CN112430075A - Ferrite magnetic material and manufacturing method thereof - Google Patents

Ferrite magnetic material and manufacturing method thereof Download PDF

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CN112430075A
CN112430075A CN202011378750.4A CN202011378750A CN112430075A CN 112430075 A CN112430075 A CN 112430075A CN 202011378750 A CN202011378750 A CN 202011378750A CN 112430075 A CN112430075 A CN 112430075A
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sintering
ball milling
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main component
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陈国良
陈有标
汤小明
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Jiangxi Yao Run Magnetoelectric Technology Co ltd
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Jiangxi Yao Run Magnetoelectric Technology Co ltd
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Abstract

The invention belongs to the technical field of ferrite, and particularly relates to a ferrite magnetic material which comprises a main component, auxiliary components and an additive, wherein the main component comprises Fe2O3、Mo2O3、Yb2O3NiO and ZnO, and the auxiliary component comprises WO3And Nd2O3(ii) a Fe in the main component based on the amount of the main component2O348 to 52 mol% of Mo2O316 to 24 mol% of Yb2O3The content is 12-20 mol%, the NiO content is 9-15 mol%, and the ZnO content is 6-10 mol%; based on the weight of the main component, WO30.1 to 1 wt% of Nd2O3The content is 0.1-1 wt%; the additive is composed of2O5、SiO2And CuO. The ferrite material disclosed by the invention has higher magnetic conductivity and smaller magnetic loss at the same time under 13.56MHz, and meets the application requirements of NFC.

Description

Ferrite magnetic material and manufacturing method thereof
Technical Field
The invention belongs to the technical field of ferrite, and particularly relates to a ferrite magnetic material and a manufacturing method thereof.
Background
In the application of the 13.56MHzRFID electronic tag, the electronic tag needs to be attached to the metal surface or the adjacent position, so that in the identification process, the signal strength is greatly weakened by the attenuation effect of the metal eddy current, the reading process fails, therefore, a thin magnetic sheet needs to be added to reduce the eddy current effect, the magnetic conductivity of the magnetic sheet is higher, and the conduction effect is better. However, in general, a material having a high magnetic permeability has a large loss, and is not suitable for use in an NFC antenna module.
Currently, in the prior art, the magnetic permeability is mostly controlled to be about one hundred, and although the magnetic permeability can meet the use requirement, the magnetic permeability is still low, so that the development of the device towards small, thin and light directions is hindered.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provide a ferrite material with high real part of magnetic permeability (mu '≧ 185) and small imaginary part (mu' <1.5), and solve the technical problem that the prior ferrite material is difficult to obtain high magnetic permeability and low magnetic loss at the same time under the frequency of 13.56 MHz.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a ferrite magnetic material comprises a main component, an auxiliary component and an additive, wherein the main component comprises Fe2O3、Mo2O3、Yb2O3NiO and ZnO, the auxiliary component comprises WO3And Nd2O3(ii) a Based on the amount of the main component, Fe in the main component2O3The content of (A) is 48-52 mol%, Mo2O3Is 16 to 24 mol% of Yb2O3The content of the NiO is 12-20 mol%, the content of the NiO is 9-15 mol%, and the content of the ZnO is 6-10 mol%; based on the weight of the main component, WO in the auxiliary component3In an amount of 0.1 to 1 wt%, Nd2O3The content of (A) is 0.1-1 wt%; the additive is composed of V2O5、SiO2And CuO according to the weight ratio of 1: 2-3: 1-2, wherein the additive accounts for 0.1-0.6 wt% of the total weight of the whole material.
Based on one general inventive concept, another object of the present invention is to provide a method for preparing the above ferrite magnetic material, comprising the steps of:
s1, mixing, weighing Fe according to mole percentage2O3、Mo2O3、Yb2O3NiO and ZnO are put into a vibration mill for dry mixingCombining;
s2, carrying out primary wet grinding, namely filling the raw materials mixed in the step S1 into a ball milling tank, adding zirconia balls and deionized water, and carrying out primary wet mixing ball milling;
s3, presintering, namely drying the slurry obtained after primary wet grinding in the step S2, and putting the slurry into a sintering furnace for presintering, wherein the presintering temperature is 820-960 ℃, and the heat preservation time is 1.8-2.6 hours;
s4, secondary wet grinding, namely filling the materials subjected to pre-sintering in the step S3 into a ball milling tank, and adding WO by weight3、Nd2O3、V2O5、SiO2And CuO, adding zirconia balls and deionized water, and performing secondary wet mixing ball milling;
s5, granulating, namely drying the slurry subjected to secondary wet grinding in the step S4, and adding a binder for granulation;
s6, forming, namely putting the particles obtained in the step S5 into a mold for pressing, and pressing into a sample of a circular magnetic ring, wherein the sample has an outer diameter of 14-18 mm, an inner diameter of 6-10 mm and a height of 3-5 mm;
s7, sintering, namely sintering the circular magnetic ring obtained in the step S6 in a box type sintering furnace, wherein the sintering temperature is 980-1090 ℃, and the heat preservation time is 3-6 hours, so that the ferrite magnetic material is obtained.
Preferably, step S1, the Fe2O3、Mo2O3、Yb2O3And the purity of ZnO were all analytically pure.
Preferably, in the step S1, the NiO is in an approximately spherical shape and has a specific surface area of 50-60 m2The NiO is nano and has an average particle size of 50-100 nm.
Preferably, in the step S2, the mass ratio of the raw materials to the zirconia balls to the deionized water is 1: 2-4: 0.5-1.5, and the ball milling time is 1-24 h.
