A nickel-zinc ferrite material, its preparation method and application

By adding cobalt trioxide and aluminum dihydrogen phosphate to nickel-zinc ferrite materials, the magnetocrystalline anisotropy, resistivity and mechanical strength are adjusted, solving the problems of unstable magnetic permeability and high magnetic loss of existing nickel-zinc ferrite materials at high frequencies. High-frequency, wide-bandwidth, low-loss and high-reliability nickel-zinc ferrite materials suitable for 5G communication and new energy vehicles are prepared.

CN120329025BActive Publication Date: 2025-11-14广东泛瑞新材料股份有限公司
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Patent Information

Application Number
CN202510481409.8
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-04-17
Publication Date
2025-11-14
Estimated Expiration
2045-04-17

AI Technical Summary

Technical Problem

Existing nickel-zinc ferrite materials suffer from unstable magnetic permeability, high magnetic loss, low reliability, narrow operating temperature range, low density, weak mechanical strength, and large magnetostriction coefficient at high frequencies, which cannot meet the application requirements of fields such as 5G communication and new energy vehicles.

Method used

By adding cobalt trioxide and aluminum dihydrogen phosphate to nickel-zinc ferrite materials, the anisotropy of the magnetic crystal is adjusted, the resistivity is increased, the microstructure is improved, the operating temperature range is widened, and the mechanical strength is enhanced. With appropriate sintering processes and molding methods, high-frequency, wide-bandwidth, low-loss, and highly reliable nickel-zinc ferrite materials can be prepared.

Benefits of technology

The method achieves stable magnetic permeability, low magnetic loss, high reliability, wide operating temperature range, high density, and high mechanical strength of nickel-zinc ferrite materials at high frequencies, meeting the performance requirements of 5G communication and new energy vehicles. Moreover, the preparation method is simple and low-cost, making it suitable for large-scale production.

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Abstract

This invention discloses a nickel-zinc ferrite material, its preparation method, and its applications. The preparation method of the nickel-zinc ferrite material of this invention includes the following steps: 1) preparing Fe2O3, NiO, ZnO, and CuO as the main material, and preparing Fe2O3, NiO, and CuO as the black material; 2) preparing nickel-zinc ferrite particles from the main material, black material, Co2O3, and Al(H2PO4)3; 3) mixing the nickel-zinc ferrite particles and zinc stearate evenly, followed by sieving, pressing, and sintering. The nickel-zinc ferrite material of this invention has advantages such as high frequency, wide bandwidth, high impedance, low loss, high reliability, wide operating temperature range, high density, high mechanical strength, and low magnetostriction coefficient, fully meeting the performance requirements for applications in 5G communication, new energy vehicles, and other fields. Furthermore, its preparation method is simple, and its production cost is low, making it suitable for large-scale industrial production and application.
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Description

Technical Field

[0001] This invention relates to the field of soft magnetic materials technology, specifically to a nickel-zinc ferrite material, its preparation method, and its application. Background Technology

[0002] Nickel-zinc ferrite is an important soft magnetic material with advantages such as high frequency, wide bandwidth, high impedance, and low loss, and is widely used in high-frequency electronic devices. In recent years, with the rapid development of 5G communication, new energy vehicles, and other fields, the performance requirements for nickel-zinc ferrite have become increasingly stringent. However, existing nickel-zinc ferrites generally suffer from problems such as unstable permeability at high frequencies, high magnetic losses (e.g., eddy current losses and hysteresis losses), low reliability at high temperatures, narrow operating temperature range, low density, low mechanical strength, and large magnetostriction coefficient. These issues make it impossible to fully meet the growing practical application requirements, thus greatly limiting its application.

[0003] Therefore, it is of great significance to develop a nickel-zinc ferrite material with high frequency, wide bandwidth, high impedance, low loss, high reliability, wide operating temperature range, high density, high mechanical strength, and low magnetostriction coefficient.

[0004] The above statements are merely background information related to the present invention and do not necessarily constitute prior art. Summary of the Invention

[0005] The purpose of this invention is to provide a nickel-zinc ferrite material, its preparation method, and its application.

