CN115677336A - High-density nickel-copper-zinc ferrite material and preparation method thereof - Google Patents
High-density nickel-copper-zinc ferrite material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a high-density nickel-copper-zinc ferrite material and a preparation method thereof, and relates to the technical field of ferrite preparation. According to the invention, the raw materials are matched into large and small particles, so that the materials reach the closest packing state, and a blank with higher density is obtained; meanwhile, the proportion of the copper oxide content in the material is increased, the sintering temperature of the material is reduced, and the material performance is improved. The invention refines the crystal grains by low-temperature sintering, and improves the saturation magnetic flux density and the inductance of the material by high density. The nickel-copper-zinc ferrite material prepared by the invention has higher density, and can solve the problem that the existing nickel-copper-zinc ferrite can not meet the application requirements of 5G high frequency and product miniaturization.
Description
Technical Field
The invention relates to the technical field of ferrite preparation, in particular to a high-density nickel-copper-zinc ferrite material and a preparation method thereof.
Background
With the development of the miniaturization trend of 5G terminals and electronic products, the power inductor is required to have higher saturation magnetic flux density (Bs) at higher use frequency, and the existing nickel-copper-zinc ferrite cannot meet the requirement of high Bs. Generally speaking, the higher the Bs of the material, the better the dc deflection performance of the material, and meanwhile, the Bs of the material is closely related to the density of the material, and the higher the density of the material, the higher the inductance and Bs of the material. Therefore, how to develop a high-density nickel-copper-zinc ferrite material to meet the demand of miniaturization of products on the material is a technical problem to be overcome urgently.
Disclosure of Invention
The invention aims to provide a high-density nickel-copper-zinc ferrite material and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a high-density nickel-copper-zinc ferrite material, which comprises the following steps:
large particles of Fe 2 O 3 Small particle Fe 2 O 3 Mixing nickel oxide, copper oxide and zinc oxide to obtain a mixed material; the large particles of Fe 2 O 3 The particle diameter of (A) is 0.6-1.5 μm; the small particles of Fe 2 O 3 The grain diameter of the particles is 0.2-0.5 mu m; large granular Fe in the mixed material 2 O 3 With a content of 44-55 wt.%, small Fe particles 2 O 3 12-20 wt%, nickel oxide 2-24 wt%, copper oxide 2-10 wt%, and zinc oxide in balance;
pelletizing the mixed material to obtain a ball body;
pre-burning the spheres to obtain pre-burned bodies; the temperature of the pre-sintering is 600-800 ℃;
crushing the pre-sintered body to obtain a granular material; the grading of the particle materials is consistent with the grading of the mixed materials;
mixing the granular material with a binder, and granulating to obtain a binder-coated granular material;
pressing the particle material coated by the binder to obtain a blank;
and sintering the blank to obtain the high-density nickel-copper-zinc ferrite material.
Preferably, the sphere diameter of the sphere is 2-10 mm.
Preferably, before the granule and the binder are mixed, the method further comprises the following steps: and mixing the particle material and the sintering aid.
Preferably, the sintering aid is Bi 2 O 3 And SiO 2 。
Preferably, the binder comprises polyvinyl alcohol, peach gum or terephthalic acid.
Preferably, the mass of the binder is 0.6-2% of the mass of the granules.
Preferably, the granulation is spray granulation.
Preferably, the density of the blank is 3.2-4.2 g/cm 3 。
Preferably, the sintering temperature is 1000-1080 ℃.
The invention provides the high-density nickel-copper-zinc ferrite material obtained by the preparation method of the technical scheme, and the density is 5.2-5.4 g/cm 3 。
The invention provides a preparation method of a high-density nickel-copper-zinc ferrite material, which enables the material to reach a most dense packing state by matching large and small particles of raw materials to obtain a blank with higher density; meanwhile, the proportion of the copper oxide content in the material is increased, the sintering temperature of the material is reduced, and the material performance is improved. The invention refines crystal grains through low-temperature sintering, and improves the saturation magnetic flux density and inductance of the material through high density.
