CN106495128A - A kind of single dispersing N doping hollow carbon nanometer polyhedral and preparation method thereof - Google Patents
A kind of single dispersing N doping hollow carbon nanometer polyhedral and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of single dispersing N doping hollow carbon nanometer polyhedral and preparation method thereof, the present invention is with ZnO nano ball as template and Zn sources, 2 Methylimidazole .s are used as organic ligand, 8 nano crystal composites of synthetic kernel core-shell ZnO@ZIF, it is placed in high temperature furnace, 2 4h are calcined in inert gas atmosphere, and calcining heat is 800 900 DEG C, directly obtains the carbon nanomaterial with hollow structure after calcining.Preparation process is simple of the present invention, nothing remove template procedure.Hollow structure material with carbon element obtained in the inventive method has homogeneous polyhedron pattern, and specific surface area is high, and nitrogen content is high, and there is very big application potential in fields such as electrochemical energy storage, catalysis and fuel cells.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, more particularly to a kind of single dispersing N doping hollow carbon nanometer multiaspect
Body and preparation method thereof.
Background technology
The hollow carbon nanometer material that the hollow carbon nanomaterial of single dispersing, particularly hetero atom (such as nitrogen, cobalt, nickel, ferrum etc.) adulterate
Material, because which has good heat stability and chemical stability, excellent electric conductivity, larger specific surface area and pore volume, compared with
Low density, and the advantages of abundant reactivity site, have in fields such as electrochemical energy storage, catalysis and fuel cells wide
General using value.
The hollow carbon nanomaterial of the single dispersing of most reports is hollow carbon balls, its main preparation method electrochemistry gas
Phase sedimentation, template and hydro-thermal method.Wherein template is that to prepare hollow carbon balls in recent years most common be also the most used
Method.The ultimate principle of the method is with template as configuration basis, by the series of physical such as precipitation adsorption, interfacial reaction, change
Process or self assembling process form shell (such as polymer) in template, remove template by means such as pyrolysis, dissolvings and obtain
Hollow material with carbon element.According to the property of template, template can also be divided into hard template method and soft template method.Hard template method is current template
Method prepares hollow carbon balls most common method, the shape that can efficiently control hollow material with carbon element by the physical aspect of Control architecture
Looks and size.At present, common hard template has silicon dioxide (SiO2) nanosphere, metal/metal oxide nano-particle, polymerization
Thing latex particle etc.；Conventional carbon source material has glucose, organic polymer etc..
Hard template method prepares hollow material with carbon element and still suffers from many defects, particularly SiO2Template is present removes template procedure,
Remove SiO2The solvent used by template is usually Fluohydric acid., sodium hydroxide solution etc., and environment non-green is had.
In recent years, metal-organic framework materials, particularly class zeolitic imidazolate framework material ZIF-8 are as presoma, high
Warm carbonization can directly obtain the porous carbon materials of N doping.In document " Facile synthesis of nanoporous
carbons with controlled particle sizes by direct carbonization of
In monodispersed ZIF-8crystals.Chem.Commun., 49 (2013) 2521-2523 ", Yusuke Yamauchi
Etc. the monodisperse porous carbon nanometer polyhedral granule for reporting size tunable, but carbon granule does not have hollow structure.
In document " Well-dispersed hollow porous carbon spheres synthesized by
direct pyrolysis of core-shell type metal-organic frameworks and their
In sorption properties.Chem.Commun., 50 (2014) 4492-4495 ", Moonhyun Oh etc. are reported and are based on
Hollow porous carbon (the Nitrogen-doped hollow of the N doping of nucleocapsid structure polystyrene@ZIF-8 composites
Porous carbon, N-HPC) nanosphere.The method can achieve the one-step method of the hollow carbon balls of single dispersing N doping and prepare, and
And carbon layers having thicknesses are controllable.But the carbon-coating of the hollow material with carbon element is made up of short grained carbon granule in a large number, so as to form particle diameter
Larger hollow carbon balls (0.7-1.0 μm).
