A kind of porous carbon load nano nickel absorbing material and preparation method thereof
Technical field
The present invention relates to a kind of porous carbon load nano nickel absorbing materials and preparation method thereof, belong to microwave absorbing material neck
Domain.
Background technique
With the fast development of electronic science and technology and electronic electric equipment, wireless communication system, radar stealth technology
It is commonly used, electromagnetic pollution and interference problem become increasingly severe, so that the research of electro-magnetic wave absorption material is by increasingly
More concerns.Absorbing material is whether also more and more extensive in civilian or military use, wants to the performance of absorbing material
Ask also higher and higher.Other than having required higher uptake, also require that material thickness is thin as far as possible, quality is as light as possible, absorbs
Frequency band is as wide as possible.The study found that the complex dielectric permittivity of wave absorbing agent, complex permeability and electromagnetic impedance match have codetermined its
Electromagnetic performance, individual dielectric loss material and magnetic loss consumption material are extremely difficult to electromagnetic impedance match.It therefore, include magnetic components
Compound absorbing material with dielectric composites is at research hotspot in recent years, because these materials can be effectively combined magnetism
The magnetic loss of material and the dielectric loss of dielectric material are conducive to the microwave absorption capacity for improving material, and meet absorbing material
Synthesis requirement.
In recent years, extensive pass of the carbon material due to its excellent dielectric properties and low-density by absorbing material researcher
Note.Magnetic Nano material and carbon material are combined, not only the magnetic materials such as ferrite, magnetic metal, alloy can be overcome close
Big defect is spent, and electromagnetic matching can be improved, realizes electro-magnetic wave absorption more more excellent than single absorbing material.Currently,
Preparing carbon material used in magnetic material/carbon composite wave-suction material is mainly carbon fiber, carbon nanotube and graphene etc., by magnetic
Property material and the compound method of carbon material mainly include chemical vapor deposition, chemical plating, plating and atomic layer deposition etc..However,
Existing process is difficult to realize the low cost of these materials and prepared by high yield, and raw material is cheap, process is simple, environmentally protective
And the higher preparation method of yield is the key that carbon microwave receptor material development and application.
Cotton has extensive planting range in China, low in cost.In addition, it is cellulose that cotton main component, which is, about
98 wt% of gross weight are accounted for, it is considerably less containing inorganic impurity.In a vacuum or inert atmosphere, cotton fiber wood substance component (cellulose, half
Cellulose and lignin) in a series of reaction, such as dehydration, degradation, dehydrogenation, carbonization, organic molecule gradually depolymerization can occur
As small molecule.Some volatile gas, such as CO2、 H2O、 CH4Deng gradually generation and major part releases, and finally only stays
Under porous amorphous carbon, but the overall structure of vegetable material is not destroyed, it can fully be carried over.In addition, grinding
Study carefully discovery, porous structure, which has electro-magnetic wave absorption, to be significantly affected, and the improvement of this microwave absorption property is mainly derived from electromagnetism
Reflection and scattering of the wave in porous media.Therefore, on the one hand porous structure has the advantage of lightweight, on the other hand shows as dielectric
Constant real part becomes smaller and increase is lost, and not only improves absorbing material impedance matching, and facilitates energy loss and adjust material
Electromagnetic parameter.
The magnetic conductivity of nano nickel particles is higher, and dielectric constant is larger, can by nano nickel particles load capacity and
The controllable preparation of granularity adjusts the electromagnetic parameter of C-base composte material, this feature is conducive to broaden the frequency band of wave absorbing agent.Separately
Outside, absorbent cotton is very fluffy, and surface hydrophilicity is good, is conducive to the load of metal salt.It is contemplated that choosing absorbent cotton is carbon
Source retains the original one-dimensional porous structure of cotton fiber using chemically and physically method, and various by the assembling of modulation process condition
Required nano nickel magnetic components, can preparation structure and material dual effect electromagnet absorbing material.This can not only overcome
The shortcomings that carbon fiber is as microwave absorbing material widens the application range of biological material, and can be carbon-based absorbing material
It develops and new thinking and approach is provided.
Summary of the invention
The present invention is intended to provide a kind of porous carbon load nano nickel absorbing material and preparation method thereof.
The present invention is catalyzed the carbon nano-structured nickel salt presoma for being formed, being grown using absorbent cotton as carbon source, by introducing to have,
The concentration of nickel salt and the temperature and time of thermal decomposition are controlled, nano nickel/porous carbon of different-grain diameter and nickel loading is prepared
Composite material, and this material is applied to field of microwave absorption, it is provided to obtain cheap, lightweight, efficient microwave absorbing material
Theoretical foundation and experimental basis.
