CN106675516A - Transition metal chalcogenide-carbonyl iron powder composite microwave absorbent and preparation method thereof - Google Patents
Transition metal chalcogenide-carbonyl iron powder composite microwave absorbent and preparation method thereof Download PDFInfo
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- CN106675516A CN106675516A CN201611084463.6A CN201611084463A CN106675516A CN 106675516 A CN106675516 A CN 106675516A CN 201611084463 A CN201611084463 A CN 201611084463A CN 106675516 A CN106675516 A CN 106675516A
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- transition metal
- metal chalcogenide
- carbonyl iron
- iron dust
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Abstract
The invention discloses a transition metal chalcogenide-carbonyl iron powder composite microwave absorbent and a preparation method thereof. The composite microwave absorbent is mainly composed of transition metal chalcogenide flakes and carbonyl iron powder, wherein the chemical formula of the transition metal chalcogenide is AB2; A is Mo, W or Ti; B is S, Se or Te. The preparation method comprises the following steps: mixing coarse transition metal chalcogenide powder with an organic solvent; preparing the transition metal chalcogenide flakes by a liquid phase ultrasonic stripping method; then mixing the transition metal chalcogenide flakes with the carbonyl iron powder to obtain the composite microwave absorbent. The composite microwave absorbent provided by the invention can effectively increase the microwave absorption peak, broaden the microwave absorption frequency band, and greatly reduce the matching thickness, and is an ideal high-performance microwave absorbent.
Description
Technical field
The invention belongs to microwave absorption and technical field of electromagnetic shielding, and in particular to a kind of transition metal sulfur family
Thing-carbonyl iron dust composite microwave absorbent and preparation method thereof.
Background technology
Absorbing material refers to electromagnetic wave energy absorbable, that attenuating space is incident, and reduces or eliminates reflection of electromagnetic wave
One class functional material, it gradually develops from after nineteen forties, is initially applied to the stealthy of weaponry.Absorbing material
It is made up of binding agent and absorbent mixing, loss mode of the absorbent by electromagnetic wave in material internal is divided into dielectric loss type absorbent
（Such as metal powder, graphite, carbon black, carbon fiber, CNT, conducting polymer, piezoelectric ceramics）With magnetic loss type absorbent（Such as
Ferrite, magnetic metal）Two major classes.Dielectric loss type includes two kinds of resistive heat losses type and directric relaxation loss-type again.Resistance heat
The principle of loss is that electromagnetic wave senses generation electric current in material, and electric current is obstructed in material internal transmission and is converted into interior energy.Electricity
Conductance is bigger, and the macroscopic electrical current that carrier causes is bigger, is more conducive to electromagnetic energy to be changed into heat energy.The principle of directric relaxation loss
Polarization with dielectric molecule is relevant.In the presence of external electric field, the particle positive and negative charge center of gravity of medium is separated, and is changed into it
Dipole, this process is referred to as electric polarization.Electric polarization needs the regular hour, in the presence of alternating electric field, when this polarization
When lagging behind the frequency of external electric field, the delayed of polarization is just generated, so as to produce directric relaxation to be lost.Dielectric loss type absorbent
Often there is dielectric constant higher and electrical loss angle tangent.The principle of magnetic loss is magnetic material in magnetic history and magnetic reversal
During some energy be irreversibly changed into heat energy, including magnetic hystersis loss, eddy-current loss and residual loss.Magnetic loss type
Absorbent often has magnetic conductivity higher and magnetic loss angle tangent.
The carbon such as graphite, carbon black, carbon fiber and CNT system absorbent has the advantages that density is small and dielectric constant is larger,
But the impedance matching property of itself is poor when being applied to inhale ripple field, and effective Absorber Bandwidth is narrower.Conduction high polymer has pi-electron
Conjugated system, free radical is introduced by being entrained in its chain structure, the presence and transition of this kind of dipole make it have electric conductivity.
