CN116101999A - Discontinuous light hollow carbon sphere wave-absorbing material and preparation method and application thereof - Google Patents
Discontinuous light hollow carbon sphere wave-absorbing material and preparation method and application thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000011358 absorbing material Substances 0.000 title claims abstract description 9
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 46
- 239000004005 microsphere Substances 0.000 claims abstract description 30
- 239000011780 sodium chloride Substances 0.000 claims abstract description 23
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims abstract description 10
- 229930006000 Sucrose Natural products 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000005720 sucrose Substances 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 18
- 238000001354 calcination Methods 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 13
- 239000002243 precursor Substances 0.000 claims description 13
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims description 8
- 229960001149 dopamine hydrochloride Drugs 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
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- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 abstract description 6
- 229960003638 dopamine Drugs 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 abstract description 2
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
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- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
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- 238000002347 injection Methods 0.000 description 1
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- 239000002064 nanoplatelet Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- 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
Abstract
The invention discloses a discontinuous light hollow carbon sphere wave-absorbing material, a preparation method and application thereof, wherein the carbon sphere skeleton obtained by the invention consists of graphitized carbon derived from sucrose and carbon nitrogen derived from dopamine, and the porosity of microspheres is generated by washing sodium chloride; the method is simple and convenient, has high environmental friendliness and low price, and is suitable for large-scale production; the carbon sphere prepared by the invention has good wave absorption performance, has microwave absorption performance at a plurality of frequency bands in 2-18GHz, and has wide application prospect in the wave absorption field.
Description
Technical Field
The invention belongs to the technical field of microwave absorbing materials, and relates to a discontinuous light wave absorbing microsphere, a preparation method and application thereof.
Background
The new technological revolution and industrial revolution remodel the global economic structure, and the electronic equipment and communication technology rapidly develop, but electromagnetic radiation pollution is also caused at the same time, the normal use of electronic products is interfered, and even the life and the health of people are threatened, so the development of the efficient microwave absorbing material has important significance. The chemical components and the structures are key factors influencing the wave absorbing performance, and the connection between the microstructure of the material and the wave absorbing performance is explored through fine structure and component design, so that the method has great guiding significance for the development of subsequent high-performance wave absorbing materials.
Carbon materials are considered to be ideal wave-absorbing materials due to their good electrical conductivity and low density and low cost. In addition, in terms of structural design, the construction of the multi-stage holes and the formation of the three-dimensional hollow structure can effectively improve the material properties: on one hand, the outer shell layer, the inner air, the shell layer at the hole and the air can form a larger interface, and the existence of the air layer is beneficial to optimizing the impedance matching of the material, so that more electromagnetic waves enter the material, and the probability of electromagnetic wave loss is increased; in addition, the ordered pore walls of the three-dimensional structure can promote the electromagnetic waves to generate multiple scattering inside the microspheres, so that the electromagnetic waves are further dissipated. It can be seen that the wave-absorbing property of the material can be controlled by changing the pore size or the shell thickness of the material.
However, the synthetic strategies adopted by the porous microspheres constructed at present are complex, and effective adjustment of the pore diameters is difficult to realize, so that the microsphere structure cannot be effectively improved to control the wave absorbing performance of the material. Therefore, there is a need to develop a simple, low-cost and mass-production-promoting method for preparing porous microspheres, and to realize the adjustment of the pore size, so as to meet the application requirements of the porous microspheres in the wave-absorbing field.
Disclosure of Invention
The invention aims to provide a discontinuous light wave-absorbing microsphere, a preparation method and application thereof.
The invention discovers that the synthesis strategy adopted by the porous microsphere is complex, and the adopted templates are difficult to remove, so that the microsphere structure cannot be effectively improved to control the wave absorbing performance of the material. In addition, the used raw materials are also high in cost, and large-scale production cannot be realized. Based on the problems, the discontinuous light hollow carbon spheres are designed, and the aperture of the microspheres is regulated and controlled by a green convenient method, so that materials with different wave absorbing properties are obtained.
