CN109705808A - A kind of cobalt-nickel alloy with MOF structure-porous carbon composite wave-suction material and preparation method thereof - Google Patents
A kind of cobalt-nickel alloy with MOF structure-porous carbon composite wave-suction material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of cobalt-nickel alloy with MOF structure-porous carbon composite wave-suction material, the absorbing material is in porous flaky nanometer structure, is inlaid with cobalt-nickel alloy particle in pore structure, cobalt-nickel alloy particle is wrapped with graphitization carbon-coating.The invention also discloses above-mentioned cobalt-nickel alloy-porous carbon composite wave-suction material preparation methods: the cobalt nitrate, nickel nitrate and trimesic acid of more requirements being added into DMF, after reaction mass is completely dissolved, the desired amount of 4 ' 4- bipyridyl is added into mixed solution again, carries out solvent thermal reaction after dissolution is sufficiently stirred；After reaction product it is washed, it is dry after, obtain the predecessor in MOF structure；Predecessor is subjected to calcination processing, obtains cobalt-nickel alloy-porous carbon composite wave-suction material.Preparation method of the present invention has the advantages that preparation cost is low, simple process, and composite wave-suction material absorbing property obtained is excellent, is suitble to large-scale industrial production.
Description
Technical field
The present invention relates to a kind of cobalt-nickel alloy with MOF structure-porous carbon composite wave-suction materials, further relate to above-mentioned cobalt nickel
Alloy-porous carbon composite wave-suction material preparation method, belongs to absorbing material technical field.
Background technique
Rapid development with electromagnetic wave technology in civilian and military field, such as emerging miniaturized electronic of new generation,
There are many serious electromagnetic interference problems in automobile, radar and satellite communication etc. in daily life.Therefore, high-performance electromagnetism
Wave absorbing material is concerned as the effective ways solved these problems.Ideal efficient electromagnetic wave absorbent material should have suction
Receive the features such as characteristic is strong, absorption frequency range is wide, matching thickness is thin, density is light.Traditional absorbent, such as metal, due to having
Higher conductivity and dielectric constant and there is stronger electromagnetic wave absorption performance, but there are corrosion resistants for pure metal in its practical application
The disadvantages of corrosion is poor, cost is high, density is big.And according to impedance matching condition, ideal electromagnetic wave absorption agent should have moderate
Dielectric property and high magnetic conductivity.In addition, porous structure can effective reflection electromagnetic wave, and then more lose electromagnetism
Wave.Therefore, the design porous microwave absorption of novel low density is necessary.
In recent years, have and largely reported about research low-density microwave absorbing material.Beijing Institute of Technology's Qu Liangti project
Group has studied 3D graphene-Fe3O4Compound, the compound features go out good microwave absorbing property.When with a thickness of 3mm,
When compactedness is 10wt%, under 11.25GHz frequency, maximum reflectivity reaches -23dB, frequency bandwidth 9.2-15.0GHz.
The Zhao Haibo seminar of China Engineering Physics Research Institute have studied nickel carbon based composites and compactedness be 10wt% when
It waits, when filling thickness is 2mm, most strong reflection may be up to -45dB, and frequency bandwidth can achieve 4.6GHz.But prepare these materials
The method of material, which requires to be divided into multistep, to be handled, and is difficult to realize for large-scale industrial production.
Summary of the invention
Goal of the invention: technical problem to be solved by the invention is to provide a kind of cobalt-nickel alloy-with MOF structure is porous
Carbon composite wave-suction material, the composite wave-suction material is under low compactedness and low thickness still with strong reflection loss and wide effective
Absorption band.
The present invention also technical problems to be solved are to provide above-mentioned cobalt-nickel alloy-porous carbon composite wave-suction material preparation side
Method, this method can be used for large-scale industrial production without using hypertoxic organic solvent, at low cost, simple process.
In order to solve the above technical problems, the technology used in the present invention means are as follows:
A kind of cobalt-nickel alloy with MOF structure-porous carbon composite wave-suction material, the absorbing material are in porous nanometer
Laminated structure is inlaid with cobalt-nickel alloy particle in pore structure, and cobalt-nickel alloy particle is wrapped with graphitization carbon-coating.
Wherein, the absorbing material specific surface area is not less than 150m2The average pore size of/g, pore structure are less than 20nm.
Above-mentioned cobalt-nickel alloy-porous carbon composite wave-suction material preparation method, specifically comprises the following steps:
Step 1, reaction mass cobalt nitrate, nickel nitrate and trimesic acid are sequentially added into DMF, reaction mass is completely molten
Xie Hou, then the desired amount of 4 ' 4- bipyridyl is added into mixed solution, solvent thermal reaction is carried out after dissolution is sufficiently stirred；After reaction
Product is washed, it is dry after, obtain the carbon skeleton predecessor in MOF structure；
Step 2, the predecessor of step 1 is subjected to calcination processing, obtains cobalt-nickel alloy-porous carbon composite wave-suction material.