Conducting polymer is because density is small, the layout of structure diversity and uniqueness, is increasingly favored, but problem absorbs with carbon system
Agent is the same, and impedance matching is poor, it is narrow to inhale wave frequency band.Ferrite Absorber includes hexaplanar Magnetoplumbate-type, cubic system spinelle
Three major families of type and rare earth garnet type, with absorbing, ripple is strong, effective Absorber Bandwidth is wider, resistance to corrosion is strong and low cost
The advantages of, but there is the deficiencies such as density is big, matching thickness is big.Magnetic metal material（Such as Fe, Co, Ni metal and its alloy）Bag
Include two classes：One class is magnetic metal micro mist, such as Co powder, Ni powder；Another kind of is metal carbonyl wave absorbing agent.This kind of material has full
The advantages of, magnetic conductivity high with the intensity of magnetization and big dielectric constant, but corrosion resistance is low, and becoming caused by high conductivity
Skin effect can cause the magnetic conductivity to reduce, and absorbing property declines.As can be seen here, existing traditional absorbing material be difficult to meet " it is thin,
Gently, it is wide, strong " technical requirements.
The content of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, there is provided one kind can improve microwave absorption peak
It is worth, widens microwave absorption frequency band and can make transition metal chalcogenide-carbonyl iron dust composite microwave that matching thickness is substantially reduced
Absorbent and preparation method thereof.
In order to solve the above technical problems, the present invention uses following technical scheme：
A kind of transition metal chalcogenide-carbonyl iron dust composite microwave absorbent, the composite microwave absorbent is main by transition
Metal chalcogenide thin slice is constituted with carbonyl iron dust, and the chemical formula of transition metal chalcogenide is AB2, wherein, A be Mo, W or
Ti, B are S, Se or Te.
In above-mentioned transition metal chalcogenide-carbonyl iron dust composite microwave absorbent, it is preferred that the Transition Metal Sulfur
The mass ratio 1: 0.5~6 of race's compound thin slice and carbonyl iron dust；And/or, the sheet of transition metal chalcogenide thin slice described in 0 ＜
10 μm of horizontal particle diameter ＜.
In above-mentioned transition metal chalcogenide-carbonyl iron dust composite microwave absorbent, it is preferred that the Transition Metal Sulfur
Race's compound thin slice is prepared through liquid phase ultrasound stripping method with organic solvent by transition metal chalcogenide meal；The transition
Metal chalcogenide meal is 0.5g~4g: 1L with the mass volume ratio of organic solvent；The organic solvent is N- methyl -2- pyrroles
Pyrrolidone（NMP）, N- ethyl-2-pyrrolidones（NVP）And isopropanol（IPA）In one or more.
It is compound present invention also offers a kind of transition metal chalcogenide-carbonyl iron dust as a total technology design
The preparation method of microwave absorption, including transition metal chalcogenide meal is mixed with organic solvent, shelled using liquid phase ultrasound
Transition metal chalcogenide thin slice is prepared from method, then transition metal chalcogenide thin slice is mixed with carbonyl iron dust, obtained
Cross metal chalcogenide-carbonyl iron dust composite microwave absorbent.
In the preparation method of above-mentioned transition metal chalcogenide-carbonyl iron dust composite microwave absorbent, it is preferred that including
Following steps：
（1）Transition metal chalcogenide meal is mixed with organic solvent, after gained mixed liquor is through ultrasound, stripping product is obtained molten
Glue；
（2）Gained stripping product colloidal sol is centrifuged, gained sediment is cleaned and is centrifuged repeatedly, obtains removal organic molten
The sediment of agent（Basic removal）；
（3）The sediment for removing organic solvent is dried, transition metal chalcogenide thin slice is obtained；
（4）Transition metal chalcogenide thin slice is well mixed with carbonyl iron dust, transition metal chalcogenide-carbonyl iron dust is obtained
Composite microwave absorbent.
In the preparation method of above-mentioned transition metal chalcogenide-carbonyl iron dust composite microwave absorbent, it is preferred that described
Step（1）In, the chemical formula of transition metal chalcogenide is AB2, wherein, A is Mo, W or Ti, and B is S, Se or Te；And/or, institute
It is 0.5g~4g: 1L that transition metal chalcogenide meal is stated with the mass volume ratio of organic solvent；And/or, the organic solvent
It is one or more in METHYLPYRROLIDONE, N- ethyl-2-pyrrolidones and isopropanol.
In the preparation method of above-mentioned transition metal chalcogenide-carbonyl iron dust composite microwave absorbent, it is preferred that described
Step（1）In, the ultrasound is interval ultrasound, and, each 20min~40min ultrasonic 1 time every 10min~20min is described super
The total time of sound is 1h~11h.
