CN106563816B - A kind of preparation method of porous carbon load graphene coated nano nickle granules absorbing material - Google Patents
A kind of preparation method of porous carbon load graphene coated nano nickle granules absorbing material Download PDFInfo
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Abstract
A kind of preparation method of porous carbon load graphene coated nano nickle granules absorbing material is immersed in using algae as carbon source in the salting liquid of nickel, and nickel ion is made to enter alga cells.Low Temperature Heat Treatment is carried out after freeze-drying to it, algae is changed into carbon, and nickel salts are oxidized to nickel oxide；Then it increases temperature and continues high-temperature heat treatment, nickel oxide is made to be reduced into nickel, and realize that the agraphitic carbon for being coated on nano nickel particles by catalyzed graphitization, finally obtains the composite material of porous carbon load graphene coated nano nickle granules during heat treatment.The present invention is economical and practical using algae as carbon source, keeps nickel evenly dispersed on the carbon material using the abundant feature of natural algae plant hole；The porous carbon materials with network structure are obtained after heat treatment, porous carbon materials surface is dispersed in by the nickel particle of graphene coated so that the excellent microwave absorbing property that material has.
Description
Technical field
The invention belongs to nanocomposite preparing technical fields, are related to a kind of porous carbon load graphene coated nano nickel
The preparation method of particle absorbing material.
Background technology
Nickel nano particle has caused since it is with higher saturation magnetization and magnetic conductivity 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 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 oxidation, and density is larger, is not suitable for directly application.Graphene is as a kind of single
Electrical loss material, exclusive use are difficult to that the wide absorbing material of absorption band is made, and using the good adsorptivity of graphene and surpass
High specific surface area characteristic forms nickel nano particle-graphene composite material.This composite material not only has Jie of graphene
Electrical loss, and with transiting metal nickel magnetic loss, while there is likely to be between graphene and nickel since nanometer couples effect
Caused loss is answered, there is light specific gravity, absorption band is wide, electromagnetic parameter is adjustable and the characteristics such as big are lost, be a kind of ideal
Absorbing material.
Application No. is 201410759742.2 Chinese invention patents to disclose a kind of preparation of graphene nickel composite material
Method, this method is 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 graphene surface.Application No. is the Chinese invention patents of 201510017358.X to disclose one
The preparation method of kind graphene-nano nickel mesoporous material, this method pass through complicated acidification, pre-oxidation, oxygen by raw material of 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, is handled eventually by high temperature cabonization and a kind of mesoporous material is made.Fang Jianjun etc. is with electroless plating method in graphite
Alkene plating nickel on surface improves 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 nickel nano particle-graphene composite material of two kinds of different-shapes to improve material microwave absorbability
It can [Acta PhySico-Chimica Sinica, 2012,28 (11):2754-2760.]；
It has been all made of expensive however, the above method prepares graphene/nanometer nickel composite material, has prepared complicated graphite
Alkene is as raw material so that the cost of composite material is more high-leveled and difficult to promote and apply.
In view of disadvantages described above, a kind of easy to operate it is really necessary to provide, at low cost, graphene coated nano nickle granules are compound
The preparation method of material.
Invention content
In order to overcome the defect of above-mentioned preparation method, the purpose of the present invention is to provide a kind of porous carbons to load graphene packet
The preparation method of nano nickel compound absorbing material is covered, graphene coated nano nickle granules prepared by this method can be improved effectively
Electro-magnetic wave absorption efficiency, and graded porous structure plays multipath reflection to the electromagnetic wave for entering composite inner, improves
The absorption loss of material, porous carbon loads graphene coated nano nickle granules has at low cost, lightweight, width as absorbing material
Frequently, efficient advantage.
To achieve the above object, the present invention is to be achieved through the following technical solutions：
A kind of preparation method of porous carbon load graphene coated nano nickle granules absorbing material, will be with pore structure
Carbon source is immersed in 20~30h in nickel salt solution, is then blended with blender, centrifugal treating, by centrifugation product freeze-drying, to dry
Dry product heats at 200~250 DEG C makes nickel salt decompose, and then heating makes biological material carbon at 300~400 DEG C
Change, the catalyzed graphitization for realizing carbon is finally heated at 500~800 DEG C, obtains porous carbon load graphene coated nano nickel
The composite material of grain.