The technical scheme of the invention is as follows:
a preparation method of discontinuous light wave-absorbing microspheres comprises the following steps:
(1) Mixing sucrose solution, dopamine hydrochloride solution and sodium chloride, performing ultrasonic dispersion to obtain clear mixed solution, and performing spray drying on the obtained mixed solution to obtain precursor powder;
wherein, the concentration of the sucrose solution is 5-10 mg/mL, and the concentration of the dopamine hydrochloride solution is 15-30 mg/mL; the ratio of sucrose solution, dopamine hydrochloride solution and sodium chloride was 50 (mL): 50 (mL): 3 to 5 (g);
preferably, the ultrasonic dispersion time is 20-30 min;
preferred parameters for spray drying are: the air inlet temperature is 160-180 ℃, the feeding rate is 6-10 mL/min, and the air flow rate is 30-35 m 3 And/h, nozzle size 0.7mm;
(2) The precursor powder obtained in the step (1) is added in N 2 Calcining under the atmosphere at 400-500 ℃ for 2h to obtain precursor carbon spheres;
preferably, the temperature rising rate of calcination is 5 ℃/min;
(3) Adding the precursor carbon spheres obtained in the step (2) into deionized water, stirring to remove sodium chloride, filtering, drying (60-80 ℃), and adding the precursor carbon spheres into N 2 Calcining again in the atmosphere at 800-900 ℃ for 2h to obtain the discontinuous light wave-absorbing microsphere;
preferably, the ratio of precursor carbon spheres to deionized water is 0.1:0.5 g/L; stirring to remove sodium chloride for 12h;
specifically, the membrane used for suction filtration is a 0.22 μm aqueous membrane;
preferably, the rate of temperature rise for the re-calcination is 5 ℃/min.
The invention also relates to the discontinuous light wave-absorbing microsphere prepared by the preparation method.
The discontinuous light wave-absorbing microsphere forms multistage holes, and a microsphere framework is formed by assembling a graphitized carbon sheet derived from sucrose and a nitrogen-doped carbon sheet derived from dopamine; the pore volume of the carbon sphere is 0.24-0.33 cm 3 Per gram, specific surface area of 321.2-397.6 m 2 The average size of the pores per gram is 2.82-3.39 nm.
The discontinuous light wave-absorbing microsphere can be used for preparing microwave absorbing materials, realizes absorption of a plurality of frequency bands within 2-18GHz, and has a minimum reflection loss value of-30.1 dB.
The technical principle of the invention is as follows:
according to the invention, the single dopamine hydrochloride spraying effect is poor, so that a small amount of sucrose is added as a binder to better assemble the carbon sheets, and a more regular three-dimensional sphere is formed. When preparing spray solution, sodium chloride is dissolved uniformly, so that the crystallized sodium chloride can be dispersed uniformly on the carbon spheres after the liquid drops from the spray nozzle evaporate water.
The spray drying principle is that the high-temperature air flow dries small liquid drops rapidly, a precursor aqueous solution is adopted, the precursor aqueous solution is changed into small liquid drops through a nozzle and then meets the high-temperature air flow in a very short time, so that water is evaporated, and finally dry powder is collected.
In addition, the twice calcination of the invention is mainly formulated according to the melting point of NaCl, if the initial calcination is 800 ℃, the NaCl can be melted to damage the pore structure of the sphere, so that the melting point of NaCl (801 ℃) is combined, and the NaCl is carbonized (400-500 ℃) at a certain temperature to conveniently wash away the NaCl; if only calcining is carried out at 400-500 ℃, the dielectric constant and the wave absorbing performance of the sample obtained by testing are poor, and the improvement of the conductivity of the carbon material after calcining at high temperature is considered, so that the dielectric performance of the material is enhanced, and the sample is divided into two calcining.
Compared with the prior art, the invention has the following advantages:
(1) The material provided by the invention is applied to the field of microwave absorption, and has the advantage of realizing reflection loss in multiple frequency bands. Multi-frequency absorption below-10 dB is achieved at different thicknesses, including low-frequency to high-frequency C-band (4-8 GHz), X-band (8-12 GHz) and Ku-band (12-18 GHz).
(2) The preparation method provided by the invention has the advantages of simple synthesis process, low cost and high environmental friendliness of the used raw materials, and can be popularized and realize large-scale production.
(3) The microsphere provided by the invention has multistage holes, and the hole size is convenient to regulate and control, so that the wave absorbing performance of the material is improved by regulating and controlling the dielectric performance.
Drawings
FIG. 1 is a scanning electron microscope image of each sample: (a), (b) discontinuous lightweight hollow carbon spheres HC-1; (c) and (d) discontinuous lightweight hollow carbon spheres HC-2; (e) and (f) discontinuous light hollow carbon spheres HC-3.
Fig. 2 is a transmission electron microscope image: discontinuous light hollow carbon spheres HC-2.
FIG. 3N of different pore sizes 2 Adsorption and desorption graphs and size distribution graphs.
Fig. 4 is a graph of the wave absorbing properties of different samples.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples. The present embodiment is implemented on the premise of the technical scheme of the present invention, and a detailed implementation manner and a specific operation process are given, but the protection scope of the present invention is not limited to the following examples.
In the following examples, unless otherwise indicated, materials or processing techniques are all typical of those commercially available in the art.