In the preparation method of above-mentioned transition metal chalcogenide-carbonyl iron dust composite microwave absorbent, it is preferred that described
Step（2）In, the speed of the stripping product colloidal sol and sediment centrifugation is 6000rpm~12000rpm, and the stripping is produced
The time of thing colloidal sol and sediment centrifugation is 15min~30min；The sediment is cleaned repeatedly and the number of times that is centrifuged is 3~5
It is secondary.
In the preparation method of above-mentioned transition metal chalcogenide-carbonyl iron dust composite microwave absorbent, it is preferred that described
Step（3）In, the dry condition is vacuum condition, and the dry temperature is 80 DEG C~90 DEG C, the dry time
It is 2h~10h.
In the preparation method of above-mentioned transition metal chalcogenide-carbonyl iron dust composite microwave absorbent, it is preferred that described
Step（4）In, the step（4）In, the mass ratio 1: 0.5~6 of the transition metal chalcogenide thin slice and carbonyl iron dust.
Main innovation point of the invention is：Will be with MoS2It is the transition metal chalcogenide TMDs for representing（AB2Such as MoS2、
WS2、TiS2、MoSe2、WSe2）Meal is moderately peeled off and obtains thin slice, and A rooms or B can be introduced while specific surface area is increased
Room, it is highly beneficial to improving electrical loss by the introduced defect polarization in room and high-specific surface area.TMDs is to electromagnetic wave
Absorb based on dielectric loss, therefore, it can mix by the carbonyl iron dust absorbent with magnetic loss type, material is had electric damage concurrently
Consumption and magnetic loss characteristic, so can not only improve absorptivity of the material to electromagnetic wave, and can improve impedance matching, make many
Number electromagnetic wave can enter the inside of absorbing material.Additionally, TMDs is non-conductive, it is combined with the carbonyl iron dust of high conductivity,
Conducting particles can be made effectively to disperse, so as to avoid adverse effect of the Kelvin effect to magnetic conductivity, it is ensured that carbonyl iron dust magnetic
The normal performance of loss ability.It is this to be designed with beneficial to a kind of new and effective microwave absorption of acquisition.
Compared with prior art, the advantage of the invention is that：
1st, composite microwave absorbent of the invention matching thickness be 2mm when, to the electromagnetic wave highest of 2~18GHz frequency ranges
Absorptivity reaches -46.68dB, and the effective bandwidth that decay reaches -10dB reaches 7.6GHz.The material can be used as simulation and stealthy and hand
The protection occasion of some electromagnetic radiation such as machine, household electrical appliance.
2nd, preparation method of the invention carries out liquid phase ultrasound stripping to transition metal chalcogenide meal and obtains thin slice first,
The dielectric loss of powder is improve, then mixes this magnetic loss type absorbent of itself and carbonyl iron dust, material is had electric damage concurrently
Consumption and magnetic loss characteristic, so can not only improve absorptivity of the material to electromagnetic wave, and can improve impedance matching, make many
Number electromagnetic wave can enter the inside of absorbing material.Additionally, TMDs is non-conductive, it is combined with the carbonyl iron dust of high conductivity,
Conducting particles can be made effectively to disperse, so as to avoid adverse effect of the Kelvin effect to magnetic conductivity, it is ensured that carbonyl iron dust magnetic
The normal performance of loss ability.Test result shows that above treatment can improve microwave absorption peak really, widen microwave absorption
Frequency band, and matching thickness is substantially reduced, the target of " thin, light, wide, strong " required by absorbing material is met, it is a kind of
Preferable high performance microwave absorbent.
3rd, preparation method of the invention is simple and easy to apply, and production cost is relatively low, is adapted to the industrialized production of certain scale.
Brief description of the drawings
Fig. 1 is MoS prepared by the embodiment of the present invention 12Peel off the XRD spectrum of product.
Fig. 2 is MoS prepared by the embodiment of the present invention 12Peel off the SEM image of product.
Fig. 3 is the reflection loss collection of illustrative plates of composite microwave wave absorbing agent prepared by the embodiment of the present invention 1（Absorbent contents
80wt%）.
Fig. 4 is the reflection loss collection of illustrative plates of composite microwave wave absorbing agent prepared by the embodiment of the present invention 2（Absorbent contents
80wt%）.
Fig. 5 is the reflection loss collection of illustrative plates of composite microwave wave absorbing agent prepared by the embodiment of the present invention 3（Absorbent contents
80wt%）.
