CN105036723A - Nickel-zinc-copper ferrite powder and preparation method thereof - Google Patents

Nickel-zinc-copper ferrite powder and preparation method thereof Download PDF

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CN105036723A
CN105036723A CN201510359965.4A CN201510359965A CN105036723A CN 105036723 A CN105036723 A CN 105036723A CN 201510359965 A CN201510359965 A CN 201510359965A CN 105036723 A CN105036723 A CN 105036723A
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powder
nickel
copper
zinc ferrite
ball milling
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欧阳辰鑫
朱建华
施威
王智会
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Shenzhen Zhenhua Ferrite and Ceramic Electronics Co Ltd
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Shenzhen Zhenhua Ferrite and Ceramic Electronics Co Ltd
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Abstract

The invention relates to nickel-zinc-copper ferrite powder and a preparation method thereof. The preparation method comprises the following steps: mixing Fe2O3 powder, CuO powder, ZnO powder and NiO powder with the particle sizes of 0.18-0.52 through adding water, so as to obtain slurry; drying the slurry, so as to obtain mixed powder; calcining the mixed powder at the temperature of 700-900 DEG C for 4-6 hours, so as to obtain the nickel-zinc-copper ferrite powder. According to the invention, the particle sizes of the nickel-zinc-copper ferrite powder prepared through the preparation method are mainly distributed between 0.4 micron and 1.0 micron, and the nickel-zinc-copper ferrite powder is enabled to have relatively low sintering temperature; the nickel-zinc-copper ferrite powder prepared through the preparation method has better low temperature co-firing property, and can be well co-fired with other ceramic materials or silver electrode in a matching manner.

Description

Nickel-copper-zinc ferrite powder and preparation method thereof
Technical field
The present invention relates to the manufacture field of Ferrite Material, particularly relate to a kind of nickel-copper-zinc ferrite powder and preparation method thereof.
Background technology
Laminated inductive is as preventing one of the most effective element of electromagnetic interference, and it gets final product the larger galvanic current of load, can absorb power supply noise preferably again, and the slice structure of its surface mounting also can adapt to little, the lightweight requirement of novel electron equipment volume.
Wherein, low temperature co-fired technology is the important technology of such laminated inductor of research and production, and it adopts low temperature sintered ferrite material as main raw materials for production, prepares the laminated inductance with unique texture by advanced technologies such as curtain coating, printings, altogether burning.Low temperature co-firedly usually occur in 900 DEG C to 950 DEG C, this just requires that Ferrite Material must obtain higher sintered density in this temperature range.
Realize the low sintering method of ferrite to have a lot, mainly comprise: 1) add fusing assistant, introducing low melting point and base ingredients form the additive of eutectic mixture, to form liquid phase sintering at a lower temperature, facilitate the low-temperature sintering densification of material.Normally used fusing assistant has bismuth oxide, molybdenum oxide, vanadium oxide etc.; 2) substitutional ion, the ion that employing can enter lattice generation single phase solid solution carries out appropriate substitutional ion, make its component as body material in sintering process, participate in forming the modified compound had compared with low melting point, to reach the object reducing sintering temperature; 3) meticulous powder process, superfine powder due to specific surface area large, the contact area between particle is large, by the high surface free energy acceleration of sintering of powder, reaches and reduces solid state reaction temperature, realize the object of low temperature densification.
In recent years, domestic and international many researchers adopt the wet chemistry methods such as sol-gel method, coprecipitation method, self-propagating high-temperature synthesis to prepare meticulous ferrite powder, but the grain diameter of ferrite powder prepared by these methods is less, and preparation cost is higher, output is lower, limits its commercial application.And prepare in the synthesis technique of Ferrite Material multiple, because solid-phase synthesis possesses, preparation cost is cheap, repeatability is higher, output advantages of higher, by all multiple enterprises and research unit favor, but the grain diameter of ferrite powder prepared by traditional solid-phase synthesis is larger, low temperature co-fired characteristic is poor, still limits its commercial application.
