CN117840429A - Carbon micrometer sheet loaded nickel particle composite wave-absorbing material and preparation method thereof - Google Patents
Carbon micrometer sheet loaded nickel particle composite wave-absorbing material and preparation method thereof Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 133
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 121
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 113
- 239000002131 composite material Substances 0.000 title claims abstract description 59
- 239000011358 absorbing material Substances 0.000 title claims abstract description 58
- 239000002245 particle Substances 0.000 title claims abstract description 55
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000002028 Biomass Substances 0.000 claims abstract description 45
- 239000002105 nanoparticle Substances 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 65
- 150000002815 nickel Chemical class 0.000 claims description 33
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 32
- 238000001816 cooling Methods 0.000 claims description 25
- 238000000137 annealing Methods 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 23
- 238000001035 drying Methods 0.000 claims description 23
- 229910052757 nitrogen Inorganic materials 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000002184 metal Substances 0.000 abstract description 12
- 229910052751 metal Inorganic materials 0.000 abstract description 12
- 230000007246 mechanism Effects 0.000 abstract description 4
- 230000009471 action Effects 0.000 abstract description 3
- 230000005672 electromagnetic field Effects 0.000 abstract description 3
- 230000010287 polarization Effects 0.000 abstract description 3
- 230000001105 regulatory effect Effects 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 19
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 13
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 13
- 238000009656 pre-carbonization Methods 0.000 description 9
- 230000008569 process Effects 0.000 description 9
- 238000012360 testing method Methods 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 6
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 5
- 240000008042 Zea mays Species 0.000 description 5
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 5
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 5
- 239000003575 carbonaceous material Substances 0.000 description 5
- 235000005822 corn Nutrition 0.000 description 5
- 229910001453 nickel ion Inorganic materials 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 description 4
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 4
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 4
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 4
- ZVHHIDVFSYXCEW-UHFFFAOYSA-L nickel(ii) nitrite Chemical compound [Ni+2].[O-]N=O.[O-]N=O ZVHHIDVFSYXCEW-UHFFFAOYSA-L 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000012188 paraffin wax Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 244000137852 Petrea volubilis Species 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000002134 carbon nanofiber Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Abstract
The invention discloses a carbon micron sheet loaded nickel particle composite wave-absorbing material and a preparation method thereof, and relates to the technical field of composite wave-absorbing materials; in order to solve the defect problem of the electromagnetic wave absorbing material in the prior art; specifically comprises carbon micrometer sheets and nickel particles, wherein the carbon micrometer sheets are biomass corncob derivatives; the nickel particles are attached to the surface of the carbon micro-sheet to form a heterostructure; the composite wave-absorbing material is CMs/Ni; the carbon micro-sheet is of a two-dimensional sheet structure; the nickel particles are nano-sized. According to the composite wave-absorbing material, the dielectric constant of the carbon micro-sheet is regulated after the metal nickel particles are loaded, so that good impedance matching characteristics can be obtained, and under the action of an alternating electromagnetic field, a large number of heterogeneous interfaces exist between the carbon micro-sheet and the metal nickel particles to enhance interface polarization, so that more electromagnetic waves are lost, and the technical problems of poor impedance matching and single loss mechanism of the electromagnetic wave-absorbing material in the prior art are solved.
Description
Technical Field
The invention relates to the technical field of composite wave-absorbing materials, in particular to a carbon micrometer sheet loaded nickel particle composite wave-absorbing material and a preparation method thereof.
Background
With the rapid development of electromagnetic technology, various electronic devices and wireless equipment are widely applied to civil and military fields, however, the problem of electromagnetic wave pollution is increasingly serious, and potential threats are caused to the physical health of people and the safe operation of the electronic equipment. In recent years, an electromagnetic wave absorbing material has been attracting attention because it can convert electromagnetic waves into heat energy or other forms of energy, and reduce adverse effects of excessive electromagnetic waves on human bodies and electronic devices. Therefore, research on efficient and environment-friendly electromagnetic wave absorbing materials has important significance for protecting the physical health of people and the safe operation of electronic equipment.
