CN106563816A - Preparation method of wave absorbing material with nickel nanoparticles wrapped with porous carbon-loaded graphene - Google Patents
Preparation method of wave absorbing material with nickel nanoparticles wrapped with porous carbon-loaded graphene Download PDFInfo
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Abstract
The invention provides a preparation method of a wave absorbing material with nickel nanoparticles wrapped with porous carbon-loaded graphene. The preparation method of the wave absorbing material with the nickel nanoparticles wrapped with the porous carbon-loaded graphene comprises the steps that alga are used as a carbon source and soaked in a nickel saline solution, and nickel ions are made to enter algal cells; low-temperature heat treatment is conducted on the alga after the alga are frozen and dried, so that the alga are converted into carbon, and metallic nickel slat is oxidized into nickel oxide; and then the temperature is increased to continue to conduct high-temperature heat treatment, so that the nickel oxide is reduced into nickel, the amorphous carbon wrapping the nickel nanoparticles is catalyzed and graphitized in the heat treatment process, and finally the composite material with the nickel nanoparticles wrapped with the porous carbon-loaded graphene is obtained. According to the preparation method of the wave absorbing material with the nickel nanoparticles wrapped with the porous carbon-loaded graphene, the alga are used as the carbon source, and thus the preparation method is economical and practical; nickel is evenly dispersed onto a carbon material by means of the characteristic that holes of natural algal plants are abundant; a porous carbon material of a network structure is obtained after heat treatment, the nickel particles wrapped with the graphene are dispersed on the surface of the porous carbon material, and thus the material has excellent micro-wave absorption performance.
Description
Technical field
The invention belongs to nano composite material preparing technical field, is related to a kind of porous carbon load graphene coated nano nickel
The preparation method of granule absorbing material.
Background technology
Nickel nano particle has higher saturation magnetization and pcrmeability due to which, has caused in terms of microwave applications
Enough attention.These materials have high complex permeability, adjustable resonant frequency, low eddy-current loss in microwave range, are expected to into
For high-density recording media, magnetic field sensor or electromagnetic wave absorbent material.But the larger specific surface area of nickel nano particle and higher
Reactivity easily cause reunion and aoxidize, and density is larger, is not suitable for directly application.Graphene is used as a kind of single
Electrical loss material, exclusive use are difficult to make the wide absorbing material of absorption band, using the good adsorptivity of Graphene and super
High specific surface area characteristic, forms nickel nano particle-graphene composite material.This composite not only has Jie of Graphene
Electrical loss, and the magnetic loss with transiting metal nickel, while there is likely to be between Graphene and nickel as nanometer couples effect
The loss that should cause, with light specific gravity, absorption band width, electromagnetic parameter is adjustable and the characteristic such as big is lost, and is a kind of ideal
Absorbing material.
The Chinese invention patent of Application No. 201410759742.2 discloses a kind of preparation of Graphene nickel composite material
Method, the method to be fixed on the grapheme material piece of Ni substrate as carrier, using electrochemical deposition method, method of chemical immersion, electricity
Swimming sedimentation, metallic nickel are deposited on graphenic surface.The Chinese invention patent of Application No. 201510017358.X discloses one
The preparation method of Graphene-nano nickel mesoporous material is planted, the method is that raw material passes through complicated acidifying, pre-oxidation, oxygen with graphite
The processes such as change, heat treatment, by nano nickel particle growth in graphene sheet layer, then by polyaniline-coated in its layer surface system of load
A kind of absorbing material is obtained, a kind of mesoporous material is obtained eventually through high temperature cabonization process.The electroless plating method such as Fang Jianjun is in graphite
Alkene plating nickel on surface come improve its microwave absorption capacity [Journal of Inorganic Materials, 2011,26 (5):467-471];Li Songmei et al. is used
In-situ chemical reducing process prepares the nickel nano particle-graphene composite material of two kinds of different-shapes improving material microwave absorbability
Can [Acta PhySico-Chimica Sinica, 2012,28 (11):2754-2760.];
However, said method prepares graphene/nanometer nickel composite material employs expensive, the complicated graphite of preparation
Alkene is used as raw material so that the relatively costly of composite is difficult to popularization and application.