Summary of the invention
Given this, one is necessary to provide can to prepare the less and good nickel-copper-zinc ferrite raw powder's production technology of low temperature co-fired characteristic of grain diameter.
In addition, a kind of nickel-copper-zinc ferrite powder is also provided.
A kind of nickel-copper-zinc ferrite raw powder's production technology, comprises the steps:
Grain diameter is the described Fe of 0.18 ~ 0.52 micron 2o 3powder, CuO powder, ZnO powder and NiO powder add water mixing, obtain slurry;
By described slurry drying, obtain mixed powder; And
By described mixed powder in 700 ~ 900 DEG C of insulation calcinings 4 ~ 6 hours, obtain nickel-copper-zinc ferrite powder.
Wherein in an embodiment, by described Fe 2o 3powder, CuO powder, ZnO powder and NiO powder add water mixing step before also comprise described Fe 2o 3powder, CuO powder, ZnO powder and NiO powder respectively ball milling are refined to the step of 0.18 ~ 0.52 micron; Wherein, described Fe 2o 3in the step of powder ball milling refinement, ball milling and described Fe 2o 3the mass ratio of powder is 10:1 ~ 20:1; In the step of described CuO powder ball milling refinement, ball milling is 10:1 ~ 20:1 with the mass ratio of described CuO powder; In the step of described ZnO powder ball milling refinement, ball milling is 10:1 ~ 20:1 with the mass ratio of described ZnO powder; In the step of described NiO powder ball milling refinement, ball milling is 10:1 ~ 20:1 with the mass ratio of described NiO powder.
Wherein in an embodiment, grain diameter is the described Fe of 0.18 ~ 0.52 micron 2o 3powder, CuO powder, ZnO powder and NiO powder add water in the step of mixing, described Fe 2o 3the molar percentage of powder, CuO powder, ZnO powder and NiO powder is 47 ~ 49%:8 ~ 15%:15 ~ 28%:15 ~ 28%.
Wherein in an embodiment, by described Fe 2o 3powder, CuO powder, ZnO powder and NiO powder add water mixing step be specially: by described Fe 2o 3powder, CuO powder, ZnO powder and NiO powder add water for ball milling mixing 4 ~ 8 hours.
Wherein in an embodiment, the step of described slurry drying is specially: by described slurry in 100 ~ 150 DEG C of dryings 5 ~ 10 hours.
Wherein in an embodiment, described mixed powder is carried out in the step of 700 ~ 900 DEG C of insulation calcinings is atmosphere at air.
Wherein in an embodiment, by described mixed powder before the step of 700 ~ 900 DEG C of insulation calcinings, also comprise the step described mixed powder being crossed 100 ~ 120 mesh sieves.
The nickel-copper-zinc ferrite powder prepared by above-mentioned nickel-copper-zinc ferrite raw powder's production technology, and the grain diameter of described nickel-copper-zinc ferrite powder is mainly distributed in 0.4 micron ~ 1.0 microns.
The step of above-mentioned nickel-copper-zinc ferrite raw powder's production technology is simple, relative to wet chemical methods such as sol-gel methodes, has with low cost, that output is large advantage.And the Fe of above-mentioned nickel-copper-zinc ferrite raw powder's production technology by adopting grain diameter to be 0.18 ~ 0.52 micron 2o 3powder, CuO powder, ZnO powder and NiO powder, the grain diameter of final nickel-copper-zinc ferrite powder is reduced with the grain diameter reducing the front each raw material of mixing, thus make the grain diameter of the nickel-copper-zinc ferrite powder obtained lower than 1.0 microns, compared with the nickel-copper-zinc ferrite powder prepared with traditional solid-phase synthesis, the nickel-copper-zinc ferrite powder that above-mentioned preparation method prepares has less grain diameter, be conducive to reducing sintering temperature, and the nickel-copper-zinc ferrite powder that aforesaid method prepares has higher surface energy, contribute to reducing sintering temperature, the nickel-copper-zinc ferrite powder that aforesaid method is prepared has good low temperature co-fired characteristic, can with other stupalith or electrode silver well matching co-firing.
