CN107760954B - A kind of new electromagnetic wave absorbing material and preparation method thereof - Google Patents
A kind of new electromagnetic wave absorbing material and preparation method thereof Download PDFInfo
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- CN107760954B CN107760954B CN201610685649.0A CN201610685649A CN107760954B CN 107760954 B CN107760954 B CN 107760954B CN 201610685649 A CN201610685649 A CN 201610685649A CN 107760954 B CN107760954 B CN 107760954B
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- C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
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- C22C1/02—Making non-ferrous alloys by melting
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
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Abstract
The present invention discloses a kind of new electromagnetic wave absorbing material and preparation method thereof.The electromagnetic wave absorbent material is Mn-Sb alloy cpd, chemical general formula MnxSb or (Mn, T)xSb, wherein one of 0.8 < x < 1.4, T Zr, Cr, Cu, V, Si, Zn, C, B, Al, Cd or a variety of any combination.The preparation method of the material is: being Mn:Sb or (Mn by atom ratio, T): Mn the and Sb element mixed smelting or rapid hardening ingot casting of Sb=0.8~1.4, the alloy of NiAs type hexagonal structure is made, is then broken for the other particle of submicron order, can be used as radio-radar absorber.The material has significant absorbability to 1G to 100G frequency range electromagnetic wave, and absorbability is strong, working frequency range is wide；And frequency range position can be adjusted according to use condition, can effectively meet the electro-magnetic wave absorption demand in civil and military field.
Description
Technical field
The present invention relates to electromagnetic wave absorbent materials, add in particular with Mn sill control Mn element ratio to material property
After accurately modulating, it is specially adapted for the electromagnetic wave to work in the case where being higher than the high frequencies of 1G hertz of frequency ranges, broadband environmental requirement
Absorbing material.
Background technique
In recent years, information technology rapidly develops, and the transmission rate and processing frequency that information is continuously improved continue as people
The target of pursuit, widely used working frequency is transformed to working frequency in 1.8- in the 2G mobile phone of 0.9-1.8GHz in the past
The 3G mobile of 2.4GHz develops into working frequency in the 4G cell phone of 3.5GHz or so again soon.Further, since Computing is fast
The raising of degree, clock frequency approach 2GHz, and transmission line actually also works in ghz band.In mechanics of communication and computer
While the working frequency of technology is continuously improved, the electromagnetic interference of microwave and electronic device such as between LSI, CPU also becomes day
It is beneficial serious, this requires develop the high-performance for being applied to ghz band, micromation, low energy consumption novel high-frequency electronic device and
Absorbing material needed for electromagnetism interference.
The development of modern military technology is unprecedented swift and violent, the military target of every country be increasingly easy by enemy radar detection,
Tracking and attack, this allows the stealth technology of weapon system to obtain the extensive attention of various countries, and forms a special skill
Art --- stealth technology.The core of radar stealth technology is to reduce the radar cross section (RCS) of target.Reduce target RCS
Product mainly passes through three approach: shape is stealthy, impedance is stealthy and Material-stealth.Wherein Material-stealth technology inhales wave since it has
Have excellent performance, technique production it is simple the advantages that, occupy an important position in stealth technology.Developing stealth technology is military technology
The important directions of development, so the research of absorbing material as the most important component part of stealth technology, also just becomes each military affairs
Power contends one of the hot spot of military hi-tech.
Now widely used electromagnetic wave absorbing material is Ferrite Material."Broadband and thin microwave
absorber of nickel-zinc ferrite/carbonyl iron”(Journal of Alloys and
Compounds 487 (2009) 708-711) disclose the Wave suction composite material of ferrite and metallic particles；"Dependence
of Microwave Absorbing Property on Ferrite Volume Fraction in MnZn Ferrite-
RubberComposites " (D.Y.Kim, Y.C.Chung, T.W.Kang, and H.C.Kim IEEETRANSACTIONS
ONMAGNETICS, VOL 32, NO 2, MARCH 1996) disclose ferritic electromagnetic wave absorption material；And Ferrite Material
Frequency band it is narrow, density is big, and absorptivity is low, and its working frequency be generally also extremely difficult to GHz to tens GHz superfrequency,
Microwave band in hyperfrequency or even extremely high frequency part range.
But still have the following aspects in place of the shortcomings of the prior art: 1. absorptivities are not high, especially in 5,6GHz
Above frequency range, it is difficult to reach effective absorption intensity.2. working frequency range narrow range, can especially reach effective absorptivity (<-
Bandwidth range 20dB) is smaller.3. matching thickness is excessive, generally for reaching the absorption intensity needs for meeting groundwork needs
Matching thickness is in 3mm or more, or even up to 6-7mm.For such case in some special dimensions, especially military aspect is several
It can not apply.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of new electromagnetic wave absorbing material and preparation method thereof, can
It realizes relatively thin matching thickness, there is significant absorbability to 1G to 100G frequency electromagnetic waves.
