CN101090017A - High saturated flux low consumption MnZn power ferrite and its preparation method - Google Patents
High saturated flux low consumption MnZn power ferrite and its preparation method Download PDFInfo
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- CN101090017A CN101090017A CN 200610051943 CN200610051943A CN101090017A CN 101090017 A CN101090017 A CN 101090017A CN 200610051943 CN200610051943 CN 200610051943 CN 200610051943 A CN200610051943 A CN 200610051943A CN 101090017 A CN101090017 A CN 101090017A
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Abstract
This invention relates to an MnZn power ferrite of high saturated flux density and low loss and its preparation method, which develops a MnZn power ferrite with less than or equal to 260mW/cm3 power loss under the valley temperature of 90deg.C and 100KHz and 200mT, the saturated flux density greater than or equal to 530mT under 25deg.C, 1000A/m and 50Hz and the saturated flux density greater than or equal to 420mT at 100deg.C under the condition of 1000A/m and 50Hz.
Description
Technical field
The present invention relates to a kind of manganese-zinc ferrite and preparation method thereof, relate in particular to a kind of high saturated flux low consumption MnZn power ferrite and preparation method thereof,
Background technology
Be accompanied by popularizing of portable mobile electronic device, the high speed development of multimedia communication, digital network, and the demand in fields such as electromagnetic compatibility and anti-electromagnetic interference have proposed the more requirement of Gao Gengxin to power MnZn Ferrite Material at present.Along with the expansion of emerging application, power MnZn ferrite except requiring low loss, is also required to have high saturation flux density.Simultaneously, at different operational environments, on power consumption～temperature curve, should have different lowest power consumption temperature spots.High performance power MnZn ferrite, except that selecting anisotropy, magnetostriction is little and purity is high raw material for use, suitable trace element mixes and the control of technology is crucial.
The working temperature of most relevant MnZn power ferrites is all at 80 ℃～100 ℃, all with SiO in the prior art
2So that improve the resistivity of material, reach the purpose that reduces the wastage as additive.With SiO
2Add in the pre-imitation frosted glass as additive, though can improve the resistivity of material, occur liquid phase easily in the process of sintering, the probability that abnormal grain occurs can increase.If abnormal grain appears in material internal, the performance of material will worsen so.The somebody improves the performance of material by sulfur removal technology or employing fine grinding technology in addition, but has so just increased production cost, has increased the difficulty that material is applied.
Summary of the invention
The present invention is directed to the technical problem that MnZn power ferrite in the prior art and preparation technology thereof occur, a kind of high saturated flux low consumption MnZn power ferrite and preparation method thereof is provided.The present invention directly utilizes the SiO in the raw material
2, and the control SiO that the preparation method brought into
2, rather than adopt and add SiO
2Mode improve the magnetic property of MnZn power ferrite; Thereby obtain high saturated flux low consumption MnZn power ferrite.
Above-mentioned purpose of the present invention solves by the following technical programs: a kind of high saturated flux low consumption MnZn power ferrite, this ferrite comprise following composition by mole percentage:
Fe
2O
3： 51～53mol％；
MnO： 34～43mol％；
ZnO： 6～13mol％。
At above-mentioned high saturated flux low consumption MnZn power ferrite, this ferrite also contain in the following auxiliary element by weight percentage four kinds or more than:
CaCO
3：0.01～0.07wt％；
TiO
2：0.01～0.08％；
SnO
2：0.01～0.07wt％；
Nb
2O
5：0.01～0.06wt％；
ZrO
2：0.01～0.09wt％；
Co
2O
3：0.01～0.06wt％。
The present invention also provides a kind of preparation method of high saturated flux low consumption MnZn power ferrite, and this method is made up of following steps:
(1) batching: adopting main component is Fe by the mole percentage by weight
2O
3: 51～53mol%; MnO:34～43mol%; ZnO:6～13mol% carries out weighing, and the back of weighing adds deionized water and carries out sand milling in sand mill, and the time of sand milling is 30～80 minutes;
(2) pre-burning: carry out pre-burning with above-mentioned through the composition behind the sand milling, calcined temperature is 750 ℃～980 ℃, and the pre-burning time is 1～9 hour;
(3) secondary sand milling: four or more in by weight percentage the auxiliary element below in above-mentioned pre-imitation frosted glass, adding: CaCO
3: 0.01～0.07wt%, TiO
2: 0.01～0.08%, SnO
2: 0.01～0.07wt%, Nb
2O
5: 0.01～0.06wt%, ZrO
2: 0.01～0.09wt%, Co
2O
3: 0.01～0.06wt%; Then powder is added and put into sand mill behind the deionized water and carry out the secondary sand milling, the secondary sand milling time is 1～3 hour;
(4) mist projection granulating and moulding: above-mentioned secondary sand milling material is carried out mist projection granulating in spray tower, mist projection granulating is made the particle that particle diameter is 50～200 μ m; Be shaped to blank then with definite shape;
(5) sintering: the blank after the above-mentioned moulding is carried out carrying out sintering under 1260 ℃～1350 ℃ scope, promptly form high saturated flux low consumption MnZn power ferrite behind the sintering.