[0006] The technical solution adopted in this invention is:

[0007] A method for preparing a nickel-zinc ferrite material includes the following steps:

[0008] 1) Preparation of main material and black material:

[0009] Preparation of main materials: Fe2O3, NiO, ZnO and CuO are added to a vibratory mill for grinding, then pressed into blocks, then calcined, and then crushed to obtain the main materials;

[0010] Preparation of black material: Fe2O3, NiO and CuO are added to a vibratory mill for grinding, then pressed into blocks, then calcined, and then crushed to obtain black material;

[0011] 2) Preparation of nickel-zinc ferrite particles: The main material, black material, Co2O3, Al(H2PO4)3, dispersant and water are added to a sand mill for sand milling, then polyvinyl alcohol is added and mixed evenly, and then spray granulation is performed to obtain nickel-zinc ferrite particles.

[0012] 3) Molding and sintering: Mix nickel-zinc ferrite particles and zinc stearate evenly, then sieve, press into shape, and then sinter to obtain nickel-zinc ferrite material.

[0013] Preferably, the main material in step 1) comprises the following components in molar percentage:

[0014] Fe2O3: 47.5%–49.5%;

[0015] NiO: 19%–24%;

[0016] ZnO: 19%–25%;

[0017] CuO: 5%–8%.

[0018] Preferably, the black material in step 1) comprises the following components in molar percentage:

[0019] Fe2O3: 48%–53%;

[0020] NiO: 40%–45%;

[0021] CuO: 5%–8%.

[0022] Preferably, the pressing in step 1) is carried out under a pressure of 1MPa to 3MPa and a holding time of 1s to 5s.

[0023] Preferably, the calcination in step 1) is carried out at a temperature of 900℃ to 1000℃ for 2 hours to 5 hours.

[0024] Preferably, the particle size of the main material in step 1) is 1μm to 5μm.

[0025] Preferably, the particle size of the black material in step 1) is 1μm to 5μm.

[0026] Preferably, the mass ratio of the main material to the black material in step 2) is 1:0.05 to 0.12.

[0027] Preferably, the amount of Co2O3 used in step 2) is 1.0% to 1.5% of the total weight of the main material and the black material.

[0028] Preferably, the amount of Al(H2PO4)3 used in step 2) is 0.15% to 0.25% of the total weight of the main material and the black material.

[0029] Preferably, the amount of dispersant used in step 2) is 0.15% to 0.25% of the total weight of the main material and the black material.

[0030] Preferably, the dispersant in step 2) is fatty alcohol polyoxyethylene ether methylsilane.

[0031] More preferably, the dispersant in step 2) is Solverodia's wetting and dispersing agent WA-40 (the main component of which is fatty alcohol polyoxyethylene ether methylsilane).

[0032] Preferably, the target particle size of the grinding in step 2) is D. 50 = 0.95μm ± 0.05μm.

[0033] Preferably, the amount of polyvinyl alcohol used in step 2) is 0.8% to 1.2% of the total weight of the main material and the black material.

[0034] Preferably, the number-average molecular weight of the polyvinyl alcohol in step 2) is 1500 g / mol to 2000 g / mol.

[0035] Preferably, the process parameters for spray granulation in step 2) include: the inlet temperature of the spray granulator is 210℃~230℃, and the outlet temperature is 100℃~120℃.

[0036] Preferably, the particle size of the nickel-zinc ferrite particles in step 2) is 48μm to 180μm.

[0037] Preferably, the mass ratio of nickel-zinc ferrite particles to zinc stearate in step 3) is 1:0.001 to 0.003.

[0038] Preferably, the sieve used in step 3) has a mesh size of 80 to 250.

[0039] Preferably, the pressing in step 3) is carried out under a pressure of 15MPa to 30MPa and a holding time of 2s to 3s.

[0040] Preferably, the sintering in step 3) is carried out at a temperature of 1080℃~1100℃ for a time of 12h~16h.

[0041] A nickel-zinc ferrite material, which is prepared by the above-described method.

[0042] Application of a nickel-zinc ferrite material as described above in the fields of 5G communication or new energy vehicles.

[0043] The beneficial effects of this invention are: the nickel-zinc ferrite material of this invention has the advantages of high frequency, wide bandwidth, high impedance, low loss, high reliability, wide operating temperature range, high density, high mechanical strength, and small magnetostriction coefficient, which fully meet the performance requirements for applications in 5G communication, new energy vehicles and other fields. Moreover, its preparation method is simple and the production cost is low, making it suitable for large-scale industrial production and application.