Fig. 6 is the reflection loss collection of illustrative plates of composite microwave wave absorbing agent prepared by the embodiment of the present invention 4（Absorbent contents
80wt%）.
Specific embodiment
Below in conjunction with Figure of description and specific preferred embodiment, the invention will be further described, but not therefore and
Limit the scope of the invention.
Material and instrument employed in following examples are commercially available.
Embodiment 1：
A kind of transition metal chalcogenide-carbonyl iron dust composite microwave absorbent, the composite microwave absorbent is main by transition gold
Category chalkogenide thin slice is constituted with carbonyl iron dust, and the chemical formula of transition metal chalcogenide is AB2, wherein, A is Mo, and B is S, i.e.,
MoS2.The microscopic appearance of transition metal chalcogenide is flake, 4 μm of 0 ＜ sheets transverse direction particle diameter ＜.
A kind of preparation method of the transition metal chalcogenide of above-mentioned the present embodiment-carbonyl iron dust composite microwave absorbent,
Comprise the following steps：
（1）0.1g MoS are weighed with assay balance2Meal, with 50.0mL organic solvent METHYLPYRROLIDONEs（NMP）It is mixed
Close, be placed in beaker, be made into the mixed liquor that concentration is 2g/L, then sealed beaker with preservative film and rubber band, be placed in constant temperature
In ultrasonic cleaning machine, interval ultrasound 5h, each 30min ultrasonic 1 time every 10min obtain peeling off product colloidal sol；
（2）Product colloidal sol will be peeled off and be transferred to centrifuge tube, it is with glue head dropper that upper strata is clear with 12000rpm centrifugation 15min
Liquid is carefully removed, and is precipitated thing；Sediment is cleaned with absolute ethyl alcohol, with 12000rpm centrifugation 15min, is retained
Precipitation, repeats above-mentioned cleaning-centrifugally operated to sediment 3 times, obtains removing substantially the sediment of organic solvent；
（3）The sediment of basic removal organic solvent is put into vacuum drying chamber, is dried at 80 DEG C, drying time is 8h,
Obtain dry MoS2Peel off product, i.e. MoS2Thin slice.As shown in figure 1, using X-ray diffractometer（Bruker, D8 Advance）Survey
Examination peel off product crystal structure and with stripping before contrasted, as a result show：MoS2It is hexagonal crystal system（PDF No. 37-
1492）.Wherein, 14.39 °, 29.02 °, 33.51 °, 44.15 °, 60.14 ° of characteristic diffraction peak correspond respectively to MoS2's
（002）、（004）、（101）、（006）With（008）Crystal face.（002）Diffraction maximum is MoS2Stratiform piles up the important indicator of degree.Peak
Value is stronger, then the explanation accumulation number of plies is more；Peak value is weaker, shows that stratiform piles up the number of plies fewer.After ultrasonically treated, in powder
（002）Peak with（101）Signal than substantially decrease, it is meant that successfully realize peel off.As shown in Fig. 2 using Flied emission scanning electron
Microscope（The SBH of TESCAN, VEGA 3）Observation powder morphology, as a result shows that stripping product is flaky texture, and horizontal particle diameter exists
Micron dimension.
（4）By step（3）The MoS for obtaining2Thin slice is well mixed with carbonyl iron dust in mass ratio 1: 3, that is, obtain required product
Product transition metal chalcogenide-carbonyl iron dust composite microwave absorbent.By composite microwave absorbent and melt paraffin in mass ratio 4
: 1 is well mixed, and internal diameter is pressed into a mold for 3mm, and external diameter is 7mm, coaxial rings sample of the thickness in 2.5mm.Using waveguide
Method, using vector network analyzer（Agilent8720ET）Detect suction of the product to the electromagnetic wave of 2~18GHz frequency ranges
Characteristic is received, as shown in figure 3, the matching thickness of composite microwave absorbent has substantially reduction, reflection compared with two kinds of single group unit absorbents
Effective bandwidth of the loss more than -10dB is then substantially widened, respectively 2mm and 5.68GHz（9.36~15.04GHz scopes it
Difference）, maximum reflection is lost apparently higher than carbonyl iron dust absorbent, reaches -32.31dB, and peak value is located at 11.92GHz.With it is compound
The microwave absorption property of first two single group unit absorbent is contrasted, between MoS2Absworption peak（6.88GHz）Inhaled with carbonyl iron dust
Receive peak（16.08GHz）Centre.
