CN109219336A - A kind of preparation method of the micro-nano composite wave-suction material of BN/C based on poly- ammonia borine - Google Patents
A kind of preparation method of the micro-nano composite wave-suction material of BN/C based on poly- ammonia borine Download PDFInfo
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- CN109219336A CN109219336A CN201811426965.1A CN201811426965A CN109219336A CN 109219336 A CN109219336 A CN 109219336A CN 201811426965 A CN201811426965 A CN 201811426965A CN 109219336 A CN109219336 A CN 109219336A
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Abstract
The present invention proposes a kind of preparation method of micro-nano composite wave-suction material of BN/C based on poly- ammonia borine, the following steps are included: step 1, GNFs or CNTs evenly spread in ammonia Borane solution, start blender stirring, open water-bath heater heating, temperature is set as 90 DEG C ~ 100 DEG C, reaction time is 23h ~ 25h, poly- ammonia borine and the mixing viscous liquid of GNFs or CNTs can be obtained after reaction, the molar content that wherein molar content of the poly- ammonia borine is 20% ~ 80%, GNFs or CNTs is 20% ~ 80%；Step 2, the air-distillation that the resulting liquid of step 1 is placed in the vessel to 90 DEG C ~ 100 DEG C of progress, to obtain precursor；Above-mentioned precursor is sintered by step 3 under protective gas; when sintering temperature is 1200 DEG C ~ 1400 DEG C; temperature 0.5h ~ 1.5h is kept under protective gas, i.e. soaking time is 0.5h ~ 1.5h, and the micro-nano composite wave-suction material of BN/C can be obtained later.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 compound suctions of BN/C based on poly- ammonia borine
The preparation method of wave 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 poly- ammonia borine is micro-nano
The preparation method of composite wave-suction material makes the micro-nano compound suction of BN/C of preparation to adjust the impedance matching property of carbon material
Wave material has good absorbing property.
To achieve the goals above, the invention proposes a kind of micro-nano composite wave-suction materials of BN/C based on poly- ammonia borine
Preparation method, comprising the following steps:
Step 1, mixing: GNFs or CNTs are evenly spread in ammonia Borane solution, and water is opened in starting blender stirring
Heater heating is bathed, temperature is set as 90 DEG C~100 DEG C, and the reaction time is 23h~25h, and poly- ammonia boron can be obtained after reaction
The mixing viscous liquid of alkane and GNFs, or poly- ammonia borine and the mixing viscous liquid of CNTs are obtained, wherein the poly- ammonia
The molar content that the molar content of borine is 20%~80%, GNFs or CNTs is 20%~80%；
Step 2, drying: the resulting liquid of step 1 is placed in the vessel to the air-distillation of 90 DEG C~100 DEG C of progress, to obtain
Obtain precursor；
Step 3, sintering and feeding: above-mentioned precursor is sintered under protective gas, sintering temperature 1200
DEG C~1400 DEG C when, keep temperature 0.5h~1.5h under protective gas, i.e., soaking time is 0.5h~1.5h, later
The micro-nano composite wave-suction material of BN/C can be obtained.
Preferably, in the step 1, under sonic oscillation and churned mechanically collective effect, by GNFs or
CNTs is evenly spread in ammonia Borane solution.
Preferably, in the step 2, air-distillation temperature is 95 DEG C.
Preferably, in the step 3, sintering temperature is 1400 DEG C, soaking time 1h.
Preferably, in the step 3, precursor is placed in crucible, utilizes high-temperature tubular in a nitrogen environment
Furnace carries out pressureless sintering.
The beneficial effect of the program of the present invention is through the above-mentioned micro-nano composite wave-absorbing of BN/C based on poly- ammonia borine
The preparation method of material can successfully synthesize the micro-nano composite wave-suction material of BN/C, and the above method has easy stable, operation
Simply, the advantages that low for equipment requirements, and the absorbing material prepared also has good absorbing property, can be used as and is widely used
Absorbing material come using.The micro-nano composite wave-suction material of BN/C has reached to a certain degree between impedance matching and attenuation characteristic
Balance, it was demonstrated that being mixed into of this electromagnetic wave transparent material of BN is conducive to improve the absorbing property of material, the furthermore micro-nano compound suction of BN/C
The microwave absorbing property of wave 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
Fig. 8 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 that the micro-nano composite wave-suction material of BN/C respectively match time raw material powder, wherein 20%, 40%,
60%, 80% be GNFs content.
