CN101880817A - Electromagnetic wave absorbing material formed by planar 2:17 rare earth-3d transition intermetallic compounds - Google Patents
Electromagnetic wave absorbing material formed by planar 2:17 rare earth-3d transition intermetallic compounds Download PDFInfo
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- CN101880817A CN101880817A CN 201010230672 CN201010230672A CN101880817A CN 101880817 A CN101880817 A CN 101880817A CN 201010230672 CN201010230672 CN 201010230672 CN 201010230672 A CN201010230672 A CN 201010230672A CN 101880817 A CN101880817 A CN 101880817A
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Abstract
The invention provides a material which can absorb electromagnetic waves and is formed by transition intermetallic compounds. The general formula of the material is R2(Co1-xFex)17, wherein R in the general formula is Nd or Ce; when R is Nd, x is not more than 1 and not less than 0, when R is Ce, x is not more than 0.8 and not less than 0.6; and the direction of easy magnetization of the material is vertical to the C axis. The special description is as follows: if the components meet the above general formula but the direction of easy magnetization of the material is parallel to the C axis, the material is not suitable for serving as the material absorbing electromagnetic waves. A method for preparing a composite material by utilizing the material of the invention is characterized by placing the material of the invention into non-cured binding materials, after fully mixing the material and the non-cured binding materials uniformly, placing the mixture into a die manufactured by nonmagnetic materials, placing the die in the magnetic field and ensuring the die to rotate in the magnetic field, and carrying out orientation.
Description
Technical field
The present invention relates to a kind of electromagnetic material that absorbs, but and by a kind of electromagnetic-power-absorbing composite of this material preparation, the present invention a kind ofly absorbs electromagnetic material by what transition intermetallic compounds constituted.
Background technology
Along with the development of science and technology and mechanics of communication, computer, mobile phone, disk etc. have been widely used in the generation and the transmission course of information, but the widespread use of this hertzian wave material has brought serious day by day electromagnetic radiation and electromagnetic interference problem.The effective ways that overcome Electromagnetic Interference are to adopt electromagnetic wave absorbent material.
The rare earth Fe basis suction wave material that the disclosed rare earth of Chinese invention patent application 200710049468.X mixes based on α-Fe.In addition, " Broadband and thin microwave absorber of nickel-zinc ferrite/carbonyl iron " (Journal of Alloys and Compounds 487 (2009) 708-717) (hereinafter to be referred as document 1) discloses the Wave suction composite material of ferrite and metallic particles; " Dependence of Microwave Absorbing Property on Ferrite Volume Fraction in MnZn Ferrite-Rubber Composites " (D.Y.Kim, Y.C.Chung, T.W.Kang, and H.C.Kim IEEE TRANSACTIONS ONMAGNETICS, VOL 32, NO 2, and MARCH 1996) (hereinafter to be referred as document 2) disclose ferritic electromagnetic wave absorption material; Gigahertz range electromagnetic wave absorbers made of amorphous-carbon-based magnetic nanocomposites (Jiu Rong Liu, Masahiro Itoh, Takashi Horikawa, and Ken-ichi Machida JOURNAL OF APPLIED PHYSICS 98,054305_2005) (hereinafter to be referred as document 3) discloses the wave absorbtion matter of the matrix material of iron and carbon formation.
The matching thickness that the common deficiency that prior art exists is a material is bigger, for example the matching thickness of the disclosed material of Chinese patent application 200710049468.X about 3GHz is about 4 millimeter, and will be greater than 7 millimeters (referring to contents of this patent accompanying drawing) at the corresponding thickness of 2GHz; And the material of document 1 is when frequency 3GHz, and corresponding thickness is 3.5～4 millimeters; The material of document 2 frequency during less than 8GHz the thickness of correspondence all surpassed 4 millimeters; The thickness of correspondence was 4 millimeters when the material of document 3 was 3GHz in frequency, and when frequency is 2GHz, its thickness will reach 6 millimeter.Because the match materials thickness of prior art is bigger, and its application is restricted, in some special Application Areass even can't use fully.
