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 PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 36
- 239000000956 alloy Substances 0.000 title claims abstract description 36
- 230000002745 absorbent Effects 0.000 title claims abstract description 28
- 239000002250 absorbent Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229910052742 iron Inorganic materials 0.000 claims abstract description 22
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 56
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 40
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 39
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical group [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 24
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 11
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 10
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 229910017052 cobalt Inorganic materials 0.000 claims description 7
- 239000010941 cobalt Substances 0.000 claims description 7
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000012456 homogeneous solution Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 7
- 230000007480 spreading Effects 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 6
- 230000009467 reduction Effects 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000002159 nanocrystal Substances 0.000 claims description 4
- 150000007524 organic acids Chemical class 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 230000014759 maintenance of location Effects 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 230000035699 permeability Effects 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 6
- 229910000859 α-Fe Inorganic materials 0.000 abstract description 6
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- 239000002184 metal Substances 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 230000002925 chemical effect Effects 0.000 abstract description 3
- 239000000696 magnetic material Substances 0.000 abstract description 3
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- 230000005476 size effect Effects 0.000 abstract description 3
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- 150000002431 hydrogen Chemical class 0.000 description 5
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- 239000012188 paraffin wax Substances 0.000 description 5
- 239000010453 quartz Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 239000011358 absorbing material Substances 0.000 description 4
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- 239000002105 nanoparticle Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
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- 239000006229 carbon black Substances 0.000 description 1
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
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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
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).
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| CN101299914B true CN101299914B (en) | 2011-04-13 |
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| CN106535595A (en) * | 2016-11-10 | 2017-03-22 | 无锡市明盛强力风机有限公司 | FeNiCo wave-absorbing material |
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