The general formula of electromagnetic wave absorbent material of the invention is MnxSb or (Mn, T)xSb, wherein the original of 0.8 < x < 1.4, Mn and T
Sub- proportional region is 13 > Mn:T > 8, and T is that one of element Zr, Cr, Cu, V, Si, Zn, C, B, Al, Cd or a variety of are any
Combination.
It is easy that material may be implemented for NiAs type hexagonal structure in master alloy after the present invention is matched by Mn content appropriate
The direction of magnetization is from basal plane to uniaxial direction continuous transition, to meet the technical indicator that practical suction wave working environment needs.
The chemical formula of the optimal electromagnetic wave absorbent material of the present invention is Mn1.1Sb or (Mn, T)1.0Sb。
The preparation method of electromagnetic wave absorbent material of the invention, comprising the following steps:
1) metal simple-substance Mn, Sb of high-purity, appropriate proportioning Mn are obtainedxSb；Or obtain the metal list of high-purity
Matter Mn, Sb and T, appropriate proportioning are (Mn, T)xSb；The atomic ratio of wherein 0.8 < x < 1.4, Mn and T range preferably from 13 >
Mn:T > 8；
2) by high purity metal simple substance Mn, Sb of step 1) or high purity metal simple substance Mn, Sb and T, by melting system
Standby alloy cast ingot or rapid hardening thin slice；
3) by the alloy cast ingot being smelted into or rapid hardening thin slice, it is broken for the other particle of submicron order, obtains granular electricity
Electro-magnetic wave absorption material, can be used as radio-radar absorber.
Further, after evenly mixing by granular electromagnetic wave absorbent material and bonding agent, satisfaction application is prepared into want
The electro-magnetic wave absorption device asked.
Above-mentioned steps 2) in, Sb and non-volatile when melting is tested by multiple melting, compares the sample quality before and after melting
Variation, it is contemplated that Mn volatilization determines and the Mn of 5~15% mass fractions of additional addition is needed to compensate volatilization.
Above-mentioned steps 2) in, melting electric current is 100-250A, is in addition the uniformity for guaranteeing alloy cast ingot, sample melting 2
~3 times, each 1~5min of melting.In addition it is the uniformity for guaranteeing alloy cast ingot or thin slice, when sample melting and carries out appropriate electricity
Magnetic stirring.
Above-mentioned steps 2) in, gained Mn-Sb rapid hardening sheet length about 1~2cm, thickness about 0.2-0.4mm.
Above-mentioned steps 3) in, for the alloy cast ingot or rapid hardening thin slice being smelted into, progress coarse crushing first is no more than 50
The powder of micron, is then ground to sub-micron rank, then equal with bonding agent, dispersing agent etc. as radio-radar absorber
After even mixing, it is prepared into absorbent, becomes the sample of electromagnetic parameter to be measured through pressing mold.
In addition, the present invention can also mix the metal powder of high-purity Mn and Sb of proper proportion (or by high-purity
Metal simple-substance Mn, Sb and T mixing), carry out being milled to 1~5 micron, be then heat-treated 1~10 hour at 500~860 DEG C,
Also it can get as the alloy or powder of NiAs type hexagonal structure.By alloy or powder according to step 3), it is broken for sub-micron rank
Particle after evenly mixing by particle and bonding agent be prepared into the electro-magnetic wave absorption device for meeting application requirement.The device also has
There is good microwave absorbing property.
It is thick in relatively thin matching that material may be implemented in new electromagnetic wave absorbing material provided by the invention and its technology of preparing
Degree has significant stronger absorbability to 1G to 100G frequency electromagnetic waves.Meanwhile utilizing main preparation provided in the present invention
It is adjustable within the scope of 10GHz that working frequency range may be implemented in technology --- the performance for improving material using the ratio of control Mn element
Distribution；And it may be implemented according to different use conditions, the accurate characteristic for modulating working frequency.The sub-micro meter ruler that the present invention obtains
The Mn-Sb alloy powder of degree, has that absorbability is strong, working frequency range is wide as radio-radar absorber and frequency range position can be with
The characteristic adjusted according to use condition can effectively meet the electro-magnetic wave absorption demand in civil and military field.
Detailed description of the invention
Fig. 1 is the X-ray diffraction figure of the sample of the acquisition of embodiment 1.
Fig. 2 is the X-ray diffraction figure of the sample of the acquisition of embodiment 2.
Fig. 3 is the electro-magnetic wave absorption spectrum curve of embodiment 3.
Fig. 4 is the electro-magnetic wave absorption spectrum curve of embodiment 4.