Summary of the invention
The invention reside in provides a kind of and can overcome the prior art deficiency, be better than prior art, suitable frequency is 1G to 100G, the electromagnetic wave absorbent material that stronger absorption of electromagnetic wave performance is arranged under the thickness condition thinner than prior art is the material that hertzian wave more than the 1G has stronger sorption to frequency under the thin condition of material thickness particularly; The present invention provides the preparation technology of this material simultaneously, and the method that goes out the better matrix material of its wave-absorbing effect with this material preparation.
Electromagnetic wave absorbent material general formula of the present invention is R
2(Co
1-xFe
x)
17, R is Nd or Ce in the general formula, and when R is the Nd element, 0≤x≤1, when R is the Ce element, 0.6≤x≤0.8, and the easy magnetization axis of material is vertical with the C axle.What need special instruction is if composition satisfies aforementioned formula, but its easy magnetization axis is parallel with the C axle, and the material of this class then is not suitable as and absorbs electromagnetic material.
The chemical formula of the electromagnetic wave absorbent material of the best of the present invention is: Nd
2Fe
17, perhaps Ce
2(Co
0.7Fe
0.3)
17
Electromagnetic wave absorbent material preparation method of the present invention is smelted into alloy with rare earth element, iron and cobalt, and quenches after the full and uniformization processing at high temperature, carries out ball-milling processing after the alloy powder breakdown mill being become tiny particle again, obtains metal-powder.
Adopt the aforesaid electromagnetic wave absorbent material of the present invention can prepare matrix material with better absorption of electromagnetic wave performance, the preparation method of this matrix material puts into uncured matrix material with described material, after thorough mixing is even, put into the mould that nonmagnetic substance is made again, mould is placed magnetic field, mould is rotated in magnetic field, so material being carried out orientation process solidifies up to matrix material, matrix material described here is resin or paraffin wax, or polyethylene, or macromolecular material such as polypropylene.
In the aforesaid Composite Preparation, magnetic field is 10 during its orientation process
-4～10T, the mould speed of rotation is 1～200 rev/min.
Used sticking material was a heat-curable epoxy resin when the present invention recommended to prepare matrix material.
Show through relevant experimental study, electromagnetic wave absorbent material of the present invention and by the matrix material of this material preparation under thin material thickness condition, as at 2～3 millimeters, has the hertzian wave performance that is better than prior art, can satisfy the strong requirement that absorbs, material of the present invention is a kind of novel absorbing material of excellent property, can be used for electromagnetic radiation shielding and eliminates electromagnetic interference, also can satisfy modern instrument to miniaturization, integrated and high efficiency requirement.
Description of drawings
Accompanying drawing 1 is X-ray diffraction spectrogram before and after the example 1 material orientation of the present invention.
Accompanying drawing 2 is the absorption of electromagnetic wave spectrogram of the matrix material of adhesive preparation for the material paraffin of example 1 of the present invention, and wherein zero curve is the absorption curve of the matrix material of not oriented processing, and the ■ curve is the absorption curve of the matrix material after orientation process.2mm among the figure and 2.5mm are meant that respectively the one-tenth-value thickness 1/10 of the material of sample reflection loss correspondence is 2 millimeters and 2.5 millimeters.
Accompanying drawing 3 is the absorption of electromagnetic wave spectrogram of the matrix material of adhesive preparation for example 1 material heat-curable epoxy resin of the present invention, and 2mm among the figure and 2.5mm are meant that respectively the one-tenth-value thickness 1/10 of the material of sample reflection loss correspondence is 2 millimeters and 2.5 millimeters.
Accompanying drawing 4 is XRD diffraction spectrogram before and after the example 2 materials orientation of the present invention.
Accompanying drawing 5 is the absorption of electromagnetic wave spectrogram of the matrix material of adhesive preparation for the material paraffin of example 2 of the present invention, and wherein zero curve is the absorption curve of the matrix material of not oriented processing, and the ■ curve is the absorption curve of the matrix material after orientation process.2mm among the figure and 2.5mm are meant that respectively the one-tenth-value thickness 1/10 of the material of the loss correspondence that is reflected is 2 millimeters and 2.5 millimeters.