At present, carbon materials such as carbon nanotubes, carbon nanofibers, graphene and the like are attracting attention as electromagnetic wave absorbing materials due to their excellent electronic, mechanical and thermal properties, but their complex preparation process and poor dispersibility have limited their development. Among various carbon materials, biomass-derived carbon has the characteristics of reproducibility, environmental protection and abundant resources, and meanwhile, has a unique structure, abundant surface functional groups and high specific surface area, and has great potential in the field of electromagnetic wave absorption. However, carbon materials have common disadvantages, such as high dielectric constants, which can lead to impedance mismatch of the biomass carbon material, large amounts of electromagnetic waves being reflected from the material surface rather than absorbed, and furthermore, the loss mechanism of a single carbon material is single. Based on the above, we provide a carbon micro-sheet loaded nickel particle composite wave-absorbing material and a preparation method thereof.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a carbon micrometer sheet loaded nickel particle composite wave-absorbing material and a preparation method thereof.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the composite wave-absorbing material comprises carbon micrometer sheets and nickel particles, wherein the carbon micrometer sheets are biomass corncob derivatives;
the nickel particles are attached to the surface of the carbon micro-sheet to form a heterostructure;
the composite wave-absorbing material is CMs/Ni.
Preferably: the carbon micro-sheet is of a two-dimensional sheet structure.
Preferably: the nickel particles are nano-sized.
Preferably: the preparation method of the composite wave-absorbing material comprises the following steps:
s1: pre-treating biomass corncob, crushing, and then placing the crushed biomass corncob into a tube furnace for annealing treatment to obtain carbon micro-sheets;
s2: adding the carbon micro-sheet into a nickel salt-containing solution, stirring and mixing, drying, and cooling to obtain a nickel salt-loaded carbon micro-sheet;
s3: and (3) placing the carbon micro-sheet loaded with the nickel salt into a graphite boat, adopting a joule heating device to perform joule heating treatment under the protection of nitrogen, and obtaining the composite wave-absorbing material CMs/Ni of the nickel particles loaded with the raw carbon micro-sheet after the temperature is cooled to the room temperature.
Preferably: the content of the preprocessing comprises the following contents:
a1: washing and centrifuging biomass corncobs by sequentially using deionized water and absolute ethyl alcohol;
a2: the cleaned biomass corncob is vacuum dried and pre-carbonized under nitrogen protection.
Preferably: in the step S1, the annealing temperature is 700-900 ℃, the annealing time is 2-5 h, and the heating and cooling rates of the annealing treatment are 5 ℃/min.
Preferably: in the S2, the addition amount of the carbon micro-sheet is 50-300 mg.
Preferably: in the step S2, the solution is absolute ethyl alcohol;
the dosage of the nickel salt is 0.5-2 mmol, and the dosage of the absolute ethyl alcohol is 5-10 mL.
Preferably: in the step S2, the drying temperature is 60-90 ℃, and the drying time is 8-12 h.
Preferably: in the step S3, the temperature of the Joule heat treatment is 1000-1500 ℃, and the heat treatment time is 10-30S.
The beneficial effects of the invention are as follows:
1. according to the composite wave-absorbing material, the dielectric constant of the carbon micro-sheet is regulated after the metal nickel particles are loaded, so that good impedance matching characteristics can be obtained, and under the action of an alternating electromagnetic field, a large number of heterogeneous interfaces exist between the carbon micro-sheet and the metal nickel particles to enhance interface polarization, so that more electromagnetic waves are lost, and the technical problems of poor impedance matching and single loss mechanism of the electromagnetic wave-absorbing material in the prior art are solved.
2. According to the preparation method, biomass corn cob is crushed and then subjected to pre-carbonization treatment to obtain biomass derivative carbon micro-sheets, then the carbon micro-sheets are soaked in an absolute ethanol solution containing nickel chloride and mixed, then the drying treatment is carried out, finally the obtained nickel salt-loaded carbon micro-sheets are subjected to Joule heating treatment, nickel ions are reduced by the carbon micro-sheets in the ultra-fast heating and cooling processes of Joule heating, and finally the carbon micro-sheet-loaded metal nickel particle composite material CMs/Ni is obtained, and the preparation process is efficient and easy to popularize.
