CN106675516B - A kind of transition metal chalcogenide-carbonyl iron dust composite microwave absorbent and preparation method thereof - Google Patents
A kind of transition metal chalcogenide-carbonyl iron dust composite microwave absorbent and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of transition metal chalcogenide carbonyl iron dust composite microwave absorbents and preparation method thereof.Composite microwave absorbent is mainly made of transition metal chalcogenide thin slice with carbonyl iron dust, and the chemical formula of transition metal chalcogenide is AB2, A Mo, W or Ti, B S, Se or Te.Preparation method includes mixing transition metal chalcogenide coarse powder with organic solvent, and transition metal chalcogenide thin slice is prepared, then transition metal chalcogenide thin slice is mixed with carbonyl iron dust to get composite microwave absorbent using liquid phase ultrasound stripping method.The composite microwave absorbent of the present invention can effectively improve microwave absorption peak, widen microwave absorption frequency band, and can substantially reduce matching thickness, be a kind of ideal high performance microwave absorbent.
Description
Technical field
The invention belongs to microwave absorptions and technical field of electromagnetic shielding, and in particular to a kind of transition metal sulfur family
Object-carbonyl iron dust composite microwave absorbent and preparation method thereof.
Background technology
Absorbing material refers to can absorb, the electromagnetic wave energy of attenuating space incidence, and reduces or eliminates reflection of electromagnetic wave
A kind of functional material, it gradually develops after nineteen forties, is initially applied to the stealthy of weaponry.Absorbing material
It is made of binding agent and absorbent mixing, absorbent is divided into dielectric loss type absorbent by loss mode of the electromagnetic wave in material internal
（Such as metal powder, graphite, carbon black, carbon fiber, carbon nanotube, conducting polymer, piezoelectric ceramics）With magnetic loss type absorbent（Such as
Ferrite, magnetic metal）Two major class.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 macroscopic electrical current is bigger caused by carrier, is more conducive to electromagnetic energy and is changed into thermal energy.The principle of directric relaxation loss
It is related with the polarization of dielectric molecule.Under the action of external electric field, the particle positive and negative charge center of gravity separation of medium is changed into it
Dipole, this process are known as electric polarization.Electric polarization needs the regular hour, under the action of alternating electric field, when this polarization
When lagging behind the frequency of external electric field, polarized lag is just produced, so as to generate directric relaxation loss.Dielectric loss type absorbent
Often there is higher dielectric constant and electrical loss angle tangent.The principle of magnetic loss is magnetic material in magnetic history and magnetic reversal
Some energy is irreversibly changed into thermal energy in the process, including magnetic hystersis loss, eddy-current loss and residual loss.Magnetic loss type
Absorbent often has higher magnetic conductivity and magnetic loss angle tangent.
The carbon such as graphite, carbon black, carbon fiber and carbon nanotube system absorbent has many advantages, such as that density is small and dielectric constant is larger,
But the impedance matching property of itself is poor during applied to suction wave field, and effective Absorber Bandwidth is relatively narrow.Conduction high polymer has pi-electron
Conjugated system introduces free radical by being entrained in its chain structure, and the presence and transition of this kind of dipole make it have electric conductivity.
Conducting polymer is increasingly favored since density is small, structure diversity and unique layout, but problem is absorbed 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, wave is strong, effective Absorber Bandwidth is wider, resistance to corrosion is strong and at low cost
The advantages that, but there are the deficiencies of density is big, matching thickness is big.Magnetic metal material（Such as Fe, Co, Ni metal and its alloy）Packet
Include two classes：One kind 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
With the advantages that intensity of magnetization is high, magnetic conductivity and dielectric constant are big, but corrosion resistance is low, and becoming caused by high conductivity
Skin effect can cause magnetic conductivity to reduce, and absorbing property declines.It can be seen that existing tradition absorbing material be difficult to meet " it is thin,
Gently, it is wide, strong " technology requirement.
