CN101586019B - Ferriferous oxide/tin oxide core-shell nanometer rod absorbing high-frequency electromagnetic wave and preparing method thereof - Google Patents

Ferriferous oxide/tin oxide core-shell nanometer rod absorbing high-frequency electromagnetic wave and preparing method thereof Download PDF

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CN101586019B
CN101586019B CN2009100716773A CN200910071677A CN101586019B CN 101586019 B CN101586019 B CN 101586019B CN 2009100716773 A CN2009100716773 A CN 2009100716773A CN 200910071677 A CN200910071677 A CN 200910071677A CN 101586019 B CN101586019 B CN 101586019B
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nanometer rod
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autoclave
core
ethanol
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CN101586019A (en
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陈玉金
朱春玲
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Harbin Engineering University
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Abstract

The present invention provides a ferriferous oxide/tin oxide core-shell nanometer rod absorbing high-frequency electromagnetic wave and a preparing method thereof. The FeCl3 solution with the concentration of 0.25-1.0mol/L is placed in a hermetical high-pressure autoclave made of stainless steel and is kept for 12 hours in a baking oven in the temperature of 100-120 DEG C. After the high-pressure autoclave is naturally cooled to the room temperature, the deposit in the autoclave is cleaned with water and ethanol. After being dried at the temperature of 80 DEG C, the beta-FeOOH nanometer rod is obtained. Then the beta-FeOOH nanometer rod is annealed for 2.5 hours at the temperature of 500 DEG C to obtain the alpha-Fe2O3 nanometer rod. The 0.08g of alpha-Fe2O3 nanometer rod is ultrasonically dispersed into 32ml of water-ethanol solution. Then 0.75g of urea and 0.115g of potassium stannate are added. After being mixed, the obtained solution is placed in the hermetical high-pressure autoclave made of stainless steel and is kept for 36 hours in the baking oven at the temperature of 170 DEG C. After the high-pressure autoclave is naturally cooled to the room temperature, the deposit in the autoclave is cleaned with water and ethanol. After being dried at the temperature of 80 DEG C, the alpha-Fe2O3/SnO2 core-shell nanometer rod is obtained. The alpha-Fe2O3/SnO2 core-shell nanometer rod is annealed for 7 hours in the atmosphere of N2/H2 in which the volume of the H2 accounts for 8% for obtaining the porous ferriferous oxide/tin oxide nanometer rod. The method of the invention has the advantages of simple operation and suitability for the industrial production.

