Highly magnetic magnetite material and method for producing the same

Abstract

This invention relates to the field of novel magnetic materials, providing a high-magnetic magnetite (Fe3O4) material and its preparation method. The method includes: S1 Electrolyte immersion: cleaning the magnetite workpiece material and immersing it in an electrolyte for a set time; S2 Hydrogenation modification treatment: using the electrolyte-immersed magnetite workpiece material as a cathode, performing electrochemical atomic hydrogenation treatment. The atomic hydrogen generated by the cathode electrolysis reaction is adsorbed on the surface of the magnetite workpiece material and diffuses into the material's interior under the action of a concentration gradient, modifying the magnetite workpiece material; S3 Cleaning and drying. The magnetite material prepared by this invention has significantly improved saturation magnetization and coercivity, and enhanced remanent magnetization. The material maintains high magnetic induction intensity even under demagnetizing conditions, significantly improving the magnetic properties of magnetite. This invention's method is low-cost, simple, environmentally friendly, and conducive to industrial production.

Description

Technical Field

[0001] This invention relates to the field of novel magnetic materials, and in particular to a highly magnetic iron oxide material and its preparation method. Background Technology

[0002] Ferric oxide (Fe3O4) is a multifunctional magnetic material with wide applications in magnetic recording, magnetic fluids, biomedicine, and permanent magnets. The properties of ferric oxide can be tailored using methods such as ion doping, compositional composites, and structural modulation. Patent CN105271431A combines the sol-gel method with self-combustion to prepare a magnetically controllable ferric oxide material and its composite materials. Patent CN101279769A utilizes the directional aggregation and growth of nanocrystals to prepare a strongly magnetic ferric oxide polyhedron.

[0003] Currently, with the rapid development of information technology and industry, various demands have been placed on the functionality of magnetic materials, with new magnetic materials possessing higher coercivity and higher magnetization being a hot technological need. For example, patent CN1004641309C utilizes a one-step crystal transformation method to prepare magnetite powder with a magnetic saturation strength exceeding 85 emu / g and a coercivity less than 35 Oe, exhibiting high saturation magnetization. Patent CN105348775B employs a solvothermal crystallization reaction to prepare a crosslinkable polyarylene ether nitrile / magnetite tetroxide hybrid microsphere magnetic material, with a saturation magnetization of 40–80 emu / g and a remanent magnetization of 15–40 emu / g. Summary of the Invention

[0004] The purpose of this invention is to overcome the shortcomings of the prior art and provide a high magnetic iron oxide material and its preparation method. By performing electrochemical atomic hydrogenation treatment on the iron oxide material, its saturation magnetization and coercivity are greatly improved, and its remanent magnetization is enhanced, thereby improving the magnetic properties of the iron oxide material.

[0005] The present invention adopts the following technical solution:

[0006] On one hand, the present invention provides a method for preparing a highly magnetic iron oxide material, comprising:

[0007] S1. Electrolyte Immersion: Clean the iron oxide workpiece material and immerse it in the electrolyte for a set time.

[0008] S2, Hydrogenation Modification Treatment: Using the iron oxide workpiece material soaked in the electrolyte of step S1 as the cathode, electrochemical atomic hydrogenation treatment is carried out. The atomic hydrogen generated by the cathode electrolysis reaction is adsorbed on the surface of the iron oxide workpiece material and diffuses into the interior of the material under the action of the concentration gradient, thereby modifying the iron oxide workpiece material.

[0009] S3. Clean and dry the iron oxide workpiece material after the hydrogenation modification treatment in step S2 to obtain the high magnetic iron oxide material.

[0010] In addition to any of the possible implementations described above, another implementation is provided in which, in step S1, the electrolyte is a Na2SO4 or K2SO4 solution with a concentration of 0.1–0.6 mol / L, a temperature of 0–60°C, and a pH value of 4.4–11.

[0011] In addition to any of the possible implementations described above, another implementation is provided in which the set time in step S1 is 1 to 10 minutes.

[0012] In addition to any of the possible implementations described above, another implementation is provided in which, in step S1, the workpiece material of the iron oxide is one or more of the following: iron oxide particles, sheets, rods, columns, spheres, and blocks.

[0013] In addition to any of the possible implementations described above, another implementation is provided in which the electrochemical atomic hydrogen treatment process in step S2 is one of the wet electroplating processes of vibration plating, rack plating, and barrel plating.

[0014] In addition to any of the possible implementations described above, another implementation is provided in which, in step S2, during the electrochemical atomic hydrogenation treatment, the anode is an insoluble, shape-stable electrode.

