CN115028202A - Preparation of high saturation magnetization Mn 3 O 4 Method for magnetic nano rod - Google Patents
Preparation of high saturation magnetization Mn 3 O 4 Method for magnetic nano rod Download PDFInfo
- Publication number
- CN115028202A CN115028202A CN202210035468.9A CN202210035468A CN115028202A CN 115028202 A CN115028202 A CN 115028202A CN 202210035468 A CN202210035468 A CN 202210035468A CN 115028202 A CN115028202 A CN 115028202A
- Authority
- CN
- China
- Prior art keywords
- saturation magnetization
- high saturation
- magnetic nano
- nano rod
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- 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
Abstract
The invention belongs to the technical field of preparation processes of inorganic nano materials, and particularly relates to a method for preparing high saturation magnetization Mn 3 O 4 The method of the magnetic nano rod comprises the steps of mixing and stirring manganese oxalate, sodium gluconate, citric acid and sodium dodecyl benzene sulfonate to form a mixed solution, ultrasonically dispersing and dissolving the mixed solution in deionized water, transferring the mixed solution to a self-pressure kettle to perform hydrothermal reaction, naturally cooling, ultrasonically washing and drying in vacuum to obtain a target product; the mass ratio of the manganese oxalate to the sodium gluconate to the citric acid to the sodium dodecyl benzene sulfonate is 1: 0.5-5: 2-7 in sequence. The magnetic Mn prepared by the invention 3 O 4 Uniform distribution of nanorod particle size, Mn 3 O 4 The surface of the particle can be modified, the aqueous solution has good dispersibility and larger saturation magnetization.
Description
Technical Field
The invention belongs to the technical field of preparation processes of inorganic nano materials, and particularly relates to a method for preparing high saturation magnetization Mn 3 O 4 A method of magnetic nanorods.
Background
Mangano manganic oxide (Mn) 3 O 4 ) Is an inorganic compound, and is black powder. Belongs to a spinel structure, is an important inorganic functional material, Mn 3 O 4 The method is widely applied to the fields of catalysis, electrochemistry, soft magnetic materials, air purification and the like. In recent years, Mn has been developed by various new techniques 3 O 4 New materials, e.g. electronic grade Mn 3 O 4 ，Mn 3 O 4 Ultra fine powder of Mn 3 O 4 Nanobelts, nanorods, nanofibers, hollow nanospheres, and the like. The domestic mangano-manganic oxide production method can only adopt a metal manganese powder oxidation method for production, and the technical principle is derived from U.S. patents. From a process perspective, there are currently major problems: the technical content is low; the production cost is high; the granularity is not uniform, the grain diameter is larger and is larger than about 2 mm; the content of various impurities is generally higher, and only products of common grade can be produced. The method for producing manganese tetraoxide abroad is also mainly a metal manganese powder oxidation method.
Disclosure of Invention
The invention aims to provide a method for preparing high saturation magnetization Mn with simple process flow 3 O 4 A method of magnetic nanorods. The magnetic Mn with high saturation magnetization prepared by the invention 3 O 4 Uniform distribution of nanorod particle size, Mn 3 O 4 The surface of the particle can be modified and modified, and the saturation magnetization is high.
In order to solve the technical problem, the invention is realized as follows:
preparation of high saturation magnetization Mn 3 O 4 The method of the magnetic nanorod comprises the steps of mixing and stirring manganese oxalate, sodium gluconate, citric acid and sodium dodecyl benzene sulfonate to form a mixed solution, ultrasonically dispersing and dissolving the mixed solution in deionized water, transferring the mixed solution to a self-pressure kettle to perform hydrothermal reaction, naturally cooling, ultrasonically washing, and drying in vacuum to obtain a target product.
As a preferable scheme, the mass ratio of the manganese oxalate to the sodium gluconate to the citric acid to the sodium dodecyl benzene sulfonate is 1: 0.5-5: 2-7 in sequence.
Furthermore, the concentration of the manganese oxalate is 0.05-0.5 g/mL.
Further, the present invention was stirred at 80 ℃ for 2 hours to form a mixed solution.