3. The carbon micro sheet with the sheet-shaped structure prepared by the invention can lead incident electromagnetic waves to be reflected and scattered for multiple times and further be dissipated; experiments prove that the CMs/Ni composite wave-absorbing material has good electromagnetic wave absorptivity.
Drawings
FIG. 1 is a schematic flow chart of a preparation method of a carbon micro-sheet loaded nickel particle composite wave-absorbing material;
FIG. 2 is an XRD pattern of CMs/Ni composite wave-absorbing material in test example 1 of a method for preparing a carbon micro-sheet loaded nickel particle composite wave-absorbing material according to the present invention;
FIG. 3 is an SEM image of the CMS/Ni composite wave-absorbing material in test example 2 of a preparation method of a carbon micro-sheet loaded nickel particle composite wave-absorbing material according to the present invention;
fig. 4 is an electromagnetic wave absorption performance diagram of the CMs/Ni composite wave absorbing material in test example 3 of a preparation method of a carbon micro-sheet loaded nickel particle composite wave absorbing material according to the present invention.
Detailed Description
The technical scheme of the patent is further described in detail below with reference to the specific embodiments.
Embodiments of the present patent are described in detail below, examples of which are illustrated in the accompanying drawings, wherein the same or similar reference numerals refer to the same or similar elements or elements having the same or similar functions throughout. The embodiments described below by referring to the drawings are exemplary only for explaining the present patent and are not to be construed as limiting the present patent.
Example 1:
the composite wave-absorbing material is shown in figure 1, is CMs (Carbon micrometer sheet)/Ni and comprises carbon micrometer sheets and nickel particles, wherein the carbon micrometer sheets are biomass corncob derivatives;
further, the nickel particles are attached to the surface of the carbon microchip to form a heterostructure, which can form a large number of heterogeneous interfaces.
Preferably, the carbon micro-sheet is a two-dimensional sheet structure.
Further, the nickel particles are nano-sized; the metal nano nickel particles are uniformly distributed on the surface of the carbon micro-sheet.
The composite wave-absorbing material can be applied to the field of electromagnetic wave absorption; the magnetic nickel particles provide a magnetic loss mechanism for the composite material for electromagnetic wave loss, so that the composite wave absorbing material has excellent electromagnetic wave absorbing performance.
When the embodiment is used, the prepared sheet-like structure carbon micro sheet can enable incident electromagnetic waves to be reflected and scattered for multiple times and further be dissipated; in addition, the dielectric constant of the carbon micro-sheet is regulated after the metal nickel particles are loaded, so that good impedance matching characteristics can be obtained, and under the action of an alternating electromagnetic field, a large number of heterogeneous interfaces exist between the carbon micro-sheet and the metal nickel particles to enhance interface polarization, so that more electromagnetic waves are lost.
Example 2:
a preparation method of a carbon micro-sheet loaded nickel particle composite wave-absorbing material is shown in figure 1; the method comprises the following steps:
s1: 10g of biomass corncob is pretreated and crushed for 5min, and then is put into a tube furnace for annealing treatment under the protection of nitrogen to obtain carbon micro-sheets;
preferably, the pre-processed content includes the following:
a1: washing biomass corncobs with 100ml of deionized water for 10min, and centrifuging for 5min at 4000 r/min;
a1: washing biomass corncobs with 100ml of absolute ethanol for 10min, and centrifuging for 5min at 4000 r/min; to wash out impurities therein.
A2: the cleaned biomass corncob is dried in vacuum for 12 hours at 80 ℃ and is subjected to pre-carbonization treatment in nitrogen atmosphere.
Preferably, the crushing device can be a wall breaking machine and the like.
Preferably, the annealing temperature is 800 ℃, the annealing time is 2 hours, and the heating and cooling rates of the annealing treatment are 5 ℃/min.