Description

The electromagnetic Z 250 of absorbing high-frequency/White tin oxide core-shell nanometer rod and method for making
(1) technical field
The present invention relates to a kind of nano material, specifically a kind of porous ferroferric oxide/White tin oxide core-shell nanometer rod that frequency electromagnetic waves is had strong absorption characteristic.The invention still further relates to a kind of preparation method who frequency electromagnetic waves is had the porous ferroferric oxide/White tin oxide core-shell nanometer rod of strong absorption characteristic.
(2) background technology
Along with developing rapidly of nanosecond science and technology, the application of nano material in the absorption of electromagnetic wave field received extensive concern both domestic and external.Metal magnetic nano particle such as iron, cobalt, nickel etc. have the bigger specific magnetising moment and " the Snooker limit " in high-frequency range.Therefore, they can the absorbing high-frequency hertzian wave.But the electricity of these metallic particles is led bigger, under the effect in outfield, can produce eddy-current loss, thereby its absorption of electromagnetic wave performance is significantly descended.Carbon nanotube has special construction and excellent electrology characteristic, and Recent study person has carried out research comparatively widely to their high-frequency electromagnetic response characteristic.From microcosmic electromagnetic response mechanism analysis, the electromagnetic attenuation characteristic of simple carbon nanotube only comes from dielectric loss.For fear of the influence of husband's effect to hertzian wave fade performance in high-frequency range that become, the addition of carbon nanotube in body material can not be too high.Yet the reduction meeting of addition significantly reduces their electromagnetic response characteristic.At inner magnetic, coating or the doped magnetic medium of filling of carbon nanotube, make it have ferromagnetism, can introduce magnetic loss factor.In this case, the carbon nanotube of filling magnetic medium has demonstrated the enhanced absorption characteristic to the hertzian wave in the high-frequency range.Yet, consider the length of carbon nanotube and the complexity that port is opened, realize that magnetic is a large amount of in carbon nanotube, evenly filling is still waiting further perfect.Therefore, realize that a large amount of, controlled preparation, high-level efficiency electromagnetic absorber also exist problems to need to solve at present.For example, 2004 we utilize thermal evaporation techniques to synthesize the ZnO nano material.This nano material can absorb hertzian wave, but the width of absorption frequency and absorption intensity are all lower.This work was published on " Appl.Phys.Lett. " 91 phases in 2004, and thesis topic is " Microwave absorption propertiesand mechanism of cagelike ZnO/SiO 2Nanocomposites ".According to electromagnetic transmission lineation opinion, when dielectric loss and magnetic loss were mated each other, material could show the strongest electromaganic wave absorbing property.Therefore, how to realize to frequency electromagnetic waves have absorption characteristic nano material a large amount of preparations and how to mate electrical loss and magnetic loss is current main difficult technical.
(3) summary of the invention
The object of the present invention is to provide a kind of Z 250/White tin oxide core-shell nanometer rod that frequency electromagnetic waves is had the absorbing high-frequency hertzian wave tool of strong absorption characteristic.The present invention also aims to provide a kind of method for making of Z 250/White tin oxide core-shell nanometer rod of simple to operate, the absorbing high-frequency hertzian wave tool that is suitable for suitability for industrialized production.
The objective of the invention is to realize like this:
The Z 250 of absorbing high-frequency hertzian wave tool of the present invention/White tin oxide core-shell nanometer rod is: (1) is with the FeCl of 0.25-1.0mol/L 3Solution places in the autoclave of stainless steel sealing, in baking oven, keeps 12 hours in 100-120 ℃, treat that autoclave naturally cools to room temperature after; Deposition water in the still and ethanol are cleaned; Obtain β-FeOOH nanometer rod after 80 ℃ of following dryings, in 500 ℃ of annealing 2.5 hours, obtain α-Fe again 2O 3Nanometer rod; (2) with 0.08g α-Fe 2O 3The nanometer rod ultra-sonic dispersion is in 32ml water-ethanol solution; Add 0.75g urea and 0.115g potassium stannate then, after the stirring, above-mentioned solution is placed in the autoclave of stainless steel sealing; In baking oven, kept 36 hours in 170 ℃; After treating that autoclave naturally cools to room temperature, deposition water in the still and ethanol are cleaned, obtain α-Fe after 80 ℃ of following dryings 2O 3/ SnO 2Core-shell nanometer rod; (3) with α-Fe 2O 3/ SnO 2Core-shell nanometer rod is at H 2Volume accounts for 8% N 2/ H 2Under the atmosphere, in 400 ℃ of annealing 7 hours, the length in the hole that obtains and diameter were respectively the porous ferroferric oxide/tin oxide nano rod of 10-60 and 5-30 nanometer.
The method for making of the Z 250 of absorbing high-frequency hertzian wave tool of the present invention/White tin oxide core-shell nanometer rod is:
(1) with the FeCl of 0.25-1.0mol/L 3Solution places in the autoclave of stainless steel sealing, in baking oven, keeps 12 hours in 100-120 ℃, treat that autoclave naturally cools to room temperature after; Deposition water in the still and ethanol are cleaned; Obtain β-FeOOH nanometer rod after 80 ℃ of following dryings, in 500 ℃ of annealing 2.5 hours, obtain α-Fe again 2O 3Nanometer rod;
(2) with 0.08g α-Fe 2O 3The nanometer rod ultra-sonic dispersion is in 32ml water-ethanol solution; Add 0.75g urea and 0.115g potassium stannate then, after the stirring, above-mentioned solution is placed in the autoclave of stainless steel sealing; In baking oven, kept 36 hours in 170 ℃; After treating that autoclave naturally cools to room temperature, deposition water in the still and ethanol are cleaned, obtain α-Fe after 80 ℃ of following dryings 2O 3/ SnO 2Core-shell nanometer rod;
(3) with α-Fe 2O 3/ SnO 2Core-shell nanometer rod is at H 2Volume accounts for 8% N 2/ H 2Under the atmosphere,, obtain porous ferroferric oxide/tin oxide nano rod in 400 ℃ of annealing 7 hours.
