CN103170640B

CN103170640B - A kind of method of Microwave synthesize FeNi nanometer rods

Info

Publication number: CN103170640B
Application number: CN201110436654.5A
Authority: CN
Inventors: 温佳昊; 彭锦; 吴庆生; 黄再娣; 王娜
Original assignee: Tongji University
Current assignee: Tongji University
Priority date: 2011-12-22
Filing date: 2011-12-22
Publication date: 2015-08-19
Anticipated expiration: 2031-12-22
Also published as: CN103170640A

Abstract

The present invention relates to a kind of method of Microwave synthesize FeNi nanometer rods, the method is using nickeliferous inorganic salts and contain iron complex as pre-reaction material, pre-reaction material, hydrazine hydrate reduction agent, reaction medium ethylene glycol are placed in heating using microwave instrument, be heated to 180 DEG C with certain heating rate, react and can obtain FeNi nanometer rods in 4 minutes.Compared with prior art, the inventive method is consuming time short, easy to operate, easy to control, and can prepare size uniform, has the FeNi nanometer rods of magnetic and catalytic activity.

Description

A kind of method of Microwave synthesize FeNi nanometer rods

Technical field

The invention belongs to technical field of nano material, relate to a kind of new method of Microwave synthesize FeNi nanometer rods.

Background technology

One dimension ferrous metals nano material not only has the various special effectses of common nano particle, and there is unique shape anisotropy and magnetic anisotropy, be the important constituent element constructing electromagnet functional material, in fields such as high density magnetic recording, sensitive components, electro-magnetic wave absorption, catalyst, medical science and Biofunctional materials, there is important application.Wherein the functional material synthesizing a new generation of Fe base Nanoalloy material opens new approach.

Fe, Co, Ni transition elements is considered to element the most outstanding in above field, and because the material such as nanotube and nanometer rods of its one dimension have many excellent properties, being studied by physics and chemistry method and being applied in the method prepared on these materials is had: ball-milling method, electrochemical deposition, laser ablation, chemical vapour deposition (CVD), sputtering method, spray-on process, chemical reduction method etc.These methods prepare not only complex process, are not easy operation and control, and length consuming time.Therefore, how obtaining the FeNi alloy nano-material of one dimension by a kind of simply controlled and short method consuming time, is a significant research topic.

Summary of the invention

Object of the present invention is exactly the defect existed to overcome existing technology of preparing, and provides a kind of new microwave synthesis method to prepare the FeNi nanometer rods with magnetic and excellent catalytic activity.

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

A kind of method of Microwave synthesize FeNi nanometer rods, it is characterized in that, the method is using nickeliferous inorganic salts and contain iron complex as precursors, precursors, reducing agent hydrazine hydrate, reaction medium ethylene glycol are placed in heating using microwave instrument by a certain percentage, 180 DEG C are heated to the heating rate of 30-60 DEG C/min, by the heating using microwave reaction that total time is 4-8 minute, prepare FeNi nanometer rods.

The method specifically comprises the following steps:

(1) nickeliferous inorganic salts are dissolved in deionized water are mixed with certain density solution with containing iron complex, then adding a certain proportion of ethylene glycol and hydrazine hydrate is mixed with mixed solution, is wherein 5: 1 ~ 10: 1 containing iron complex and nickeliferous inorganic salts mole ratio; The mol ratio of total material amount of ethylene glycol and molysite and nickel salt is 50: 1 ~ 80: 1; The mol ratio of total amount of substance of hydrazine hydrate and molysite and nickel salt is 1: 15 ~ 1: 50;

(2) mixed solution step (1) obtained moves in microwave reaction flask, is heated to 180 DEG C with the heating rate of 30-60 DEG C/min, and setting computer heating control program makes whole heating process continue 4-8 minute.Reaction is cooled under field conditions (factors), is repeatedly washed by centrifugation deionized water and ethanol after stopping, and obtaining end product is black FeNi alloy nano rod.

Described nickeliferous inorganic salts are nickel chloride or nickel nitrate.

Described is ferric oxalate or ferrous oxalate containing iron complex.

Described heating rate is 40-45 DEG C/min.

Washing described in step (2) uses deionized water and absolute ethyl alcohol to carry out alternately washing respectively.

Compared with prior art, the inventive method is consuming time short, easy to operate and easy to control, can prepare size uniformity, has the FeNi nanometer rods of magnetic and excellent degraded catalytic activity.

Accompanying drawing explanation

Fig. 1 is the scanning electron microscope (SEM) photograph of the product of embodiment 1;

Fig. 2 is the scanning electron microscope (SEM) photograph of the product of embodiment 2;

Fig. 3 is products therefrom power spectrum (EDS) in embodiment 1;

Fig. 4 is the X-alpha spectrum (XRD) of products therefrom in embodiment 1.

Detailed description of the invention

Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.