In document " Interlocked multi-armed carbon for stable oxygen
Reduction.Chem.Commun., in 52 (2016) 5520-5522 ", Xuebo Cao etc. are reported and are spent based on ZnO@ZIF-8
The flower-shaped hollow structure carbon nanomaterial of shape nanometer rods presoma.But, there is obvious shortcoming in the method：Substep carbonization.Palpus
Under the conditions of compared with low temperature first by presoma carbonization after, with pickling remove ZnO cores, then again further for hollow carbon high-temperature process is obtained
Arrive target product.The method cannot realize that one-step method directly prepares hollow structure carbon nanomaterial.
Content of the invention
It is an object of the invention to a kind of preparation method of single dispersing N doping hollow carbon nanometer polyhedral is proposed, specifically
Preparation method is to obtain the hollow carbon nano-particle of single dispersing by carbonization nucleocapsid structure ZnO ZIF-8 presomas.Present invention system
Preparation Method can achieve one-step method carbonization presoma and prepare hollow material with carbon element, have unique without template procedure, the hollow carbon of gained is removed
Polyhedron pattern.
The single dispersing N doping hollow carbon nanometer polyhedral that the present invention is provided, is preparing nucleocapsid structure ZnO@ZIF-8 nanometers
During Polyhedral Particles presoma, the particle diameter of ZnO nano ball is controlled in 100-250nm so as to be generated during high temperature carbonization
Material with carbon element reduction-evaporation, a step obtains hollow structure carbon nano-particle, and the carbon nano-particle keeps the multiaspect of original presoma
Bodily form looks.
According to the first aspect of the invention, the invention provides a kind of single dispersing N doping hollow carbon nanometer polyhedral,
The single dispersing N doping hollow carbon nanometer polyhedral is obtained through high temperature carbonization is direct by nucleocapsid structure ZnO@ZIF-8 predecessors
Arrive, the single dispersing N doping hollow carbon nanometer polyhedral particle diameter be 250-350nm, a diameter of 100-250nm of hollow core, shell
The thickness of carbon is 10-20nm；The ZnO@ZIF-8 predecessors particle diameter of the nucleocapsid structure is 250-400nm；
The nucleocapsid structure ZnO@ZIF-8 predecessors be with ZnO nano ball as core, with ZIF-8 as hull shape into polyhedron；
The particle diameter of the ZnO nano ball is 100-250nm；The shell thickness of the ZIF-8 is 30-70nm；The ZIF-8 represents one kind
Class zeolitic imidazolate framework material ([Zn (MeIm)2]n, MeIM=2- Methylimidazole .s)
According to another aspect of the present invention, the invention provides the single dispersing N doping hollow carbon nanometer polyhedral
Preparation method, comprises the following steps：
1) preparation of ZnO nano ball
It is 0.1mol/L zinc acetate aqueous solutions to add 40mL concentration in reaction bulb, and 200mL concentration is 0.1-0.2mol/L
Triethanolamine aqueous solution, under room temperature stir 30min, then in 20-50 DEG C of water-bath reaction 20min after, stand 12h；Logical
Cross and be collected by centrifugation, wash, being vacuum dried, obtain the ZnO nano ball that particle size range is 100-250nm；
2) preparation of nucleocapsid structure ZnO@ZIF-8 presomas
By step 1) obtain in the mixed solvent that ZnO nano ball is added to DMF/ water, under room temperature, ultrasound 10min makes which abundant
Diffusion, is subsequently adding 2-methylimidazole, is placed in reaction 4-12h in 50-70 DEG C of baking oven after ultrasonic 5min, and reaction terminates rear product and leads to
Centrifugation, washing, vacuum drying is crossed, nucleocapsid structure ZnO@ZIF-8 predecessors are obtained；
3) preparation of single dispersing N doping hollow carbon nanometer polyhedral
By step 2) the nucleocapsid structure ZnO@ZIF-8 predecessors that obtain are placed in high temperature furnace, are warming up in an inert atmosphere
800-900℃；Carbonization is carried out in 800-900 DEG C of calcining at constant temperature, room temperature is then naturally cooled to, the product for obtaining is single dispersing
N doping hollow carbon nanometer polyhedral.