Invention content
The technical problem to be solved by the present invention is to overcome the deficiencies in the prior art, and microwave absorption peak can be improved by providing one kind
Transition metal chalcogenide-carbonyl iron dust the composite microwave for being worth, widening microwave absorption frequency band and can substantially reduce matching thickness
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 mainly by
Transition metal chalcogenide thin slice is formed with carbonyl iron dust, and the chemical formula of transition metal chalcogenide is AB2, wherein, A Mo, W
Or Ti, B 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 0 transition metal chalcogenide thin slice described in ＜ sheet
Lateral 10 μm of grain size ＜.
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 to be prepared by transition metal chalcogenide coarse powder with organic solvent through liquid phase ultrasound stripping method；The transition
The mass volume ratio of metal chalcogenide coarse powder and organic solvent is 0.5g~4g: 1L；The organic solvent is N- methyl -2- pyrroles
Pyrrolidone（NMP）, N- ethyl-2-pyrrolidones（NVP）And isopropanol（IPA）In it is one or more.
The technical concept total as one, the present invention also provides a kind of transition metal chalcogenide-carbonyl iron dust is compound
The preparation method of microwave absorption including transition metal chalcogenide coarse powder is mixed with organic solvent, is shelled using liquid phase ultrasound
Transition metal chalcogenide thin slice is prepared, then transition metal chalcogenide thin slice is mixed with carbonyl iron dust from method, 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 coarse powder is mixed with organic solvent, gained mixed liquor obtains stripping production after ultrasound
Object colloidal sol；
（2）Gained stripping product colloidal sol is centrifuged, gained sediment clean and centrifuge repeatedly, and obtaining removal has
The sediment of solvent（Basic removal）；
（3）The sediment for removing organic solvent is dried, obtains transition metal chalcogenide thin slice；
（4）Transition metal chalcogenide thin slice with carbonyl iron dust is uniformly mixed, obtains transition metal chalcogenide-carbonyl
Iron powder 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 Mo, W or Ti, B S, Se or Te；And/or institute
The mass volume ratio for stating transition metal chalcogenide coarse powder and organic solvent is 0.5g~4g: 1L；And/or the organic solvent
It is one or more in n-methyl-2-pyrrolidone, 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, 1 time, each 20min~40min ultrasonic every 10min~20min, 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, the stripping production
The time of object colloidal sol and sediment centrifugation is 15min~30min；The number that the sediment is cleaned and centrifuged repeatedly 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 condition of the drying is vacuum condition, and the temperature of the drying is 80 DEG C~90 DEG C, the time of the drying
For 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.
The main innovation point of the present invention is：It will be with MoS2Transition metal chalcogenide TMDs for representative（AB2Such as MoS2、
WS2、TiS2、MoSe2、WSe2）Moderately stripping obtains thin slice to coarse powder, and A vacancy or B can be introduced while specific surface area is increased
Vacancy, by vacancy it is introduced the defects of polarization and high-specific surface area to improve electrical loss it is highly beneficial.TMDs is to electromagnetic wave
It absorbs based on dielectric loss, therefore, can be mixed by the carbonyl iron dust absorbent with magnetic loss type, material is made to have both electric damage
Consumption and magnetic loss characteristic, can not only improve absorptivity of the material to electromagnetic wave, but also can improve impedance matching, make more in this way
Number electromagnetic wave can enter the inside of absorbing material.In addition, TMDs is non-conductive, its carbonyl iron dust with high conductivity is compound,
Conducting particles can be made effectively to disperse, so as to avoid Kelvin effect to the adverse effect of magnetic conductivity, ensure that carbonyl iron dust magnetic
The normal performance of loss ability.It is this to be designed with to obtain a kind of new and effective microwave absorption.
