CN116354712A - Ferrite material, preparation method, near field communication antenna and communication equipment - Google Patents

Ferrite material, preparation method, near field communication antenna and communication equipment Download PDF

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CN116354712A
CN116354712A CN202310334108.3A CN202310334108A CN116354712A CN 116354712 A CN116354712 A CN 116354712A CN 202310334108 A CN202310334108 A CN 202310334108A CN 116354712 A CN116354712 A CN 116354712A
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ferrite material
weight
preparation
precursor powder
slurry
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谢国勇
何传海
冉滢
刁开常
王宗顺
任金荣
柯立炎
李可明
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Dongguan Demen Electronics Co ltd
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Abstract

The application discloses ferrite material, preparation method, near field communication antenna and communication equipment, the preparation method of ferrite material includes: ball milling the main components and the additives to obtain slurry, wherein the main components comprise the following components in percentage by weight: fe (Fe) 2 O 3 60-70%, 15-22% ZnO, 7-10% CuO and 7-9% NiO; the additive comprises the following components in percentage by weight of 1: co (Co) 2 O 3 0.6 to 1.0 percent, liF0.2 to 0.4 percent; sieving the slurry and presintering to obtain precursor powder; and pressing and forming the precursor powder, and performing final sintering to obtain the ferrite material. The ferrite material prepared by the application has the magnetic permeability imaginary part inNo more than 5 at 13.56MHz, while the real part of permeability is greater than 235. In addition, the content of NiO in the ferrite material is lower, so that the cost of the ferrite material can be reduced.

Description

Ferrite material, preparation method, near field communication antenna and communication equipment
Technical Field
The application relates to the technical field of ferrite materials, in particular to a ferrite material, a preparation method, a near field communication antenna and communication equipment.
Background
With the development of electronic products toward small, thin and light, the market has put higher demands on magnetic sheets for near field communication (Near Field Communication, NFC) antennas, requiring that the real part (u') of magnetic permeability at 13.56MHz frequency after the fragments of the magnetic sheet (including the air gap) is not lower than 180 and the imaginary part (u ") of magnetic permeability is smaller than 5, which requires that the real part of magnetic permeability before the fragments of the magnetic sheet is 200 or more and even greater than 235 and the imaginary part of magnetic permeability is smaller than 5.
The magnetic sheet made of the existing ferrite material can not meet the requirement of the real part of magnetic permeability or the imaginary part of magnetic permeability exceeds 5, and the loss is overlarge.
Disclosure of Invention
Aiming at the technical problems, the application provides a ferrite material, a preparation method, a near field communication antenna and communication equipment, which can solve the problems that the real part of magnetic permeability of a magnetic sheet manufactured by the existing ferrite material cannot meet the requirement or the imaginary part of magnetic permeability exceeds 5, so that the loss is overlarge.
In order to solve the above technical problems, in a first aspect, an embodiment of the present application provides a method for preparing a ferrite material, including:
ball milling is carried out on the main components and the additives to obtain slurry, wherein the main components comprise the following components in percentage by weight: fe (Fe) 2 O 3 60～70％，ZnO 15～22％，CuO 7～10 percent, 7 to 9 percent of NiO; the additive comprises the following components in percentage by weight of 1: co (Co) 2 O 3 0.6～1.0％，LiF 0.2～0.4％；
Sieving the slurry and presintering to obtain precursor powder;
and pressing and forming the precursor powder, and performing final sintering to obtain the ferrite material.
Optionally, in the presintering step, the presintering temperature is 785-815 ℃ and the heat preservation time is 100-150 min.
Optionally, in the final firing step, the final firing temperature is 945-965 ℃ and the heat preservation time is 100-150 min.
Optionally, in the ball milling step, the weight ratio of the total weight of the main component and the additive to the grinding body and the water is 1:1:1.
Optionally, the sieving treatment includes:
the slurry was dried and then screened through a 40 mesh screen.
Optionally, the compacting the precursor powder includes:
the precursor powder is put into a mould and then is mixed with the powder at a ratio of 0.9 to 1.1t/cm 2 Is formed by pressure pressing.
