CN100340525C - NiZn ferrite material with high initial permeability and low loss and preparation method thereof - Google Patents
NiZn ferrite material with high initial permeability and low loss and preparation method thereof Download PDFInfo
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- CN100340525C CN100340525C CNB2005100606525A CN200510060652A CN100340525C CN 100340525 C CN100340525 C CN 100340525C CN B2005100606525 A CNB2005100606525 A CN B2005100606525A CN 200510060652 A CN200510060652 A CN 200510060652A CN 100340525 C CN100340525 C CN 100340525C
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 37
- 239000000463 material Substances 0.000 title claims abstract description 36
- 230000035699 permeability Effects 0.000 title claims abstract description 25
- 229910003962 NiZn Inorganic materials 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000203 mixture Substances 0.000 claims description 39
- 238000005245 sintering Methods 0.000 claims description 38
- 239000005338 frosted glass Substances 0.000 claims description 33
- 238000000498 ball milling Methods 0.000 claims description 30
- 239000002245 particle Substances 0.000 claims description 19
- 239000002994 raw material Substances 0.000 claims description 18
- 239000007858 starting material Substances 0.000 claims description 18
- 150000001875 compounds Chemical class 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 15
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 15
- 238000000227 grinding Methods 0.000 claims description 10
- 230000005415 magnetization Effects 0.000 claims description 6
- 239000000470 constituent Substances 0.000 claims description 5
- 238000012360 testing method Methods 0.000 claims description 3
- 238000000748 compression moulding Methods 0.000 claims description 2
- 229910015427 Mo2O3 Inorganic materials 0.000 abstract 1
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 abstract 1
- 238000002156 mixing Methods 0.000 description 18
- 238000001816 cooling Methods 0.000 description 12
- 239000013078 crystal Substances 0.000 description 12
- 238000005516 engineering process Methods 0.000 description 9
- 238000005303 weighing Methods 0.000 description 8
- 238000013461 design Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 238000005469 granulation Methods 0.000 description 6
- 230000003179 granulation Effects 0.000 description 6
- 238000002791 soaking Methods 0.000 description 6
- 239000000843 powder Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 229910018605 Ni—Zn Inorganic materials 0.000 description 3
- 238000004891 communication Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910001053 Nickel-zinc ferrite Inorganic materials 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 125000000129 anionic group Chemical group 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008054 signal transmission Effects 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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Abstract
The invention relates to a high initial permeability and low loss NiZn ferrite and a preparation method thereof, wherein the main components of the ferrite are calculated by oxides as follows: fe2O3 40～50mol%、NiO10～18mol%、ZnO 30～38mol%、Mn3O40 to 5mol% of CuO, 0 to 10mol% of CuO, and an auxiliary component V2O50 to 1wt% of Mo2O30 to 0.5 wt%. The invention can prepare the product with initial permeability of more than 2500 and specific loss of less than 20 x 10-6(100kHz) and specific temperature coefficient less than 4 x 10-6a/DEG C (25-65 ℃) NiZn ferrite material with high magnetic permeability and Curie temperature of more than 100 ℃.
Description
Technical field
The present invention relates to a kind of magneticsubstance and preparation method thereof, relate in particular to a kind of high initial magnetoconductivity, low-loss NiZn ferrite material and preparation method thereof.
