CN101979360A CN101979360A CN 201010564047 CN201010564047A CN101979360A CN 101979360 A CN101979360 A CN 101979360A CN 201010564047 CN201010564047 CN 201010564047 CN 201010564047 A CN201010564047 A CN 201010564047A CN 101979360 A CN101979360 A CN 101979360A
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Abstract
The invention relates to a nanocrystalline Mn-Zn ferrite for a high-speed switcher and a preparation method thereof. The nanocrystalline Mn-Zn ferrite has a chemical formula shown as MnxZn1-xFe2O4, wherein x is greater than or equal to 0.1 and less than or equal to 0.5. In the preparation method of the invention, the process is simple; the cost is low; the method is easy to perform industrialized production; and the prepared nanocrystalline Mn-Zn ferrite has the particle size of between 10 to 20nm, the initial permeability up to 7,000 and the coercive force low to 1.9Oe, can meet a requirement on the performance of the high-speed switcher, and can be widely applied to the high-speed switcher.
Description
Technical field
The present invention relates to a kind of MnZn ferrite material, relate in particular to a kind of nano crystal iron ferrite that can be applicable to high-speed switches and preparation method thereof, belong to the oxidate magnetic material technical field.
Technical background
Mn-Zn ferrite is the soft magnetic ferrite with spinel structure, also be electronic industry and the mechanotronics base mateiral that a kind of purposes is wide, output is big, cost is low, be widely used as electronic switching element, high speed switchover element, magnetic head materials, magnetic recording material etc.Especially in the high speed change-over switch, the application of nano-crystal soft-magnetic ferrite is subjected to especially paying close attention to.Along with information technology and the digitized development of electronic product, for adapting to the development trend of various electrical equipment miniaturizations, chip type, high frequencyization, it is particularly important to prepare the soft magnetic ferrite that crystal grain is tiny evenly, initial permeability is high, coercive force is low, saturation magnetization is high.Yet, the Mn-Zn ferrite that traditional method is prepared, its grain-size and performance all can not well be applicable in the high-speed switches.Therefore, the scientific research personnel of scientific research field and technical applications has carried out deep research around the relation between chemical ingredients, preparation method and the electromagnetic performance thereof of Mn-Zn ferrite, wishes to develop the nanocrystalline Mn-Zn ferrite that can be applicable to high-speed switches.
Summary of the invention
The present invention is directed to shortcomings such as the grain-size that has Mn-Zn ferrite now is relatively large, magnetic permeability is low in fact, coercive force is big and be difficult to be applied in the high-speed switches, a kind of nanocrystalline MnZn ferrite material that can be applicable to high-speed switches is provided.The present invention also provides a kind of nanocrystalline MnZn ferrite material that can be applicable to high-speed switches to get the preparation method.
The present invention is directed to existing the problems referred to above, mainly solved by the following technical programs: a kind of nanocrystalline MnZn ferrite material that can be applied to high-speed switches, its chemical formula can be expressed as Mn
1-xZn
xFeO
4, 0.1≤x≤0.5 wherein.
A kind of nanocrystalline MnZn ferrite material that can be applicable to high-speed switches provided by the invention gets the preparation method and may further comprise the steps:
(1) according to chemical formula Mn
1-xZn
xFeO
4The proportion design of corresponding x (Zn)=0.1～0.5 goes out the MnZn ferrite of heterogeneity ratio in (wherein 0.1≤x≤0.5).Take by weighing purity according to the mol ratio of Mn, Zn, Fe and be respectively 96% Manganous chloride tetrahydrate (MnCl
24H
2O), 96% zinc sulfate (ZnSO
47H
2O), 98% iron(ic) chloride (FeCl
36H
2O), configuration mixing solutions;
(2) mixed solution in the step (1) is joined in the deionized water, oily temperature is heated to 65～100 ℃ of design temperatures and even with magnetic stirrer;
(3) accelerate stirring velocity, in mixed solution, add NaOH solution rapidly, regulate pH value to 11～13 and carry out co-precipitation, under this temperature, keep 1～1.5h;
(4) be cooled to room temperature, ageing 3～5d regulates pH to 6～8, removes impurity with ethanol and washed with de-ionized water;
(5) cleaned throw out is dewatered under 100～120 ℃ of temperature filter oven dry, label is ground into powder;
(6) moulding: use the desktop electric tabletting machine powder to be pressed into the blank of specified shape size;
(7) sintering: blank is put into resistance furnace heat-treat, be heated to 450 ℃～800 ℃ insulation 6～10h down with the heat-up rate of 100～120 ℃/h, last powered-down is cooled to room temperature.
