CN109294520A - A kind of preparation method of the micro-nano composite wave-suction material of BN/C based on urea - Google Patents
A kind of preparation method of the micro-nano composite wave-suction material of BN/C based on urea Download PDFInfo
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- CN109294520A CN109294520A CN201811426987.8A CN201811426987A CN109294520A CN 109294520 A CN109294520 A CN 109294520A CN 201811426987 A CN201811426987 A CN 201811426987A CN 109294520 A CN109294520 A CN 109294520A
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Abstract
The present invention proposes a kind of preparation method of micro-nano composite wave-suction material of the BN/C based on urea, comprising the following steps: mixed liquor is made as solvent with deionized water in step 1, by dry boric acid, urea, GNFs/CNTs and dispersant；The molar content of boric acid is 20% ~ 30%, and the molar content that the molar content of urea is 40% ~ 60%, GNFs/CNTs is 10% ~ 40%, and the molar ratio of boric acid and urea is 1:2；Step 2, by above-mentioned mixed liquor, heating stirring 4h ~ 6h, heating temperature are 90 DEG C ~ 100 DEG C in magnetic stirring apparatus, then put 55 DEG C ~ 65 DEG C of drying box into and are evaporated, obtain dry presoma；Step 3, taking-up presoma carry out grinding obtained powder；Above-mentioned powder is placed in crucible by step 4; it is sintered under protective gas using tube furnace; when sintering temperature is 1200 DEG C ~ 1400 DEG C, temperature 2.5h ~ 3.5h is kept under protective gas, and taking out after cooling can be obtained the micro-nano composite wave-suction material of BN/C.There is good absorbing property by the micro-nano composite wave-suction material of BN/C prepared by the above method.
Description
Technical field
The present invention relates to composite wave-suction material field more particularly to a kind of micro-nano composite wave-absorbing materials of BN/C based on urea
The preparation method of material.
Background technique
With the application scenarios of electromagnetic wave and widening for field, the development and use of electromagnetic wave absorbent material receive therewith
Universal concern.Preparing, there is the microwave absorbing material of " thin, light, wide, strong " characteristic to not only contribute to reduce electromagnetic wave for day
The harm of crowd in often living, it is often more important that the stealthy spy of weaponry can be enhanced as a kind of special military defense material
Property.
Carbon material is considered as a kind of good microwave absorbing material due to its lower density and preferable electric conductivity.But
It is that simple carbon absorbing material forms biggish electrical loss often through stronger polarization and impedance matching property is caused to lose
Weighing apparatus, so that reflection of electromagnetic wave ratio increases.How impedance matching is adjusted to make full use of carbon material height loss decaying electromagnetic wave
As one of domestic and foreign scholars' research hotspot.
Summary of the invention
In order to solve the problems in the existing technology, the invention proposes a kind of BN/C based on urea is micro-nano compound
The preparation method of absorbing material makes the micro-nano composite wave-absorbing material of BN/C of preparation to adjust the impedance matching property of carbon material
Material has good absorbing property.
To achieve the goals above, the invention proposes a kind of systems of micro-nano composite wave-suction material of the BN/C based on urea
Preparation Method, comprising the following steps:
Step 1, mixing: by dried boric acid, urea, GNFs and dispersant, it is mixed to make solvent with deionized water
Mixed liquor is made in conjunction；Or by dried boric acid, urea, CNTs and dispersant, make solvent mixing with deionized water
Mixed liquor is made, wherein the molar content of boric acid is 20%~30%, the molar content of urea is 40%~
The molar content of 60%, GNFs or CNTs are 10%~40%, and the molar ratio of boric acid and urea is always 1:2；
It is step 2, dry: by the mixed liquor in step 1 in magnetic stirring apparatus heating stirring 4h~6h, wherein heating temperature
90 DEG C~100 DEG C are set as, 55 DEG C~65 DEG C of drying box is put into again later and is evaporated, to obtain dry presoma；
Step 3, grinding: it takes out the resulting presoma of step 2 and is ground, powder is made；
Step 4, sintering and feeding: step 3 gained powder is placed in crucible, utilizes tube furnace under protective gas
It is sintered, when sintering temperature is 1200 DEG C~1400 DEG C, keeps temperature 2.5h~3.5h under protective gas, that is, protect
The warm time is 2.5h~3.5h, takes out after cooling, the micro-nano composite wave-suction material of BN/C can be obtained.