Background technology
The same with the Mn-Zn ferrite of high initial magnetoconductivity, the high initial magnetoconductivity nickel-zinc ferrite also is the target that people extremely pay close attention to, development along with mechanics of communication, particularly along with the development of the transmitted in both directions technology and the network communications technology, in 5MHz～1000MHz broad frequency range, ferrite wide frequency band device (as splitter, divider, frequency mixer, directional coupler, line transformer etc.) is used more and more widely.As everyone knows, ferrite core plays the function of signal transmission and impedance conversion in wide frequency band device, mainly decide in front end wide frequency band device performance, and at the low frequency end of device, the performance of wide frequency band device is mainly by ferrite complex permeability u ', u by distribution parameter " decide.The Ferrite Material initial permeability is high more, the frequency of utilization of wide frequency band device is low more, and the frequency of utilization scope of wide frequency band device is also wide more, the effect of device transmission is also good more, the high μ i nickel-zinc-ferrite material initial permeability of domestic widespread usage so far is less than or equal to 2000, can not satisfy the requirement of the modern transmitted in both directions technology and the network communications technology far away, so initial permeability greater than 2000 often by external several families big company such as siemens, Hitachi, Ltd monopolizes, though but the initial permeability of these produced products of company can reach 2200～2300, but because the unreasonable configuration of its prescription, calcined temperature is controlled at about 1000 ℃, sintering temperature is controlled under the situation about 1200 ℃, the easy generation of crystal grain is grown up unusually, it is inhomogeneous that crystal grain becomes, cause the deterioration of loss and temperature factor, produced product often can not satisfy the requirement in market.So adopt new preparation method usually, add solubility promoter, adjusting process, the method for refinement powder, adjustment main formula improves ferritic initial permeability, discloses a kind of low-loss, low-temperature coefficient and high magnetic conductivity ferrite material and preparation method thereof as Chinese patent application (200410053951.1) low-loss, low-temperature coefficient and high magnetic conductivity ferrite material and preparation method thereof this patent application.Its principal phase is a spinel structure, with consisting of of composition calculated by content of oxides: Fe
2O
3Be 43～52mol%; ZnO is 28～42mol%; CuO is 3～12mol%; NiO is 5～12mol%.Preparation method's step is: 1) starting material mix, and 2) pre-burning, 3) the impurity interpolation, 4) secondary ball milling, 5) forming and sintering.Though this patent application can reach the NiZn Ferrite Material even grain size of preparation, crystal boundary is clear, and crystal grain is complete, does not have hole, dense structure.Grain-size is in 3～5 mu m ranges.But by discovering: Fe
2O
3Content can cause after being higher than 50% in addition and separate out mutually mutually or in addition, after the content of ZnO is higher than 38%, not only can cause initial permeability to reduce, and ferritic Curie temperature is reduced.This patent application also uses a large amount of CuO to substitute NiO, has reduced pre-burning and sintering temperature, makes that the energy consumption in the preparation process is little, design requirements to equipment is low, reduced production cost, but, made ferrite Curie temperature and saturation magnetization descend because the CuO of this patent adds too much.
Summary of the invention
The present invention is primarily aimed at technical problems such as the existing initial permeability of ferrite that prior art relates to is low, loss is bigger, provides a kind of initial permeability more than 2500, and the specific loss coefficient is less than 20 * 10
-6(100kHz), Curie temperature is greater than 100 ℃, and saturation magnetization is greater than the NiZn Ferrite Material of 260mT when 1600A/m.
It is a kind of by adjusting the ferritic production technique of NiZn that component prescription and processing parameter are fit to improve initial permeability, reduce the ferrite loss that the present invention also provides.
Above-mentioned technical problem of the present invention is mainly solved by following technical proposals: a kind of high initial magnetoconductivity, low-loss NiZn Ferrite Material, and its principal constituent and content (by mole per-cent) are calculated as with oxide compound:
Fe
2O
3Be 44～50mol%;
NiO is 10～18mol%;
ZnO is 30～38mol%;
Mn
3O
4Be 0～5mol%; (but not comprising 0)
CuO is 0～10mol%; (but not comprising 0)
Ancillary component and content (percentage composition by weight) are calculated as with oxide compound:
V
2O
50～1wt%, Mo
2O
30～0.5wt%:(but do not comprise 0).