[0044] Specifically:

[0045] 1) This invention achieves the following effects by adding cobalt trioxide (Co2O3) to nickel-zinc ferrite materials:

[0046] a) Adjusting the anisotropy of the magnetocrystalline material: Cobalt ions (Co 2+ / Co 3+ Entering the ferrite spinel lattice will replace some of the Fe. 3+ or Ni 2+ This can change the lattice parameters and the anisotropy constant of the magnetocrystalline material. Adding an appropriate amount of cobalt ions can reduce the anisotropy of the magnetocrystalline material, making the permeability of the nickel-zinc ferrite material more stable at high frequencies, reducing magnetic losses (eddy current losses and hysteresis losses), and improving the high-frequency performance of the nickel-zinc ferrite material.

[0047] b) Increase resistivity: Cobalt ion doping can suppress Fe 2+ The formation of (Fe) 2+ This increases electron hopping conductivity, thereby improving the resistivity of nickel-zinc ferrite materials and reducing eddy current losses in high-frequency applications, which is crucial for the efficiency of high-frequency transformers, inductors, and other devices.

[0048] c) Improved temperature stability: The addition of cobalt ions can regulate the Curie temperature (T) of nickel-zinc ferrite materials. c This expands the operating temperature range of nickel-zinc ferrite materials. Furthermore, by suppressing the change in permeability with temperature, it enhances the reliability of nickel-zinc ferrite materials in high-temperature environments. In addition, cobalt trioxide not only freezes domain walls and increases the cutoff frequency of nickel-zinc ferrite materials, but also reduces the temperature coefficient, allowing the nickel-zinc ferrite material to maintain its initial permeability (μ) over a wider temperature range. i The stability of the Q value;

[0049] d) Optimizing the microstructure: During sintering, cobalt trioxide can act as a flux to promote uniform grain growth and reduce porosity, thereby improving the density and mechanical strength of nickel-zinc ferrite materials. Furthermore, the uniform grain structure helps reduce the coercivity (H) of nickel-zinc ferrite materials. c This can improve the soft magnetic properties of nickel-zinc ferrite materials;

[0050] e) Suppressing magnetostriction effect: The addition of cobalt ions can reduce the magnetostriction coefficient (λ) of nickel-zinc ferrite materials, which can reduce vibration noise under alternating magnetic fields and is suitable for high-frequency electronic devices that are sensitive to noise.

[0051] f) Increase saturation magnetization: Cobalt ions have a higher ionic magnetic moment (Co 2+ The magnetic moment is 3 μB. Appropriate doping can increase the saturation magnetization (M) of nickel-zinc ferrite materials. s );

[0052] 2) This invention achieves the following effects by adding aluminum dihydrogen phosphate (Al(H2PO4)3) during the preparation of nickel-zinc ferrite materials:

[0053] a) Fluxing: Aluminum dihydrogen phosphate decomposes into active phosphate at high temperatures, which can reduce the surface energy of ferrite particles, promote grain boundary migration and interparticle diffusion, thereby significantly reducing the sintering temperature and saving energy. In addition, the decomposition products of aluminum dihydrogen phosphate can form a low-melting-point liquid phase at the grain boundary through the liquid phase sintering mechanism to fill the pores, thereby improving the density of nickel-zinc ferrite materials and reducing the negative impact of pores on the magnetic properties of nickel-zinc ferrite materials.

[0054] b) Improve mechanical properties: Aluminum dihydrogen phosphate decomposes into active phosphate at high temperatures. During the cooling process, the phosphate forms a glassy phase covering the grain boundaries, which can improve the bending strength and hardness of nickel-zinc ferrite materials and reduce the risk of brittle fracture. In addition, the viscous liquid phase formed by phosphate during the molding stage helps the bonding between particles, which can improve the strength of the green blank and reduce the processing breakage rate.

[0055] c) Improve magnetic properties: Aluminum dihydrogen phosphate can suppress abnormal grain growth, make the grain distribution more uniform, reduce the domain wall movement resistance, improve the permeability of nickel-zinc ferrite materials, and the dense structure and uniform grain boundaries reduce the eddy current loss of nickel-zinc ferrite materials in high-frequency applications, which can significantly reduce the core loss per unit volume (PCV).