S2: adding the carbon micro-sheets into a nickel salt-containing solution, magnetically stirring for 10min, mixing into a uniform solution, drying, and cooling to obtain nickel salt-loaded carbon micro-sheets;
preferably, the carbon micro-sheet is added in an amount of 0.1g.
Preferably, the solution is absolute ethanol.
Preferably, the nickel salt is one of nickel chloride, nickel sulfate, nickel nitrite, nickel hydroxide, etc., and in this example, nickel chloride, especially nickel chloride hexahydrate, is preferred;
further preferably, the nickel salt is used in an amount of 0.5mmol and the absolute ethanol is used in an amount of 10mL;
still more preferably, the drying temperature is 90℃and the drying time is 10 hours.
S3: placing the carbon micro-sheet loaded with nickel salt in a graphite boat, adopting a joule heating device to perform joule heating treatment under the protection of nitrogen, and obtaining a composite wave-absorbing material CMs/Ni of biomass-derived carbon micro-sheet loaded nickel particles after cooling to room temperature; the joule heating equipment chamber is purged with high purity nitrogen to create an oxygen free environment.
Preferably, the temperature of the joule heating treatment is 1200 ℃, and the time of the heating treatment is 20s. The joule heat treatment can realize ultra-fast heating and cooling processes, so that the preparation time is greatly shortened, sample preparation can be completed in tens of seconds, and the joule heat treatment can easily realize a high-temperature environment, and is more efficient compared with the traditional heating mode.
When the method is used, biomass corn cob is crushed and then subjected to pre-carbonization treatment to obtain biomass derivative carbon micro-sheets, then the carbon micro-sheets are soaked in an absolute ethanol solution containing nickel chloride and mixed, then the drying treatment is carried out, finally the obtained nickel salt-loaded carbon micro-sheets are subjected to Joule heating treatment, nickel ions are reduced by the carbon micro-sheets in the ultra-fast heating and cooling process of Joule heating, and finally the carbon micro-sheet-loaded metal nickel particle composite CMs/Ni is obtained.
Example 3:
a preparation method of a carbon micro-sheet loaded nickel particle composite wave-absorbing material is shown in figure 1; the method comprises the following steps:
s1: 10g of biomass corncob is pretreated and crushed for 5min, and then is put into a tube furnace for annealing treatment under the protection of nitrogen to obtain carbon micro-sheets;
preferably, the pre-processed content includes the following:
a1: washing biomass corncobs with 100ml of deionized water for 10min, and centrifuging for 5min at 4000 r/min;
a1: washing biomass corncobs with 100ml of absolute ethanol for 10min, and centrifuging for 5min at 4000 r/min; to wash out impurities therein.
A2: the cleaned biomass corncob is dried in vacuum for 12 hours at 80 ℃ and is subjected to pre-carbonization treatment in nitrogen atmosphere.
Preferably, the crushing device can be a wall breaking machine and the like.
Preferably, the annealing temperature is 800 ℃, the annealing time is 2 hours, and the heating and cooling rates of the annealing treatment are 5 ℃/min.
S2: adding the carbon micro-sheets into a nickel salt-containing solution, magnetically stirring for 10min, mixing into a uniform solution, drying, and cooling to obtain nickel salt-loaded carbon micro-sheets;
preferably, the carbon micro-sheet is added in an amount of 0.1g.
Preferably, the solution is absolute ethanol.
Preferably, the nickel salt is one of nickel chloride, nickel sulfate, nickel nitrite, nickel hydroxide, etc., and in this example, nickel chloride, especially nickel chloride hexahydrate, is preferred;
further preferably, the nickel salt is used in an amount of 1mmol and the absolute ethanol is used in an amount of 10mL;
still more preferably, the drying temperature is 90℃and the drying time is 10 hours.