Fig. 5 is the electro-magnetic wave absorption spectrum curve of embodiment 5.
Specific embodiment
Below by specific embodiments and the drawings, the present invention will be further described.
Embodiment 1:
The manganese and antimony (atomic ratio Mn:Sb=x:1) for weighing proper proportion are prepared into master alloy by melting, or by molten
Refining is quickly solidified as alloy thin band (1-2cm wide, 0.2-0.4mm are thick), is then broken for 50-100 microns of coarse powder, utilizes x-ray
Diffractometer measures its diffraction spectra.Fig. 1 is different MnxThe XRD diagram of Sb alloy, alloy main phase show as NiAs hexagonal structure, wherein x
Value be 1.0,1.1,1.22,1.3 respectively.
Embodiment 2:
The manganese, antimony and the third element T (atomic ratio Mn:T:Sb=0.9:0.1:1) for weighing proper proportion, by melting system
It is standby or alloy thin band (1-2cm wide, 0.2-0.4mm are thick) to be quickly solidified as by melting at master alloy, then it is broken for 50-100
Micron coarse powder, measures its diffraction spectra using x-ray diffraction instrument.Fig. 2 is the Mn for adding different T elements0.9T0.1The XRD of Sb alloy
Figure, alloy main phase show as NiAs hexagonal structure, and wherein T is respectively Zr, Cr, Cu, V, Si, Zn, C, B, Al, Cd.Third is added
The effect of kind element T is: improving the stability of material, improves the intensity of magnetization and Curie temperature of its material, obtain excellent suction
Wave property.
Embodiment 3:
73g Mn and 147g Sb is weighed, alloy cast ingot is quickly solidified as by melting or rapid hardening is alloy strap, then machine
Tool is broken for 50-100 microns of coarse powder, and powder is ball milling 15 hours in gasoline and grinding aid agent solution.Liquid is drained after ball milling discharging,
It dries magnetic powder, does compound bonding pressing mold with paraffin (internal diameter is 3.04 millimeters, and outer diameter is 7.00 millimeters of cylinder rings).In Agilent
Electromagnetic property is measured on vector network analyzer.According to surveyed electromagnetic parameter, the calculation shows that, material is matched in 1.4-2.35mm
Absorption peak strength in thickness range is more than -20dB, and the bandwidth less than -10dB is up to 5.3GHz.When frequency is 8.2GHz
Absorption intensity reach -50dB (matching thickness only 2.35mm).It is as shown in Figure 3 to inhale wave profile.
Embodiment 4:
77g Mn and 143g Sb is weighed, alloy cast ingot is quickly solidified as by melting or rapid hardening is alloy strap, then machine
Tool is broken for 50-100 microns of coarse powder, and powder is ball milling 15 hours in gasoline and grinding aid agent solution.Liquid is drained after ball milling discharging,
It dries magnetic powder, does compound bonding pressing mold with paraffin (internal diameter is 3.04 millimeters, and outer diameter is 7.00 millimeters of cylinder rings).In Agilent
Electromagnetic property is measured on vector network analyzer.According to surveyed electromagnetic parameter, the calculation shows that, material is in 2-5mm matching thickness
Absorption peak strength in range can be more than -20dB, and the bandwidth less than -10dB is up to 4GHz.Suction when frequency is 9.86GHz
It receives intensity and reaches -57dB (matching thickness only 2.099mm).It is as shown in Figure 4 to inhale wave profile.
Embodiment 5:
The metal powder of high-purity Mn and Sb of proper proportion is mixed (or by metal simple-substance Mn, Sb and T of high-purity
Mixing), it carries out being milled to 1~5 micron, is then heat-treated 1~10 hour, is also can get as NiAs type six at 500~860 DEG C
The alloy or powder of corner structure.Alloy or powder are further broken for the other particle of submicron order, particle is equal with bonding agent
After even mixing, it is prepared into the electro-magnetic wave absorption device for meeting application requirement.Electromagnetism is measured on Agilent vector network analyzer
Property.According to surveyed electromagnetic parameter, the calculation shows that, absorption peak strength of the material within the scope of 1.4-2.2mm matching thickness is equal
More than -20dB, the bandwidth less than -10dB is up to 4.7GHz.Absorption intensity when frequency is 10.5GHz reaches -59dB (matching
Thickness is only 2.1mm) device have good microwave absorbing property.It is as shown in Figure 5 to inhale wave profile.
The above embodiments are merely illustrative of the technical solutions of the present invention rather than is limited, the ordinary skill of this field
Personnel can be with modification or equivalent replacement of the technical solution of the present invention are made, without departing from the spirit and scope of the present invention, this
The protection scope of invention should be subject to described in claims.
