CN105253877A - Preparation method of three-dimensional interpenetrating ordered mesoporous graphene spheres - Google Patents
Preparation method of three-dimensional interpenetrating ordered mesoporous graphene spheres Download PDFInfo
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- CN105253877A CN105253877A CN201510755443.6A CN201510755443A CN105253877A CN 105253877 A CN105253877 A CN 105253877A CN 201510755443 A CN201510755443 A CN 201510755443A CN 105253877 A CN105253877 A CN 105253877A
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Abstract
The invention discloses a preparation method of three-dimensional interpenetrating ordered mesoporous graphene spheres. The preparation method of the three-dimensional interpenetrating ordered mesoporous graphene spheres comprises the following steps: carrying out high-temperature cracking on a ferric oleate precursor in the presence of oleic acid in a solvent, so as to obtain ferroferric oxide nano particles; dissolving the ferroferric oxide nano particles in an organic solvent, forming an O/W oil-in-water type emulsion, distilling off the organic solvent, and adsorbing or centrifuging a product with a magnet, so as to obtain ferroferric oxide nano particle microspheres of a highly ordered secondary structure; then calcining at the temperature more than 300 DEG C in the presence of nitrogen or argon, so as to obtain ferroferric oxide nano particle microspheres which are formed by highly ordered arranged and piled nano particles; then etching with acid, so as to obtain ordered mesoporous carbon spheres with high specific surface area; and finally carrying out graphitization at the temperature more than 1000 DEG C in a nitrogen or argon atmosphere, so as to obtain the three-dimensional interpenetrating ordered mesoporous graphene spheres. The preparation method of the three-dimensional interpenetrating ordered mesoporous graphene spheres is simple in operation, the prepared graphene spheres are thin in pore walls, stable in structure, extremely large in specific surface area and controllable in pore diameter and shape, and porous channels are highly ordered in arrangement and are through.
Description
Art
The invention belongs to technical field of inorganic material, be specifically related to the preparation method of the order mesoporous Graphene ball of a kind of three-dimensional communication.
Technical background
Graphene is a kind of Two-dimensional Carbon material, is the general designation of single-layer graphene, bilayer graphene and few layer graphene.2004, scientist successfully obtained single-layer graphene lamella by stripping method, and theoretic throat is only 0.335nm, was considered to " the thinnest two-dimensional material ".Graphene has excellent physical property, as high connductivity, the capacity of heat transmission etc., causes the research boom of scientists.
The existing method preparing Graphene mainly contains: mechanically peel method, chemical Vapor deposition process, oxidation reduction process, arc process and organic synthesis method.Graphene is due to its high-ratio surface sum surface tension, and the Graphene that traditional method obtains is sheet single-layer graphene, bilayer graphene and few layer graphene, and these products easily occur curling and reunite, and are difficult to independent stable existence; In use, usually need to spend a large amount of energy for dispersion, constrain the performance of its performance.
Summary of the invention
Easily reuniting to solve Graphene existing structure, being difficult to independent stable existence, and need the problem of dispersion, improve the performance of its effective performance simultaneously, the invention provides the preparation method of the order mesoporous Graphene ball of a kind of three-dimensional communication.
The preparation method of the order mesoporous Graphene ball of a kind of three-dimensional communication of the present invention, concrete steps are as follows:
(1) by nanoparticle precursor iron oleate in solvent under oleic acid effect Pintsch process, nitrogen protection lower 280 DEG C-320 DEG C reaction 1 hour, obtain the ferriferrous oxide nano-particle of different-grain diameter and pattern, its Surface coating has oleic acid molecular;
(2) gained ferriferrous oxide nano-particle is dissolved in organic solvent, again the instillation of this solution is formed O/W emulsion oil-in-water containing in the aqueous phase of tensio-active agent under stirring, heat up and blow, after organic solvent is steamed, product magnet adsorption or centrifugal, give up supernatant liquid, gained precipitation obtains the ferriferrous oxide nano-particle microballoon with high-sequential secondary structure after cleaning with ethanol;
(3) step (2) gained ferriferrous oxide nano-particle microballoon is calcined under nitrogen or argon more than 300 DEG C, make surface coated oleic acid molecular carbonization, obtain arranging by nanoparticle high-sequential the ferriferrous oxide nano-particle microballoon be piled into, each nanoparticle in thus obtained microsphere is all coated by carbon-coating;
(4) step (3) gained high-sequential is arranged the ferriferrous oxide nano-particle microballoon acid etch be piled into, obtain the ordered mesopore carbon ball with high-specific surface area;
(5) by step 4 gained ordered mesopore carbon ball under nitrogen or argon gas atmosphere in more than 1000 DEG C graphitization processing, obtain the order mesoporous Graphene ball of three-dimensional communication.