Drawings
FIG. 1 is a process flow chart of the present invention for preparing high density Ni-Cu-Zn ferrite material.
Detailed Description
The invention provides a preparation method of a high-density nickel-copper-zinc ferrite material, which comprises the following steps of:
large particles of Fe 2 O 3 Small particle Fe 2 O 3 Mixing nickel oxide, copper oxide and zinc oxide to obtain a mixed material; the large particles of Fe 2 O 3 The grain diameter of the particles is 0.6-1.5 mu m; the small particles of Fe 2 O 3 The grain diameter of the particles is 0.2-0.5 mu m; large particle Fe in the mixed material 2 O 3 44-55 wt% of small particle Fe 2 O 3 12-20 wt%, nickel oxide 2-24 wt%, copper oxide 2-10 wt%, and zinc oxide in balance;
pelletizing the mixed material to obtain a ball body;
pre-burning the spheres to obtain pre-burned bodies; the temperature of the pre-sintering is 600-800 ℃;
crushing the pre-sintered body to obtain a granular material; the grading of the particle materials is consistent with the grading of the mixed materials;
mixing the granular material with a binder, and granulating to obtain a binder-coated granular material;
pressing the particle material coated by the binder to obtain a blank;
and sintering the blank to obtain the high-density nickel-copper-zinc ferrite material.
The invention mixes large granular Fe 2 O 3 Small particle of Fe 2 O 3 Mixing the nickel oxide, the copper oxide and the zinc oxide to obtain a mixed material. In the present invention, the large particles of Fe 2 O 3 The particle diameter of (A) is 0.6 to 1.5. Mu.m, more preferably 1.0 to 1.2. Mu.m; the smallGranular Fe 2 O 3 The particle diameter of (2) is 0.2 to 0.5. Mu.m, more preferably 0.3 to 0.4. Mu.m. In the present invention, the particle size of the nickel oxide, copper oxide and zinc oxide is preferably 2 μm.
In the present invention, large particles of Fe are present in the mix 2 O 3 The content of (B) is 44 to 55wt%, preferably 50 to 54wt%; small particle of Fe 2 O 3 The content of (B) is 12 to 20wt%, preferably 15 to 18wt%; the content of nickel oxide is 2 to 24wt%, preferably 8 to 12wt%; the content of copper oxide is 2 to 10wt%, preferably 5 to 8wt%; the balance being zinc oxide.
In the present invention, the mixing is preferably carried out by using a cone mixer and a vibration mill in this order.
After the mixed material is obtained, the mixed material is pelletized to obtain a sphere. In the present invention, the sphere diameter of the sphere is preferably 2 to 10mm, more preferably 5 to 8mm. In the present invention, the pelletizing is preferably carried out in a pelletizer.
After obtaining the sphere, the invention presinteres the sphere to obtain a presintered body. In the present invention, the temperature of the pre-firing is preferably 600 to 800 ℃, and more preferably 700 to 750 ℃. In the present invention, the atmosphere of the above-mentioned calcination is preferably an air atmosphere. In the present invention, the pre-firing is preferably performed in a rotary kiln. The invention forms part of ferrite components through pre-burning, thereby preventing the material from having too high activity and the magnetic core from deforming and cracking after molding caused by subsequent one-time sintering.
After the pre-sintered body is obtained, the pre-sintered body is crushed to obtain the granular material. In the invention, the gradation of the granular material is consistent with the gradation of the mixed material. In the present invention, the crushing preferably includes coarse crushing and fine crushing which are sequentially performed. In the present invention, the coarse crushing is preferably carried out in a vibrating mill; the particle size of the particles obtained by the coarse crushing is preferably 2 to 5 μm. In the present invention, the fine crushing is preferably carried out in a sand mill; the time for the fine crushing is preferably 10 to 15min.
The invention breaks the false agglomeration among the particles by crushing, reduces the granularity collocation of the mixed material, and returns to the initial large and small particle collocation state, so that the material reaches the closest packing state, and a blank with higher density is obtained.