With porous ferroferric oxide of the present invention/tin oxide nano rod preparation 80wt% porous ferroferric oxide/tin oxide nano rod-paraffin composite film material, utilize its electromagnetic parameter of T/R coaxial transmission line test.Utilize electromagnetic transmission lineation opinion to calculate the reflection of electromagnetic wave rate of different film thicknesses at last.
The invention provides a kind of porous Fe that frequency electromagnetic waves is had strong absorption characteristic 3O 4/ SnO 2The preparation method of core-shell nanometer rod.Utilize the film of porous ferroferric oxide/tin oxide nano rod preparation, when thickness was 4mm, bill of material revealed the double frequency absorption characteristic, and its absorption intensity all reached-below the 20dB.
Preparing method of the present invention is simple to operate, be suitable for suitability for industrialized production, can prepare the porous ferroferric oxide/White tin oxide core-shell nanometer rod that frequency electromagnetic waves is had strong absorption characteristic.
(4) description of drawings
Fig. 1 is α-Fe 2O 3/ SnO 2The pattern of core-shell nanometer rod and structure.A) transmission electron microscope picture, illustration are α-Fe 2O 3SEAD b) transmission electron microscope picture that amplifies.
Fig. 2 is the pattern and the structure of porous ferroferric oxide/tin oxide nano rod.A) transmission electron microscope picture, illustration is respectively Fe 3O 4Full resolution pricture and SEAD b) transmission electron microscope picture that amplifies.
Fig. 3 is the electromagnetic parameter of porous ferroferric oxide/tin oxide nano rod-paraffin mixture.Fig. 3 (a) complex permittivity, Fig. 3 (b) complex permeability.
Fig. 4 is the dielectric loss and the magnetic loss tangent value of porous ferroferric oxide/tin oxide nano rod-paraffin mixture.
Fig. 5 is the porous ferroferric oxide/reflection of electromagnetic wave rate of tin oxide nano rod-paraffin mixture under different concns.
(5) embodiment
For example the present invention is done in more detail below and describes:
Embodiment 1:
(1) with the FeCl of 40 milliliters 0.5mol/L 3Solution places in the autoclave of 50ml stainless steel sealing.In baking oven, kept 12 hours in 120 ℃.After treating that autoclave naturally cools to room temperature, with deposition water in the still and ethanol cleaning many times.Obtain β-FeOOH nanometer rod after 80 ℃ of following dryings, in 500 ℃ of annealing 2.5 hours, obtain α-Fe again 2O 3Nanometer rod;
(2) 0.08g α-Fe 2O 3The nanometer rod ultra-sonic dispersion adds 0.75g urea and 0.115g potassium stannate (K then in 32ml water-ethanol solution 2SnO 3.3H 2O, 95%).After the stirring, above-mentioned solution is placed in the autoclave of 50ml stainless steel sealing.In baking oven, kept 36 hours in 170 ℃.After treating that autoclave naturally cools to room temperature, with deposition water in the still and ethanol cleaning many times.Obtain α-Fe after 80 ℃ of following dryings 2O 3/ SnO 2Core-shell nanometer rod, its pattern and microstructure characterize with transmission electron microscope, and be as shown in Figure 1;
(3) with α-Fe 2O 3/ SnO 2Core-shell nanometer rod is at N 2/ H 2(8%/H 2) under the atmosphere,, obtaining porous ferroferric oxide/tin oxide nano rod at last in 400 ℃ of annealing 7 hours, its pattern and microstructure characterize with transmission electron microscope, and be as shown in Figure 2.The length of its mesopore and diameter are respectively 10-60 and 5-30 nanometer;
(4) preparation 80wt% porous ferroferric oxide/tin oxide nano rod-paraffin composite film material utilizes its electromagnetic parameter of T/R coaxial transmission line test, and measuring result is seen Fig. 3.The dielectric loss of the mixture of data computation and magnetic loss tangent value are as shown in Figure 4 thus, can find out that the two has realized coupling preferably.Utilize electromagnetic transmission lineation opinion to calculate the reflection of electromagnetic wave rate of different film thicknesses at last, see Fig. 5.
Embodiment 2:
(1) with the FeCl of 40 milliliters 1.0mol/L 3Solution places in the autoclave of 50ml stainless steel sealing.In baking oven, kept 12 hours in 100 ℃.After treating that autoclave naturally cools to room temperature, with deposition water in the still and ethanol cleaning many times.Obtain β-FeOOH nanometer rod after 80 ℃ of following dryings, in 500 ℃ of annealing 2.5 hours, obtain α-Fe again 2O 3Nanometer rod;
(2) 0.08g α-Fe 2O 3The nanometer rod ultra-sonic dispersion adds 0.75g urea and 0.115g potassium stannate (K then in 32ml water-ethanol solution 2SnO 3.3H 2O, 95%).After the stirring, above-mentioned solution is placed in the autoclave of 50ml stainless steel sealing.In baking oven, kept 36 hours in 170 ℃.After treating that autoclave naturally cools to room temperature, with deposition water in the still and ethanol cleaning many times.Obtain α-Fe after 80 ℃ of following dryings 2O 3/ SnO 2Core-shell nanometer rod;
(3) with α-Fe 2O 3/ SnO 2Core-shell nanometer rod is at N 2/ H 2(8%/H 2) under the atmosphere,, obtain porous ferroferric oxide/tin oxide nano rod at last in 400 ℃ of annealing 7 hours.
Embodiment 3:
(1) with the FeCl of 40 milliliters 0.25mol/L 3Solution places in the autoclave of 50ml stainless steel sealing.In baking oven, kept 12 hours in 110 ℃.After treating that autoclave naturally cools to room temperature, with deposition water in the still and ethanol cleaning many times.Obtain β-FeOOH nanometer rod after 80 ℃ of following dryings, in 500 ℃ of annealing 2.5 hours, obtain α-Fe again 2O 3Nanometer rod;
(2) 0.08g α-Fe 2O 3The nanometer rod ultra-sonic dispersion adds 0.75g urea and 0.115g potassium stannate (K then in 32ml water-ethanol solution 2SnO 3.3H 2O, 95%).After the stirring, above-mentioned solution is placed in the autoclave of 50ml stainless steel sealing.In baking oven, kept 36 hours in 170 ℃.After treating that autoclave naturally cools to room temperature, with deposition water in the still and ethanol cleaning many times.Obtain α-Fe after 80 ℃ of following dryings 2O 3/ SnO 2Core-shell nanometer rod;
(3) with α-Fe 2O 3/ SnO 2Core-shell nanometer rod is at N 2/ H 2(8%/H 2) under the atmosphere,, obtain porous ferroferric oxide/tin oxide nano rod at last in 400 ℃ of annealing 7 hours.