[0056] d) Improved electrical properties: Aluminum dihydrogen phosphate decomposes into active phosphate at high temperatures. During cooling, the phosphate forms a glassy phase, blocking the direct conductive path between grains. This can increase the resistivity of nickel-zinc ferrite materials by approximately 12 orders of magnitude, further suppressing high-frequency eddy current losses. Furthermore, the appropriate addition of aluminum dihydrogen phosphate can adjust the dielectric constant of nickel-zinc ferrite materials and reduce their remanence (B). r ) and coercivity (H c This allows for matching specific high-frequency circuit requirements;

[0057] 3) Through the synergistic effect of cobalt trioxide and aluminum dihydrogen phosphate, this invention can not only significantly improve the resistivity, density, mechanical strength and magnetic properties of nickel-zinc ferrite materials, but also greatly reduce the magnetic loss of nickel-zinc ferrite materials.

[0058] 4) The nickel-zinc ferrite material of the present invention has the advantages of high frequency, wide bandwidth, high impedance, low loss, high reliability, wide operating temperature range, high density, high mechanical strength and small magnetostriction coefficient, which fully meet the performance requirements for applications in 5G communication, new energy vehicles and other fields.

[0059] 5) The preparation method of the nickel-zinc ferrite material of the present invention is simple and has low production cost, making it suitable for large-scale industrial production and application. Detailed Implementation

[0060] The present invention will be further explained and described below with reference to specific embodiments.

[0061] Example 1:

[0062] A nickel-zinc ferrite material, the preparation method of which is as follows:

[0063] 1) Preparation of main material and black material:

[0064] Preparation of main materials: 6622g of Fe2O3, 1306g of NiO, 1636g of ZnO and 436g of CuO were added to a vibratory mill and ground for 1 hour. Then, the mixture was placed into a sagger with dimensions of 320mm×280mm×120mm and pressed under a pressure of 3MPa for 3 seconds to form a block. The block was then calcined in a muffle furnace at 950℃ for 3 hours. After coarse crushing, the block was further crushed using a vibratory mill to obtain the main material (particle size 1.7μm~3.0μm; molar percentage of each component in the main material: Fe2O3: 49%; NiO: 20.7%; ZnO: 23.8%; CuO: 6.5%; mass percentage of each component in the main material: Fe2O3: 66.22%; NiO: 13.06%; ZnO: 16.36%; CuO: 4.36%).

[0065] Preparation of black material: 6976g of Fe2O3, 2632g of NiO, and 392g of CuO were added to a vibratory mill and ground for 1 hour. The mixture was then placed into a sagger with dimensions of 320mm×280mm×120mm, and a pressure of 3MPa was applied and held for 3 seconds to form a block. The block was then calcined in a muffle furnace at 950℃ for 3 hours. After coarse crushing, the block was further crushed using a crusher and then pulverized a second time using a vibratory mill to obtain black material (particle size 1.7μm~3.0μm; molar percentage of each component in the black material: Fe2O3: 52.05%; NiO: 42.07%; CuO: 5.88%; mass percentage of each component in the black material: Fe2O3: 69.76%; NiO: 26.32%; CuO: 3.92%).

[0066] 2) Preparation of nickel-zinc ferrite particles: 8000g of main material, 800g of black material, 105.6g of Co2O3, 17.6g of Al(H2PO4)3, 17.6g of wetting and dispersing agent WA-40, and 4300g of water were added to a high-speed sand mill and milled for 2 hours. The target particle size was D. 50=0.95μm±0.05μm, then add 88g of polyvinyl alcohol (number average molecular weight of 1799g / mol) and stir evenly, then add to a spray granulator for spray granulation. The inlet temperature of the spray granulator is 220℃ and the outlet temperature is 110℃ to obtain nickel-zinc ferrite particles (particle size of 48μm~180μm).

[0067] 3) Molding and sintering: Nickel-zinc ferrite particles and zinc stearate are mixed evenly at a mass ratio of 1:0.001, then passed through an 80-mesh sieve, and then poured into a ring mold with an outer diameter of 25 mm, an inner diameter of 15 mm, and a depth of 6 mm. A pressure of 15 MPa is applied and held for 2 seconds to form a billet. Then, it is placed in a tunnel furnace at 1090℃±10℃ for 14 hours to obtain nickel-zinc ferrite material (magnetic ring).