Embodiment 2：
A kind of transition metal chalcogenide-carbonyl iron dust composite microwave absorbent, the composite microwave absorbent is main by transition gold
Category chalkogenide thin slice is constituted with carbonyl iron dust, and the chemical formula of transition metal chalcogenide is AB2, wherein, A is Mo, and B is S, i.e.,
MoS2.The microscopic appearance of transition metal chalcogenide is flake, 4 μm of 0 ＜ sheets transverse direction particle diameter ＜.
A kind of preparation method of the transition metal chalcogenide of above-mentioned the present embodiment-carbonyl iron dust composite microwave absorbent,
Comprise the following steps：
（1）0.1g MoS are weighed with assay balance2Meal, with 50.0mL organic solvent METHYLPYRROLIDONEs（NMP）It is mixed
Close, be placed in beaker, be made into the mixed liquor that concentration is 2g/L, then sealed beaker with preservative film and rubber band, be placed in constant temperature
In ultrasonic cleaning machine, interval ultrasound 5h, each 30min ultrasonic 1 time every 10min obtain peeling off product colloidal sol；
（2）Product colloidal sol will be peeled off and be transferred to centrifuge tube, it is with glue head dropper that upper strata is clear with 12000rpm centrifugation 15min
Liquid is carefully removed, and is precipitated thing；Sediment is cleaned with absolute ethyl alcohol, with 12000rpm centrifugation 15min, is retained
Precipitation, repeats above-mentioned cleaning-centrifugally operated to sediment 3 times, obtains removing substantially the sediment of organic solvent；
（3）The sediment of basic removal organic solvent is put into vacuum drying chamber, in 80 DEG C of drying, drying time is 8h, is obtained
Dry MoS2Thin slice；
（4）By MoS2Thin slice is well mixed with carbonyl iron dust in mass ratio 1: 4, obtain final product required product transition metal chalcogenide-
Carbonyl iron dust composite microwave absorbent.Composite microwave absorbent is well mixed with melt paraffin in mass ratio 4: 1, in a mold
Internal diameter is pressed into for 3mm, external diameter is 7mm, coaxial rings sample of the thickness in 3mm.As shown in figure 4, detecting the product using waveguide method
When matching thickness is 2mm, the electromagnetic wave maximum reflection loss to 2~18GHz frequency ranges reaches -46.68dB to product, reflects
Loss reaches effective loss bandwidth of -10dB up to 7.6GHz, and absorption peak is located at 11.2GHz.
Embodiment 3：
A kind of transition metal chalcogenide-carbonyl iron dust composite microwave absorbent, the composite microwave absorbent is main by transition gold
Category chalkogenide thin slice is constituted with carbonyl iron dust, and the chemical formula of transition metal chalcogenide is AB2, wherein, A is Mo, and B is Se,
That is MoSe2.The microscopic appearance of transition metal chalcogenide is flake, 10 μm of 0 ＜ sheets transverse direction particle diameter ＜.
A kind of preparation method of the transition metal chalcogenide of above-mentioned the present embodiment-carbonyl iron dust composite microwave absorbent,
Comprise the following steps：
（1）0.1g MoSe are weighed with assay balance2Meal, with 50.0mL organic solvent METHYLPYRROLIDONEs（NMP）It is mixed
Close, be placed in beaker, be made into the mixed liquor that concentration is 2g/L, then sealed beaker with preservative film and rubber band, be placed in constant temperature
In ultrasonic cleaning machine, interval ultrasound 3h, each 30min ultrasonic 1 time every 10min obtain peeling off product colloidal sol；
（2）Product colloidal sol will be peeled off and be transferred to centrifuge tube, it is with glue head dropper that upper strata is clear with 12000rpm centrifugation 15min
Liquid is carefully removed, and is precipitated thing；Sediment is cleaned with absolute ethyl alcohol, with 12000rpm centrifugation 15min, is retained
Precipitation, repeats above-mentioned cleaning-centrifugally operated to sediment 3 times, obtains removing substantially the sediment of organic solvent；
（3）The sediment of basic removal organic solvent is put into vacuum drying chamber, in 80 DEG C of drying, drying time is 8h, is obtained
Dry MoSe2Thin slice；
（4）By the MoSe2Thin slice is well mixed with carbonyl iron dust in mass ratio 1: 3, obtains final product required product transition metal sulfur family
Thing-carbonyl iron dust composite microwave absorbent.Composite microwave absorbent is well mixed with melt paraffin in mass ratio 4: 1, in mould
Internal diameter is pressed into tool for 3mm, external diameter is 7mm, coaxial rings sample of the thickness in 2.7mm.As shown in figure 5, waveguide method detection should
When matching thickness is 2mm, the electromagnetic wave maximum reflection loss to 2~18GHz frequency ranges reaches -44.55dB to product, instead
Penetrate loss and reach effective loss bandwidth of -10dB up to 4.88GHz, absorption peak is located at 10.64GHz.