In a second aspect, embodiments of the present application also provide a ferrite material comprising a main component and an additive;
the main components comprise the following components in percentage by weight: fe (Fe) 2 O 3 60～70％，ZnO 15～22％，CuO7～10％，NiO 7～9％；
The additive comprises the following components in percentage by weight of 1: co (Co) 2 O 3 0.6～1.0％，LiF0.2～0.4％。
Optionally, the main components comprise, in weight percent: fe (Fe) 2 O 3 63％，ZnO 20％，CuO 9％，NiO 8％。
In a third aspect, embodiments of the present application further provide a near field communication antenna, including a magnetic sheet, where the magnetic sheet includes the ferrite material described in each embodiment above, or is prepared by the preparation method described in each embodiment above.
In a fourth aspect, embodiments of the present application further provide a communication device, including a near field communication antenna as described in the foregoing embodiments.
As described above, the present embodiment provides a method for preparing a ferrite material, wherein the ferrite material includes a main component and an additive, and the main component includes, in weight percent: fe (Fe) 2 O 3 60-70%, 15-22% ZnO, 7-10% CuO and 7-9% NiO; the additive comprises the following components in percentage by weight of 1: co (Co) 2 O 3 0.6 to 1.0 percent, and 0.2 to 0.4 percent of LiF. In the embodiment, the main components and the additives are ball-milled to obtain slurry, and then the slurry is screened and presintered to obtain precursor powder; and finally, compacting and forming the precursor powder, and finally sintering to obtain the ferrite material. The ferrite material prepared by the embodiment has uniform crystal grains and compact structure, the magnetic permeability imaginary part of the ferrite material can not exceed 5 under 13.56MHz, and the magnetic permeability real part is larger than 235. In addition, due to the high cost of NiO, the composition of NiO in the ferrite material of the embodiment is controlled below 9%, and the minimum composition can be 7%, compared with the existing ferrite materials, the NiO content is greatly reduced, and therefore the cost of the ferrite material can be reduced.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the application and together with the description, serve to explain the principles of the application. In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the description of the embodiments will be briefly described below, and it will be obvious to those skilled in the art that other drawings can be obtained from these drawings without inventive effort.
Fig. 1 is a schematic flow chart of a method for preparing ferrite material according to an embodiment of the present application;
FIG. 2 is a cross-sectional view of a ferrite material of example 1 of the present application;
fig. 3 is a cross-sectional view of the ferrite material of comparative example 1.
The realization, functional characteristics and advantages of the present application will be further described with reference to the embodiments, referring to the attached drawings. Specific embodiments thereof have been shown by way of example in the drawings and will herein be described in more detail. These drawings and the written description are not intended to limit the scope of the inventive concepts in any way, but to illustrate the concepts of the present application to those skilled in the art by reference to specific embodiments.
Detailed Description
With the development of electronic products in the directions of small, thin and light, the market has put higher demands on magnetic sheets for near field communication antennas, and the real part of magnetic permeability at 13.56MHz frequency after the magnetic sheet fragments (including air gaps) is required to be not less than 180, and the imaginary part of magnetic permeability is required to be less than 5, which requires that the real part of magnetic permeability before the magnetic sheet fragments is above 200, even more than 235, and the imaginary part of magnetic permeability is required to be less than 5. The magnetic sheet made of the existing ferrite material can not meet the requirement of the real part of magnetic permeability or the imaginary part of magnetic permeability exceeds 5, and the loss is overlarge. Based on the above, the application provides a ferrite material, a preparation method, a near field communication antenna and communication equipment.
The ferrite material provided by the embodiment of the application comprises a main component and an additive. Wherein, the main components comprise the following components in percentage by weight: fe (Fe) 2 O 3 60-70%, 15-22% ZnO, 7-10% CuO and 7-9% NiO; the additive comprises the following components in percentage by weight of 1: co (Co) 2 O 3 0.6 to 1.0 percent, and 0.2 to 0.4 percent of LiF. For example, the ferrite material may include the following components in 100 parts by weight of the main component: fe (Fe) 2 O 3 63 parts of ZnO20 parts, cuO 9 parts, niO8 parts and Co 2 O 3 0.8 part of LiF and 0.3 part of a glass fiber.
