CN103170640A - Method for FeNi nanorod synthesis through microwaves - Google Patents

Abstract

The invention relates to a method for synthesizing FeNi nanorods by microwave. In the method, nickel-containing inorganic salts and iron-containing complexes are used as reaction precursors, and the reaction precursors, hydrazine hydrate reducing agent, and reaction medium ethylene glycol are placed in a microwave heating instrument. FeNi nanorods can be prepared by heating to 180°C at a certain heating rate and reacting for 4 minutes. Compared with the prior art, the method of the invention is short in time consumption, easy to operate and easy to control, and can prepare FeNi nanorods with uniform size, magnetism and catalytic activity.

Description

A method for microwave synthesis of FeNi nanorods

technical field

The invention belongs to the technical field of nanometer materials, and relates to a new method for synthesizing FeNi nanorods by microwave.

Background technique

One-dimensional iron-based metal nanomaterials not only have various special effects of ordinary nanoparticles, but also have unique shape anisotropy and magnetic anisotropy. They are important components in the construction of new electromagnetic functional materials. It has important applications in the fields of components, electromagnetic wave absorption, catalysts, medicine and biofunctional materials. Among them, the synthesis of Fe-based nano-alloy materials has opened up a new way for a new generation of functional materials.

Fe, Co, and Ni transition elements are considered to be the most outstanding elements in the above fields. Due to their one-dimensional materials such as nanotubes and nanorods have many excellent properties, they are studied and applied in the preparation of these materials by physical and chemical methods. The above methods are: ball milling method, electrochemical deposition, laser etching, chemical vapor deposition, sputtering method, spray method, chemical reduction method and so on. These methods are not only complicated in process, not easy to operate and control, but also time-consuming. Therefore, how to use a simple, controllable and short time-consuming method to obtain one-dimensional FeNi alloy nanomaterials is a research topic of great significance.

Contents of the invention

The purpose of the present invention is to provide a new microwave synthesis method to prepare FeNi nanorods with magnetism and excellent catalytic activity in order to overcome the defects in the existing preparation technology.

The purpose of the present invention can be achieved through the following technical solutions:

A method for microwave synthesis of FeNi nanorods, characterized in that the method uses nickel-containing inorganic salts and iron-containing complexes as reaction precursors, and the reaction precursors, reducing agent hydrazine hydrate, and reaction medium ethylene glycol are placed in a certain proportion. In a microwave heating apparatus, heat up to 180° C. at a heating rate of 30-60° C./min, and prepare FeNi nanorods through a microwave heating reaction with a total time of 4-8 minutes.

The method specifically includes the following steps:

(1) Dissolve nickel-containing inorganic salts and iron-containing complexes in deionized water to prepare a solution of a certain concentration, and then add a certain proportion of ethylene glycol and hydrazine hydrate to prepare a mixed solution, wherein the iron-containing complexes and nickel-containing inorganic salts The molar ratio is 5:1 to 10:1; the molar ratio of ethylene glycol to the total mass of iron salt and nickel salt is 50:1 to 80:1; the total mass of hydrazine hydrate to iron salt and nickel salt The molar ratio is 1:15～1:50;

(2) Transfer the mixed solution obtained in step (1) into a microwave reaction flask, heat to 180° C. at a heating rate of 30-60° C./min, and set a heating control program so that the entire heating process lasts for 4-8 minutes. After the reaction was stopped, it was cooled under natural conditions, and washed several times with deionized water and ethanol by centrifugation to obtain the final product as black FeNi alloy nanorods.

The nickel-containing inorganic salt is nickel chloride or nickel nitrate.

The iron-containing complex is ferric oxalate or ferrous oxalate.

The heating rate is 40-45° C./min.

The washing described in step (2) is alternately washed with deionized water and absolute ethanol respectively.

Compared with the prior art, the method of the invention is time-consuming, easy to operate and easy to control, and can prepare FeNi nanorods with uniform size, magnetism and excellent degradation catalytic activity.

Description of drawings

Fig. 1 is the scanning electron micrograph of the product of embodiment 1;

Fig. 2 is the scanning electron micrograph of the product of embodiment 2;

Fig. 3 is obtained product energy spectrum (EDS) in embodiment 1;

FIG. 4 is the X-ray spectrum (XRD) of the product obtained in Example 1.

Detailed ways

The present invention will be described in detail below in conjunction with the accompanying drawings and specific embodiments.

Example 1

The first step, weigh 0.9318g ferric oxalate (AR) and dissolve in 50mL volumetric flask to make 0.04mol/L ferric oxalate solution, weigh 0.2378g hexahydrate nickel chloride (AR) and dissolve in 25mL volumetric flask to make 0.04mol /L of nickel chloride hexahydrate solution.

In the second step, measure 1.00 mL of 0.04 mol/L ferric oxalate solution, 0.20 mL of 0.04 mol/L nickel chloride hexahydrate solution, and 10 mL of ethylene glycol (AR) solution in a 50 mL beaker, and sonicate for ten minutes. Then in the MAS-II atmospheric pressure microwave synthesis/extraction reaction workstation, select the following microwave heating treatment scheme.

P/w T/℃ t/s 300 80 60 300 120 60 300 180 120

In the third step, the reaction product was washed out with 10 ml of ethanol solution, and a black powder precipitate appeared in the product mixture. Sonicate the mixed solution to disperse it in the ethanol solution as much as possible, then centrifuge at a speed of 5000 rpm for 10 minutes, discard the supernatant, use the same method to wash and centrifuge alternately with deionized water and absolute ethanol 5-10 times. Finally, the sample was dispersed in absolute ethanol, and the sample was analyzed.