S3: placing the carbon micro-sheet loaded with nickel salt in a graphite boat, adopting a joule heating device to perform joule heating treatment under the protection of nitrogen, and obtaining a composite wave-absorbing material CMs/Ni of biomass-derived carbon micro-sheet loaded nickel particles after cooling to room temperature; the joule heating equipment chamber is purged with high purity nitrogen to create an oxygen free environment.
Preferably, the temperature of the joule heating treatment is 1200 ℃, and the time of the heating treatment is 20s. The joule heat treatment can realize ultra-fast heating and cooling processes, so that the preparation time is greatly shortened, sample preparation can be completed in tens of seconds, and the joule heat treatment can easily realize a high-temperature environment, and is more efficient compared with the traditional heating mode.
When the method is used, biomass corn cob is crushed and then subjected to pre-carbonization treatment to obtain biomass derivative carbon micro-sheets, then the carbon micro-sheets are soaked in an absolute ethanol solution containing nickel chloride and mixed, then the drying treatment is carried out, finally the obtained nickel salt-loaded carbon micro-sheets are subjected to Joule heating treatment, nickel ions are reduced by the carbon micro-sheets in the ultra-fast heating and cooling process of Joule heating, and finally the carbon micro-sheet-loaded metal nickel particle composite CMs/Ni is obtained.
Example 4:
a preparation method of a carbon micro-sheet loaded nickel particle composite wave-absorbing material is shown in figure 1; the method comprises the following steps:
s1: 10g of biomass corncob is pretreated and crushed for 5min, and then is put into a tube furnace for annealing treatment under the protection of nitrogen to obtain carbon micro-sheets;
preferably, the pre-processed content includes the following:
a1: washing biomass corncobs with 100ml of deionized water for 10min, and centrifuging for 5min at 4000 r/min;
a1: washing biomass corncobs with 100ml of absolute ethanol for 10min, and centrifuging for 5min at 4000 r/min; to wash out impurities therein.
A2: the cleaned biomass corncob is dried in vacuum for 12 hours at 80 ℃ and is subjected to pre-carbonization treatment in nitrogen atmosphere.
Preferably, the crushing device can be a wall breaking machine and the like.
Preferably, the annealing temperature is 800 ℃, the annealing time is 2 hours, and the heating and cooling rates of the annealing treatment are 5 ℃/min.
S2: adding the carbon micro-sheets into a nickel salt-containing solution, magnetically stirring for 10min, mixing into a uniform solution, drying, and cooling to obtain nickel salt-loaded carbon micro-sheets;
preferably, the carbon micro-sheet is added in an amount of 0.1g.
Preferably, the solution is absolute ethanol.
Preferably, the nickel salt is one of nickel chloride, nickel sulfate, nickel nitrite, nickel hydroxide, etc., and in this example, nickel chloride, especially nickel chloride hexahydrate, is preferred;
further preferably, the nickel salt is used in an amount of 1.5mmol and the absolute ethanol is used in an amount of 10mL;
still more preferably, the drying temperature is 90℃and the drying time is 10 hours.
S3: placing the carbon micro-sheet loaded with nickel salt in a graphite boat, adopting a joule heating device to perform joule heating treatment under the protection of nitrogen, and obtaining a composite wave-absorbing material CMs/Ni of biomass-derived carbon micro-sheet loaded nickel particles after cooling to room temperature; the joule heating equipment chamber is purged with high purity nitrogen to create an oxygen free environment.
Preferably, the temperature of the joule heating treatment is 1200 ℃, and the time of the heating treatment is 20s. The joule heat treatment can realize ultra-fast heating and cooling processes, so that the preparation time is greatly shortened, sample preparation can be completed in tens of seconds, and the joule heat treatment can easily realize a high-temperature environment, and is more efficient compared with the traditional heating mode.
When the method is used, biomass corn cob is crushed and then subjected to pre-carbonization treatment to obtain biomass derivative carbon micro-sheets, then the carbon micro-sheets are soaked in an absolute ethanol solution containing nickel chloride and mixed, then the drying treatment is carried out, finally the obtained nickel salt-loaded carbon micro-sheets are subjected to Joule heating treatment, nickel ions are reduced by the carbon micro-sheets in the ultra-fast heating and cooling process of Joule heating, and finally the carbon micro-sheet-loaded metal nickel particle composite CMs/Ni is obtained.