Preferably, in step S3, the burn-in specifically includes: heating from room temperature to 520-580 ℃ at the speed of 1.2 ℃/min, preserving heat at 520-580 ℃ for 0.8-1 h, heating to 820-960 ℃ at the speed of 1.8 ℃/min, preserving heat at 820-960 ℃ for 1-2 h, and cooling along with a furnace.
Preferably, in the step S4, the mass ratio of the raw materials to the zirconia balls to the deionized water is 1: 2-4: 0.5-1.5, and the ball milling time is 1-24 h.
Preferably, in step S5, the binder is polyvinyl butyral, and the amount of the polyvinyl butyral is 12-25 wt% of the weight of the dried slurry after the second wet grinding.
Preferably, in step S7, the sintering specifically includes: heating from room temperature to 520-580 ℃ at the speed of 1.2 ℃/min, preserving heat at 520-580 ℃ for 1-1.5 h, heating to 820-960 ℃ at the speed of 1.6 ℃/min, preserving heat at 820-960 ℃ for 1.5-2 h, heating to 980-1090 ℃ at the speed of 3.2 ℃/min, preserving heat at 980-1090 ℃ for 2.5-4 h, and cooling along with a furnace.
Compared with the prior art, the invention adds Mo, Yb, W, Nd, V, Si and Cu elements in the main formula at the same time, thus improving the magnetic property of the ferrite material. The loss of ferrite mainly comprises three parts of eddy current loss, hysteresis loss and residual loss, but only one loss generally occupies a dominant position under certain conditions, and the nickel-zinc ferrite is divided into three formulas of iron deficiency, positive iron and iron passing according to different iron contents; when the residual loss of the nickel-zinc ferrite is less than the resonance frequency, the hysteresis loss of the ferrite is mainly hysteresis loss, the hysteresis loss of the ferrite gradually increases with the increase of the operating frequency and becomes a main part of the loss, and when the hysteresis loss is mainly loss, more Fe can be provided2+With Fe, however, the over-iron formulation has less loss2+Increase in content eddy current loss is also increasing continuously, Fe2+Too high a content increases the total losses, not the more the iron content the better, so in the main formulation Mo passes3+And Yb3+The doping of (A) can promote Fe2+Formation of ions, more Fe2+The iron-passing formula has smaller hysteresis aftereffect loss, and the introduced excessive positive charges can realize the balance of electrovalence by reducing the equivalent amount of positively charged oxygen vacancies existing in the system, so that the lattice distortion of the system is favorably reduced; addition of W6+Solid-dissolved in crystal grains, and reduced in lattice strain to reduce the saturation magnetostriction constant λ S and the magnetic anisotropy constant K1, thereby improving magnetic permeability while suppressing increase in material lossAdding; nd (neodymium)2O3Can increase lattice constant, prevent domain wall movement, and improve quality factor Q, V at cut-off frequency and high frequency2O5Forming liquid phase in ferrite crystal boundary to raise the density of sintered magnetic sheet, raise strength of sample and reduce brittleness, but its content must not be too high, otherwise it can affect the performance of magnetic sheet, SiO2The abnormal growth of crystal grains can be inhibited, the effect of refining the crystal grains is achieved, the sintering at low temperature can be effectively accelerated by adding a proper amount of CuO, the sintering temperature is reduced, and the sintering density is increased. The ferrite material disclosed by the invention has higher magnetic conductivity and smaller magnetic loss at the same time under 13.56MHz through tests, and meets the application requirements of NFC.
Detailed Description
The present invention will be further described with reference to specific embodiments for the purpose of making the objects, technical solutions and advantages of the present invention more apparent, but the present invention is not limited to these examples. It should be noted that, without conflict, any combination between the embodiments or technical features described below may form a new embodiment. In the invention, all parts and percentages are mass units, and the adopted equipment, raw materials and the like can be purchased from the market or are commonly used in the field. The methods in the following examples are conventional in the art unless otherwise specified.
Example 1
A ferrite magnetic material comprises a main component, an auxiliary component and an additive, wherein the main component comprises Fe2O3、Mo2O3、Yb2O3NiO and ZnO, the auxiliary component comprises WO3And Nd2O3(ii) a Based on the amount of the main component, Fe in the main component2O3Content of (3) Mo2O3Is 20 mol% of Yb2O3The content of (A) is 14 mol%, the content of NiO is 10 mol%, and the content of ZnO is 6 mol%; based on the weight of the main component, WO in the auxiliary component3Content of (B) 0.52 wt%, Nd2O3The content of (B) is 0.48 wt%; the additive isThe additive is composed of V2O5、SiO2And CuO in a weight ratio of 1: 2.5: 1.5, said additive comprising 0.32 wt% of the total weight of the entire material.