Preferably, step 1) in react in 20-50 DEG C of water-bath and carry out under the conditions of ultrasonic radiation.
Preferably, step 2) in DMF/ water volume ratios be 2-3:1.
Preferably, step 2) in the mol ratio of 2-methylimidazole and ZnO be 2-32：1.
Preferably, step 3) noble gases can be high pure nitrogen or argon, inert gas flow velocity is 50-150mL/
Min, the heating rate for being warming up to 800-900 DEG C in an inert atmosphere is 3-5 DEG C/min, and carbonization time is 1-3h.
Compared with prior art, the invention has the advantages that：
1) present invention is anti-with C by ZnO in the i.e. controllable carbonization process of the particle diameter 100-250nm for controlling ZnO nano ball
Answer degree so that ZnO is completely transformed into Zn and evaporates at high temperature, generate hollow carbon granule；
2) hollow carbon nano-particle prepared by the present invention can achieve uniform N doping, and keep polyhedron pattern；
3) present invention is not required to remove stratum nucleare template with pickling, you can realize eco-friendly preparation technology.
Description of the drawings
Fig. 1 is scanning electron microscope (SEM) photo (under 100nm scales) of the ZnO nano ball prepared in embodiment 1.
Fig. 2 is transmission electron microscope (TEM) photo of the nucleocapsid structure ZnO@ZIF-8 nanometer polyhedrals prepared in embodiment 1
(under 50nm scales).
Fig. 3 is transmission electron microscope (TEM) photo (under 50nm scales) of the hollow carbon nanometer polyhedral prepared in embodiment 1.
Fig. 4 is X-ray diffraction (XRD) spectrogram of the hollow carbon nanometer polyhedral prepared in embodiment 1.
Specific embodiment
For making the object, technical solutions and advantages of the present invention of greater clarity, with reference to specific embodiment, to this
Invention is further described.It should be understood that these descriptions are simply exemplary, and it is not intended to limit the scope of the present invention.
Embodiment 1
(1) preparation of ZnO nano ball
It is 0.1mol/L zinc acetate aqueous solutions to add 40mL concentration in 250mL conical flasks, and 200mL concentration is 0.1mol/L
Triethanolamine aqueous solution, stirs 30min under room temperature, after ultrasonic irradiation 20min, which is stood 12h in 20 DEG C of water-bath then.
By being collected by centrifugation, washing, be vacuum dried, ZnO nano ball is obtained.
(2) preparation of nucleocapsid structure ZnO@ZIF-8 presomas
By step 1) obtain 40.0mg ZnO nano balls and be added to filling DMF and water mixed solvent (32mL, volume ratio 3:1)
40ml vials in, under room temperature, ultrasound 10min makes which fully spread, and is subsequently added into 0.33g 2-methylimidazoles, ultrasonic 5min
Afterwards, vial is covered tightly and is placed in reaction 6h in 50 DEG C of baking ovens, after reaction terminates, product is done by centrifugation, washing, vacuum
Dry, obtain nucleocapsid structure ZnO@ZIF-8 predecessors.
(3) preparation of single dispersing N doping hollow carbon nanometer polyhedral
By step 2) the 1.0g nucleocapsid structure ZnO@ZIF-8 predecessors that obtain are placed in high temperature furnace, with 5 in nitrogen atmosphere
DEG C/ramp of min to 900 DEG C, inert gas flow velocity is 50mL/min.After carbonization 3h at 900 DEG C, room is naturally cooled to
Temperature, obtains single dispersing N doping hollow carbon nanometer polyhedral of the present invention.
Scanning electron microscope (SEM) photos (100nm scale under) of the Fig. 1 for ZnO nano ball；Fig. 2 nucleocapsid structure ZnO@ZIF-8 receive
Rice polyhedral transmission electron microscope (TEM) photo (under 50nm scales)；Transmission electron microscopes (TEM) of the Fig. 3 for hollow carbon nanometer polyhedral
Photo (under 50nm scales).