In the present invention, described in step 1, ferriferrous oxide nano-particle presoma Pintsch process temperature is 270 DEG C to 330 DEG C, and solvent for use can be hexadecylene, octyl ether, octadecylene or icosa alkene, and pyrolysis time is 30-90 minute.
In the present invention, in described step (1), oleic acid concentration is 1.5mM ~ 4.5mM).
In the present invention, described step (3) high-temperature calcination temperature is 300 ~ 600 DEG C, and calcination time is 2-4 hour.
In the present invention, described step (5) graphitization processing temperature is 1000-1600 DEG C, and the treatment time is 2-10 hour.
The present invention by the nanoparticle dispersion of uniform particle diameter in organic solvent, oil-in-water (O/W) type emulsion is formed again by the effect of tensio-active agent, by the solvent in evaporation emulsion droplet, self-assembly is impelled to form the microballoon of ordered arrangement, again by microballoon high-temperature calcination, make the carbonization of nanoparticle surface part, simultaneously because ferriferrous oxide nano-particle in carbonization process expands, cause, between adjacent nano particle, focal adhesion occurs, then with acid, nanoparticle etching can be obtained highly ordered mesosize pores carbon ball, the position sticked together is formed " wicket " of connected pore channel after etching, last again by mesoporous carbon spheres greying, obtain three-dimensional ordered mesoporous Graphene ball.
The present invention program, by the method for solvent evaporates induction self-assembly, under Action of Surfactant, makes low boiling point solvent volatilize, solvent evaporates speed is fast, self-assembly arrangement high-sequential, Graphene ball size adjustable, namely obtain product at lesser temps, operation is simple.Simultaneously, because the mesoporous wall of the mesoporous Graphene ball of gained is graphene layer, and be only layer 2-4, the number of plies is few, Stability Analysis of Structures, the most important is mesoporous has " wicket " to be communicated with, ensure that the continuous of the graphene layer in whole ball, under the prerequisite keeping high-specific surface area, in turn ensure that graphene sheet layer is thin and continuous, although graphene layer has bending, but still maintain the two-dimension plane structure of Graphene to a certain extent, maintain the good characteristic of graphene film, in catalysis, medicine and energy storage etc., have very high using value.。
The inventive method, simple to operate, raw material is easy to get, and preparation amount is large, and prepared Graphene ball road arrangement high-sequential is through, and hole wall is thin, is only layer 2-4 graphene layer, Stability Analysis of Structures, has very high specific surface area and aperture and morphology controllable.
Product of the present invention can be widely used in energy storage and electromagnetism, medicine and other fields.
Accompanying drawing explanation
Fig. 1 is the hot weightless picture of the order mesoporous Graphene ball of three-dimensional communication prepared by the present invention;
Fig. 2 is the Raman spectrogram of the order mesoporous Graphene ball of three-dimensional communication prepared by the present invention;
Fig. 3 is the scanning electron microscope (SEM) photograph of ferriferrous oxide nano-particle microballoon prepared by the present invention;
Fig. 4 is the transmission electron microscope picture of the order mesoporous Graphene ball of three-dimensional communication prepared by the present invention;
Fig. 5 is the Regional High Resolution transmission electron microscope picture of the order mesoporous Graphene ball of three-dimensional communication prepared by the present invention;
Fig. 6 is the small angle X ray scattering collection of illustrative plates of the order mesoporous Graphene ball of three-dimensional communication prepared by the present invention;
Fig. 7 is isothermal adsorption desorption curve (a) and pore analysis collection of illustrative plates (b) of the order mesoporous Graphene ball of three-dimensional communication prepared by the present invention.
Embodiment
Embodiment 1:
By 36g iron oleate, 8.5g oleic acid, is dissolved in 200g octadecylene, and the lower 320 DEG C of reactions of nitrogen protection 1 hour, obtain particle diameter about 14nm ferriferrous oxide nano-particle.Gained ferriferrous oxide nano-particle is dissolved in 40ml normal hexane, again this solution 20ml is instilled under stirring in the 200ml water containing 4g Trimethyllaurylammonium bromide and form O/W (oil-in-water) type emulsion, heat up and blow, after organic solvent is steamed, product magnet adsorption or centrifugation, give up supernatant liquid, after gained precipitation is cleaned with ethanol, obtaining particle diameter is the ferriferrous oxide nano-particle microballoon that about 300nm has high-sequential secondary structure.By gained ferriferrous oxide nano-particle microballoon under a nitrogen 500 DEG C of calcinings 2 hours, the oleic acid molecular carbonization making nanoparticle surface coated, obtains arranging by nanoparticle high-sequential the ferriferrous oxide nano-particle microballoon be piled into.Arrange by nanoparticle high-sequential the ferriferrous oxide nano-particle microballoon hydrochloric acid be piled into etch away Z 250 wherein by obtained, namely obtaining particle diameter is that about 300nm is containing about 14nm ordered mesopore carbon ball.Finally, by gained ordered mesopore carbon ball at 1600 DEG C, 2 hours graphitization processing, maintain original pattern, obtain the order mesoporous Graphene ball of three-dimensional communication.