After the granular material is obtained, the granular material and the binder are mixed and granulated to obtain the granular material coated by the binder. In the present invention, before mixing the granule and the binder, it is preferable that the granule further comprises: and mixing the granules and the sintering aid. In the present invention, the sintering aid is preferably Bi 2 O 3 And SiO 2 . In the present invention, the Bi 2 O 3 The mass of (b) is preferably 0.02 to 0.5%, more preferably 0.3 to 0.4% of the mass of the granules; the SiO 2 The mass of (b) is preferably 0.05 to 0.2%, more preferably 0.1 to 0.15% of the mass of the granules. In the present invention, bi 2 O 3 The low-melting-point oxide can reduce the sintering temperature, refine crystal grains and improve the welding resistance of the magnetic core; siO 2 2 The magnetic permeability of the material can be improved.
In the present invention, the binder preferably includes polyvinyl alcohol (PVA), peach gum, or terephthalic acid (PTA). In the present invention, the mass of the binder is preferably 0.6 to 2%, more preferably 1.0 to 1.8% of the mass of the pellet. In the present invention, the binder coats the surface of the granules during granulation, and serves to bind the granules during molding.
In the present invention, the granulation is preferably spray granulation. In the present invention, the granulation is preferably performed in a centrifugal spray granulation tower or a pressure type spray granulation tower. The invention forms the state of coating thick and thin matched particles by the binder through granulation.
After the binder-coated granular material is obtained, the binder-coated granular material is pressed to obtain a blank. In the present invention, the temperature of the pressing is preferably room temperature; the pressing pressure is preferably 2 to 8 tons/square centimeter; the pressing time is preferably 0.5 to 2 seconds.
In the present invention, the density of the blank is preferably 3.2 to 4.2g/cm 3 More preferably 3.8 to 4.0g/cm 3 。
After obtaining the blank, the invention sinters the blank to obtain the high-density nickel-copper-zinc ferrite material. In the present invention, the sintering temperature is preferably 1000 to 1080 ℃, and more preferably 1020 to 1050 ℃. In the present invention, the atmosphere for the sintering is preferably air.
In the invention, because of the higher density blank and the higher copper content obtained by particle collocation, the density can reach 5.2-5.4 g/cm when sintering at 1000 DEG C 3 。
The invention provides a high-density nickel-copper-zinc ferrite material obtained by the preparation method in the technical scheme. In the invention, the density of the high-density nickel-copper-zinc ferrite material is 5.2-5.4 g/cm 3 Preferably 5.25 to 5.32g/cm 3 . In the invention, the magnetic permeability of the high-density nickel-copper-zinc ferrite material is preferably 350-460, and the saturation magnetic flux density Bs is preferably 410-440 mT.
In the present invention, the high-density nickel-copper-zinc ferrite material is preferably used as a magnetic core.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
The high-density nickel-copper-zinc ferrite material is prepared by adopting the process of FIG. 1:
large particles of Fe 2 O 3 Small particle Fe 2 O 3 The nickel oxide, the copper oxide and the zinc oxide are sequentially subjected to preliminary mixing by using a cone mixer and a vibration mill to obtain a mixed material; the large particles of Fe 2 O 3 The particle diameter of (A) is 1.5 μm; the small particles of Fe 2 O 3 The particle diameter of (2) is 0.5 μm; large granular Fe in the mixed material 2 O 3 Has a content of 54wt% and small particles of Fe 2 O 3 12wt%, nickel oxide 12wt%, copper oxide 5wt%, and zinc oxide the balance.
Pelletizing by using a pelletizer, wherein the diameter of the pellet is 10mm.
And (3) pre-burning at 800 ℃ by using a rotary kiln to form partial ferrite to obtain a pre-burnt body.
Coarsely crushing the pre-sintered body by using a vibration mill, finely crushing for 10min by using a sand mill, reducing the granularity of the mixed material, and simultaneously adding 0.4wt% of Bi 2 O 3 And 0.05wt% SiO 2 。
Adding 0.6wt% of PVA slurry, granulating, and granulating by using a centrifugal spray granulation tower to obtain the PVA-coated granular material.