Fig. 2 is the scanning electron microscope map of GNFs and the micro-nano composite wave-suction material of BN/C, wherein (a) and (b) is pure GNFs
Scanning electron microscope (SEM) photograph；It (c) is the scanning electron microscope (SEM) photograph of the micro-nano composite wave-suction material of BN/C with (d).
Fig. 3 is 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) constituency electricity
Sub- diffraction pattern figure (c) is high power figure, and (d) for flaky substance HRTEM figure, (illustration is interplanar distance.
Fig. 4 shows the EDAX analysis chart of the micro-nano composite wave-suction material of BN/C of preparation, wherein (a) is absorbing material
Transmission electron microscope map is (b) element score contained by the region (a), is (c) to carry out its distribution situation to C element region shown in (a)
Detection figure, be (d) the detection figure that its distribution situation is carried out to N element region shown in (a).
Fig. 5 shows the reflection loss figure of the micro-nano composite wave-suction material different-thickness of BN/C of different GNFs additive amounts.
Fig. 6 be the XRD spectrum of the micro-nano composite wave-suction material of BN/C at different temperatures, wherein (a) be 1200 DEG C and
1300 DEG C, (b) be 1400 DEG C.
Fig. 7 is the scanning electron microscope map of the micro-nano composite wave-suction material of BN/C at different temperatures, wherein (a) and (b) is equal
It is 1200 DEG C, (c) and (d) is 1300 DEG C.
Fig. 8 shows the reflection loss of the micro-nano composite wave-suction material of BN/C different-thickness under 2GHz-18GHz frequency
Figure.
Specific embodiment
A specific embodiment of the invention is further described with reference to the accompanying drawing.
The preparation method of BN/C micro-nano composite wave-suction material according to the present invention based on poly- ammonia borine includes following
Step:
Step 1, mixing: GNFs (graphene microchip) or CNTs (carbon nanotube) are evenly spread into ammonia Borane solution
In, water-bath heater heating is opened in starting blender stirring, and temperature is set as 90 DEG C~100 DEG C, and the reaction time is 23h~25h,
Poly- ammonia borine and the mixing viscous liquid of GNFs can be obtained after reaction, or obtain the mixing of poly- ammonia borine and CNTs
Viscous liquid, wherein the molar content of the poly- ammonia borine is the Mole percent of 20%~80%, GNFs or CNTs
Content is 20%~80%.
Specifically GNFs or CNTs can be evenly spread into ammonia under sonic oscillation and churned mechanically collective effect
In Borane solution.
Step 2, drying: the resulting liquid of step 1 is placed in container (such as open beaker) and carries out 90 DEG C~100 DEG C
Air-distillation, to obtain precursor.Wherein air-distillation temperature is best with 95 DEG C.
Step 3, sintering and feeding: above-mentioned precursor is sintered under protective gas, sintering temperature 1200
DEG C~1400 DEG C when, keep temperature 0.5h~1.5h under protective gas, i.e., soaking time is 0.5h~1.5h, later
The micro-nano composite wave-suction material of BN/C can be obtained.Wherein sintering temperature is best with 1400 DEG C, and soaking time is best with 1h.
In step 3, precursor can be placed in crucible, carries out pressureless sintering using tube furnace in a nitrogen environment,
In the present embodiment, using high temperature process furnances.It is micro-nano compound that it is just prepared for the BN/C that mass fraction is 20%~80% in this way
Absorbing material, what wherein numerical value indicated is the mass fraction of GNFs or CNTs in the composite.
The preparation method of the micro-nano composite wave-suction material of BN/C based on poly- ammonia borine involved in through the invention is obtained
The micro-nano composite wave-suction material of BN/GNFs microstructure be core-shell structure, BN be wrapped in graphite nano plate surface and
Around.For the diameter of the absorbing material close to 3 μm, lamellar spacing is maintained at 10nm or so.Back reflection of the GNFs in compound BN
Absolute value of decaying is promoted obviously, and when with a thickness of 2mm, reflection loss can achieve -33dB, Absorber Bandwidth under 11.2GHz frequency
Reach 3.8GHz.Reached a degree of balance between impedance matching and attenuation characteristic, this demonstrate that BN (boron nitride) this
Kind electromagnetic wave transparent material is mixed into the absorbing property for being conducive to improve material, illustrates that this absorbing material can be used as good medium-high frequency and inhale
Wave material.
