CN115010479A - Non-shrinkage nickel-copper-zinc ferrite material and preparation method thereof - Google Patents
Non-shrinkage nickel-copper-zinc ferrite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a non-shrinkage nickel-copper-zinc ferrite material and a preparation method thereof, wherein the preparation method comprises the following steps: firstly, according to the mol ratio of NiO to CuO to ZnO to Fe 2 O 3 Mixing the raw materials according to the ratio of 0.2:0.22:0.6:0.98, and sequentially carrying out first ball milling and drying to obtain mixed powder; then pre-burning the mixed powder to obtain a pre-burned material; then, mixing the pre-sintered material and the supplementary material, adding an additive, and sequentially carrying out second ball milling, drying, granulation and compression molding to obtain a green body; the supplementary material comprises a simple substance of iron, NiO, CuO and ZnO; and finally, sintering the green body to obtain the shrinkage-free nickel-copper-zinc ferrite material. The non-shrinkage nickel-copper-zinc ferrite material is obtained by the preparation method. The non-shrinkage nickel-copper-zinc ferrite material provided by the invention can realize no shrinkage under low-temperature sintering, and has a uniform and compact structure. The preparation method provided by the invention is simple to operate and can be applied industrially.
Description
Technical Field
The invention relates to the technical field of permanent magnet material ferrite, in particular to a non-shrinkage nickel-copper-zinc ferrite material and a preparation method thereof.
Background
As electronic devices are developed to be portable, miniaturized, networked, and multimedia, circuit assembly technology is rapidly developed to be surface mounting technology, and the core foundation of the development is electronic materials. The mainstream direction of electronic materials is laminated chip components with a monolithic structure, wherein chip capacitors and chip resistors are the mainstream, and chip inductors are relatively lagged behind. At present, the industrial production of the laminated inductor is realized, and the co-firing matching of the ferrite and the silver electrode is a technical key.
Ferrite materials generally need to satisfy the following characteristics: easy synthesis, low cost, low sintering temperature (co-firing with silver electrodes) and high performance (high permeability and high resistivity). The current chip inductor material mainly focuses on NiCuZn ferrite material sintered at low temperature, but the material has large magnetostriction coefficient, so the material is sensitive to stress, the ferrite material can generate 10-15% of size shrinkage during sintering, the size dispersion of the product is large, and high size precision is difficult to realize; in addition, the size shrinkage can also generate stress, strain, cracks and the like among different materials, so that the composition with the different materials is difficult to realize; furthermore, the stress from the inner conductor and the stress generated at the time of substrate mounting also cause deterioration of the magnetic properties of the material.
CN107857581A discloses a low-temperature sintered NiCuZn ferrite material and a preparation method thereof, wherein the molecular structure expression of the material obtained by the method is Ni 0.29-x-y Zn 0.53+x Cu 0.18+y Fe 1.95 O 4 (x is 0-0.02; y is 0-0.02) and BBSZ glass and Co are used simultaneously 2 O 3 、TiO 2 And CaCO 3 As a dopant. Through the optimization design of the material formula and the process and the combination modification of 4 dopants, the low-temperature sintering at 900 ℃ is realized, and the initial permeability mu is considered i Between 80 and 96.
CN108503349A discloses a high magnetic field resistant low temperature sintered NiCuZn ferrite material and a preparation method thereof, and the method adopts 1 wt% Bi on the basis of the NiCuZn ferrite material formula 2 O 3 And 2.5-3.5 wt% Zn 2 SiO 4 The pre-sintering material is subjected to combined doping, so that low-temperature sintering at 900 ℃ is realized, and the initial permeability mu is i Between 65.3 and 70.4.
CN113603472A discloses a preparation method of NiCuZn ferrite based on LTCC technology, which comprises the steps of material preparation, first ball milling, first drying, presintering, doping, second ball milling, seventh drying, granulation molding, binder removal, sintering and the like, and Bi is used for preparing the ferrite through Bi 2 O 3 And Co 2 O 3 The NiCuZn ferrite with high density, small pores and excellent magnetic performance can be obtained by binary doping.
