CN112551596A - Preparation method of nano nickel-zinc ferrite magnetic material - Google Patents
Preparation method of nano nickel-zinc ferrite magnetic material Download PDFInfo
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- CN112551596A CN112551596A CN202011352014.1A CN202011352014A CN112551596A CN 112551596 A CN112551596 A CN 112551596A CN 202011352014 A CN202011352014 A CN 202011352014A CN 112551596 A CN112551596 A CN 112551596A
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- 229910001053 Nickel-zinc ferrite Inorganic materials 0.000 title claims abstract description 35
- 239000000696 magnetic material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000010438 heat treatment Methods 0.000 claims abstract description 40
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 39
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000011259 mixed solution Substances 0.000 claims abstract description 25
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229920002643 polyglutamic acid Polymers 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000004132 cross linking Methods 0.000 claims abstract description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000005303 weighing Methods 0.000 claims abstract description 7
- 230000005855 radiation Effects 0.000 claims description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 9
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 claims description 6
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 6
- -1 iron ions Chemical class 0.000 claims description 6
- 229910001453 nickel ion Inorganic materials 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000011701 zinc Substances 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 2
- 230000005415 magnetization Effects 0.000 abstract description 4
- 230000000536 complexating effect Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 6
- 229910000859 α-Fe Inorganic materials 0.000 description 6
- QELJHCBNGDEXLD-UHFFFAOYSA-N nickel zinc Chemical compound [Ni].[Zn] QELJHCBNGDEXLD-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y25/00—Nanomagnetism, e.g. magnetoimpedance, anisotropic magnetoresistance, giant magnetoresistance or tunneling magnetoresistance
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/342—Oxides
- H01F1/344—Ferrites, e.g. having a cubic spinel structure (X2+O)(Y23+O3), e.g. magnetite Fe3O4
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
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- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Power Engineering (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Soft Magnetic Materials (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention discloses a preparation method of a nano nickel-zinc ferrite magnetic material, which comprises the following steps: s1, weighing nickel nitrate, zinc nitrate and ferric nitrate according to a certain stoichiometric ratio, dissolving in deionized water, and then adding citric acid to obtain a mixed solution; s2, fully complexing the mixed solution, adding gamma-polyglutamic acid, and adjusting the pH value with ammonia water to obtain mixed sol; s3, radiating and crosslinking the mixed sol under the action of 60Co gamma rays, and then drying to obtain dry gel; and S4, carrying out heat treatment on the dried gel to obtain the nano nickel-zinc ferrite magnetic material. The invention can effectively improve the saturation magnetization of the nano nickel-zinc ferrite magnetic material, so that the nano nickel-zinc ferrite magnetic material has excellent magnetic performance.
Description
Technical Field
The invention relates to the technical field of ferrite magnetic materials, in particular to a preparation method of a nano nickel-zinc ferrite magnetic material.
Background
The nano nickel-zinc soft magnetic ferrite has the advantages of high saturation magnetization, high Curie temperature, good chemical stability, low coercive force, large specific surface area and the like, and is a magnetic nano material with the most application prospect. At present, the main preparation method of the nano nickel-zinc soft magnetic ferrite material comprises the following steps: hydrothermal method, chemical coprecipitation method, sol-gel method, etc. In recent years, with the development of electronic information technology, the requirements for integration and miniaturization of devices are gradually increased, and the performance requirements of nickel-zinc soft magnetic ferrite materials, which are key materials of the devices, are also upgraded. How to improve the saturation magnetization of the nickel-zinc soft magnetic ferrite material and make it have excellent magnetic properties becomes a research and development direction of great concern.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a preparation method of a nano nickel-zinc ferrite magnetic material.