The preparation method of the ferrite magnetic material comprises the following steps:
s1, mixing, weighing Fe according to mole percentage2O3、Mo2O3、Yb2O3NiO and ZnO are put into a vibration mill for dry mixing;
wherein, the Fe2O3、Mo2O3、Yb2O3And the purities of ZnO and NiO are analytically pure, the NiO is in an approximately spherical shape, and the specific surface area is 50-60 m2The NiO is nano and has an average particle size of 75 nm;
s2, carrying out primary wet grinding, namely filling the raw materials mixed in the step S1 into a ball milling tank, adding zirconia balls and deionized water, and carrying out primary wet mixing ball milling;
wherein, the mass ratio of the raw materials to the zirconia balls to the deionized water is 1: 3: 1, and the ball milling time is 3.5 h;
s3, presintering, namely drying the slurry obtained after the primary wet grinding in the step S2, and putting the dried slurry into a sintering furnace for presintering, wherein the presintering specifically comprises the following steps: heating from room temperature to 550 ℃ at the speed of 1.2 ℃/min, preserving heat at 550 ℃ for 0.92h, heating to 910 ℃ at the speed of 1.8 ℃/min, preserving heat at 820-960 ℃ for 1.5h, and cooling along with the furnace;
s4, secondary wet grinding, namely filling the materials subjected to pre-sintering in the step S3 into a ball milling tank, and adding WO by weight3、Nd2O3、V2O5、SiO2And CuO, adding zirconia balls and deionized water, and performing secondary wet mixing ball milling;
wherein, the raw materials (material after S3 pre-burning + WO by weight)3、Nd2O3、V2O5、SiO2Mixing with CuO, zirconia balls and deionized water in a mass ratio of 1: 3: 1, and ball milling for 2.5 h;
s5, granulating, namely drying the slurry subjected to secondary wet grinding in the step S4, and adding a binder for granulation;
wherein the adhesive is polyvinyl butyral, and the dosage of the polyvinyl butyral is 18.5 wt% of the weight of the dried slurry after the secondary wet grinding;
s6, forming, namely putting the particles obtained in the step S5 into a mold for pressing, maintaining the pressure at 25MPa for 2min for forming, and pressing into a sample of a circular magnetic ring, wherein the sample has the outer diameter of 16mm, the inner diameter of 8mm and the height of 4 mm;
s7, sintering, namely sintering the circular magnetic ring obtained in the step S6 in a box type sintering furnace, wherein the sintering specifically comprises the following steps: raising the temperature from room temperature to 560 ℃ at the speed of 1.2 ℃/min, preserving the heat at 560 ℃ for 1.2h, raising the temperature to 890 ℃ at the speed of 1.6 ℃/min, preserving the heat at 820-960 ℃ for 1.6h, raising the temperature to 980-1090 ℃ at the speed of 3.2 ℃/min, preserving the heat at 1035 ℃ for 3.2h, and cooling along with a furnace to obtain the ferrite magnetic material.
Example 2
A ferrite magnetic material comprises a main component, an auxiliary component and an additive, wherein the main component comprises Fe2O3、Mo2O3、Yb2O3NiO and ZnO, the auxiliary component comprises WO3And Nd2O3(ii) a Based on the amount of the main component, Fe in the main component2O3Content of (2) Mo2O3Is 16 mol% of Yb2O3The content of (A) is 12 mol%, the content of NiO is 12.5 mol%, and the content of ZnO is 7.5 mol%; based on the weight of the main component, WO in the auxiliary component3Content of (B) 0.26 wt%, Nd2O3Is 0.15 wt%; the additive is composed of V2O5、SiO2And CuO in a weight ratio of 1: 3: 1, the additive accounting for 0.5 wt% of the total weight of the whole material.
The preparation method of the ferrite magnetic material comprises the following steps:
s1, mixing, weighing Fe according to mole percentage2O3、Mo2O3、Yb2O3NiO and ZnO are put into a vibration mill for dry mixing;
wherein, the Fe2O3、Mo2O3、Yb2O3And the purities of ZnO and NiO are analytically pure, the NiO is in an approximately spherical shape, and the specific surface area is 50-60 m2The NiO is nano and has an average particle size of 100 nm;
s2, carrying out primary wet grinding, namely filling the raw materials mixed in the step S1 into a ball milling tank, adding zirconia balls and deionized water, and carrying out primary wet mixing ball milling;
wherein, the mass ratio of the raw materials to the zirconia balls to the deionized water is 1: 4: 0.9, and the ball milling time is 2.7 h;
s3, presintering, namely drying the slurry obtained after the primary wet grinding in the step S2, and putting the dried slurry into a sintering furnace for presintering, wherein the presintering specifically comprises the following steps: heating from room temperature to 580 deg.C at a rate of 1.2 deg.C/min, maintaining at 580 deg.C for 0.8h, heating to 960 deg.C at a rate of 1.8 deg.C/min, maintaining at 960 deg.C for 1.2h, and furnace cooling;
s4, secondary wet grinding, namely filling the materials subjected to pre-sintering in the step S3 into a ball milling tank, and adding WO by weight3、Nd2O3、V2O5、SiO2And CuO, adding zirconia balls and deionized water, and performing secondary wet mixing ball milling;
wherein, the raw materials (material after S3 pre-burning + WO by weight)3、Nd2O3、V2O5、SiO2Mixing with CuO, zirconia balls and deionized water in a mass ratio of 1: 4: 1, and ball milling for 3.5 h;
s5, granulating, namely drying the slurry subjected to secondary wet grinding in the step S4, and adding a binder for granulation;
wherein the adhesive is polyvinyl butyral, and the dosage of the polyvinyl butyral is 25 wt% of the weight of the dried slurry after the secondary wet grinding;
s6, forming, namely putting the particles obtained in the step S5 into a mold for pressing, maintaining the pressure at 25MPa for 2min for forming, and pressing into a sample of a circular magnetic ring, wherein the sample has the outer diameter of 16mm, the inner diameter of 8mm and the height of 4 mm;
s7, sintering, namely sintering the circular magnetic ring obtained in the step S6 in a box type sintering furnace, wherein the sintering specifically comprises the following steps: heating from room temperature to 520 ℃ at the speed of 1.2 ℃/min, preserving heat at 520 ℃ for 1h, heating to 960 ℃ at the speed of 1.6 ℃/min, preserving heat at 960 ℃ for 2h, heating to 1090 ℃ at the speed of 3.2 ℃/min, preserving heat at 980-1090 ℃ for 3h, and cooling along with a furnace to obtain the ferrite magnetic material.