Wherein, in step 1, solvent thermal reaction temperature is 100~200 DEG C.
Wherein, in step 1, the solvent thermal reaction time is 4~8h.
Wherein, in step 2, the heating rate of calcination processing is 1~5 DEG C/min.
Wherein, in step 2, the temperature of calcination processing is 700~900 DEG C, and the time is 1~5h.
The preparation principle of composite wave-suction material of the present invention: there is the CoNi/C two dimension of MOF structure using solvent-thermal method preparation
Nanometer sheet prepares bimetallic alloy/porous carbon composite wave-suction material, the absorbing material using its high-temperature calcination pyrolysis
Electromagnetic property can be by Co2+And Ni2+Molar ratio regulation；The catalytic action for finally utilizing metallic cobalt, the porous carbon for obtaining sheet are multiple
Absorbing material is closed, porous structure effectively reduces the density of absorbing material, thereby reduces the compactedness of material when in use, from
And achieve the effect that light.
Compared with prior art, technical solution of the present invention has the beneficial effect that
Compared to traditional microwave absorption, composite wave-suction material of the present invention still has under low thickness and extremely low compactedness
Wide effective absorption band and high microwave absorption intensity, to have fabulous microwave absorbing property；The present invention is not required to simultaneously
Hypertoxic chemical reagent is used to prepare, it is simple process, at low cost, it can be used for large-scale industrial production.
Detailed description of the invention
Fig. 1 is Co made from the embodiment of the present invention 1,2,3xNiyThe X ray diffracting spectrum of/C；
Fig. 2 is the BET result figure of CoNi/C made from the embodiment of the present invention 2；
Fig. 3 is Co made from the embodiment of the present invention 13Ni7The SEM picture of/C；
Fig. 4 is the SEM picture of CoNi/C made from the embodiment of the present invention 2；
Fig. 5 is Co made from the embodiment of the present invention 37Ni3The SEM picture of/C；
Fig. 6 is the TEM picture of CoNi/C made from the embodiment of the present invention 2；
Fig. 7 is Co made from the embodiment of the present invention 13Ni7The reflection loss figure of/C；
Fig. 8 is the reflection loss figure of CoNi/C made from the embodiment of the present invention 2；
Fig. 9 is Co made from the embodiment of the present invention 37Ni3The reflection loss figure of/C.
Specific embodiment
The embodiment of the present invention scheme is described further below in conjunction with attached drawing.
The CoNi/C composite material that preparation method of the present invention obtains shows the laminated structure of surface porosity, and sheet knot
The size of structure can be controlled by the ratio of Co and Ni, mainly include following two step: solvent hot preparation CoNi-MOF: by one
Cobalt salt and the nickel salt dissolution of certainty ratio, are added complexing agent, continue stirring to dissolving, it is anti-to be then placed in hydrothermal reaction kettle progress hydro-thermal
It answers, be collected by centrifugation after the reaction was completed and dry；Dried CoNi-MOF predecessor is put into and is calcined to obtain in tube furnace
Porous CoNi/C composite material.
Embodiment 1
Cobalt-nickel alloy of the present invention-porous carbon composite wave-suction material preparation method, specifically comprises the following steps:
Step 1, it weighs 263mg cobalt nitrate and 610mg nickel nitrate is dissolved in together in 60mL n,N-Dimethylformamide,
Stirring to cobalt nitrate and nickel nitrate is completely dissolved；Measure 3mmol trimesic acid again and 4 ' 4- bipyridyl of 3mmol be added to it is above-mentioned
In mixed solution, continues to stir 30min, above-mentioned mixed liquor is transferred in autoclave, is placed in air dry oven and heats
To 120 DEG C, 4h is kept the temperature；Gained sediment is centrifugated to after cooled to room temperature and is washed drying, is obtained in MOF structure
Predecessor；
Step 2, step 1 gained predecessor is put into tube furnace under nitrogen atmosphere in 800 DEG C of calcining 2h, heating rate is
2℃/min；Natural cooling obtains product Co after calcining3Ni7/ C composite wave-suction material, composite wave-suction material are loose porous carbon
Material, cobalt-nickel alloy is particle studded in pore structure, and cobalt-nickel alloy particle is wrapped with graphitization carbon-coating.