[0068] Example 2:

[0069] A nickel-zinc ferrite material, the preparation method of which is as follows:

[0070] 1) Preparation of nickel-zinc ferrite particles: 8000g of main material (same as in Example 1), 480g of black material (same as in Example 1), 101.8g of Co2O3, 17g of Al(H2PO4)3, 17g of wetting and dispersing agent WA-40, and 4300g of water were added to a high-speed sand mill and milled for 2 hours. The target particle size was D. 50 =0.95μm±0.05μm, then add 84.8g of polyvinyl alcohol (number average molecular weight of 1799g / mol) and stir evenly, then add to a spray granulator for spray granulation. The inlet temperature of the spray granulator is 220℃ and the outlet temperature is 110℃ to obtain nickel-zinc ferrite particles (particle size of 48μm~180μm);

[0071] 2) Molding and sintering: Nickel-zinc ferrite particles and zinc stearate are mixed evenly at a mass ratio of 1:0.001, then passed through an 80-mesh sieve, and then poured into a ring mold with an outer diameter of 25 mm, an inner diameter of 15 mm, and a depth of 6 mm. A pressure of 15 MPa is applied and held for 2 seconds to form a billet. Then it is placed in a tunnel furnace at 1090℃±10℃ for 14 hours to obtain nickel-zinc ferrite material (magnetic ring).

[0072] Example 3:

[0073] A nickel-zinc ferrite material, the preparation method of which is as follows:

[0074] 1) Preparation of main material: 6620g of Fe2O3, 1280g of NiO, 1700g of ZnO and 400g of CuO were added to a vibratory mill and ground for 1 hour. Then, the mixture was placed into a sagger with dimensions of 320mm×280mm×120mm and pressed under a pressure of 3MPa for 3 seconds to form a block. The block was then calcined in a muffle furnace at 950℃ for 3 hours. After coarse crushing, the block was further crushed using a vibratory mill to obtain the main material (particle size 1.7μm~3.0μm; molar percentage of each component in the main material: Fe2O3: 49%; NiO: 20.3%; ZnO: 24.7%; CuO: 6%; mass percentage of each component in the main material: Fe2O3: 66.2%; NiO: 12.8%; ZnO: 17%; CuO: 4%).

[0075] 2) Preparation of nickel-zinc ferrite particles: 8000g of main material, 560g of black material (same as in Example 1), 102.7g of Co2O3, 17g of Al(H2PO4)3, 17g of wetting and dispersing agent WA-40, and 4300g of water were added to a high-speed sand mill and milled for 2 hours. The target particle size was D. 50 =0.95μm±0.05μm, then add 85.6g of polyvinyl alcohol (number average molecular weight of 1799g / mol) and stir evenly, then add to a spray granulator for spray granulation. The inlet temperature of the spray granulator is 220℃ and the outlet temperature is 110℃ to obtain nickel-zinc ferrite particles (particle size of 48μm~180μm);

[0076] 3) Molding and sintering: Nickel-zinc ferrite particles and zinc stearate are mixed evenly at a mass ratio of 1:0.001, then passed through an 80-mesh sieve, and then poured into a ring mold with an outer diameter of 25 mm, an inner diameter of 15 mm, and a depth of 6 mm. A pressure of 15 MPa is applied and held for 2 seconds to form a billet. Then, it is placed in a tunnel furnace at 1090℃±10℃ for 14 hours to obtain nickel-zinc ferrite material (magnetic ring).

[0077] Comparative Example 1 (without Co2O3 and Al(H2PO4)3):

[0078] A nickel-zinc ferrite material, the preparation method of which is as follows:

[0079] 1) Preparation of main material: 6577g of Fe2O3, 2301g of NiO, 699g of ZnO and 423g of CuO were added to a vibratory mill and ground for 1 hour. Then, the mixture was placed into a sagger with dimensions of 320mm×280mm×120mm and pressed under a pressure of 3MPa for 3 seconds to form a block. The block was then calcined in a muffle furnace at 950℃ for 3 hours. After coarse crushing, the block was further crushed using a vibratory mill to obtain the main material (particle size 1.7μm~3.0μm; molar percentage of each component in the main material: Fe2O3: 47.9%; NiO: 35.9%; ZnO: 10%; CuO: 6.2%; mass percentage of each component in the main material: Fe2O3: 65.77%; NiO: 23.01%; ZnO: 6.99%; CuO: 4.23%).