Accompanying drawing 6 is for the material of example 2 of the present invention is the absorption of electromagnetic wave spectrogram of the matrix material of adhesive preparation with the thermoset epoxy resin, and 2mm among the figure and 2.5mm are meant that respectively the one-tenth-value thickness 1/10 of the material of sample reflection loss correspondence is 2 millimeters and 2.5 millimeters.
Embodiment
The specific embodiment of the present invention is:
A. earlier rare earth element, iron and cobalt are smelted into alloy, and quench after the full and uniformization processing at high temperature, carry out ball-milling processing after again the alloy powder breakdown mill being become tiny particle, obtain metal-powder.
B. be the mould of putting into the nonmagnetic substance making after 1～9: 9～1 uncured matrix material mixes with compound powder and volume ratio between the rare-earth transiting group metal of preparation, place 10
-4In the magnetic field of～10T (tesla), mould rotating speed with 1～200 rev/min in magnetic field is rotated simultaneously, solidifies up to matrix material.
Preferable material preparation method of the present invention is that mould is positioned over 10
-4The magnetic field of～10T (tesla), mould speed of rotation are 1～200 rev/min.
Below be two most preferred embodiments of the present invention:
Embodiment 1
Take by weighing 2.080 gram neodymiums and 6.518 gram iron, under argon shield, be smelted into ingot casting.One week of annealing in the vitreosil pipe under 1000 ℃.Grind to form about 70 microns particle with moving back the ingot casting that overdoes with agate mortar, then particle is added 60 ml n-hexane wet-millings with planetary ball mill in agate jar, ratio of grinding media to material is 10: 1, ball milling speed is 200 rev/mins, adopt the mode of rotating ball milling, in 1 hour timed interval, ball milling total time is set at 16 hours, with the sample oven dry, obtain Nd at last
2Fe
17Material.Then sample is divided 3 kinds of situations compound: the paraffin that (1) and normal hexane have diluted is 35 with volume ratio; 65 mix, and after the oven dry it are inserted in the mould (internal diameter is 3.04 millimeters, and external diameter is 7.00 millimeters), and compression moulding under 1 MPa pressure is taken out then and carried out microwave test.(2) paraffin that has diluted with normal hexane is to mix at 35: 65 with volume ratio, (internal diameter is 3.04 millimeters after the oven dry it to be inserted the mould of nonmagnetic substance preparation, external diameter is 7.00 millimeters) in, mould is placed 90 ℃ of insulations of baking oven 15 minutes, paraffin is melted, just mould is put into magnetic field internal rotation orientation then, the magnetic field size is 0.8～1.2T (tesla), the speed of rotation is about 120 rev/mins, sample is solidified fully in lasting 20 minutes, takes out then and carries out microwave test.(3) with acetone diluted epoxy be to mix at 35: 65 with volume ratio, being pressed into internal diameter after the oven dry is 3.04 millimeters, and external diameter is 7.00 millimeters, and thickness is 2-3 millimeter ring-type sample, then sample is put into vacuum drying oven and solidified 1 hour for 140 ℃, test then.Its X-ray diffraction spectrogram is listed in Fig. 1, and the absorption of electromagnetic wave performance is seen Fig. 2 and Fig. 3.
This material of present embodiment 1 gained is pure 2: 17 phase samples as shown in Figure 1.After orientation, have only a strong diffraction peak to be (006) peak, present embodiment 1 gained material has planar magnetacrystalline anisotropy at normal temperatures as can be known.
As shown in Figure 2 material and paraffin compound after, do not having the orientation situation under, at 2～10GHz, thickness is at 2～2.5 millimeters, reflection loss can reach-22dB about, and through after the orientation, at 4～5GHz, thickness is at the 2-2.5 millimeter, and the minimal reflection absorption value can reach-34dB.Under the situation that the thickness of sample remains unchanged substantially, after orientation process, can improve the maximum reflection loss value greatly as can be seen.
