CN103170640A

CN103170640A - Method for FeNi nanorod synthesis through microwaves

Info

Publication number: CN103170640A
Application number: CN2011104366545A
Authority: CN
Inventors: 温佳昊; 彭锦; 吴庆生; 王娜
Original assignee: Tongji University
Current assignee: Tongji University
Priority date: 2011-12-22
Filing date: 2011-12-22
Publication date: 2013-06-26
Anticipated expiration: 2031-12-22
Also published as: CN103170640B

Abstract

The invention relates to a method for FeNi narorod synthesis through microwaves. According to the method, nickeliferous inorganic salt and coordination compound containing iron serve as reaction precursors. The reaction precursor, a hydrazine hydrate reducing agent and reaction medium ethylene glycol are placed in a microwave heating instrument and are heated to the temperature of 180 DEG C at a certain heating rate and after 4 minutes of reaction, a FeNi nanorod can be obtained. Compared with the prior art, the method for the FeNi narorod synthesis through the microwaves is short in time consumption, easy to operate and control and capable of preparing the FeNi narorod with even dimension, magnetism and catalytic activity.

Description

The method of the synthetic FeNi nanometer rods of a kind of microwave

Technical field

The invention belongs to technical field of nano material, relate to the new method of the synthetic FeNi nanometer rods of a kind of microwave.

Background technology

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

Fe, Co, the Ni transition elements is considered to element the most outstanding in above field, due to the material of its one dimension for example nanotube and nanometer rods have many excellent properties, the method for studying and being applied on these materials of preparation by the physics and chemistry method has: 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, and be not easy operation and control, and length consuming time.Therefore, how obtaining the FeNi alloy nano-material of one dimension with a kind of simple controlled and short method consuming time, is a significant research topic.

Summary of the invention

Purpose of the present invention is exactly the defective that exists in order 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.

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

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

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 and hydrazine hydrate to be mixed with mixed solution, wherein contain iron complex and nickeliferous inorganic salts mole ratio is 5: 1～10: 1; The mol ratio of total 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 that step (1) obtained moves in the microwave reaction flask, is heated to 180 ℃ with the heating rate of 30-60 ℃/min, sets to add thermal control program and makes whole heating process continue 4-8 minute.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.

Described nickeliferous inorganic salts are nickel chloride or nickel nitrate.

The described iron complex that contains is ferric oxalate or ferrous oxalate.

Described heating rate is 40-45 ℃/min.

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

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

Description of drawings

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.

The specific embodiment

The present invention is described in detail below in conjunction with the drawings and specific embodiments.

Embodiment 1

The first step takes 0.9318g ferric oxalate (AR) and is dissolved in the ferric oxalate solution that the 50mL volumetric flask is made into 0.04mol/L, takes 0.2378g Nickel dichloride hexahydrate (AR) and is dissolved in the Nickel dichloride hexahydrate solution that the 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 the 50mL beaker, ultrasonic ten minutes.Again MAS-II type normal pressure microwave synthetic/the extractive reaction work station in, select following microwave heating treatment scheme.

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

The 3rd step washed out product with the 10ml ethanolic solution, occur the black powder precipitation in the product mixed liquor.Ultrasonic processing mixed liquor disperses it as far as possible in ethanolic solution, and then under the speed of 5000 rev/mins centrifugal 10 minutes, discard supernatant liquor, the deionized water that uses the same method, absolute ethyl alcohol alternately washs, centrifugal 5-10 time.Final sample is scattered in absolute ethyl alcohol, and sample is analyzed.

(Fig. 1) can find out by ESEM, and product is the one-dimensional rod-like structure.Can be found out by energy chromatogram (EDS, accompanying drawing 3), product composition is Fe and Ni, and the copper mesh substrate of using when the Cu in figure is test causes.The structural characterization XRD collection of illustrative plates (Fig. 4) that is undertaken by the powder x-ray diffraction instrument as seen, 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 the 50mL beaker, ultrasonic ten minutes.Again MAS-II type normal pressure microwave synthetic/the extractive reaction work station in, the microwave heating treatment scheme.

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

Reaction is cooled to room temperature after finishing, and all the other steps operate by embodiment 1.

(Fig. 2) can find out by ESEM, and product is the one-dimensional rod-like structure.

Embodiment 3

The method of the synthetic FeNi nanometer rods of a kind of microwave, with nickeliferous inorganic salts and contain iron complex as precursors, precursors, reducing agent hydrazine hydrate, 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, specifically comprise the following steps:

(1) nickel chloride and ferric oxalate are dissolved in are mixed with solution in deionized water, then add ethylene glycol and hydrazine hydrate to be mixed with mixed solution, wherein ferric oxalate and nickel chloride mole ratio are 5: 1; The mol ratio of total 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 that step (1) is obtained moves in the microwave reaction flask, and controlling heating rate is that heating rate is 30 ℃/min, is heated to 180 ℃, then cooling under field conditions (factors), after reaction finishes, washing, centrifugation obtains end product black alloy FeNi nanometer rods.

Embodiment 4

(1) nickel nitrate and ferrous oxalate are dissolved in are mixed with solution in deionized water, then add ethylene glycol and hydrazine hydrate to be mixed with mixed solution, wherein ferrous oxalate and nickel nitrate mole ratio are 10: 1; The mol ratio of total 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 that step (1) is obtained moves in the microwave reaction flask, and controlling heating rate is that heating rate is that 40 ℃/min is heated to 180 ℃, then cooling under field conditions (factors), after reaction finishes, washing, centrifugation obtains end product black alloy FeNi nanometer rods.

Claims

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.