In conclusion, although the existing research reports a lot of methods for preparing NiCuZn ferrite, no effective solution is available for solving the problem of NiCuZn ferrite low-temperature sintering shrinkage. Therefore, the development of the low-temperature sintering shrinkage-free nickel-copper-zinc ferrite material and the preparation method thereof have important significance for solving the problems of large size dispersion, poor high size precision, low magnetic performance and the like of the ferrite.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a non-shrinkage nickel-copper-zinc ferrite material and a preparation method thereof, wherein compared with the prior art, the non-shrinkage nickel-copper-zinc ferrite material provided by the present invention can realize non-shrinkage at low temperature sintering, and has uniform and compact microstructure and excellent magnetic property.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a preparation method of a non-shrinkage nickel-copper-zinc ferrite material, which comprises the following steps:
(1) according to the mol ratio of NiO to CuO to ZnO to Fe 2 O 3 Mixing the raw materials according to the ratio of 0.2:0.22:0.6:0.98, and then sequentially carrying out first ball milling and drying to obtain mixed powder;
(2) pre-burning the mixed powder obtained in the step (1) to obtain a pre-burnt material;
(3) mixing the pre-sintered material and the supplementary material obtained in the step (2), adding an additive, and then sequentially carrying out second ball milling, drying, granulation and compression molding to obtain a green body;
the supplementary material comprises a simple substance of iron, NiO, CuO and ZnO;
(4) and (4) sintering the green body obtained in the step (3) to obtain the non-shrinkage nickel-copper-zinc ferrite material.
The invention utilizes the oxidation expansion reaction of metallic iron simple substance (iron powder)The control of the ferrite dimensional change rate can be achieved. In one aspect, the molecular formula of the pre-sintering material is controlled to be Ni 0.2 Cu 0.22 Zn 0.6 Fe 1.96 O x While controlling the composition of the supplementary material to maintain the molecular formula of the product, thereby obtaining Ni 0.2 Cu 0.22 Zn 0.6 Fe 1.96 O x The ferrite material, namely the invention can freely regulate and control the size change from shrinkage to expansion by controlling the pre-sintering material and the supplementary material and changing the ratio of the pre-sintering material and the supplementary material so as to finally realize that the size change rate is 0. On the other hand, the simple substance of the metallic iron is accompanied with uneven grain growth under sintering, so the invention also controls the synergistic effect of the simple substance of the metallic iron and the additive of the low-melting-point oxide to supply the simple substance of the metallic iron and the surrounding oxide with oxygen in the sintering process of the additive of the low-melting-point oxide, thereby promoting ferrite transformation, ensuring uniform ferrite structure and completely eliminating residual metallic iron.
Preferably, the powder mixture of step (1) has an average particle size of 1.5 to 1.9. mu.m, which may be, for example, 1.5. mu.m, 1.6. mu.m, 1.7. mu.m, 1.8. mu.m or 1.9. mu.m, but is not limited to the values recited, and other values not recited in the numerical ranges are equally applicable.
Preferably, the drying temperature in step (1) is 150-200 ℃, for example, 150 ℃, 160 ℃, 170 ℃, 180 ℃, 190 ℃ or 200 ℃, but not limited to the recited values, and other unrecited values within the range of values are equally applicable.
Preferably, the temperature of the pre-sintering in step (2) is 850-.
Preferably, the pre-firing time is 1.5-2.5h, for example, 1.5h, 1.6h, 1.7h, 1.8h, 1.9h, 2.0h, 2.1h, 2.2h, 2.3h, 2.4h or 2.5h, but not limited to the recited values, and other values in the range of values are also applicable.
Preferably, the volume of the supplementary material in step (3) is 60-65% of the volume of the calcined material, such as 60%, 61%, 62%, 63%, 64% or 65%, but not limited to the recited values, and other values not recited in the range of values are also applicable.
The invention preferably controls the volume of the supplementary material in percentage of the volume of the pre-sintering material, and can enhance the magnetism of the ferrite while controlling the size change rate.
Preferably, the molar ratio of the simple substance of iron, NiO, CuO and ZnO in the supplement is 1.96:0.2:0.22: 0.6.
