CN109121375B - Fill the dielectric material composite microwave absorbing body and preparation method of magnetic metal - Google Patents
Fill the dielectric material composite microwave absorbing body and preparation method of magnetic metal Download PDFInfo
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- CN109121375B CN109121375B CN201810810948.1A CN201810810948A CN109121375B CN 109121375 B CN109121375 B CN 109121375B CN 201810810948 A CN201810810948 A CN 201810810948A CN 109121375 B CN109121375 B CN 109121375B
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- H—ELECTRICITY
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- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
- H05K9/0088—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising a plurality of shielding layers; combining different shielding material structure
Abstract
The invention belongs to field of microwave absorption, disclose the dielectric material composite microwave absorbing body and preparation method of filling magnetic metal.Absorber fills metal nanoparticle using semiconductor material as the dielectric material of cladded type structural outer.Semiconductor material is one of multi-walled carbon nanotube, zinc oxide, graphene, silicon carbide；Metal nanoparticle is one of Fe, Co, Ni or several alloys.Magnetic metal nano particle is completely filled in the inside of semiconductor by the present invention, dielectric material having an open structure is prepared first, it is transferred in the solution with magnetic metal, the mode of the warm-up movement of power and molecule, ion is filled in the inside of semiconductor material through capillary action.Composite microwave absorbing body prepared by the present invention,, absorbing property easy with preparation method it is excellent and can by adjusting different magnetic metal and metal alloy ratio to the response performance of external microwave field, and then obtain efficiently, the good microwave-absorbing body of lightweight, stability.
Description
Technical field
The invention belongs to field of microwave absorption, are related to a kind of dielectric material composite microwave absorbing body for filling magnetic metal
And preparation method.
Background technique
Nearly ten years, along with the raising of scientific and technological level and the development of human society, high band electronic equipment is obtained
The use of a large amount of application, a large amount of electronic equipments generates a large amount of electromagnetic wave, causes Contamination of Electromagnetic Wave, has seriously affected people's
Health and normal communication.The high-frequency electromagnetic pulse that electronic equipment issues makes space be full of different wave length and frequency
Electromagnetic wave.Existing correlative study shows the electromagnetic field of this distribution in an atmosphere if it exceeds some strength will become one kind
New environmental pollution --- electromagenetic wave radiation pollution.On the other hand, since the working frequency of electronic component is higher and higher, and it is electric
The also higher and higher while current electronic component integrated level of sub- component sensitivity is higher and higher, from each other mutual
It influences that these complicated electromagnetic waves will certainly also be made to become the protrusion obstacle that related High performance electronics operate normally.
Therefore, it has very important significance in high frequency band to the research of electromagnetic wave absorbent material.It is ideal to inhale wave material
Material should have the characteristics that absorb that strong, bandwidth, thickness is thin and light weight, the exploration and fast development of nano material, Performances of Novel Nano-Porous
Rice absorbing material preferably meets these requirements, and therefore, preparing novel nano absorbing material becomes current research hotspot.From
From the point of view of the state of development of current absorbing material, single absorbing material is difficult to meet effective absorption to electromagnetic wave, is difficult full
The composite request of foot " wide, strong, light ", it is therefore desirable to carry out a variety of absorbing materials compound to obtain best electro-magnetic wave absorption effect
Fruit.For example, disclosing a kind of Fe-Co alloy/C/C composite nano fiber microwave absorption, preparation side in patent 2013103371935
Method and application, and patent 2013103383171 disclose a kind of Co/C composite nano fiber microwave absorption preparation method and its
Using.
The preparation method of traditional radio-radar absorber is more complicated, and reaction condition is relatively harsh, and operating process is relatively numerous
It is trivial, it is difficult to carry out large-scale industrial production, therefore its there is also many problems in actual application.In addition, ferromagnetic material
Material is assembled in the composite material that the inside of dielectric material is formed, and electromagnetic parameter and impedance matching are linkages, that is, changes internal
Or arbitrary portion externally within, the real and imaginary parts of complex dielectric permittivity, the real and imaginary parts of complex permeability all change together.This
All the coverage area of wave-absorber and absorption intensity are had an impact a bit.