The preparation method of the micro-nano composite wave-suction material of BN/C based on poly- ammonia borine involved in through the invention is obtained
The micro-nano composite wave-suction material of BN/CNTs obtained, the CNTs of addition are attached together, and most of region CNTs disperses more equal
Even, the winding between Guan Yuguan, which is crosslinked, to be reduced, and silk ribbon shape substance occurs in product, width range is substantially in 200nm~8 μm
Between.Maximum RL (reflection loss) value of the micro-nano composite wave-suction material of BN/CNTs reaches -18dB at 3mm, is located at 12GHz
Place, the frequency bandwidth greater than -10dB are 4GHz, are located at 10-14GHz, it is good to illustrate that the absorbing material under this thickness can be used as
Good medium-high frequency absorbing material；Also reach -16dB with a thickness of the maximum RL value of 3.5mm, is located at 10GHz, the frequency lower than -10dB
Bandwidth is located at 8-13GHz, can also be used as preferable intermediate frequency absorbing material.
The preparation method of the micro-nano composite wave-suction material of BN/C based on poly- ammonia borine involved in through the invention can be at
The micro-nano composite wave-suction material of synthesis BN/C of function, and the above method is stable, easy to operate, low for equipment requirements etc. with simplicity
Advantage, and prepare absorbing material also there is good absorbing property, can be used as widely used absorbing material come using.
The micro-nano composite wave-suction material of BN/C has reached a degree of balance between impedance matching and attenuation characteristic, it was demonstrated that BN is this
Electromagnetic wave transparent material is mixed into the absorbing property for being conducive to improve material, and furthermore the microwave absorbing property of the micro-nano composite wave-suction material of BN/C is said
The bright material can be used as good medium-high frequency absorbing material come using.
Claims (5)
1. a kind of preparation method of the micro-nano composite wave-suction material of BN/C based on poly- ammonia borine, it is characterised in that: including following
Step:
Step 1, mixing: GNFs or CNTs are evenly spread in ammonia Borane solution, and starting blender stirring is opened water-bath and added
The heating of hot device, temperature are set as 90 DEG C~100 DEG C, and the reaction time is 23h~25h, can be obtained after reaction poly- ammonia borine and
The mixing viscous liquid of GNFs, or poly- ammonia borine and the mixing viscous liquid of CNTs are obtained, wherein the poly- ammonia borine
Molar content be 20%~80%, GNFs or CNTs molar content be 20%~80%；
Step 2, drying: the resulting liquid of step 1 is placed in the vessel to the air-distillation of 90 DEG C~100 DEG C of progress, to obtain elder generation
Drive body；
Step 3, sintering and feeding: above-mentioned precursor is sintered under protective gas, sintering temperature be 1200 DEG C~
At 1400 DEG C, temperature 0.5h~1.5h is kept under protective gas, i.e. soaking time is 0.5h~1.5h, later
Obtain the micro-nano composite wave-suction material of BN/C.
2. the preparation method of the BN/C micro-nano composite wave-suction material according to claim 1 based on poly- ammonia borine, special
Sign is: under sonic oscillation and churned mechanically collective effect, GNFs or CNTs is evenly dispersed in the step 1
Into ammonia Borane solution.
3. the preparation method of the BN/C micro-nano composite wave-suction material according to claim 1 or 2 based on poly- ammonia borine,
Be characterized in that: in the step 2, air-distillation temperature is 95 DEG C.
4. the preparation method of the BN/C micro-nano composite wave-suction material according to claim 3 based on poly- ammonia borine, special
Sign is: in the step 3, sintering temperature is 1400 DEG C, soaking time 1h.
5. the preparation method of the BN/C micro-nano composite wave-suction material according to claim 4 based on poly- ammonia borine, special
Sign is: in the step 3, precursor being placed in crucible, is carried out in a nitrogen environment using high temperature process furnances without pressure
Sintering.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113716581A (en) * | 2021-09-13 | 2021-11-30 | 中国人民解放军国防科技大学 | High-ceramic-yield carbon-free boron nitride precursor and synthesis method thereof |
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| CN106028768A (en) * | 2016-05-17 | 2016-10-12 | 国网重庆市电力公司电力科学研究院 | Iron-plated graphene and preparation method |
| CN106041113A (en) * | 2016-05-17 | 2016-10-26 | 国网重庆市电力公司电力科学研究院 | Nanometer wave absorbing material and preparation method |
Non-Patent Citations (1)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113716581A (en) * | 2021-09-13 | 2021-11-30 | 中国人民解放军国防科技大学 | High-ceramic-yield carbon-free boron nitride precursor and synthesis method thereof |
| CN113716581B (en) * | 2021-09-13 | 2023-03-14 | 中国人民解放军国防科技大学 | High-ceramic-yield carbon-free boron nitride precursor and synthesis method thereof |
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