The invention preferably controls the molar ratio of the iron simple substance, NiO, CuO and ZnO to be 1.96:0.2:0.22:0.6, because the combination of the iron simple substance and oxygen is controlled, the components in the supplement material are oxidized and expanded to be ferrite, and the method is specifically as follows, wherein (alpha is 0.99-1.49):
(1.96Fe+0.2NiO+0.22CuO+0.6ZnO)+αO 2 →Ni 0.2 Cu 0.22 Zn 0.6 Fe 1.96 O x
preferably, the average particle size of the pre-sinter from step (3) is from 0.8 to 1.2. mu.m, and may be, for example, 0.8. mu.m, 0.9. mu.m, 1.0. mu.m, 1.1. mu.m or 1.2. mu.m, although not limited to the values recited, and other values not recited in the range of values are equally applicable.
Preferably, the average particle size of the elemental iron in the supplement is 7-9 μm, and may be, for example, 7 μm, 7.2 μm, 7.4 μm, 7.6 μm, 7.8 μm, 8 μm, 8.2 μm, 8.4 μm, 8.6 μm, 8.8 μm, or 9 μm, but is not limited to the recited values, and other values not recited in the range of values are equally applicable.
The invention preferably controls the average particle size of the iron simple substance in the supplementary material within a specific range, can control the size change rate, and improves the magnetism and the uniformity.
Preferably, the average particle size of the NiO in the supplement is in the range of 1 to 1.4. mu.m, and may be, for example, 1 μm, 1.1. mu.m, 1.2. mu.m, 1.3. mu.m, or 1.4. mu.m, although not limited to the values recited, and other values not recited within the range of values are equally applicable.
Preferably, the CuO in the supplement has an average particle size of 0.8 to 1.2. mu.m, and may be, for example, 0.8. mu.m, 0.9. mu.m, 1.0. mu.m, 1.1. mu.m, or 1.2. mu.m, but is not limited to the recited values, and other values not recited in the numerical ranges are equally applicable.
Preferably, the ZnO in the replenisher has an average particle size of 0.6 to 1 μm, and may be, for example, 0.6 μm, 0.7 μm, 0.8 μm, 0.9 μm or 1 μm, but is not limited to the recited values, and other values not recited within the range of values are equally applicable.
Preferably, the additive of step (3) comprises Bi 2 O 3 、V 2 O 5 、B 2 O 3 Or PbO, wherein a typical but non-limiting combination includes Bi 2 O 3 And V 2 O 5 Combination of (1), V 2 O 5 And B 2 O 3 Combination of (5) or (V) 2 O 5 、B 2 O 3 And PbO, preferably Bi 2 O 3 And/or PbO.
Preferably, the additive is present in an amount of 0.4 to 0.6% by mass of the sum of the pre-sinter and make-up, for example 0.4%, 0.42%, 0.44%, 0.46%, 0.48%, 0.5%, 0.52%, 0.54%, 0.56%, 0.58% or 0.6%, but not limited to the recited values, and other values not recited in the range of values are equally applicable.
The invention preferably controls the quality of the additive in a specific range, and can improve the uniformity and magnetism of the ferrite.
Preferably, the average particle size after the second ball milling in step (3) is 0.8 to 1.2 μm, and may be, for example, 0.8 μm, 0.9 μm, 1 μm, 1.1 μm or 1.2 μm, but is not limited to the values recited, and other values not recited in the numerical range are also applicable.
Preferably, the drying temperature in step (3) is 150-200 ℃, for example, 150 ℃, 160 ℃, 170 ℃, 180 ℃, 190 ℃ or 200 ℃, but not limited to the recited values, and other unrecited values within the range of values are equally applicable.
Preferably, the granulated binder comprises polyvinyl alcohol.
Preferably, the pressure of the press molding is 280-320MPa, such as 280MPa, 290MPa, 300MPa, 310MPa or 320MPa, but not limited to the values listed, and other values not listed in the range are also applicable.
Preferably, the sintering temperature in step (4) is 900-920 ℃, such as 900 ℃, 902 ℃, 904 ℃, 906 ℃, 908 ℃, 910 ℃, 912 ℃, 914 ℃, 916 ℃, 918 ℃ or 920 ℃, but not limited to the recited values, and other values not recited in the numerical range are also applicable.