Prior art is thought: the spin exchange interaction of Fe is all stronger than other compound of ferrite system, its Curie temperature is also the highest, discovery is along with the increase of the alternative Fe content of Cu, and the Curie temperature of compound, saturation magnetization and magnetocrystalline anisotropy performance all decrease.And Cu
2+Bohr's magnetic moment less than Ni
2+, Cu ion substitution Ni ion will reduce the specific saturation magnetization of material, and
Therefore the Cu ionic substitutes and will have a negative impact to magnetic permeability, and this is a technology barrier, can improve the interior magnetic moment M of unit volume but suitable adding Cu has higher density
s, and the more uniform crystal grain of complete sum more helps moving of domain wall, this also is very favorable for improving magnetic permeability, therefore can effectively reduce this disadvantageous effect, thereby guarantee that sintered compact has high initial permeability.And because the saturation magnetization of amorphous phase relies on crystallization volume fraction mutually strongly with Curie temperature, along with the crystallization volume fraction increases, Curie temperature raises.
High density and crystal grain distribution uniformly are that sintered compact has more low-loss major cause.But because Fe
2O
3The production technique decision, anionic existence is inevitable, the inhomogeneous dispersion of ferrite crystal boundary is to change the thickness that causes grain boundary layer due to reducing owing to negatively charged ion causes grain boundary structure, by adding the ancillary component of certain optimization component, to the adjustment a little of crystal boundary do, make is not that very inhomogeneous dispersive crystal boundary becomes very even originally, in the range of frequency below this external 1MHz, the ferritic loss of NiZn can also be made of magnetic hysteresis loss, and its magnetized mechanism mainly is that domain wall moves.And higher sintered density and more uniform grain-size will help moving of domain wall, reduce magnetic hysteresis loss.
Therefore in ferrite, added Mn
3O
4, suppressed the Fe in the material
2+, improved the loss characteristic of material, auxiliary material V
2O
5Adding can not only improve density, reduce the sintering sintering temperature, the specific loss of material is descended, improve magnetic property.
The preparation method of a kind of high initial magnetoconductivity, low-loss NiZn Ferrite Material comprises the steps:
A: mixed raw material: take by weighing each starting material, put into ball mill, add deionized water, ball milling 6～8 hours, the mean particle size that makes raw material is 0.8 μ m～1.0 μ m.
B: pre-burning: the material oven dry that mix grinding is good, put into the stove pre-burning.Calcined temperature is 900 ℃～1120 ℃, and the pre-burning time is 1～4 hour, and atmosphere is air.
C: secondary ball milling: pre-imitation frosted glass is put into ball mill, and adding auxiliary composition is V
2O
50.1～0.4WT% such as puts at the deionized water of weight, ball milling 20～24 hours makes pre-imitation frosted glass through behind the secondary ball milling, and the particulate mean particle size is 1.0 μ m～1.5 μ m.
D: forming and sintering: with pre-imitation frosted glass oven dry, add the polyvinyl alcohol (PVA) of 8～15wt%, the stove sintering is put in compression moulding.Sintering temperature is 1100～1200 ℃, and sintering time is 2～4 hours, and sintering atmosphere is an air; Wherein said starting material comprise Fe
2O
3, NiO, ZnO, Mn
3O
4, CuO; Described starting material (by mole per-cent) are calculated as with oxide compound: Fe
2O
3Be 44～50mol%; NiO is 10～18mol%; ZnO is 30～38mol%; 0＜Mn
3O
4≤ 5mol%; 0＜CuO≤10mol%;
Described auxiliary composition is V
2O
5, Mo
2O
3Wherein the content (percentage composition by weight) of auxiliary composition is calculated as with oxide compound: V
2O
50～1wt%, Mo
2O
30～0.5wt%; (but not comprising 0).