In the preparation method of above-mentioned high saturated flux low consumption MnZn power ferrite, be 1～1.18 μ m in the granularity of powder described in the step (3), SiO in the secondary sand milling material
2Weight percentage be 0.005～0.023wt%.
In the preparation method of above-mentioned high saturated flux low consumption MnZn power ferrite, in step (4), add PVA and defoamer during mist projection granulating, wherein both ratios are 20: 1, described defoamer is a kind of in ammoniacal liquor, the n-octyl alcohol.
In the preparation method of above-mentioned high saturated flux low consumption MnZn power ferrite, be that environment at oxygen and nitrogen carries out in the sintering process described in the step (5), wherein the scope of partial pressure of oxygen is: 1～10%.
As everyone knows, the loss of MnZn power ferrite is by magnetic hysteresis loss, eddy current loss and left in that loss forms.At 100kHz, under the 200mT condition, loss mainly is made up of magnetic hysteresis and two kinds of losses of eddy current, and it is less to left in the shared ratio of loss.In order to be reduced in the loss under this test condition, all be to adopt in the prior art by adding SiO
2The method that improves the resistivity of material reduces eddy current loss.But the inventor is by the discovery that studies for a long period of time: with SiO
2Add in the pre-imitation frosted glass as additive, though can improve the resistivity of material, occur liquid phase easily in the process of sintering, the probability that abnormal grain occurs can increase.If abnormal grain appears in material internal, the performance of material will worsen so.So the inventor wants the method by other and improves the resistivity of material that the phenomenon that can avoid crystal grain to grow up unusually again occurs.Consider SiO in the raw material
2Existence and secondary sand milling technology in bring SiO into
2Inevitable property, so can be by not adding SiO
2, directly utilize SiO in the raw material
2With bring SiO in the sand milling technology
2Improve the resistivity of material.So just can reduce the probability that liquid phase occurs in the sintering process, can also reduce production costs simultaneously.Certainly only still can not optimize the performance of MnZn power ferrite like this, also need to optimize the composition of material and adopt appropriate preparation method, and the inventor obtains a kind of high saturated flux low consumption MnZn power ferrite by above-mentioned material composition and preparation method.This high saturated flux low consumption MnZn power ferrite power consumption valley point is at 90 ℃, and at 100kHz, power consumption is smaller or equal to 260mW/cm under the condition of 200mT
3, at 1000A/m, the following 25 ℃ saturation flux density of the condition of 50Hz is more than or equal to 530mT, and at 1000A/m, the following 100 ℃ saturation flux density of the condition of 50Hz is more than or equal to 420mT.So just be well positioned to meet working temperature at 80 ℃～100 ℃ device to the low-loss of MnZn power ferrite, the requirement of high Bs.
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 to these embodiment.
Embodiment 1:
1, batching:
Take by weighing Fe
2O
3: 52.7mol%; MnO:37.1mol%; Three kinds of raw materials of ZnO:10.2mol%, the adding deionized water mixes and is broken in sand mill then,, broken 30 minutes, circulate and mix after 10 minutes, carry out mist projection granulating.
2. pre-burning:
Spraying material is put into pre-burning stove, carry out pre-burning under 920 ℃, total pre-burning time is 6 hours.
3. secondary sand milling:
Press the auxiliary element of pre-imitation frosted glass percentage by weight: CaCO below in pre-imitation frosted glass, adding
3: 0.03wt%, TiO
2: 0.04wt%, Nb
2O
5: 0.03wt%, Co
2O
3: 0.025wt%, ZrO
2: 0.02wt%.Then powder is put into sand mill adding deionized water and carried out the secondary sand milling, the sand milling time is 1 hour, and powder particles is controlled at 1～1.18 μ m.