In order to meet the performance requirement of the NFC antenna, the ferrite material of this embodiment is NiCuZn, and the content of each component has strict requirements, and the influence of the content of each component on the performance is generally as follows:
for Fe 2 O 3 ，Fe 2 O 3 Is a ferromagnetic substance that helps to boost the magnetic moment of the material. If it isFe 2 O 3 If the content of the ferrite is lower than 60wt%, the real part of the magnetic permeability of the obtained ferrite material at 13.56MHz is less than 235, if Fe 2 O 3 The content of the ferrite material is higher than 70 weight percent, and although the real part of the magnetic permeability of the ferrite material can meet the requirement (namely more than 235), the imaginary part of the magnetic permeability is far more than 5, and the requirement of the NFC antenna on low loss can not be met.
For ZnO, if the content of ZnO is lower than 15wt%, the real part of magnetic permeability of ferrite material at 13.56MHz can not reach 235, and if the content of ZnO is higher than 22wt%, although the real part of magnetic permeability of ferrite material meets the requirement, the imaginary part of magnetic permeability is far greater than 5, and the requirement of NFC antenna on low loss can not be met.
For CuO, if the content of CuO is lower than 7wt%, the sintering activity of the ferrite material is poor, resulting in low density after sintering, so that the real part of magnetic permeability of the ferrite material at 13.56MHz is difficult to reach more than 235, and if the content of CuO is higher than 10wt%, the sintering activity of the ferrite material is too high, resulting in excessive growth of material grains, so that the magnetic property of the ferrite material is deteriorated, resulting in the imaginary part of magnetic permeability being far greater than 5, and the low loss requirement cannot be met.
For Co 2 O 3 If Co 2 O 3 The content of the ferrite material is lower than 0.6wt%, the magnetic permeability imaginary part of the ferrite material is far more than 5, the requirement of NFC on low loss is not met, if Co 2 O 3 If the content of (2) is higher than 1wt%, the real part of the magnetic permeability of the ferrite material at 13.56MHz is difficult to reach more than 235.
For LiF, liF contains Li+ with larger ionic radius and smaller charge number, and the Li+ is easy to occupy the B ion position of a spinel structure in the ferrite material presintering or sintering process, and more oxygen vacancy defects are formed in a crystal structure, so that the presintering temperature of ferrite powder is easy to be reduced, the effect of refining grains is achieved, and the sintering activity of the ferrite material is improved. If the content of LiF is less than 0.1wt%, it is difficult to play a role in refining ferrite grains during sintering, so that it is difficult to improve the sintering activity of the material, and if the content of LiF is more than 0.5wt%, the magnetic permeability of the ferrite material is reduced.
It should be noted that, ferriteWhen the bulk material is sintered, if the grain growth of the ferrite material is not perfect, the real part of the magnetic permeability of the ferrite material is lower; if the grains grow excessively, the magnetic property of the ferrite material is deteriorated to lead the imaginary part of the magnetic permeability to be larger than 5, and the low-loss requirement cannot be met. The ferrite material of the embodiment has strict proportioning requirements on each component, and the additive can improve the microstructure (such as grain size, uniformity, density and the like) of the ferrite material during sintering. Wherein Co is 2 O 3 The NiCuZn ferrite material has the function of improving the high-frequency performance of the material, is matched with LiF to improve the green density of the ferrite material and achieve the semi-fusion state of crystal grains, so that the magnetic permeability imaginary part of the NiCuZn ferrite material of the embodiment can not exceed 5 at 13.56MHz, and meanwhile, the magnetic permeability real part basically achieves a larger value, thereby meeting the requirement of being more than 235.
In addition, due to the high cost of NiO, the composition of NiO in the ferrite material of the embodiment is controlled below 9%, and according to researches and tests, the minimum composition can be 7%, and compared with the existing ferrite materials, the NiO content is greatly reduced, so that the cost of the ferrite material can be reduced.
The embodiment of the application also provides a preparation method of the ferrite material, referring to fig. 1, fig. 1 is a schematic flow chart of the preparation method of the ferrite material, and the method includes:
s101, ball milling is carried out on the main components and the additives to obtain slurry, wherein the main components comprise the following components in percentage by weight: fe (Fe) 2 O 3 60-70%, 15-22% ZnO, 7-10% CuO and 7-9% NiO; the additive comprises the following components in percentage by weight of 1: co (Co) 2 O 3 0.6～1.0％，LiF 0.2～0.4％。
For example, the main component and the additive are firstly respectively compounded according to the components, and then the main component and the additive are mixed for ball milling. As some examples, deionized water may be used as a solvent for ball milling, and the milling bodies may be zirconia balls having a diameter of 3 to 5 mm.
