CN100518480C - Rare earth Fe basis suction wave material and method for making the same - Google Patents
Rare earth Fe basis suction wave material and method for making the same Download PDFInfo
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- CN100518480C CN100518480C CNB200710049468XA CN200710049468A CN100518480C CN 100518480 C CN100518480 C CN 100518480C CN B200710049468X A CNB200710049468X A CN B200710049468XA CN 200710049468 A CN200710049468 A CN 200710049468A CN 100518480 C CN100518480 C CN 100518480C
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Abstract
The invention discloses a nano-crystal tombar thite ferrous absorbing material with good absorbing property and a preparation method thereof. The material is characterized in that the lanthanon with the weight percentage of 2% and 70%, the iron with the weight percentage of 5% and 98% and the little amount of doping element are smelted into tombar thite-ferrous alloy; the tombar thite-ferrous alloy is reacted with hydrogen by hydrogen decrepitation method under the temperature range from 0 to 700 DEG C, is broken into fine powder or be ball grinded into fine powder, and then is reacted with hydrogen to generate composite material of rare earths hydride (RHx) and Alpha-Fe under the temperature range from 100 DEG C to 1000 DEG C; finally, the composite material is oxidized, nitridized or oxidized and nitridized under low temperature to produce the composite material mainly being rare earth oxide or nitride/Alpha-Fe composite material. The material of the invention has the advantages of high absorbing capability, wide shield wave band, good anti-corrosion property, anti-oxidation property and low price, and can be used in the fields of electro-magnetic shielding in building, information and communication technical secrecy and military cloaking technique, and so on.
Description
Technical field
The invention belongs to the absorbing material field, particularly a kind of composite material and preparation method with electro-magnetic wave absorption of nanostructure.
Background technology
Along with the high speed development of progress of science and technology and information industry, equipment such as computer, mobile phone, facsimile machine, telephone set and network (system) have been widely used in processing procedures such as the generation, transmission, reception, storage of information.This kind equipment be unable to do without electromagnetic effect when work.Electromagnetic extensive use has brought serious day by day electromagnetic interference (EMI), and a kind of minimizing electromagnetic interference effective method adopts microwave absorbing material exactly, and unwanted or harmful electromagnetic energy is converted into heat energy.Metal soft magnetic material has the high saturation magnetization and the Snoeck limit, and its complex permeability still can keep high value in various wireless communication system medium and low frequency section microwaves (1-5GHz) scope, can be used to prepare the thin layer absorbing material.Existingly simultaneously studies show that to have the metal soft magnetic material of nanocrystalline structure, its initial permeability, resistivity are increased dramatically, and help the raising of microwave magnetic permeability of material and the reduction of dielectric constant, can improve the absorbing property of material.But metal soft magnetic material has the high coefficient of conductivity and reduce because of eddy current loss causes soft magnet performance easily in electromagnetic wave, is unfavorable for the raising of absorbing property.Traditional preparation method is broken into very thin particle with it, and coated with insulating material, but is subjected to granularity, the form of powder, and the influence of coating thickness and uniformity etc., and it is difficult to satisfy high performance requirement.
Rare earth--ferrous alloy can obtain using widely because of its excellent magnetic as permanent magnetic material, but it rarely has the report of this respect both at home and abroad at present as electromagnetic wave absorbent material.In the research process of people to the rare earth-iron base permanent magnetic material, discovery rare earth-iron base alloy can be inhaled concurrent estranged the separating of hydrogen (disproportionation) reaction at a certain temperature, generates a kind of nanocrystalline rare-earth hydride and nanocrystalline α-Fe structure.Nanocrystalline α-Fe has good soft magnet performance in this structure, and the low (3*10 of nanocrystalline rare-earth hydride resistivity
7Ω m), if can improve the resistive performance of rare earth compound phase and significantly do not change the structure and α-Fe soft magnet performance mutually of product, can obtain to have the absorbing material of the excellent performance of ideal structure.In view of the foregoing, we are with this rare earth with nanostructure--ferroalloy (R-Fe, R represents rare earth element) disproportionation products carry out nitrogenize or oxidation or nitrogenize at low temperatures and add oxidation and handle, make RHx change the oxide of rare earth into, nitride or nitrogen oxide are with the resistivity of this phase of raising, thereby obtained a kind of dielectric loss type absorbing material rare earth oxide with nanostructure or rare earth nitride and the electromagnetic consumable type absorbing material α-Fe electromagnetic wave absorbent material that is composited mutually, it has excellent electro-magnetic wave absorption performance and purposes widely, thereby is a kind of novel wave-absorbing material that development potentiality is arranged very much.