Pressing the PVA-coated granules to obtain granules with the density of 4.0g/cm 3 The blank of (2); the pressing temperature is room temperature; the pressing pressure is 3 tons/square centimeter; the pressing time was 1.5 seconds.
Sintering at 1050 ℃ by adopting an air muffle furnace to obtain the product with the density of 5.32g/cm 3 The high-density nickel-copper-zinc ferrite material.
The permeability of the high-density nickel-copper-zinc ferrite material prepared in the embodiment is 450, and the saturation magnetic flux density Bs is 440mT.
Example 2
The high-density nickel-copper-zinc ferrite material is prepared by adopting the process of FIG. 1:
large particles of Fe 2 O 3 Small particle of Fe 2 O 3 Preliminarily mixing nickel oxide, copper oxide and zinc oxide by using a cone mixer and a vibrating mill to obtain a mixed material; the large particles of Fe 2 O 3 The particle diameter of (2) is 0.6 μm; the small particles of Fe 2 O 3 The particle diameter of (2) is 0.2 μm; large granular Fe in the mixed material 2 O 3 With a content of 53 wt.%, small particle Fe 2 O 3 12wt%, nickel oxide 8wt%, copper oxide 8wt%, and zinc oxide the balance.
Pelletizing with a pelletizer, wherein the diameter of the pellet is 2mm.
And (3) pre-burning at a low temperature of 750 ℃ by using a rotary kiln to form part of ferrite to obtain a pre-burning body.
Coarsely crushing the pre-sintered body by using a vibration mill, and finely crushing by using a sand mill for 10min, reducing the particle size of the mixed material, and simultaneously adding 0.5wt% of Bi 2 O 3 And 0.15wt% SiO 2 。
Adding 2wt% of PVA slurry, granulating, and granulating by using a centrifugal spray granulation tower to obtain the PVA-coated granular material.
Pressing the PVA-coated granules to obtain granules with the density of 3.8g/cm 3 The blank of (2); the pressing temperature is room temperature; the pressing pressure is 3 tons/square centimeter; the pressing time was 1.5 seconds.
Sintering at 1020 ℃ by using an air muffle furnace to obtain the product with the density of 5.25g/cm 3 The high-density nickel-copper-zinc ferrite material.
The permeability of the high-density nickel-copper-zinc ferrite material prepared by the embodiment is 350, and the saturation magnetic flux density Bs is 430mT.
Example 3
The high-density nickel-copper-zinc ferrite material is prepared by adopting the process of FIG. 1:
large particles of Fe 2 O 3 Small particle Fe 2 O 3 Preliminarily mixing the nickel oxide, the copper oxide and the zinc oxide by using a cone mixer and a vibration mill to obtain a mixed material; the large particles of Fe 2 O 3 The particle diameter of (2) is 1 μm; the small particles of Fe 2 O 3 The particle diameter of (2) is 0.4 μm; large granular Fe in the mixed material 2 O 3 In an amount of 50wt%, small particles of Fe 2 O 3 15wt%, nickel oxide 24wt%, copper oxide 7wt%, and zinc oxide the balance.
Pelletizing by using a pelletizer, wherein the diameter of the pellet is 5mm.
And pre-sintering at 600 ℃ by using a rotary kiln to form part of ferrite to obtain a pre-sintered body.
Coarsely crushing the pre-sintered body by using a vibration mill, finely crushing for 12min by using a sand mill, reducing the granularity matching of the mixed materials, and simultaneously adding 0.3wt% of Bi 2 O 3 And 0.1% by weight of SiO 2 。
Adding 1.8wt% of PVA slurry, granulating, and granulating by using a centrifugal spray granulation tower to obtain PVA-coated granules.
Pressing the PVA-coated granules to obtain granules with the density of 3.2g/cm 3 The blank of (2); the pressing temperature is room temperature; the pressing pressure is 3 tons/square centimeter; the pressing time was 1.5 seconds.