Accompanying drawing explanation
Fig. 1 is the preparation flow figure of the nickel-copper-zinc ferrite raw powder's production technology of an embodiment;
Fig. 2 is the scanning electron microscope (SEM) photograph of the nickel-copper-zinc ferrite powder of embodiment 1;
Fig. 3 is the scanning electron microscope (SEM) photograph of the nickel-copper-zinc ferrite powder of embodiment 2.
Embodiment
Mainly in conjunction with the drawings and the specific embodiments nickel-copper-zinc ferrite powder and preparation method thereof is described in further detail below.
As shown in Figure 1, the nickel-copper-zinc ferrite raw powder's production technology of an embodiment, comprises the steps:
Step S110: Fe grain diameter being 0.18 ~ 0.52 micron 2o 3powder, CuO powder, ZnO powder and NiO powder add water mixing, obtain slurry.
Wherein, by Fe 2o 3powder, CuO powder, ZnO powder and NiO powder add water mixing step before, also comprise Fe 2o 3the step of powder, CuO powder, ZnO powder and the refinement of NiO powder ball milling, to make Fe 2o 3the grain diameter of powder, CuO powder, ZnO powder and NiO powder is 0.18 ~ 0.52 micron.
Wherein, Fe 2o 3in the step of powder ball milling refinement, ball milling and Fe 2o 3the mass ratio of powder is 10:1 ~ 20:1; In the step of CuO powder ball milling refinement, ball milling is 10:1 ~ 20:1 with the mass ratio of CuO powder; In the step of ZnO powder ball milling refinement, ball milling is 10:1 ~ 20:1 with the mass ratio of ZnO powder; In the step of NiO powder ball milling refinement, ball milling is 10:1 ~ 20:1 with the mass ratio of NiO powder.
Wherein, in step S110, by Fe 2o 3powder, CuO powder, ZnO powder and NiO powder add water in the step of mixing, Fe 2o 3the molar percentage of powder, CuO powder, ZnO powder and NiO powder is 47 ~ 49%:8 ~ 15%:15 ~ 28%:15 ~ 28%.
Wherein, by Fe 2o 3powder, CuO powder, ZnO powder and NiO powder add water mixing step in water be deionized water.
Wherein, grain diameter is the Fe of 0.18 ~ 0.52 micron 2o 3powder, CuO powder, ZnO powder and NiO powder add water mixing step be specially: Fe grain diameter being 0.18 ~ 0.52 micron 2o 3powder, CuO powder, ZnO powder and NiO powder add water for ball milling mixing 4 ~ 8 hours.
Step S120: by slurry drying, obtains mixed powder.
Wherein, the step of slurry drying is specially: by slurry in 100 ~ 150 DEG C of dryings 5 ~ 10 hours.
Step S130: by mixed powder in 700 ~ 900 DEG C of insulation calcinings 4 ~ 6 hours, obtain nickel-copper-zinc ferrite powder.
Wherein, by mixed powder before the step of 700 ~ 900 DEG C of insulation calcinings, also comprise step mixed powder being crossed 100 ~ 120 mesh sieves, thus obtain the comparatively uniform mixed powder of grain diameter.
Wherein, mixed powder is carried out in the step of 700 DEG C ~ 900 DEG C insulation calcinings is atmosphere at air.
Wherein, by mixed powder after the step of 700 DEG C ~ 900 DEG C insulation calcinings, by nickel-copper-zinc ferrite powder naturally cooling.
Wherein, the grain diameter of nickel-copper-zinc ferrite powder that step S130 obtains mainly is distributed in 0.4 micron ~ 1.0 microns.