Embodiment 2:
By 36g iron oleate, 8.5g oleic acid, is dissolved in 200g octadecylene, and the lower 320 DEG C of reactions of nitrogen protection 1 hour, obtain particle diameter about 14nm ferriferrous oxide nano-particle.Gained ferriferrous oxide nano-particle is dissolved in 40ml normal hexane, again this solution 40ml is instilled under stirring in the 200ml water containing 8g Trimethyllaurylammonium bromide and form O/W (oil-in-water) type emulsion, heat up and blow, after organic solvent is steamed, product magnet adsorption or centrifugation, give up supernatant liquid, after gained precipitation is cleaned with ethanol, obtaining particle diameter is about the 1 μm ferriferrous oxide nano-particle hollow microsphere with high-sequential secondary structure.Gained had the ferriferrous oxide nano-particle hollow microsphere of high-sequential secondary structure, under a nitrogen 500 DEG C of calcinings 2 hours, the oleic acid molecular carbonization making nanoparticle surface coated, obtains arranging by nanoparticle high-sequential the ferriferrous oxide nano-particle microballoon be piled into.Obtained nanoparticle high-sequential is arranged the ferriferrous oxide nano-particle microballoon hydrochloric acid be piled into and etch away Z 250 wherein, namely obtain particle diameter and be about 1 μm and contain about 14nm ordered mesopore carbon ball.Finally, by gained ordered mesopore carbon ball at 1000 DEG C, 10 hours graphitization processing, maintain original pattern, obtain the order mesoporous Graphene ball of three-dimensional communication.
Embodiment 3:
By 36g iron oleate, 8.5g oleic acid, is dissolved in 200g octadecylene, and the lower 280 DEG C of reactions of nitrogen protection 1 hour, obtain particle diameter about 6nm ferriferrous oxide nano-particle.Gained ferriferrous oxide nano-particle is dissolved in 40ml normal hexane, again this solution 20ml is instilled under stirring in the 200ml water containing 4g Trimethyllaurylammonium bromide and form O/W (oil-in-water) type emulsion, heat up and blow, after organic solvent is steamed, product magnet adsorption or centrifugation, give up supernatant liquid, after gained precipitation is cleaned with ethanol, obtaining particle diameter is the ferriferrous oxide nano-particle hollow microsphere that about 300nm has high-sequential secondary structure.Gained had the ferriferrous oxide nano-particle hollow microsphere of high-sequential secondary structure under a nitrogen 500 DEG C of calcinings 2 hours, the oleic acid molecular carbonization making nanoparticle surface coated, obtains arranging by nanoparticle high-sequential the ferriferrous oxide nano-particle microballoon be piled into.Obtained nanoparticle high-sequential is arranged the ferriferrous oxide nano-particle microballoon hydrochloric acid be piled into and etch away Z 250 wherein, namely obtaining particle diameter is that about 300nm is containing about 6nm ordered mesopore carbon ball.Finally, by gained ordered mesopore carbon ball at 1000 DEG C, 10 hours graphitization processing, maintain original pattern, obtain the order mesoporous Graphene ball of three-dimensional communication.
Embodiment 4:
By 36g iron oleate, 8.5g oleic acid, is dissolved in 200g octadecylene, and the lower 320 DEG C of reactions of nitrogen protection 1 hour, obtain particle diameter about 14nm ferriferrous oxide nano-particle.Gained ferriferrous oxide nano-particle is dissolved in 40ml normal hexane, again this solution 30ml is instilled under stirring in the 200ml water containing 6g Trimethyllaurylammonium bromide and form O/W (oil-in-water) type emulsion, heat up and blow, after organic solvent is steamed, product magnet adsorption or centrifugation, give up supernatant liquid, after gained precipitation is cleaned with ethanol, obtaining particle diameter is the ferriferrous oxide nano-particle hollow microsphere that about 500nm has high-sequential secondary structure.Gained had the ferriferrous oxide nano-particle hollow microsphere of high-sequential secondary structure under a nitrogen 500 DEG C of calcinings 2 hours, the oleic acid molecular carbonization making nanoparticle surface coated, obtains high-sequential and arranges the ferriferrous oxide nano-particle microballoon be piled into.Obtained high-sequential is arranged the ferriferrous oxide nano-particle microballoon hydrochloric acid be piled into and etch away Z 250 wherein, namely obtaining particle diameter is that about 500nm is containing about 6nm ordered mesopore carbon ball.Finally, by gained ordered mesopore carbon ball at 1600 DEG C, 2 hours graphitization processing, maintain original pattern, obtain the order mesoporous Graphene ball of three-dimensional communication.
