CN108946711A - A kind of preparation method of N doping redox graphene aeroge absorbing material - Google Patents
A kind of preparation method of N doping redox graphene aeroge absorbing material Download PDFInfo
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Abstract
The invention discloses a kind of N doping redox graphene aeroge (NGA) absorbing materials and preparation method thereof.Using graphene oxide (GO) aqueous dispersions as template, ethylenediamine (EDA) is nitrating agent and reducing agent, N doping redox graphene hydrogel is formed by one step hydro thermal method primary reconstruction, dialysis, freeze-drying obtain N doping redox graphene aeroge.The preparation method is environmentally protective, without any toxic by-product generates, preparation process is simple, reaction condition is mild, low in cost.Aeroge absorbing material electromagnetic wave absorption ability obtained is strong, absorption band is wide, density is low, packing ratio is low, and the thickness by adjusting N doping amount and microwave absorbing coating may be implemented effectively to absorb the electromagnetic wave of different-waveband, have important application value in electromagnetic absorption and electromagnetic shielding field.
Description
Technical field
The invention belongs to electromagnetism stealth field of material technology, and in particular to a kind of N doping redox graphene aeroge
The preparation method of absorbing material.
Background technique
In recent years, electromagnetic pollution problem increasingly aggravates, the electromagnetic radiation meeting that the electronic equipment being seen everywhere in life issues
The generations such as nervous system, the immune system of human body are directly endangered by fuel factor.In addition to this, the electromagnetism in military field is hidden
Body technology is also evolving progress, and electromagnetic wave absorbent material is increasingly becoming the research hotspot of field of functional materials.
The honeycomb two dimensional crystal that graphene is made of carbon hexatomic ring, i.e. mono-layer graphite.Its with high specific surface area,
The advantageous properties such as superhigh current carrying transport factor, good thermal stability, but graphene itself has hydrophobicity, easily rolls into a ball in water
It is poly-, and graphene does not have band gap, is not easy to react with other materials.Compared to graphene, the surface of graphene oxide (GO)
Oxygen-containing functional group (- COOH ,-OH ,-C-O-C- etc.) abundant is carried with edge, this not only improves its dispersibility in water,
And help to react with other substances；GO is obtained redox graphene (RGO) after hydrothermal reduction, on RGO lamella by
Introducing and remaining oxygen-containing functional group in defect, so that RGO has stronger dielectric loss and electro-magnetic wave absorption ability.So
And two-dimensional sheet RGO is used for electromagnetic wave attenuation mechanism poor and single due to impedance matching when electromagnetic wave absorbent material, makes it
Electro-magnetic wave absorption intensity is poor, is not able to satisfy the requirement of practical application.
Thickness in order to meet new electromagnetic wave absorbing material is thin, light weight, absorption band is wide, absorbent properties are strong (" thin,
Gently, wide, strong ") etc. require, can choose suitable method and processing be modified to RGO, regulate and control its physics, chemical property, thus
Enhance RGO to the absorbability of electromagnetic wave.Wherein, nitrogen-atoms is adulterated in RGO lattice to prepare N doping RGO not only and can be improved
Its electric conductivity, and a large amount of defects can be introduced in RGO sheet surfaces, distortion of lattice is generated, can be increased by defect polarization
Its strong damping capacity to electromagnetic wave.
When RGO is used for electromagnetic wave absorbent material at present, research focuses primarily upon the structure of low-dimensional (zero dimension, two dimension) composite material
It builds, generally there are the disadvantages of percentage is higher and Absorber Bandwidth is relatively narrow is filled when wave absorbing agent makees filler.Graphene aerogel is one
The new carbon of kind of tridimensional network, not only have flourishing pore structure, huge specific surface area, extremely low density and
Good dielectric properties；Moreover, complicated three-dimensional open-framework increases the transmission path of electromagnetic wave inside it, by multiple
Reflection and scattering can be with the electromagnetic waves etc. of effective attenuation incidence, therefore graphene aerogel has extensively in electro-magnetic wave absorption field
Application prospect.