Preferably, the dispersing agent uses SDS.
Preferably, mixed liquor manufactured in step 1 is put into ultrasonic cleaning instrument ultrasound 20min~40min.
Preferably, in the step 4, precursor powder is placed on graphite paper, is put into crucible again later,
It is sintered under nitrogen environment using high temperature process furnances, sintering temperature is 1400 DEG C, soaking time 3h.
The beneficial effect of the program of the present invention is through the above-mentioned micro-nano composite wave-suction material of the BN/C based on urea
Preparation method can successfully synthesize the micro-nano composite wave-suction material of BN/C, and the above method have it is easy it is stable, easy to operate,
The advantages that low for equipment requirements, and the absorbing material prepared also has good absorbing property, can be used as widely used suction
Wave material come using.The micro-nano composite wave-suction material of BN/C has reached a degree of flat between impedance matching and attenuation characteristic
Weighing apparatus, it was demonstrated that this electromagnetic wave transparent material of BN is mixed into the absorbing property for being conducive to improve material, furthermore the micro-nano composite wave-absorbing material of BN/C
The microwave absorbing property of material illustrate the material can be used as good medium-high frequency absorbing material come using.
Detailed description of the invention
Fig. 1 to Fig. 5 is the diagram of the micro-nano composite wave-suction material of BN/C of BN/GNFs composite system preparation, and Fig. 6 is extremely
Figure 10 is the diagram of the micro-nano composite wave-suction material of BN/C of BN/CNTs composite system preparation.
Fig. 1 is the XRD spectrum of the micro-nano composite wave-suction material of BN/C, wherein ratio indicate boric acid, urea and GNFs it
Between ratio.
Fig. 2 shows the scanning electron microscope maps of the micro-nano composite wave-suction material of BN/C, wherein (a) and (b) is pure GNFs
Low power and high power figure, (c) and (d) be 1GNFs/BN composite material low power and high power figure.
Fig. 3 shows the transmission electron microscope map of the micro-nano composite wave-suction material of BN/C, wherein (a) is low power figure, it is (b) choosing
Area's electron diffraction pattern figure, is (c) high power figure, is (d) flaky substance HRTEM figure (illustration is interplanar distance).
Fig. 4 is the elemental analysis EDX map of the micro-nano composite wave-suction material of BN/C, wherein (a) is transmission electron microscope picture, (b)
It is C element distribution map, is (c) N element distribution map, is (d) O distribution diagram of element.
Fig. 5 is the suction wave of 2GNFs/BN composite material of the micro-nano composite wave-suction material thickness of BN/C between 3-3.5mm
The relational graph of performance and frequency.
Fig. 6 shows the micro-nano composite wave-suction material powder of BN/C and sintered pure boron nitride, pure carbon nanometer after sintering
The XRD diagram of pipe.
Fig. 7 shows the scanning electron microscope map of the micro-nano composite wave-suction material of BN/C, wherein (a) and (b) is pure carbon nanometer
The low power and high power figure of pipe are (c) low power and high power figure of 1CNTs/BN composite wave-suction material with (d).
Fig. 8 shows the transmission electron microscope picture of the micro-nano composite wave-suction material of BN/C, wherein (a) is low power figure, it is (b) high power
Figure is (c) flaky substance HRTEM figure (illustration is interplanar distance), is (d) selective electron diffraction style figure.