The present invention, which further improves, to be, the natural algae plant is seaweed, purple ball algae or sea lettuce.
The present invention, which further improves, to be, the nickel salt solution is nickel nitrate, nickel sulfate or nickel chloride solution.
The present invention, which further improves, to be, a concentration of 0.05~0.50mol/L of nickel salt solution.
The present invention further improve is, at 200~250 DEG C heat and heated at 300~400 DEG C be
It is carried out in vacuum reaction stove, the time of heating is 30~60min.
The present invention, which further improves, to be, heating is carried out in high temperature process furnances at 500~800 DEG C, heating
Time is 30~60min.
The present invention further improve is, it is described at 500~800 DEG C heating be under argon gas or nitrogen atmosphere into
Row.
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, at low cost, being immersed in the inorganic salt solution of nickel can have
The absorption nickel ion of effect, by Low Temperature Heat Treatment so that the inorganic salts of nickel are 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 carbon material near nickel oxide particle, and hole is formed in carbon material, on the other hand in the shape of metal nickel particle
Cheng Shi forms graphene-structured, this method is realized to cladding using nickel to the catalyzed graphitization of agraphitic carbon on nickel particle surface
It can be adjusted by controlling heating time in the number of plies of the catalyzed graphitization of the agraphitic carbon on nickel particle surface, and graphene layer
It is whole.The doping of nickel makes the degree of graphitization for changing carbon and porosity, and being dispersed in by the nickel particle of graphene coated has
On the porous carbon materials of three-dimensional net structure.The porous carbon of last gained loads graphene coated nano nickle granules absorbing material ruler
Very little small, large specific surface area, particle surface relative atom increases, thus, dissipative electromagnetic larger with the area of electromagnetic wave phase interaction
The energy of wave increases, and to improve the microwave absorbing property of material on the whole, and the present invention is easy to operate, at low cost,
It is economic and environment-friendly.
Description of the drawings
Fig. 1 is the XRD diagram of porous carbon load graphene coated nano nickle granules absorbing material prepared by the present invention.
Fig. 2 is the SEM photograph of porous carbon load graphene coated nano nickle granules absorbing material prepared by the present invention.
Fig. 3 is magnified partial view in Fig. 2.
Fig. 4 is the TEM photos of porous carbon load graphene coated nano nickle granules absorbing material prepared by the present invention.
Fig. 5 is magnified partial view in Fig. 4.
Specific implementation mode
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：Compound concentration is the nickel nitrate solution of 0.05mol/L, chooses 20g natural algae plants, algae is impregnated
In prepared nickel nitrate solution for 24 hours.Wherein, natural algae plant is seaweed.
Step 2：Soaked algae is smashed with blender, takes centrifugation product to be freeze-dried after centrifugation, waits for completely
Drying and crushing grinds to obtain powdered samples A.
Step 3：Appropriate amount of sample A is weighed, is placed in vacuum reaction stove, 30min is heated at 200 DEG C, obtains sample B.
Step 4：Suitable sample B is weighed, is placed in vacuum reaction stove, 30min is heated at 300 DEG C, obtains sample C.
Step 5：Suitable 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.
Obtained porous carbon loads graphene coated nano nickle granules absorbing material, and nano nickle granules are 10~15nm,
Reflection loss in 2~18GHz frequency ranges is below -15dB.
Embodiment 2
Step 1：Compound concentration is the nickel nitrate solution of 0.05mol/L, chooses 20g natural algae plants, algae is impregnated
In prepared nickel nitrate solution for 24 hours.Wherein, natural algae plant is purple ball algae.
Step 2：Soaked algae is smashed with blender, takes centrifugation product to be freeze-dried after centrifugation, waits for completely
Drying and crushing grinds to obtain powdered samples A.
Step 3：Appropriate amount of sample A is weighed, is placed in vacuum reaction stove, 30min is heated at 200 DEG C, obtains sample B.
Step 4：Suitable sample B is weighed, is placed in vacuum reaction stove, 30min is heated at 350 DEG C, obtains sample C.