Example 5:
a preparation method of a carbon micro-sheet loaded nickel particle composite wave-absorbing material is shown in figure 1; the method comprises the following steps:
s1: 10g of biomass corncob is pretreated and crushed for 5min, and then is put into a tube furnace for annealing treatment under the protection of nitrogen to obtain carbon micro-sheets;
preferably, the pre-processed content includes the following:
a1: washing biomass corncobs with 100ml of deionized water for 10min, and centrifuging for 5min at 4000 r/min;
a1: washing biomass corncobs with 100ml of absolute ethanol for 10min, and centrifuging for 5min at 4000 r/min; to wash out impurities therein.
A2: the cleaned biomass corncob is dried in vacuum for 12 hours at 80 ℃ and is subjected to pre-carbonization treatment in nitrogen atmosphere.
Preferably, the crushing device can be a wall breaking machine and the like.
Preferably, the annealing temperature is 800 ℃, the annealing time is 2 hours, and the heating and cooling rates of the annealing treatment are 5 ℃/min.
S2: adding the carbon micro-sheets into a nickel salt-containing solution, magnetically stirring for 10min, mixing into a uniform solution, drying, and cooling to obtain nickel salt-loaded carbon micro-sheets;
preferably, the carbon micro-sheet is added in an amount of 0.1g.
Preferably, the solution is absolute ethanol.
Preferably, the nickel salt is one of nickel chloride, nickel sulfate, nickel nitrite, nickel hydroxide, etc., and in this example, nickel chloride, especially nickel chloride hexahydrate, is preferred;
further preferably, the nickel salt is used in an amount of 2mmol and the absolute ethanol is used in an amount of 10mL;
still more preferably, the drying temperature is 90℃and the drying time is 10 hours.
S3: placing the carbon micro-sheet loaded with nickel salt in a graphite boat, adopting a joule heating device to perform joule heating treatment under the protection of nitrogen, and obtaining a composite wave-absorbing material CMs/Ni of biomass-derived carbon micro-sheet loaded nickel particles after cooling to room temperature; the joule heating equipment chamber is purged with high purity nitrogen to create an oxygen free environment.
Preferably, the temperature of the joule heating treatment is 1200 ℃, and the time of the heating treatment is 20s. The joule heat treatment can realize ultra-fast heating and cooling processes, so that the preparation time is greatly shortened, sample preparation can be completed in tens of seconds, and the joule heat treatment can easily realize a high-temperature environment, and is more efficient compared with the traditional heating mode.
When the method is used, biomass corn cob is crushed and then subjected to pre-carbonization treatment to obtain biomass derivative carbon micro-sheets, then the carbon micro-sheets are soaked in an absolute ethanol solution containing nickel chloride and mixed, then the drying treatment is carried out, finally the obtained nickel salt-loaded carbon micro-sheets are subjected to Joule heating treatment, nickel ions are reduced by the carbon micro-sheets in the ultra-fast heating and cooling process of Joule heating, and finally the carbon micro-sheet-loaded metal nickel particle composite CMs/Ni is obtained.
Test example 1:
taking example 3 as an example, XRD analysis was performed on the phase of the obtained CMs/Ni composite wave-absorbing material, the XRD diffraction pattern of which is shown in FIG. 2, and it can be seen from the diffraction peaks in the XRD pattern that the composite wave-absorbing material consists of carbon and metallic nickel.
Test example 2:
taking example 3 as an example, SEM observation of the morphology of the obtained CMs/Ni composite wave-absorbing material shows that the SEM image is shown in fig. 3, and it can be seen that the surface of the carbon microchip is loaded with nano particles.
Test example 3:
taking example 3 as an example, the electromagnetic wave absorption performance of the obtained CMs/Ni composite wave absorbing material was tested, and the electromagnetic wave absorption performance results are shown in FIG. 4.