Compared with prior art, the advantage of the invention is that：
1st, composite microwave absorbent of the invention is when matching thickness is 2mm, to the electromagnetic wave of 2~18GHz frequency ranges
Maximum absorption rate reaches -46.68dB, and the effective bandwidth that attenuation reaches -10dB reaches 7.6GHz.The material can be used as simulation and stealthy
And the protection occasion of some electromagnetic radiation such as mobile phone, household electrical appliance.
2nd, preparation method of the invention is removed to obtain thin slice to transition metal chalcogenide coarse powder progress liquid phase ultrasound first,
The dielectric loss of powder is improved, then it with this magnetic loss type absorbent of carbonyl iron dust is mixed, material is made to have both electric damage
Consumption and magnetic loss characteristic, can not only improve absorptivity of the material to electromagnetic wave, but also can improve impedance matching, make more in this way
Number electromagnetic wave can enter the inside of absorbing material.In addition, TMDs is non-conductive, its carbonyl iron dust with high conductivity is compound,
Conducting particles can be made effectively to disperse, so as to avoid Kelvin effect to the adverse effect of magnetic conductivity, ensure that carbonyl iron dust magnetic
The normal performance of loss ability.Test result handles more than showing and can improve microwave absorption peak really, widens microwave absorption
Frequency band, and substantially reduce matching thickness meets the target of " thin, light, wide, strong " required by absorbing material, is a kind of
Ideal high performance microwave absorbent.
3rd, preparation method of the invention is simple and practicable, and production cost is relatively low, is suitble to the industrialized production of certain scale.
Description of the drawings
Fig. 1 is MoS prepared by the embodiment of the present invention 12Remove the XRD spectrum of product.
Fig. 2 is MoS prepared by the embodiment of the present invention 12Remove 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
It limits the scope of the invention.
Material and instrument employed in following embodiment are commercially available.
Embodiment 1：
A kind of transition metal chalcogenide-carbonyl iron dust composite microwave absorbent, the composite microwave absorbent is mainly by mistake
It crosses metal chalcogenide thin slice to form with carbonyl iron dust, the chemical formula of transition metal chalcogenide is AB2, wherein, A Mo, B are
S, i.e. MoS2.The microscopic appearance of transition metal chalcogenide is laminar, 04 μm of ＜ sheet transverse direction grain sizes ＜.
A kind of preparation method of the transition metal chalcogenide of above-mentioned the present embodiment-carbonyl iron dust composite microwave absorbent,
Include the following steps：
（1）0.1g MoS are weighed with assay balance2Coarse powder, with 50.0mL organic solvent n-methyl-2-pyrrolidone（NMP）
Mixing, is placed in beaker, is made into the mixed liquor of a concentration of 2g/L, is then sealed beaker with preservative film and rubber band, be placed in perseverance
In warm ultrasonic cleaning machine, intermittently ultrasound 5h, 1 time, each 30min ultrasonic every 10min, obtains stripping product colloidal sol；
（2）Stripping product colloidal sol is transferred to centrifuge tube, 15min is centrifuged with 12000rpm speed, it will be upper with rubber head dropper
Layer clear liquid carefully removes, and obtains sediment；Sediment is cleaned with absolute ethyl alcohol, 15min is centrifuged with 12000rpm speed,
Retain precipitation, repeat above-mentioned cleaning-centrifugally operated to sediment 3 times, obtain removing the sediment of organic solvent substantially；
（3）The sediment of basic removal organic solvent is put into vacuum drying chamber, is dried at 80 DEG C, drying time is
8h obtains dry MoS2Remove product, i.e. MoS2Thin slice.As shown in Figure 1, use X-ray diffractometer（Bruker, D8
Advance）Test removes the crystal structure of product and with being compared before stripping, the results showed that：MoS2For hexagonal crystal system（PDF
No. 37-1492）.Wherein, 14.39 °, 29.02 °, 33.51 °, 44.15 °, 60.14 ° of characteristic diffraction peak corresponds respectively to
MoS2's（002）、（004）、（101）、（006）With（008）Crystal face.（002）Diffraction maximum is MoS2Stratiform accumulates the important finger of degree
Mark.Peak value is stronger, then illustrates that the accumulation number of plies is more；Peak value is weaker, shows that the stratiform accumulation number of plies is fewer.After supersound process, powder
In（002）Peak with（101）Signal weaken than apparent, it is meant that successfully realize stripping.As shown in Fig. 2, scan electricity with Flied emission
Sub- microscope（3 SBH of TESCAN, VEGA）Powder morphology is observed, as a result shows stripping product as flaky texture, lateral grain size
In micron dimension.