In view of disadvantages described above, is necessary to provide a kind of simple to operate, low cost in fact, graphene coated nano nickle granules are combined
The preparation method of material.
The content of the invention
In order to overcome the defect of above-mentioned preparation method, it is an object of the invention to provide a kind of porous carbon load Graphene bag
The preparation method of nano nickel compound absorbing material is covered, graphene coated nano nickle granules prepared by the method effectively can be improved
Electro-magnetic wave absorption efficiency, and graded porous structure plays multipath reflection effect to the electromagnetic wave into composite inner, improves
The absorption loss of material, porous carbon load graphene coated nano nickle granules have low cost, lightweight, width as absorbing material
Frequently, efficient advantage.
For achieving the above object, the present invention is to be achieved through the following technical solutions:
A kind of porous carbon loads the preparation method of graphene coated nano nickle granules absorbing material, by with pore structure
Carbon source is immersed in 20~30h in nickel salt solution, is then blended with blender, centrifugal treating, product lyophilization will be centrifuged, to dry
Dry product is heated at 200~250 DEG C makes nickel salt decompose, and then at 300~400 DEG C, heating makes biological material carbon
Change, finally the catalyzed graphitization of carbon is realized in heating at 500~800 DEG C, obtain porous carbon load graphene coated nano nickel
The composite of grain.
The present invention is further improved by, and the natural algae plant is Thallus Porphyrae, Porphyridium cruentum or ulva.
The present invention is further improved by, and the nickel salt solution is nickel nitrate, nickel sulfate or nickel chloride solution.
The present invention is further improved by, and the nickel salt solution concentration is 0.05~0.50mol/L.
The present invention be further improved by, at 200~250 DEG C heat and heat at 300~400 DEG C be
Carry out in vacuum response stove, the time of heating is 30~60min.
The present invention is further improved by, and at 500~800 DEG C, heating is carried out in high temperature process furnances, heating
Time is 30~60min.
The present invention is further improved by, and the heating at 500~800 DEG C is entered under argon or nitrogen atmosphere
OK.
Compared with prior art, the present invention has following beneficial effect:
The present invention uses natural algae as carbon source, and natural algae has abundant pore structure, high specific surface area, tool
There are very strong characterization of adsorption, and algae abundance, low cost, can have in being immersed in the inorganic salt solution of nickel
The absorption nickel ion of effect, by Low Temperature Heat Treatment so that the inorganic salt of nickel is changed into nickel oxide, algal biomass is carbonized;Then
High-temperature heat treatment is carried out, nickel oxide is reduced to the metal nickel particle of nanometer.Nickel oxide is reduced to one side of metallic nickel of nanometer
Face can consume the material with carbon element near nickel oxide particle, and hole is formed in material with carbon element, on the other hand in the shape of metal nickel particle
Cheng Shi, using catalyzed graphitization of the nickel to agraphitic carbon, forms graphene-structured on nickel particle surface, and this method is realized to cladding
In the catalyzed graphitization of the agraphitic carbon on nickel particle surface, and the number of plies of graphene layer can be by controlling to be adjusted heat time heating time
It is whole.The doping of nickel makes to change the degree of graphitization of carbon and porosity, is dispersed in by the nickel particle of graphene coated and is had
On the porous carbon materials of three-dimensional net structure.The porous carbon load graphene coated nano nickle granules absorbing material chi of last gained
Very little little, specific surface area is big, and particle surface relative atom increases, thus, dissipative electromagnetic larger with the area of electromagnetic wave phase interaction
The energy increase of ripple, so as to improve the microwave absorbing property of material, and simple to operate, low cost of the invention on the whole,
It is economic and environment-friendly.
Description of the drawings
Fig. 1 is the XRD figure that porous carbon prepared by the present invention loads graphene coated nano nickle granules absorbing material.
Fig. 2 is the SEM photograph that porous carbon prepared by the present invention loads graphene coated nano nickle granules absorbing material.