[0080] 2) Preparation of nickel-zinc ferrite particles: 8000g of the main material, 17g of wetting and dispersing agent WA-40, and 4000g of water were added to a high-speed sand mill and milled for 2 hours. The target particle size was D. 50 =0.95μm±0.05μm, then add 80g of polyvinyl alcohol (number average molecular weight of 1799g / mol) and stir evenly, then add to a spray granulator for spray granulation. The inlet temperature of the spray granulator is 220℃ and the outlet temperature is 110℃ to obtain nickel-zinc ferrite particles (particle size of 48μm~180μm).

[0081] 3) Molding and sintering: Nickel-zinc ferrite particles and zinc stearate are mixed evenly at a mass ratio of 1:0.001, then passed through an 80-mesh sieve, and then poured into a ring mold with an outer diameter of 25 mm, an inner diameter of 15 mm, and a depth of 6 mm. A pressure of 15 MPa is applied and held for 2 seconds to form a billet. Then, it is placed in a tunnel furnace at 1090℃±10℃ for 14 hours to obtain nickel-zinc ferrite material (magnetic ring).

[0082] Comparative Example 2 (without Al(H2PO4)3):

[0083] A nickel-zinc ferrite material, the preparation method of which is as follows:

[0084] 1) Preparation of nickel-zinc ferrite particles: 8000g of main material (same as in Example 1), 560g of black material (same as in Example 1), 102.72g of Co2O3, 17g of wetting and dispersing agent WA-40, and 4300g of water were added to a high-speed sand mill and milled for 2 hours. The target particle size was D. 50=0.95μm±0.05μm, then add 85.6g of polyvinyl alcohol (number average molecular weight of 1799g / mol) and stir evenly, then add to a spray granulator for spray granulation. The inlet temperature of the spray granulator is 220℃ and the outlet temperature is 110℃ to obtain nickel-zinc ferrite particles (particle size of 48μm~180μm);

[0085] 2) Molding and sintering: Nickel-zinc ferrite particles and zinc stearate are mixed evenly at a mass ratio of 1:0.001, then passed through an 80-mesh sieve, and then poured into a ring mold with an outer diameter of 25 mm, an inner diameter of 15 mm, and a depth of 6 mm. A pressure of 15 MPa is applied and held for 2 seconds to form a billet. Then it is placed in a tunnel furnace at 1090℃±10℃ for 14 hours to obtain nickel-zinc ferrite material (magnetic ring).

[0086] Comparative Example 3 (without Co2O3):

[0087] A nickel-zinc ferrite material, the preparation method of which is as follows:

[0088] 1) Preparation of nickel-zinc ferrite particles: 8000g of the main material (same as Comparative Example 1), 16g of Al(H2PO4)3, 17g of wetting and dispersing agent WA-40, and 4300g of water were added to a high-speed sand mill and milled for 2 hours. The target particle size was D. 50 =0.95μm±0.05μm, then add 80g of polyvinyl alcohol (number average molecular weight of 1799g / mol) and stir evenly, then add to a spray granulator for spray granulation. The inlet temperature of the spray granulator is 220℃ and the outlet temperature is 110℃ to obtain nickel-zinc ferrite particles (particle size of 48μm~180μm).

[0089] 2) Molding and sintering: Nickel-zinc ferrite particles and zinc stearate are mixed evenly at a mass ratio of 1:0.001, then passed through an 80-mesh sieve, and then poured into a ring mold with an outer diameter of 25 mm, an inner diameter of 15 mm, and a depth of 6 mm. A pressure of 15 MPa is applied and held for 2 seconds to form a billet. Then it is placed in a tunnel furnace at 1090℃±10℃ for 14 hours to obtain nickel-zinc ferrite material (magnetic ring).

[0090] Comparative Example 4 (Insufficient Co2O3):

[0091] A nickel-zinc ferrite material, the preparation method of which is as follows:

[0092] 1) Preparation of nickel-zinc ferrite particles: 8000g of main material (same as in Example 1), 960g of black material (same as in Example 1), 44.8g of Co2O3, 18g of Al(H2PO4)3, 17g of wetting and dispersing agent WA-40, and 4300g of water were added to a high-speed sand mill and milled for 2 hours. The target particle size was D. 50=0.95μm±0.05μm, then add 89.6g of polyvinyl alcohol (number average molecular weight of 1799g / mol) and stir evenly, then add to a spray granulator for spray granulation. The inlet temperature of the spray granulator is 220℃ and the outlet temperature is 110℃ to obtain nickel-zinc ferrite particles (particle size of 48μm~180μm).