The present invention is using GO aqueous dispersions as template, and ethylenediamine (EDA) is nitrating agent and reducing agent, using simple step water
Thermal method primary reconstruction forms N doping redox graphene hydrogel, and dialysis, freeze-drying obtain N doping reduction-oxidation
Graphene aerogel (NGA).The electromagnetic wave to different-waveband may be implemented in thickness by adjusting N doping amount and microwave absorbing coating
It effectively absorbs, and has the characteristics that lightweight, efficient, wideband and low packing ratio.
Summary of the invention
The purpose of the present invention is to provide a kind of N doping redox graphene aeroge absorbing material and its preparation sides
Method, the composite material not only have the characteristics that low-density, strong absorption, broadband, low packing ratio and absorbing property easy-regulating, and
Its preparation process is simple, reaction condition is mild, environmentally protective.
The invention is realized by the following technical scheme:
A kind of N doping redox graphene aeroge absorbing material, the absorbing material is by two-dimentional nitrating RGO piece
The three-dimensional space network structure that layer is self-assembly of is constituted.
A kind of preparation method of N doping redox graphene aeroge absorbing material, its step are as follows:
Step 1: taking 4 100mL beakers, be separately added into 30mL deionized water, be then respectively adding 60mg graphite oxide, surpass
Sound 1h, the GO aqueous dispersions that 30min obtains concentration as 2mg/mL are vigorously stirred.
Step 2: in whipping process, the EDA that volume is 180,240,300,360 μ L being slowly added dropwise respectively, continues to stir
30min。
Step 3: the reaction solution in beaker being poured into 50mL reaction kettle, in 120 DEG C of hydro-thermal reaction 12h.
Step 4: after reaction, obtaining N doping redox graphene hydrogel, hydrogel is slowly added into 100mL
In the ethanol water that percentage by volume is 10%, dialysis for 24 hours, changes an ethanol water at interval of 6h.
Step 5: the hydrogel dialysed being put into pre-freeze 12h in refrigerator, 36h is then freeze-dried and obtains N doping reduction
Graphite oxide aerogel.
Compared with prior art, advantageous effects of the invention embody in the following areas:
1, N doping redox graphene hydrogel, dialysis, freeze-drying is made using one step of hydro-thermal reaction in the present invention
Obtain aeroge.Easy to operate, reaction condition is mild, green safe, and no any poisonous and harmful substance generates, is any without being added
Surfactant and inert gas shielding.
2, the present invention is by changing addition volume of the EDA in GO dispersion liquid to regulate and control N doping amount in RGO, Ke Yishi
Now to effective absorption of electromagnetic wave.
3, N doping redox graphene aerogel material absorbing property prepared by the present invention is excellent, have low-density,
The features such as strong absorption, broadband, low packing ratio and absorbing property easy-regulating.Filling quality percentage is in paraffin matrix
When 6wt%, the absorption maximum intensity of composite material reaches -67.3dB, and effective Absorber Bandwidth is 3.2GHz；By adjusting microwave absorbing coating
Thickness may be implemented effectively to absorb the electromagnetic wave of different-waveband.
4, N doping redox graphene aeroge prepared by the present invention, existing defects polarization, dipole polarization, dielectric damage
The synergistic effect of a variety of wave-absorbing mechanisms such as consumption, conductance loss, multipath reflection and scattering, may be implemented effective absorption to electromagnetic wave
With decaying.
Detailed description of the invention
Fig. 1 is the XRD spectra of product in embodiment 1,2,3,4；
Fig. 2 is the FT-IR spectrogram of product in embodiment 1,2,3,4；
Fig. 3 is the TEM photo of product S4 in embodiment 4；
Fig. 4 is the reflection loss of product S1 in embodiment 1 with the change curve of frequency；
Fig. 5 is the reflection loss of product S2 in embodiment 2 with the change curve of frequency；
Fig. 6 is the reflection loss of product S3 in embodiment 3 with the change curve of frequency；
Fig. 7 is the reflection loss of product S4 in embodiment 4 with the change curve of frequency.