It will be seen from figure 1 that ZnO nano ball prepared by step (1) has uniform particle diameter (130 ± 20nm).Can from Fig. 2
To be clear that nucleocapsid structure ZnO@ZIF-8 nano-particle, its pattern is polyhedron, and the particle diameter of ZnO cores is reduced to 70nm, shell
Layer ZIF-8 thickness is 40 ± 10nm.As shown in figure 3, the hollow carbon obtained after carbonization maintains original polyhedron pattern, hollow
Core diameter is 140nm, and carbon wall thickness is 15 ± 5nm.XRD spectra of the Fig. 4 for gained hollow carbon nanometer polyhedral, diffraction maximum position
About in 2 θ=25 ° and 43 °, (002) and (101) crystal face of corresponding graphite-structure, it was confirmed that the structure of hollow carbon nano-particle.
Embodiment 2
(1) preparation of ZnO nano ball
It is 0.1mol/L zinc acetate aqueous solutions to add 40mL concentration in 250mL conical flasks, and 200mL concentration is 0.2mol/L
Triethanolamine aqueous solution, stirs 30min under room temperature, after ultrasonic irradiation 20min, which is stood 12h in 50 DEG C of water-bath then.
By being collected by centrifugation, washing, be vacuum dried, ZnO nano ball is obtained.
(2) preparation of nucleocapsid structure ZnO@ZIF-8 presomas
By step 1) obtain 40.0mg ZnO nano balls and be added to filling DMF and water mixed solvent (32mL, volume ratio 3:1)
40ml vials in, under room temperature, ultrasound 10min makes which fully spread, and is subsequently added into 0.33g 2-methylimidazoles, ultrasonic 5min
Afterwards, vial is covered tightly and is placed in reaction 4h in 70 DEG C of baking ovens, after reaction terminates, product is done by centrifugation, washing, vacuum
Dry, obtain nucleocapsid structure ZnO@ZIF-8 predecessors.
(3) preparation of single dispersing N doping hollow carbon nanometer polyhedral
By step 2) the 1.0g nucleocapsid structure ZnO@ZIF-8 predecessors that obtain are placed in high temperature furnace, in N2With 3 in atmosphere
DEG C/ramp of min to 800 DEG C, inert gas flow velocity is 100mL/min.Room is being naturally cooled to after carbonization 3h at 800 DEG C
Temperature, obtains single dispersing N doping hollow carbon nanometer polyhedral.
Embodiment 3
(1) preparation of ZnO nano ball
It is 0.1mol/L zinc acetate aqueous solutions to add 40mL concentration in 250mL conical flasks, and 200mL concentration is 0.1mol/L
Triethanolamine aqueous solution, stirs 30min under room temperature, after ultrasonic irradiation 20min, which is stood 12h in 50 DEG C of water-bath then.
By being collected by centrifugation, washing, be vacuum dried, ZnO nano ball is obtained.
(2) preparation of nucleocapsid structure ZnO@ZIF-8 presomas
By step 1) obtain 40.0mg ZnO nano balls and be added to filling DMF and water mixed solvent (32mL, volume ratio 2:1)
40ml vials in, under room temperature, ultrasound 10min makes which fully spread, and is subsequently added into 0.66g 2-methylimidazoles, ultrasonic 5min
Afterwards, vial is covered tightly and is placed in reaction 4h in 50 DEG C of baking ovens, after reaction terminates, product is done by centrifugation, washing, vacuum
Dry, obtain nucleocapsid structure ZnO@ZIF-8 predecessors.
(3) preparation of single dispersing N doping hollow carbon nanometer polyhedral
By step 2) the 1.0g nucleocapsid structure ZnO@ZIF-8 predecessors that obtain are placed in high temperature furnace, in N2With 3 in atmosphere
DEG C/ramp of min to 800 DEG C, inert gas flow velocity is 100mL/min.Room is being naturally cooled to after carbonization 3h at 800 DEG C
Temperature, obtains single dispersing N doping hollow carbon nanometer polyhedral.