The invention provides a preparation method of a nano nickel-zinc ferrite magnetic material, which comprises the following steps:
s1, according to Ni0.6Zn0.4Fe2O4Weighing nickel nitrate, zinc nitrate and ferric nitrate according to the stoichiometric ratio, dissolving the nickel nitrate, the zinc nitrate and the ferric nitrate into deionized water, and then adding a proper amount of citric acid to completely dissolve the mixture to obtain a mixed solution;
s2, stirring the mixed solution for 1.5-2.5h, adding a proper amount of gamma-polyglutamic acid for complete dissolution, and adjusting the pH value to 6-6.5 by using ammonia water to obtain mixed sol;
s3, carrying out radiation crosslinking on the mixed sol under the action of 60Co gamma rays, and then drying to obtain dry gel;
s4, heating the xerogel to 950-1100 ℃ in air atmosphere, and then carrying out heat treatment for 1.5-3h to obtain the nano nickel-zinc ferrite magnetic material.
Preferably, the mole number of the citric acid is 1 to 1.5 times of the sum of the mole numbers of the nickel ions, the zinc ions and the iron ions.
Preferably, the concentration of the ferric nitrate in the mixed solution is 0.1-0.15 mol/L.
Preferably, the ratio of the mass of the gamma-polyglutamic acid to the volume of the mixed solution is (1-3) g: 100 mL.
Preferably, in the step S3, the dose rate for crosslinking the radiation is 1-1.5kGy/h, and the total radiation dose is 8-15 kGy.
Preferably, in the step S3, the drying temperature is 90 to 120 ℃, and the drying time is 12 to 24 hours.
Preferably, in the step S4, the xerogel is heated to 200-250 ℃ at a heating rate of 2-3 ℃/min, then heated to 500-600 ℃ at a heating rate of 4-6 ℃/min, and finally heated to 950-1100 ℃ at a heating rate of 10-15 ℃/min in the air atmosphere.
A nano nickel-zinc ferrite magnetic material is prepared by the preparation method.
The invention has the following beneficial effects:
in the sol-gel synthesis process of the nickel-zinc ferrite, the gamma-polyglutamic acid is introduced, and the gamma-polyglutamic acid macromolecules are crosslinked through radiation, so that composite gel consisting of a ferrite precursor and the gamma-polyglutamic acid is synchronously formed, nickel-zinc ferrite nano crystals are formed through drying and heat treatment, and meanwhile, the gamma-polyglutamic acid is decomposed at high temperature to obtain the nano nickel-zinc ferrite magnetic material. By introducing the gamma-polyglutamic acid in the gel forming process and utilizing the steric hindrance and the electrostatic repulsion of the macromolecular chain of the gamma-polyglutamic acid, the gel is not easy to agglomerate during drying, has uniform components, large surface area of formed crystal grains, small grain diameter and uniform distribution, and has a good microstructure, thereby improving the saturation magnetization of the nano nickel-zinc ferrite material and ensuring that the nano nickel-zinc ferrite material has excellent magnetic performance.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A preparation method of a nano nickel-zinc ferrite magnetic material comprises the following steps:
s1, according to Ni0.6Zn0.4Fe2O4Weighing nickel nitrate, zinc nitrate and ferric nitrate according to the stoichiometric ratio, dissolving the nickel nitrate, the zinc nitrate and the ferric nitrate in deionized water, and then adding citric acid to completely dissolve the nickel nitrate, the zinc nitrate and the ferric nitrate to obtain a mixed solution, wherein the concentration of the ferric nitrate in the mixed solution is 0.1mol/L, and the mole number of the citric acid is 1 time of the sum of the mole numbers of nickel ions, zinc ions and iron ions;
s2, stirring the mixed solution for 1.5h, adding gamma-polyglutamic acid for complete dissolution, and adjusting the pH to 6 by using ammonia water to obtain mixed sol, wherein the mass ratio of the gamma-polyglutamic acid to the volume of the mixed solution is 1 g: 100 mL;
s3, carrying out radiation crosslinking on the mixed sol under the action of 60Co gamma rays, wherein the dose rate of the radiation crosslinking is 1kGy/h, the total radiation dose is 8kGy, and then drying for 24h at 90 ℃ to obtain dry gel;
s4, heating the xerogel to 200 ℃ at a heating rate of 2 ℃/min in an air atmosphere, heating to 500 ℃ at a heating rate of 4 ℃/min, heating to 950 ℃ at a heating rate of 10 ℃/min, and then carrying out heat treatment for 3h to obtain the nano nickel-zinc ferrite magnetic material.