Fig. 9 is the transmission electron microscope and corresponding elemental analysis EDX map of the micro-nano composite wave-suction material of BN/C, wherein (a)
It is transmission electron microscope picture, is (b) N element distribution map, be (c) O distribution diagram of element, is (d) C element distribution map.
Figure 10 is reflection loss figure of the micro-nano composite wave-suction material of BN/C in different-thickness.
Specific embodiment
A specific embodiment of the invention is further described with reference to the accompanying drawing.
The preparation method of the micro-nano composite wave-suction material of BN/C according to the present invention based on urea the following steps are included:
Step 1, mixing: by dried boric acid, urea, GNFs (graphene microchip) and dispersant, spend from
Sub- water as solvent is mixed and made into mixed liquor；Or it is dried boric acid, urea, CNTs (carbon nanotube) and dispersing agent is mixed
It closes, is mixed and made into mixed liquor as solvent with deionized water, wherein the molar content of boric acid is 20%~30%, urea
The molar content that molar content is 40%~60%, GNFs or CNTs is 10%~40%, and boric acid and urine
The molar ratio of element is always 1:2.
Since perhaps CNTs and deionized water solvent immiscible GNFs or CNTs can float on aqueous solvent surface to GNFs, it is
The product made uniformly mixes, therefore dispersing agent can just be added, and in the present embodiment, SDS can be used in the dispersing agent.
To keep GNFs or CNTs evenly dispersed in a solvent, mixed liquor manufactured in step 1 can be put into ultrasonic cleaning
Instrument ultrasound 20min~40min.
It is step 2, dry: by the mixed liquor in step 1 in magnetic stirring apparatus heating stirring 4h~6h, wherein heating temperature
Be set as 90 DEG C~100 DEG C, be with 95 DEG C it is best, put 55 DEG C~65 DEG C of drying box into again later and be evaporated, preferably 60 DEG C, with
To dry presoma.
Step 3, grinding: it takes out the resulting presoma of step 2 and is ground, powder is made.
Step 4, sintering and feeding: step 3 gained powder is placed in crucible, utilizes tube furnace under protective gas
It is sintered, when sintering temperature is 1200 DEG C~1400 DEG C, keeps temperature 2.5h~3.5h under protective gas, that is, protect
The warm time is 2.5h~3.5h, takes out after cooling, the micro-nano composite wave-suction material of BN/C can be obtained.
In the step 4, precursor powder can be placed on graphite paper, be put into crucible again later, in nitrogen ring
Be sintered under border using high temperature process furnances, sintering temperature with 1400 DEG C be it is best, soaking time is best with 3h.
The preparation method of the micro-nano composite wave-suction material of BN/C based on urea involved in through the invention is obtained
The micro-nano composite wave-suction material of BN/GNFs, pattern are that the BN (boron nitride) of fractionlet shape is more evenly distributed in graphene
Nanometer sheet surface, the micro-nano composite wave-suction material of BN/GNFs is when with a thickness of 3.35mm, our its available reflection loss value
For -43.1dB, -40dB has been lower than it, Absorber Bandwidth reaches 4.1GHz, and electromagnetic wave absorptivity has reached 99.99%, absorbing property
It is excellent.
The preparation method of the micro-nano composite wave-suction material of BN/C based on urea involved in through the invention is obtained
The micro-nano composite wave-suction material of BN/CNTs, pattern is that sheet boron nitride connects different carbon nanotubes, with nitridation
The pattern of boron agglomerates into bulk.When thickness only has 2mm, the absorption band of this sample is most wide to reach 4GHz, reflection loss value
For -26.9dB, when with a thickness of 2.5mm, the reflection loss value of sample has reached maximum, is -36.5dB, at this time absorption band width
For 3GHz, absorbing property is excellent.