Summary of the invention
The present invention is directed to the deficiency that existing absorbing material exists, a kind of novel nanocrystalline composite wave-suction material and preparation method thereof is provided, it is good that this material has an absorbing property, and the shielding wide waveband is corrosion-resistant, anti-oxidant and characteristics that cost is cheap relatively.
Technical scheme of the present invention is:
1, rare earth, iron and interpolation element etc. are smelted into ingot casting or are prepared into strip (sheet) by the fast melt-quenching technology according to certain proportioning, rare-earth-iron alloy with method for preparing is broken into it fine powder or the rare-earth-iron alloying pellet is worn into fine powder with hydrogen reaction (the quick-fried method of hydrogen) in 0-700 ℃ temperature range again, and again this powder being generated principal phase with hydrogen reaction in 100 ℃ of-1000 ℃ of temperature ranges is the composite material of rare earth hydride (RHx) and α-Fe.
2, above-mentioned composite material is added oxidation in low-temperature oxidation or nitrogenize or nitrogenize, prepare the composite material that rare earth oxide, nitride or nitrogen oxide and principal phase α-Fe forms.
Above-mentioned absorbing material chemical composition is:
Other doped chemical content is lower than 10%
Further be, rare earth metal has been selected from least a in the elements such as La, Ce, Nd, Sm, Pr, Eu, Gd, Dy, Tb, Ho, and metal-doped element is from IA, IIA, IIIA family or transition group.
The present invention is owing to adopt rare earth metal and iron as raw material, and by mixing, it is good that the absorbing material that obtains has an absorbing property, the shielding wide waveband, corrosion-resistant, the characteristics anti-oxidant and cost is cheap relatively, in a word, the present invention can be used for building fields such as electromagnetic shielding, information and mechanics of communication are maintained secrecy, military stealth technology, precision instrumentation.
Description of drawings
Accompanying drawing 1 is the suction ripple curve of embodiment 1 gained.
Accompanying drawing 2 is the suction ripple curve of embodiment 2 gained.
Accompanying drawing 3 is the suction ripple curve of embodiment 3 gained.
Accompanying drawing 4 is the suction ripple curve of embodiment 4 gained.
Accompanying drawing 5 is the suction ripple curve of embodiment 5 gained.
Embodiment
Embodiment 1:
Operating weight percentage is that 25% samarium and 75% pure iron are smelted into ingot casting under the protection of argon gas in the present embodiment; adopt the method for hydrogen quick-fried (HD) to make its fragmentation and be decomposed into nanocrystalline SmHx/ α-Fe composite construction; be nitrided into nanocrystalline samarium nitride/α-Fe two-phase powder then; alloy powder mixes with paraffin in 1: 5 ratio; be pressed into ring-type (D=7mm then respectively; d=3.01mm; h=3mm) and rectangle (L*W=7.2*3.6mm; thickness 0.9mm), the reflection coefficient of sample records with Agilent E8363 electromagnetic wave vector network analyzer.Relevant parameter μ
r, ε
r" reach 10 in frequency during for 5GHz, μ ' is 3.21 to the maximum, μ " be 0.95 to the maximum, its absworption peak reaches-45 decibels (dB) by the decision of scattering coefficient and sample thickness, ε, and absorptivity is 5GHz less than the bandwidth of-10dB, inhales the ripple curve as shown in Figure 1.