The step of above-mentioned nickel-copper-zinc ferrite raw powder's production technology is simple, relative to wet chemical methods such as sol-gel methodes, has with low cost, that output is large advantage.And the Fe of above-mentioned nickel-copper-zinc ferrite raw powder's production technology by adopting grain diameter to be 0.18 ~ 0.52 micron 2o 3powder, CuO powder, ZnO powder and NiO powder, the grain diameter of final nickel-copper-zinc ferrite powder is reduced with the grain diameter reducing the front each raw material of mixing, thus make the grain diameter of the nickel-copper-zinc ferrite powder obtained mainly be distributed in 0.4 micron ~ 1.0 microns, compared with the nickel-copper-zinc ferrite powder prepared with traditional solid-phase synthesis, the nickel-copper-zinc ferrite powder that above-mentioned preparation method prepares has less grain diameter, be conducive to reducing sintering temperature, and the nickel-copper-zinc ferrite powder that aforesaid method prepares has higher surface energy, contribute to reducing sintering temperature, the nickel-copper-zinc ferrite powder that aforesaid method is prepared has good low temperature co-fired characteristic, can with other stupalith or electrode silver well matching co-firing.
The nickel-copper-zinc ferrite powder prepared by above-mentioned nickel-copper-zinc ferrite raw powder's production technology, the grain diameter of this nickel-copper-zinc ferrite powder is mainly distributed in 0.4 micron ~ 1.0 microns.And this nickel-copper-zinc ferrite powder has lower sintering temperature (sintering temperature is 850 DEG C ~ 920 DEG C), and make it have good low temperature co-fired characteristic, can with other stupalith or electrode silver well matching co-firing.
Be below specific embodiment part:
Embodiment 1
The preparation process of the nickel-copper-zinc ferrite powder of the present embodiment is as follows:
(1) by Fe 2o 3the refinement of powder ball milling, to make Fe 2o 3the grain diameter of powder is 0.18 ~ 0.22 micron, wherein, and ball milling and Fe 2o 3the mass ratio of powder is 20:1; By the refinement of CuO powder ball milling, to make CuO powder granule particle diameter be 0.18 ~ 0.22 micron, wherein, ball milling is 20:1 with the mass ratio of CuO powder; By the refinement of ZnO powder ball milling, to make ZnO powder granule particle diameter be 0.18 ~ 0.22 micron, wherein, ball milling is 20:1 with the mass ratio of ZnO powder; By the refinement of NiO powder ball milling, to make NiO powder granule particle diameter be 0.18 ~ 0.22 micron, wherein, ball milling is 20:1 with the mass ratio of NiO powder.
(2) according to molar percentage, by the Fe after the ball milling of 49% 2o 3powder, 8% ball milling after CuO powder, 28% ball milling after ZnO powder and 15% ball milling after NiO powder in ball mill, add deionized water ball milling mix 6 hours, obtain slurry.
(3) by slurry in 150 DEG C of dryings 8 hours, obtain mixed powder, then mixed powder crossed 120 mesh sieves.
(4) under the atmosphere of air, by the 850 DEG C of insulation calcinings 4 hours in High Temperature Furnaces Heating Apparatus of the mixed powder after sieving, then with stove naturally cooling, nickel-copper-zinc ferrite powder is obtained.
In the nickel-copper-zinc ferrite powder of the present embodiment, add mass percentage concentration is that the aqueous solution of the polyvinyl alcohol of 5% carries out granulation, and adopts the axle pressure compression moulding of 300MPa, in 900 DEG C of heat preservation sinterings 2 hours, obtains nickel-copper-zinc ferrite.
Fig. 2 is the scanning electron microscope (SEM) photograph of the nickel-copper-zinc ferrite powder of the present embodiment, as can see from Figure 2, the grain diameter of the nickel-copper-zinc ferrite powder of the present embodiment is mainly distributed in 0.4 micron ~ 1.0 microns, and the grain diameter of nearly all nickel-copper-zinc ferrite powder is all below 1.0 microns.