The compound matrix material that obtains of material and heat-curable epoxy resin as shown in Figure 3, minimal reflection is absorbed in 2～2.5 millimeters and can reaches-28dB.Therefore to recommend to adopt heat-curable epoxy resin be caking agent in the present invention, can improve the reflection loss value greatly under the situation that sample thickness remains unchanged substantially like this.On the other hand, as being carried out orientation process again, material can obtain the better matrix material of absorbing property.
Take by weighing 2.312 gram ceriums, 2.254 gram cobalts and 4.984 gram iron, under argon shield, be smelted into ingot casting.One week of annealing in the vitreosil pipe under 1000 ℃.Grind to form about 70 microns particle with moving back the ingot casting that overdoes with agate mortar, then particle is added 60 ml n-hexane wet-millings with planetary ball mill in agate jar, ratio of grinding media to material is 10: 1, ball milling speed is 200 rev/mins, adopt the mode of rotating ball milling, in 1 hour timed interval, ball milling total time is set at 16 hours, with the sample oven dry, obtain Nd at last
2Fe
17Material.Then sample is divided 3 kinds of situations compound: the paraffin that (1) and normal hexane have diluted is 35 with volume ratio; 65 mix, and after the oven dry it are inserted in the mould (internal diameter is 3.04 millimeters, and external diameter is 7.00 millimeters), and compression moulding under 1 MPa pressure is taken out then and carried out microwave test.(2) paraffin that has diluted with normal hexane is to mix at 35: 65 with volume ratio, (internal diameter is 3.04 millimeters after the oven dry it to be inserted the mould of nonmagnetic substance preparation, external diameter is 7.00 millimeters) in, mould is placed 90 ℃ of insulations of baking oven 15 minutes, paraffin is melted, just mould is put into magnetic field internal rotation orientation then, the magnetic field size is 0.8～1.2T (tesla), the speed of rotation is about 120 rev/mins, sample is solidified fully in lasting 20 minutes, takes out then and carries out microwave test.(3) with acetone diluted epoxy be to mix at 35: 65 with volume ratio, being pressed into internal diameter after the oven dry is 3.04mm, external diameter is 7.00 millimeters, thickness is 2-3 millimeter ring-type sample, then sample is put into vacuum drying oven and is solidified 1 hour for 140 ℃, tests then.Its X-ray diffraction spectrogram is listed in Fig. 1, and the absorption of electromagnetic wave performance is seen Fig. 2 and Fig. 3.
This material of present embodiment 2 gained is pure 2: 17 phase samples as shown in Figure 4.After orientation, have only a strong diffraction peak to be (006) peak, present embodiment 1 gained material has planar magnetacrystalline anisotropy at normal temperatures as can be known.
As shown in Figure 5 material and paraffin compound after, do not have the orientation situation under, be 2～6GHz in frequency, thickness is at 2～2.5 millimeters, and reflection loss is about-9dB, and through after the orientation, at 3～6GHz, thickness is at 2～2.5 millimeters, and the minimal reflection absorption value can reach-21dB.Under the situation that thickness remains unchanged substantially, orientation can improve the maximum reflection loss value as can be seen.
The compound matrix material that obtains of material and heat-curable epoxy resin as shown in Figure 6, minimal reflection is absorbed in 2～2.5 millimeters and can reaches-29dB.Therefore to recommend to adopt heat-curable epoxy resin be caking agent in the present invention, can improve the reflection loss value greatly under the situation that sample thickness remains unchanged substantially like this.On the other hand, as being carried out orientation process again, material can obtain the better matrix material of absorbing property.
Claims (7)
1. electromagnetic wave absorbent material, the general formula that it is characterized in that material is R
2(Co
1-xFe
x)
17, R is Nd or Ce in the general formula, and when R is the Nd element, 0≤x≤1, when R is the Ce element, 0.6≤x≤0.8, and the easy magnetization axis of material is vertical with the C axle.