The preparation method of the micro-nano composite wave-suction material of BN/C based on urea involved in through the invention can be successfully
Synthesize the micro-nano composite wave-suction material of BN/C, and the above method have it is easy to be stable, easy to operate, low for equipment requirements etc. excellent
Point, and prepare absorbing material also there is good absorbing property, can be used as widely used absorbing material come using.BN/C
Micro-nano composite wave-suction material has reached a degree of balance between impedance matching and attenuation characteristic, it was demonstrated that this wave transparent of BN
Material is mixed into the absorbing property for being conducive to improve material, and furthermore the microwave absorbing property explanation of the micro-nano composite wave-suction material of BN/C should
Material can be used as good medium-high frequency absorbing material come using.
Claims (4)
1. a kind of preparation method of the micro-nano composite wave-suction material of BN/C based on urea, it is characterised in that: the following steps are included:
Step 1, mixing: by dried boric acid, urea, GNFs and dispersant, make solvent mixing system with deionized water
At mixed liquor；Or by dried boric acid, urea, CNTs and dispersant, it is mixed with deionized water as solvent
Mixed liquor, wherein the molar content of boric acid is 20%~30%, and the molar content of urea is 40%~60%,
The molar content of GNFs or CNTs is 10%~40%, and the molar ratio of boric acid and urea is always 1:2；
Step 2, drying: heating stirring 4h~6h, wherein heating temperature setting in magnetic stirring apparatus by the mixed liquor in step 1
It is 90 DEG C~100 DEG C, puts 55 DEG C~65 DEG C of drying box into again later and be evaporated, to obtain dry presoma；
Step 3, grinding: it takes out the resulting presoma of step 2 and is ground, powder is made；
Step 4, sintering and feeding: step 3 gained powder is placed in crucible, is carried out under protective gas using tube furnace
Sintering when sintering temperature is 1200 DEG C~1400 DEG C, keeps temperature 2.5h~3.5h, that is, when keeping the temperature under protective gas
Between be 2.5h~3.5h, taken out after cooling, the micro-nano composite wave-suction material of BN/C can be obtained.
2. the preparation method of the micro-nano composite wave-suction material of the BN/C according to claim 1 based on urea, feature exist
In: the dispersing agent uses SDS.
3. the preparation method of the micro-nano composite wave-suction material of the BN/C according to claim 1 based on urea, feature exist
In: mixed liquor manufactured in step 1 is put into ultrasonic cleaning instrument ultrasound 20min~40min.
4. the preparation method of the micro-nano composite wave-suction material of the BN/C according to claim 3 based on urea, feature exist
In: in the step 4, precursor powder is placed on graphite paper, is put into crucible again later, is utilized in a nitrogen environment
High temperature process furnances are sintered, and sintering temperature is 1400 DEG C, soaking time 3h.
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| CN201811426987.8A CN109294520A (en) | 2018-11-27 | 2018-11-27 | A kind of preparation method of the micro-nano composite wave-suction material of BN/C based on urea |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111154455A (en) * | 2020-01-09 | 2020-05-15 | 吉林大学 | Boron-doped mesoporous flower-like ferroferric oxide/carbon composite wave-absorbing material and preparation method thereof |
| CN113772637A (en) * | 2021-10-18 | 2021-12-10 | 青海大学 | Heat-conducting and wave-absorbing integrated nano composite material and preparation method thereof |
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| US20130032765A1 (en) * | 2011-08-04 | 2013-02-07 | Nokia Corporation | Composite for Providing Electromagnetic Shielding |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111154455A (en) * | 2020-01-09 | 2020-05-15 | 吉林大学 | Boron-doped mesoporous flower-like ferroferric oxide/carbon composite wave-absorbing material and preparation method thereof |
| CN111154455B (en) * | 2020-01-09 | 2022-12-30 | 吉林大学 | Boron-doped mesoporous flower-like ferroferric oxide/carbon composite wave-absorbing material and preparation method thereof |
| CN113772637A (en) * | 2021-10-18 | 2021-12-10 | 青海大学 | Heat-conducting and wave-absorbing integrated nano composite material and preparation method thereof |
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