Step 5：Suitable 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.
Obtained porous carbon loads graphene coated nano nickle granules absorbing material, and nano nickle granules are 15nm or so,
Reflection loss in 2~18GHz frequency ranges is below -18dB.
Embodiment 3
Step 1：Compound concentration is the nickel nitrate solution of 0.10mol/L, chooses 20g natural algae plants, algae is impregnated
In prepared nickel nitrate solution for 24 hours.Wherein, natural algae plant is sea lettuce.
Step 2：Soaked algae is smashed with blender, takes centrifugation product to be freeze-dried after centrifugation, waits for completely
Drying and crushing grinds to obtain powdered samples A.
Step 3：Appropriate amount of sample A is weighed, is placed in vacuum reaction stove, 30min is heated at 250 DEG C, obtains sample B.
Step 4：Suitable sample B is weighed, is placed in vacuum reaction stove, 30min is heated at 400 DEG C, obtains sample C.
Step 5：Suitable 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.
Obtained porous carbon loads graphene coated nano nickle granules absorbing material, and nano nickle granules are 20nm or so,
Reflection loss in 2~18GHz frequency ranges is below -21dB.
Embodiment 4
Step 1：Compound concentration is the nickel nitrate solution of 0.20mol/L, chooses 20g natural algae plants, algae is impregnated
In prepared nickel nitrate solution for 24 hours.Wherein, natural algae plant is seaweed.
Step 2：Soaked algae is smashed with blender, takes centrifugation product to be freeze-dried after centrifugation, waits for completely
Drying and crushing grinds to obtain powdered samples A.
Step 3：Appropriate amount of sample A is weighed, is placed in vacuum reaction stove, 30min is heated at 250 DEG C, obtains sample B.
Step 4：Suitable sample B is weighed, is placed in vacuum reaction stove, 30min is heated at 400 DEG C, obtains sample C.
Step 5：Suitable 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.
Obtained porous carbon loads graphene coated nano nickle granules absorbing material, and nano nickle granules are 25nm or so,
Reflection loss in 2~18GHz frequency ranges is below -23dB.
Embodiment 5
Step 1：Compound concentration is the nickel nitrate solution of 0.25mol/L, chooses 20g natural algae plants, algae is impregnated
In prepared nickel nitrate solution for 24 hours.Wherein, natural algae plant is seaweed.
Step 2：Soaked algae is smashed with blender, takes centrifugation product to be freeze-dried after centrifugation, waits for completely
Drying and crushing grinds to obtain powdered samples A.
Step 3：Appropriate amount of sample A is weighed, is placed in vacuum reaction stove, 30min is heated at 200 DEG C, obtains sample B.
Step 4：Suitable sample B is weighed, is placed in vacuum reaction stove, 60min is heated at 400 DEG C, obtains sample C.
Step 5：Suitable 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.
Obtained porous carbon loads graphene coated nano nickle granules absorbing material, and nano nickle granules are 30nm or so,
Reflection loss in 2~18GHz frequency ranges is below -25dB.
Embodiment 6
Step 1：Compound concentration is the nickel chloride solution of 0.5mol/L, chooses 20g natural algae plants, algae is immersed in
30h in prepared nickel nitrate solution.Wherein, natural algae plant is seaweed.
Step 2：Soaked algae is smashed with blender, takes centrifugation product to be freeze-dried after centrifugation, waits for completely
Drying and crushing grinds to obtain powdered samples A.
Step 3：Appropriate amount of sample A is weighed, is placed in vacuum reaction stove, 60min is heated at 200 DEG C, obtains sample B.
Step 4：Suitable sample B is weighed, is placed in vacuum reaction stove, 30min is heated at 400 DEG C, obtains sample C.
Step 5：Suitable sample C is weighed, is placed in high temperature process furnances, 30min is heated under 800 DEG C, nitrogen atmosphere, obtains
Graphene coated nano nickle granules absorbing material is loaded to porous carbon.
Embodiment 7
Step 1：Compound concentration is the nickel sulfate solution of 0.4mol/L, chooses 20g natural algae plants, algae is immersed in
20h in prepared nickel nitrate solution.Wherein, natural algae plant is seaweed.