Preferably, the sintering time is 5.5 to 6.5 hours, for example 5.5 hours, 5.6 hours, 5.7 hours, 5.8 hours, 5.9 hours, 6 hours, 6.1 hours, 6.2 hours, 6.3 hours, 6.4 hours or 6.5 hours, but not limited to the values listed, and other values not listed in the numerical range are equally applicable.
As a preferred technical solution of the first aspect of the present invention, the preparation method comprises the steps of:
(1) according to the mol ratio of NiO to CuO to ZnO to Fe 2 O 3 Mixing raw materials according to the ratio of 0.2:0.22:0.6:0.98, then carrying out first ball milling, and then drying at the temperature of 150 ℃. 200 ℃ to obtain mixed powder, wherein the average particle size of the mixed powder is 1.5-1.9 μm;
(2) pre-burning the mixed powder obtained in the step (1) at the temperature of 850-;
(3) mixing the pre-sintering material obtained in the step (2) with a supplement material, wherein the volume of the supplement material is 60-65% of the volume of the pre-sintering material, the molar ratio of the iron simple substance, NiO, CuO and ZnO in the supplement material is 1.96:0.2:0.22:0.6, and then adding an additive, wherein the additive comprises Bi 2 O 3 、V 2 O 5 、B 2 O 3 Or PbO or the combination of at least two of the above, the additive mass is 0.4-0.6% of the sum of the mass of the pre-sintering material and the supplementary material, then the second ball milling is carried out until the average particle diameter is 0.8-1.2 μm, the drying is carried out at the temperature of 150-;
(4) and (4) sintering the green body obtained in the step (3) at the temperature of 900-920 ℃ for 5.5-6.5h to obtain the shrinkage-free nickel-copper-zinc ferrite material.
In the invention, the non-shrinkage nickel-copper-zinc ferrite material is subsequently processed into a ring shape
The ring sample of (2).
In a second aspect, the present invention further provides a non-shrinkage nickel-copper-zinc ferrite material obtained by the preparation method of the non-shrinkage nickel-copper-zinc ferrite material according to the first aspect of the present invention, wherein the molecular structure expression of the non-shrinkage nickel-copper-zinc ferrite material is Ni 0.2 Cu 0.22 Zn 0.6 Fe 1.96 O x Wherein x is in the range of 3-4.
Where x is in the range of 3 to 4, for example 3.2, 3.4, 3.6, 3.8 or 4, but is not limited to the values recited, and other values not recited in the numerical ranges are equally applicable.
The shrinkage-free nickel-copper-zinc ferrite material provided by the invention utilizes the oxidation expansion reaction of a metal Fe simple substance, can control the change rate of the size to be almost 0 during low-temperature sintering, and has uniform and compact microstructure.
Compared with the prior art, the invention has the following beneficial effects:
(1) the preparation method of the shrinkage-free nickel-copper-zinc ferrite material provided by the invention can freely adjust and control the size change from shrinkage to expansion by changing the ratio of the pre-sintering material to the supplementary material, can realize the shrinkage-free ferrite sintering at low temperature, and promotes the homogenization and densification of the ferrite.
(2) The non-shrinkage nickel-copper-zinc ferrite material provided by the invention has no size shrinkage under low-temperature sintering, uniform and compact structure, excellent magnetic property and initial permeability mu i Can reach over 525 and the size change rate can reach over-0.65 percent.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a preparation method of a non-shrinkage nickel-copper-zinc ferrite material, which comprises the following steps:
(1) according to the mol ratio of NiO to CuO to ZnO to Fe 2 O 3 Mixing raw materials at a ratio of 0.2:0.22:0.6:0.98, then carrying out first ball milling, and then drying at 175 ℃ to obtain a mixed powder material, wherein the average particle size of the mixed powder material is 1.7 mu m;
(2) pre-burning the mixed powder obtained in the step (1) at 950 ℃ for 2h to obtain a pre-burnt material;
(3) mixing the pre-sintering material obtained in the step (2) with a supplement material, wherein the volume of the supplement material is 62% of the volume of the pre-sintering material, the molar ratio of the iron simple substance, NiO, CuO and ZnO in the supplement material is 1.96:0.2:0.22:0.6, and then adding Bi 2 O 3 The additive accounts for 0.5 mass percent of the sum of the mass of the pre-sintering material and the mass of the supplementary material, the average particle size of the pre-sintering material is 1 mu m, the average particle size of an iron simple substance in the supplementary material is 8 mu m, the average particle size of NiO is 1.2 mu m, the average particle size of CuO is 1 mu m, and the average particle size of ZnO is 0.8 mu m;
carrying out second ball milling until the average particle size is 1 mu m, drying at 175 ℃, adding polyvinyl alcohol for granulation, and carrying out compression molding under 300MPa to obtain a green body;
(4) and (4) sintering the green body obtained in the step (3) at 910 ℃ for 6h to obtain the shrinkage-free nickel-copper-zinc ferrite material.