Furthermore, the vibration frequency of the ultrasonic dispersion is 90-120 Hz, and the time is 20-80 seconds.
Furthermore, the hydrothermal reaction temperature is 150-250 ℃, and the reaction time is 5-36 hours.
Further, the ultrasonic washing step of the present invention comprises: washing with anhydrous alcohol and deionized water for 3 times, and drying to obtain the target product.
Further, the vacuum drying conditions of the present invention: controlling the temperature to be 60-80 ℃; controlling the vacuum degree to be-60 to-100 Kpa; the time is 1-3 hours.
Furthermore, the particle size of the target product is 100-200 nanometers, and the target product is of a rod-shaped structure with the length of 1000 nanometers.
Compared with the prior art, the invention has the following characteristics:
(1) high saturation magnetization magnetic Mn 3 O 4 The shape of the nano particles is a regular rod-shaped structure with the particle size of 100-200 nanometers and the length of about 1000 nanometers.
(2) Preparation of nanostructured Mn 3 O 4 There are many methods for particles, such as a template method, a sol-gel method, a microwave-assisted method, etc., and the structure of the particles affects the physicochemical properties and magnetism thereof. Hydrothermal temperature and other conditions influence Mn 3 O 4 The nanoparticles differ in their magnetic properties due to their geometric size. In contrast to the literature, the Mn synthesized by the present invention 3 O 4 The particles are not the smallest but provide a synthetic Mn 3 O 4 A novel method of particle formation.
(3) Mn is found 3 O 4 The grain size of the nano-rod is the main factor influencing the magnetization, and the length of the nano-rod influences the magnetization, and the synergistic effect of the two factors can influence Mn 3 O 4 The saturation magnetization of the nanorods has an important influence. Mn of the invention 3 O 4 The shape of the nano particles adopts a more regular bar-shaped junction with the particle diameter of 100-200 nanometers and the length of 1000 nanometersAnd (5) forming. Mn of the invention 3 O 4 The surface can be applied to the fields of electrochemistry, magnetism, catalysis and the like after being modified.
Drawings
The invention is further described with reference to the following figures and detailed description. The scope of the invention is not limited to the following expressions.
FIG. 1 shows magnetic Mn prepared in example 1 3 O 4 SEM photograph of nanorods.
FIG. 2 shows magnetic Mn prepared in example 2 3 O 4 SEM photograph of nanorods.
FIG. 3 shows magnetic Mn prepared in example 3 3 O 4 SEM photograph of the nanorods.
FIG. 4 shows magnetic Mn prepared in example 4 3 O 4 SEM photograph of nanorods.
FIG. 5 shows magnetic Mn prepared in example 5 3 O 4 XRD pattern of the nanorods.
FIG. 6 shows magnetic Mn prepared in example 5 3 O 4 Hysteresis loop of nanorod.
Detailed Description
Example 1
The preparation method comprises the steps of uniformly mixing manganese oxalate, sodium gluconate, citric acid and sodium dodecyl benzene sulfonate according to the mass ratio of 1:1:1:2, and stirring at 80 ℃ for 2 hours to form a mixed solution. The concentration of manganese oxalate is 0.1 g/mL, 100 Hz ultrasonic oscillation treatment is carried out for 30 seconds to obtain a mixture, the mixture is transferred into a self-pressurized kettle to carry out hydrothermal reaction, the reaction temperature is 180 ℃, and the reaction time is 8 hours. Naturally cooling, ultrasonic washing (washing with anhydrous ethanol and deionized water for 3 times respectively), and vacuum drying at 80 deg.C under-100 Kpa for 1 hr to obtain the final product. Mn thus prepared 3 O 4 The nano particles are uniform rod-shaped particles with the size of 100 nm multiplied by 3 mu m, the distribution is uniform, and the saturation magnetization is 1.2 emu/g.
