CN111850389B - Method for preparing iron nitride nanorod material - Google Patents
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- CN111850389B CN111850389B CN201910352344.1A CN201910352344A CN111850389B CN 111850389 B CN111850389 B CN 111850389B CN 201910352344 A CN201910352344 A CN 201910352344A CN 111850389 B CN111850389 B CN 111850389B
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/10—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of tubular bodies
- C21D8/105—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of tubular bodies of ferrous alloys
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- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
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- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
- C22C33/0285—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with Cr, Co, or Ni having a minimum content higher than 5%
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- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/28—Ferrous alloys, e.g. steel alloys containing chromium with titanium or zirconium
Abstract
The invention aims to provide a method for preparing ironThe nitride nanorod material is prepared by adopting a chemical liquid phase method, and the carbon wraps Fe16N2The outer shell layer of the nano rod material is carbon, and the inner core is Fe16N2And (4) nanorods. The method can be used for preparing magnetic carbon-coated Fe with diameter of 20-30 nm and length of 0.5-3 μm16N2And (4) nanorods. Carbon coated Fe16N2The nano-rod has excellent magnetism, utilizes special properties of surface effect, catalysis, optics or magnetism and the like, and can be widely applied to the fields of biology, medicine, permanent magnetism and the like under the condition of combining the unique biological function of biological molecules.
Description
Technical Field
The invention belongs to the field of inorganic functional nano materials, and particularly relates to a method for preparing an iron nitride magnetic nano material.
Background
The binary iron nitride has black gray color and belongs to a metal interstitial compound. The binary iron nitride comprises Fe according to the iron-nitrogen phase diagram2N、γ'-Fe4N、ε-Fe2N1-xAnd alpha' -Fe16N2And the like. The general formula of the α "-phase iron nitride having a tetragonal crystal structure (I4/mmm) therein can be written as α" -Fe16N2The content of nitrogen element was 11.1 at.% (atomic percent). At room temperature, it has ferromagnetism. Alpha' -Fe16N2The compound has great potential in the aspect of permanent magnet application due to good magnetic property. Containing magnetic gamma' -Fe4N、ε-Fe2N1-xColloidal solutions of nanoparticles can be used to make magnetic fluids. The iron nitride can also be used as a catalyst, and has good catalytic reaction activity for Fischer-Tropsch synthesis, ammonia synthesis and other reactions.
Generally, there are three conventional nitriding methods, including gas nitriding, liquid nitriding, and nitrogen ion implantationA method. The structure and magnetic properties of iron nitride powders were studied using the mechanical alloying method P.Y.Lee et al (J.alloys Compd.1995,222, 179-183.). W.A.Kaczmarek (Scr.Metal.Mater., 1995,33,1687-3/H2Or NH3The carbonyl iron is heated and decomposed in the nitriding atmosphere to prepare the iron nitride nano particles. Grimes et al (J.appl.Phys.,2000,87,5642-5644.) magnetic gamma' -Fe was obtained by laser pyrolysis from carbonyl iron and ethylene as starting materials4N nano particles. Lida et al (J.Magn.Magn.Mater.2004, 277(1-2),64-70, J.Magn.Magn.Mater.2004, 283(1),8-15.) synthesized nano iron nitride powder by using a chemical vapor condensation method, and studied experimental conditions such as types and flow rates of carrier gas, working chamber atmosphere, and raw material decomposition temperature, and influence on phase formation, microstructure and magnetism of the iron nitride nano powder. The invention patent application 20171036578.2 discloses a method for synthesizing carbon-coated Fe by using soluble iron precursor as raw material and organic amine as nitrogen source through chemical solution method3N and a method for preparing the magnetic nanoparticles.