In addition, the initial permeability of prepared NiZn Ferrite Material is greater than 2500, and the ratio temperature factor in 25～65 ℃ temperature range is less than 4 * 10
-6/ ℃, the specific loss coefficient under the test condition of 100kHz and 0.25mT is less than 20 * 10
-6The Fe that starting material are selected
2O
3Purity more than or equal to 99.3%, the purity of ZnO more than or equal to 99.5%, the purity of NiO is more than or equal to 98%, Mn
3O
4Purity is more than or equal to 99.8%, and the purity of CuO is more than or equal to 99%, V
2O
5Purity more than or equal to 99%, after having taken by weighing various starting material, carry out mix grinding according to the component molecules formula, in the mix grinding process, not only to mix starting material, also to carry out preliminary pulverizing to starting material, make raw-material mean particle size less than 1.0 μ m.
The processing parameter that influences Ni-Zn ferrite ferrite electromagnetic property is a lot, wherein have the greatest impact, the number sintering process parameters the most just of difficult grasp, because about these parameters microstructures such as the grain-size of material, uniform crystal particles, crystal boundary ion distribution and grain boundary layer thickness, most important to the material electromagnetic property.
Those of ordinary skill in the art thinks the refinement powder; The mean particle size of powder is reduced to Nano grade, increased the particulate specific surface area, improved the activity of powder, but the granularity that reduces owing to simple will propose higher requirement to equipment, be unfavorable for the decline of cost, and reducing granularity by adjusting process also has certain limit merely, can not be unlimited reduce granularity, after granularity drops to a certain degree, easy long-living reunion.
So the temperature the when inventor finds pre-burning by studying for a long period of time is adjusted between 950～1020 ℃, and make that by ball milling raw-material mean particle size is all less than 1.0 μ m before the pre-burning, pre-imitation frosted glass is carried out secondary ball milling, and requiring the particulate mean particle size behind the ball milling is 1.0～1.5 μ m.The reactive behavior that this has improved powder has greatly reduced sintering temperature.
Auxiliary material V
2O
5Though interpolation can more effectively improve initial permeability, reduce sintering temperature, along with increasing of addition, the ferritic loss of NiZn will increase; Mo
2O
3Be added on when promoting grain growing, also caused the increase of void content in the material, and this hinders the growth of crystal grain conversely, so material initial permeability and grain-size are with Mo
2O
3The increase of addition be the back downward trend that rises earlier.The present invention is by secular experimental study in addition: its principal constituent and content (by a mole per-cent) are adjusted into oxide compound: Fe
2O
3Be 44～50mol%; NiO is 10～18mol%; ZnO is 30～38mol%; Mn
3O
4Be 0～5mol%; (but not comprising 0), CuO was 0～10mol%; (but not comprising 0) ancillary component and content (percentage composition by weight) is adjusted into oxide compound: V
2O
50～1wt%; Mo
2O
3It is 0～0.5wt% (but not comprising 0); Preferred especially Fe
2O
3Be 49mol%; NiO is 16mol% or 15.5mol%; ZnO is 32.5mol% or 33mol%; Mn
3O
4Be 1mol%; CuO is 1.5mol%; Auxiliary composition is V
2O
50.4wt%, Mo
2O
3Be 0.15wt% or 0.1wt%.Neither can have influence on the reduction of sintering temperature because of the interpolation of auxiliary material less, the raising of initial permeability can be because of not the increasing of addition yet, and the ferritic loss of Ni-Zn will increase, and magnetic permeability descends.
Therefore the present invention has the following advantages:
The present invention utilize high-quality raw material carry out reasonable proportioning and suitable ferrite preparation technology prepare initial permeability greater than 2500, the specific loss coefficient is less than 20 * 10
-6(100kHz), Curie temperature is greater than 100 ℃ high initial magnetoconductivity, low-loss NiZn Ferrite Material.
Embodiment
Below by embodiment, technical scheme of the present invention is described in further detail.
The Fe that the starting material of high initial magnetoconductivity provided by the invention, low-loss Ni-Zn Ferrite Material are selected
2O
3Purity more than or equal to 99.3%, the purity of ZnO more than or equal to 99.5%, the purity of NiO more than or equal to 98%, the purity of CuO more than or equal to 99%, Mn
3O
4Purity more than or equal to 99.8%, V
2O
5Purity more than or equal to 99%, Mo
2O
3Purity more than or equal to 99%.