In the test example, electromagnetic parameters are obtained by using a vector network analyzer, and the specific operation method is as follows:
(1) uniformly mixing paraffin (90 wt%) with the prepared biomass-derived carbon micrometer sheet-loaded nickel particle composite material (10 wt%) and placing the mixture in a 70 ℃ oven for heat preservation for 10min to completely melt the paraffin, placing the sample into a self-made stainless steel die after the paraffin is solidified to prepare a sample to be detected with the inner diameter of 3.04mm and the outer diameter of 7mm, and polishing the sample by sand paper with different types to finally prepare a concentric ring sample with the diameter of 2 mm;
(2) electromagnetic parameters of the sample in the frequency range of 2-18GHz are tested by using a vector network analyzer (AV 3656D), and simulation calculation is carried out according to the transmission line theory.
The results show that: the maximum reflection loss of the CMs/Ni composite wave absorbing material can reach-42.8 dB when the corresponding frequency is 6.96GHz under the thickness of 4.0mm, and the maximum effective absorption frequency bandwidth (the reflection loss is less than-10 dB) under the single thickness can reach 5.2GHz.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (10)
1. The composite wave-absorbing material comprises carbon micrometer sheets and nickel particles, and is characterized in that the carbon micrometer sheets are biomass corncob derivatives;
the nickel particles are attached to the surface of the carbon micro-sheet to form a heterostructure;
the composite wave-absorbing material is CMs/Ni.
2. The carbon micro sheet supported nickel particle composite wave absorbing material according to claim 1, wherein the carbon micro sheet is a two-dimensional sheet structure.
3. The carbon microchip-supported nickel particle composite wave absorbing material as defined by claim 2, wherein the nickel particles are nano-sized.
4. The carbon microchip-supported nickel particle composite wave-absorbing material as defined in claim 1, wherein the preparation method of the composite wave-absorbing material comprises the following steps:
s1: pre-treating biomass corncob, crushing, and then placing the crushed biomass corncob into a tube furnace for annealing treatment to obtain carbon micro-sheets;
s2: adding the carbon micro-sheet into a nickel salt-containing solution, stirring and mixing, drying, and cooling to obtain a nickel salt-loaded carbon micro-sheet;
s3: and (3) placing the carbon micro-sheet loaded with the nickel salt into a graphite boat, adopting a joule heating device to perform joule heating treatment under the protection of nitrogen, and obtaining the composite wave-absorbing material CMs/Ni of the nickel particles loaded with the raw carbon micro-sheet after the temperature is cooled to the room temperature.
5. The carbon microchip-loaded nickel particle composite wave-absorbing material as defined by claim 4, wherein the content of the pretreatment comprises the following content:
a1: washing and centrifuging biomass corncobs by sequentially using deionized water and absolute ethyl alcohol;
a2: the cleaned biomass corncob is vacuum dried and pre-carbonized under nitrogen protection.
6. The carbon micro sheet supported nickel particle composite wave-absorbing material according to claim 5, wherein in the step S1, the annealing temperature is 700-900 ℃, the annealing time is 2-5 h, and the heating and cooling rates of the annealing treatment are 5 ℃/min.
7. The carbon-micron-sheet-loaded nickel particle composite wave-absorbing material according to claim 6, wherein in the S2, the adding amount of the carbon micron sheet is 50-300 mg.
8. The carbon microchip-loaded nickel particle composite wave-absorbing material as defined by claim 7, wherein in S2, the solution is absolute ethanol;
the dosage of the nickel salt is 0.5-2 mmol, and the dosage of the absolute ethyl alcohol is 5-10 mL.
9. The carbon micro-sheet supported nickel particle composite wave-absorbing material according to claim 8, wherein in the step S2, the drying temperature is 60-90 ℃ and the drying time is 8-12 h.
10. The carbon micro sheet supported nickel particle composite wave-absorbing material according to claim 9, wherein in the step S3, the temperature of the joule heating treatment is 1000-1500 ℃, and the time of the heating treatment is 10-30S.
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