Specific implementation method
Now in conjunction with embodiment and attached drawing, the invention will be further described:
Embodiment 1
1,1 100mL beaker is taken, 30mL deionized water is added, 60mg graphite oxide is then added, ultrasonic 1h, acutely stirs
It mixes 30min and obtains the GO aqueous dispersions that concentration is 2mg/mL.
2, in whipping process, the EDA that volume is 180 μ L is slowly added dropwise, continues to stir 30min.
3, the reaction solution in beaker is poured into 50mL reaction kettle, in 120 DEG C of hydro-thermal reaction 12h.
4, N doping redox graphene hydrogel after reaction, is obtained, hydrogel is slowly added to 100mL volume
In the ethanol water that percentage is 10%, dialysis for 24 hours, changes an ethanol water at interval of 6h.
5, the hydrogel dialysed is put into pre-freeze 12h in refrigerator, is then freeze-dried 36h and obtains N doping reduction-oxidation
Graphene aerogel is denoted as S1.
The XRD spectra of 1 product S1 of embodiment is shown in that Fig. 1, FT-IR spectrogram are shown in Fig. 2.Weigh the aeroge and solid of certain mass
Paraffin makes its mass ratio 6:94, and load weighted solid paraffin is melted at 80 DEG C, is sliced aeroge using infusion process and soaks
Enter in melt paraffin, the coaxial sample of outer diameter 7.00mm, internal diameter 3.04mm, thickness about 2mm be then pressed into particular manufacturing craft,
Its absorbing property, test frequency 2-18GHz are tested with model AV3629D vector network analyzer.Its reflection loss is with frequency
The change curve of rate is as shown in figure 4, the matching thickness of the sample is 4.5mm, and in 7.36GHz, absorption maximum reaches -17.35dB,
Absorption intensity is in -10dB hereinafter, effectively Absorber Bandwidth is 2.48GHz in 6.16-8.64GHz frequency range.
Embodiment 2
1,1 100mL beaker is taken, 30mL deionized water is added, 60mg graphite oxide is then added, ultrasonic 1h, acutely stirs
It mixes 30min and obtains the GO aqueous dispersions that concentration is 2mg/mL.
2, in whipping process, the EDA that volume is 240 μ L is slowly added dropwise, continues to stir 30min.
3, the reaction solution in beaker is poured into 50mL reaction kettle, in 120 DEG C of hydro-thermal reaction 12h.
4, N doping redox graphene hydrogel after reaction, is obtained, hydrogel is slowly added to 100mL volume
In the ethanol water that percentage is 10%, dialysis for 24 hours, changes an ethanol water at interval of 6h.
5, the hydrogel dialysed is put into pre-freeze 12h in refrigerator, is then freeze-dried 36h and obtains N doping reduction-oxidation
Graphene aerogel is denoted as S2.
The XRD spectra of 2 product S2 of embodiment is shown in that Fig. 1, FT-IR spectrogram are shown in Fig. 2.Weigh the aeroge and solid of certain mass
Paraffin makes its mass ratio 6:94, and load weighted solid paraffin is melted at 80 DEG C, is sliced aeroge using infusion process and soaks
Enter in melt paraffin, the coaxial sample of outer diameter 7.00mm, internal diameter 3.04mm, thickness about 2mm be then pressed into particular manufacturing craft,
Its absorbing property, test frequency 2-18GHz are tested with model AV3629D vector network analyzer.Its reflection loss is with frequency
The change curve of rate is as shown in figure 5, the matching thickness of the sample is 5.0mm, and in 6.64GHz, absorption maximum reaches -13.48dB,
Absorption intensity is in -10dB hereinafter, effectively Absorber Bandwidth is 1.76GHz in 5.92-7.68GHz frequency range.