Embodiment 4：
A kind of transition metal chalcogenide-carbonyl iron dust composite microwave absorbent, the composite microwave absorbent is main by transition gold
Category chalkogenide thin slice is constituted with carbonyl iron dust, and the chemical formula of transition metal chalcogenide is AB2, wherein, A is W, and B is Se, i.e.,
WSe2.The microscopic appearance of transition metal chalcogenide is flake, 10 μm of sheet transverse direction particle diameter 0 ＜ sheets transverse direction particle diameter ＜.
A kind of preparation method of the transition metal chalcogenide of above-mentioned the present embodiment-carbonyl iron dust composite microwave absorbent,
Comprise the following steps：
（1）0.1g WSe are weighed with assay balance2Meal, mixes with 50.0mL organic solvents NMP, is made into concentration mixing for 2g/L
Liquid is closed, then beaker is sealed with preservative film and rubber band, is placed in thermostatic ultrasonic washer, interval ultrasound 3h, every 10min
Ultrasound 1 time, each 30min obtains peeling off product colloidal sol；
（2）Product colloidal sol will be peeled off and be transferred to centrifuge tube, it is with glue head dropper that upper strata is clear with 12000rpm centrifugation 15min
Liquid is carefully removed, and is precipitated thing；Sediment is cleaned with absolute ethyl alcohol, with 12000rpm centrifugation 15min, is retained
Precipitation, repeats above-mentioned cleaning-centrifugally operated to sediment 3 times, obtains removing substantially the sediment of organic solvent；
（3）The sediment of basic removal organic solvent is put into vacuum drying chamber, in 80 DEG C of drying, drying time is 8h, is obtained
Dry WSe2Thin slice；
（4）By the WSe2Thin slice is well mixed with carbonyl iron dust in mass ratio 1: 3, obtains final product required product transition metal sulfur family
Thing-carbonyl iron dust composite microwave absorbent.Composite microwave absorbent is well mixed with melt paraffin in mass ratio 4: 1, in mould
Internal diameter is pressed into tool for 3mm, external diameter is 7mm, coaxial rings sample of the thickness in 3.1mm.As shown in fig. 6, waveguide method detection should
When matching thickness is 2mm, the electromagnetic wave maximum reflection loss to 2~18GHz frequency ranges reaches -35.29dB to product, instead
Penetrate loss and reach effective loss bandwidth of -10dB up to 5.52GHz, absorption peak is located at 11.52GHz.
Comparative example 1：
A kind of transition metal chalcogenide-barium ferrite composite microwave absorbent, the composite microwave absorbent is main by transition gold
Category chalkogenide thin slice is constituted with barium ferrite, and the chemical formula of transition metal chalcogenide is AB2, wherein, A is Mo, and B is Se,
That is MoSe2.The microscopic appearance of transition metal chalcogenide is flake, 4 μm of 0 ＜ sheets transverse direction particle diameter ＜.
A kind of preparation method of the transition metal chalcogenide of above-mentioned the present embodiment-barium ferrite composite microwave absorbent,
Comprise the following steps：
（1）MoSe2Stripping and drying means with embodiment 3；
（2）By the MoSe2Thin slice is well mixed with barium ferrite in mass ratio 1: 3, obtains final product required product transition metal sulfur family
Thing-ferrite composite microwave absorbent.Composite microwave absorbent is well mixed with melt paraffin in mass ratio 4: 1, in mould
In be pressed into internal diameter for 3mm, external diameter is 7mm, coaxial rings sample of the thickness in 2.6mm.Waveguide method detects that the product is thick in matching
To spend during for 5mm, reach -30.11dB to the loss of the electromagnetic wave maximum reflection of 2~18GHz frequency ranges, reflection loss reaches -
Effective loss bandwidth of 10dB reaches 2.02GHz, and absorption peak is located at 16.4GHz.