Claims (9)
1. a kind of electromagnetic wave absorbent material, which is characterized in that it is MnxSb, wherein 0.8 < x < 1.4；The electromagnetic wave absorbent material is adopted
It is made of following steps:
1) metal simple-substance Mn, Sb of high-purity are obtained, proportion is MnxSb, wherein 0.8 < x < 1.4；
2) by metal simple-substance Mn, Sb, alloy cast ingot or rapid hardening thin slice are prepared by melting；
3) alloy cast ingot being smelted into or rapid hardening thin slice are broken for the other particle of submicron order, obtain granular electromagnetic wave and inhales
Receive agent.
2. electromagnetic wave absorbent material as described in claim 1, which is characterized in that x=1.1.
3. a kind of electromagnetic wave absorbent material, which is characterized in that it is (Mn, T)xSb, wherein the atomic ratio of 0.8 < x < 1.4, Mn and T
Example range is 13 > Mn:T > 8, one of T Zr, Cr, Cu, V, Si, Zn, C, B, Al, Cd or a variety of any combination；It should
Electromagnetic wave absorbent material is made of following steps:
1) metal simple-substance Mn, Sb and T of high-purity are obtained, proportion is (Mn, T)xSb, wherein the atom of 0.8 < x < 1.4, Mn and T
Proportional region is 13 > Mn:T > 8；
2) by metal simple-substance Mn, Sb and T, alloy cast ingot or rapid hardening thin slice are prepared by melting；
3) alloy cast ingot being smelted into or rapid hardening thin slice are broken for the other particle of submicron order, obtain granular electromagnetic wave and inhales
Receive agent.
4. electromagnetic wave absorbent material as claimed in claim 3, which is characterized in that x=1.0.
5. a kind of method for preparing electromagnetic wave absorbent material described in claim 1 or 3, which comprises the following steps:
1) metal simple-substance Mn, Sb of high-purity are obtained, proportion is MnxSb, wherein 0.8 < x < 1.4；Or obtain the gold of high-purity
Belong to simple substance Mn, Sb and T, proportion is (Mn, T)xSb, wherein the atomic ratio range of 0.8 < x < 1.4, Mn and T are 13 > Mn:T
> 8；
2) by metal simple-substance Mn, Sb or metal simple-substance Mn, Sb and T, alloy cast ingot or rapid hardening thin slice are prepared by melting；
3) alloy cast ingot being smelted into or rapid hardening thin slice are broken for the other particle of submicron order, obtain granular electromagnetic wave and inhales
Receive agent.
6. method as claimed in claim 5, which is characterized in that for step 2) in melting, melting electric current is 100-250A, sample
Melting 2~3 times, each 1~5min of melting；Electromagnetic agitation appropriate is carried out in sample melting to guarantee alloy cast ingot or thin slice
Uniformity, and add the Mn of 5~15% mass fractions additionally to compensate the volatilization of Mn.
7. method as claimed in claim 5, which is characterized in that the length of the resulting rapid hardening thin slice of step 2) is 1~2cm, thick
Degree is 0.2-0.4mm.
8. method as claimed in claim 5, which is characterized in that thin for the alloy cast ingot or rapid hardening that are smelted into step 3)
Piece, first progress coarse crushing, obtains the powder no more than 50 microns, is then ground to sub-micron rank.
9. method as claimed in claim 5, which is characterized in that by the resulting granular radio-radar absorber of step 3) and glue
It connects agent, dispersing agent after evenly mixing, is prepared into the electro-magnetic wave absorption composite material for meeting application requirement.
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| CN1767757A (en) * | 2005-09-16 | 2006-05-03 | 浙江工业大学 | Electromagnetic wave absorbing material |
| CN101166413A (en) * | 2006-10-20 | 2008-04-23 | 财团法人工业技术研究院 | Electromagnetic wave absorption materials |
| CN104039122A (en) * | 2014-06-25 | 2014-09-10 | 北京大学 | Electromagnetic-wave absorbing material with interstitial modulation characteristics and production method of electromagnetic-wave absorbing material |
| CN104073664A (en) * | 2014-04-01 | 2014-10-01 | 广西大学 | Preparation method for obtaining accurate-composition Mn-Sb-based alloy |
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| CN1767757A (en) * | 2005-09-16 | 2006-05-03 | 浙江工业大学 | Electromagnetic wave absorbing material |
| CN101166413A (en) * | 2006-10-20 | 2008-04-23 | 财团法人工业技术研究院 | Electromagnetic wave absorption materials |
| CN104073664A (en) * | 2014-04-01 | 2014-10-01 | 广西大学 | Preparation method for obtaining accurate-composition Mn-Sb-based alloy |
| CN104039122A (en) * | 2014-06-25 | 2014-09-10 | 北京大学 | Electromagnetic-wave absorbing material with interstitial modulation characteristics and production method of electromagnetic-wave absorbing material |
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