（4）By step（3）Obtained MoS2Thin slice is uniformly mixed with carbonyl iron dust in mass ratio 1: 3 to get to required production
Product transition metal chalcogenide-carbonyl iron dust composite microwave absorbent.By composite microwave absorbent and melt paraffin in mass ratio 4
: 1 is uniformly mixed, and is pressed into internal diameter in a mold as 3mm, outer diameter 7mm, thickness is in the coaxial rings sample of 2.5mm.Using waveguide
Method utilizes 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 is substantially reduced compared with two kinds of single group member absorbents, reflection
Effective bandwidth of the loss more than -10dB is then significantly widened, respectively 2mm and 5.68GHz（9.36~15.04GHz ranges it
Difference）, maximum reflection loss be apparently higher than carbonyl iron dust absorbent, reach -32.31dB, peak value is located at 11.92GHz.With it is compound
The microwave absorption property of first two single group member absorbent is compared, between MoS2Absorption peak（6.88GHz）It is 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 mainly by mistake
It crosses metal chalcogenide thin slice to form with carbonyl iron dust, the chemical formula of transition metal chalcogenide is AB2, wherein, A Mo, B are
S, i.e. MoS2.The microscopic appearance of transition metal chalcogenide is laminar, 04 μm of ＜ sheet transverse direction grain sizes ＜.
A kind of preparation method of the transition metal chalcogenide of above-mentioned the present embodiment-carbonyl iron dust composite microwave absorbent,
Include the following steps：
（1）0.1g MoS are weighed with assay balance2Coarse powder, with 50.0mL organic solvent n-methyl-2-pyrrolidone（NMP）
Mixing, is placed in beaker, is made into the mixed liquor of a concentration of 2g/L, is then sealed beaker with preservative film and rubber band, be placed in perseverance
In warm ultrasonic cleaning machine, intermittently ultrasound 5h, 1 time, each 30min ultrasonic every 10min, obtains stripping product colloidal sol；
（2）Stripping product colloidal sol is transferred to centrifuge tube, 15min is centrifuged with 12000rpm speed, it will be upper with rubber head dropper
Layer clear liquid carefully removes, and obtains sediment；Sediment is cleaned with absolute ethyl alcohol, 15min is centrifuged with 12000rpm speed,
Retain precipitation, repeat above-mentioned cleaning-centrifugally operated to sediment 3 times, obtain removing the sediment of organic solvent substantially；
（3）The sediment of basic removal organic solvent is put into vacuum drying chamber, is dried at 80 DEG C, drying time 8h,
Obtain dry MoS2Thin slice；
（4）By MoS2Thin slice is uniformly mixed with carbonyl iron dust in mass ratio 1: 4 to get required product transition metal sulfur family
Object-carbonyl iron dust composite microwave absorbent.Composite microwave absorbent is uniformly mixed with melt paraffin in mass ratio 4: 1, in mould
Internal diameter is pressed into tool as 3mm, outer diameter 7mm, thickness is in the coaxial rings sample of 3mm.As shown in figure 4, it is detected using waveguide method
The product reaches -46.68dB when matching thickness is 2mm, to the electromagnetic wave maximum reflection loss of 2~18GHz frequency ranges,
Reflection 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 mainly by mistake
It crosses metal chalcogenide thin slice to form with carbonyl iron dust, the chemical formula of transition metal chalcogenide is AB2, wherein, A Mo, B are
Se, i.e. MoSe2.The microscopic appearance of transition metal chalcogenide is laminar, 0 10 μm of ＜ sheet transverse direction grain sizes ＜.
