CN102886270B - SiC is nanocrystalline/Graphene hetero-junctions and preparation method and application - Google Patents
SiC is nanocrystalline/Graphene hetero-junctions and preparation method and application Download PDFInfo
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Abstract
A kind of nanometer silicon carbide crystalline substance/Graphene hetero-junctions, the outer surface of SiC nano-crystalline granule is coated with at least one layer graphene, obtained by following method: by SiC nano-crystalline granule in vacuum or argon gas atmosphere, carry out annealing in process in 1000 DEG C-1600 DEG C, obtain SiC nanocrystalline/Graphene hetero-junctions.The present invention according to SiC thermal decomposition principle, by regulation and control annealing temperature, annealing time and ambiance, can obtain by the SiC nano-crystalline granule of the graphene coated of the different number of plies, thus obtain SiC nanocrystalline/Graphene heterojunction structure.Utilize the SiC prepared by the present invention nanocrystalline/Graphene heterojunction structure, at surface catalysis field (in surperficial photocatalysis to degrade organic matter and photocatalysis hydrogen production etc.), have a wide range of applications potential.
Description
Technical field
The invention belongs to field of material technology, relate to particularly a kind of SiC nanocrystalline/Graphene hetero-junctions.
The invention still further relates to above-mentioned SiC nanocrystalline/preparation method of Graphene hetero-junctions.
The invention still further relates to above-mentioned SiC nanocrystalline/application of Graphene hetero-junctions in surface catalysis.
Background technology
Along with technological progress and social development, the consumption of people to the energy gets more and more, and the pollution brought to environment is more and more serious.The effective ways finding the new energy (as obtained the fuel gas such as methane by the hydrogen manufacturing of photo catalytic reduction reaction water, reduction organic pollution) and degradable organic pollutant become one of current study hotspot.Traditional semiconductor light-catalyst mainly contains WO
3, TO
2, ZnO and SiC powder etc.In order to improve the catalytic action of conductor photocatalysis medium, two kinds of technical methods are often used to improve photocatalysis: one is the effective absorption (by doping, introducing impurity energy level increases light absorption) increasing light, produces more photo-generated carrier; Two is that the space of accelerating photo-generated carrier is separated (by forming metal/oxide composite construction, accelerating electronics to metal transfer), reduces the compound of photo-generated carrier.A large amount of experimental studies shows, it is the effective ways improving photocatalysis usefulness that the space of accelerating photo-generated carrier is separated.Since Graphene in 2004 is found, due to the distinctive high carrier mobility of Graphene and king-sized specific area, make Graphene/TiO
2the research of (or other oxide) compound becomes the focus of New Generation Optical catalysis material research.Experiment has found Graphene/TiO
2photocatalysis hydrogen production [Xiao-YanZhang, Hao-PengLi, Xiao-LiCuiandYueheLin, the Graphene/TiO of compound
2nanocomposites:synthesis, characterizationandapplicationinhydrogenevolutionfromwat erphotocatalyticsplitting, J.Mater.Chem., 20,2801-2806 (2010)] or degradation of organic substances ability be much better than TiO
2catalytic capability [JiangDu, XiaoyongLai, NailiangYang, JinZhai, DavidKisailus, FabingSu, DanWangandLeiJiang, HierarchicallyOrderedMacro-MesoporousTiO
2grapheneCompositeFilms:ImprovedMassTransfer, ReducedChargeRecombination, andTheirEnhancedPhotocatalyticActivities, ACSNANO5,590 (2011)].But, due to Graphene/TiO
2the compound of (or oxide) is mixed by physics or chemical method, Graphene and TiO
2the combination interface of (oxide) is random joint, and be not that perfect coated heterogeneous interface combines, the carrier transfer performance of this compound with randomness combination depends on Graphene/TiO to a great extent
2(oxide) surface conjunction quality.
Summary of the invention
The object of the present invention is to provide a kind of nanometer silicon carbide crystalline substance/Graphene hetero-junctions.