The present invention provides a kind of porous carbons to load nano nickel absorbing material, using absorbent cotton as carbon source, passes through dipping and carbon
The method combined is heat-treated, partial size and the adjustable nano nickel particles of load capacity are loaded on porous carbon, obtains porous carbon load
Nano nickel absorbing material.
Carbon source used in the present invention is medical absorbent cotton, and nano nickel particles derive from nickel salt, and used nickel salt is nitre
Sour nickel or nickel sulfate, nickel nitrate include nickel nitrate and its hydrate (Ni (NO3)2Or Ni (NO3)2·6H2O);Nickel sulfate includes
Nickel sulfate and its hydrate (NiSO4、NiSO4·6H2O or NiSO4·7H2O).The ratio of the two are as follows: 0.01-100 g absorbent cotton
It is dissolved in the nickel salt solution of 0.0001 mol/L -2 mol/L, guarantees that absorbent cotton is totally submerged in the solution.
The present invention provides the preparation methods of above-mentioned porous carbon load nano nickel absorbing material, comprising the following steps:
Step 1, absorbent cotton load nickel salt:
0.01-100 g absorbent cotton is added in the nickel salt solution of 0.0001mol/L-2 mol/L, guarantees absorbent cotton submergence
In the solution, the absorbent cotton that load has nickel salt is taken out after impregnating 12-48 h, after excluding extra solution, wet absorbent cotton is 40-
80 oIt is dry at a temperature of C;
Step 2 loads nano nickel on porous carbon:
By product obtained by step 1 400-1000oC, N2 Or 1-4 h is roasted under inert atmosphere protection, heating speed
Rate is 1-10 oC/ min obtains the product of uniform load nano nickel on porous carbon.
Further, the dip time in step 1 is 24-48h, and the load capacity of nano nickel is with nickel salt in products obtained therefrom
The increase of solution concentration and increase, highest load capacity can reach 85 wt%.
In the above method, used protective atmosphere is N2Or one of He, Ar inert atmosphere.
In the above method, according to the difference of maturing temperature and time, the partial size of nano nickle granules is 2-200 in products obtained therefrom
nm。
In the above method, nano nickel is evenly dispersed on porous carbon, according to the negative of the structure of porous carbon and nano nickel
The difference of carrying capacity and partial size, the reflection loss peak of composite material are smaller than -50 dB, -10 dB of reflection loss absorption below
Bandwidth may be up to 5 GHz.
Beneficial effects of the present invention:
(1) raw material used in method of the invention be absorbent cotton and nickel salt, it is cheap and easy to get;
(2) method of the invention uses infusion process and high-temperature roasting method, and process is simple, and product yield is higher, synthesis cost
It is low;
(3) nano nickel is evenly dispersed on porous carbon, and in conjunction with very close, and the load capacity of nano nickel and partial size can
It adjusts;
(4) according to the difference of the load capacity and partial size of the structure of porous carbon and nano nickel, the microwave absorption of composite material
Performance is adjustable;
(5) porous structure and electromagnetic matching of porous carbon load nano nickel absorbing material, makes the microwave-absorbing of material
It can be excellent.
Detailed description of the invention
Fig. 1 is the technological process block-diagram that porous carbon loads nano nickel;
Fig. 2 is the scanning electron microscope (SEM) photograph that 1 gained porous carbon of embodiment loads nano nickel;
Fig. 3 is the transmission electron microscope picture that 1 gained porous carbon of embodiment loads nano nickel;
Fig. 4 is the reflection loss figure that 1 gained porous carbon of embodiment loads nano nickel;
Fig. 5 is the reflection loss figure that 2 gained porous carbon of embodiment loads nano nickel.
Specific embodiment
The present invention is further illustrated below by embodiment, but is not limited to following embodiment.
The present invention provides the preparation method of porous carbon load nano nickel absorbing material, embodiment 1 is shown in process flow, with de-
Rouge cotton is carbon source, and the method by impregnating and carbon thermal reduction combines loads partial size and the adjustable nickel of load capacity on porous carbon
Nano particle obtains porous carbon load nano nickel absorbing material.