Example 2
A preparation method of a nano nickel-zinc ferrite magnetic material comprises the following steps:
s1, according to Ni0.6Zn0.4Fe2O4Weighing nickel nitrate, zinc nitrate and ferric nitrate according to the stoichiometric ratio, dissolving the nickel nitrate, the zinc nitrate and the ferric nitrate in deionized water, and then adding citric acid to completely dissolve the nickel nitrate, the zinc nitrate and the ferric nitrate to obtain a mixed solution, wherein the concentration of the ferric nitrate in the mixed solution is 0.15mol/L, and the mole number of the citric acid is 1.5 times of the sum of the mole numbers of nickel ions, zinc ions and iron ions;
s2, stirring the mixed solution for 2.5h, adding gamma-polyglutamic acid for complete dissolution, and adjusting the pH to 6.5 by using ammonia water to obtain mixed sol, wherein the mass ratio of the gamma-polyglutamic acid to the volume of the mixed solution is 3 g: 100 mL;
s3, carrying out radiation crosslinking on the mixed sol under the action of 60Co gamma rays, wherein the dose rate of the radiation crosslinking is 1.5kGy/h, the total radiation dose is 15kGy, and then drying at 120 ℃ for 12h to obtain xerogel;
s4, heating the xerogel to 250 ℃ at a heating rate of 3 ℃/min in an air atmosphere, heating to 600 ℃ at a heating rate of 6 ℃/min, heating to 1100 ℃ at a heating rate of 15 ℃/min, and then carrying out heat treatment for 1.5h to obtain the nano nickel-zinc ferrite magnetic material.
Example 3
A preparation method of a nano nickel-zinc ferrite magnetic material comprises the following steps:
s1, according to Ni0.6Zn0.4Fe2O4Weighing nickel nitrate, zinc nitrate and ferric nitrate according to the stoichiometric ratio, dissolving the nickel nitrate, the zinc nitrate and the ferric nitrate in deionized water, and then adding citric acid to completely dissolve the nickel nitrate, the zinc nitrate and the ferric nitrate to obtain a mixed solution, wherein the concentration of the ferric nitrate in the mixed solution is 0.14mol/L, and the mole number of the citric acid is 1.2 times of the sum of the mole numbers of nickel ions, zinc ions and iron ions;
s2, stirring the mixed solution for 2 hours, adding gamma-polyglutamic acid to dissolve completely, and adjusting the pH to 6.2 by using ammonia water to obtain mixed sol, wherein the mass ratio of the gamma-polyglutamic acid to the volume of the mixed solution is 2 g: 100 mL;
s3, carrying out radiation crosslinking on the mixed sol under the action of 60Co gamma rays, wherein the dose rate of the radiation crosslinking is 1.2kGy/h, the total radiation dose is 12kGy, and then drying at 100 ℃ for 20h to obtain xerogel;
s4, heating the xerogel to 225 ℃ at a heating rate of 2.5 ℃/min in an air atmosphere, heating to 550 ℃ at a heating rate of 5 ℃/min, heating to 1030 ℃ at a heating rate of 12 ℃/min, and then carrying out heat treatment for 2h to obtain the nano nickel-zinc ferrite magnetic material.
Comparative example 1
A preparation method of a nano nickel-zinc ferrite magnetic material comprises the following steps:
s1, according to Ni0.6Zn0.4Fe2O4Weighing nickel nitrate, zinc nitrate and ferric nitrate according to the stoichiometric ratio, dissolving the nickel nitrate, the zinc nitrate and the ferric nitrate in deionized water, and then adding citric acid to completely dissolve the nickel nitrate, the zinc nitrate and the ferric nitrate to obtain a mixed solution, wherein the concentration of the ferric nitrate in the mixed solution is 0.14mol/L, and the mole number of the citric acid is 1.2 times of the sum of the mole numbers of nickel ions, zinc ions and iron ions;
s2, stirring the mixed solution for 2 hours, and then adjusting the pH to 6.2 by using ammonia water to obtain mixed sol;
s3, drying the mixed sol at 100 ℃ for 20h to obtain dry gel;
s4, heating the xerogel to 225 ℃ at a heating rate of 2.5 ℃/min in an air atmosphere, heating to 550 ℃ at a heating rate of 5 ℃/min, heating to 1030 ℃ at a heating rate of 12 ℃/min, and then carrying out heat treatment for 2h to obtain the nano nickel-zinc ferrite magnetic material.