[0093] 2) Molding and sintering: Nickel-zinc ferrite particles and zinc stearate are mixed evenly at a mass ratio of 1:0.001, then passed through an 80-mesh sieve, and then poured into a ring mold with an outer diameter of 25 mm, an inner diameter of 15 mm, and a depth of 6 mm. A pressure of 15 MPa is applied and held for 2 seconds to form a billet. Then it is placed in a tunnel furnace at 1090℃±10℃ for 14 hours to obtain nickel-zinc ferrite material (magnetic ring).

[0094] Comparative Example 5 (Insufficient Al(H2PO4)3):

[0095] A nickel-zinc ferrite material, the preparation method of which is as follows:

[0096] 1) Preparation of nickel-zinc ferrite particles: 8000g of main material (same as in Example 1), 560g of black material (same as in Example 1), 102.7g of Co2O3, 8.6g of Al(H2PO4)3, 17.6g of wetting and dispersing agent WA-40, and 4300g of water were added to a high-speed sand mill and milled for 2 hours. The target particle size was D. 50 =0.95μm±0.05μm, then add 85.6g of polyvinyl alcohol (number average molecular weight of 1799g / mol) and stir evenly, then add to a spray granulator for spray granulation. The inlet temperature of the spray granulator is 220℃ and the outlet temperature is 110℃ to obtain nickel-zinc ferrite particles (particle size of 48μm~180μm);

[0097] 2) Molding and sintering: Nickel-zinc ferrite particles and zinc stearate are mixed evenly at a mass ratio of 1:0.001, then passed through an 80-mesh sieve, and then poured into a ring mold with an outer diameter of 25 mm, an inner diameter of 15 mm, and a depth of 6 mm. A pressure of 15 MPa is applied and held for 2 seconds to form a billet. Then it is placed in a tunnel furnace at 1090℃±10℃ for 14 hours to obtain nickel-zinc ferrite material (magnetic ring).

[0098] Performance testing:

[0099] The performance of the nickel-zinc ferrite materials (magnetic rings) in Examples 1-3 and Comparative Examples 1-5 was tested using an LCR meter, a BH meter, and a SY-8218 power consumption meter. The test data are as follows:

[0100] Table 1. Basic properties and BH test data of nickel-zinc ferrite materials in Examples 1-3

[0101]

[0102] Table 2 shows the PCV, resonant frequency, and T of the nickel-zinc ferrite materials in Examples 1-3. c Test data

[0103]

[0104] Table 3 shows the basic properties and BH test data of the nickel-zinc ferrite materials in Comparative Examples 1–5.

[0105]

[0106]

[0107] Table 4 shows the PCV, resonant frequency, and T of the nickel-zinc ferrite materials in Examples 1-5. c Test data

[0108]

[0109] As can be seen from Tables 1-4:

[0110] a) Compared with the nickel-zinc ferrite material in Comparative Example 1 (without Co2O3 and Al(H2PO4)3), the nickel-zinc ferrite materials in Examples 1-4 showed significantly improved resistivity (R), significantly better magnetic properties, and significantly reduced core loss per unit volume (PCV). This indicates that the synergistic effect of cobalt trioxide and aluminum dihydrogen phosphate can not only significantly improve the resistivity, density, mechanical strength, and magnetic properties of nickel-zinc ferrite materials, but also significantly reduce the magnetic loss of nickel-zinc ferrite materials.

[0111] b) Compared with the nickel-zinc ferrite material in Comparative Example 2 (without Al(H2PO4)3), the resistivity (R) of the nickel-zinc ferrite material in Example 1 is significantly increased and the core loss per unit volume (PCV) is significantly reduced. This shows that Al(H2PO4)3 can not only significantly improve the resistivity and mechanical strength of nickel-zinc ferrite materials, but also significantly reduce the magnetic loss of nickel-zinc ferrite materials.