Embodiment 1

The first step, take 0.9318g ferric oxalate (AR) and be dissolved in the ferric oxalate solution that 50mL volumetric flask is made into 0.04mol/L, take 0.2378g Nickel dichloride hexahydrate (AR) and be dissolved in the Nickel dichloride hexahydrate solution that 25mL volumetric flask is made into 0.04mol/L.

Second step, measures the ferric oxalate solution of the 0.04mol/L of 1.00mL, the Nickel dichloride hexahydrate solution of the 0.04mol/L of 0.20mL, 10mL ethylene glycol (AR) solution in 50mL beaker, ultrasonic ten minutes.Again in MAS-II type normal pressure microwave synthesis/extractive reaction work station, select following microwave heating treatment scheme.

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

3rd step, washes out product 10ml ethanolic solution, occurs that black powder precipitates in product mixture.Ultrasonic process mixed liquor, makes its as far as possible dispersion in ethanolic solution, and then under the speed of 5000 revs/min centrifugal 10 minutes, discard supernatant liquor, used the same method deionized water, absolute ethyl alcohol, alternately washs, centrifugal 5-10 time.Final sample is scattered in absolute ethyl alcohol, analyzes sample.

As can be seen from ESEM (Fig. 1), product is one-dimensional rod-like structure.Can be found out by energy chromatogram (EDS, accompanying drawing 3), product consists of Fe and Ni, and the copper mesh substrate used when the Cu in figure is test causes.The structural characterization XRD collection of illustrative plates (Fig. 4) carried out from Powder X-ray Diffractometer, product is the FCC structure of FeNi alloy.

Embodiment 2

Measure the ferric oxalate solution of the 0.04mol/L of 1.0mL, the Nickel dichloride hexahydrate solution of the 0.04mol/L of 0.10mL, pvp0.0103g, 10mL ethylene glycol (AR) solution in 50mL beaker, ultrasonic ten minutes.Again in MAS-II type normal pressure microwave synthesis/extractive reaction work station, microwave heating treatment scheme.

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

After reaction terminates, be cooled to room temperature, all the other steps operate by embodiment 1.

As can be seen from ESEM (Fig. 2), product is one-dimensional rod-like structure.

Embodiment 3

A kind of method of Microwave synthesize FeNi nanometer rods, using nickeliferous inorganic salts and containing iron complex as precursors, precursors, reducing agent hydrazine hydrate, reaction medium ethylene glycol are placed in heating using microwave instrument, 180 DEG C are heated to certain heating rate, prepare FeNi nanometer rods, specifically comprise the following steps:

(1) nickel chloride and ferric oxalate are dissolved in deionized water and are mixed with solution, then add ethylene glycol and hydrazine hydrate is mixed with mixed solution, wherein ferric oxalate and nickel chloride mole ratio are 5: 1; The mol ratio of total material amount of ethylene glycol and nickel chloride and ferric oxalate is 50: 1; The mol ratio of total amount of substance of hydrazine hydrate and nickel chloride and ferric oxalate is 1: 15;

(2) mixed solution step (1) obtained moves in microwave reaction flask, control heating rate is heating rate is 30 DEG C/min, be heated to 180 DEG C, then cool under field conditions (factors), after reaction terminates, washing, centrifugation, obtains end product black alloy FeNi nanometer rods.

Embodiment 4

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

(2) mixed solution step (1) obtained moves in microwave reaction flask, control heating rate is heating rate is that 40 DEG C/min is heated to 180 DEG C, then cool under field conditions (factors), after reaction terminates, washing, centrifugation, obtains end product black alloy FeNi nanometer rods.

Claims

1. the method for a Microwave synthesize FeNi nanometer rods, it is characterized in that, the method is using nickeliferous inorganic salts and contain iron complex as precursors, precursors, hydrazine hydrate reduction agent, reaction medium ethylene glycol are placed in heating using microwave instrument, 180 DEG C are heated to certain heating rate, prepare FeNi nanometer rods by the reaction time of 4-8 minute, utilize the predecessor reaction system of the certain proportioning of short time heating using microwave, the method specifically comprises the following steps:

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

(2) mixed solution step (1) obtained moves in microwave reaction flask, 180 DEG C are heated to the heating rate of 30 ~ 60 DEG C/min, setting computer heating control program makes whole heating process continue 4 ~ 8 minutes, after reaction stops, cool under field conditions (factors), repeatedly washed by centrifugation deionized water and ethanol, obtaining end product is black FeNi alloy nano rod.

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

3. the method for a kind of Microwave synthesize FeNi nanometer rods according to claim 1, is characterized in that described is ferric oxalate or ferrous oxalate containing iron complex.

4. the method for a kind of Microwave synthesize FeNi nanometer rods according to claim 1, it is characterized in that, described heating rate is 40 ~ 45 DEG C/min.

5. the method for a kind of Microwave synthesize FeNi nanometer rods according to claim 1, is characterized in that the washing described in step (2) uses deionized water and absolute ethyl alcohol to carry out alternately washing respectively.