The nano nickel zinc ferrite magnetic materials prepared in examples 1 to 3 and comparative example 1 were subjected to a performance test at room temperature using a vibration sample magnetometer, and the results are shown in table 1:
TABLE 1 nanometer nickel-zinc ferrite magnetic material performance test results
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. A preparation method of a nano nickel-zinc ferrite magnetic material is characterized by comprising the following steps:
s1, according to Ni0.6Zn0.4Fe2O4Weighing nickel nitrate, zinc nitrate and ferric nitrate according to the stoichiometric ratio, dissolving the nickel nitrate, the zinc nitrate and the ferric nitrate into deionized water, and then adding a proper amount of citric acid to completely dissolve the mixture to obtain a mixed solution;
s2, stirring the mixed solution for 1.5-2.5h, adding a proper amount of gamma-polyglutamic acid for complete dissolution, and adjusting the pH value to 6-6.5 by using ammonia water to obtain mixed sol;
s3, carrying out radiation crosslinking on the mixed sol under the action of 60Co gamma rays, and then drying to obtain dry gel;
s4, heating the xerogel to 950-1100 ℃ in air atmosphere, and then carrying out heat treatment for 1.5-3h to obtain the nano nickel-zinc ferrite magnetic material.
2. The method for preparing a nano nickel-zinc ferrite magnetic material according to claim 1, wherein the mole number of the citric acid is 1 to 1.5 times of the sum of the mole numbers of the nickel ions, the zinc ions and the iron ions.
3. The method for preparing a nano nickel zinc ferrite magnetic material according to claim 1 or 2, wherein the concentration of ferric nitrate in the mixed solution is 0.1-0.15 mol/L.
4. The method for preparing a nano nickel zinc ferrite magnetic material according to any one of claims 1 to 3, wherein the ratio of the mass of the gamma-polyglutamic acid to the volume of the mixed solution is (1-3) g: 100 mL.
5. The method for preparing a nano nickel zinc ferrite magnetic material according to any one of claims 1 to 4, wherein in the step S3, the dosage rate of the radiation cross-linking is 1 to 1.5kGy/h, and the total radiation dosage is 8 to 15 kGy.
6. The method for preparing a nano nickel zinc ferrite magnetic material according to any one of claims 1 to 5, wherein the drying temperature is 90 to 120 ℃ and the drying time is 12 to 24 hours in the step S3.
7. The method for preparing a nano nickel-zinc ferrite magnetic material as claimed in any one of claims 1 to 6, wherein in step S4, the dried gel is heated to 200-250 ℃ at a heating rate of 2-3 ℃/min, then heated to 500-600 ℃ at a heating rate of 4-6 ℃/min, and finally heated to 950-1100 ℃ at a heating rate of 10-15 ℃/min.
8. A nano nickel zinc ferrite magnetic material, characterized by being prepared by the preparation method of any one of claims 1 to 7.
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| CN116041053A (en) * | 2022-11-30 | 2023-05-02 | 国网智能电网研究院有限公司 | Preparation method of honeycomb nickel-zinc ferrite material |
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| US20100055500A1 (en) * | 2008-09-03 | 2010-03-04 | Tdk Corporation | Oxide fine particle powder and process for its production, and magnetic recording medium |
| CN106913885A (en) * | 2015-12-28 | 2017-07-04 | 中国科学院宁波材料技术与工程研究所 | A kind of magnetic nano-particle and its preparation method and application |
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| CN116041053A (en) * | 2022-11-30 | 2023-05-02 | 国网智能电网研究院有限公司 | Preparation method of honeycomb nickel-zinc ferrite material |
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