Comparative example 2：
A kind of preparation method of transition metal chalcogenide-carbonyl iron dust composite microwave absorbent, comprises the following steps：
（1）0.1g MoS are weighed with assay balance2Meal, with 50.0mL organic solvent METHYLPYRROLIDONEs（NMP）It is mixed
Close, be placed in beaker, be made into the mixed liquor that concentration is 2g/L, then sealed beaker with preservative film and rubber band, be placed in constant temperature
In ultrasonic cleaning machine, interval ultrasound 3h, each 30min ultrasonic 1 time every 10min obtain peeling off product colloidal sol；
（2）Product colloidal sol will be peeled off and be transferred to centrifuge tube, with 6000rpm centrifugation 15min, taken supernatant and be transferred to new centrifugation
Pipe, then with 12000rpm centrifugation 15min, carefully removed supernatant liquor with glue head dropper, it is precipitated thing；Use anhydrous second
Alcohol is cleaned to sediment, with 12000rpm centrifugation 15min, retains precipitation, repeat above-mentioned cleaning to sediment-from
The heart is operated 3 times, obtains removing substantially the sediment of organic solvent；
（3）The sediment of basic removal organic solvent is put into vacuum drying chamber, in 90 DEG C of drying, drying time is 9h, is obtained
Dry MoSe2Thin slice；
（4）By the MoS2Thin slice is well mixed with carbonyl iron dust in mass ratio 1: 3, obtains final product required product transition metal sulfur family
Thing-carbonyl iron dust composite microwave absorbent.Composite microwave absorbent is well mixed with melt paraffin in mass ratio 4: 1, in mould
Internal diameter is pressed into tool for 3mm, external diameter is 7mm, coaxial rings sample of the thickness in 2.4mm.Waveguide method detects the product in matching
When thickness is 2.7mm, the electromagnetic wave maximum reflection loss to 2~18GHz frequency ranges reaches -18.03dB, and reflection loss reaches
Effective loss bandwidth to -10dB reaches 2.81GHz, and absorption peak is located at 15.02GHz.
The above, is only presently preferred embodiments of the present invention, and any formal limitation is not made to the present invention.Though
So the present invention is disclosed as above with preferred embodiment, but is not limited to the present invention.It is any to be familiar with those skilled in the art
Member, in the case where Spirit Essence of the invention and technical scheme is not departed from, all using in the methods and techniques of the disclosure above
Appearance makes many possible variations and modification, or the Equivalent embodiments for being revised as equivalent variations to technical solution of the present invention.Therefore,
Every content without departing from technical solution of the present invention, according to technical spirit of the invention to made for any of the above embodiments any simple
Modification, equivalent, equivalence changes and modification, still fall within the range of technical solution of the present invention protection.
Claims (10)
1. a kind of transition metal chalcogenide-carbonyl iron dust composite microwave absorbent, it is characterised in that the composite microwave absorbs
Agent is mainly made up of transition metal chalcogenide thin slice and carbonyl iron dust, and the chemical formula of transition metal chalcogenide is AB2, its
In, A is Mo, W or Ti, and B is S, Se or Te.
2. transition metal chalcogenide according to claim 1-carbonyl iron dust composite microwave absorbent, it is characterised in that
The transition metal chalcogenide thin slice is 1: 0.5~6 with the mass ratio of carbonyl iron dust；And/or, Transition Metal Sulfur described in 0 ＜
10 μm of the sheet transverse direction particle diameter ＜ of race's compound thin slice.
3. transition metal chalcogenide according to claim 1 and 2-carbonyl iron dust composite microwave absorbent, its feature exists
In the transition metal chalcogenide thin slice is through liquid phase ultrasound stripping method by transition metal chalcogenide meal and organic solvent
Prepare；The transition metal chalcogenide meal is 0.5g~4g: 1L with the mass volume ratio of organic solvent；It is described organic
Solvent is one or more in METHYLPYRROLIDONE, N- ethyl-2-pyrrolidones and isopropanol.