Embodiment 1:
1. composition designs and weighing: Fe
2O
3Be preferably 49mol%, NiO is preferably 16mol%, and ZnO is preferably 32.5mol%, Mn
3O
4Be preferably 1mol%, CuO is preferably 1.5mol%, ancillary component V
2O
50.4wt%, Mo
2O
3Be 0.15wt%.
2. raw-material mixing: the major ingredient that weighs up is put into ball mill, the deionized water of weight such as adding, ball milling 7 hours, the mean particle size that makes raw material is 0.8 μ m.
3. pre-burning: the starting material oven dry that mix grinding is good, put into the stove pre-burning.Calcined temperature is 980 ℃, and the pre-burning time is 3h, and atmosphere is air, furnace cooling after the pre-burning.
4. secondary ball milling: in pre-imitation frosted glass, be weighed into auxiliary composition V
2O
50.4wt%, Mo
2O
3The deionized water of weight such as 0.15wt% adding and pre-imitation frosted glass is put into ball mill with the pre-imitation frosted glass that adds auxiliary composition, ball milling 22h, and the mean particle size that makes pre-imitation frosted glass is 1.2 μ m.
5. forming and sintering: with pre-imitation frosted glass oven dry, add the polyvinyl alcohol (PVA) of 10wt%, uniform mixing uses thorough mixing, use 45 order sub-sieve granulations, and be pressed into φ 20 sample rings, put into the box-type furnace sintering, sintering temperature is controlled to be 1120 ℃, and soaking time is 3h, and furnace cooling is to room temperature.
Embodiment 2
1. composition designs and weighing: Fe
2O
3Be preferably 49mol%, NiO is preferably 15.5mol%, and ZnO is preferably 33mol%, Mn
3O
4Be preferably 1mol%, CuO is preferably 1.5mol%, ancillary component V
2O
50.4wt%, Mo
2O
30.1wt%.
2. raw-material mixing: the major ingredient that weighs up is put into ball mill, the deionized water of weight such as adding and pre-imitation frosted glass, ball milling 8 hours, the mean particle size that makes raw material is 0.6 μ m.
3. pre-burning: the starting material oven dry that mix grinding is good, put into the stove pre-burning.Calcined temperature is 950 ℃, and the pre-burning time is 2h, and atmosphere is air, furnace cooling after the pre-burning.
4. secondary ball milling: in pre-imitation frosted glass, be weighed into auxiliary composition V
2O
50.4wt%, Mo
2O
30.1wt%, the deionized water of weight such as adding is put into ball mill with the pre-imitation frosted glass that adds auxiliary composition, ball milling 22h, the mean particle size of pre-imitation frosted glass is 1.2 μ m.
5. forming and sintering: with pre-imitation frosted glass oven dry, add the polyvinyl alcohol (PVA) of 10wt%, uniform mixing uses thorough mixing, use 45 order sub-sieve granulations, and be pressed into φ 20 sample rings, put into the box-type furnace sintering, sintering temperature is controlled to be 1120 ℃, and soaking time is 4h, and furnace cooling is to room temperature.
Embodiment 3
1. composition designs and weighing: Fe
2O
3Be preferably 49mol%, NiO is preferably 15.2mol%, and ZnO is preferably 33.3mol%, Mn
3O
4Be preferably 1mol%, CuO is preferably 1.5mol%, ancillary component V
2O
50.3wt%, Mo
2O
3Be 0.1wt%.
2. raw-material mixing: the major ingredient that weighs up is put into ball mill, the deionized water of weight such as adding and pre-imitation frosted glass, ball milling 8 hours, the mean particle size that makes raw material is 0.5 μ m.