Example 1:
preparation of discontinuous light hollow carbon spheres HC-1:
firstly, 50mL of sucrose solution with the concentration of 10mg/mL, 50mL of dopamine hydrochloride solution with the concentration of 30mg/mL and 3g of sodium chloride are taken, and a clear solution is obtained after mixing and ultrasonic treatment for 20min, so that uniform dispersion of a sample is ensured;
then, the solution is introduced into a spray dryer, the parameters are that the air inlet temperature is 180 ℃, the sample injection rate is 6mL/min, and the gas flow rate is 35m 3 Selecting a nozzle with the size of 0.7mm, and collecting powder after finishing;
then, the spray-dried powder was subjected to N at 400 DEG C 2 Calcining and carbonizing for 2 hours under the protection, wherein the heating rate is 5 ℃/min. The initially calcined sample was then added to deionized water (0.1 g/0.5L) and vigorously stirred for 12 hours to thoroughly wash away the sodium chloride attached to the sample.
Finally, filtering the washed solution, collecting a sample, drying, and calcining at a high temperature of 800 ℃ under the atmosphere of N 2 The calcination time is 2 hours, the heating rate is 5 ℃/min, and the target product of the discontinuous light hollow carbon sphere material is obtained.
Example 2:
preparation of discontinuous light hollow carbon spheres HC-2:
in comparison with example 1, the same operation was carried out in a large part except that the amount of sodium chloride added was changed to 4 g.
Example 3:
preparation of discontinuous light hollow carbon spheres HC-3:
in comparison with example 1, the same operation was carried out in a large part except that the amount of sodium chloride added was changed to 5 g.
Characterization and Performance test experiments
The microstructure of the discontinuous lightweight hollow carbon spheres in the above examples was characterized by scanning electron microscopy (SEM, hitachi SEM S-4800), sample preparation method: and taking a small amount of powder sample, dispersing the powder sample in ethanol by ultrasonic waves, dripping the powder sample on a conductive silicon wafer, and drying the conductive silicon wafer for testing. The microstructure of the composite material can be further observed through transmission electron microscope characterization (TEM, JEOL JEM-2100F), and the preparation method comprises the following steps: and taking a small amount of powder sample, dispersing the powder sample in ethanol by ultrasonic, and then dripping the powder sample on a carbon-supported copper mesh for drying to test.
FIG. 1 is a Scanning Electron Microscope (SEM) of a series of discontinuous light hollow carbon sphere materials synthesized by a regulation means, a, b are microscopic morphologies of a calcined product HC-1 of a sample with NaCl content of 3g in example 1, the whole is assembled by calcined carbon nano-sheets, the hollow porous spherical morphology is presented, and pores are orderly arranged; if the NaCl content is increased to 4g, the shell pore size of the final product HC-2 is increased, as shown in FIGS. 1 c-d (i.e., the product obtained in example 2); if the NaCl content is increased to 5g, the shell pore size of the final product HC-3 increases significantly and still maintains a hollow sphere like structure, e-f in FIG. 2 (i.e., the product produced in example 3).
FIG. 2 is a Transmission Electron Microscope (TEM) image of the HC-2 porous hollow sphere obtained in example 2 described above. As shown in fig. 2 a, the sample as a whole exhibited a hollow sphere structure, assembled from a number of carbon nanoplatelets, and it can also be seen that the microspheres had a number of voids, consistent with the results seen by the scan, which revealed successful preparation of hollow microspheres with discontinuous dielectrics.
FIG. 3 is N of the non-continuous dielectric hollow carbon spheres with controllable pore diameters prepared in the above examples 1-3 2 And (5) analyzing an adsorption and desorption curve and a pore size distribution diagram. In FIG. 3 a, N of example 1 2 The adsorption-desorption curve corresponds to type IV and shows obvious mesoporous structure, wherein the pore volume is 0.28cm 3 Per gram, specific surface area of 397.66m 2 The average size of the pores per gram is according to the formula: pore volume/specific surface area, the average pore size was calculated to be 2.82nm, which is consistent with the pore size distribution diagram of b in fig. 3, the pore size is mainly distributed at 2-5nm, again confirming that the microsphere pores are mesoporous; whereas example 2, HC-2 material and N of example 1 2 The adsorption and desorption curve is also IV type and corresponds to a mesoporous structure, wherein the pore volume is 0.24cm 3 Per gram, specific surface area of 321.26m 2 The specific surface area is reduced, but the average size of the pores is 2.99nm according to the formula, the pores show slight increase, the pore size distribution diagram is mainly 2-10nm, and the pores are correspondingly mesoporous; example 3 adsorption and desorption curves for HC-3 are also of type IV, corresponding to mesoporous structures with pore volume sizes of 0.33cm 3 Ratio of/gSurface area of 391.9m 2 The average pore size per g was also 3.39nm according to the above formula, and was increased again in comparison with the above, and was consistent with the pore size distribution chart in the main distribution range of 2 to 10 nm. BET spectrum analysis proves the pore structure of the composite material, which is of great significance to the analysis of the subsequent material wave absorbing performance.