Claims (2)

1. the electromagnetic porous ferroferric oxide of absorbing high-frequency/White tin oxide core-shell nanometer rod, it is characterized in that: it is (1) FeCl with 0.25-1.0mol/L 3Solution places in the autoclave of stainless steel sealing, in baking oven, keeps 12 hours in 100-120 ℃, treat that autoclave naturally cools to room temperature after; Deposition water in the still and ethanol are cleaned; Obtain β-FeOOH nanometer rod after 80 ℃ of following dryings, in 500 ℃ of annealing 2.5 hours, obtain α-Fe again 2O 3Nanometer rod; (2) with 0.08g α-Fe 2O 3The nanometer rod ultra-sonic dispersion is in 32ml water-ethanol solution, and the alcoholic acid volume ratio is 38% in the said water-ethanol solution, adds 0.75g urea and 0.115g potassium stannate then; After the stirring; Above-mentioned solution is placed in the autoclave of stainless steel sealing, in baking oven, kept 36 hours in 170 ℃, treat that autoclave naturally cools to room temperature after; Deposition water in the still and ethanol are cleaned, obtain α-Fe after 80 ℃ of following dryings 2O 3/ SnO 2Core-shell nanometer rod; (3) with α-Fe 2O 3/ SnO 2Core-shell nanometer rod is at H 2Volume accounts for 8% N 2/ H 2Under the atmosphere, in 400 ℃ of annealing 7 hours, the length in the hole that obtains and diameter were respectively the porous ferroferric oxide/tin oxide nano rod of 10-60 and 5-30 nanometer.
2. the method for making of the electromagnetic porous ferroferric oxide of absorbing high-frequency/White tin oxide core-shell nanometer rod is characterized in that:
(1) with the FeCl of 0.25-1.0mol/L 3Solution places in the autoclave of stainless steel sealing, in baking oven, keeps 12 hours in 100-120 ℃, treat that autoclave naturally cools to room temperature after; Deposition water in the still and ethanol are cleaned; Obtain β-FeOOH nanometer rod after 80 ℃ of following dryings, in 500 ℃ of annealing 2.5 hours, obtain α-Fe again 2O 3Nanometer rod;
(2) with 0.08g α-Fe 2O 3The nanometer rod ultra-sonic dispersion is in 32ml water-ethanol solution, and the alcoholic acid volume ratio is 38% in the said water-ethanol solution, adds 0.75g urea and 0.115g potassium stannate then; After the stirring; Above-mentioned solution is placed in the autoclave of stainless steel sealing, in baking oven, kept 36 hours in 170 ℃, treat that autoclave naturally cools to room temperature after; Deposition water in the still and ethanol are cleaned, obtain α-Fe after 80 ℃ of following dryings 2O 3/ SnO 2Core-shell nanometer rod;
(3) with α-Fe 2O 3/ SnO 2Core-shell nanometer rod is at H 2Volume accounts for 8% N 2/ H 2Under the atmosphere,, obtain porous ferroferric oxide/tin oxide nano rod in 400 ℃ of annealing 7 hours.
CN2009100716773A 2009-03-31 2009-03-31 Ferriferous oxide/tin oxide core-shell nanometer rod absorbing high-frequency electromagnetic wave and preparing method thereof Expired - Fee Related CN101586019B (en)

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