Embodiment 1:
A kind of preparation method of porous carbon load nano nickel absorbing material, which is characterized in that its step are as follows:
Step 1, absorbent cotton load nickel nitrate
4 g of extracting degreasing cotton is immersed in the Ni (NO of 100 ml, 0.5 mol/L3)2·6H2In O solution, taken after impregnating 24 h
Absorbent cotton and extra solution is squeezed out out, wet absorbent cotton is 60oDry 24 h under C.
Step 2 loads nano nickel on porous carbon
By product obtained by step 1 in tube furnace N2700 under atmosphere protectionoC roasts 2 h, i.e., on porous carbon
Nano nickel is loaded, calculates and learns that the load capacity of nano nickel is 33 wt%.
Fig. 2 is the scanning electron microscope (SEM) photograph that embodiment 1 gained porous carbon loads nano nickel, as can be seen from the figure porous carbon
Cellular structure is high-visible, and all loads with surface inside duct and have Ni nano particle.
Fig. 3 is the transmission electron microscope picture that 1 gained porous carbon of embodiment loads nano nickel, as can be seen from the figure nanometer Nickel particle
20-60 nm of diameter.
The microwave absorbing property of porous carbon load nano nickel absorbing material, reflection damage are evaluated using network vector analyzer
Consumption, which is equal to -10 dB, means that 90% microwave is absorbed, frequency range when effective bandwidth represents reflection loss less than -10 dB
Width.Reflection loss, which is equal to -20 dB, means that 99% microwave is absorbed.Reflection loss, which is equal to -30 dB, means 99.9%
Microwave is absorbed.
Fig. 4 is the reflection loss figure that 1 gained porous carbon of embodiment loads nano nickel, and as can be seen from the figure porous carbon is negative
The reflection loss peak for carrying nano nickel absorbing material is -30.7 dB, and -10 dB of reflection loss Absorber Bandwidth below is 5 GHz
(11.7-16.7 GHz), comprehensive absorbing property are excellent.
Embodiment 2:
A kind of preparation method of porous carbon load nano nickel absorbing material, which is characterized in that its step are as follows:
Step 1, absorbent cotton load nickel nitrate
4 g of extracting degreasing cotton is immersed in the Ni (NO of 100 ml, 0.5 mol/L3)2·6H2In O solution, taken after impregnating 24 h
Absorbent cotton and extra solution is squeezed out out, wet absorbent cotton is 60oDry 24 h under C.
Step 2 loads nano nickel on porous carbon
By product obtained by step 1 in tube furnace N2600 under atmosphere protectionoC roasts 2 h, i.e., on porous carbon
Nano nickel is loaded, nano nickle granules partial size is about 10-18 nm, calculates and learns that the load capacity of nano nickel is 35 wt%.
The microwave absorbing property of porous carbon load nano nickel absorbing material is evaluated using network vector analyzer, Fig. 5 is
2 gained porous carbon of embodiment loads the reflection loss figure of nano nickel, and as can be seen from the figure porous carbon load nano nickel inhales wave material
The reflection loss peak of material is-51.6 dB, and-10 dB of reflection loss Absorber Bandwidth below is 4.9 GHz(13.1-18
GHz), comprehensive absorbing property is excellent.
Embodiment 3:
A kind of preparation method of porous carbon load nano nickel absorbing material, which is characterized in that its step are as follows:
Step 1, absorbent cotton load nickel nitrate
4 g of extracting degreasing cotton is immersed in the Ni (NO of 100 ml, 1.5 mol/L3)2·6H2In O solution, taken after impregnating 48 h
Absorbent cotton and extra solution is squeezed out out, wet absorbent cotton is 60oDry 24 h under C.
Step 2 loads nano nickel on porous carbon
By product obtained by step 1 in tube furnace N2600 under atmosphere protectionoC roasts 2 h, i.e., on porous carbon
Nano nickel is loaded, calculates and learns that the load capacity of nano nickel is 85.7 wt%.
Embodiment 4:
A kind of preparation method of porous carbon load nano nickel absorbing material, which is characterized in that its step are as follows:
Step 1, absorbent cotton load nickel nitrate
4 g of extracting degreasing cotton is immersed in the Ni (NO of 100 ml, 0.2 mol/L3)2·6H2In O solution, taken after impregnating 24 h
Absorbent cotton and extra solution is squeezed out out, wet absorbent cotton 80oDry 6 h under C.
Step 2 loads nano nickel on porous carbon
By product obtained by step 1 in tube furnace N2800 under atmosphere protectionoC roasts 2 h, i.e., on porous carbon
Nano nickel is loaded, 70-120 nm of nano nickel partial size is calculated and learnt that the load capacity of nano nickel is 18 wt%.