Example 2
Uniformly mixing manganese oxalate, sodium gluconate, citric acid and sodium dodecyl benzene sulfonate according to the mass ratio of 1:1:2:3, and stirring for 2 hours at 80 DEG CThe resulting mixed solution. The concentration of manganese oxalate is 0.2 g/mL, the mixture is obtained by ultrasonic oscillation treatment at 100 Hz for 40 seconds, and the mixture is transferred into a self-pressure kettle for hydrothermal reaction, the reaction temperature is 200 ℃, and the reaction time is 8 hours. Naturally cooling, ultrasonic washing (washing with anhydrous ethanol and deionized water for 3 times respectively), and vacuum drying at 80 deg.C under-100 Kpa for 1 hr to obtain the final product. Mn produced 3 O 4 The nano particles are uniform rod-shaped particles with the size of 100nm multiplied by 2 mu m, the distribution is uniform, and the saturation magnetization is 1.3 emu/g.
Example 3
Manganese oxalate, sodium gluconate, citric acid and sodium dodecyl benzene sulfonate are uniformly mixed according to the mass ratio of 1:1:2:4, and are stirred for 2 hours at the temperature of 80 ℃ to form a mixed solution. The concentration of manganese oxalate is 0.3 g/mL, the mixture is obtained by ultrasonic oscillation treatment at 100 Hz for 50 seconds, and the mixture is transferred into a self-pressure kettle for hydrothermal reaction, the reaction temperature is 220 ℃, and the reaction time is 8 hours. Naturally cooling, ultrasonic washing (washing with anhydrous ethanol and deionized water for 3 times respectively), and vacuum drying at 80 deg.C under-100 Kpa for 1 hr to obtain the final product. Mn thus prepared 3 O 4 The nano particles are uniform rod-shaped particles with the particle size of 50nm multiplied by 2 mu m, the distribution is uniform, and the saturation magnetization is 1.4 emu/g.
Example 4
Manganese oxalate, sodium gluconate, citric acid and sodium dodecyl benzene sulfonate are uniformly mixed according to the mass ratio of 1:2:3:4, and are stirred for 2 hours at the temperature of 80 ℃ to form a mixed solution. The concentration of manganese oxalate is 0.3 g/mL, the mixture is obtained by ultrasonic oscillation treatment at 100 Hz for 50 seconds, and the mixture is transferred into a self-pressure kettle for hydrothermal reaction, the reaction temperature is 220 ℃, and the reaction time is 8 hours. Naturally cooling, ultrasonic washing (washing with anhydrous ethanol and deionized water for 3 times respectively), and vacuum drying at 80 deg.C under-100 Kpa for 1 hr to obtain the final product. Mn produced 3 O 4 The nano particles are uniform rod-shaped particles of 40nm multiplied by 500nm, the distribution is uniform, and the saturation magnetization is 1.5 emu/g.
Example 5
The preparation method comprises the steps of uniformly mixing manganese oxalate, sodium gluconate, citric acid and sodium dodecyl benzene sulfonate according to the mass ratio of 1:3:3:3, and stirring at 80 ℃ for 3 hours to form a mixed solution. The concentration of manganese oxalate is 0.3 g/mL, 100 Hz ultrasonic oscillation treatment is carried out for 50 seconds to obtain a mixture, the mixture is transferred into a self-pressurized kettle to carry out hydrothermal reaction, the reaction temperature is 240 ℃, and the reaction time is 8 hours. Naturally cooling, ultrasonic washing (washing with anhydrous ethanol and deionized water for 3 times respectively), and vacuum drying at 80 deg.C under-100 Kpa for 1 hr to obtain the final product. Mn produced 3 O 4 The nano particles are uniform rod-shaped particles with the size of 50 nm multiplied by 500nm, the distribution is uniform, and the saturation magnetization is 1.4 emu/g.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. Preparation of Mn with high saturation magnetization 3 O 4 The method for preparing the magnetic nanorod is characterized by comprising the following steps: mixing and stirring manganese oxalate, sodium gluconate, citric acid and sodium dodecyl benzene sulfonate to form a mixed solution, ultrasonically dispersing and dissolving the mixed solution in deionized water, transferring the deionized water to a self-pressure kettle to perform hydrothermal reaction, naturally cooling, ultrasonically washing, and drying in vacuum to obtain a target product.
2. The method for preparing Mn with high saturation magnetization according to claim 1 3 O 4 The method of the magnetic nano rod is characterized in that: the mass ratio of the manganese oxalate to the sodium gluconate to the citric acid to the sodium dodecyl benzene sulfonate is 1: 0.5-5: 2-7 in sequence.