The embodiment also provides a non-shrinkage nickel-copper-zinc ferrite material obtained by the preparation method, wherein the molecular structure expression of the non-shrinkage nickel-copper-zinc ferrite material is Ni 0.2 Cu 0.22 Zn 0.6 Fe 1.96 O 4 。
Example 2
The embodiment provides a preparation method of a non-shrinkage nickel-copper-zinc ferrite material, which comprises the following steps:
(1) according to the mol ratio of NiO to CuO to ZnO to Fe 2 O 3 Mixing raw materials at a ratio of 0.2:0.22:0.6:0.98, then carrying out first ball milling, and then drying at 150 ℃ to obtain a mixed powder material, wherein the average particle size of the mixed powder material is 1.9 mu m;
(2) pre-burning the mixed powder obtained in the step (1) at 850 ℃ for 2.5h to obtain a pre-burnt material;
(3) mixing the pre-sintering material obtained in the step (2) with a supplement material, wherein the volume of the supplement material is 60% of that of the pre-sintering material, the molar ratio of the iron simple substance, NiO, CuO and ZnO in the supplement material is 1.96:0.2:0.22:0.6, and then adding Bi 2 O 3 And V 2 O 5 The additive accounts for 0.6 mass percent of the sum of the mass of the pre-sintering material and the mass of the supplement material, the average particle size of the pre-sintering material is 0.8 mu m, the average particle size of an iron simple substance in the supplement material is 9 mu m, the average particle size of NiO is 1 mu m, the average particle size of CuO is 1.2 mu m, and the average particle size of ZnO is 0.6 mu m;
carrying out second ball milling until the average particle size is 0.8 mu m, drying at 150 ℃, adding polyvinyl alcohol for granulation, and pressing under 320MPa to form a green body;
(4) and (4) sintering the green body obtained in the step (3) at 900 ℃ for 6.5h to obtain the shrinkage-free nickel-copper-zinc ferrite material.
The embodiment also provides a non-shrinkage nickel-copper-zinc ferrite material obtained by the preparation method, wherein the molecular structure expression of the non-shrinkage nickel-copper-zinc ferrite material is Ni 0.2 Cu 0.22 Zn 0.6 Fe 1.96 O 4 。
Example 3
The embodiment provides a preparation method of a non-shrinkage nickel-copper-zinc ferrite material, which comprises the following steps:
(1) according to the mol ratio of NiO to CuO to ZnO to Fe 2 O 3 Mixing raw materials at 0.2:0.22:0.6:0.98, then carrying out first ball milling, and then drying at 200 ℃ to obtain a mixed powder material, wherein the average particle size of the mixed powder material is 1.5 mu m;
(2) pre-burning the mixed powder obtained in the step (1) at 1050 ℃ for 1.5h to obtain a pre-burnt material;
(3) mixing the pre-sintered material obtained in the step (2) with a supplement material, wherein the volume of the supplement material is 65% of that of the pre-sintered material, the molar ratio of the simple substance of iron, NiO, CuO and ZnO in the supplement material is 1.96:0.2:0.22:0.6, and then adding B 2 O 3 And PbO additive, the quality of the said additive is 0.4% of the sum of quality of pre-burning material and supplementary material, the average grain size of the said pre-burning material is 1.2 μm, the average grain size of iron simple substance in the said supplementary material is 7 μm, the average grain size of NiO is 1.4 μm, the average grain size of CuO is 0.8 μm, the average grain size of ZnO is 1 μm;
carrying out second ball milling until the average particle size is 1.2 mu m, drying at 200 ℃, adding polyvinyl alcohol for granulation, and pressing under 280MPa to form a green body;
(4) and (4) sintering the green body obtained in the step (3) at 920 ℃ for 5.5h to obtain the shrinkage-free nickel-copper-zinc ferrite material.