Embodiment 2
Cobalt-nickel alloy of the present invention-porous carbon composite wave-suction material preparation method, specifically comprises the following steps:
Step 1, it weighs 438mg cobalt nitrate and 316.5mg nickel nitrate is dissolved in 60mL n,N-Dimethylformamide together
In, stirring to cobalt nitrate and nickel nitrate is completely dissolved；3mmol trimesic acid is measured again and 4 ' 4- bipyridyl of 3mmol is added to
It states in mixed solution, continues to stir 30min, above-mentioned mixed liquor is transferred in autoclave, be placed in air dry oven and add
Heat keeps the temperature 4h to 120 DEG C；Gained sediment is centrifugated to after cooled to room temperature and is washed drying, is obtained in MOF structure
Predecessor；
Step 2, step 1 gained predecessor is put into tube furnace under nitrogen atmosphere in 800 DEG C of calcining 2h, heating rate is
2℃/min；Natural cooling obtains product CoNi/C composite wave-suction material after calcining, and composite wave-suction material is loose porous carbon materials
Material, cobalt-nickel alloy is particle studded in pore structure, and cobalt-nickel alloy particle is wrapped with graphitization carbon-coating.
Embodiment 3
Cobalt-nickel alloy of the present invention-porous carbon composite wave-suction material preparation method, specifically comprises the following steps:
Step 1, it weighs 613mg cobalt nitrate and 261mg nickel nitrate is dissolved in together in 60mL n,N-Dimethylformamide,
Stirring to cobalt nitrate and nickel nitrate is completely dissolved；Measure 3mmol trimesic acid again and 4 ' 4- bipyridyl of 3mmol be added to it is above-mentioned
In mixed solution, continues to stir 30min, above-mentioned mixed liquor is transferred in autoclave, is placed in air dry oven and heats
To 120 DEG C, 4h is kept the temperature；Gained sediment is centrifugated to after cooled to room temperature and is washed drying, is obtained in MOF structure
Predecessor；
Step 2, step 1 gained predecessor is put into tube furnace under nitrogen atmosphere in 800 DEG C of calcining 2h, heating rate is
2℃/min；Natural cooling obtains product Co after calcining7Ni3/ C composite wave-suction material, composite wave-suction material are loose porous carbon
Material, cobalt-nickel alloy is particle studded in pore structure, and cobalt-nickel alloy particle is wrapped with graphitization carbon-coating.
Fig. 1 is Co obtained by embodiment 1,2,33Ni7/ C, CoNi/C and Co7Ni3The X-ray diffractogram of/C, from Fig. 1
As can be seen that embodiment 1,2,3 has similar diffraction maximum, there are three apparent diffraction maximums within the scope of surveyed, respectively
(111) of CoNi alloy, (200) and (220) crystal face.
Fig. 2 is the BET test result of the resulting CoNi/C of embodiment 2, and Fig. 2 can illustrate that CoNi/C is mesoporous material, see
Curve is it can be concluded that CoNi/C has mesoporous material characteristic, specific area 178m2/ g, average pore size 16nm, mainly has benefited from
Catalytic action of the microcellular structure and metallic of CoNi-MOF to carbon-coating.
Fig. 3,4,5 be respectively the resulting Co of embodiment 1,2,33Ni7/ C, CoNi/C and Co7Ni3The SEM picture of/C, by Fig. 3
As can be seen that the compound laminated structure of increasing with cobalt nitrate additional amount, obtained CoNi and carbon is more and more brighter in~5
It is aobvious, while shrinkage of the carbon MOF skeleton when being heat-treated calcining will increase, thus the hole density of finally obtained material and ratio
Surface area will increase, and then improve the performance of product.
Fig. 6 is the TEM picture of CoNi/C that embodiment 2 obtains, in Fig. 6 it can be seen from alloying pellet be embedded in it is more
Inside the carbon-coating of hole, only there is small part CoNi alloying pellet to be reunited.
Fig. 7 is Co made from embodiment 13Ni7The reflection loss figure of/C, it will be seen in fig. 7 that Co3Ni7/ C composite
Show good microwave absorbing property, matching thickness 1.8mm, when frequency is 16GHz, maximum reflection loss be can reach-
13dB, effective absorption band are 14.5-17.5GHz.
Fig. 8 be embodiment 2 made from CoNi/C reflection loss figure, in Fig. 8 it can be seen from CoNi/C composite material table
Reveal excellent microwave absorbing property, when frequency is 14.9GHz, and matching thickness is 1.7mm, maximum reflection, which is lost, may be up to-
42.5dB, effective absorption band are 13-18GHz.
Fig. 9 is Co made from embodiment 37Ni3The reflection loss figure of/C, in Fig. 9 it can be seen from Co7Ni3/ C composite wood
The microwave absorbing property of material is when matching thickness is 1.5mm, and when frequency is 17.6GHz, reflection loss is -11.2dB.