Step 2：Soaked algae is smashed with blender, takes centrifugation product to be freeze-dried after centrifugation, waits for completely
Drying and crushing grinds to obtain powdered samples A.
Step 3：Appropriate amount of sample A is weighed, is placed in vacuum reaction stove, 30min is heated at 250 DEG C, obtains sample B.
Step 4：Suitable sample B is weighed, is placed in vacuum reaction stove, 60min is heated at 300 DEG C, obtains sample C.
Step 5：Suitable sample C is weighed, is placed in high temperature process furnances, 60min is heated under 500 DEG C, nitrogen atmosphere, obtains
Graphene coated nano nickle granules absorbing material is loaded to porous carbon.
It please refers to shown in Fig. 1, is that graphene coated nanometer is loaded by the porous carbon prepared by the method for the present invention embodiment 1
The XRD spectrum of nickel particle absorbing material.As seen from Figure 1：Porous carbon prepared by the present invention loads graphene coated nano nickel
Particle absorbing material contains carbon and nickel diffraction maximum.
Please refer to is to load graphene packet by the porous carbon prepared by the method for the present invention embodiment 1 shown in Fig. 2 and Fig. 3
Cover scanning electron microscope (SEM) picture of nano nickle granules absorbing material.It can be seen that by Fig. 2 and Fig. 3：The network-like knot of carbon material
Structure, nickel particle are evenly distributed on porous carbon materials surface.
Please refer to is to load graphene packet by the porous carbon prepared by the method for the present invention embodiment 1 shown in Fig. 4 and Fig. 5
Cover transmission electron microscope (TEM) picture of nano nickle granules absorbing material.It 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 has very strong characterization of adsorption, and algae abundance, economical and practical.It is immersed in the inorganic of nickel
Nickel ion can be effectively adsorbed in salting liquid, by Low Temperature Heat Treatment so that the inorganic salts of nickel are changed into nickel oxide, algae life
Substance 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 carbon material near nickel oxide particle, form hole in carbon material, on the other hand exist
When the formation of metal nickel particle, using nickel to the catalyzed graphitization of agraphitic carbon, graphene-structured is formed on nickel particle surface, it is real
Cladding of the existing 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, obtain, by the nickel particle of graphene coated, being dispersed in three-dimensional network knot after carbonized graphite
On the porous carbon materials surface of structure, the porous carbon load graphene coated nano nickle granules absorbing material size of last gained is small,
Large specific surface area, particle surface relative atom increases, thus, the energy of dissipative electromagnetic wave larger with the area of electromagnetic wave phase interaction
Amount increases, to improve the microwave absorbing property of material on the whole.
Claims (3)
1. a kind of preparation method of porous carbon load 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, and centrifugal treating is cold by product is centrifuged
It is lyophilized dry, being heated at 200~250 DEG C to desciccate makes nickel salt decompose, and then heating makes life at 300~400 DEG C
Material is carbonized, and the catalyzed graphitization for realizing carbon is finally heated at 500~800 DEG C, obtains porous carbon load graphene packet
Cover the composite material of nano nickle granules；
Heating is carried out in high temperature process furnances at 500~800 DEG C, and the time of heating is 30~60min；
The heating at 500~800 DEG C is carried out under argon gas or nitrogen atmosphere；
The carbon source with pore structure is seaweed, purple ball algae or sea lettuce；
A concentration of 0.05~the 0.50mol/L of nickel salt solution.
2. a kind of preparation side of porous carbon load graphene coated nano nickle granules absorbing material according to claim 1
Method, it is characterised in that：The nickel salt solution is nickel nitrate, nickel sulfate or nickel chloride solution.
3. a kind of preparation side of porous carbon load graphene coated nano nickle granules absorbing material according to claim 1
Method, it is characterised in that：Heating and heated at 300~400 DEG C at 200~250 DEG C is carried out in vacuum reaction stove,
The time of heating is 30~60min.
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| CN102218349B (en) * | 2011-04-02 | 2013-05-15 | 中山大学 | Method for one-step localization for synthesizing nanometer carbide-graphitized carbon composite material |
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