The embodiment also provides a non-shrinkage nickel-copper-zinc ferrite material obtained by the preparation method, wherein the molecular structure expression of the non-shrinkage nickel-copper-zinc ferrite material is Ni 0.2 Cu 0.22 Zn 0.6 Fe 1.96 O 4 。
Example 4
This example provides a method of making a non-shrinking nickel-copper-zinc ferrite material which differs from that of example 1 only in that the volume of the supplementary material is 50% of the volume of the pre-fired material.
Example 5
This example provides a method of making a non-shrinking nickel copper zinc ferrite material which differs from that of example 1 only in that the volume of the supplementary material is 70% of the volume of the pre-fired material.
Example 6
This example provides a method of making a non-shrinking nickel copper zinc ferrite material which differs from that of example 1 only in that the mean particle size of the elemental iron in the supplement is 6 μm.
Example 7
This example provides a method of making a non-shrinking nickel copper zinc ferrite material which differs from that of example 1 only in that the mean particle size of the elemental iron in the supplement is 10 μm.
Example 8
This example provides a method of making a non-shrinking nickel copper zinc ferrite material which differs from that of example 1 only in that the mass of the additive is 0.2% of the sum of the mass of the pre-sinter and the mass of the supplementary material.
Example 9
This example provides a method of making a non-shrinking nickel copper zinc ferrite material which differs from that of example 1 only in that the mass of the additive is 0.8% of the sum of the mass of the pre-sinter and the mass of the supplementary material.
Comparative example 1
This comparative example provides a method for preparing a non-shrinking NiCuZnFe material, which differs from example 1 only in that no Bi is added 2 O 3 。
Comparative example 2
The comparative example provides a preparation method of a non-shrinkage nickel-copper-zinc ferrite material, and compared with the preparation method of example 1, the preparation method is only different in that no supplementary material is added, the additive is directly added into the pre-sintered material, then secondary ball milling, drying, granulation and compression molding are carried out to obtain a green body, and sintering is carried out to obtain the non-shrinkage nickel-copper-zinc ferrite material.
Comparative example 3
This comparative example provides a method for preparing a non-shrinking nickel-copper-zinc ferrite material, which is different from example 1 only in that an additive is added to a pre-sintered material and then mixed with a supplementary material.
Initial permeability μ of shrinkage-free NiCuZnFe ferrite materials prepared in examples 1-9 and comparative examples 1-3 using Agilent E4980A LCR tester i The results of the measurements are shown in Table 1.
The change rate of the non-shrinkage nickel-copper-zinc ferrite materials prepared in examples 1 to 9 and comparative examples 1 to 3 was measured by the following method: the green body was heated at 5 ℃/min and the dimensional change rate (outer diameter of sintered body-outer diameter of green body)/outer diameter of green body, the sintered body, that is, the resultant shrinkage-free nickel-copper-zinc ferrite material was measured by using a thermomechanical analyzer (TMA), and the results are shown in table 1.
TABLE 1
| μ i Initial permeability | Rate of change in dimension/%) | |
| Example 1 | 550 | -0.4％ |
| Example 2 | 548 | -0.42％ |
| Example 3 | 543 | -0.48％ |
| Example 4 | 539 | -0.53％ |
| Example 5 | 536 | -0.56％ |
| Example 6 | 534 | -0.59％ |
| Example 7 | 530 | -0.60％ |
| Example 8 | 528 | -0.62％ |
| Example 9 | 525 | -0.65％ |
| Comparative example 1 | 413 | -0.7％ |
| Comparative example 2 | 406 | -0.73％ |
| Comparative example 3 | 397 | -0.75％ |
From table 1, the following points can be seen:
(1) as can be seen from the data of examples 1-9, the non-shrinkage nickel-copper-zinc ferrite material provided by the invention has excellent magnetic performance, almost has no shrinkage under low-temperature sintering, has initial permeability of more than 525, and has dimensional change rate of more than-0.65%.