Fig. 3 is magnified partial view in Fig. 2.
Fig. 4 is the TEM photos that porous carbon prepared by the present invention loads graphene coated nano nickle granules absorbing material.
Fig. 5 is magnified partial view in Fig. 4.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
Embodiment 1
Step 1:Nickel nitrate solution of the compound concentration for 0.05mol/L, chooses 20g natural algae plants, algae is soaked
The 24h in the nickel nitrate solution prepared.Wherein, natural algae plant is Thallus Porphyrae.
Step 2:Soaked algae is smashed with blender, centrifugation product is taken after centrifugation carries out lyophilization, treats completely
Drying and crushing grinding obtains powdered samples A.
Step 3:Appropriate amount of sample A is weighed, and is placed in vacuum response stove, 30min is heated at 200 DEG C, obtains sample B.
Step 4:Appropriate sample B is weighed, and is placed in vacuum response stove, 30min is heated at 300 DEG C, obtains sample C.
Step 5:Appropriate sample C is weighed, is placed in high temperature process furnances, at 500 DEG C, heat treated under argon 30min is obtained
Graphene coated nano nickle granules absorbing material is loaded to porous carbon.
Resulting porous carbon load graphene coated nano nickle granules absorbing material, nano nickle granules are 10~15nm,
Reflection loss in 2~18GHz frequency ranges is below -15dB.
Embodiment 2
Step 1:Nickel nitrate solution of the compound concentration for 0.05mol/L, chooses 20g natural algae plants, algae is soaked
The 24h in the nickel nitrate solution prepared.Wherein, natural algae plant is Porphyridium cruentum.
Step 2:Soaked algae is smashed with blender, centrifugation product is taken after centrifugation carries out lyophilization, treats completely
Drying and crushing grinding obtains powdered samples A.
Step 3:Appropriate amount of sample A is weighed, and is placed in vacuum response stove, 30min is heated at 200 DEG C, obtains sample B.
Step 4:Appropriate sample B is weighed, and is placed in vacuum response stove, 30min is heated at 350 DEG C, obtains sample C.
Step 5:Appropriate sample C is weighed, is placed in high temperature process furnances, at 500 DEG C, heat treated under argon 30min is obtained
Graphene coated nano nickle granules absorbing material is loaded to porous carbon.
Resulting porous carbon load graphene coated nano nickle granules absorbing material, nano nickle granules are 15nm or so,
Reflection loss in 2~18GHz frequency ranges is below -18dB.
Embodiment 3
Step 1:Nickel nitrate solution of the compound concentration for 0.10mol/L, chooses 20g natural algae plants, algae is soaked
The 24h in the nickel nitrate solution prepared.Wherein, natural algae plant is ulva.
Step 2:Soaked algae is smashed with blender, centrifugation product is taken after centrifugation carries out lyophilization, treats completely
Drying and crushing grinding obtains powdered samples A.
Step 3:Appropriate amount of sample A is weighed, and is placed in vacuum response stove, 30min is heated at 250 DEG C, obtains sample B.
Step 4:Appropriate sample B is weighed, and is placed in vacuum response stove, 30min is heated at 400 DEG C, obtains sample C.
Step 5:Appropriate sample C is weighed, is placed in high temperature process furnances, at 600 DEG C, heat treated under argon 30min is obtained
Graphene coated nano nickle granules absorbing material is loaded to porous carbon.
Resulting porous carbon load graphene coated nano nickle granules absorbing material, nano nickle granules are 20nm or so,
Reflection loss in 2~18GHz frequency ranges is below -21dB.
Embodiment 4
Step 1:Nickel nitrate solution of the compound concentration for 0.20mol/L, chooses 20g natural algae plants, algae is soaked
The 24h in the nickel nitrate solution prepared.Wherein, natural algae plant is Thallus Porphyrae.
Step 2:Soaked algae is smashed with blender, centrifugation product is taken after centrifugation carries out lyophilization, treats completely
Drying and crushing grinding obtains powdered samples A.
Step 3:Appropriate amount of sample A is weighed, and is placed in vacuum response stove, 30min is heated at 250 DEG C, obtains sample B.