Embodiment 3
1,1 100mL beaker is taken, 30mL deionized water is added, 60mg graphite oxide is then added, ultrasonic 1h, acutely stirs
It mixes 30min and obtains the GO aqueous dispersions that concentration is 2mg/mL.
2, in whipping process, the EDA that volume is 300 μ L is slowly added dropwise, continues to stir 30min.
3, the reaction solution in beaker is poured into 50mL reaction kettle, in 120 DEG C of hydro-thermal reaction 12h.
4, N doping redox graphene hydrogel after reaction, is obtained, hydrogel is slowly added to 100mL volume
In the ethanol water that percentage is 10%, dialysis for 24 hours, changes an ethanol water at interval of 6h.
5, the hydrogel dialysed is put into pre-freeze 12h in refrigerator, is then freeze-dried 36h and obtains N doping reduction-oxidation
Graphene aerogel is denoted as S3.
The XRD spectra of 3 product S3 of embodiment is shown in that Fig. 1, FT-IR spectrogram are shown in Fig. 2.Weigh the aeroge and solid of certain mass
Paraffin makes its mass ratio 6:94, and load weighted solid paraffin is melted at 80 DEG C, is sliced aeroge using infusion process and soaks
Enter in melt paraffin, the coaxial sample of outer diameter 7.00mm, internal diameter 3.04mm, thickness about 2mm be then pressed into particular manufacturing craft,
Its absorbing property, test frequency 2-18GHz are tested with model AV3629D vector network analyzer.Its reflection loss is with frequency
The change curve of rate is as shown in fig. 6, the matching thickness of the sample is 5.0mm, and in 6.64GHz, absorption maximum reaches -12.40dB,
Absorption intensity is in -10dB hereinafter, effectively Absorber Bandwidth is 1.44GHz in 6.08-7.52GHz frequency range.
Embodiment 4
1,1 100mL beaker is taken, 30mL deionized water is added, 60mg graphite oxide is then added, ultrasonic 1h, acutely stirs
It mixes 30min and obtains the GO aqueous dispersions that concentration is 2mg/mL.
2, in whipping process, the EDA that volume is 360 μ L is slowly added dropwise, continues to stir 30min.
3, the reaction solution in beaker is poured into 50mL reaction kettle, in 120 DEG C of hydro-thermal reaction 12h.
4, N doping redox graphene hydrogel after reaction, is obtained, hydrogel is slowly added to 100mL volume
In the ethanol water that percentage is 10%, dialysis for 24 hours, changes an ethanol water at interval of 6h.
5, the hydrogel dialysed is put into pre-freeze 12h in refrigerator, is then freeze-dried 36h and obtains N doping reduction-oxidation
Graphene aerogel is denoted as S4.
The XRD spectra of 4 product S4 of embodiment is shown in that Fig. 1, FT-IR spectrogram are shown in that Fig. 2, TEM photo are shown in Fig. 3.Weigh certain mass
Aeroge and solid paraffin make its mass ratio 6:94, load weighted solid paraffin is melted at 80 DEG C, using infusion process
Aeroge is sliced and is immersed in melt paraffin, outer diameter 7.00mm, internal diameter 3.04mm, thickness are then pressed into particular manufacturing craft about
The coaxial sample of 2mm tests its absorbing property, test frequency 2-18GHz with model AV3629D vector network analyzer.