Embodiment 2:
Operating weight percentage is that 40% samarium and 60% pure iron are smelted into ingot casting under the protection of argon gas in the present embodiment; adopt the method for hydrogen quick-fried (HD) to make its fragmentation and be decomposed into nanocrystalline SmHx/ α-Fe composite construction; reoxidize and change into nanocrystalline samarium oxide/α-Fe two-phase powder; alloy powder mixes with paraffin in 1: 5 ratio; be pressed into ring-type (D=7mm then respectively; d=3.01mm; h=3mm) and rectangle (L*W=7.2*3.6mm; thickness 0.9mm), the reflection coefficient of sample records with Agilent E8363 electromagnetic wave vector network analyzer.Relevant parameter μ
r, ε
r" reach 3.15 in frequency during for 7.6GHZ, μ ' is 2.9 to the maximum, μ " be 0.86 to the maximum, its absworption peak reaches-50 decibels (dB) by the decision of scattering coefficient and sample thickness, ε, and absorptivity is 5.1GHz less than the bandwidth of-10dB, inhales the ripple curve as shown in Figure 2.
Embodiment 3:
Operating weight percentage is 12% neodymium in the present embodiment; the tungsten and the chromium element of 86% pure iron and trace; under the protection of argon gas, be smelted into ingot casting; adopt the method for hydrogen quick-fried (HD) to make its fragmentation and be decomposed into nanocrystalline NdHx/ α-Fe composite construction; be broken into powder again; be nitrided into nanocrystalline samarium nitride/α-Fe two-phase composite granule then; alloy powder mixes with paraffin in 1: 5 ratio; be pressed into ring-type (D=7mm then respectively; d=3.01mm; h=3mm) and the reflection coefficient of rectangle (L*W=7.2*3.6mm, thickness 0.9mm) sample record with Agilent E8363 electromagnetic wave vector network analyzer.Relevant parameter μ
r, ε
r" reach 4.0 in frequency during for 8GHZ, μ ' is 4 to the maximum, μ " be 1.2 to the maximum, its absworption peak reaches-50 decibels (dB) by the decision of scattering coefficient and sample thickness, ε, and absorptivity is 4.5GHz less than the bandwidth of-10dB, inhales the ripple curve as shown in Figure 3
Embodiment 4:
Using atomic percent in the present embodiment is that the ferro-boron of 14% neodymium, 80% pure iron 6% is smelted into ingot casting under the protection of argon gas; method with fast quenching is prepared into band (or amorphous ribbon) with it; be broken into nanocrystalline; be reoxidised into the oxide/α-heterogeneous composite granules such as Fe of nanocrystalline neodymium; alloy powder mixes with paraffin in 5: 1 ratio; be pressed into ring-type (D=7mm then respectively; d=3.01mm; h=3mm) and the reflection coefficient of rectangle (L*W=7.2*3.6mm, thickness 0.9mm) sample record with Agilent E8363 electromagnetic wave vector network analyzer.Relevant parameter μ
r, ε
r" reach 4.2 in frequency during for 6GHZ, μ ' is 2.8 to the maximum, μ " be 0.83 to the maximum, its absworption peak reaches-38 decibels (dB) by the decision of scattering coefficient and sample thickness, ε, and absorptivity is 1.9GHz less than the bandwidth of-10dB, inhales the ripple curve as shown in Figure 4.
Embodiment 5:
Operating weight percentage is that the titanium valve of 34% praseodymium and 65% pure iron and 1% is smelted into ingot casting under the protection of argon gas in the present embodiment; adopt the method for hydrogen quick-fried (HD) to make its fragmentation and be decomposed into nanocrystalline PrHx/ α-Fe composite construction; be broken into powder again; nitrogenize then; change into the heterogeneous composite granule of nitrogenize Pr or nitrogen praseodymium oxide or praseodymium oxide and α-Fe in cryogenic oxygen; alloy powder mixes with paraffin in 5: 1 ratio; be pressed into ring-type (D=7mm then respectively; d=3.01mm; h=3mm) and the reflection coefficient of rectangle (L*W=7.2*3.6mm, thickness 0.9mm) sample record with AgilentE8363 electromagnetic wave vector network analyzer.Relevant parameter μ
r, ε
r" reach 4.5 in frequency during for 6.2GHZ, μ ' is 3.1 to the maximum, μ " be 0.9 to the maximum, its absworption peak reaches-50 decibels (dB) by the decision of scattering coefficient and sample thickness, ε, and absorptivity is 7.0GHz less than the bandwidth of-10dB, inhales the ripple curve as shown in Figure 5.