Summary of the invention
The present invention provides a kind of magnetic metal and is completely filled in dielectric material to overcome problems of the prior art
Composite microwave absorbing body and preparation method thereof inside material, wherein being made by chemical method with semiconductor for basic dielectric material
Defect and duct are formed, and the mode of the warm-up movement of power and molecule, ion is filled in semiconductor material through capillary action
Inside forms a kind of composite electromagnetic absorber.Meanwhile passing through Jie of the ingredient and content and outside that improve magnetic material
The regulation of absorbing property may be implemented in electric material.
Technical scheme is as follows:
A kind of dielectric material composite microwave absorbing body for filling magnetic metal, the absorber is using semiconductor material as packet
Cover the dielectric material of type structural outer, inside filling metal nanoparticle；Wherein, the metal nanoparticle is in Fe, Co, Ni
One or several kinds of alloys；The partial size of metal nanoparticle is 1~30nm.Composite microwave absorbing body is micro- with what be can be changed
Wave response characteristic.Metal nanoparticle soilless sticking phenomenon in occupied state generates.
Further, the semiconductor material be one of multi-walled carbon nanotube, zinc oxide, graphene, silicon carbide or
It is a variety of.
The present invention also provides a kind of preparation methods for realizing above-mentioned absorber: the following steps are included:
Step 1: the semiconductor material as dielectric material is placed in the concentrated nitric acid of 68wt.%, and 140 DEG C of oil bath heating,
8~14h, then be washed with deionized to neutrality, dry 12 are transferred in 60~80 DEG C of baking ovens~for 24 hours；
Step 2: the processed dielectric material of step 1 and deionized water are mixed with mass ratio 1:20, at ultrasound
5~15min is managed, solvent is formed；
Step 3: 1~2M magnetic metal ion solution corresponding with the metal nanoparticle to be filled is added to
In the solvent that step 2 is equipped with, ultrasound simultaneously stirs 1h or more, forms mixed solution, utilizes the suction-operated pair of dielectric material itself
Mixed solution is adsorbed；
Step 4: the mixed solution of step 3 is filtered, then is washed with deionized once, and the amount of the deionized water is
Corresponding 50~100 ml deionized waters of every 1mol magnetic metal ion；It is then transferred to 60~80 DEG C of drying box, it is 24 hours dry
More than；
Step 5: mixture is placed in 140~170 DEG C of heating 8h or more, then under protection of argon gas, with 5~8 DEG C/min
Rate is heated to 350~400 DEG C of 3~4h of heat preservation.
The beneficial effects of the present invention are: the present invention provides a kind of magnetic metals to be completely filled in answering inside dielectric material
Mould assembly microwave-absorbing body and preparation method thereof, can make up for it traditional electromagnetic wave absorbent material can only generate response in special frequency channel
Disadvantage.Meanwhile the electromagnetic wave absorbent material has that coverage area is wide, response characteristic is obvious, simple process, at low cost, process can
The advantages that control.
Detailed description of the invention
Fig. 1 is the schematic diagram of composite wave absorption material structure in the method for the present invention；
Fig. 2 is composite wave absorption material preparation method flow chart in the method for the present invention；
Fig. 3 is transmission electron microscope picture corresponding to composite wave absorption material in the method for the present invention；(a) chemical Treatment after-opening
Carbon nanotube appearance figure, (b) embodiment 1 fills the carbon nanotube shape appearance figure of magnetic metal, and (c) embodiment 2 fills magnetic metal
Carbon nanotube shape appearance figure, (d) embodiment 3 fill magnetic metal carbon nanotube shape appearance figure；
Fig. 4 is electromagnetic parameter response diagram (dielectric constant) corresponding to composite wave absorption material in the method for the present invention；
Fig. 5 is electromagnetic parameter response diagram (magnetic conductivity) corresponding to composite wave absorption material in the method for the present invention.
In figure: 101 dielectric materials；102 magnetic metal nano particles.
Specific embodiment
To be more clear the objectives, technical solutions, and advantages of the present invention, below in conjunction with drawings and concrete examples to this hair
Bright operating process is described in further detail.Need to illustrate, specific example described herein for explaining only the invention, wherein
It is illustrated as illustrative nature, is not intended to limit the scope of the present invention.
Fig. 1 is the schematic diagram of composite wave absorption material structure in the method for the present invention.As shown in Figure 1, absorber includes: partly to lead
Body base dielectric material 101 selects multi-walled carbon nanotube in this embodiment；Magnetic metal nano wave-absorbing material 102, in this embodiment
Select simple substance iron nano-particle.