The nickel-copper-zinc ferrite powder of the present embodiment is prepared laminated chip inductor sample, wherein, sintering schedule is 900 DEG C of heat preservation sinterings 2 hours, the two-phase of the nickel-copper-zinc ferrite and stupalith of observing the laminated chip inductor sample prepared respectively burns the bonding state at interface altogether, and nickel-copper-zinc ferrite and electrode silver two-phase burn the bonding state at interface altogether, thus obtain the low temperature co-fired performance of the nickel-copper-zinc ferrite powder of the present embodiment, wherein, the nickel-copper-zinc ferrite powder of the present embodiment respectively with the low temperature co-fired performance of stupalith and electrode silver in table 1.
Embodiment 2
The preparation process of the nickel-copper-zinc ferrite powder of the present embodiment is as follows:
(1) by Fe 2o 3powder ball milling, to make Fe 2o 3the grain diameter of powder is 0.48 ~ 0.52 micron, wherein, and ball milling and Fe 2o 3the mass ratio of powder is 10:1; By CuO powder ball milling, to make CuO powder granule particle diameter be 0.48 ~ 0.52 micron, wherein, ball milling is 10:1 with the mass ratio of CuO powder; By ZnO powder ball milling, to make ZnO powder granule particle diameter be 0.48 ~ 0.52 micron, wherein, ball milling is 10:1 with the mass ratio of ZnO powder; By NiO powder ball milling, to make NiO powder granule particle diameter be 0.48 ~ 0.52 micron, wherein, ball milling is 10:1 with the mass ratio of NiO powder.
(2) according to molar percentage, by the Fe after the ball milling of 47% 2o 3powder, 15% ball milling after CuO powder, 15% ball milling after ZnO powder and 23% ball milling after NiO powder in ball mill, add deionized water ball milling mix 6 hours, obtain slurry.
(3) by slurry in 150 DEG C of dryings 8 hours, obtain mixed powder, then mixed powder crossed 120 mesh sieves.
(4) under the atmosphere of air, by the 850 DEG C of insulation calcinings 4 hours in High Temperature Furnaces Heating Apparatus of the mixed powder after sieving, then with stove naturally cooling, nickel-copper-zinc ferrite powder is obtained.
In the nickel-copper-zinc ferrite powder of the present embodiment, add mass percentage concentration is that the aqueous solution of the polyvinyl alcohol of 5% carries out granulation, and adopts the axle pressure compression moulding of 300MPa, in 880 DEG C of heat preservation sinterings 3 hours, obtains nickel-copper-zinc ferrite.
Fig. 3 is the scanning electron microscope (SEM) photograph of the nickel-copper-zinc ferrite powder of the present embodiment, as can see from Figure 3, the grain diameter of the nickel-copper-zinc ferrite powder of the present embodiment is mainly distributed in 0.6 micron ~ 1.0 microns, and the grain diameter of nearly all nickel-copper-zinc ferrite powder is all below 1.0 microns.
Adopt the identical testing method of embodiment 1 to test the low temperature co-fired performance of the nickel-copper-zinc ferrite powder of the present embodiment, the nickel-copper-zinc ferrite powder obtaining the present embodiment respectively with the low temperature co-fired performance of stupalith and electrode silver in table 1
Embodiment 3
The preparation process of the nickel-copper-zinc ferrite powder of the present embodiment is as follows:
(1) by Fe 2o 3powder ball milling, to make Fe 2o 3the grain diameter of powder is 0.28 ~ 0.32 micron, wherein, and ball milling and Fe 2o 3the mass ratio of powder is 15:1; By CuO powder ball milling, to make CuO powder granule particle diameter be 0.28 ~ 0.32 micron, wherein, ball milling is 15:1 with the mass ratio of CuO powder; By ZnO powder ball milling, to make ZnO powder granule particle diameter be 0.28 ~ 0.32 micron, wherein, ball milling is 15:1 with the mass ratio of ZnO powder; By NiO powder ball milling, to make NiO powder granule particle diameter be 0.28 ~ 0.32 micron, wherein, ball milling is 15:1 with the mass ratio of NiO powder.