T.k.kim et al (appl.phys.lett.,1972,20,492.) under nitrogen (N)2) Middle evaporated iron to prepare Fe as main phase16N2Magnetic thin film of (2), found Fe16N2Having the highest saturation magnetization value. Nakajima et al (IEEE trans. Magn.,1998,34,542-548.) obtained Fe by implanting nitrogen ions into a single-crystal iron film16N2. In NH, Q.Huang et al (J.appl.Phys.,1994,75,6574-3/H2Iron powder is treated in a mixed atmosphere to prepare Fe16N2The composition of which was 50% of the powder sample. S.Kikkawa et al (mater.Res. bulletin,2008,43,3352-2O3Powder and nitriding at 130 ℃ for 100 hours by ammonia gas to obtain Fe16N2And (3) granules. Preparation of carbon-coated alpha' -Fe by chemical solution16N2The method for preparing the magnetic nanorod material is not reported.
Disclosure of Invention
The invention aims to provide a method for preparingPreparation of Fe16N2Method for preparing carbon-coated Fe by using nano rod material through chemical liquid phase method16N2The method has simple preparation operation and low preparation temperature, and can be used for synthesizing the carbon-coated Fe with magnetism, diameter of 20-30 nanometers, length of 0.5-3 micrometers and core-shell microstructure16N2A nanorod material.
The technical scheme of the invention is as follows:
the invention provides a method for preparing an iron nitride nanorod material, which is prepared by adopting a chemical liquid phase method and comprises the following specific steps:
(1) mixing one or more of organic solvent and surfactant, removing air, and heating to a certain temperature to obtain reaction solution.
(2) The raw material transferred into the syringe was slowly injected into the reaction solution. After the injection, the temperature is kept for a period of time.
(3) And (3) cooling the reaction system to the reaction temperature, preserving the temperature until the reaction is finished, and cooling to room temperature.
(4) The reaction product solution was centrifuged, and the supernatant was discarded to obtain a precipitated product.
(5) Washing with absolute ethyl alcohol, and drying to obtain product powder.
In the scheme, the organic solvent in the step (1) is a mixed solvent of octadecene and tetraethylenepentamine, and the volume ratio of the octadecene to the tetraethylenepentamine in the mixed organic solvent is 2:1 to 1: 2; the surfactant is oleylamine. The heating temperature is 200-220 ℃.
The dosage of the organic solvent in the step (1) of the scheme of the invention is 50-120ml, and the dosage of the surfactant is 0-40 ml. On the basis, the volume ratio of the mixed organic solvent to the surfactant is 60:1 to 60: 10.
In the scheme of the invention, in the step (2), the raw material is carbonyl iron, the dosage of the raw material is 0.05-15mmol, and the volume ratio of the reaction solution to the carbonyl iron is 60: 0.1-60: 5; and keeping the temperature for 0-30min after the injection.
The reaction temperature in step (3) of the scheme of the invention is 120-160 ℃. The heat preservation time is 3-12 days.
Hair brushThe nitride nanorod material prepared by the method for preparing the iron nitride nanorod material is Fe coated with carbon16N2The nano-rod has magnetic property; carbon coated Fe16N2The nano-rod has a shell-core microstructure, wherein the outer shell layer is carbon, and the inner core is Fe16N2。
The invention adopts a chemical liquid phase method to prepare Fe by carbon coating16N2The nano-rod material has the advantages that: simple process, low cost, no need of expensive or special reagent and equipment, and magnetic carbon-coated Fe16N2The nano rod material can be widely applied to the fields of biology, medicine, permanent magnetism and the like by utilizing the special properties of surface effect, catalysis, optics, magnetism and the like and combining the unique biological functions of biomolecules.
Drawings
FIG. 1 shows carbon-coated Fe prepared by the present invention16N2An x-ray diffraction pattern of the magnetic nanomaterial; (a) the reaction temperature is 120 ℃; (b) the reaction temperature is 130 ℃; (c) fe16N2Data of (1) x-ray diffraction standard card (# 78-1865).
FIG. 2 shows carbon-coated Fe prepared by the present invention16N2Transmission Electron Microscope (TEM) pictures of magnetic nanomaterials.
FIG. 3 shows the carbon coated Fe prepared by the present invention16N2High Resolution Transmission Electron Microscopy (HRTEM) of magnetic nanomaterials.
FIG. 4 shows the carbon coated Fe prepared by the present invention16N2X-ray photoelectron spectrum of (a).
FIG. 5 shows the carbon coated Fe prepared at 160 deg.C16N2Room temperature hysteresis loop of magnetic nanomaterials.