In one embodiment, the weight ratio of the total weight of the main ingredients and additives to the abrasive body, water, is 1:1:1. The rotating speed and the ball milling time of the ball mill can be set according to the final particle size requirement of the powder, and the slurry is obtained after the ball milling is completed.
S102, sieving the slurry and presintering to obtain precursor powder.
For example, the resulting slurry may be subjected to a drying treatment, for example, the slurry may be baked in an oven at 150 ℃ for 48 hours. Sieving, for example, a 40 mesh sieve can be adopted to obtain uniform and fine primary powder, and the primary powder is presintered in air atmosphere to obtain precursor powder.
In one embodiment, the process conditions for burn-in may be: the presintering temperature is 785-815 ℃, the heat preservation time is 100-150 min, and the sintering activity of the precursor powder can be increased by presintering.
And S103, pressing and forming the precursor powder, and finally firing to obtain the ferrite material.
After the precursor powder is prepared, the precursor powder can be pressed and molded. For example, compression molding may be employed. As an example, the precursor powder may be placed in a mold of a preset shape and then at 0.9 to 1.1t/cm 2 Is formed by pressure pressing. The predetermined shape may be regarded as a shape of the precursor powder after being pressed to be molded (e.g., the obtained magnetic sheet).
And finally sintering the formed ferrite material to obtain a finished product made of the ferrite material, for example, the finished product can be a magnetic sheet. In one embodiment, the process conditions for the final firing may be: the final firing temperature is 945 to 965 ℃ and the heat preservation time is 100 to 150min. For example, the shaped ferrite material may be sintered in a box-type sintering furnace at 950 ℃ for 2 hours.
The NiCuZn ferrite material prepared by the embodiment has the magnetic permeability imaginary part smaller than 5 at 13.56MHz, and the magnetic permeability real part larger than 235, and can reduce the cost simultaneously due to the lower NiO content.
The embodiment of the application also provides a near field communication antenna, which comprises a magnetic sheet. Wherein the magnetic sheet comprises the ferrite material described in each embodiment or is prepared by the preparation method described in each embodiment.
The embodiments of the present application also provide a communication device, which includes the near field communication antenna as described in the foregoing embodiments, so that the communication device may also generate the beneficial effects of the near field communication antenna of the embodiments. As some examples, the communication device may be a mobile device such as a mobile phone, a smart watch/bracelet, a tablet computer, or a fixed device such as a router, a communication base station, or the like.
The present application is further illustrated by the following examples.
Example 1
(1) Slurry preparation
The preparation method comprises the following steps of: fe (Fe) 2 O 3 63 parts of ZnO20 parts, cuO 9 parts, niO8 parts and Co 2 O 3 0.8 part and LiF 0.3 part, then according to the raw materials: grinding body: water = 1:1:1, ball milling and mixing uniformly to obtain slurry.
(2) Precursor powder preparation
Baking the slurry in an oven at 150 ℃ for 48 hours, sieving by a 40-mesh sieve, and finally presintering the powder obtained by sieving in an air atmosphere, wherein the sintering temperature is 800 ℃ and the sintering time is 120min.
(3) Ferrite material preparation
Filling the precursor powder into a mold, and then carrying out the process at a speed of 1.0t/cm 2 And finally sintering the mixture for 120min in an air atmosphere at 955 ℃, cooling the mixture along with a furnace, and completing the preparation of the ferrite material.
Example 2
(1) Slurry preparation
The preparation method comprises the following steps of: fe (Fe) 2 O 3 60 parts of ZnO 22 parts, cuO 10 parts, niO8 parts and Co 2 O 3 0.8 part and LiF 0.3 part, then according to the raw materials: grinding body: water = 1:1:1, ball milling and mixing uniformly to obtain slurry.
(2) Precursor powder preparation
Baking the slurry in an oven at 150 ℃ for 48 hours, sieving by a 40-mesh sieve, and finally presintering the powder obtained by sieving in an air atmosphere at 790 ℃ for 140min.