[0112] c) Compared with the nickel-zinc ferrite material in Comparative Example 3 (without Co2O3), the nickel-zinc ferrite material in Example 1 has a significantly higher resistivity (R), significantly better magnetic properties, and a significantly lower core loss per unit volume (PCV). This indicates that cobalt trioxide can not only significantly improve the resistivity, density, mechanical strength, and magnetic properties of nickel-zinc ferrite materials, but also significantly reduce the magnetic loss of nickel-zinc ferrite materials.

[0113] d) The nickel-zinc ferrite material in Example 1 has a significantly higher resonant frequency compared to the nickel-zinc ferrite material in Comparative Example 4 (where the amount of Co2O3 was too small), indicating that cobalt trioxide has the effect of adjusting the resonant frequency.

[0114] e) Compared with the nickel-zinc ferrite material in Comparative Example 5 (where the amount of Al(H2PO4)3 was too small), the resistivity (R) of the nickel-zinc ferrite material in Example 1 was significantly improved and the magnetic properties were significantly better, indicating that Al(H2PO4)3 can significantly improve the resistivity and magnetic properties of nickel-zinc ferrite materials.

[0115] In summary, this invention, through the synergistic effect of Co2O3 and Al(H2PO4)3, enables nickel-zinc ferrite materials to possess advantages such as high frequency, wide bandwidth, high impedance, low loss, high reliability, wide operating temperature range, high density, high mechanical strength, and low magnetostriction coefficient, fully meeting the performance requirements for applications in 5G communication, new energy vehicles, and other fields.

[0116] The above embodiments are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above embodiments. Any changes, modifications, substitutions, combinations, or simplifications made without departing from the spirit and principle of the present invention shall be considered equivalent substitutions and shall be included within the protection scope of the present invention.

Claims

1. A method for preparing a nickel-zinc ferrite material, characterized in that, Includes the following steps: 1) Preparation of main material and black material: Preparation of main materials: Fe2O3, NiO, ZnO and CuO are added to a vibratory mill for grinding, then pressed into blocks, then calcined, and then crushed to obtain the main materials; Preparation of black material: Fe2O3, NiO and CuO are added to a vibratory mill for grinding, then pressed into blocks, then calcined, and then crushed to obtain black material; 2) Preparation of nickel-zinc ferrite particles: The main material, black material, Co2O3, Al(H2PO4)3, dispersant and water are added to a sand mill for sand milling, then polyvinyl alcohol is added and mixed evenly, and then spray granulation is performed to obtain nickel-zinc ferrite particles. 3) Molding and sintering: Mix nickel-zinc ferrite particles and zinc stearate evenly, then sieve, press into shape, and then sinter to obtain nickel-zinc ferrite material. Step 1) The main material comprises the following components in molar percentage: Fe2O3: 47.5%–49.5%; NiO: 19%–24%; ZnO: 19%–25%; CuO: 5%–8%; Step 1) The black material comprises the following components in molar percentage: Fe2O3: 48%–53%; NiO: 40%–45%; CuO: 5%–8%; Step 2) The mass ratio of the main material to the black material is 1:0.05 to 0.12; Step 2) The amount of Co2O3 used is 1.0% to 1.5% of the total weight of the main material and the black material; Step 2) The amount of Al(H2PO4)3 used is 0.15% to 0.25% of the total weight of the main material and the black material; Step 2) The amount of polyvinyl alcohol used is 0.8% to 1.2% of the total weight of the main material and the black material.

2. The preparation method according to claim 1, characterized in that: Step 1) The calcination is carried out at a temperature of 900℃~1000℃ for 2h~5h.

3. The preparation method according to claim 1, characterized in that: Step 2) The amount of dispersant used is 0.15% to 0.25% of the total weight of the main material and the black material.

4. The preparation method according to claim 1 or 3, characterized in that: Step 2) The particle size of the nickel-zinc ferrite particles is 48μm to 180μm.

5. The preparation method according to claim 1, characterized in that: Step 3) The mass ratio of the nickel-zinc ferrite particles to zinc stearate is 1:0.001 to 0.

003.

6. The preparation method according to claim 1 or 5, characterized in that: Step 3) The sintering is carried out at a temperature of 1080℃~1100℃ for 12h~16h.

7. A nickel-zinc ferrite material, characterized in that, It is prepared by the preparation method described in any one of claims 1 to 6.

8. The application of the nickel-zinc ferrite material as described in claim 7 in the field of 5G communication or new energy vehicles.

Citation Information

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