2. the described electromagnetic wave absorbent material of claim 1, its chemical formula is: Nd
2Fe
17
3. the described electromagnetic wave absorbent material of claim 1, its chemical formula is: Ce
2(Co
0.7Fe
0.3)
17
4. according to the preparation method of the described arbitrary electromagnetic wave absorbent material of claim 1 to 3, it is characterized in that rare earth element, iron and cobalt are smelted into alloy, and quench after the full and uniformization processing at high temperature, carry out ball-milling processing after again the alloy powder breakdown mill being become tiny particle, obtain metal-powder.
5. the method for preparing matrix material with the described electromagnetic wave absorbent material of claim 1, it is characterized in that described material is put into uncured matrix material, after thorough mixing is even, put into the mould that nonmagnetic substance is made again, mould is placed magnetic field, mould is rotated in magnetic field, so material is carried out orientation process and solidify up to matrix material, matrix material described here is resin or paraffin wax, or polyethylene, or macromolecular material such as polypropylene.
6. the described method of claim 5, magnetic field is 10 when it is characterized in that orientation process
-4～10T, the mould speed of rotation is 1～200 rev/min.
7. claim 5 or 6 described composite process is characterized in that used matrix material is a heat-curable epoxy resin.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104319049A (en) * | 2014-11-06 | 2015-01-28 | 钢铁研究总院 | Easy-plane type bi-phase nano-crystalline high-frequency soft magnetic material and preparation method thereof |
| CN104835610A (en) * | 2014-07-04 | 2015-08-12 | 兰州大学 | Flake high frequency soft magnetic micro powder fracturing along C crystal face, preparation method therefor and application thereof |
| CN105647333A (en) * | 2014-10-11 | 2016-06-08 | 邓智平 | Preparation method of rare earth transition intermetallic compound/ferrite composite radar absorbing coating |
| CN106848597A (en) * | 2016-12-28 | 2017-06-13 | 北京大学 | A kind of electromagnetic wave absorbent material with substitution atoms modulating characteristic and preparation method thereof |
| CN107474618A (en) * | 2017-08-25 | 2017-12-15 | 中国科学院宁波材料技术与工程研究所 | A kind of high-temperature electromagnetic wave absorbent, microwave absorbing coating and preparation method thereof |
| CN113795133A (en) * | 2021-09-13 | 2021-12-14 | 合肥工业大学 | Preparation method of layered magnetic orientation photosensitive resin-based electromagnetic wave absorber |
| CN114683570A (en) * | 2022-04-13 | 2022-07-01 | 福州大学 | Dip-dyed embedded artificial magnetite with controllable magnetic parameters and manufacturing method thereof |
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Cited By (8)
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|---|---|---|---|---|
| CN104835610A (en) * | 2014-07-04 | 2015-08-12 | 兰州大学 | Flake high frequency soft magnetic micro powder fracturing along C crystal face, preparation method therefor and application thereof |
| CN105647333A (en) * | 2014-10-11 | 2016-06-08 | 邓智平 | Preparation method of rare earth transition intermetallic compound/ferrite composite radar absorbing coating |
| CN104319049A (en) * | 2014-11-06 | 2015-01-28 | 钢铁研究总院 | Easy-plane type bi-phase nano-crystalline high-frequency soft magnetic material and preparation method thereof |
| CN106848597A (en) * | 2016-12-28 | 2017-06-13 | 北京大学 | A kind of electromagnetic wave absorbent material with substitution atoms modulating characteristic and preparation method thereof |
| CN107474618A (en) * | 2017-08-25 | 2017-12-15 | 中国科学院宁波材料技术与工程研究所 | A kind of high-temperature electromagnetic wave absorbent, microwave absorbing coating and preparation method thereof |
| CN113795133A (en) * | 2021-09-13 | 2021-12-14 | 合肥工业大学 | Preparation method of layered magnetic orientation photosensitive resin-based electromagnetic wave absorber |
| CN113795133B (en) * | 2021-09-13 | 2024-01-26 | 合肥工业大学 | Preparation method of layered magnetically oriented photosensitive resin-based electromagnetic wave absorber |
| CN114683570A (en) * | 2022-04-13 | 2022-07-01 | 福州大学 | Dip-dyed embedded artificial magnetite with controllable magnetic parameters and manufacturing method thereof |
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Application publication date: 20101110 |