Sintering at 1080 ℃ by adopting an air muffle furnace to obtain the product with the density of 5.2g/cm 3 The high-density nickel-copper-zinc ferrite material.
The permeability of the high-density nickel-copper-zinc ferrite material prepared by the embodiment is 460, and the saturation magnetic flux density Bs is 410mT.
Comparative example 1
Large particles of Fe 2 O 3 Preliminarily mixing the nickel oxide, the copper oxide and the zinc oxide by using a cone mixer and a vibration mill to obtain a mixed material; the large particles of Fe 2 O 3 The particle diameter of (a) is 1.5 μm; large granular Fe in the mixed material 2 O 3 66wt%, nickel oxide 12wt%, copper oxide 5wt%, and zinc oxide the balance.
Pelletizing by using a pelletizer, wherein the diameter of the pellet is 10mm.
And (3) presintering at a high temperature of 950 ℃ by using a rotary kiln to form a part of ferrite to obtain a presintering body.
Coarsely crushing the pre-sintered body by using a vibration mill, finely crushing for 60min by using a sand mill to ensure that the sand grinding granularity reaches 1.2 mu m, and simultaneously adding 0.4wt% of Bi 2 O 3 And 0.05wt% SiO 2 。
Adding 0.6wt% of PVA slurry, granulating, and granulating by using a centrifugal spray granulation tower to obtain the PVA-coated granular material.
Pressing the PVA-coated granules to obtain granules with the density of 3.0g/cm 3 The blank of (2); the pressing temperature is room temperature; the pressing pressure is 3 tons/square centimeter; the pressing time was 1.5 seconds.
Sintering at 1050 ℃ by using an air muffle furnace to obtain the product with the density of 5.1g/cm 3 The high-density nickel-copper-zinc ferrite material.
The permeability of the high-density nickel-copper-zinc ferrite material prepared in the embodiment is 430, and the saturation magnetic flux density Bs is 425mT.
Comparative example 2
Mixing small particles of Fe 2 O 3 Preliminarily mixing nickel oxide, copper oxide and zinc oxide by using a cone mixer and a vibrating mill to obtain a mixed material; the small particles of Fe 2 O 3 The particle diameter of (2) is 0.5 μm; small particles of Fe in said mixture 2 O 3 66wt%, nickel oxide 12wt%, copper oxide 5wt%, and zinc oxide the balance.
Pelletizing by using a pelletizer, wherein the diameter of the pellet is 10mm.
And (3) presintering at a high temperature of 950 ℃ by using a rotary kiln to form a part of ferrite to obtain a presintering body.
Coarsely crushing the pre-sintered body by using a vibration mill, finely crushing for 60min by using a sand mill to ensure that the sand grinding granularity reaches 0.5 mu m, and simultaneously adding 0.4wt% of Bi 2 O 3 And 0.05wt% SiO 2 。
Adding 0.6wt% of PVA slurry, granulating, and granulating by using a centrifugal spray granulation tower to obtain the PVA-coated granular material.
Pressing the PVA-coated granules to obtain granules with the density of 2.8g/cm 3 The blank of (2); the pressing temperature is room temperature; the pressing pressure is 3 tons/square centimeter; the pressing time was 1.5 seconds.
Sintering at 1050 ℃ by adopting an air muffle furnace to obtain the product with the density of 5.0g/cm 3 The high-density nickel-copper-zinc ferrite material.
The permeability of the high-density nickel-copper-zinc ferrite material prepared in the embodiment is 440, and the saturation magnetic flux density Bs is 410mT.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and amendments can be made without departing from the principle of the present invention, and these modifications and amendments should also be considered as the protection scope of the present invention.