(3) Ferrite material preparation
Filling the precursor powder into a mold, and then carrying out the process at a speed of 0.9t/cm 2 And finally sintering for 110min in air atmosphere at 960 ℃, cooling along with a furnace, and completing the preparation of the ferrite material.
Example 3
(1) Slurry preparation
The preparation method comprises the following steps of: fe (Fe) 2 O 3 70 parts of ZnO 15 parts, cuO 8 parts, niO 7 parts and Co 2 O 3 0.8 part and LiF 0.3 part, then according to the raw materials: grinding body: water = 1:1:1, ball milling and mixing uniformly to obtain slurry.
(2) Precursor powder preparation
Baking the slurry in an oven at 150 ℃ for 48 hours, sieving by a 40-mesh sieve, and finally presintering the powder obtained by sieving in an air atmosphere at 810 ℃ for 110min.
(3) Ferrite material preparation
Filling the precursor powder into a mold, and then carrying out the process at a speed of 1.1t/cm 2 And (3) the ferrite material is finally sintered for 140 minutes in an air atmosphere at 950 ℃ and cooled along with a furnace, and the ferrite material is prepared.
Example 4
(1) Slurry preparation
The preparation method comprises the following steps of: fe (Fe) 2 O 3 65 parts of ZnO 18 parts, cuO 9 parts, niO8 parts and Co 2 O 3 0.8 part and LiF 0.3 part, then according to the raw materials: grinding body: water = 1:1:1, ball milling and mixing uniformly to obtain slurry.
(2) Precursor powder preparation
Baking the slurry in an oven at 150 ℃ for 48 hours, sieving by a 40-mesh sieve, and finally presintering the powder obtained by sieving in an air atmosphere at the sintering temperature of 805 ℃ for 120min.
(3) Ferrite material preparation
Filling the precursor powder into a mold, and then carrying out the process at a speed of 1.0t/cm 2 And finally sintering for 135min in an air atmosphere at 952 ℃, cooling along with a furnace, and completing the preparation of the ferrite material.
Example 5
(1) Slurry preparation
The preparation method comprises the following steps of: fe (Fe) 2 O 3 63 parts of ZnO20 parts, cuO 9 parts, niO8 parts and Co 2 O 3 0.6 part and LiF 0.4 part, then according to the raw materials: grinding body: water = 1:1:1, ball milling and mixing uniformly to obtain slurry.
(2) Precursor powder preparation
Baking the slurry in an oven at 150 ℃ for 48 hours, sieving by a 40-mesh sieve, and finally presintering the powder obtained by sieving in an air atmosphere, wherein the sintering temperature is 800 ℃ and the sintering time is 120min.
(3) Ferrite material preparation
Filling the precursor powder into a mold, and then carrying out the process at a speed of 1.0t/cm 2 And finally sintering the mixture for 120min in an air atmosphere at 955 ℃, cooling the mixture along with a furnace, and completing the preparation of the ferrite material.
Example 6
(1) Slurry preparation
The preparation method comprises the following steps of: fe (Fe) 2 O 3 63 parts of ZnO20 parts, cuO 9 parts, niO8 parts and Co 2 O 3 1.0 part and LiF0.2 part, then according to the raw materials: grinding body: water = 1:1:1, ball milling and mixing uniformly to obtain slurry.
(2) Precursor powder preparation
Baking the slurry in an oven at 150 ℃ for 48 hours, sieving by a 40-mesh sieve, and finally presintering the powder obtained by sieving in an air atmosphere, wherein the sintering temperature is 800 ℃ and the sintering time is 120min.
(3) Ferrite material preparation
Filling the precursor powder into a mold, and then carrying out the process at a speed of 1.0t/cm 2 Is a pressure of (2)And (3) forming, and finally sintering for 120min in an air atmosphere at 955 ℃, cooling along with a furnace, and completing the preparation of the ferrite material.
Comparative example 1
Compared with example 2, the raw material formula is only different in that: fe (Fe) 2 O 3 55 parts of ZnO 28 parts, cuO 10 parts, niO 7 parts and Co 2 O 3 0.8 parts and LiF 0.3 parts.
Comparative example 2
Compared with example 1, the raw material formula is only different in that: fe (Fe) 2 O 3 74 parts of ZnO 7 parts, cuO6 parts, niO 13 parts and Co 2 O 3 0.8 parts and LiF 0.3 parts.