Example 3
A ferrite magnetic material comprises a main component, an auxiliary component and an additive, wherein the main component comprises Fe2O3、Mo2O3、Yb2O3NiO and ZnO, the auxiliary component comprises WO3And Nd2O3(ii) a Based on the amount of the main component, Fe in the main component2O3Content of (3) is 48 mol%, Mo2O3In an amount of 24 mol%, Yb2O3The content of (2) is 12 mol%, the content of NiO is 9 mol%, and the content of ZnO is 7 mol%; based on the weight of the main component, WO in the auxiliary component3Content of (B) 0.62 wt%, Nd2O3Is 0.12 wt%; the additive is composed of V2O5、SiO2And CuO in a weight ratio of 1: 2, the additive accounting for 0.25 wt% of the total weight of the whole material.
The preparation method of the ferrite magnetic material comprises the following steps:
s1, mixing, weighing Fe according to mole percentage2O3、Mo2O3、Yb2O3NiO and ZnO are put into a vibration mill for dry mixing;
wherein, the Fe2O3、Mo2O3、Yb2O3And the purities of ZnO and NiO are analytically pure, the NiO is in an approximately spherical shape, and the specific surface area is 50-60 m2The NiO is nano and has an average particle size of 50 nm;
s2, carrying out primary wet grinding, namely filling the raw materials mixed in the step S1 into a ball milling tank, adding zirconia balls and deionized water, and carrying out primary wet mixing ball milling;
wherein, the mass ratio of the raw materials to the zirconia balls to the deionized water is 1: 2: 1.5, and the ball milling time is 3.2 h;
s3, presintering, namely drying the slurry obtained after the primary wet grinding in the step S2, and putting the dried slurry into a sintering furnace for presintering, wherein the presintering specifically comprises the following steps: heating from room temperature to 520 ℃ at the speed of 1.2 ℃/min, preserving heat at 520 ℃ for 1h, heating to 820 ℃ at the speed of 1.8 ℃/min, preserving heat at 820 ℃ for 1.5h, and then cooling along with the furnace;
s4, secondary wet grinding, namely filling the materials subjected to pre-sintering in the step S3 into a ball milling tank, and adding WO by weight3、Nd2O3、V2O5、SiO2And CuO, adding zirconia balls and deionized water, and performing secondary wet mixing ball milling;
wherein, the raw materials (material after S3 pre-burning + WO by weight)3、Nd2O3、V2O5、SiO2And CuO, zirconia balls and deionized water in a mass ratio of 1: 2: 1.5, and ball milling time is 5 hours;
s5, granulating, namely drying the slurry subjected to secondary wet grinding in the step S4, and adding a binder for granulation;
wherein the adhesive is polyvinyl butyral, and the dosage of the polyvinyl butyral is 12 wt% of the weight of the dried slurry after the secondary wet grinding;
s6, forming, namely putting the particles obtained in the step S5 into a mold for pressing, maintaining the pressure at 25MPa for 2min for forming, and pressing into a sample of a circular magnetic ring, wherein the sample has the outer diameter of 16mm, the inner diameter of 8mm and the height of 4 mm;
s7, sintering, namely sintering the circular magnetic ring obtained in the step S6 in a box type sintering furnace, wherein the sintering specifically comprises the following steps: and heating the ferrite magnetic material from room temperature to 580 ℃ at the speed of 1.2 ℃/min, preserving heat at 580 ℃ for 1h, heating the ferrite magnetic material to 820 ℃ at the speed of 1.6 ℃/min, preserving heat at 820-960 ℃ for 1.5h, heating the ferrite magnetic material to 1090 ℃ at the speed of 3.2 ℃/min, preserving heat at 1090 ℃ for 2.5h, and cooling the ferrite magnetic material along with a furnace to obtain the ferrite magnetic material.
Comparative example 1
A ferrite magnetic material comprising a main component including Fe2O3NiO and ZnO; based on the amount of the main component, Fe in the main component2O3In an amount of84mol percent of the NiO, 10mol percent of the NiO and 6mol percent of the ZnO;
the preparation method of the ferrite magnetic material comprises the following steps:
s1, mixing, and weighing Fe according to mole percentage2O3NiO and ZnO are put into a vibration mill for dry mixing;
wherein, the Fe2O3And the purities of ZnO and NiO are analytically pure, the NiO is in an approximately spherical shape, and the specific surface area is 50-60 m2The NiO is nano and has an average particle size of 75 nm;
s2, carrying out primary wet grinding, namely filling the raw materials mixed in the step S1 into a ball milling tank, adding zirconia balls and deionized water, and carrying out primary wet mixing ball milling;
wherein, the mass ratio of the raw materials to the zirconia balls to the deionized water is 1: 3: 1, and the ball milling time is 3.5 h;
s3, presintering, namely drying the slurry obtained after the primary wet grinding in the step S2, and putting the dried slurry into a sintering furnace for presintering, wherein the presintering specifically comprises the following steps: heating from room temperature to 550 ℃ at the speed of 1.2 ℃/min, preserving heat at 550 ℃ for 0.92h, heating to 910 ℃ at the speed of 1.8 ℃/min, preserving heat at 820-960 ℃ for 1.5h, and cooling along with the furnace;
s4, secondary wet grinding, namely filling the pre-sintered material obtained in the step S3 into a ball milling tank, adding zirconia balls and deionized water, and performing secondary wet mixing ball milling;
wherein, the mass ratio of the raw materials (the materials after S3 is preburnt) to the zirconia balls to the deionized water is 1: 3: 1, and the ball milling time is 2.5 h;
s5, granulating, namely drying the slurry subjected to secondary wet grinding in the step S4, and adding a binder for granulation;
wherein the adhesive is polyvinyl butyral, and the dosage of the polyvinyl butyral is 18.5 wt% of the weight of the dried slurry after the secondary wet grinding;
s6, forming, namely putting the particles obtained in the step S5 into a mold for pressing, maintaining the pressure at 25MPa for 2min for forming, and pressing into a sample of a circular magnetic ring, wherein the sample has the outer diameter of 16mm, the inner diameter of 8mm and the height of 4 mm;
s7, sintering, namely sintering the circular magnetic ring obtained in the step S6 in a box type sintering furnace, wherein the sintering specifically comprises the following steps: raising the temperature from room temperature to 560 ℃ at the speed of 1.2 ℃/min, preserving the heat at 560 ℃ for 1.2h, raising the temperature to 890 ℃ at the speed of 1.6 ℃/min, preserving the heat at 820-960 ℃ for 1.6h, raising the temperature to 980-1090 ℃ at the speed of 3.2 ℃/min, preserving the heat at 1035 ℃ for 3.2h, and cooling along with a furnace to obtain the ferrite magnetic material.