Its reflection loss is with the change curve of frequency as shown in fig. 7, the matching thickness of the sample is 4.6mm, and in 6.08GHz, maximum is inhaled
It receives and reaches -67.3dB, absorption intensity is in -10dB hereinafter, effectively Absorber Bandwidth is in 4.96-8.16GHz frequency range
3.2GHz。
By the test result of above embodiments it is found that N doping oxygen reduction is made using simple one step of hydro-thermal method in the present invention
Graphite alkene aeroge, this method is easy to operate, reaction condition is mild, safe green, nonhazardous substance generate, the electromagnetism of product
Wave absorbent properties are excellent, and absorption maximum intensity reaches -67.3dB；By the thickness for adjusting N doping amount and microwave absorbing coating in RGO
Effective absorption to different-waveband electromagnetic wave may be implemented, therefore N doping redox graphene aeroge is a kind of ideal
Electromagnetic wave absorbent material.
Claims (9)
1. a kind of N doping redox graphene aeroge (NGA) absorbing material, it is characterised in that: the absorbing material by
The three-dimensional space network structure that two-dimentional nitrating redox graphene (RGO) lamella is self-assembly of is constituted.
2. NGA absorbing material according to claim 1, which is characterized in that the absorbing material is prepared by the following method:
Step 1: 4 100mL beakers are taken, 30mL deionized water is separately added into, are then respectively adding 60mg graphite oxide, ultrasound
1h, graphene oxide (GO) aqueous dispersions that 30min obtains concentration as 2mg/mL are vigorously stirred.
Step 2: in whipping process, the ethylenediamine (EDA) that volume is 180,240,300,360 μ L being slowly added dropwise respectively, continues
Stir 30min.
Step 3: the reaction solution in beaker being poured into 50mL reaction kettle, in 120 DEG C of hydro-thermal reaction 12h.
Step 4: after reaction, obtaining N doping redox graphene hydrogel, hydrogel is slowly added to 100mL volume
In the ethanol water that percentage is 10%, dialysis for 24 hours, changes an ethanol water at interval of 6h.
Step 5: the hydrogel dialysed being put into pre-freeze 12h in refrigerator, 36h is then freeze-dried and obtains N doping reduction-oxidation
Graphene aerogel.
3. preparation method according to claim 2, it is characterised in that: the ultrasonic time of the step 1 is 1h.Ultrasonic time
It is too long the structure snd size of GO lamella to be damaged, the too short GO dispersion liquid for being difficult to form monolithic layer of ultrasonic time.
4. preparation method according to claim 2, it is characterised in that: in the step 2 when EDA is added dropwise, slowly by
Drop is added dropwise, and the EDA being added dropwise is enable to be uniformly mixed with GO aqueous dispersions rapidly, avoids reaction excessively strong, and it is existing gelation occur
As；Meanwhile avoiding bringing into the generation of impurity and side reaction.
5. preparation method according to claim 2, it is characterised in that: in the step 3, hydrothermal temperature is 120 DEG C,
Time is 12h.Temperature is too low, the time too short cannot be effectively formed N doping redox graphene hydrogel；Temperature is excessively high, when
Between it is too long, energy consumption is larger, and preparation cost is higher.
6. preparation method according to claim 2, it is characterised in that: in the step 4, dialyzate is that percentage by volume is
10% ethanol water reduces the freezing point of system, avoids in freezing dry process by displacing the water in hydrogel, ice
Crystals growth is excessive to cause gel structure to collapse.
7. preparation method according to claim 2, it is characterised in that: the drying of the step 5 is vacuum freeze drying, and
Hydrogel after dialysis must first pass through the pre-freeze of 12h, then be freeze-dried, and otherwise gel can collapse, and generate cotton-shaped
Product.
8. preparation method according to claim 2, it is characterised in that: the content of GO in control reaction system passes through change
The addition volume of EDA, hydro-thermal reaction obtain the NGA of different N doping amounts, study electromagnetic parameter and suction of the itrogen content of getter with nitrogen doped to aeroge
The influence of wave performance.