Claims (2)
1, a kind of nanocrystalline rare-earth-Fe basis suction wave material, it is characterized in that: rare earth element, iron and a small amount of doped chemical of certain proportioning are smelted into the rare earth-iron base alloy, in 0-700 ℃ temperature range, be broken into fine powder again or first ball milling becomes fine powder with hydrogen reaction, generating principal phase with hydrogen reaction then in 100 ℃ of-1000 ℃ of temperature ranges is the composite material of rare earth hydride and α-Fe, above-mentioned composite material is added in low-temperature oxidation or nitrogenize or nitrogenize to be oxidized to nanocrystalline rare-earth-Fe basis suction wave material at last; In the wherein said rare earth-iron base alloy, rare earth metal has been selected from least a in the elements such as La, Ce, Nd, Sm, Pr, Eu, Gd, Dy, Tb, Ho, its content percentage by weight is 2%-98%, the content percentage by weight of iron is 2%-98%, doped chemical is made up of IA, IIA, IIIA family or transiting group metal elements, and the content percentage by weight of doped chemical is less than 10%.
2, rare earth-iron base absorbing material according to claim 1 is characterized in that what nanocrystalline rare-earth-Fe basis suction wave material was made up of the rare earth oxide of nanostructure or rare earth nitride or rare earth nitrogen oxide and principal phase α-Fe.
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| CNB200710049468XA CN100518480C (en) | 2007-07-09 | 2007-07-09 | Rare earth Fe basis suction wave material and method for making the same |
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| CNB200710049468XA CN100518480C (en) | 2007-07-09 | 2007-07-09 | Rare earth Fe basis suction wave material and method for making the same |
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| CN104831161A (en) * | 2015-05-07 | 2015-08-12 | 黄鹏腾 | Iron-based alloy wave absorbing material and preparation method thereof |
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| CN104858438A (en) * | 2015-05-11 | 2015-08-26 | 黄鹏腾 | Preparation method of neodymium-iron alloy wave-absorbing micro powder doped with titanium |
| CN104894461A (en) * | 2015-05-13 | 2015-09-09 | 黄鹏腾 | Low-frequency wave absorbing material and preparation method thereof |
| CN104846272A (en) * | 2015-05-14 | 2015-08-19 | 黄鹏腾 | Nd and La-doped iron base alloy wave absorption material |
| CN104942299A (en) * | 2015-05-15 | 2015-09-30 | 黄鹏腾 | Rare earth and iron-based wave-absorbing micro powder preparation method |
| CN106609326A (en) * | 2015-10-25 | 2017-05-03 | 杨欣睿 | La-doped Fe-Ni-based alloy wave absorbing material |
| CN106220230A (en) * | 2016-07-29 | 2016-12-14 | 望江振东新型墙材有限公司 | A kind of building face wall iron tailings base inhales ripple radioprotective porous light insulating brick and preparation technology thereof |
| CN106424705B (en) * | 2016-10-09 | 2019-04-30 | 中国科学院宁波材料技术与工程研究所 | A kind of metal-powder and its preparation and application |
| CN106433269A (en) * | 2016-11-10 | 2017-02-22 | 无锡市明盛强力风机有限公司 | FeNiCo polypyrrole wave-absorbing material |
| CN114045435B (en) * | 2021-11-11 | 2022-12-20 | 泉州天智合金材料科技有限公司 | Iron-based amorphous nanocrystalline wave-absorbing material and preparation method thereof |
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