Comparative example 2
A ferrite magnetic material comprises a main component, an auxiliary component and an additive, wherein the main component comprises Fe2O3NiO and ZnO, the auxiliary component comprises WO3And Nd2O3(ii) a Based on the amount of the main component, Fe in the main component2O3The content of (A) is 84 mol%, the content of NiO is 10 mol%, the content of ZnO is 6 mol%, and the additive is prepared from V2O5、SiO2And CuO according to the weight ratio of 1: 2.5: 1.5, wherein the additive accounts for 0.32 wt% of the total weight of the whole material;
the preparation method of the ferrite magnetic material comprises the following steps:
s1, mixing, and weighing Fe according to mole percentage2O3NiO and ZnO are put into a vibration mill for dry mixing;
wherein, the Fe2O3And the purities of ZnO and NiO are analytically pure, the NiO is in an approximately spherical shape, and the specific surface area is 50-60 m2The NiO is nano and has an average particle size of 75 nm;
s2, carrying out primary wet grinding, namely filling the raw materials mixed in the step S1 into a ball milling tank, adding zirconia balls and deionized water, and carrying out primary wet mixing ball milling;
wherein, the mass ratio of the raw materials to the zirconia balls to the deionized water is 1: 3: 1, and the ball milling time is 3.5 h;
s3, presintering, namely drying the slurry obtained after the primary wet grinding in the step S2, and putting the dried slurry into a sintering furnace for presintering, wherein the presintering specifically comprises the following steps: heating from room temperature to 550 ℃ at the speed of 1.2 ℃/min, preserving heat at 550 ℃ for 0.92h, heating to 910 ℃ at the speed of 1.8 ℃/min, preserving heat at 820-960 ℃ for 1.5h, and cooling along with the furnace;
s4, secondary wet grinding, namely filling the materials subjected to pre-sintering in the step S3 into a ball milling tank, and adding WO by weight3、Nd2O3、V2O5、SiO2And CuO, adding zirconia balls and deionized water, and performing secondary wet mixing ball milling;
wherein, the raw materials (material after S3 pre-burning + WO by weight)3、Nd2O3、V2O5、SiO2Mixing with CuO, zirconia balls and deionized water in a mass ratio of 1: 3: 1, and ball milling for 2.5 h;
s5, granulating, namely drying the slurry subjected to secondary wet grinding in the step S4, and adding a binder for granulation;
wherein the adhesive is polyvinyl butyral, and the dosage of the polyvinyl butyral is 18.5 wt% of the weight of the dried slurry after the secondary wet grinding;
s6, forming, namely putting the particles obtained in the step S5 into a mold for pressing, maintaining the pressure at 25MPa for 2min for forming, and pressing into a sample of a circular magnetic ring, wherein the sample has the outer diameter of 16mm, the inner diameter of 8mm and the height of 4 mm;
s7, sintering, namely sintering the circular magnetic ring obtained in the step S6 in a box type sintering furnace, wherein the sintering specifically comprises the following steps: raising the temperature from room temperature to 560 ℃ at the speed of 1.2 ℃/min, preserving the heat at 560 ℃ for 1.2h, raising the temperature to 890 ℃ at the speed of 1.6 ℃/min, preserving the heat at 820-960 ℃ for 1.6h, raising the temperature to 980-1090 ℃ at the speed of 3.2 ℃/min, preserving the heat at 1035 ℃ for 3.2h, and cooling along with a furnace to obtain the ferrite magnetic material.