Although embodiments of the present invention are described in detail, it should be understood that, without departing from the present invention's
In the case of spirit and scope, embodiments of the present invention can be made with various changes, replacement and change.
Claims (6)
1. a kind of single dispersing N doping hollow carbon nanometer polyhedral, the single dispersing N doping hollow carbon nanometer polyhedral is by core
Core-shell ZnO@ZIF-8 predecessors are directly obtained through high temperature carbonization, the single dispersing N doping hollow carbon nanometer polyhedral particle diameter
For 250-350nm, a diameter of 100-250nm of hollow core, the thickness of shell carbon is 10-20nm；The ZnO@of the nucleocapsid structure
ZIF-8 predecessors particle diameter is 250-400nm；
The nucleocapsid structure ZnO@ZIF-8 predecessors be with ZnO nano ball as core, with ZIF-8 as hull shape into faceted material；
The particle diameter of the ZnO nano ball is 100-250nm；The shell thickness of the ZIF-8 is 30-70nm；The ZIF-8 represents class boiling
Stone imidazate framework material.
2. a kind of preparation method of single dispersing N doping hollow carbon nanometer polyhedral, comprises the following steps：
1) preparation of ZnO nano ball
It is 0.1mol/L zinc acetate aqueous solutions to add 40mL concentration in reaction bulb, and 200mL concentration is the three of 0.1-0.2mol/L
Aqueous ethanolamine, stirs 30min under room temperature, then stand 12h after reaction 20min in 20-50 DEG C of water-bath；By from
The heart is collected, is washed, vacuum drying, obtains the ZnO nano ball that particle size range is 100-250nm；
2) preparation of nucleocapsid structure ZnO@ZIF-8 presomas
By step 1) obtain in the mixed solvent that ZnO nano ball is added to DMF/ water, under room temperature, ultrasound 10min makes which fully expand
Dissipate, be subsequently adding 2-methylimidazole, after ultrasonic 5min, be placed in reaction 4-12h in 50-70 DEG C of baking oven, reaction terminates rear product and passes through
Centrifugation, washing, vacuum drying, obtain nucleocapsid structure ZnO@ZIF-8 predecessors；
3) preparation of single dispersing N doping hollow carbon nanometer polyhedral
By step 2) the nucleocapsid structure ZnO@ZIF-8 predecessors that obtain are placed in high temperature furnace, are warming up to 800- in an inert atmosphere
900℃；Carbonization is carried out in 800-900 DEG C of calcining at constant temperature, room temperature is then naturally cooled to, the product for obtaining is that single dispersing nitrogen is mixed
Miscellaneous hollow carbon nanometer polyhedral.
3. the preparation method of a kind of single dispersing N doping hollow carbon nanometer polyhedral according to claim 2, its feature exist
In：Step 1) in react in 20-50 DEG C of water-bath and carry out under the conditions of ultrasonic radiation.
4. the preparation method of a kind of single dispersing N doping hollow carbon nanometer polyhedral according to claim 2, its feature exist
In：Step 2) in DMF/ water volume ratios be 2-3:1.
5. the preparation method of a kind of single dispersing N doping hollow carbon nanometer polyhedral according to claim 2, its feature exist
In：Step 2) in the mol ratio of 2-methylimidazole and ZnO be 2-32：1.
6. the preparation method of a kind of single dispersing N doping hollow carbon nanometer polyhedral according to claim 2, its feature exist
In：Step 3) noble gases can be high pure nitrogen or argon, inert gas flow velocity is 50-150mL/min, in inert atmosphere
In be warming up to 800-900 DEG C heating rate be 3-5 DEG C/min, carbonization time is 1-3h.
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| CN106904595A (en) * | 2017-03-20 | 2017-06-30 | 中国工程物理研究院化工材料研究所 | A kind of preparation method of the hollow carbon nanomaterial of nitrating |
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