Dielectric material 101 based on the semiconductor material is generally the dielectric of multi-walled carbon nanotube or equivalent constructions
Material.
The magnetic metal nano particle 102 is generally one of Fe, Co, Ni or several alloys.
Further, chemical method preparation can be used in the dielectric material 101 based on semiconductor material described in this example, has
Certain density nitric acid handles the regular hour under heating conditions, and the dielectric material of acquisition has certain defect or hole
Road.
Embodiment 1
The present invention provides above-described embodiment preparation method:
Fig. 2 show the flow chart of composite microwave absorbing preparation, illustrates to prepare below with reference to Fig. 3 (a) (b)
Process:
Step B101 prepares the semiconductor material of hatch frame.
As shown in Fig. 3 (a), according to preparation flow, the semiconductor material for the hatch frame that chemical Treatment obtains is used.In
In the present embodiment, the Fe magnetic metal particle internal as it is chosen, carbon nanotube is as external dielectric material, by carbon nanometer
Pipe is placed in the concentrated nitric acid of 68wt.%, 140 DEG C of oil bath heating, 14 hours, the material of processing is adopted and is washed with deionized into
Property, it is transferred in 60 DEG C of baking ovens 24 hours dry.
Step B102 is equipped with magnetic metal solution.The nitric acid iron powder for weighing certain mass, is dissolved in deionized water, matches
The iron nitrate solution of standby 1M.
Magnetic metal solution is absorbed into inside semiconductor material by step B103 as shown in Fig. 3 (b).
(1) dielectric material of preparation 101 and deionized water are mixed with mass ratio 1:20, using ultrasonic treatment 5 minutes, shape
At solvent；
(2) the 1M solution for containing magnetic metal ion is added in the solvent matched and got ready, ultrasound simultaneously mechanical stirring 1 hour
More than, mixed solution is formed, mixed solution is adsorbed using the suction-operated of dielectric material itself；
(3) mixed solution is filtered, is washed once using 50 ml deionized waters, be transferred to 60 DEG C of drying box, it is dry
24 hours.
Step B104, washing, annealing composite material.Mixture is placed in 140 degrees Centigrade 8 hours, then in argon gas
Under protection, 350 degrees Celsius are heated to 5 DEG C/min rate and keeps the temperature 3 hours.
Embodiment 2
Illustrate preparation process below with reference to Fig. 3 (c):
Step B101 prepares the semiconductor material of hatch frame.
According to preparation flow, the semiconductor material for the hatch frame that chemical Treatment obtains is used.In the present embodiment, it selects
The magnetic metal particle that Fe is internal as it is taken, carbon nanotube is placed in 68wt.% as external dielectric material by carbon nanotube
Concentrated nitric acid in, 140 DEG C of oil bath heating, 8 hour, the material of processing is adopted and is washed with deionized to neutrality, be transferred to 60 DEG C
It is 24 hours dry in baking oven.
Step B102 is equipped with magnetic metal solution.The nitric acid iron powder for weighing certain mass, is dissolved in deionized water, matches
The iron nitrate solution of standby 1M.
Magnetic metal solution is absorbed into inside semiconductor material by step B103 as shown in Fig. 3 (c).
(1) dielectric material of preparation 101 and deionized water are mixed with mass ratio 1:20, using ultrasonic treatment 5 minutes, shape
At solvent；
(2) the 1M solution for containing magnetic metal ion is added in the solvent matched and got ready, ultrasound simultaneously mechanical stirring 1 hour
More than, mixed solution is formed, mixed solution is adsorbed using the suction-operated of dielectric material itself；
(3) mixed solution is filtered, is washed once using 100 ml deionized waters, be transferred to 60 DEG C of drying box, it is dry
24 hours.
Step B104, washing, annealing composite material.Mixture is placed in 140 degrees Centigrade 8 hours, then in argon gas
Under protection, 350 degrees Celsius are heated to 5 DEG C/min rate and keeps the temperature 3 hours.
Embodiment 3
Illustrate preparation process below with reference to Fig. 3 (d):
Step B101 prepares the semiconductor material of hatch frame.