Comparative example 3
A ferrite magnetic material comprises a main component and an additive, wherein the main component comprises Fe2O3、Mo2O3、Yb2O3NiO and ZnO; based on the amount of the main component, Fe in the main component2O3Content of (3) Mo2O3Is 20 mol% of Yb2O3The content of (A) is 14 mol%, the content of NiO is 10 mol%, and the content of ZnO is 6 mol%; the additive is composed of V2O5、SiO2And CuO according toThe weight ratio is 1: 2.5: 1.5, and the additive accounts for 0.32 wt% of the total weight percentage of the whole material;
the preparation method of the ferrite magnetic material comprises the following steps:
s1, mixing, weighing Fe according to mole percentage2O3、Mo2O3、Yb2O3NiO and ZnO are put into a vibration mill for dry mixing;
wherein, the Fe2O3、Mo2O3、Yb2O3And the purities of ZnO and NiO are analytically pure, the NiO is in an approximately spherical shape, and the specific surface area is 50-60 m2The NiO is nano and has an average particle size of 75 nm;
s2, carrying out primary wet grinding, namely filling the raw materials mixed in the step S1 into a ball milling tank, adding zirconia balls and deionized water, and carrying out primary wet mixing ball milling;
wherein, the mass ratio of the raw materials to the zirconia balls to the deionized water is 1: 3: 1, and the ball milling time is 3.5 h;
s3, presintering, namely drying the slurry obtained after the primary wet grinding in the step S2, and putting the dried slurry into a sintering furnace for presintering, wherein the presintering specifically comprises the following steps: heating from room temperature to 550 ℃ at the speed of 1.2 ℃/min, preserving heat at 550 ℃ for 0.92h, heating to 910 ℃ at the speed of 1.8 ℃/min, preserving heat at 820-960 ℃ for 1.5h, and cooling along with the furnace;
s4, secondary wet grinding, namely filling the materials subjected to pre-sintering in the step S3 into a ball milling tank, and adding V in weight2O5、SiO2And CuO, adding zirconia balls and deionized water, and performing secondary wet mixing ball milling;
wherein, the raw material (material after S3 pre-burning + V by weight)2O5、SiO2Mixing with CuO, zirconia balls and deionized water in a mass ratio of 1: 3: 1, and ball milling for 2.5 h;
s5, granulating, namely drying the slurry subjected to secondary wet grinding in the step S4, and adding a binder for granulation;
wherein the adhesive is polyvinyl butyral, and the dosage of the polyvinyl butyral is 18.5 wt% of the weight of the dried slurry after the secondary wet grinding;
s6, forming, namely putting the particles obtained in the step S5 into a mold for pressing, maintaining the pressure at 25MPa for 2min for forming, and pressing into a sample of a circular magnetic ring, wherein the sample has the outer diameter of 16mm, the inner diameter of 8mm and the height of 4 mm;
s7, sintering, namely sintering the circular magnetic ring obtained in the step S6 in a box type sintering furnace, wherein the sintering specifically comprises the following steps: raising the temperature from room temperature to 560 ℃ at the speed of 1.2 ℃/min, preserving the heat at 560 ℃ for 1.2h, raising the temperature to 890 ℃ at the speed of 1.6 ℃/min, preserving the heat at 820-960 ℃ for 1.6h, raising the temperature to 980-1090 ℃ at the speed of 3.2 ℃/min, preserving the heat at 1035 ℃ for 3.2h, and cooling along with a furnace to obtain the ferrite magnetic material.
Comparative example 4
A ferrite magnetic material comprises a main component and an auxiliary component additive, wherein the main component comprises Fe2O3、Mo2O3、Yb2O3NiO and ZnO, the auxiliary component comprises WO3And Nd2O3(ii) a Based on the amount of the main component, Fe in the main component2O3Content of (3) Mo2O3Is 20 mol% of Yb2O3The content of (A) is 14 mol%, the content of NiO is 10 mol%, and the content of ZnO is 6 mol%; based on the weight of the main component, WO in the auxiliary component3Content of (B) 0.52 wt%, Nd2O3The content of (B) is 0.48 wt%.
The preparation method of the ferrite magnetic material comprises the following steps:
s1, mixing, weighing Fe according to mole percentage2O3、Mo2O3、Yb2O3NiO and ZnO are put into a vibration mill for dry mixing;
wherein, the Fe2O3、Mo2O3、Yb2O3And the purities of ZnO and NiO are analytically pure, the NiO is in an approximately spherical shape, and the specific surface area is 50-60 m2The NiO is nano and has an average particle size of 75 nm;
s2, carrying out primary wet grinding, namely filling the raw materials mixed in the step S1 into a ball milling tank, adding zirconia balls and deionized water, and carrying out primary wet mixing ball milling;
wherein, the mass ratio of the raw materials to the zirconia balls to the deionized water is 1: 3: 1, and the ball milling time is 3.5 h;
s3, presintering, namely drying the slurry obtained after the primary wet grinding in the step S2, and putting the dried slurry into a sintering furnace for presintering, wherein the presintering specifically comprises the following steps: heating from room temperature to 550 ℃ at the speed of 1.2 ℃/min, preserving heat at 550 ℃ for 0.92h, heating to 910 ℃ at the speed of 1.8 ℃/min, preserving heat at 820-960 ℃ for 1.5h, and cooling along with the furnace;
s4, secondary wet grinding, namely filling the materials subjected to pre-sintering in the step S3 into a ball milling tank, and adding WO by weight3、Nd2O3、V2O5、SiO2And CuO, adding zirconia balls and deionized water, and performing secondary wet mixing ball milling;
wherein, the raw materials (material after S3 pre-burning + WO by weight)3、Nd2O3) The mass ratio of the zirconia balls to the deionized water is 1: 3: 1, and the ball milling time is 2.5 h;
s5, granulating, namely drying the slurry subjected to secondary wet grinding in the step S4, and adding a binder for granulation;
wherein the adhesive is polyvinyl butyral, and the dosage of the polyvinyl butyral is 18.5 wt% of the weight of the dried slurry after the secondary wet grinding;
s6, forming, namely putting the particles obtained in the step S5 into a mold for pressing, maintaining the pressure at 25MPa for 2min for forming, and pressing into a sample of a circular magnetic ring, wherein the sample has the outer diameter of 16mm, the inner diameter of 8mm and the height of 4 mm;
s7, sintering, namely sintering the circular magnetic ring obtained in the step S6 in a box type sintering furnace, wherein the sintering specifically comprises the following steps: raising the temperature from room temperature to 560 ℃ at the speed of 1.2 ℃/min, preserving the heat at 560 ℃ for 1.2h, raising the temperature to 890 ℃ at the speed of 1.6 ℃/min, preserving the heat at 820-960 ℃ for 1.6h, raising the temperature to 980-1090 ℃ at the speed of 3.2 ℃/min, preserving the heat at 1035 ℃ for 3.2h, and cooling along with a furnace to obtain the ferrite magnetic material.