Above-described embodiment, solvent for use is not limited to octadecylene, also can be hexadecylene, octyl ether, icosa alkene.Above embodiment is only for illustration of the present invention but not for limiting the scope of the invention simultaneously.
Below by means such as thermogravimetric analysis, Raman spectrum, transmission electron microscope, scanning electron microscope, low-angle scattering of X-rays, Structure and Properties of the present invention is characterized.
1. thermogravimetric analysis
Fig. 1 is the thermal weight loss result of the order mesoporous Graphene ball of the three-dimensional communication obtained at 1600 DEG C after greying, and as can be seen from the figure, after 600 DEG C, Graphene ball just starts to decompose, and shows that gained Graphene ball has very high thermostability.
2, Raman spectrum
Fig. 2 is the Raman spectrum spectrogram of the order mesoporous Graphene ball of the three-dimensional communication obtained under wavelength 532nm utilizing emitted light at 1600 DEG C after greying, in 1340.3cm-1 and 1583.7cm-1 punishment although to D, G bis-peak of high separation, 2D peak can also be found at 2668.2cm-1 place, show that material is high-graphitized.
3. scanning electron microscope analysis
Fig. 3 is the scanning electron microscopic picture of 14nm ferriferrous oxide nano-particle microballoon after 500 DEG C of calcinings.As can be seen from the figure, by the microballoon obtained under self-assembly and Action of Surfactant, after 500 DEG C of calcinings, the ordered arrangement of nanometer example still can keep extraordinary pattern, and the globosity be simultaneously piled into obtains maintenance.
4. TEM (transmission electron microscope) analysis
Fig. 4 is the transmission electron microscope picture of the order mesoporous Graphene ball of the three-dimensional communication obtained at 1000 DEG C after greying.As can be seen from the figure, gained Graphene ball is of a size of about 600nm, maintains globosity
Fig. 5 is the Regional High Resolution transmission electron microscope picture of the order mesoporous Graphene ball of the three-dimensional communication obtained at 1000 DEG C after greying, and hole wall is layer 2-4 graphene layer as we can see from the figure.
5. small angle X ray scattering
As can be seen from small-angle scattering figure Fig. 6, the order mesoporous Graphene ball of gained three-dimensional communication has the meso-hole structure of long-range order, occurs multiple diffraction peak, can characterize the ordered mesopore structure of different crystal face respectively.
6. specific surface area and pore size distribution
From the adsorption isothermal curve of Fig. 7 a, calculating known material specific surface area through BET method is 680m3/g, has larger specific surface area.
As can be seen from Fig. 7 b we, the Graphene ball obtained maintains meso-hole structure, and mesoporous pore size is 9.6nm, basically identical with ferriferrous oxide nano-particle particle diameter used, also have significantly empty distribution in addition at 2.45nm place, this illustrate adjacent mesoporous by microporous connectivity.
In sum, hinge structure of the present invention has following characteristics:
The present invention utilizes similar template first to make carbon ball containing highly ordered mesosize pores, then mesoporous carbon spheres greying is obtained the order mesoporous Graphene ball of three-dimensional communication, and the ferriferrous oxide nano-particle using common magnetic property superior, as template, take oleic acid as carbon source.By iron oleate cracking, obtain the even ferriferrous oxide nano-particle of different-grain diameter, nanoparticle surface is coated with part oleic acid.By the method for solvent evaporates induction self-assembly, under Action of Surfactant, in solvent evaporates process, the arrangement of self-assembly high-sequential forms the microballoon of certain particle diameter, the microballoon containing high-sequential carbon coated ferriferrous oxide nanoparticle is obtained again through high temperature cabonization, simultaneously because ferriferrous oxide nano-particle in carbonization process expands, cause, between adjacent nano particle, focal adhesion occurs.By the microballoon acidifying etching obtained, obtain the carbon ball containing highly ordered mesosize pores, the position sticked together is formed " wicket " of connected pore channel after etching.Final high temperature greying obtains three-dimensional ordered mesoporous Graphene ball.The present invention has the following advantages, material height is orderly on the one hand, specific surface area is large, mesoporous pore size and pattern control by nano particle diameter and pattern, the size of Graphene ball and pattern are controlled by the concentration of nanoparticle and tensio-active agent, realize the Morphological control from nanoscale to micro-meter scale; Simultaneously, because obtained mesoporous wall is only layer 2-4 graphene layer, and Stability Analysis of Structures, the most important is mesoporous has " wicket " to be communicated with, ensure that the continuous of the graphene layer in whole ball, thin graphene directly contacts with other materials by mesopore orbit, and compound is simple, because its duct is continuous, although graphene layer has bending, but still maintain the two-dimension plane structure of Graphene to a certain extent, maintain the good characteristic of graphene film, there is great practical advantages.