[0015] In addition to any of the possible implementations described above, another implementation is provided in which the current density of the cathode in step S2 is 0.05–1.0 A / cm². 2 .

[0016] In addition to any of the possible implementations described above, another implementation is provided in which, after processing in steps S1-S3, the iron oxide workpiece material is pulverized to obtain iron oxide powder with high coercivity and high magnetization.

[0017] In addition to any of the possible implementations described above, another implementation is provided in which the pulverization process specifically involves grinding the iron oxide workpiece material using a hard friction pair to obtain powder.

[0018] On the other hand, the present invention also provides a highly magnetic iron oxide material, which is obtained by the above-described method.

[0019] The beneficial effects of this invention are as follows:

[0020] Iron(III) oxide (Fe3O4) is an important magnetic material. This invention involves electrochemical atomic hydrogenation treatment of Fe3O4, resulting in a significantly improved saturation magnetization and coercivity, along with enhanced remanent magnetization. This allows the material to maintain high magnetic induction even under demagnetizing conditions, thus significantly improving the magnetic properties of Fe3O4. Furthermore, the preparation method provided by this invention offers advantages such as low cost, simple process, environmental friendliness, and suitability for industrial production. Attached Figure Description

[0021] Figure 1 The diagram shown is a flowchart illustrating a method for preparing a highly magnetic iron oxide material according to an embodiment of the present invention.

[0022] Figure 2 The figure shows the hysteresis loops of the Fe3O4 workpiece material before and after electrochemical atomic hydrogenation treatment in Example 1. Detailed Implementation

[0023] The specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings. It should be noted that the technical features or combinations of technical features described in the following embodiments should not be considered in isolation, but can be combined with each other to achieve better technical effects.

[0024] like Figure 1 As shown, an embodiment of the present invention provides a method for preparing a highly magnetic iron oxide (Fe3O4) material, comprising:

[0025] S1. Electrolyte Immersion: Clean the iron oxide workpiece material and immerse it in the electrolyte for a set time.

[0026] S2, Hydrogenation Modification Treatment: Using the iron oxide workpiece material soaked in the electrolyte of step S1 as the cathode, electrochemical atomic hydrogenation treatment is carried out. The atomic hydrogen generated by the cathode electrolysis reaction is adsorbed on the surface of the iron oxide workpiece material and diffuses into the interior of the material under the action of the concentration gradient, thereby modifying the iron oxide workpiece material.

[0027] S3. Clean and dry the iron oxide workpiece material after the hydrogenation modification treatment in step S2 to obtain the high magnetic iron oxide material.

[0028] In one specific embodiment, in step S1, the electrolyte is a Na2SO4 or K2SO4 solution with a concentration of 0.1–0.6 mol / L, a temperature of 0–60°C, and a pH value of 4.4–11.

[0029] In one specific embodiment, in step S1, the set time is 1 to 10 minutes.

[0030] In one specific embodiment, in step S1, the workpiece material of the iron oxide is one or more of the following: iron oxide particles, sheets, rods, columns, spheres, and blocks.

[0031] In one specific embodiment, in step S2, the electrochemical atomic hydrogen treatment process is one of the following wet electroplating processes: vibration plating, rack plating, and barrel plating.

[0032] In one specific embodiment, during step S2, when performing electrochemical atomic hydrogenation treatment, the anode is an insoluble, shape-stable electrode.

[0033] In one specific embodiment, in step S2, the current density of the cathode is 0.05–1.0 A / cm². 2 .

[0034] In one specific embodiment, after processing in steps S1-S3, the iron oxide workpiece material is pulverized to obtain iron oxide powder with high coercivity and high magnetization.

[0035] In one specific embodiment, the pulverization process specifically involves grinding the iron oxide workpiece material using a hard friction pair to obtain powder.

[0036] Example 1

[0037] Twenty iron oxide ceramic sheets with a diameter of 2cm and a thickness of 2mm were selected for electrochemical atomic hydrogenation treatment.

[0038] Using a Pt electrode as the anode and a 1 mm diameter steel ball as the cathode conductive medium, an ultrasonic electroplating process was employed. The cleaned ceramic sheet and steel ball were placed together in an open vibrating basket and pre-soaked in 0.1 mol / L Na₂SO₄ electrolyte for 10 minutes. The iron oxide ceramic sheet then underwent electrochemical atomic hydrogenation treatment with an applied cathode current density of 0.1 A / cm². 2 The temperature is 20℃.