3. pre-burning: the starting material oven dry that mix grinding is good, put into the stove pre-burning.Calcined temperature is 960 ℃, and the pre-burning time is 2h, and atmosphere is air, furnace cooling after the pre-burning.
4. secondary ball milling: in pre-imitation frosted glass, be weighed into auxiliary composition V
2O
50.3wt%, Mo
2O
30.1wt%, the deionized water of weight such as adding is put into ball mill with the pre-imitation frosted glass that adds auxiliary composition, ball milling 22h, the mean particle size that makes pre-imitation frosted glass is 1.0 μ m.
5. forming and sintering: with pre-imitation frosted glass oven dry, add the polyvinyl alcohol (PVA) of 10wt%, uniform mixing uses thorough mixing, use 45 order sub-sieve granulations, and be pressed into φ 20 sample rings, put into the box-type furnace sintering, sintering temperature is controlled to be 1140 ℃, and soaking time is 4h, and furnace cooling is to room temperature.
Embodiment 4
1. composition designs and weighing: Fe
2O
3Be preferably 49mol%, NiO is preferably 15mol%, and ZnO is preferably 33.5mol%, Mn
3O
4Be preferably 1mol%, CuO is preferably 1.5mol%, ancillary component V
2O
50.3wt%, Mo
2O
3Be 0.1wt%.
2. raw-material mixing: the major ingredient that weighs up is put into ball mill, the deionized water of weight such as adding and pre-imitation frosted glass, ball milling 7 hours, the mean particle size that makes raw material is 0.9 μ m.
3. pre-burning: the starting material oven dry that mix grinding is good, put into the stove pre-burning.Calcined temperature is 960 ℃, and the pre-burning time is 2h, and atmosphere is air, furnace cooling after the pre-burning.
4. secondary ball milling: in pre-imitation frosted glass, be weighed into auxiliary composition V
2O
50.3wt%, Mo
2O
30.1wt%, the deionized water of weight such as adding is put into ball mill with the pre-imitation frosted glass that adds auxiliary composition, ball milling 23h, the mean particle size that makes pre-imitation frosted glass is 1.3 μ m.
5. forming and sintering: with pre-imitation frosted glass oven dry, add the polyvinyl alcohol (PVA) of 10wt%, uniform mixing uses thorough mixing, use 45 order sub-sieve granulations, and be pressed into φ 20 sample rings, put into the box-type furnace sintering, sintering temperature is controlled to be 1150 ℃, and soaking time is 3h, and furnace cooling is to room temperature.
Comparative example 1 (according to existing preparation technology)
1. composition designs and weighing: Fe
2O
3Be preferably 49mol%, NiO is preferably 15.5mol%, and ZnO is preferably 34mol%, Mn
3O
4Be preferably 1mol%, CuO is preferably 0.5mol%.
2. raw-material mixing: the starting material that weigh up are put into ball mill, the deionized water of weight such as adding, ball milling 5 hours.
3. pre-burning: the starting material oven dry that mix grinding is good, put into the stove pre-burning.Calcined temperature is 980 ℃, and the pre-burning time is 3h, and atmosphere is air, furnace cooling after the pre-burning.
4. secondary ball milling: add and the deionized water of weight such as pre-imitation frosted glass, ball milling 12h, the mean particle size that makes pre-imitation frosted glass is 1.6 μ m.
5. forming and sintering: with pre-imitation frosted glass oven dry, add the polyvinyl alcohol (PVA) of 10wt%, uniform mixing uses thorough mixing, use 45 order sub-sieve granulations, and be pressed into φ 20 sample rings, put into the box-type furnace sintering, sintering temperature is controlled to be 1190 ℃, and soaking time is 6h, and furnace cooling is to room temperature.
Comparative example 2 (according to existing preparation technology)
1, composition design and weighing: Fe
2O
3Be preferably 49mol%, NiO is preferably 15.5mol%, and ZnO is preferably 33mol%, Mn
3O
4Be preferably 1mol%, CuO is preferably 1.5mol%.