It can be seen from the scanning electron microscope (Fig. 1) that the product has a one-dimensional rod-like structure. It can be seen from the energy chromatogram (EDS, Figure 3) that the product is composed of Fe and Ni, and the Cu in the figure is caused by the copper mesh substrate used in the test. Structural characterization by powder X-ray diffractometer The XRD spectrum ( FIG. 4 ) shows that the product is the FCC structure of FeNi alloy.

Example 2

Measure 1.0mL of 0.04mol/L ferric oxalate solution, 0.10mL of 0.04mol/L nickel chloride hexahydrate solution, pvp0.0103g, 10mL ethylene glycol (AR) solution in a 50mL beaker, and ultrasonic for ten minutes. Then in the MAS-II atmospheric pressure microwave synthesis/extraction reaction workstation, microwave heating treatment scheme.

P/w T/℃ t/s 300 80 60 300 120 60 300 180 120

After the reaction was finished, it was cooled to room temperature, and the rest of the steps were operated as in Example 1.

It can be seen from the scanning electron microscope (Fig. 2) that the product has a one-dimensional rod-like structure.

Example 3

A method for synthesizing FeNi nanorods by microwave, using nickel-containing inorganic salts and iron-containing complexes as reaction precursors, placing the reaction precursors, reducing agent hydrazine hydrate, and reaction medium ethylene glycol in a microwave heating instrument, with a certain The heating rate is heated to 180° C. to prepare FeNi nanorods, which specifically includes the following steps:

(1) Dissolving nickel chloride and ferric oxalate in deionized water is prepared into a solution, then adding ethylene glycol and hydrazine hydrate to prepare a mixed solution, wherein the molar ratio of ferric oxalate to nickel chloride is 5: 1; ethylene glycol and The mol ratio of the total substance amount of nickel chloride and ferric oxalate is 50: 1; The mol ratio of the total substance amount of hydrazine hydrate and nickel chloride and ferric oxalate is 1: 15;

(2) Move the mixed solution obtained in step (1) into a microwave reaction flask, control the heating rate to be 30°C/min, heat to 180°C, then cool under natural conditions, wash and centrifuge after the reaction is over , to obtain the final product black alloy FeNi nanorods.

Example 4

A method for synthesizing FeNi nanorods by microwave, using nickel-containing inorganic salts and iron-containing complexes as reaction precursors, placing the reaction precursors, reducing agent hydrazine hydrate, and reaction medium ethylene glycol in a microwave heating instrument, with a certain The heating rate is heated to 180° C. to prepare FeNi nanorods, which specifically includes the following steps:

(1) nickel nitrate and ferrous oxalate are dissolved in deionized water to prepare a solution, then add ethylene glycol and hydrazine hydrate to prepare a mixed solution, wherein the molar ratio of ferrous oxalate to nickel nitrate is 10:1; ethylene glycol and The mol ratio of the total substance amount of ferrous oxalate and nickel nitrate is 80: 1; The mol ratio of the total substance amount of hydrazine hydrate and ferrous oxalate and nickel nitrate is 1: 50;

(2) Move the mixed solution obtained in step (1) into a microwave reaction flask, control the heating rate to be 40° C./min and heat to 180° C., then cool under natural conditions. After the reaction is completed, wash and centrifuge, The final product black alloy FeNi nanorods was obtained.

Claims (6)

1. the method for the synthetic FeNi nanometer rods of a microwave, it is characterized in that, the method is with nickeliferous inorganic salts and contain iron complex as precursors, precursors, hydrazine hydrate reduction agent, reaction medium ethylene glycol are placed in the heating using microwave instrument, be heated to 180 ℃ with certain heating rate, prepare the FeNi nanometer rods by the reaction time of 4-8 minute.

2. a kind of microwave according to claim 1 synthesizes the method for FeNi nanometer rods, it is characterized in that utilizing the predecessor reaction system of the certain proportioning of short time heating using microwave, and the method specifically comprises the following steps:

(1) with nickeliferous inorganic salts with contain iron complex and be dissolved in and be mixed with certain density solution in deionized water, then add a certain proportion of ethylene glycol to be mixed with mixed solution as solvent and a certain amount of hydrazine hydrate as reducing agent, wherein contain iron complex and nickeliferous inorganic salts mole ratio is 5: 1～10: 1; Ethylene glycol is 50: 1～80: 1 with the mol ratio that contains total amount of iron complex and nickeliferous inorganic salts; The mol ratio that contains total amount of substance of iron complex and nickeliferous inorganic salts in hydrazine hydrate and presoma is 1: 15～1: 50;

(2) mixed solution that step (1) is obtained moves in the microwave reaction flask, heating rate with 30～60 ℃/min is heated to 180 ℃, setting adds thermal control program makes whole heating process continue 4～8 minutes, after reaction stops, cooling under field conditions (factors), use deionized water and ethanol repeatedly to wash by centrifugation, obtaining end product is black FeNi alloy nano rod.

3. the method for the synthetic FeNi nanometer rods of a kind of microwave according to claim 1 and 2, is characterized in that described nickeliferous inorganic salts are nickel chloride or nickel nitrate.

4. the method for the synthetic FeNi nanometer rods of a kind of microwave according to claim 1 and 2, is characterized in that the described iron complex that contains is ferric oxalate or ferrous oxalate.

5. the method for the synthetic FeNi nanometer rods of a kind of microwave according to claim 1 and 2, is characterized in that, described heating rate is 40～45 ℃/min.

6. the method for the synthetic FeNi nanometer rods of a kind of microwave according to claim 2 is characterized in that the washing described in step (2) uses respectively deionized water and absolute ethyl alcohol to replace washing.

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