A kind of preparation method of the transition metal chalcogenide of above-mentioned the present embodiment-carbonyl iron dust composite microwave absorbent,
Include the following steps：
（1）0.1g MoSe are weighed with assay balance2Coarse powder, with 50.0mL organic solvent n-methyl-2-pyrrolidone
（NMP）Mixing, is placed in beaker, is made into the mixed liquor of a concentration of 2g/L, is then sealed beaker with preservative film and rubber band, put
In thermostatic ultrasonic washer, intermittently ultrasound 3h, 1 time, each 30min ultrasonic every 10min, obtains stripping product colloidal sol；
（2）Stripping product colloidal sol is transferred to centrifuge tube, 15min is centrifuged with 12000rpm speed, it will be upper with rubber head dropper
Layer clear liquid carefully removes, and obtains sediment；Sediment is cleaned with absolute ethyl alcohol, 15min is centrifuged with 12000rpm speed,
Retain precipitation, repeat above-mentioned cleaning-centrifugally operated to sediment 3 times, obtain removing the sediment of organic solvent substantially；
（3）The sediment of basic removal organic solvent is put into vacuum drying chamber, is dried at 80 DEG C, drying time 8h,
Obtain dry MoSe2Thin slice；
（4）By the MoSe2Thin slice is uniformly mixed with carbonyl iron dust in mass ratio 1: 3 to get required product Transition Metal Sulfur
Race's compound-carbonyl iron dust composite microwave absorbent.Composite microwave absorbent is uniformly mixed with melt paraffin in mass ratio 4: 1,
It is pressed into internal diameter in a mold as 3mm, outer diameter 7mm, thickness is in the coaxial rings sample of 2.7mm.As shown in figure 5, waveguide method is examined
The product is surveyed when matching thickness is 2mm, the electromagnetic wave maximum reflection loss of 2~18GHz frequency ranges is reached-
44.55dB, reflection loss reach effective loss bandwidth of -10dB up to 4.88GHz, and 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 mainly by mistake
It crosses metal chalcogenide thin slice to form with carbonyl iron dust, the chemical formula of transition metal chalcogenide is AB2, wherein, A W, B are
Se, i.e. WSe2.The microscopic appearance of transition metal chalcogenide is laminar, 0 ＜ sheet transverse direction grain sizes ＜ of sheet transverse direction grain size, 10 μ
m。
A kind of preparation method of the transition metal chalcogenide of above-mentioned the present embodiment-carbonyl iron dust composite microwave absorbent,
Include the following steps：
（1）0.1g WSe are weighed with assay balance2Coarse powder mixes with 50.0mL organic solvents NMP, is made into a concentration of 2g/L
Mixed liquor, then beaker is sealed with preservative film and rubber band, is placed in thermostatic ultrasonic washer, interval ultrasound 3h, every
10min ultrasounds 1 time, each 30min obtain stripping product colloidal sol；
（2）Stripping product colloidal sol is transferred to centrifuge tube, 15min is centrifuged with 12000rpm speed, it will be upper with rubber head dropper
Layer clear liquid carefully removes, and obtains sediment；Sediment is cleaned with absolute ethyl alcohol, 15min is centrifuged with 12000rpm speed,
Retain precipitation, repeat above-mentioned cleaning-centrifugally operated to sediment 3 times, obtain removing the sediment of organic solvent substantially；
（3）The sediment of basic removal organic solvent is put into vacuum drying chamber, is dried at 80 DEG C, drying time 8h,
Obtain dry WSe2Thin slice；
（4）By the WSe2Thin slice is uniformly mixed with carbonyl iron dust in mass ratio 1: 3 to get required product transition metal sulfur family
Compound-carbonyl iron dust composite microwave absorbent.Composite microwave absorbent is uniformly mixed with melt paraffin in mass ratio 4: 1,
Internal diameter is pressed into mold as 3mm, outer diameter 7mm, thickness is in the coaxial rings sample of 3.1mm.As shown in fig. 6, waveguide method detects
The product reaches -35.29dB when matching thickness is 2mm, to the electromagnetic wave maximum reflection loss of 2~18GHz frequency ranges,
Reflection loss reaches effective loss bandwidth of -10dB up to 5.52GHz, and 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 mainly by mistake
It crosses metal chalcogenide thin slice to form with barium ferrite, the chemical formula of transition metal chalcogenide is AB2, wherein, A Mo, B are
Se, i.e. MoSe2.The microscopic appearance of transition metal chalcogenide is laminar, 04 μm of ＜ sheet transverse direction grain sizes ＜.