The micron-sized soft magnetic ferrites of general use in the switching element of using always, they have the orthogonal magnetic hysteresis loop, in the magnetization inversion process, because the non-reversibility of magnetic domain wall movement is determined by the irreversible motion of neticdomain wall switching time greatly.Therefore and in the single domain nanometer system, magnetic history realizes by the magnetization inversion of magnetic moment that mainly the displacement of domain wall disappears substantially, under the high frequency magnetic field effect, can finish magnetization inversion in the of short duration time, from but switching element has high switching rate.This shows that the size of ferrite particle is an important factor that influences its magnetic property.Therefore, it is little that the present invention adopts the nano-crystalline MnZn ferrite of chemical coprecipitation preparation to have grain-size, the advantage of the little and initial permeability of coercive force.
The present invention compared with prior art has following advantage:
(1) not only cost is low for preparation method of the present invention, and technology is simple, the production efficiency height, and also sintering temperature is low, and energy-saving and cost-reducing, help realizing large-scale industrial production.
(2) to have grain-size little for the nano-crystalline MnZn ferrite material that adopts the present invention to prepare, and the advantage of the little and initial permeability of coercive force is applicable in the high-speed converters.
Description of drawings
Accompanying drawing is a nano-crystalline MnZn ferrite preparation method's of the present invention schema.
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) according to chemical formula Mn
1-xZn
xFeZO
4In get x=0.1, corresponding to Mn
2+, Zn
2+, Fe
3+, mol ratio take by weighing purity at 9: 1: 10 and be respectively 96% Manganous chloride tetrahydrate (MnCl
24H
2O), 96% zinc sulfate (ZnSO
47H
2O), 98% iron(ic) chloride (FeCl
36H
2O);
(2) mixed solution in (1) is joined in the deionized water, oily temperature is heated to 65 ℃ of design temperatures and even with magnetic stirrer;
(3) accelerate stirring velocity, in mixed solution, add NaOH solution rapidly, regulate pH value to 12 and carry out co-precipitation, under this temperature, keep 1h;
(4) be cooled to room temperature, ageing 5d regulates about pH to 6, removes impurity with ethanol and washed with de-ionized water;
(5) cleaned throw out is dewatered under 100 ℃ of temperature filter oven dry, be ground into powder label 1;
(6) moulding: use the desktop electric tabletting machine powder to be pressed into the blank of specified shape size;
(7) sintering: blank is put into resistance furnace carry out sintering processes, be heated to 450 ℃ of insulation 10h down with the heat-up rate of 100 ℃/h, last powered-down is cooled to room temperature.
Embodiment 2
(1) according to chemical formula Mn
1-xZn
xFeZO
4In get x=0.2, corresponding to Mn
2+, Zn
2+, Fe
3+, mol ratio take by weighing purity at 8: 2: 10 and be respectively 96% Manganous chloride tetrahydrate (MnCl
24H
2O), 96% zinc sulfate (ZnSO
47H
2O), 98% iron(ic) chloride (FeCl
36H
2O);
(2) mixed solution in (1) is joined in the deionized water, oily temperature is heated to 80 ℃ of design temperatures and even with magnetic stirrer;
(3) accelerate stirring velocity, in mixed solution, add NaOH solution rapidly, regulate pH value to 11 and carry out co-precipitation, under this temperature, keep 1.5h;
(4) be cooled to room temperature, ageing 3d regulates about pH to 6, removes impurity with ethanol and washed with de-ionized water;
(5) cleaned throw out is dewatered under 115 ℃ of temperature filter oven dry, be ground into powder label 2;
(6) moulding: use the desktop electric tabletting machine powder to be pressed into the blank of specified shape size;
(7) sintering: blank is put into resistance furnace carry out anneal, be heated to 550 ℃ of insulation 10h down with the heat-up rate of 120 ℃/h, last powered-down is cooled to room temperature.
