CN101299914B - Nanocrystalline ultra-fine alloy powder electromagnetic wave absorbent and preparation method thereof - Google Patents

Nanocrystalline ultra-fine alloy powder electromagnetic wave absorbent and preparation method thereof Download PDF

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CN101299914B
CN101299914B CN2008100289251A CN200810028925A CN101299914B CN 101299914 B CN101299914 B CN 101299914B CN 2008100289251 A CN2008100289251 A CN 2008100289251A CN 200810028925 A CN200810028925 A CN 200810028925A CN 101299914 B CN101299914 B CN 101299914B
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preparation
absorbent
electromagnetic wave
alloy powder
nitrate
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CN101299914A (en
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张海燕
吴子秋
张坚
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Guangdong University of Technology
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Abstract

The invention discloses a nanocrystalline ultra-fine alloy powder electromagnetic wave absorbent and preparation method thereof. The absorbent is a binary or ternary alloy powder combined by Fe, Co, Ni, wherein Fe, Co, Ni is 10 to 90 percent of the atom percentage of the alloy. The absorbent is prepared by self-spread incendiary method, the magnetic conductivity of metal powder under microwave frequency can be regulated by heat treatment in the preparation process, thereby the effect of regulating the band of wave-absorbing can be achieved. The nanocrystalline ultra-fine alloy powder electromagnetic wave absorbent has complex permeability and complex dielectric constant, the magnetic conductivity of the microwave permeability is higher, which can make up the shortcomings of the ferrite series magnetic materials, such as large specific gravity and no ideal high-frequency characteristic; the surface effect volume effect and quantum size effect of the nanometer particle makes the nanometer particle generate a plurality of physical and chemical effects different from block materials. The electromagnetic wave absorbent of the invention has good absorbing property to electromagnetic wave, specifically to high-frequency electromagnetic.