2, raw-material mixing: the starting material that weigh up are put into ball mill, the deionized water of weight such as adding, ball milling 5 hours.
3, pre-burning: the starting material oven dry that mix grinding is good, put into the stove pre-burning.Calcined temperature is 950 ℃, and the pre-burning time is 3h, and atmosphere is air, furnace cooling after the pre-burning.
4, secondary ball milling: in pre-imitation frosted glass, be weighed into auxiliary composition V
2O
50.4wt%,, Bi
2O
3The deionized water of weight such as 0.15wt% adding is put into ball mill with the pre-imitation frosted glass that adds auxiliary composition, ball milling 12h, and the mean particle size that makes pre-imitation frosted glass is 1.2 μ m.
5, forming and sintering: with pre-imitation frosted glass oven dry, the polyvinyl alcohol (PVA) that adds 10wt%, uniform mixing, use thorough mixing, use 45 order sub-sieve granulations, and be pressed into φ 20 sample rings, put into the box-type furnace sintering, sintering temperature is controlled to be 1120 ℃, and soaking time is 6h, and furnace cooling is to room temperature.
The magnetism testing of the sample ring for preparing carries out on the Hp4284A electric impedance analyzer.
Table 1: embodiment and comparative example's magnetic property
As can be seen from Table 1: embodiments of the invention and comparative example compare, and the present invention effectively raises magnetic permeability, have reduced loss and sintering temperature, and have high Curie temperature.
Specific embodiment described herein only is that the present invention's spirit is illustrated.The technician of the technical field of the invention can make various modifications or replenishes or adopt similar mode to substitute described specific embodiment, but can't depart from spirit of the present invention or surmount the defined scope of appended claims.
Claims (6)
1. a high initial magnetoconductivity, low-loss NiZn Ferrite Material, its principal constituent and be calculated as with oxide compound by the content of mole per-cent:
Fe
2O
3Be 44～50mol%;
NiO is 10～18mol%;
ZnO is 30～38mol%;
Mn
3O
4Be 0～5mol%; But do not comprise 0;
CuO is 0～10mol%; But do not comprise 0;
Ancillary component and content by weight percentage are calculated as with oxide compound:
V
2O
50～1wt%; Mo
2O
30～0.5wt%; But do not comprise 0.
2. high initial magnetoconductivity according to claim 1, low-loss NiZn ferrite material is characterized in that: the content that principal constituent reaches by mole per-cent is calculated as with oxide compound:
Fe
2O
3Be 49mol%;
NiO is 16mol%;
ZnO is 32.5mol%;
Mn
3O
4Be 1mol%;
CuO is 1.5mol%;
Ancillary component reaches by weight percentage, and the content of content is calculated as with oxide compound:
V
2O
50.4wt%, Mo
2O
3Be 0.15wt%.