FIG. 6 shows that the carbon coated Fe prepared at 140 ℃ according to the present invention16N2Room temperature hysteresis loop of magnetic nanomaterials.
FIG. 7 shows the carbon coated Fe prepared at 120 ℃ according to the present invention16N2Room temperature hysteresis loop of magnetic nanomaterials.
Detailed Description
The following examples further illustrate the invention but are not intended to limit the invention thereto.
Example 1
(1) Mixing organic solvent octadecene (48ml), tetraethylenepentamine (10ml) and surfactant oleylamine (1.3ml), introducing nitrogen to remove air, and heating to 200 deg.C to obtain reaction solution.
(2) The carbonyl iron (2ml) transferred into the syringe was slowly injected into the reaction solution. After the injection, the temperature was maintained at 200 ℃ for 20 minutes.
(3) The reaction was cooled to 160 ℃ and incubated at this temperature for 6 days. Then, the reaction was terminated and the temperature was reduced to room temperature.
(4) The reaction product solution was centrifuged, and the supernatant was discarded to obtain a precipitated product.
(5) Washing with absolute ethyl alcohol, and drying to obtain product powder.
The crystal structure of the product was determined by X-ray diffraction, and it was confirmed that the phase was Fe having a tetragonal crystal structure16N2As shown in fig. 1 a. Transmission Electron Microscope (TEM) photograph showing carbon-coated Fe16N2The nano-rods have the diameter of 20-30 nanometers and the length of 0.5-3 micrometers. Due to the magnetic anisotropy, the nanorods are aligned in a certain manner, as shown in FIG. 2. Carbon coated Fe16N2A high resolution TEM photograph of the magnetic nanorod material is shown in fig. 3. FIG. 4 is a carbon-coated Fe16N2X-ray photoelectron spectrum of (a). The hysteresis loop at room temperature is shown in FIG. 5.
Example 2
The difference from the embodiment 1 is that: the carbonyl iron (1.5ml) transferred into the syringe was slowly injected into the reaction solution. After the injection, the temperature was maintained at 200 ℃ for 10 minutes. The reaction was cooled to 120 ℃ and incubated at this temperature for 6 days. Then, the reaction was terminated and the temperature was reduced to room temperature. The crystal structure of the product was determined by X-ray diffraction, and it was confirmed that the phase was Fe having a tetragonal crystal structure16N2As shown in fig. 1 b.
Example 3
The difference from the embodiment 1 is that: the reaction was cooled to 140 ℃ and incubated at this temperature for 6 days. Then, the reaction was terminated and the temperature was reduced to room temperature. Wrapping carbon with Fe16N2And (4) centrifugally separating the magnetic nanorod material, washing for 3 times by using absolute ethyl alcohol, and drying. The hysteresis loop at room temperature is shown in FIG. 6.
Example 4
The difference from the embodiment 1 is that: mixing organic solvent octadecene (40ml), tetraethylenepentamine (10ml) and surfactant oleylamine (20ml), introducing nitrogen to remove air, and heating to 220 deg.C to obtain reaction solution. The carbonyl iron (1ml) transferred into the syringe was slowly injected into the reaction solution. After the injection, the temperature was maintained at 200 ℃ for 5 minutes. The reaction was cooled to 120 ℃ and incubated at this temperature for 6 days. Then, the reaction was terminated and the temperature was reduced to room temperature. Wrapping carbon with Fe16N2And (4) centrifugally separating the magnetic nanorod material, washing for 3 times by using absolute ethyl alcohol, and drying. The hysteresis loop at room temperature is shown in FIG. 7.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (7)
1. A method for preparing iron nitride nano rod material is characterized in that carbon-coated Fe is prepared by adopting a chemical liquid phase method16N2The nanorod comprises the following specific steps:
(1) mixing one or more of an organic solvent and a surfactant, removing air, heating to 200-220 ℃ to obtain a reaction solution, wherein the organic solvent is a mixed solvent of octadecene and tetraethylenepentamine, and the surfactant is oleylamine;
(2) slowly injecting the raw material transferred into the syringe into the reaction solution; after the injection is finished, preserving the heat for a period of time, wherein the raw material is carbonyl iron;
(3) reducing the reaction system to the reaction temperature, preserving the temperature until the reaction is finished, and then reducing the temperature to the room temperature, wherein the reaction temperature is 120-160 ℃, and the preserving time is 3-12 days;
(4) centrifugally separating the reaction product solution, and discarding the supernatant to obtain a precipitate;
(5) washing with absolute ethyl alcohol, and drying to obtain product powder.