(2) Comparing the data of example 1 and examples 4-5 together, it can be seen that the volume of the supplemental material in example 1 is 62% of the volume of the calcined material, compared to 50% and 70% in examples 4-5, respectively, for the initial permeability μ in example 1 i The initial permeability was lower than that of example 1 at 550, the dimensional change rate was-0.4%, and the dimensional change rates of examples 4-5 were lower than that of example 1, and it was found that the body for controlling the replenisher according to the present invention was preferable because the initial permeability was lower than that of example 1 and the dimensional change rates of examples 4-5 were lower than that of example 1The volume percentage of the pre-sintering material is in a specific range, so that the magnetic property of the ferrite can be improved, and the shrinkage is reduced.
(3) A comparison of the data from example 1 and examples 6 to 7 shows that the mean particle size of the elemental iron in the supplement of example 1 is 8 μm and the initial permeability μm in example 1 is compared to 6 μm and 10 μm in examples 6 to 7, respectively i The rate of change in the dimension is 550, the rate of change in the dimension is-0.4%, while the initial permeability in examples 6-7 is lower than that in example 1, and the rate of change in the dimension in examples 6-7 is lower than that in example 1, therefore, the invention preferably controls the average particle size of the iron in the supplementary material within a specific range, and can improve the magnetic performance of the ferrite and reduce the shrinkage.
(4) A comparison of the data from example 1 and examples 8-9 shows that the mass of the additive in example 1 is 0.5% of the sum of the mass of the pre-sinter and the mass of the supplement, compared to 0.2% and 0.8% in examples 8-9, respectively, for the initial permeability μ in example 1 i The initial permeability of 550 is-0.4%, while the initial permeability of examples 8-9 is lower than that of example 1, and the initial permeability of examples 8-9 is lower than that of example 1, so that the invention preferably controls the mass percentage of the additive in the sum of the mass of the pre-sintering material and the mass of the supplementary material in a specific range, thereby improving the magnetic performance of the ferrite and reducing the shrinkage.
(5) As can be seen by combining the data of comparative example 1 and comparative examples 1-2, comparative example 1 differs from example 1 only in that no Bi is added 2 O 3 Comparative example 2 differs from example 1 only in that no supplementary material is added, and the initial permeability μ in example 1 i The initial permeability of the ferrite is 550, the dimensional change rate is-0.4%, while the initial permeability of the ferrite in comparative examples 1-2 is lower than that of example 1, and the dimensional change rate of the ferrite in comparative examples 1-2 is lower than that of example 1, so that the preparation method provided by the invention can improve the magnetic property of the ferrite and reduce the shrinkage.
(6) Comparing the data of example 1 and comparative example 3 together, it can be seen that comparative example 3 is different from example 1 only in that the additive is added to the pre-sintered material and then mixed with the supplement material, and the initial permeability and the dimensional change rate of comparative example 3 are both smaller than those of example 1, so that the shrinkage can be reduced while the magnetic properties of the ferrite are improved by adding the additive to the pre-sintered material and then mixing with the supplement material.
In conclusion, the non-shrinkage nickel-copper-zinc ferrite material provided by the invention has the advantages of no size shrinkage, uniform and compact structure and excellent magnetic property under low-temperature sintering, and the preparation method provided by the invention is simple to operate and can be applied industrially.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
1. A preparation method of a non-shrinkage nickel-copper-zinc ferrite material is characterized by comprising the following steps:
(1) according to the mol ratio of NiO to CuO to ZnO to Fe 2 O 3 Mixing the raw materials according to the ratio of 0.2:0.22:0.6:0.98, and then sequentially carrying out first ball milling and drying to obtain mixed powder;
(2) pre-burning the mixed powder obtained in the step (1) to obtain a pre-burnt material;
(3) mixing the pre-sintered material and the supplementary material obtained in the step (2), adding an additive, and then sequentially carrying out second ball milling, drying, granulation and compression molding to obtain a green body;
the supplementary material comprises a simple substance of iron, NiO, CuO and ZnO;
(4) and (4) sintering the green body obtained in the step (3) to obtain the shrinkage-free nickel-copper-zinc ferrite material.