4. the preparation method of a kind of transition metal chalcogenide-carbonyl iron dust composite microwave absorbent, including by Transition Metal Sulfur
Race's compound meal mixes with organic solvent, and transition metal chalcogenide thin slice is prepared using liquid phase ultrasound stripping method, then incited somebody to action
Cross metal chalcogenide thin slice to mix with carbonyl iron dust, obtain transition metal chalcogenide-carbonyl iron dust composite microwave absorbent.
5. the preparation method of transition metal chalcogenide according to claim 4-carbonyl iron dust composite microwave absorbent, its
It is characterised by, comprises the following steps：
（1）Transition metal chalcogenide meal is mixed with organic solvent, after gained mixed liquor is through ultrasound, stripping product is obtained molten
Glue；
（2）Gained stripping product colloidal sol is centrifuged, gained sediment is cleaned and is centrifuged repeatedly, obtains removal organic molten
The sediment of agent；
（3）The sediment for removing organic solvent is dried, transition metal chalcogenide thin slice is obtained；
（4）Transition metal chalcogenide thin slice is well mixed with carbonyl iron dust, transition metal chalcogenide-carbonyl iron dust is obtained
Composite microwave absorbent.
6. the preparation method of transition metal chalcogenide according to claim 5-carbonyl iron dust composite microwave absorbent, its
It is characterised by, the step（1）In, the chemical formula of transition metal chalcogenide is AB2, wherein, A is Mo, W or Ti, and B is S, Se
Or Te；And/or, the transition metal chalcogenide meal is 0.5g~4g: 1L with the mass volume ratio of organic solvent；And/or,
The organic solvent is one or more in METHYLPYRROLIDONE, N- ethyl-2-pyrrolidones and isopropanol.
7. the preparation side of the transition metal chalcogenide according to claim 5 or 6-carbonyl iron dust composite microwave absorbent
Method, it is characterised in that the step（1）In, the ultrasound is interval ultrasound, ultrasonic 1 time every 10min~20min, every time
20min~40min, the total time of the ultrasound is 1h~11h.
8. the preparation side of the transition metal chalcogenide according to claim 5 or 6-carbonyl iron dust composite microwave absorbent
Method, it is characterised in that the step（2）In, it is described peel off product colloidal sol and sediment centrifugation speed be 6000rpm~
The time of 12000rpm, the stripping product colloidal sol and sediment centrifugation is 15min~30min；The sediment is repeatedly clear
The number of times washed and be centrifuged is 3~5 times.
9. the preparation side of the transition metal chalcogenide according to claim 5 or 6-carbonyl iron dust composite microwave absorbent
Method, it is characterised in that the step（3）In, the dry condition is vacuum condition, and the dry temperature is 80 DEG C~90
DEG C, the dry time is 2h~10h.
10. the preparation side of the transition metal chalcogenide according to claim 5 or 6-carbonyl iron dust composite microwave absorbent
Method, it is characterised in that the step（4）In, the mass ratio 1: 0.5 of the transition metal chalcogenide thin slice and carbonyl iron dust~
6。
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| CN107286907A (en) * | 2017-07-07 | 2017-10-24 | 中国人民解放军国防科学技术大学 | The molybdenum disulfide of a kind of core shell structure/carbonyl iron composite microwave absorbent and preparation method thereof |
| CN111960468A (en) * | 2020-08-21 | 2020-11-20 | 中国科学院宁波材料技术与工程研究所 | Two-dimensional transition metal chalcogenide wave-absorbing material, preparation method and application thereof |
| CN114775330A (en) * | 2022-06-06 | 2022-07-22 | 山东大学 | Carbon fiber electromagnetic shielding paper and preparation method and application thereof |
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| JPH1013081A (en) * | 1996-06-26 | 1998-01-16 | Nkk Corp | Microwave absorbing material |
| CN105062417A (en) * | 2015-07-15 | 2015-11-18 | 北京新怡源环保科技有限公司 | Organic-inorganic composite nano microwave absorbing material and preparation method thereof |
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| JPH1013081A (en) * | 1996-06-26 | 1998-01-16 | Nkk Corp | Microwave absorbing material |
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| CN111960468A (en) * | 2020-08-21 | 2020-11-20 | 中国科学院宁波材料技术与工程研究所 | Two-dimensional transition metal chalcogenide wave-absorbing material, preparation method and application thereof |
| CN114775330A (en) * | 2022-06-06 | 2022-07-22 | 山东大学 | Carbon fiber electromagnetic shielding paper and preparation method and application thereof |
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