Embodiment 3
(1) according to chemical formula Mn
1-xZn
xFeZO
4In get x=0.3, corresponding according to Mn2+, Zn2+, Fe3+, mol ratio take by weighing purity at 7: 3: 10 and be respectively 96% Manganous chloride tetrahydrate (MnCl
24H
2O), 96% zinc sulfate (ZnSO
47H
2O), 98% iron(ic) chloride (FeCl
36H
2O);
(2) mixed solution in (1) is joined in the deionized water, oily temperature is heated to 90 ℃ of design temperatures and even with magnetic stirrer;
(3) accelerate stirring velocity, in mixed solution, add NaOH solution rapidly, regulate pH value to 12 and carry out co-precipitation, under this temperature, keep 1h;
(4) be cooled to room temperature, ageing 4d regulates about pH to 6, removes impurity with ethanol and washed with de-ionized water;
(5) cleaned throw out is dewatered under 100 ℃ of temperature filter oven dry, be ground into powder label 3;
(6) moulding: use the desktop electric tabletting machine powder to be pressed into the blank of specified shape size;
(7) sintering: blank is put into resistance furnace carry out anneal, be heated to 800 ℃ of insulation 6h down with the heat-up rate of 115 ℃/h, last powered-down is cooled to room temperature.
Embodiment 4
(1) according to chemical formula Mn
1-xZn
xFeZO
4In get x=0.4, corresponding according to Mn2+, Zn2+, Fe3+, mol ratio take by weighing purity at 6: 4: 10 and be respectively 96% Manganous chloride tetrahydrate (MnCl
24H
2O), 96% zinc sulfate (ZnSO
47H
2O), 98% iron(ic) chloride (FeCl
36H
2O);
(2) mixed solution in (1) is joined in the deionized water, oily temperature is heated to 100 ℃ of design temperatures and even with magnetic stirrer;
(3) accelerate stirring velocity, in mixed solution, add NaOH solution rapidly, regulate pH value to 13 and carry out co-precipitation, under this temperature, keep 1h;
(4) be cooled to room temperature, ageing 3d regulates about pH to 7, removes impurity with ethanol and washed with de-ionized water;
(5) cleaned throw out is dewatered under 120 ℃ of temperature filter oven dry, be ground into powder label 4;
(6) moulding: use the desktop electric tabletting machine powder to be pressed into the blank of specified shape size;
(7) sintering: blank is put into resistance furnace carry out anneal, be heated to 700 ℃ of insulation 8h down with the heat-up rate of 100 ℃/h, last powered-down is cooled to room temperature.
Embodiment 5
(1) according to chemical formula Mn
1-xZn
xFeZO
4In get x=0.5, corresponding according to Mn2+, Zn2+, Fe3+, mol ratio take by weighing purity at 1: 1: 2 and be respectively 96% Manganous chloride tetrahydrate (MnCl
24H
2O), 96% zinc sulfate (ZnSO
47H
2O), 98% iron(ic) chloride (FeCl
36H
2O);
(2) mixed solution in (1) is joined in the deionized water, oily temperature is heated to 85 ℃ of design temperatures and even with magnetic stirrer;
(3) accelerate stirring velocity, in mixed solution, add NaOH solution rapidly, regulate pH value to 11 and carry out co-precipitation, under this temperature, keep 1.5h;
(4) be cooled to room temperature, ageing 5d regulates about pH to 8, removes impurity with ethanol and washed with de-ionized water;
(5) cleaned throw out is dewatered under 100 ℃ of temperature filter oven dry, be ground into powder label 5;
(6) moulding: use the desktop electric tabletting machine powder to be pressed into the blank of specified shape size;
(7) sintering: blank is put into resistance furnace carry out anneal, be heated to 650 ℃ of insulation 10h down with the heat-up rate of 120 ℃/h, last powered-down is cooled to room temperature.