Claims (4)
1. a preparation method for the order mesoporous Graphene ball of three-dimensional communication, is characterized in that comprising the following steps:
(1) by nanoparticle precursor iron oleate in solvent under oleic acid effect Pintsch process, nitrogen protection lower 280 DEG C-320 DEG C reaction 1 hour, obtain the ferriferrous oxide nano-particle of different-grain diameter and pattern;
(2) gained ferriferrous oxide nano-particle is dissolved in organic solvent, again the instillation of this solution is formed O/W emulsion oil-in-water containing in the aqueous phase of tensio-active agent under stirring, heat up and blow, after organic solvent is steamed, product magnet adsorption or centrifugal, give up supernatant liquid, gained precipitation obtains the ferriferrous oxide nano-particle microballoon with high-sequential secondary structure after cleaning with ethanol;
(3) step (2) gained ferriferrous oxide nano-particle microballoon is calcined under nitrogen or argon more than 300 DEG C, make surface coated oleic acid molecular carbonization, obtain arranging by nanoparticle high-sequential the ferriferrous oxide nano-particle microballoon be piled into;
(4) step (3) gained high-sequential is arranged the ferriferrous oxide nano-particle microballoon acid etch be piled into, obtain the ordered mesopore carbon ball with high-specific surface area;
(5) by step (4) gained ordered mesopore carbon ball under nitrogen or argon gas atmosphere in more than 1000 DEG C graphitization processing, obtain the order mesoporous Graphene ball of three-dimensional communication;
Wherein, nanoparticle precursor Pintsch process temperature is 280 DEG C to 330 DEG C, and solvent for use can be hexadecylene, octyl ether, octadecylene or icosa alkene, and pyrolysis time is 30-90 minute.
2. the preparation method of the order mesoporous Graphene ball of a kind of three-dimensional communication according to claim 1, it is characterized in that: in described step (1), oleic acid concentration is 1.5mM ~ 4.5mM.
3. the preparation method of the order mesoporous Graphene ball of a kind of three-dimensional communication according to claim 1, it is characterized in that: described step (3) high-temperature calcination temperature is 300 ~ 600 DEG C, calcination time is 2-4 hour.
4. the preparation method of the order mesoporous Graphene ball of a kind of three-dimensional communication according to claim 1, it is characterized in that: described step (5) graphitization processing temperature is 1000-1600 DEG C, the treatment time is 2-10 hour.
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| CN107082414A (en) * | 2015-02-13 | 2017-08-22 | 大洲电子材料株式会社 | Graphene with random and irregular three-D stomata and preparation method thereof |
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| CN108722352A (en) * | 2018-05-25 | 2018-11-02 | 陕西凯蓝环保科技有限公司 | A kind of macropore carbon based material and preparation method thereof of absorption environment carbon monoxide |
| CN108722352B (en) * | 2018-05-25 | 2020-12-18 | 陕西凯蓝环保科技有限公司 | Macroporous carbon-based material for adsorbing environmental carbon monoxide and preparation method thereof |
| CN109888154A (en) * | 2019-03-14 | 2019-06-14 | 复旦大学 | A kind of preparation method of high-performance modified polypropylene diaphragm |
| CN109888154B (en) * | 2019-03-14 | 2020-05-12 | 复旦大学 | Preparation method of high-performance modified polypropylene diaphragm |
| CN111234776A (en) * | 2020-01-20 | 2020-06-05 | 东华大学 | Solid Fe3O4@ C superstructure microsphere wave-absorbing material and preparation method and application thereof |
| CN114620717A (en) * | 2022-04-08 | 2022-06-14 | 复旦大学 | Preparation method of ordered double-mesoporous carbon graphene material or ordered double-mesoporous carbon material |
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