3. Preparation of high saturation magnetization Mn according to claim 2 3 O 4 The method of the magnetic nano rod is characterized in that: the concentration of the manganese oxalate is 0.05-0.5 g/mL.
4. Preparation of high saturation magnetization Mn according to claim 3 3 O 4 The method of the magnetic nano rod is characterized in that: the mixture was stirred at 80 ℃ for 2 hours to form a mixed solution.
5. Preparation of Mn with high saturation magnetization according to claim 4 3 O 4 The method of the magnetic nano rod is characterized in that: the vibration frequency of the ultrasonic dispersion is 90-120 Hz, and the time is 20-80 seconds.
6. The method for preparing Mn with high saturation magnetization according to any one of claims 1 to 5 3 O 4 The method of the magnetic nano rod is characterized in that: the hydrothermal reaction temperature is 150-250 ℃, and the reaction time is 5-36 hours.
7. Preparation of high saturation magnetization Mn according to claim 6 3 O 4 A method of magnetic nanorods, characterized in that the ultrasonic washing step comprises: washing with anhydrous alcohol and deionized water for 3 times, and drying to obtain the target product.
8. A method for preparing Mn with high saturation magnetization according to claim 7 3 O 4 The method of the magnetic nano rod is characterized in that: the vacuum drying conditions are as follows: controlling the temperature to be 60-80 ℃; controlling the vacuum degree to be-60 to-100 Kpa; the time is 1-3 hours.
9. A method for preparing Mn with high saturation magnetization according to claim 8 3 O 4 The method of the magnetic nano rod is characterized in that: the particle size of the target product is 100-200 nanometers, and the target product is of a rod-shaped structure with the length of 1000 nanometers.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210035468.9A CN115028202B (en) | 2022-01-13 | 2022-01-13 | Preparation of high saturation magnetization Mn 3 O 4 Method for magnetic nano rod |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210035468.9A CN115028202B (en) | 2022-01-13 | 2022-01-13 | Preparation of high saturation magnetization Mn 3 O 4 Method for magnetic nano rod |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115028202A true CN115028202A (en) | 2022-09-09 |
| CN115028202B CN115028202B (en) | 2022-12-27 |
Family
ID=83120091
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210035468.9A Active CN115028202B (en) | 2022-01-13 | 2022-01-13 | Preparation of high saturation magnetization Mn 3 O 4 Method for magnetic nano rod |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115028202B (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3579452A (en) * | 1967-09-01 | 1971-05-18 | Bayer Ag | Process for the production of ferromagnetic pure or isotype manganate mixed phases crystallizing in the ilmenite lattice |
| CN101178961A (en) * | 2006-11-10 | 2008-05-14 | 中国科学院化学研究所 | water soluble magnetic nanometer crystal with high dissolvability and method of producing the same |
| JP2009233845A (en) * | 2008-03-03 | 2009-10-15 | Tohoku Univ | Method for synthesizing nanoparticle using solvothermal method |
| CN104167540A (en) * | 2014-08-13 | 2014-11-26 | 江苏华东锂电技术研究院有限公司 | Negative electrode active material and preparation method thereof and lithium ion battery |
| CN104209119A (en) * | 2014-08-29 | 2014-12-17 | 安徽工程大学 | Mn3O4-MnO2 nano rod composite oxide as well as preparation method and application of Mn3O4-MnO2 nano rod composite oxide |
| CN104261478A (en) * | 2014-09-19 | 2015-01-07 | 济南大学 | Preparation method of Mn3O4 nanowire or nanorod |
| CN113603145A (en) * | 2021-08-11 | 2021-11-05 | 南方锰业集团有限责任公司 | Method for preparing micro-nano manganous manganic oxide by manganese sulfate solution |
-
2022
- 2022-01-13 CN CN202210035468.9A patent/CN115028202B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3579452A (en) * | 1967-09-01 | 1971-05-18 | Bayer Ag | Process for the production of ferromagnetic pure or isotype manganate mixed phases crystallizing in the ilmenite lattice |