Step 4:Appropriate sample B is weighed, and is placed in vacuum response stove, 30min is heated at 400 DEG C, obtains sample C.
Step 5:Appropriate sample C is weighed, is placed in high temperature process furnances, at 700 DEG C, heat treated under argon 60min is obtained
Graphene coated nano nickle granules absorbing material is loaded to porous carbon.
Resulting porous carbon load graphene coated nano nickle granules absorbing material, nano nickle granules are 25nm or so,
Reflection loss in 2~18GHz frequency ranges is below -23dB.
Embodiment 5
Step 1:Nickel nitrate solution of the compound concentration for 0.25mol/L, chooses 20g natural algae plants, algae is soaked
The 24h in the nickel nitrate solution prepared.Wherein, natural algae plant is Thallus Porphyrae.
Step 2:Soaked algae is smashed with blender, centrifugation product is taken after centrifugation carries out lyophilization, treats completely
Drying and crushing grinding obtains powdered samples A.
Step 3:Appropriate amount of sample A is weighed, and is placed in vacuum response stove, 30min is heated at 200 DEG C, obtains sample B.
Step 4:Appropriate sample B is weighed, and is placed in vacuum response stove, 60min is heated at 400 DEG C, obtains sample C.
Step 5:Appropriate sample C is weighed, is placed in high temperature process furnances, at 800 DEG C, heat treated under argon 30min is obtained
Graphene coated nano nickle granules absorbing material is loaded to porous carbon.
Resulting porous carbon load graphene coated nano nickle granules absorbing material, nano nickle granules are 30nm or so,
Reflection loss in 2~18GHz frequency ranges is below -25dB.
Embodiment 6
Step 1:Nickel chloride solution of the compound concentration for 0.5mol/L, chooses 20g natural algae plants, algae is immersed in
30h in the nickel nitrate solution prepared.Wherein, natural algae plant is Thallus Porphyrae.
Step 2:Soaked algae is smashed with blender, centrifugation product is taken after centrifugation carries out lyophilization, treats completely
Drying and crushing grinding obtains powdered samples A.
Step 3:Appropriate amount of sample A is weighed, and is placed in vacuum response stove, 60min is heated at 200 DEG C, obtains sample B.
Step 4:Appropriate sample B is weighed, and is placed in vacuum response stove, 30min is heated at 400 DEG C, obtains sample C.
Step 5:Appropriate sample C is weighed, is placed in high temperature process furnances, at 800 DEG C, 30min is heated under nitrogen atmosphere, obtained
Graphene coated nano nickle granules absorbing material is loaded to porous carbon.
Embodiment 7
Step 1:Nickel sulfate solution of the compound concentration for 0.4mol/L, chooses 20g natural algae plants, algae is immersed in
20h in the nickel nitrate solution prepared.Wherein, natural algae plant is Thallus Porphyrae.
Step 2:Soaked algae is smashed with blender, centrifugation product is taken after centrifugation carries out lyophilization, treats completely
Drying and crushing grinding obtains powdered samples A.
Step 3:Appropriate amount of sample A is weighed, and is placed in vacuum response stove, 30min is heated at 250 DEG C, obtains sample B.
Step 4:Appropriate sample B is weighed, and is placed in vacuum response stove, 60min is heated at 300 DEG C, obtains sample C.
Step 5:Appropriate sample C is weighed, is placed in high temperature process furnances, at 500 DEG C, 60min is heated under nitrogen atmosphere, obtained
Graphene coated nano nickle granules absorbing material is loaded to porous carbon.
Refer to shown in Fig. 1, which is the porous carbon load graphene coated nanometer by prepared by the inventive method embodiment 1
The XRD spectrum of nickel particle absorbing material.As seen from Figure 1:Porous carbon load graphene coated nano nickel prepared by the present invention
Granule absorbing material contains carbon and nickel diffraction maximum.