9. the preparation of N doping redox graphene aeroge absorbing material is prepared in strict accordance with the claims.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110451492A (en) * | 2019-08-26 | 2019-11-15 | 兰州理工大学 | Sulphur nitrogen codope graphene absorbing material and preparation and absorbing property adjusting method |
| CN111389438A (en) * | 2020-02-24 | 2020-07-10 | 哈尔滨工业大学 | Preparation method and application of nitrogen-doped three-dimensional graphene-loaded manganese dioxide catalyst |
| CN112354491A (en) * | 2020-10-27 | 2021-02-12 | 浙江工业大学 | Carbon-nitrogen double-defect optimized three-dimensional honeycomb aerogel and preparation method and application thereof |
| CN112430451A (en) * | 2020-12-03 | 2021-03-02 | 安徽理工大学环境友好材料与职业健康研究院(芜湖) | Nitrogen-doped graphene/cobalt-zinc ferrite composite aerogel wave-absorbing material and preparation method thereof |
| CN109399619B (en) * | 2018-12-31 | 2021-06-04 | 太原理工大学 | Preparation method of nitrogen-doped graphene aerogel |
| CN113277501A (en) * | 2021-05-12 | 2021-08-20 | 北京化工大学 | Nitrogen-doped reduced graphene oxide aerogel and application thereof in preparation of microwave absorbing material |
| CN114853502A (en) * | 2022-05-26 | 2022-08-05 | 哈尔滨工业大学（威海） | Ceramic/graphene aerogel wave-absorbing material and preparation method and application thereof |
| CN115385715A (en) * | 2022-09-15 | 2022-11-25 | 南京信息工程大学 | Porous carbon-rich silicon carbon nitrogen ceramic wave-absorbing heat-conducting material and preparation method thereof |
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Cited By (11)
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| CN109399619B (en) * | 2018-12-31 | 2021-06-04 | 太原理工大学 | Preparation method of nitrogen-doped graphene aerogel |
| CN110451492A (en) * | 2019-08-26 | 2019-11-15 | 兰州理工大学 | Sulphur nitrogen codope graphene absorbing material and preparation and absorbing property adjusting method |
| CN111389438A (en) * | 2020-02-24 | 2020-07-10 | 哈尔滨工业大学 | Preparation method and application of nitrogen-doped three-dimensional graphene-loaded manganese dioxide catalyst |
| CN111389438B (en) * | 2020-02-24 | 2023-03-10 | 哈尔滨工业大学 | Preparation method and application of nitrogen-doped three-dimensional graphene-loaded manganese dioxide catalyst |
| CN112354491A (en) * | 2020-10-27 | 2021-02-12 | 浙江工业大学 | Carbon-nitrogen double-defect optimized three-dimensional honeycomb aerogel and preparation method and application thereof |
| CN112354491B (en) * | 2020-10-27 | 2022-04-22 | 浙江工业大学 | Carbon-nitrogen double-defect optimized three-dimensional honeycomb aerogel and preparation method and application thereof |
| CN112430451A (en) * | 2020-12-03 | 2021-03-02 | 安徽理工大学环境友好材料与职业健康研究院(芜湖) | Nitrogen-doped graphene/cobalt-zinc ferrite composite aerogel wave-absorbing material and preparation method thereof |
| CN113277501A (en) * | 2021-05-12 | 2021-08-20 | 北京化工大学 | Nitrogen-doped reduced graphene oxide aerogel and application thereof in preparation of microwave absorbing material |
| CN114853502A (en) * | 2022-05-26 | 2022-08-05 | 哈尔滨工业大学（威海） | Ceramic/graphene aerogel wave-absorbing material and preparation method and application thereof |
| CN115385715A (en) * | 2022-09-15 | 2022-11-25 | 南京信息工程大学 | Porous carbon-rich silicon carbon nitrogen ceramic wave-absorbing heat-conducting material and preparation method thereof |
| CN115385715B (en) * | 2022-09-15 | 2023-09-19 | 南京信息工程大学 | Porous carbon-rich silicon-carbon-nitrogen ceramic heat absorption waveguide material and preparation method thereof |
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Application publication date: 20181207 |