| CN101178961A (en) * | 2006-11-10 | 2008-05-14 | 中国科学院化学研究所 | water soluble magnetic nanometer crystal with high dissolvability and method of producing the same |
| JP2009233845A (en) * | 2008-03-03 | 2009-10-15 | Tohoku Univ | Method for synthesizing nanoparticle using solvothermal method |
| CN104167540A (en) * | 2014-08-13 | 2014-11-26 | 江苏华东锂电技术研究院有限公司 | Negative electrode active material and preparation method thereof and lithium ion battery |
| CN104209119A (en) * | 2014-08-29 | 2014-12-17 | 安徽工程大学 | Mn3O4-MnO2 nano rod composite oxide as well as preparation method and application of Mn3O4-MnO2 nano rod composite oxide |
| CN104261478A (en) * | 2014-09-19 | 2015-01-07 | 济南大学 | Preparation method of Mn3O4 nanowire or nanorod |
| CN113603145A (en) * | 2021-08-11 | 2021-11-05 | 南方锰业集团有限责任公司 | Method for preparing micro-nano manganous manganic oxide by manganese sulfate solution |
Non-Patent Citations (1)
| Title |
|---|
| 王春雨等: "纳米二氧化锰制备方法的研究进展", 《现代化工》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115028202B (en) | 2022-12-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Lv et al. | Controlled growth of three morphological structures of magnesium hydroxide nanoparticles by wet precipitation method | |
| Wang et al. | Microwave-assisted synthesis and magnetic property of magnetite and hematite nanoparticles | |
| Rafique et al. | Growth of monodisperse nanospheres of MnFe2O4 with enhanced magnetic and optical properties | |
| Liang et al. | Dispersibility, shape and magnetic properties of nano-Fe 3 O 4 particles | |
| Cao et al. | Fe 3 O 4 polyhedral nanoparticles with a high magnetization synthesized in mixed solvent ethylene glycol–water system | |
| Liu et al. | Hydrothermal synthesis of CoFe2O4 nanoplatelets and nanoparticles | |
| Liu et al. | Ultrasonic-assisted ultra-rapid synthesis of monodisperse meso-SiO2@ Fe3O4 microspheres with enhanced mesoporous structure | |
| Wang et al. | Morphology controllable synthesis of nickel nanopowders by chemical reduction process | |
| Liu et al. | Preparation of different shaped α-Fe 2 O 3 nanoparticles with large particles of iron oxide red | |
| CN107628648A (en) | A kind of preparation method of pattern and the controllable ferric oxide particles of size | |
| CN106335929B (en) | A kind of preparation method of the mangano-manganic oxide of micro nano structure | |
| CN101049976A (en) | Method for preparing superfine even Fe2O3 | |
| Liu et al. | High-yield synthesis and characterization of monodisperse sub-microsized CoFe2O4 octahedra | |
| CN108083316B (en) | Preparation method of nano rare earth oxide powder | |
| Liu et al. | Modified solvothermal synthesis of magnetic microspheres with multifunctional surfactant cetyltrimethyl ammonium bromide and directly coated mesoporous shell | |
| CN104860357B (en) | Mono-dispersed nano sheet and/or nano-rings and preparation thereof and application | |
| Bing et al. | Preparation of micro-sized and uniform spherical Ag powders by novel wet-chemical method | |
| CN103667887A (en) | Preparation method of FeCo alloy absorbing material | |
| CN113426999B (en) | Magnetic nanowire with core-shell heterostructure and preparation method and application thereof | |
| Liang et al. | Solvothermal synthesis and luminescence of nearly monodisperse LnVO4 nanoparticles | |
| LIU et al. | Effects of reaction parameters on preparation of Cu nanoparticles via aqueous solution reduction method with NaBH4 | |
| de Medeiros et al. | Synthesis of CoFe2O4 nanocubes | |
| CN101049977A (en) | Method for preparing Nano Fe2O3 | |
| Jiang et al. | A simple route to synthesize ZnFe2O4 hollow spheres and their magnetorheological characteristics | |
| CN1986426A (en) | Preparing process of nano Mn-Zn ferrite material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |