CN110577820B - Porous structure Ni/NiO-C composite material and preparation method and application thereof - Google Patents
Porous structure Ni/NiO-C composite material and preparation method and application thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 47
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 18
- 238000001354 calcination Methods 0.000 claims abstract description 13
- 239000000047 product Substances 0.000 claims abstract description 13
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004202 carbamide Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011246 composite particle Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 239000002244 precipitate Substances 0.000 claims abstract description 10
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 9
- 239000008103 glucose Substances 0.000 claims abstract description 9
- 239000002243 precursor Substances 0.000 claims abstract description 9
- 150000002815 nickel Chemical class 0.000 claims abstract description 8
- 239000012298 atmosphere Substances 0.000 claims abstract description 4
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 230000001681 protective effect Effects 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 9
- 239000011358 absorbing material Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 238000010521 absorption reaction Methods 0.000 abstract description 15
- 239000000463 material Substances 0.000 abstract description 7
- 239000000523 sample Substances 0.000 description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000002033 PVDF binder Substances 0.000 description 6
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 238000003917 TEM image Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000005415 magnetization Effects 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 241000080590 Niso Species 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 150000001868 cobalt Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 241000656145 Thyrsites atun Species 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000007040 multi-step synthesis reaction Methods 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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Abstract
The invention belongs to the technical field of electromagnetic wave absorption materials, and discloses a Ni/NiO-C composite material with a porous structure, and a preparation method and application thereof. The composite material consists of carbon spheres and Ni/NiO composite particles attached to the surfaces of the carbon spheres, wherein micropores are distributed on the surfaces of the carbon spheres, and the Ni/NiO composite particles are in flower-shaped configurations. The preparation method comprises the following steps: adding glucose, water-soluble nickel salt and urea into water, and uniformly stirring; controlling the temperature of the obtained solution to be 170-190 ℃, standing, and carrying out hydrothermal reaction for 15-18 h; after the hydrothermal reaction is finished, taking out the precipitate in the hydrothermal reaction, and cleaning and drying the precipitate to obtain a precursor; and (3) calcining the precursor for 2 to 3 hours at the temperature of 400 to 800 ℃ under the inert or protective atmosphere to obtain a calcined product, namely the Ni/NiO-C composite material with the porous structure. The prepared Ni/NiO-C composite material has better electromagnetic wave absorption characteristic, and can be widely applied to the corresponding electromagnetic protection and microwave stealth fields as an electromagnetic wave absorption material.
Description
Technical Field
The invention belongs to the technical field of electromagnetic wave absorption materials, and particularly relates to a Ni/NiO-C composite material with a porous structure, and a preparation method and application thereof.
Background
Over the past few decades, the rapid development of telecommunications, digital industry and electronics has resulted in excessive electromagnetic radiation. Electromagnetic interference is classified as a pollution of human living space, and becomes an important concern for physical health, biological systems, information security, and normal operation of electronic devices. Therefore, some advanced level and high efficiency of electromagnetic wave absorbing materials must be developed to eliminate the problems of electromagnetic hazard and electromagnetic interference. The efficiency of electromagnetic absorption depends primarily on the inherent electromagnetic properties of the microwave absorbing material. Among the myriad of microwave absorbing materials, carbonaceous microwave absorbers have shown many advantages, including chemical stability, adjustable chemical and physical properties, and the like. It is reported that various nanocarbons such as carbon fibers, carbon nanotubes, carbon nanocoils, carbon nanowires, carbon spheres, graphene, reduced graphene oxide, and the like have been successfully prepared, and corresponding microwave absorption properties have been studied. However, carbon materials alone, which have relatively high electrical conductivity and dielectric loss, are detrimental to impedance matching and often result in microwave reflection at the surface rather than absorption, on the basis of impedance matching.
The soft magnetic metal Ni is more attractive for electromagnetic wave absorption because it has relatively high magnetization compared to oxides, and is relatively stable compared to the easy oxidation of iron and cobalt. The high saturation magnetization of the magnetic metal results in a high Snoek limit and permeability in the high frequency region, which results in strong magnetic losses. However, metallic Ni always has a high density and is easily oxidized, which not only increases the weight of the electromagnetic wave absorption film but also causes a decrease in magnetization. Therefore, carbon composites with protected magnetic metal Ni are expected to be an effective way to improve impedance matching and oxidation resistance.
Disclosure of Invention
The invention aims to provide a porous structure Ni/NiO-C composite material and a preparation method and application thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the porous Ni/NiO-C composite material consists of carbon spheres and Ni/NiO composite particles attached to the surfaces of the carbon spheres, wherein micropores are distributed on the surfaces of the carbon spheres, and the Ni/NiO composite particles are in a flower-shaped configuration.
The preparation method comprises the following steps:
(1) Adding glucose, water-soluble nickel salt and urea into water, and uniformly stirring; wherein, calculated by the molar-volume ratio, the water-soluble cobalt salt is calculated by nickel actually provided by the water-soluble cobalt salt, and glucose, the water-soluble nickel salt, urea and water are respectively (5 to 25) mmol, (1~5) mmol, (5 to 30) mmol, and (20 to 200) mL;
(2) Controlling the temperature of the solution obtained in the step (1) to be 170-190 ℃, standing, and carrying out hydrothermal reaction for 15-18 h;
(3) After the hydrothermal reaction is finished, taking out a precipitate in the hydrothermal reaction, and cleaning and drying the precipitate to obtain a precursor;
(4) And (3) controlling the temperature of the precursor obtained in the step (3) to be 400-800 ℃ and calcining for 2-3 h under an inert or protective atmosphere to obtain a calcined product, namely the porous structure Ni/NiO-C composite material.
Preferably, in step (1), glucose is added to water, and then the water-soluble nickel salt and urea are sequentially added.
Preferably, in the step (3), the washing is performed several times by using distilled water and several times by using absolute ethyl alcohol.
Preferably, in the step (3), the drying temperature is 50 to 60 ℃ and the drying time is 8 to 12 hours.
Preferably, in the step (4), the temperature is raised to the calcination temperature at a temperature rise rate of 5 to 10 ℃/min.
The porous structure Ni/NiO-C composite material is applied as an electromagnetic wave absorption material.
Has the advantages that:
(1) Firstly, preparing a precursor through simple and clean hydrothermal reaction, and then calcining in an inert atmosphere to obtain the Ni/NiO-C composite material with the porous structure, so that the problem that the conventional nano composite material needs a multi-step synthesis process is avoided, and meanwhile, the prepared porous structure Ni/NiO-C composite material has the advantages of strong wave absorption capacity and small density;
(2) The Ni/NiO-C composite material with the porous structure prepared by the invention contains more functional groups such as C-O, O-C = O, ni-O and the like and a large number of defects, and the functional groups and the defects are used as polarization centers in an electromagnetic field and can effectively lose electromagnetic waves; meanwhile, the Ni/NiO nano-particles have larger specific surface area and more concentrated micropore distribution, and play an important role in improving the electromagnetic wave absorption active sites and the electron transfer efficiency; in addition, the Ni/NiO-C composite material contains multiple non-uniform interfaces, including C-air, C-Ni and C-NiO, can generate strong interface polarization, and the prepared Ni/NiO-C composite material has better electromagnetic wave absorption property and can be widely applied to the corresponding electromagnetic protection and microwave stealth fields as an electromagnetic wave absorption material.
Drawings
FIG. 1: XRD pattern of N-800 sample.
FIG. 2: SEM image of N-800 sample.
FIG. 3: TEM image and line scan results for N-800 sample: a TEM image, (b) a high-angle annular dark field image (HAADF) image, and (c) a line scanning result of a straight line in (b).
FIG. 4: XRD pattern of the control sample.
FIG. 5: SEM image of comparative sample.
FIG. 6: when the thickness of the wave-absorbing layer is 3.6 mm, the reflection loss of four Ni/NiO-C/PVDF-based composite materials with the sample content of 2 wt percent is shown as follows: n-400 samples, N-500 samples, N-600 samples and N-800 samples.
Detailed Description
The following examples are given only for the purpose of illustrating the present invention in further detail, and are not to be construed as limiting the invention in any way; the materials used in the following examples were obtained from conventional chemical agents companies and raw material suppliers, unless otherwise specified.
Example 1
A preparation method of a porous structure Ni/NiO-C composite material comprises the following steps:
(1) 15 mmol of glucose and 2 mmol of NiSO were weighed using an analytical balance 4 ·6H 2 O, 10 mmol urea;
(2) Measuring 60 mL deionized water and putting the deionized water into a glass beaker;
(3) Glucose was slowly added to the glass beaker first, then NiSO was slowly added in sequence 4 ·6H 2 O, urea, and magnetically stirring 1 h;
(4) Transferring the uniformly mixed solution from the glass beaker to a polytetrafluoroethylene high-pressure reaction kettle, and then reacting in a drying oven at 190 ℃ for 15 h;
(5) After the reaction is finished, taking out the black precipitate from the reaction kettle, repeatedly washing the black precipitate with distilled water for three times, repeatedly washing the black precipitate with absolute ethyl alcohol for three times, and drying the black precipitate in a drying oven at 60 ℃ for 9 h to obtain a precursor;
(6) Putting the obtained precursor into a small porcelain boat in a tubular furnace in nitrogen atmosphere, heating to the calcining temperature of 400 ℃ at the heating rate of 5 ℃/min, preserving the temperature of 2 h, and marking the obtained calcined product as an N-400 sample.
Example 2
The difference from example 1 is that: the calcination temperature in the step (6) is changed to 500 ℃, and the obtained calcination product is marked as an N-500 sample; otherwise, the same procedure as in example 1 was repeated.
Example 3
The difference from example 1 is that: the calcination temperature in the step (6) is changed to 600 ℃, and the obtained calcination product is marked as an N-600 sample; otherwise, the same procedure as in example 1 was repeated.
Example 4
The difference from example 1 is that: the calcination temperature in the step (6) is changed to 800 ℃, and the obtained calcination product is marked as an N-800 sample; otherwise, the same procedure as in example 1 was repeated.
FIG. 1 is an XRD pattern of the N-800 sample. As can be seen from fig. 1: the product obtained by the invention only contains Ni, niO and C, and no other impurity peaks appear.
FIG. 2 is an SEM image of an N-800 sample. FIG. 3 is a TEM image of an N-800 sample and the results of a line scan. As can be seen from fig. 2 and 3: the composite material of the product obtained by the invention is composed of carbon spheres and Ni/NiO composite particles attached to the surfaces of the carbon spheres, micropores are distributed on the surfaces of the carbon spheres, and the Ni/NiO composite particles are in a flower-shaped configuration, wherein the size of the carbon spheres is 1-6 micrometers, the pore size of the micropores is 2-12 nm, and the size of the Ni/NiO composite particles is 0.2-1.2 micrometers. The formation of micropores is attributed to the formation of Ni/NiO composite particles and the consumption of carbon material during carbon heat treatment. Because the obtained product has a porous structure, the product has the characteristics of low density and high specific surface area.
Comparative example
The difference from example 4 is that: the procedure is as in example 4 except that no urea is added.
The XRD pattern and SEM pattern of the product obtained in this comparative example are shown in FIGS. 4 and 5, respectively. The XRD pattern showed: the sample without adding urea is displayed by a PDF card and is not matched with Ni and NiO crystallization peaks, which shows that the required product cannot be obtained without adding urea; meanwhile, SEM pictures show that the sample has different shapes and sizes, and is seriously agglomerated and fused, ni/NiO composite particles cannot be observed, and a porous structure is not shown.
Electromagnetic absorption characteristic test
Respectively weighing the N-400 sample, the N-500 sample, the N-600 sample and the N-800 sample obtained in the examples 1-4 according to the mass ratio of the samples to PVDF = 2: 98, dissolving PVDF in DMF, uniformly mixing the samples with a DMF solution of PVDF, and drying the mixture to be in a solid state, thereby obtaining the Ni/NiO-C/PVDF-based composite material with the mass ratio of 2 wt%. The reflection loss of the Ni/NiO-C/PVDF-based composite material was calculated by Matlab software, and the results are shown in FIG. 6, which shows that: the sample calcined at 800 deg.C under nitrogen (N-800) had a minimum RL value of-34.7 dB at 5.8 GHz when the thickness of the absorbing layer was 3.6 mm.
Claims (7)
1. A porous structure Ni/NiO-C composite material is characterized in that: the composite material consists of carbon spheres and Ni/NiO composite particles attached to the surfaces of the carbon spheres, micropores are distributed on the surfaces of the carbon spheres, and the Ni/NiO composite particles are in a flower-shaped configuration.
2. A preparation method of a porous structure Ni/NiO-C composite material is characterized by comprising the following steps:
(1) Adding glucose, water-soluble nickel salt and urea into water, and uniformly stirring; wherein, calculated by the mol-volume ratio, the water-soluble nickel salt is calculated by the nickel actually provided, and glucose, the water-soluble nickel salt, urea and water are =15 mmol, 2 mmol, 10 mmol, 60 mL;
(2) Controlling the temperature of the solution obtained in the step (1) to be 180 ℃, standing for hydrothermal reaction 15 h;
(3) After the hydrothermal reaction is finished, taking out the precipitate in the hydrothermal reaction, and cleaning and drying the precipitate to obtain a precursor;
(4) And (3) calcining the precursor obtained in the step (3) at 800 ℃ for 2 h under inert or protective atmosphere to obtain a calcined product, namely the porous structure Ni/NiO-C composite material.
3. The method of preparing a porous structured Ni/NiO-C composite according to claim 2, wherein: in the step (1), glucose is added into water, and then water-soluble nickel salt and urea are sequentially added.
4. The method of preparing a porous structured Ni/NiO-C composite according to claim 2, wherein: in the step (3), the cleaning is carried out for several times by using distilled water and then by using absolute ethyl alcohol.
5. The method of preparing a porous structured Ni/NiO-C composite according to claim 2, wherein: in the step (3), the drying temperature is 50 to 60 ℃, and the drying time is 8 to 12 hours.
6. The method of preparing a porous Ni/NiO-C composite according to claim 2, wherein: in the step (4), the temperature is increased to the calcining temperature at the temperature increase rate of 5 to 10 ℃/min.
7. Use of the porous structured Ni/NiO-C composite material according to claim 1 as an electromagnetic wave absorbing material.
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| CN111244424B (en) * | 2020-01-19 | 2020-12-22 | 杭州电子科技大学 | Preparation method of sericin carbon film coated Ni/NiO microsphere composite material |
| CN111333127B (en) * | 2020-03-05 | 2021-04-23 | 西北工业大学 | Hierarchical porous honeycomb nickel oxide microsphere and preparation method thereof |
| CN111935968B (en) * | 2020-08-21 | 2021-08-27 | 山东大学 | Preparation method of iron/nitrogen/carbon composite material |
| CN112397697A (en) * | 2020-11-16 | 2021-02-23 | 河北零点新能源科技有限公司 | Preparation method of flower-shaped nickel oxide/carbon composite material |
| CN112707383B (en) * | 2020-12-31 | 2022-08-23 | 中国海洋大学 | Flower-shaped Ni/C composite material with carbon nanowires and preparation method thereof |
| CN112752496B (en) * | 2021-01-15 | 2022-01-14 | 西北工业大学 | Hollow nitrogen-doped nickel oxide/nickel/carbon composite material, preparation method and application |
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