According to preparation flow, the semiconductor material for the hatch frame that chemical Treatment obtains is used.In the present embodiment, it selects
The magnetic metal particle that Fe is internal as it is taken, carbon nanotube is placed in 68wt.% as external dielectric material by carbon nanotube
Concentrated nitric acid in, 140 DEG C of oil bath heating, 14 hour, the material of processing is adopted and is washed with deionized to neutrality, be transferred to 60 DEG C
It is 24 hours dry in baking oven.
Step B102 is equipped with magnetic metal solution.The nitric acid iron powder for weighing certain mass, is dissolved in deionized water, matches
The iron nitrate solution of standby 2M.
Magnetic metal solution is absorbed into inside semiconductor material by step B103 as shown in Fig. 3 (d).
(1) dielectric material of preparation 101 and deionized water are mixed with mass ratio 1:20, using ultrasonic treatment 5 minutes, shape
At solvent；
(2) the 1M solution for containing magnetic metal ion is added in the solvent matched and got ready, ultrasound simultaneously mechanical stirring 1 hour
More than, mixed solution is formed, mixed solution is adsorbed using the suction-operated of dielectric material itself；
(3) mixed solution is filtered, is washed once using 50 ml deionized waters, be transferred to 60 DEG C of drying box, it is dry
48 hours.
Step B104, washing, annealing composite material.Mixture is placed in 140 degrees Centigrade 8 hours, then in argon gas
Under protection, 400 degrees Celsius are heated to 8 DEG C/min rate and keeps the temperature 4 hours.
Fig. 4 and Fig. 5 tests electromagnetic response absorption characteristic by the embodiment of the present invention on vector network analyzer.
As shown in figure 4, compound microwave absorption material changes the dielectric constant of electromagnetic wave as frequency changes.As shown in figure 5,
Compound microwave absorption material changes the magnetic conductivity of electromagnetic wave as frequency changes.Fig. 4 and Fig. 5 shows compound suction wave
Material has very strong response in high frequency band to electromagnetic wave, and the present embodiment composite microwave absorbing body has and existing microwave
The similar wave-sucking performance of absorber.
Above-mentioned embodiment is only used to illustrate and not limit the technical solutions of the present invention, it is any do not depart from spirit of that invention and
The technical solution of range should all cover in patent claim of the invention.
Claims (2)
1. filling the dielectric material composite microwave absorbing body of magnetic metal, which is characterized in that the absorber is with semiconductor material
As the dielectric material of cladded type structural outer, inside filling metal nanoparticle；Wherein, the metal nanoparticle be Fe,
One of Co, Ni or several alloys；The partial size of metal nanoparticle is 1~30nm；Jie of the filling magnetic metal
The preparation method of electric material composite microwave absorbing body, comprising the following steps:
Step 1: the semiconductor material as dielectric material is placed in the concentrated nitric acid of 68wt.%, and 140 DEG C of oil bath heating, 8~
14h, then be washed with deionized to neutrality, dry 12 are transferred in 60~80 DEG C of baking ovens~for 24 hours；
Step 2: the processed dielectric material of step 1 and deionized water are mixed with mass ratio 1:20, using ultrasonic treatment 5~
15min forms solvent；
Step 3: 1~2M magnetic metal ion solution corresponding with the metal nanoparticle to be filled is added to step
In two solvents being equipped with, ultrasound simultaneously stirs 1h or more, mixed solution is formed, using the suction-operated of dielectric material itself to mixing
Solution is adsorbed；
Step 4: the mixed solution of step 3 is filtered, then is washed with deionized once, and the amount of the deionized water is every
1mol magnetic metal ion corresponds to 50~100 ml deionized waters；Be then transferred to 60~80 DEG C of drying box, dry 24 hours with
On；
Step 5: mixture is placed in 140~170 DEG C of heating 8h or more, then under protection of argon gas, with 5~8 DEG C/min rate
It is heated to 350~400 DEG C of 3~4h of heat preservation.
2. microwave-absorbing body according to claim 1, which is characterized in that the semiconductor material is multi-wall carbon nano-tube
One of pipe, zinc oxide, graphene, silicon carbide are a variety of.
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| CN102044319A (en) * | 2009-10-23 | 2011-05-04 | 中国科学院物理研究所 | Composite wave absorbing material and preparation method thereof |
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