4. mist projection granulating and moulding:
In secondary sand milling material, add a certain proportion of PVA and defoamer, in spray tower, carry out the particle that mist projection granulating becomes 50～200 μ m then; The effigurate blank of forming device then;
5. sintering:
Under the ratio of certain oxygen and nitrogen, sintering under scope under 1260 ℃ the temperature conditions, the partial pressure of oxygen during sintering is 6%, then cool to room temperature under the ratio of certain oxygen and nitrogen.
The sample that sinters is tested with SY-8258 BH analyzer, and specific performance sees Table 1:
The test result of sintered sample among table 1 embodiment 1
| Unit | Test condition | Numerical value | Probe temperature | |
| Power consumption (Pcv) | KW/m 3 | 100kHz 200mT | 583 | 25℃ |
| 257 | 90℃ | |||
| 270 | 100℃ | |||
| Saturation flux density (Bs) | mT | 1000A/m 50Hz | 532 | 25℃ |
| 420 | 100℃ | |||
| Remanent magnetism (Br) | mT | 1000A/m 50Hz | 108 | 25℃ |
| 41 | 100℃ | |||
| Curie temperature (Tc) | ℃ | 10kHz，＜0.25mT | 244 | |
| Density | Kg/m 3 | 4.8×10 3 | 25℃ |
As can be seen from the table, at 100kHz, during following 90 ℃ of 200mT condition, the loss of material is 257KW/m
3, at 1000A/m, the following 25 ℃ Bs of 50Hz condition is 532mT, 100 ℃ Bs is 420mT.Therefore this material is well positioned to meet the requirement of 80 ℃～100 ℃ devices of working down to material.Be particularly suitable for making the charger of notebook computer.
Embodiment 2:
1, batching:
Take by weighing Fe
2O
3: 51mol%; MnO:43mol%; Three kinds of raw materials of ZnO:6mol%, the adding deionized water mixes and is broken in sand mill then,, broken 40 minutes, circulate and mix after 10 minutes, carry out mist projection granulating.
2. pre-burning:
Spraying material is put into pre-burning stove, carry out pre-burning under 750 ℃, total pre-burning time is 9 hours.
3. secondary sand milling:
Press the auxiliary element of pre-imitation frosted glass percentage by weight: CaCO below in pre-imitation frosted glass, adding
3: 0.01wt%, TiO
2: 0.08wt%, SnO
2: 0.03wt%, Co
2O
3: 0.06wt%, ZrO
2: 0.01wt%.Then powder is put into sand mill adding deionized water and carried out the secondary sand milling, the sand milling time is 2 hours, and powder particles is controlled at 1～1.18 μ m.
4. mist projection granulating and moulding:
In secondary sand milling material, add a certain proportion of PVA and defoamer, in spray tower, carry out the particle that mist projection granulating becomes 50～200 μ m then; The effigurate blank of forming device then;
5. sintering:
Under the ratio of certain oxygen and nitrogen, sintering under 1290 ℃ temperature conditions, the partial pressure of oxygen during sintering is 8%, then cool to room temperature under the ratio of certain oxygen and nitrogen.
The sample that sinters is tested with SY-8258 BH analyzer, and specific performance sees Table 2:
The test result of sintered sample among table 2 embodiment 2
| Unit | Test condition | Numerical value | Probe temperature | |
| Power consumption (Pcv) | KW/m 3 | 100kHz 200mT | 585 | 25℃ |
| 256 | 90℃ | |||
| 272 | 100℃ | |||
| Saturation flux density (Bs) | mT | 1000A/m 50Hz | 536 | 25℃ |
| 420 | 100℃ | |||
| Remanent magnetism (Br) | mT | 1000A/m 50Hz | 136 | 25℃ |
| 39 | 100℃ | |||
| Curie temperature (Tc) | ℃ | 10kHz，＜0.25mT | 244 | |
| Density | Kg/m 3 | 4.9×10 3 | 25℃ |
As can be seen from the table, at 100kHz, during following 90 ℃ of 200mT condition, the loss of material is 256KW/m
3, at 1000A/m, the following 25 ℃ Bs of 50Hz condition is 536mT, 100 ℃ Bs is 420mT.Therefore this material is well positioned to meet the requirement of 80 ℃～100 ℃ devices of working down to material.Be particularly suitable for making the charger of notebook computer.
Embodiment 3
1, batching:
Take by weighing Fe
2O
3: 53mol%; MnO:34mol%; Three kinds of raw materials of ZnO:13mol%, the adding deionized water mixes and is broken in sand mill then,, broken 50 minutes, circulate and mix after 10 minutes, carry out mist projection granulating.