2. The method for preparing iron nitride nanorod material according to claim 1, wherein carbon-coated Fe is prepared by adopting a chemical liquid phase method16N2The nanorod comprises the following specific steps:
(1) mixing one or more of an organic solvent and a surfactant, heating to 200-220 ℃ under the protection of inert gas, preserving the temperature for more than 5 minutes, and removing water and oxygen in the system to obtain a reaction solution, wherein the organic solvent is a mixed solvent of octadecene and tetraethylenepentamine, and the surfactant is oleylamine;
(2) slowly injecting a raw material into the reaction solution through an injector, and keeping the temperature for 0-30min, wherein the raw material is carbonyl iron;
(3) reducing the reaction system to the reaction temperature, keeping the temperature until the reaction is finished, and reducing the reaction system to the room temperature, wherein the reaction temperature is 120-160 ℃, and the heat preservation time is 3-12 days;
(3) centrifugally separating the reaction product solution, and discarding the supernatant to obtain a precipitate;
(4) washing with absolute ethyl alcohol, and drying to obtain product powder.
3. A method for preparing a fe-nitride nanorod material according to claim 1 or 2, wherein: in the step (1), the volume ratio of octadecene to tetraethylenepentamine in the mixed organic solvent is 2:1 to 1: 2.
4. A method for preparing a fe-nitride nanorod material according to claim 1 or 2, wherein: the volume ratio of the reaction solution to the carbonyl iron in the step (2) is 60:0.1 to 60: 5.
5. A method for preparing a fe-nitride nanorod material according to claim 1 or 2, wherein: in the step (1), the dosage of the organic solvent is 50-120ml, and the dosage of the surfactant is 0-40 ml; the consumption of raw materials in the step (2) is 0.05-15 mmol.
6. The method of preparing an iron nitride nanorod material according to claim 5, wherein the iron nitride nanorod material comprises: the volume ratio of the mixed organic solvent to the surfactant in the step (1) is 60:1 to 60: 10.
7. A material produced by the method for producing an iron nitride nanorod material according to claim 1 or 2, wherein: the iron nitride nanorod material has magnetic performance, and the shell of the iron nitride nanorod is carbon.
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| ES2365082B1 (en) * | 2010-03-08 | 2012-08-08 | Consejo Superior De Investigaciones Científicas (Csic) | PROCEDURE FOR OBTAINING MATERIALS WITH SUPERPARAMAGNETIC BEHAVIOR |
| US8597420B2 (en) * | 2011-03-17 | 2013-12-03 | Xerox Corporation | Solvent-based inks comprising coated magnetic nanoparticles |
| CN106165027A (en) * | 2014-03-28 | 2016-11-23 | 明尼苏达大学董事会 | Comprise the iron nitride magnetic material of the nano-particle of coating |
| US10072356B2 (en) * | 2014-08-08 | 2018-09-11 | Regents Of The University Of Minnesota | Magnetic material including α″-Fe16(NxZ1-x)2 or a mixture of α″-Fe16Z2 and α″-Fe16N2, where Z includes at least one of C, B, or O |
| CN107162064B (en) * | 2017-06-26 | 2019-05-31 | 浙江工业大学 | A kind of method that high-temperature decomposition prepares ferrous fluoride nano material |
| CN109215913B (en) * | 2017-07-04 | 2021-03-02 | 中国科学院金属研究所 | Method for preparing carbon-coated iron nitride and composite magnetic nano material thereof |
| CN109461557B (en) * | 2017-09-06 | 2020-08-11 | 中国科学院金属研究所 | Ordered inorganic-organic hybrid nano material with room temperature ferrimagnetism and preparation |
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