(2) according to molar percentage, by the Fe after the ball milling of 48% 2o 3powder, 12% ball milling after CuO powder, 12% ball milling after ZnO powder and 28% ball milling after NiO powder in ball mill, add deionized water ball milling mix 4 hours, obtain slurry.
(3) by slurry in 100 DEG C of dryings 10 hours, obtain mixed powder, then mixed powder crossed 110 mesh sieves.
(4) under the atmosphere of air, by the 700 DEG C of insulation calcinings 6 hours in High Temperature Furnaces Heating Apparatus of the mixed powder after sieving, then with stove naturally cooling, nickel-copper-zinc ferrite powder is obtained.
In the nickel-copper-zinc ferrite powder of the present embodiment, add mass percentage concentration is that the aqueous solution of the polyvinyl alcohol of 5% carries out granulation, and adopts the axle pressure compression moulding of 300MPa, in 850 DEG C of heat preservation sinterings 4 hours, obtains nickel-copper-zinc ferrite.
The grain diameter of the nickel-copper-zinc ferrite powder of the present embodiment is mainly distributed in 0.5 micron ~ 1.0 microns, and the grain diameter of nearly all nickel-copper-zinc ferrite powder is all below 1.0 microns.
Adopt the identical testing method of embodiment 1 to test the low temperature co-fired performance of the nickel-copper-zinc ferrite powder of the present embodiment, the nickel-copper-zinc ferrite powder obtaining the present embodiment respectively with the low temperature co-fired performance of stupalith and electrode silver in table 1
Embodiment 4
The preparation process of the nickel-copper-zinc ferrite powder of the present embodiment is as follows:
(1) by Fe 2o 3powder ball milling, to make Fe 2o 3the grain diameter of powder is 0.38 ~ 0.42 micron, wherein, and ball milling and Fe 2o 3the mass ratio of powder is 15:1; By CuO powder ball milling, to make CuO powder granule particle diameter be 0.38 ~ 0.42 micron, wherein, ball milling is 15:1 with the mass ratio of CuO powder; By ZnO powder ball milling, to make ZnO powder granule particle diameter be 0.38 ~ 0.42 micron, wherein, ball milling is 15:1 with the mass ratio of ZnO powder; By NiO powder ball milling, to make NiO powder granule particle diameter be 0.38 ~ 0.42 micron, wherein, ball milling is 15:1 with the mass ratio of NiO powder.
(2) according to molar percentage, by the Fe after the ball milling of 48% 2o 3powder, 12% ball milling after CuO powder, 12% ball milling after ZnO powder and 28% ball milling after NiO powder in ball mill, add deionized water ball milling mix 8 hours, obtain slurry.
(3) by slurry in 150 DEG C of dryings 5 hours, obtain mixed powder, then mixed powder crossed 100 mesh sieves.
(4) under the atmosphere of air, by the 900 DEG C of insulation calcinings 4 hours in High Temperature Furnaces Heating Apparatus of the mixed powder after sieving, then with stove naturally cooling, nickel-copper-zinc ferrite powder is obtained.
In the nickel-copper-zinc ferrite powder of the present embodiment, add mass percentage concentration is that the aqueous solution of the polyvinyl alcohol of 5% carries out granulation, and adopts the axle pressure compression moulding of 300MPa, in 920 DEG C of heat preservation sinterings 1 hour, obtains nickel-copper-zinc ferrite.
The grain diameter of the nickel-copper-zinc ferrite powder of the present embodiment is mainly distributed in 0.45 micron ~ 1.0 microns, and the grain diameter of nearly all nickel-copper-zinc ferrite powder is all below 1.0 microns.
Adopt the identical testing method of embodiment 1 to test the low temperature co-fired performance of the nickel-copper-zinc ferrite powder of the present embodiment, the nickel-copper-zinc ferrite powder obtaining the present embodiment respectively with the low temperature co-fired performance of stupalith and electrode silver in table 1
Comparative example 1
The preparation process of the nickel-copper-zinc ferrite powder of comparative example 1 is as follows:
(1) according to molar percentage, by the Fe of the non-ball milling of 49% 2o 3powder, the CuO powder of non-ball milling of 8%, the NiO powder of the ZnO powder of the non-ball milling of 28% and the non-ball milling of 15% add deionized water ball milling and mix 6 hours in ball mill, obtain slurry.Wherein, Fe 2o 3powder, CuO powder, ZnO powder and 15% the grain diameter of NiO powder be 1.5 ~ 2.1 μm.
(2) by slurry in 150 DEG C of dryings 8 hours, obtain mixed powder, then mixed powder crossed 120 mesh sieves.
(3) under the atmosphere of air, by the 850 DEG C of insulation calcinings 4 hours in High Temperature Furnaces Heating Apparatus of the mixed powder after sieving, then with stove naturally cooling, nickel-copper-zinc ferrite powder is obtained.
In the nickel-copper-zinc ferrite powder of comparative example 1, add mass percentage concentration is that the aqueous solution of the polyvinyl alcohol of 5% carries out granulation, and adopts the axle pressure compression moulding of 300MPa, in 900 DEG C of heat preservation sinterings 2 hours, obtains nickel-copper-zinc ferrite.
By sem test, the grain diameter obtaining the nickel-copper-zinc ferrite powder of comparative example 1 is mainly distributed in 1.8 microns ~ 2.5 microns.
Adopt the identical testing method of embodiment 1 to test the low temperature co-fired performance of the nickel-copper-zinc ferrite powder of the present embodiment, the nickel-copper-zinc ferrite powder obtaining comparative example 1 respectively with the low temperature co-fired performance of stupalith and electrode silver in table 1.
What table 1 represented the is nickel-copper-zinc ferrite powder of embodiment 1 ~ 4 and comparative example 1 respectively with the low temperature co-fired performance of stupalith and electrode silver.
Table 1
As can be seen from Table 1, embodiment 1 ~ 4 nickel-copper-zinc ferrite powder can with stupalith and electrode silver well matching co-firing.
For the ease of comparing, the main distribution range of the grain diameter of the nickel-copper-zinc ferrite powder of embodiment 1 ~ 4 and comparative example 1 and sintering temperature are all listed in table 2, particle size distribution and the sintering temperature of what table 2 represented the is nickel-copper-zinc ferrite powder of embodiment 1 ~ 4 and comparative example 1.
Table 2
The ultra-fine nickel-copper-zinc ferrite powder that the preparation method of embodiment 1 ~ 4 obtains as seen from Table 2 can sinter within the scope of 850 DEG C ~ 920 DEG C, and can obtain higher sintered density, reaches the feature reducing sintering temperature.Wherein, sintering relative density after nickel-copper-zinc ferrite powder prepared by embodiment 1 is incubated 2 hours at 900 DEG C is up to 99.85%, and the nickel-copper-zinc ferrite powder of comparative example 1 is 95.21% at the sintering relative density of 900 DEG C of insulations after 2 hours, obviously, the nickel-copper-zinc ferrite powder adopting the method for embodiment 1 ~ 4 to prepare can obtain higher relative density under identical sintering schedule.
And from table 2, it can also be seen that the grain diameter of the nickel-copper-zinc ferrite powder that the preparation method of embodiment 1 ~ 4 obtains is less, the nickel-copper-zinc ferrite powder that the preparation method much smaller than comparative example 1 obtains.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.

Claims (8)

1. a nickel-copper-zinc ferrite raw powder's production technology, is characterized in that, comprises the steps:
Grain diameter is the Fe of 0.18 ~ 0.52 micron 2o 3powder, CuO powder, ZnO powder and NiO powder add water mixing, obtain slurry;
By described slurry drying, obtain mixed powder; And
By described mixed powder in 700 ~ 900 DEG C of insulation calcinings 4 ~ 6 hours, obtain nickel-copper-zinc ferrite powder.
2. nickel-copper-zinc ferrite raw powder's production technology according to claim 1, is characterized in that, by described Fe 2o 3powder, CuO powder, ZnO powder and NiO powder add water mixing step before also comprise described Fe 2o 3powder, CuO powder, ZnO powder and NiO powder respectively ball milling are refined to the step of 0.18 ~ 0.52 micron; Wherein, described Fe 2o 3in the step of powder ball milling refinement, ball milling and described Fe 2o 3the mass ratio of powder is 10:1 ~ 20:1; In the step of described CuO powder ball milling refinement, ball milling is 10:1 ~ 20:1 with the mass ratio of described CuO powder; In the step of described ZnO powder ball milling refinement, ball milling is 10:1 ~ 20:1 with the mass ratio of described ZnO powder; In the step of described NiO powder ball milling refinement, ball milling is 10:1 ~ 20:1 with the mass ratio of described NiO powder.
3. nickel-copper-zinc ferrite raw powder's production technology according to claim 1, is characterized in that, grain diameter is the described Fe of 0.18 ~ 0.52 micron 2o 3powder, CuO powder, ZnO powder and NiO powder add water in the step of mixing, described Fe 2o 3the molar percentage of powder, CuO powder, ZnO powder and NiO powder is 47 ~ 49%:8 ~ 15%:15 ~ 28%:15 ~ 28%.
4. nickel-copper-zinc ferrite raw powder's production technology according to claim 1, is characterized in that, by described Fe 2o 3powder, CuO powder, ZnO powder and NiO powder add water mixing step be specially: by described Fe 2o 3powder, CuO powder, ZnO powder and NiO powder add water for ball milling mixing 4 ~ 8 hours.
5. nickel-copper-zinc ferrite raw powder's production technology according to claim 1, is characterized in that, the step of described slurry drying is specially: by described slurry in 100 ~ 150 DEG C of dryings 5 ~ 10 hours.
6. nickel-copper-zinc ferrite raw powder's production technology according to claim 1, is characterized in that, is carried out by described mixed powder in the step of 700 ~ 900 DEG C of insulation calcinings is atmosphere at air.
7. nickel-copper-zinc ferrite raw powder's production technology according to claim 1, is characterized in that, by described mixed powder before the step of 700 ~ 900 DEG C of insulation calcinings, also comprises the step described mixed powder being crossed 100 ~ 120 mesh sieves.
8. the nickel-copper-zinc ferrite powder prepared by the nickel-copper-zinc ferrite raw powder's production technology described in claim 1 ~ 7 any one, and the grain diameter of described nickel-copper-zinc ferrite powder is mainly distributed in 0.4 micron ~ 1.0 microns.
CN201510359965.4A 2015-06-25 2015-06-25 Nickel-zinc-copper ferrite powder and preparation method thereof Pending CN105036723A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1548494A (en) * 2003-05-06 2004-11-24 千如电机工业股份有限公司 Epoxy resin and inductor assembly for preventing electromagnetic interference
CN102982957A (en) * 2012-12-03 2013-03-20 深圳顺络电子股份有限公司 NiZnCu ferrite material and laminated chip electronic element manufactured by using same
CN103265275A (en) * 2013-05-15 2013-08-28 江粉磁材（武汉）技术研发有限公司 NiCuZn ferrite material 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

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1548494A (en) * 2003-05-06 2004-11-24 千如电机工业股份有限公司 Epoxy resin and inductor assembly for preventing electromagnetic interference
CN102982957A (en) * 2012-12-03 2013-03-20 深圳顺络电子股份有限公司 NiZnCu ferrite material and laminated chip electronic element manufactured by using same
CN103265275A (en) * 2013-05-15 2013-08-28 江粉磁材（武汉）技术研发有限公司 NiCuZn ferrite material 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

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Application publication date: 20151111