2. pre-burning:
Spraying material is put into pre-burning stove, carry out pre-burning under 980 ℃, total pre-burning time is 1 hour.
3. secondary sand milling:
Press the auxiliary element of pre-imitation frosted glass percentage by weight: TiO below in pre-imitation frosted glass, adding
2: 0.01wt%, SnO
2: 0.07wt%, Co
2O
3: 0.06wt%, ZrO
2: 0.09wt%.Then powder is put into sand mill adding deionized water and carried out the secondary sand milling, the sand milling time is 3 hours, and powder particles is controlled at 1～1.18 μ m.
4. mist projection granulating and moulding:
In secondary sand milling material, add a certain proportion of PVA and defoamer n-octyl alcohol, in spray tower, carry out the particle that mist projection granulating becomes 50～200 μ m then; The effigurate blank of forming device then;
5. sintering:
Under the ratio of certain oxygen and nitrogen, sintering under 1350 ℃ temperature conditions, the partial pressure of oxygen during sintering is 9%, then cool to room temperature under the ratio of certain oxygen and nitrogen.
The sample that sinters is tested with SY-8258 BH analyzer, and specific performance sees Table 3:
The test result of sintered sample among table 3 embodiment 3
| Unit | Test condition | Numerical value | Probe temperature | |
| Power consumption (Pcv) | KW/m 3 | 100kHz 200mT | 586 | 25℃ |
| 260 | 90℃ | |||
| 276 | 100℃ | |||
| Saturation flux density (Bs) | mT | 1000A/m 50Hz | 532 | 25℃ |
| 421 | 100℃ | |||
| Remanent magnetism (Br) | mT | 1000A/m 50Hz | 128 | 25℃ |
| 41 | 100℃ | |||
| Curie temperature (Tc) | ℃ | 10kHz，＜0.25mT | 244 | |
| Density | Kg/m 3 | 4.9×10 3 | 25℃ |
As can be seen from the table, at 100kHz, during following 90 ℃ of 200mT condition, the loss of material is 258KW/m
3, at 1000A/m, the following 25 ℃ Bs of 50Hz condition is 532mT, 100 ℃ Bs is 421mT.Therefore this material is well positioned to meet the requirement of 80 ℃～100 ℃ devices of working down to material; Be particularly suitable for making the charger of notebook computer.
Embodiment 4:
1. prepare burden:
Take by weighing Fe
2O
3: 52.6mol%; MnO:37mol%; Three kinds of raw materials of ZnO:10.4mol% mix in sand mill and fragmentation then, add a certain amount of deionized water, and sand milling 70 minutes circulates and mixes after 10 minutes, carries out mist projection granulating.
2. pre-burning:
Spraying material is put into pre-burning stove, carry out pre-burning under 920 ℃, total pre-burning time is 6 hours.
3. secondary sand milling:
In pre-imitation frosted glass, add following auxiliary element: CaCO
3: 0.03wt%, SnO
2: 0.03wt%, Nb
2O
5: 0.03wt%, Co
2O
3: 0.025wt%, ZrO
2: 0.02wt%.Then powder is put into sand mill and carry out the secondary sand milling, require to add a certain amount of deionized water, the sand milling time is 2 hours, and powder particles is controlled at 1～1.18 μ m.
4. mist projection granulating and moulding:
In secondary sand milling material, add a certain proportion of PVA and defoamer, in spray tower, carry out the particle that mist projection granulating becomes 50～200 μ m then; The effigurate blank of forming device then;
5. sintering:
Under the ratio of certain oxygen and nitrogen, sintering under 1260 ℃～1350 ℃ scope, partial pressure of oxygen is 1～10% during sintering, then cool to room temperature under the ratio of certain oxygen and nitrogen.
The sample that sinters is tested with SY-8258 BH analyzer, and specific performance sees Table 4:
The test result of sintered sample among table 4 embodiment 4
| Unit | Test condition | Numerical value | Probe temperature | |
| Power consumption (Pcv) | KW/m 3 | 100kHz 200mT | 587 | 25℃ |
| 259 | 90℃ | |||
| 274 | 100℃ | |||
| Saturation flux density (Bs) | mT | 1000A/m 50Hz | 534 | 25℃ |
| 421 | 100℃ | |||
| Remanent magnetism (Br) | mT | 1000A/m 50Hz | 142 | 25℃ |
| 37 | 100℃ | |||
| Curie temperature (Tc) | ℃ | 10kHz，＜0.25mT | 244 | |
| Density | Kg/m 3 | 4.9×10 3 | 25℃ |
As can be seen from the table, at 100kHz, during following 90 ℃ of 200mT condition, the loss of material is 259KW/m
3, at 1000A/m, the following 25 ℃ Bs of 50Hz condition is 534mT, 100 ℃ Bs is 421mT.Therefore this material is well positioned to meet the requirement of 80 ℃～100 ℃ devices of working down to material.Be particularly suitable for making the charger of notebook computer.