The raw material components of the above examples and comparative examples are specifically shown in the following table 1.
Table 1 raw material components and performance test data of each of examples and comparative examples
Figure BDA0004155832790000081
Performance testing and morphology characterization
SEM tests were performed on the samples of example 1 and comparative example 1, wherein fig. 2 is a cross-sectional view of the ferrite material of example 1 of the present application, which is uniform and dense in grain size; fig. 3 is a cross-sectional view of the ferrite material of comparative example 1, which is coarser in grains and has more voids.
The real part (u ') and the imaginary part (u ') of the magnetic sheet samples of each example and comparative example were tested using a kenisight's 4990 radio frequency impedance analyzer, and the test results are shown in Table 1.
As can be seen from the data in table 1, the magnetic properties of the ferrite materials prepared in examples 1 to 6 of the present application all satisfy: the real part of the magnetic permeability is larger than 235, and the imaginary part of the magnetic permeability is smaller than 5. Furthermore, the ferrite material of example 1 has optimal overall properties.
The compositions of comparative example 1 and comparative example 2 are outside the limits defined herein compared to example 1, the real part of the magnetic permeability of the ferrite material of comparative example 1 is less than 235, and the imaginary part of the magnetic permeability of the ferrite material of comparative example 2 is greater than 5.
The ferrite material, the preparation method, the near field communication antenna and the communication equipment provided by the application are described in detail, and specific examples are used for describing the principles and the implementation modes of the application. In this application, the descriptions of the embodiments are focused on, and the details or descriptions of one embodiment may be referred to as related descriptions of other embodiments.
The foregoing description is only of the preferred embodiments of the present application, and is not intended to limit the scope of the claims, and all equivalent structures or equivalent processes using the descriptions and drawings of the present application, or direct or indirect application in other related technical fields are included in the scope of the claims of the present application.

Claims (10)

1. A method of preparing a ferrite material, comprising:
ball milling is carried out on the main components and the additives to obtain slurry, wherein the main components comprise the following components in percentage by weight: fe (Fe) 2 O 3 60-70%, 15-22% ZnO, 7-10% CuO and 7-9% NiO; the additive comprises the following components in percentage by weight of 1: co (Co) 2 O 3 0.6～1.0％，LiF 0.2～0.4％；
Sieving the slurry and presintering to obtain precursor powder;
and pressing and forming the precursor powder, and performing final sintering to obtain the ferrite material.
2. The method according to claim 1, wherein in the pre-sintering step, the pre-sintering temperature is 785 to 815 ℃ and the heat preservation time is 100 to 150min.
3. The method according to claim 1, wherein in the final firing step, the final firing temperature is 945 to 965 ℃ and the holding time is 100 to 150min.
4. The method according to claim 1, wherein in the ball milling step, the weight ratio of the total weight of the main component and the additive to the grinding body and water is 1:1:1.
5. The method of manufacturing according to claim 1, wherein the sieving treatment comprises:
the slurry was dried and then screened through a 40 mesh screen.
6. The method of claim 1, wherein the compacting the precursor powder comprises:
the precursor powder is put into a mould and then is mixed with the powder at a ratio of 0.9 to 1.1t/cm 2 Is formed by pressure pressing.
7. A ferrite material characterized by comprising a main component and an additive;
the main components comprise the following components in percentage by weight: fe (Fe) 2 O 3 60～70％，ZnO 15～22％，CuO7～10％，NiO 7～9％；
The additive comprises the following components in percentage by weight of 1: co (Co) 2 O 3 0.6～1.0％，LiF0.2～0.4％。
8. The ferrite material of claim 7, wherein the main component comprises, in weight percent: fe (Fe) 2 O 3 63％，ZnO 20％，CuO 9％，NiO 8％。
9. A near field communication antenna comprising a magnetic sheet, characterized in that the magnetic sheet comprises the ferrite material of claim 7 or 8 or is prepared by the preparation method of any one of claims 1-6.
10. A communication device comprising the near field communication antenna of claim 9.
CN202310334108.3A 2023-03-29 2023-03-29 Ferrite material, preparation method, near field communication antenna and communication equipment Pending CN116354712A (en)

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