Comparative example 5
A ferrite magnetic material is provided, which comprises a ferrite core,comprises a main component and an additive, wherein the main component comprises Fe2O3、Mo2O3、Yb2O3NiO and ZnO; based on the amount of the main component, Fe in the main component2O3Content of (3) Mo2O3Is 20 mol% of Yb2O3The content of (A) is 14 mol%, the content of NiO is 10 mol%, and the content of ZnO is 6 mol%; the additive is made of SiO based on the weight of the main component2And CuO in a weight ratio of 2.5: 1.5, said additive comprising 0.32 wt% of the total weight of the entire material.
The preparation method of the ferrite magnetic material comprises the following steps:
s1, mixing, weighing Fe according to mole percentage2O3、Mo2O3、Yb2O3NiO and ZnO are put into a vibration mill for dry mixing;
wherein, the Fe2O3、Mo2O3、Yb2O3And the purities of ZnO and NiO are analytically pure, the NiO is in an approximately spherical shape, and the specific surface area is 50-60 m2The NiO is nano and has an average particle size of 75 nm;
s2, carrying out primary wet grinding, namely filling the raw materials mixed in the step S1 into a ball milling tank, adding zirconia balls and deionized water, and carrying out primary wet mixing ball milling;
wherein, the mass ratio of the raw materials to the zirconia balls to the deionized water is 1: 3: 1, and the ball milling time is 3.5 h;
s3, presintering, namely drying the slurry obtained after the primary wet grinding in the step S2, and putting the dried slurry into a sintering furnace for presintering, wherein the presintering specifically comprises the following steps: heating from room temperature to 550 ℃ at the speed of 1.2 ℃/min, preserving heat at 550 ℃ for 0.92h, heating to 910 ℃ at the speed of 1.8 ℃/min, preserving heat at 820-960 ℃ for 1.5h, and cooling along with the furnace;
s4, secondary wet grinding, namely filling the materials subjected to pre-sintering in the step S3 into a ball milling tank, and adding WO by weight3、Nd2O3、V2O5、SiO2And CuO, then adding zirconia balls and deionized water,carrying out secondary wet mixing ball milling;
wherein, the raw material (material after S3 pre-burning + SiO by weight)2Mixing with CuO, zirconia balls and deionized water in a mass ratio of 1: 3: 1, and ball milling for 2.5 h;
s5, granulating, namely drying the slurry subjected to secondary wet grinding in the step S4, and adding a binder for granulation;
wherein the adhesive is polyvinyl butyral, and the dosage of the polyvinyl butyral is 18.5 wt% of the weight of the dried slurry after the secondary wet grinding;
s6, forming, namely putting the particles obtained in the step S5 into a mold for pressing, maintaining the pressure at 25MPa for 2min for forming, and pressing into a sample of a circular magnetic ring, wherein the sample has the outer diameter of 16mm, the inner diameter of 8mm and the height of 4 mm;
s7, sintering, namely sintering the circular magnetic ring obtained in the step S6 in a box type sintering furnace, wherein the sintering specifically comprises the following steps: raising the temperature from room temperature to 560 ℃ at the speed of 1.2 ℃/min, preserving the heat at 560 ℃ for 1.2h, raising the temperature to 890 ℃ at the speed of 1.6 ℃/min, preserving the heat at 820-960 ℃ for 1.6h, raising the temperature to 980-1090 ℃ at the speed of 3.2 ℃/min, preserving the heat at 1035 ℃ for 3.2h, and cooling along with a furnace to obtain the ferrite magnetic material.
Test example 1
The sintered circular magnetic ring is regarded as a single-turn coil, the inductance of the circular coil can be obtained by measuring the impedance of the coil, then the magnetic conductivity of the sample is calculated, an E4991 impedance analyzer and a special measuring clamp 16454A for magnetic conductivity are adopted to test the complex magnetic conductivity value mu 'and the magnetic loss value mu' of the material under the frequency of 13.56MHz, and the quality factor Q value can be obtained, and the electrical property result is shown in the following table 1.
TABLE 1 results of electrical tests of examples 1 to 3 and comparative examples 1 to 5
Figure BDA0002808819660000121
As can be seen from comparison of examples 1 to 3 of Table 1 above with comparative example 1, without the ferrite material made by doping with Mo, Yb, W, Nd, V, Si and Cu elements at specific contents,the high-frequency characteristic is poor, mu' under 13.56MHz reaches more than 12, and the loss is very large; as can be seen from comparison of examples 1-3 with comparative example 2, the ferrite material prepared without doping Mo and Yb with specific contents has larger magnetic loss, so that the invention uses Mo in the main formula3+And Yb3+The doping of (A) can promote Fe2+Formation of ions, more Fe2+The iron-passing formula has smaller hysteresis aftereffect loss, and the introduced excessive positive charges can realize the balance of electrovalence by reducing the equivalent amount of positively charged oxygen vacancies existing in the system, so that the lattice distortion of the system is favorably reduced; as can be seen from comparison between examples 1-3 and comparative example 3, the ferrite material prepared without doping W, Nd element with specific content has reduced magnetic permeability and increased magnetic loss, and is caused by increased material loss due to material lattice strain, small lattice constant, domain wall movement, and low cut-off frequency, and at the same time, higher saturated magnetostriction constant λ S and magnetic anisotropy constant K1; the invention adds W6+Solid solution is carried out in crystal grains, and lattice strain is reduced, so that the saturated magnetostriction constant lambda S and the magnetic anisotropy constant K1 are reduced, the magnetic permeability is improved, and the increase of material loss is inhibited; nd (neodymium)2O3The lattice constant can be increased, the domain wall is prevented from moving, and the quality factor Q under cut-off frequency and high frequency is improved; as can be seen from comparison of examples 1 to 3 with comparative example 4, comparative example 4 is obtained without adding V2O5The sintering is not compact, and a large number of air holes exist, so that the magnetic property is influenced; comparison of examples 1-3 with comparative example 5 shows that the comparative example has no WO added3、Nd2O3、V2O5Low magnetic permeability, high magnetic loss and low Q value.