CoNi/C composite wave-suction material of the present invention is to obtain CoNi alloy and porous carbon by calcining CoNi-MOF presoma
Composite material.In CoNi/C composite wave-suction material, CoNi alloy improves the degree of graphitization of carbon-coating around, and alloy itself
Also there is high conductivity, therefore CoNi/C composite wave-suction material has high dielectric loss ability；And it is heat-treated the process of calcining
In due to carbon skeleton contraction and there is a large amount of hole, this some holes greatly reduces the density of composite wave-suction material, further
So that material compactedness reduces, therefore the present invention still can achieve stronger reflection loss under lower compactedness and wider have
Imitate absorption band.
CoNi-MOF composite wave-suction material excellent properties of the present invention are mainly derived between graphitization carbon-coating and alloy particle
Interfacial polarization, while biggish specific surface area leads to more surface defects, the two is consumed incident electromagnetic wave simultaneously；By force
Conductance property and low-density also ensure that material has high dielectric constant under low compactedness and under low thickness, so a variety of losses
The presence of mechanism ensure that strong absorption of the composite wave-suction material of the present invention to incident electromagnetic wave.
Claims (5)
1. a kind of cobalt-nickel alloy with MOF structure-porous carbon composite wave-suction material, it is characterised in that: the absorbing material is in
Porous flaky nanometer structure is inlaid with cobalt-nickel alloy particle in pore structure, and cobalt-nickel alloy particle is wrapped with graphitization carbon-coating.
2. the cobalt-nickel alloy with MOF structure-porous carbon composite wave-suction material according to claim 1, it is characterised in that:
The absorbing material specific surface area is not less than 150m2The average pore size of/g, pore structure are less than 20nm.
3. the preparation method of the cobalt-nickel alloy with MOF structure-porous carbon composite wave-suction material described in claim 1, special
Sign is: specifically comprising the following steps:
Step 1, the cobalt nitrate, nickel nitrate and trimesic acid of more requirements are added into DMF, after reaction mass is completely dissolved, then
The desired amount of 4 ' 4- bipyridyl is added into mixed solution, carries out solvent thermal reaction after dissolution is sufficiently stirred；Product passes through after reaction
After washing, drying, the predecessor in MOF structure is obtained；
Step 2, the predecessor of step 1 is subjected to calcination processing, obtains cobalt-nickel alloy-porous carbon composite wave-suction material.
4. the preparation method of the cobalt-nickel alloy with MOF structure-porous carbon composite wave-suction material according to claim 3,
It is characterized by: in step 1, the reaction temperature of solvent thermal reaction is 100~200 DEG C, the reaction time of solvent thermal reaction is 4~
8h。
5. the preparation method of the cobalt-nickel alloy with MOF structure-porous carbon composite wave-suction material according to claim 3,
It is characterized by: in step 2, calcination processing is under the conditions of nitrogen atmosphere, 1~5 DEG C/min of heating rate, it is warming up to 700~
900 DEG C of 1~5h of calcining.
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| CN112961650B (en) * | 2021-02-06 | 2023-06-30 | 安徽理工大学 | Three-metal organic framework derived iron-nickel alloy/porous carbon ultrathin wave absorber and preparation method thereof |
| CN112877032A (en) * | 2021-03-02 | 2021-06-01 | 陕西科技大学 | Two-dimensional CoNi @ porous carbon material and preparation method and application thereof |
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| CN114346250A (en) * | 2021-12-31 | 2022-04-15 | 广东技术师范大学 | Metal-carbon composite particle and preparation method and application thereof |
| CN114346250B (en) * | 2021-12-31 | 2023-09-26 | 广东技术师范大学 | Metal-carbon composite particles and preparation method and application thereof |
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| CN115028847A (en) * | 2022-05-09 | 2022-09-09 | 复旦大学 | CoNi alloy MOF porous material and preparation and application thereof |
| CN115028847B (en) * | 2022-05-09 | 2024-01-26 | 复旦大学 | CoNi alloy MOF porous material and preparation and application thereof |
| CN115332821A (en) * | 2022-08-29 | 2022-11-11 | 盐城工学院 | Preparation method of CoNi/NC wave-absorbing material |
| CN115739095B (en) * | 2022-11-16 | 2024-01-26 | 合肥飞木生物科技有限公司 | Preparation method and application of Ni-Co@C carbon core-shell hydrophobic nanoparticle catalyst |
| CN115739095A (en) * | 2022-11-16 | 2023-03-07 | 合肥飞木生物科技有限公司 | Preparation method and application of Ni-Co @ C carbon core-shell hydrophobic nanoparticle catalyst |
| CN115947952B (en) * | 2023-02-24 | 2023-10-31 | 福建警察学院 | One-step synthesis method of hollow Co metal organic frame nanotube |
| CN115947952A (en) * | 2023-02-24 | 2023-04-11 | 福建警察学院 | One-step synthesis method of hollow Co metal organic framework nanotube |
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