3, high initial magnetoconductivity according to claim 1, low-loss NiZn Ferrite Material is characterized in that: the content that principal constituent reaches by mole per-cent is calculated as with oxide compound:
Fe
2O
3Be 49mol%,
NiO is 15.5mol%,
ZnO is 33mol%,
Mn
3O
4Be 1mol%,
CuO is 1.5mol%,
Ancillary component reaches by weight percentage, and the content of content is calculated as with oxide compound:
V
2O
50.4wt％，Mo
2O
3?0.1wt％。
4, the preparation method of a kind of high initial magnetoconductivity, low-loss NiZn Ferrite Material comprises the steps:
A: mixed raw material: starting material are put into ball mill, add deionized water, ball milling 6～8 hours, the mean particle size that makes raw material is 0.8 μ m～1.0 μ m;
B: pre-burning: the material oven dry that mix grinding is good, put into the stove pre-burning, calcined temperature is 900 ℃～1120 ℃, and the pre-burning time is 1～4 hour, and atmosphere is air;
C: secondary ball milling: pre-imitation frosted glass is put into ball mill, add auxiliary composition, put into deionized water, ball milling 20～24 hours, behind the secondary ball milling, the particulate mean particle size is 1.0 μ m～1.5 μ m;
D: forming and sintering: with pre-imitation frosted glass oven dry, add the polyvinyl alcohol of 8～15wt%, the stove sintering is put in compression moulding, and sintering temperature is 1100～1200 ℃, and sintering time is 2～4 hours, and sintering atmosphere is an air;
The content that wherein said raw-material composition reaches by mole per-cent is calculated as with oxide compound: Fe
2O
3Be 44～50mol%; NiO is 10～18mol%; ZnO is 30～38mol%; 0＜Mn
3O
4≤ 5mol%; 0＜CuO≤10mol%; Described auxiliary composition is V
2O
5, Mo
2O
3Wherein auxiliary composition and content by weight percentage are calculated as with oxide compound: V
2O
50～1wt%, Mo
2O
30～0.5wt%; But do not comprise 0.
5, the preparation method of high initial magnetoconductivity according to claim 4, low-loss NiZn Ferrite Material, the initial permeability that it is characterized in that prepared NiZn Ferrite Material is greater than 2500, and the ratio temperature factor in 25～65 ℃ temperature range is less than 4 * 10
-6/ ℃, the specific loss coefficient under the test condition of 100kHz and 0.25mT is less than 20 * 10
-6
6. according to the preparation method of claim 4 or 5 described high initial magnetoconductivities, low-loss NiZn Ferrite Material, the Curie temperature that it is characterized in that prepared NiZn Ferrite Material is greater than 100 ℃, and saturation magnetization is greater than 260mT when 1600A/m.
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| CN102390984B (en) * | 2011-07-29 | 2013-06-12 | 电子科技大学 | NiZn ferrite material with high magnetic conductivity and high Curie temperature and preparation method thereof |
| CN104193314A (en) * | 2014-08-14 | 2014-12-10 | 蕲春县蕊源电子有限公司 | High-permeability soft magnetic ferrite material and preparation method thereof |
| CN105967670A (en) * | 2016-05-06 | 2016-09-28 | 江苏泰昌电子有限公司 | Nickel-zinc soft magnetic ferrite material and preparation method thereof |
| 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 |
| CN109456050B (en) * | 2018-12-20 | 2020-12-22 | 横店集团东磁股份有限公司 | Low-temperature co-fired LTCC soft magnetic ZnNiCu ferrite material and preparation method thereof |
| CN112661501B (en) * | 2021-01-08 | 2022-10-18 | 广安市华蓥山领创电子有限公司 | NiZn ferrite material for high-frequency power conversion and preparation method thereof |
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| JP2001181033A (en) * | 1999-12-28 | 2001-07-03 | Tdk Corp | Piezoelectric ceramic composition |
| CN1388794A (en) * | 2000-08-21 | 2003-01-01 | Tdk株式会社 | Ferrite material |
| CN1420101A (en) * | 2002-07-05 | 2003-05-28 | 邓廷成 | High-conductive nickel-zinc ferrite and preparing process thereof |
| CN1587192A (en) * | 2004-08-05 | 2005-03-02 | 秦会斌 | Anti-interference magnesium-zinc ferrite and producing method |
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| JP2001181033A (en) * | 1999-12-28 | 2001-07-03 | Tdk Corp | Piezoelectric ceramic composition |
| CN1388794A (en) * | 2000-08-21 | 2003-01-01 | Tdk株式会社 | Ferrite material |
| CN1420101A (en) * | 2002-07-05 | 2003-05-28 | 邓廷成 | High-conductive nickel-zinc ferrite and preparing process thereof |
| CN1587192A (en) * | 2004-08-05 | 2005-03-02 | 秦会斌 | Anti-interference magnesium-zinc ferrite and producing method |
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