Description

A kind of nanocrystalline ultra-fine alloy powder electromagnetic wave absorbent and preparation method thereof
Technical field
The present invention relates to a kind of nanocrystalline ultra-fine alloy powder electromagnetic wave absorbent and preparation method thereof.
Background technology
At present, divide by loss mechanism, radio-radar absorber mainly contains two classes: (1) dielectric loss class absorbent, as carbon black, carbon fiber, graphite, SiC fiber etc.; (2) magnetic loss class absorbent is as ferrite, carbonyl iron dust, metal fine powder etc.Dielectric loss class absorbing material thickness is big, and absorption band is narrow, and the magnetic absorbent can be widened frequency band, thickness thinning.And ferrite has had very long phase of history as absorbent, is one of absorbing material of using always, and its existing certain dielectric loss also has bigger magnetic loss, in tens to hundreds of MHz scopes good absorbent properties is arranged.But ferrite exists a more serious problem to be: in the microwave frequency of upper frequency, ferritic magnetic permeability is generally smaller, the microwave absorbing property variation.The nanometer magnetic metal powder is (as iron, cobalt, nickel, silicon and alloy thereof etc.) have complex permeability and a complex dielectric constant, the magnetic permeability of microwave frequency is higher, have a large amount of absorption electromagnetic wave energies, temperature stability waits outstanding advantage well, become a kind of rising absorbent, the ratio that can remedy ferrite class magnetic material is great, shortcomings such as high frequency characteristics is undesirable, when particularly particle size is nanoscale, the skin effect of nano particle, bulk effect and quantum size effect make it produce a lot of physics and chemical effects different with block of material, make the nano-magnetic absorbing material to electromagnetic wave particularly frequency electromagnetic waves have the excellent absorption performance, be a kind of desirable electromagnetic wave absorbent material.
Summary of the invention
The purpose of this invention is to provide a kind of nanocrystalline ultra-fine alloy powder electromagnetic wave absorbent and preparation method thereof.
Binary or ternary nanocrystals ultra-fine alloy powder that nanocrystalline ultra-fine alloy powder electromagnetic wave absorbent of the present invention is made up of Fe, Co, three kinds of elements of Ni, the atomic percent in Fe, Co, three kinds of shared alloys of element of Ni is respectively 10~90%.
The preparation method of nanocrystalline ultra-fine alloy powder electromagnetic wave absorbent of the present invention is as follows:
(1) with wherein two or three the soluble inorganic salt dissolving mixing in deionized water in proportion respectively of iron, nickel, cobalt, add an amount of organic acid again, fully stir, after being mixed with homogeneous solution, the pH value to 7 that adds the ammoniacal liquor regulator solution, colloidal sol is placed drying baker, be dried into xerogel for 110 ℃, the xerogel heating is obtained oxide powder after spreading;
(2) oxide powder is carried out the short time ball milling, after ball milling finishes oxide powder is placed in the tube furnace, feed the air in the nitrogen eliminating reaction unit, feed hydrogen again, heat the reduced oxide powder then, reduction temperature is 300~900 ℃, reduction insulation certain hour, air-cooled fast then to taking out below 150 ℃, collect product and obtain Fe, Co, Ni binary or ternary nanocrystals ultra-fine alloy powder electromagnetic wave absorbent.
Soluble inorganic salt is ferric nitrate, cobalt nitrate, nickel nitrate in the above-mentioned steps (1).
In the above-mentioned steps (1) iron, nickel, cobalt wherein the additional proportion of two or three soluble inorganic salt be that the single-element molar content of iron in the inorganic salts, nickel, cobalt is 10~90%.
Adding organic acid in the above-mentioned steps (1) is that its mol ratio of citric acid is: ferric nitrate: citric acid=5: 6, cobalt nitrate: citric acid=5: 9, nickel nitrate: citric acid=5: 9.
The ball milling time is 1~3 hour in the above-mentioned steps (2).
The reduction temperature retention time is 1~5 hour in the above-mentioned steps (2).
The invention has the beneficial effects as follows:
1. nanocrystalline ultra-fine alloy powder electromagnetic wave absorbent has complex permeability and complex dielectric constant, the magnetic permeability of microwave frequency is higher, have a large amount of absorption electromagnetic wave energies, temperature stability is good, the ratio that can remedy ferrite class magnetic material is great, shortcomings such as high frequency characteristics is undesirable, the skin effect of nano particle, bulk effect and quantum size effect make it produce a lot of physics and chemical effects different with block of material, make the nano-magnetic absorbing material to electromagnetic wave particularly frequency electromagnetic waves have the excellent absorption performance, be a kind of desirable electromagnetic wave absorbent material.
2. super-fine metal powder prepares by self-propagating combustion, can regulate and control the magnetic permeability under microwave frequency of metal dust in the preparation process by heat treatment, thereby can reach the effect that the ripple frequency band is inhaled in regulation and control.
Embodiment
It below is the example of preparation Fe, Co, Ni binary or ternary nanocrystals ultra-fine alloy powder microwave absorption.
Embodiment 1:
1: 1 in molar ratio ratio of ferric nitrate, cobalt nitrate is mixed with deionized water, ferric nitrate in molar ratio again: citric acid=5: 6, cobalt nitrate: citric acid=5: 9 adding citric acids, after being mixed with homogeneous solution, the pH value to 7 that adds the ammoniacal liquor regulator solution, colloidal sol is placed drying baker, and 110 ℃ of oven dry 24h become xerogel, and the xerogel heating obtains oxide powder after spreading.Oxide ball milling 1h, be placed on then in the quartz ampoule, feed 50sccm hydrogen, be warmed up to 800 ℃ with stove, insulation 1h, air-cooled to 150 ℃ of taking-ups fast then, and collect product nanocrystalline ultra-fine alloy powder Fe 50Co 50(at%).Nanocrystalline ultra-fine alloy powder Fe 50Co 50Be Fe, Co bianry alloy powder, wherein the atomic percent of Fe is 50%, and the atomic percent of Co is 50%.With prepared nanometer crystal alloy powder microwave absorption Fe 50Co 50Mix by weight 8: 2 with paraffin, make external diameter 7mm, internal diameter 3mm, thickness is the coaxial annulus standard specimen of 2~4mm, the electromagnetic parameter of the alloyed powder composite material of surveying by vector network analyzer, the result shows that in 0.5~6GHz frequency range, the real part of relative permeability is up to 3.5, imaginary part be up to 1.0 and the relative dielectric constant real part be up to 12, imaginary part is up to 1.0.