[0039] After 10 minutes of treatment, the ceramic sheet and steel ball were removed, washed with water, and dried. The modified magnetite ceramic sheet was obtained, with a remanent magnetization of 11.9 emu / g, a saturation magnetization of 106.1 emu / g, and a coercivity of 75.5 Oe. After 40 minutes of treatment, its remanent magnetization was 25.6 emu / g, its saturation magnetization was 142 emu / g, and its coercivity was 415 Oe (see...). Figure 2 By repeatedly grinding the obtained iron oxide ceramic sheet with hard Al2O3 corundum abrasive, highly magnetic iron oxide powder with a particle size of approximately 10–50 μm can be obtained.

[0040] Example 2

[0041] Select 100 grains with a volume of 2cm 3 The iron oxide spheres were subjected to electrochemical atomic hydrogenation treatment.

[0042] A Ti-shaped stabilizing electrode coated with a precious metal is used as the anode, and a barrel plating process is employed. The cathode conductive device inside the barrel extends from both sides via copper wires. Ferrite balls are placed inside the barrel and naturally connect to the cathode conductive device through their own gravity.

[0043] After cleaning, the iron oxide spheres were pre-soaked in 0.35 mol / L K₂SO₄ electrolyte for 1 min, and then subjected to electrochemical atomic hydrogenation treatment with an applied cathode current density of 1 A / cm². 2 The temperature was set at 60℃, and the drum was fully immersed in the electrolyte to ensure that atomic hydrogen generated by cathode electrolysis was uniformly produced on the surface. After 6 minutes of treatment, the iron oxide balls were removed, washed with water, and dried. The modified iron oxide balls were obtained, and their remanent magnetization was measured to be 10.07 emu / g, saturation magnetization to be 96.2 emu / g, and coercivity to be 381 Oe.

[0044] This invention improves the magnetic properties of iron oxide by electrochemically hydrogenating it, thereby significantly increasing its saturation magnetization and coercivity, and enhancing its residual magnetization.

[0045] While several embodiments of the present invention have been provided herein, those skilled in the art should understand that modifications can be made to these embodiments without departing from the spirit of the invention. The above embodiments are merely exemplary and should not be construed as limiting the scope of the invention.

Claims

1. A method for preparing a highly magnetic iron oxide material, characterized in that, The method includes: S1. Electrolyte Immersion: Clean the iron oxide workpiece material and immerse it in the electrolyte for 1-10 minutes; the electrolyte is a Na2SO4 or K2SO4 solution with a concentration of 0.1-0.6 mol / L, a temperature of 0-60℃, and a pH value of 4.4-11. S2. Hydrogenation Modification Treatment: Using the iron oxide workpiece material soaked in the electrolyte of step S1 as the cathode, electrochemical atomic hydrogenation treatment is performed. The atomic hydrogen generated by the cathode electrolysis reaction is adsorbed on the surface of the iron oxide workpiece material and diffuses into the interior of the material under the action of the concentration gradient, thereby modifying the iron oxide workpiece material; the cathode current density is 0.05~1.0 A / cm. 2 ; S3. Clean and dry the iron oxide workpiece material after the hydrogenation modification treatment in step S2 to obtain the high magnetic iron oxide material.

2. The method for preparing the highly magnetic iron oxide material as described in claim 1, characterized in that, In step S1, the workpiece material of the iron oxide is one or more of the following: iron oxide particles, sheets, rods, columns, spheres, and blocks.

3. The method for preparing the highly magnetic iron oxide material as described in claim 1, characterized in that, In step S2, the electrochemical atomic hydrogen treatment process is one of the following wet electroplating processes: vibration plating, rack plating, and barrel plating.

4. The method for preparing the highly magnetic iron oxide material as described in claim 1, characterized in that, In step S2, during the electrochemical atomic hydrogenation treatment, an insoluble, shape-stable electrode is used as the anode.

5. The method for preparing the highly magnetic iron oxide material as described in claim 1, characterized in that, After processing in steps S1-S3, the iron oxide workpiece material is pulverized to obtain iron oxide powder with high coercivity and high magnetization.

6. The method for preparing the highly magnetic iron oxide material as described in claim 5, characterized in that, The pulverization process specifically involves grinding the iron oxide workpiece material using a hard friction pair to obtain powder.

7. A highly magnetic iron oxide material, characterized in that, The highly magnetic iron oxide material is obtained by the method described in any one of claims 1-6.

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