Detect the structure of implementing blank in 1,2,3,4,5 with XRD, calculate average grain size by Scherrer formula D=0.94 λ/β cos θ (D is that crystal grain diameter, λ are X ray wavelength 0.1542nm).
Adopt the saturation magnetization M of vibrating sample magnetometer VSM measure sample when room temperature
sWith coercive force H
c, the initial permeability μ when being 10kHz with 25 ℃ of frequencies of electric impedance analyzer measure sample ferrite
iThe gained result can be referring to table 1.
By measuring result as can be known, gained nano-crystalline MnZn ferrite grain-size of the present invention is very little, single domain critical size less than theory, can finish magnetic in the extremely short time switches, and have higher initial permeability and low coercive force, the performance requriements of speed-sensitive switch can be satisfied, the speed-sensitive switch element can be widely used in preparing.
Table 1
Claims (2)
1. a nanocrystalline MnZn ferrite material that can be applicable to high-speed converters is characterized in that this nanocrystalline Mn-Zn ferrite chemical formula is: Mn
1-xZn
xFe
2O
4, 0.1≤x≤0.5 wherein.
2. a preparation method who can be applicable to the nanocrystalline MnZn ferrite material of high-speed converters is characterized in that comprising the steps:
(1) according to chemical formula Mn
1-xZn
xFeO
4Proportion design go out the MnZn ferrite of heterogeneity ratio; Take by weighing purity according to the mol ratio of Mn, Zn, Fe and be respectively 96% Manganous chloride tetrahydrate, 96% zinc sulfate, 98% iron(ic) chloride, configuration mixing solutions, wherein 0.1≤x≤0.5;
(2) mixed solution in the step (1) is joined in the deionized water, oily temperature is heated to 65～100 ℃ of design temperatures and even with magnetic stirrer;
(3) accelerate stirring velocity, in mixed solution, add NaOH solution rapidly, regulate pH value to 11～13 and carry out co-precipitation, under this temperature, keep 1～1.5h;
(4) be cooled to room temperature, ageing 3～5d regulates pH to 6～8, removes impurity with ethanol and washed with de-ionized water;
(5) cleaned throw out is dewatered under 100～120 ℃ of temperature filter oven dry, label is ground into powder;
(6) moulding: use the desktop electric tabletting machine powder to be pressed into the blank of specified shape size;
(7) sintering: blank is put into resistance furnace heat-treat, be heated to 450 ℃～800 ℃ insulation 6～10h down with the heat-up rate of 100～120 ℃/h, last powered-down is cooled to room temperature.
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| CN 201010564047 CN101979360A (en) | 2010-11-29 | 2010-11-29 | Nanocrystalline Mn-Zn ferrite for high-speed switcher and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111087010A (en) * | 2019-12-24 | 2020-05-01 | 周口师范学院 | Novel ferromagnetic copper-iron composite particle and preparation method thereof |
| CN115504779A (en) * | 2022-11-01 | 2022-12-23 | 安徽虹泰磁电有限公司 | Manganese-zinc ferrite magnetic material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0980856A1 (en) * | 1998-08-19 | 2000-02-23 | Minebea Co., Ltd. | A Mn-Zn Ferrite |
| CN1359854A (en) * | 2000-12-19 | 2002-07-24 | 中国科学技术大学 | High-purity tetragonal gamma-MnO3 nano crystal and its preparing process |
| 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
- 2010-11-29 CN CN 201010564047 patent/CN101979360A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0980856A1 (en) * | 1998-08-19 | 2000-02-23 | Minebea Co., Ltd. | A Mn-Zn Ferrite |
| CN1359854A (en) * | 2000-12-19 | 2002-07-24 | 中国科学技术大学 | High-purity tetragonal gamma-MnO3 nano crystal and its preparing process |
| 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111087010A (en) * | 2019-12-24 | 2020-05-01 | 周口师范学院 | Novel ferromagnetic copper-iron composite particle and preparation method thereof |
| CN115504779A (en) * | 2022-11-01 | 2022-12-23 | 安徽虹泰磁电有限公司 | Manganese-zinc ferrite magnetic material and preparation method thereof |
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Application publication date: 20110223 |