FIG. 4 shows the reflection loss values of the discontinuous light hollow carbon sphere material prepared in the embodiment above at the frequency of 2.0-18.0GHz at the thickness of 1.0-5.0 mm. The specific method comprises the following steps: paraffin was used with the samples according to 4:1, and pressing into coaxial rings with the inner diameter and the outer diameter of 3.04mm and 7.00mm respectively, and the thickness of about 1.00mm, and simulating and testing the wave absorption performance of samples with different thicknesses by using a vector network analyzer.
As shown in figure 4 a, calcination at 900 ℃ is obtained, the maximum reflection loss value of a HC-1 sample is-22.1 dB when the thickness is 2.0mm, the effective bandwidth is 4.2GHz, and the HC-1 sample has certain wave absorbing performance; when the aperture of the carbon sphere is increased, as shown in fig. 4 b, at a thickness of 1.5mm, the maximum reflection loss value reaches-30.1 dB, the effective bandwidth (reflection loss < -10 dB) reaches 3.2GHz, and the absorption performance (< -10 dB) is provided in a plurality of frequency bands (C, X, ku bands) at different thicknesses. Then, after calcination at high temperature, the reflection loss and bandwidth of HC-3 are reduced, which may be associated with the increased pore size, which results in the porous spheres collapsing easily at high temperature, and the spherical morphology is not maintained effectively (as shown in FIG. 4 c).
The porous honeycomb structure increases reflection and loss sites of electromagnetic waves, realizes multiple reflection and enhances the probability of electromagnetic wave loss; in addition, the formation of a three-dimensional conductive network enhances the conductive loss capacity, and carbon nitrogen derived from dopamine also has the capacity of dipole polarization, and the formed polarization center further dissipates electromagnetic waves.
In summary, thanks to the highly conductive three-dimensional network and the porous hollow structure, the sample achieves the minimum reflection loss of-30.1 dB, and the effective response frequency bands of the sample relate to C (4-8 GHz), X (8-12 GHz) and Ku (12-18 GHz) bands by adjusting the thickness of the test sample, which indicates that the material has broadband response characteristics. Therefore, the discontinuous hollow carbon sphere material can meet the practical application requirements of strong absorption, broadband response and low density, and has great application potential.
Claims (8)
1. The preparation method of the discontinuous light wave-absorbing microsphere is characterized by comprising the following steps of:
(1) Mixing sucrose solution, dopamine hydrochloride solution and sodium chloride, performing ultrasonic dispersion to obtain clear mixed solution, and performing spray drying on the obtained mixed solution to obtain precursor powder;
(2) The precursor powder obtained in the step (1) is added in N 2 Calcining under the atmosphere at 400-500 ℃ for 2h to obtain precursor carbon spheres;
(3) Adding the precursor carbon spheres obtained in the step (2) into deionized water, stirring to remove sodium chloride, filtering, drying, and adding N 2 Calcining again in the atmosphere at 800-900 ℃ for 2h to obtain the discontinuous light wave-absorbing microsphere.
2. The method for producing discontinuous light wave-absorbing microspheres according to claim 1, wherein in step (1), the concentration of the sucrose solution is 5 to 10mg/mL and the concentration of the dopamine hydrochloride solution is 15 to 30mg/mL; the ratio of sucrose solution, dopamine hydrochloride solution and sodium chloride was 50 (mL): 50 (mL): 3 to 5 (g).
3. The method for preparing discontinuous light-weight wave-absorbing microspheres according to claim 1, wherein in step (1), the parameters of spray drying are: the air inlet temperature is 160-180 ℃, the feeding rate is 6-10 mL/min, and the air flow rate is 30-35 m 3 And/h, nozzle size 0.7mm.
4. The method for producing discontinuous light-weight wave-absorbing microspheres according to claim 1, wherein in step (2) or step (3), the temperature rising rate of calcination is 5 ℃/min.
5. The method for preparing discontinuous light wave-absorbing microspheres according to claim 1, wherein in step (3), the ratio of precursor carbon spheres to deionized water is 0.1:0.5 g/L; the time for stirring to remove sodium chloride was 12h.
6. The method for producing discontinuous light-weight wave-absorbing microspheres according to claim 1, wherein the membrane used in the suction filtration in the step (3) is a 0.22 μm aqueous membrane.
7. The discontinuous light-weight wave-absorbing microsphere produced by the production method according to any one of claims 1 to 6.
8. The use of the discontinuous light-weight wave-absorbing microsphere according to claim 7 for the preparation of a microwave absorbing material.
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