A kind of preparation method of the transition metal chalcogenide of above-mentioned the present embodiment-barium ferrite composite microwave absorbent,
Include the following steps：
（1）MoSe2Stripping and drying means with embodiment 3；
（2）By the MoSe2Thin slice is uniformly mixed with barium ferrite in mass ratio 1: 3 to get required product Transition Metal Sulfur
Race's compound-ferrite composite microwave absorbent.Composite microwave absorbent is uniformly mixed with melt paraffin in mass ratio 4: 1,
Internal diameter is pressed into mold as 3mm, outer diameter 7mm, thickness is in the coaxial rings sample of 2.6mm.Waveguide method detect the product
During with thickness for 5mm, -30.11dB is reached to the electromagnetic wave maximum reflection loss of 2~18GHz frequency ranges, reflection loss reaches
Effective loss bandwidth to -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, includes the following steps：
（1）0.1g MoS are weighed with assay balance2Coarse powder, with 50.0mL organic solvent n-methyl-2-pyrrolidone（NMP）
Mixing, is placed in beaker, is made into the mixed liquor of a concentration of 2g/L, is then sealed beaker with preservative film and rubber band, be placed in perseverance
In warm ultrasonic cleaning machine, intermittently ultrasound 3h, 1 time, each 30min ultrasonic every 10min, obtains stripping product colloidal sol；
（2）Will stripping product colloidal sol be transferred to centrifuge tube, with 6000rpm speed centrifuge 15min, take supernatant be transferred to newly from
Heart pipe, then 15min is centrifuged with 12000rpm speed, supernatant liquor is carefully removed with rubber head dropper, obtains sediment；With anhydrous
Ethyl alcohol cleans sediment, centrifuges 15min with 12000rpm speed, retains precipitation, repeat above-mentioned cleaning to sediment-
Centrifugally operated 3 times obtains removing the sediment of organic solvent substantially；
（3）The sediment of basic removal organic solvent is put into vacuum drying chamber, is dried at 90 DEG C, drying time 9h,
Obtain dry MoSe2Thin slice；
（4）By the MoS2Thin slice is uniformly mixed with carbonyl iron dust in mass ratio 1: 3 to get required product transition metal sulfur family
Compound-carbonyl iron dust composite microwave absorbent.Composite microwave absorbent is uniformly mixed with melt paraffin in mass ratio 4: 1,
Internal diameter is pressed into mold as 3mm, outer diameter 7mm, thickness is in the coaxial rings sample of 2.4mm.Waveguide method detect the product
During with thickness for 2.7mm, -18.03dB, reflection loss are reached to the electromagnetic wave maximum reflection loss of 2~18GHz frequency ranges
Reach effective loss bandwidth of -10dB up to 2.81GHz, absorption peak is located at 15.02GHz.