2. The production method according to claim 1, wherein the average particle diameter of the powder mixture of step (1) is 1.5 to 1.9 μm;
preferably, the temperature for the drying in step (1) is 150-200 ℃.
3. The method as claimed in claim 1 or 2, wherein the pre-sintering temperature in step (2) is 850-;
preferably, the pre-burning time is 1.5-2.5 h.
4. A method of manufacturing as claimed in any one of claims 1 to 3, wherein the volume of the supplementary material in step (3) is 60 to 65% of the volume of the pre-fired material;
preferably, the molar ratio of the simple substance of iron, NiO, CuO and ZnO in the supplement is 1.96:0.2:0.22: 0.6.
5. The production method according to any one of claims 1 to 4, wherein the average particle size of the pre-sintered compact in the step (3) is 0.8 to 1.2 μm;
preferably, the average particle size of the elementary substance iron in the supplementary material is 7-9 μm;
preferably, the average grain diameter of NiO in the supplement is 1-1.4 μm;
preferably, the CuO in the supplement has an average particle size of 0.8-1.2 μm;
preferably, the ZnO in the supplement has an average particle size of 0.6 to 1 μm.
6. The method according to any one of claims 1 to 5, wherein the additive of step (3) comprises Bi 2 O 3 、V 2 O 5 、B 2 O 3 Or PbO or a combination of at least two thereof, preferably Bi 2 O 3 And/or PbO;
preferably, the mass of the additive is 0.4-0.6% of the sum of the mass of the pre-sintering material and the mass of the supplementary material.
7. The production method according to any one of claims 1 to 6, wherein the average particle diameter after the second ball milling in step (3) is 0.8 to 1.2 μm;
preferably, the temperature for drying in step (3) is 150-200 ℃;
preferably, the granulated binder comprises polyvinyl alcohol;
preferably, the pressure of the compression molding is 280-320 MPa.
8. The method as claimed in any one of claims 1 to 7, wherein the sintering temperature in step (4) is 900-920 ℃;
preferably, the sintering time is 5.5-6.5 h.
9. The method of any one of claims 1 to 9, comprising the steps of:
(1) according to the mol ratio of NiO to CuO to ZnO to Fe 2 O 3 Mixing raw materials according to the ratio of 0.2:0.22:0.6:0.98, then carrying out first ball milling, and then drying at the temperature of 150 ℃. 200 ℃ to obtain mixed powder, wherein the average particle size of the mixed powder is 1.5-1.9 μm;
(2) pre-burning the mixed powder obtained in the step (1) at the temperature of 850-;
(3) mixing the pre-sintering material obtained in the step (2) with a supplement material, wherein the volume of the supplement material is 60-65% of the volume of the pre-sintering material, the molar ratio of the iron simple substance, NiO, CuO and ZnO in the supplement material is 1.96:0.2:0.22:0.6, and then adding an additive, wherein the additive comprises Bi 2 O 3 、V 2 O 5 、B 2 O 3 Or PbO or the combination of at least two of the above, the additive mass is 0.4-0.6% of the sum of the mass of the pre-sintering material and the supplementary material, then the second ball milling is carried out until the average particle diameter is 0.8-1.2 μm, the drying is carried out at the temperature of 150-;
(4) and (4) sintering the green body obtained in the step (3) at the temperature of 900-920 ℃ for 5.5-6.5h to obtain the shrinkage-free nickel-copper-zinc ferrite material.
10. A non-shrinking nickel-copper-zinc ferrite material obtained by the method for preparing a non-shrinking nickel-copper-zinc ferrite material according to any one of claims 1 to 9, wherein the non-shrinking nickel-copper-zinc ferrite material is prepared by the method for preparing a non-shrinking nickel-copper-zinc ferrite material according to any one of claims 1 to 9The molecular structure expression of the non-shrinkage nickel-copper-zinc ferrite material is Ni 0.2 Cu 0.22 Zn 0.6 Fe 1.96 O x Wherein x is in the range of 3-4.
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