Claims (10)
1. A preparation method of a high-density nickel-copper-zinc ferrite material comprises the following steps:
large particles of Fe 2 O 3 Small particle Fe 2 O 3 Mixing nickel oxide, copper oxide and zinc oxide to obtain a mixed material; the large particles of Fe 2 O 3 The grain diameter of the particles is 0.6-1.5 mu m; the small particles of Fe 2 O 3 The grain diameter of the particles is 0.2-0.5 mu m; large granular Fe in the mixed material 2 O 3 44-55 wt% of small particle Fe 2 O 3 The content of (A) is 12-20 wt%, the content of nickel oxide is 2-24 wt%, the content of copper oxide is 2-10 wt%, and the balance is zinc oxide;
pelletizing the mixed material to obtain a ball body;
pre-burning the spheres to obtain pre-burned bodies; the temperature of the pre-sintering is 600-800 ℃;
crushing the pre-sintered body to obtain a granular material; the grading of the particle materials is consistent with the grading of the mixed materials;
mixing the granular material with a binder, and granulating to obtain a binder-coated granular material;
pressing the particle material coated by the binder to obtain a blank;
and sintering the blank to obtain the high-density nickel-copper-zinc ferrite material.
2. The method according to claim 1, wherein the sphere has a spherical diameter of 2 to 10mm.
3. The method of claim 1, wherein prior to mixing the particulate material and the binder, further comprising: and mixing the particle material and the sintering aid.
4. The method according to claim 3, wherein the sintering aid is Bi 2 O 3 And SiO 2 。
5. The method of claim 1, wherein the binder comprises polyvinyl alcohol, peach gum, or terephthalic acid.
6. A method as claimed in claim 1 or 5, wherein the binder is present in an amount of 0.6 to 2% by mass of the granules.
7. The method according to claim 1 or 5, wherein the granulation is spray granulation.
8. The method of claim 1, wherein the matte has a density of 3.2 to 4.2g/cm 3 。
9. The method according to claim 1, wherein the sintering temperature is 1000 to 1080 ℃.
10. The high-density nickel-copper-zinc ferrite material obtained by the preparation method of any one of claims 1 to 9, which has a density of 5.2 to 5.4g/cm 3 。
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| JPH11340024A (en) * | 1998-05-26 | 1999-12-10 | Tokin Corp | Low-loss oxide magnetic material |
| JP2008127230A (en) * | 2006-11-17 | 2008-06-05 | Jfe Ferrite Corp | MnZnNi FERRITE |
| CN101388268A (en) * | 2008-07-11 | 2009-03-18 | 临沂中瑞电子有限公司 | High magnetic conductive low temperature sintered NiCuZn ferrite material |
| CN101412622A (en) * | 2008-10-31 | 2009-04-22 | 天通控股股份有限公司 | High-frequency nickel-copper-zinc ferrite and preparation thereof |
| JP2010215453A (en) * | 2009-03-17 | 2010-09-30 | Fdk Corp | NiCuZn FERRITE |
| CN113943153A (en) * | 2021-09-29 | 2022-01-18 | 江西瑞佳磁电子科技有限公司 | High-energy-storage and high-temperature-resistant magnetic core material and preparation method thereof |
| CN114773046A (en) * | 2022-04-25 | 2022-07-22 | 西安锐磁电子科技有限公司 | High-saturation-flux-density low-loss NiCuZn soft magnetic ferrite material and preparation method thereof |
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2022
- 2022-11-09 CN CN202211397597.9A patent/CN115677336B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH11340024A (en) * | 1998-05-26 | 1999-12-10 | Tokin Corp | Low-loss oxide magnetic material |
| JP2008127230A (en) * | 2006-11-17 | 2008-06-05 | Jfe Ferrite Corp | MnZnNi FERRITE |
| CN101388268A (en) * | 2008-07-11 | 2009-03-18 | 临沂中瑞电子有限公司 | High magnetic conductive low temperature sintered NiCuZn ferrite material |
| CN101412622A (en) * | 2008-10-31 | 2009-04-22 | 天通控股股份有限公司 | High-frequency nickel-copper-zinc ferrite and preparation thereof |
| JP2010215453A (en) * | 2009-03-17 | 2010-09-30 | Fdk Corp | NiCuZn FERRITE |
| CN113943153A (en) * | 2021-09-29 | 2022-01-18 | 江西瑞佳磁电子科技有限公司 | High-energy-storage and high-temperature-resistant magnetic core material and preparation method thereof |
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