The above described is only a preferred embodiment of the present invention, not make limitation in any form to the present invention.Though
So the present invention is disclosed as above with preferred embodiment, however is not limited to the present invention.It is any to be familiar with those skilled in the art
Member, in the case where not departing from the Spirit Essence of the present invention and technical solution, all using in the methods and techniques of the disclosure above
Appearance makes technical solution of the present invention many possible changes and modifications or is revised as the equivalent embodiment of equivalent variations.Therefore,
Every content without departing from technical solution of the present invention, technical spirit according to the present invention are made to the above embodiment any simple
Modification, equivalent replacement, equivalence changes and modification, still fall within technical solution of the present invention protection in the range of.
Claims (5)
1. a kind of transition metal chalcogenide-carbonyl iron dust composite microwave absorbent, which is characterized in that the composite microwave absorbs
Agent is mainly made of transition metal chalcogenide thin slice with carbonyl iron dust, and the chemical formula of transition metal chalcogenide is AB2,
In, A Mo, W or Ti, B S, Se or Te；
The mass ratio of the transition metal chalcogenide thin slice and carbonyl iron dust is 1: 0.5~6；Transition metal sulfur family described in 0 ＜
10 μm of the sheet transverse direction grain size ＜ of compound thin slice；
The transition metal chalcogenide thin slice is to be removed by transition metal chalcogenide coarse powder and organic solvent through liquid phase ultrasound
Method is prepared；The mass volume ratio of the transition metal chalcogenide coarse powder and organic solvent is 0.5g~4g: 1L；It is described to have
Solvent is one or more in n-methyl-2-pyrrolidone, N- ethyl-2-pyrrolidones and isopropanol.
2. a kind of preparation method of transition metal chalcogenide-carbonyl iron dust composite microwave absorbent, including by Transition Metal Sulfur
Race's compound coarse powder is mixed with organic solvent, and transition metal chalcogenide thin slice is prepared, then incited somebody to action using liquid phase ultrasound stripping method
It crosses metal chalcogenide thin slice to mix with carbonyl iron dust, obtains transition metal chalcogenide-carbonyl iron dust composite microwave absorbent；
Include the following steps：
（1）Transition metal chalcogenide coarse powder is mixed with organic solvent, it is molten to obtain stripping product after ultrasound for gained mixed liquor
Glue；
（2）Gained stripping product colloidal sol is centrifuged, gained sediment clean and centrifuge repeatedly, obtains removing organic molten
The sediment of agent；
（3）The sediment for removing organic solvent is dried, obtains transition metal chalcogenide thin slice；
（4）Transition metal chalcogenide thin slice with carbonyl iron dust is uniformly mixed, obtains transition metal chalcogenide-carbonyl iron dust
Composite microwave absorbent；
The step（1）In, the chemical formula of transition metal chalcogenide is AB2, wherein, A Mo, W or Ti, B S, Se or Te；
And/or the mass volume ratio of the transition metal chalcogenide coarse powder and organic solvent is 0.5g~4g: 1L；It is and/or described
Organic solvent is one or more in n-methyl-2-pyrrolidone, N- ethyl-2-pyrrolidones and isopropanol；
The step（4）In, the mass ratio 1: 0.5~6 of the transition metal chalcogenide thin slice and carbonyl iron dust.
3. the preparation method of transition metal chalcogenide according to claim 2-carbonyl iron dust composite microwave absorbent,
It is characterized in that, the step（1）In, the ultrasound is interval ultrasound, 1 time ultrasonic every 10min~20min, each 20min~
40min, the total time of the ultrasound is 1h~11h.
4. the preparation method of transition metal chalcogenide according to claim 2-carbonyl iron dust composite microwave absorbent,
It is characterized in that, the step（2）In, it is described stripping 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 washed and centrifuged is 3~5 times.
5. the preparation method of transition metal chalcogenide according to claim 2-carbonyl iron dust composite microwave absorbent,
It is characterized in that, the step（3）In, the condition of the drying is vacuum condition, and the temperature of the drying is 80 DEG C~90 DEG C, institute
The dry time is stated as 2h~10h.
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