Specific embodiment described in the present invention only is that the present invention's spirit is illustrated.The technical staff 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.
Although the present invention has been made detailed explanation and has quoted some instantiations as proof, to those skilled in the art, only otherwise leave that the spirit and scope of the present invention can be done various variations or correction is obvious.
Claims (8)
1. high saturated flux low consumption MnZn power ferrite, this ferrite comprises following composition by mole percentage:
Fe
2O
3： 51～53mol％；
MnO： 34～43mol％；
ZnO： 6～13mol％。
2, a kind of high saturated flux low consumption MnZn power ferrite according to claim 1, it is characterized in that this ferrite also contain in the following auxiliary element by weight percentage four kinds or more than:
CaCO
3：0.01～0.07wt％；
TiO
2：0.01～0.08％；
SnO
2：0.01～0.07wt％；
Nb
2O
5：0.01～0.06wt％；
ZrO
2：0.01～0.09wt％；
Co
2O
3：0.01～0.06wt％。
3, high saturated flux low consumption MnZn power ferrite according to claim 1 and 2 is characterized in that described MnZn power ferrite power consumption valley point at 90 ℃, and at 100kHz, power consumption is smaller or equal to 260mW/cm under the condition of 200mT
3, at 1000A/m, the following 25 ℃ saturation flux density of the condition of 50Hz is more than or equal to 530mT, and at 1000A/m, the following 100 ℃ saturation flux density of the condition of 50Hz is more than or equal to 420mT.
4, a kind of preparation method of high saturated flux low consumption MnZn power ferrite, this method is made up of following steps:
(1) batching: adopting main component is Fe by the mole percentage by weight
2O
3: 51～53mol%; MnO:34～43mol%; ZnO:6～13mol% carries out weighing, and the back of weighing adds deionized water and carries out sand milling in sand mill, and the time of sand milling is 30～80 minutes;
(2) pre-burning: carry out pre-burning with above-mentioned through the composition behind the sand milling, calcined temperature is 750 ℃～980 ℃, and the pre-burning time is 1～9 hour;
(3) secondary sand milling: four or more in by weight percentage the auxiliary element below in above-mentioned pre-imitation frosted glass, adding: CaCO
3: 0.01～0.07wt%, TiO
2: 0.01～0.08%, SnO
2: 0.01～0.07wt%, Nb
2O
5: 0.01～0.06wt%, ZrO
2: 0.01～0.09wt%, Co
2O
3: 0.01～0.06wt%; Then powder is added and put into sand mill behind the deionized water and carry out the secondary sand milling, the secondary sand milling time is 1～3 hour;
(4) mist projection granulating and moulding: above-mentioned secondary sand milling material is carried out mist projection granulating in spray tower, mist projection granulating is made the particle that particle diameter is 50～200 μ m; Be shaped to blank then with definite shape;
(5) sintering: the blank after the above-mentioned moulding is carried out carrying out sintering under 1260 ℃～1350 ℃ temperature range, promptly form high saturated flux low consumption MnZn power ferrite behind the sintering.
5, the preparation method of a kind of high saturated flux low consumption MnZn power ferrite according to claim 4, the granularity that it is characterized in that powder described in the step (3) are 1～1.18 μ m, SiO in the secondary sand milling material
2Weight percentage be 0.005～0.023wt%.
6, the preparation method of a kind of high saturated flux low consumption MnZn power ferrite according to claim 4, add PVA and defoamer when it is characterized in that in the step (4) mist projection granulating, wherein both ratios are 20: 1, and described defoamer is a kind of in ammoniacal liquor, the n-octyl alcohol.
7, the preparation method of a kind of high saturated flux low consumption MnZn power ferrite according to claim 4 is characterized in that the sintering process described in the step (5) carries out at the environment of oxygen and nitrogen, and wherein the scope of partial pressure of oxygen is: 1～10%.
8, a kind of high saturated flux low consumption MnZn power ferrite according to the described preparation method's preparation of claim 4～7.
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