The above embodiments are merely preferred embodiments of the present invention, and any simple modification, modification and substitution changes made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.

Claims (9)

1. A ferrite magnetic material is characterized by comprising a main componentA main component, an auxiliary component and an additive, wherein the main component comprises Fe2O3、Mo2O3、Yb2O3NiO and ZnO, the auxiliary component comprises WO3And Nd2O3(ii) a Based on the amount of the main component, Fe in the main component2O3The content of (A) is 48-52 mol%, Mo2O3Is 16 to 24 mol% of Yb2O3The content of the NiO is 12-20 mol%, the content of the NiO is 9-15 mol%, and the content of the ZnO is 6-10 mol%; based on the weight of the main component, WO in the auxiliary component3In an amount of 0.1 to 1 wt%, Nd2O3The content of (A) is 0.1-1 wt%; the additive is composed of V2O5、SiO2And CuO according to the weight ratio of 1: 2-3: 1-2, wherein the additive accounts for 0.1-0.6 wt% of the total weight of the whole material.
2. The method of claim 1, comprising the steps of:
s1, mixing, weighing Fe according to mole percentage2O3、Mo2O3、Yb2O3NiO and ZnO are put into a vibration mill for dry mixing;
s2, carrying out primary wet grinding, namely filling the raw materials mixed in the step S1 into a ball milling tank, adding zirconia balls and deionized water, and carrying out primary wet mixing ball milling;
s3, presintering, namely drying the slurry obtained after primary wet grinding in the step S2, and putting the slurry into a sintering furnace for presintering, wherein the presintering temperature is 820-960 ℃, and the heat preservation time is 1.8-2.6 hours;
s4, secondary wet grinding, namely filling the materials subjected to pre-sintering in the step S3 into a ball milling tank, and adding WO by weight3、Nd2O3、V2O5、SiO2And CuO, adding zirconia balls and deionized water, and performing secondary wet mixing ball milling;
s5, granulating, namely drying the slurry subjected to secondary wet grinding in the step S4, and adding a binder for granulation;
s6, forming, namely putting the particles obtained in the step S5 into a mold for pressing, and pressing into a sample of a circular magnetic ring, wherein the sample has an outer diameter of 14-18 mm, an inner diameter of 6-10 mm and a height of 3-5 mm;
s7, sintering, namely sintering the circular magnetic ring obtained in the step S6 in a box type sintering furnace, wherein the sintering temperature is 980-1090 ℃, and the heat preservation time is 3-6 hours, so that the ferrite magnetic material is obtained.
3. The method as claimed in claim 2, wherein in step S1, the Fe is added2O3、Mo2O3、Yb2O3And the purity of ZnO were all analytically pure.
4. The method for preparing a ferrite magnetic material as claimed in claim 2, wherein in step S1, said NiO is in the form of nearly spherical shape with a specific surface area of 50-60 m2The NiO is nano and has an average particle size of 50-100 nm.
5. The method for preparing a ferrite magnetic material according to claim 2, wherein in step S2, the mass ratio of the raw materials, the zirconia balls and the deionized water is 1: 2-4: 0.5-1.5, and the ball milling time is 1-24 hours.
6. The method for preparing a ferrite magnetic material according to claim 2, wherein the pre-sintering specifically comprises, in step S3: heating from room temperature to 520-580 ℃ at the speed of 1.2 ℃/min, preserving heat at 520-580 ℃ for 0.8-1 h, heating to 820-960 ℃ at the speed of 1.8 ℃/min, preserving heat at 820-960 ℃ for 1-2 h, and cooling along with a furnace.
7. The method for preparing a ferrite magnetic material according to claim 2, wherein in step S4, the mass ratio of the raw materials, the zirconia balls and the deionized water is 1: 2-4: 0.5-1.5, and the ball milling time is 1-24 hours.
8. The method as claimed in claim 2, wherein in step S5, the binder is polyvinyl butyral, and the amount of polyvinyl butyral is 12-25 wt% of the weight of the dried slurry after the second wet grinding.
9. The method as claimed in claim 2, wherein the sintering step S7 includes: heating from room temperature to 520-580 ℃ at the speed of 1.2 ℃/min, preserving heat at 520-580 ℃ for 1-1.5 h, heating to 820-960 ℃ at the speed of 1.6 ℃/min, preserving heat at 820-960 ℃ for 1.5-2 h, heating to 980-1090 ℃ at the speed of 3.2 ℃/min, preserving heat at 980-1090 ℃ for 2.5-4 h, and cooling along with a furnace.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113735573A (en) * 2021-08-27 2021-12-03 西安交通大学 Low-loss NiCuZn soft magnetic ferrite material for NFC and preparation method and application thereof
CN114005669A (en) * 2021-10-28 2022-02-01 江西尚朋电子科技有限公司 Process for manufacturing special-shaped ferrite magnetic core

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113735573A (en) * 2021-08-27 2021-12-03 西安交通大学 Low-loss NiCuZn soft magnetic ferrite material for NFC and preparation method and application thereof
CN114005669A (en) * 2021-10-28 2022-02-01 江西尚朋电子科技有限公司 Process for manufacturing special-shaped ferrite magnetic core

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