Embodiment 2:
1: 3 in molar ratio ratio of ferric nitrate, nickel nitrate is mixed with deionized water, ferric nitrate in molar ratio again: citric acid=5: 6, nickel nitrate: citric acid=5: 9 adding citric acids, after being mixed with homogeneous solution, the pH value to 7 that adds the ammoniacal liquor regulator solution, colloidal sol is placed drying baker, and 110 ℃ of oven dry 24h become xerogel, and the xerogel heating obtains oxide powder after spreading.Oxide ball milling 2h, be placed on then in the quartz ampoule, feed 50sccm hydrogen, be warmed up to 900 ℃ with stove, insulation 3h, air-cooled to 150 ℃ of taking-ups fast then, and collect product nanocrystalline ultra-fine alloy powder Fe 25Ni 75(at%).Nanocrystalline ultra-fine alloy powder Fe 25Ni 75Be Fe, Ni bianry alloy powder, wherein the atomic percent of Fe is 25%, and the atomic percent of Ni is 75%.With prepared nanometer crystal alloy powder microwave absorption Fe 25Ni 75Mix by weight 8: 2 with paraffin, make external diameter 7mm, internal diameter 3mm, thickness is the coaxial annulus standard specimen of 2~4mm, the electromagnetic parameter of the alloyed powder composite material of surveying by vector network analyzer, the result shows that in 0.5~6GHz frequency range, the real part of relative permeability is up to 2.3, imaginary part be up to 1.4 and the relative dielectric constant real part be up to 21, imaginary part is up to 1.5.
Embodiment 3:
1: 1 in molar ratio ratio of ferric nitrate, nickel nitrate is mixed with deionized water, ferric nitrate in molar ratio again: citric acid=5: 6, nickel nitrate: citric acid=5: 9 adding citric acids, after being mixed with homogeneous solution, the pH value to 7 that adds the ammoniacal liquor regulator solution, colloidal sol is placed drying baker, and 110 ℃ of oven dry 24h become xerogel, and the xerogel heating obtains oxide powder after spreading.Oxide ball milling 3h, be placed on then in the quartz ampoule, feed 50sccm hydrogen, be warmed up to 900 ℃ with stove, insulation 1h, air-cooled to 150 ℃ of taking-ups fast then, and collect product nanocrystalline ultra-fine alloy powder Fe 50Ni 50(at%).Nanocrystalline ultra-fine alloy powder Fe 50Ni 50Be Fe, Ni bianry alloy powder, wherein the atomic percent of Fe is 50%, and the atomic percent of Ni is 50%.With prepared nanometer crystal alloy powder microwave absorption Fe 50Ni 50Mix by weight 8: 2 with paraffin, make external diameter 7mm, internal diameter 3mm, thickness is the coaxial annulus standard specimen of 2~4mm, the electromagnetic parameter of the alloyed powder composite material of surveying by vector network analyzer, the result shows that in 0.5~6GHz frequency range, the real part of relative permeability is up to 4.3, imaginary part be up to 1.8 and the relative dielectric constant real part be up to 22, imaginary part is up to 3.5.
Embodiment 4:
5: 4: 1 in molar ratio ratio of ferric nitrate, nickel nitrate, cobalt nitrate is mixed with deionized water, ferric nitrate in molar ratio again: citric acid=5: 6, nickel nitrate (cobalt nitrate): citric acid=5: 9 adding citric acids, after being mixed with homogeneous solution, the pH value to 7 that adds the ammoniacal liquor regulator solution, colloidal sol is placed drying baker, and 110 ℃ of oven dry 24h become xerogel, and the xerogel heating obtains oxide powder after spreading.Oxide ball milling 1h, be placed on then in the quartz ampoule, feed 50sccm hydrogen, be warmed up to 700 ℃ with stove, insulation 5h, air-cooled to 150 ℃ of taking-ups fast then, and collect product nanocrystalline ultra-fine alloy powder Fe 50Ni 40Co 10(at%).Nanocrystalline ultra-fine alloy powder Fe 50Ni 40Co 10Be Fe, Ni, Co ternary alloy three-partalloy powder, wherein the atomic percent of Fe is 50%, and the atomic percent of Ni is 40%, and the atomic percent of Co is 10%.With prepared nanometer crystal alloy powder microwave absorption Fe 50Ni 40Co 10Mix by weight 8: 2 with paraffin, make external diameter 7mm, internal diameter 3mm, thickness is the coaxial annulus standard specimen of 2~4mm, the electromagnetic parameter of the alloyed powder composite material of surveying by vector network analyzer, the result shows that in 0.5~6GHz frequency range, the real part of relative permeability is up to 4.1, imaginary part be up to 1.9 and the relative dielectric constant real part be up to 16.5, imaginary part is up to 1.5.
Embodiment 5:
8: 2 in molar ratio ratio of nickel nitrate, cobalt nitrate is mixed with deionized water, nickel nitrate (cobalt nitrate): citric acid=5: 9 adding citric acids, after being mixed with homogeneous solution, the pH value to 7 that adds the ammoniacal liquor regulator solution, colloidal sol is placed drying baker, 110 ℃ of oven dry 24h become xerogel, and the xerogel heating obtains oxide powder after spreading.Oxide ball milling 1h, be placed on then in the quartz ampoule, feed 50sccm hydrogen, be warmed up to 800 ℃ with stove, insulation 3h, air-cooled fast then to 150 ° of C taking-ups, and collect product nanocrystalline ultra-fine alloy powder Ni 80Co 20(at%).Nanocrystalline ultra-fine alloy powder Ni 80Co 20Be Ni, Co bianry alloy powder, wherein the atomic percent of Ni is 80%, and the atomic percent of Co is 20%.With prepared nanometer crystal alloy powder microwave absorption Ni 80Co 20Mix by weight 8: 2 with paraffin, make external diameter 7mm, internal diameter 3mm, thickness is the coaxial annulus standard specimen of 2~4mm, the electromagnetic parameter of the alloyed powder composite material of surveying by vector network analyzer, the result shows that in 0.5~6GHz frequency range, the real part of relative permeability is up to 3.2, imaginary part be up to 1.3 and the relative dielectric constant real part be up to 14, imaginary part is up to 0.7.