Refer to shown in Fig. 2 and Fig. 3, which is the porous carbon load Graphene bag by prepared by the inventive method embodiment 1
Cover scanning electron microscope (SEM) picture of nano nickle granules absorbing material.Can be seen that by Fig. 2 and Fig. 3:The network-like knot of material with carbon element
Structure, nickel particle are evenly distributed on porous carbon materials surface.
Refer to shown in Fig. 4 and Fig. 5, which is the porous carbon load Graphene bag by prepared by the inventive method embodiment 1
Cover transmission electron microscope (TEM) picture of nano nickle granules absorbing material.Can be seen that by Fig. 4 and Fig. 5:The surface of nickel particle is by graphite
Alkene is coated.
The invention has the advantages that:Using natural algae as carbon source, natural algae has abundant pore structure, high
Specific surface area, with very strong characterization of adsorption, and algae abundance, it is economical and practical.It is immersed in the inorganic of nickel
Nickel ion can effectively be adsorbed in saline solution, by Low Temperature Heat Treatment so that the inorganic salt of nickel is changed into nickel oxide, algae life
Material is carbonized;Then high-temperature heat treatment is carried out, nickel oxide is reduced to the metal nickel particle of nanometer.Nickel oxide is reduced to receive
On the one hand the metallic nickel of rice can consume the material with carbon element near nickel oxide particle, form hole, on the other hand exist in material with carbon element
During the formation of metal nickel particle, using catalyzed graphitization of the nickel to agraphitic carbon, graphene-structured is formed on nickel particle surface, it is real
Existing cladding of the Graphene to nano nickle granules.The generation method of Graphene is simple, easy to operate.The doping of nickel makes the graphitization journey of carbon
Degree, porosity are all changed, are obtained by the nickel particle of graphene coated after carbonized graphite, are dispersed in and tie with three-dimensional network
On the porous carbon materials surface of structure, the porous carbon load graphene coated nano nickle granules absorbing material size of last gained is little,
Specific surface area is big, and particle surface relative atom increases, thus, the energy of dissipative electromagnetic ripple larger with the area of electromagnetic wave phase interaction
Amount increase, so as to improve the microwave absorbing property of material on the whole.
Claims (7)
1. a kind of porous carbon loads the preparation method of graphene coated nano nickle granules absorbing material, it is characterised in that:To have
The carbon source of pore structure is immersed in 20~30h in nickel salt solution, is then blended with blender, centrifugal treating, product will be centrifuged cold
Lyophilizing is dry, and desciccate is heated at 200~250 DEG C makes nickel salt decompose, and then at 300~400 DEG C, heating makes life
Material is carbonized, and finally at 500~800 DEG C, the catalyzed graphitization of carbon is realized in heating, obtains porous carbon load Graphene bag
Cover the composite of nano nickle granules.
2. a kind of porous carbon according to claim 1 loads the preparation side of graphene coated nano nickle granules absorbing material
Method, it is characterised in that:The natural algae plant is Thallus Porphyrae, Porphyridium cruentum or ulva.
3. a kind of porous carbon according to claim 1 loads the preparation side of graphene coated nano nickle granules absorbing material
Method, it is characterised in that:The nickel salt solution is nickel nitrate, nickel sulfate or nickel chloride solution.
4. a kind of porous carbon according to claim 1 or 3 loads the preparation of graphene coated nano nickle granules absorbing material
Method, it is characterised in that:The nickel salt solution concentration is 0.05~0.50mol/L.
5. a kind of porous carbon according to claim 1 loads the preparation side of graphene coated nano nickle granules absorbing material
Method, it is characterised in that:It is to carry out in vacuum response stove at 200~250 DEG C to heat and heats at 300~400 DEG C,
The time of heating is 30~60min.
6. a kind of porous carbon according to claim 1 loads the preparation side of graphene coated nano nickle granules absorbing material
Method, it is characterised in that:At 500~800 DEG C, heating is carried out in high temperature process furnances, and the time of heating is 30~60min.
7. a kind of porous carbon according to claim 1 loads the preparation side of graphene coated nano nickle granules absorbing material
Method, it is characterised in that:The heating at 500~800 DEG C is carried out under argon or nitrogen atmosphere.
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