Claims (6)

1. the preparation method of a nanocrystalline ultra-fine alloy powder electromagnetic wave absorbent is characterized in that this preparation method's step is as follows:
(1) with wherein two or three the soluble inorganic salt dissolving mixing in deionized water in proportion respectively of iron, nickel, cobalt, add an amount of organic acid again, fully stir, after being mixed with homogeneous solution, the pH value to 7 that adds the ammoniacal liquor regulator solution, colloidal sol is placed drying baker, be dried into xerogel for 110 ℃, the xerogel heating is obtained oxide powder after spreading;
(2) oxide powder is carried out the short time ball milling, after ball milling finishes oxide powder is placed in the tube furnace, feed the air in the nitrogen eliminating reaction unit, feed hydrogen again, heat the reduced oxide powder then, reduction temperature is 300~900 ℃, reduction insulation certain hour, air-cooled to 150 ℃ of taking-ups fast then, collect product and obtain Fe, Co, Ni binary or ternary nanocrystals ultra-fine alloy powder electromagnetic wave absorbent.
2. the preparation method of absorbent according to claim 1 is characterized in that soluble inorganic salt is ferric nitrate, cobalt nitrate, nickel nitrate in the above-mentioned steps (1).
3. the preparation method of absorbent according to claim 1 and 2, it is characterized in that iron, nickel, cobalt in the above-mentioned steps (1) wherein the ratio of two or three soluble inorganic salt be that the single-element molar content of iron in the inorganic salts, nickel, cobalt is respectively 10~90%.
4. the preparation method of absorbent according to claim 1 and 2 is characterized in that adding organic acid in the above-mentioned steps (1) is that its mol ratio of citric acid is: ferric nitrate: citric acid=5: 6, cobalt nitrate: citric acid=5: 9, nickel nitrate: citric acid=5: 9.
5. the preparation method of absorbent according to claim 1 is characterized in that the ball milling time is 1~3 hour in the above-mentioned steps (2).
6. the preparation method of absorbent according to claim 1 is characterized in that the reduction temperature retention time is 1~5 hour in the above-mentioned steps (2).
CN2008100289251A 2008-06-20 2008-06-20 Nanocrystalline ultra-fine alloy powder electromagnetic wave absorbent and preparation method thereof Expired - Fee Related CN101299914B (en)

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