Another object of the present invention is to provide a kind of method preparing nanometer silicon carbide crystalline substance/Graphene hetero-junctions.
For achieving the above object, nanometer silicon carbide crystalline substance/Graphene hetero-junctions provided by the invention, the outer surface of SiC nano-crystalline granule is coated with at least one layer graphene, obtained by following method: by SiC nano-crystalline granule in vacuum or argon gas atmosphere, carry out annealing in process in 1000 DEG C-1600 DEG C, obtain SiC nanocrystalline/Graphene hetero-junctions.
The method preparing nanometer silicon carbide crystalline substance/Graphene hetero-junctions provided by the invention, by SiC nano-crystalline granule in vacuum or argon gas atmosphere, carry out annealing in process in 1000 DEG C-1600 DEG C, obtain by the SiC nano-crystalline granule of graphene coated, thus obtain SiC nanocrystalline/Graphene hetero-junctions.
Described method, wherein, described its crystal formation of SiC nano-crystalline granule is the single crystal form of 4H, 6H, 3C or the mixture of these crystal formations.
Described method, wherein, described SiC nano-crystalline granule grain size is within the scope of 50nm-500 μm.
Described method, wherein, described vacuum pressure is 1 × 10
-5between Pa-1kPa.
Described method, wherein, the described annealing in process time is 10 minutes-60 minutes.
Described method, wherein, in the SiC nano-crystalline granule of described graphene coated, the number of plies of Graphene controls the number of plies of Graphene between 1-10 layer by regulating annealing temperature, annealing time and ambiance.
SiC of the present invention is nanocrystalline/and Graphene hetero-junctions granular materials can be used in photocatalysis field, such as: the aspects such as photocatalysis field (comprising photocatalysis to degrade organic matter Sum decomposition water hydrogen manufacturing etc.), photocatalysis hydrogen production and sensitization solar battery.
Accompanying drawing explanation
Fig. 1 be the particle diameter yardstick prepared of the embodiment of the present invention 1 the SiC of 150 μm-300 μm nanocrystalline/the SEM shape appearance figure of Graphene hetero-junctions.
Fig. 2 be the particle diameter yardstick prepared of the embodiment of the present invention 2 the SiC of 50 μm-100 μm nanocrystalline/the SEM shape appearance figure of Graphene hetero-junctions.
Fig. 3 be under high-amplification-factor SiC nanocrystalline/Graphene heterojunction structure SEM shape appearance figure, the gauffer that Graphene produces due to thermal mismatching in surface of SiC is high-visible.
Fig. 4 be the particle diameter yardstick for preparing of the embodiment of the present invention 2 the SiC of 50nm-100nm nanocrystalline/the TEM X rays topographs of Graphene hetero-junctions.
Fig. 5 be SiC nanocrystalline/the Raman spectrogram of Graphene heterojunction material.Obvious G and 2D peak shows the surface of graphene growth at SiC crystal grain, forms SiC crystal grain/Graphene hetero-junctions.Wherein:
In Fig. 5 (a), G peak is comparatively strong, shows the Graphene thicker (thickness is about 2-3 nanometer) grown, and in Fig. 5 (b), G peak is more weak, shows the Graphene thinner (thickness is about 0.6-1.5 nanometer) grown.
Fig. 6 be particle diameter yardstick the SiC of 50 μm-100 μm nanocrystalline/Graphene heterojunction material and there is the comparison diagram of light degradation organic dyestuff (rhodamine B) of pure SiC particle of same size.Can obviously see from figure SiC nanocrystalline/photocatalytic degradation effect of Graphene hetero-junctions (red line) doubles than the photocatalytic degradation effect of pure SiC particle (black line).
Detailed description of the invention
In order to improve the interface quality of graphene/oxide compound, the compound of development and the perfect coated heterogeneous interface structure of preparation is the effective way and the method that improve photocatalysis performance further.Simultaneously, the SiC crystal grain that the present invention adopts has good photocatalysis performance [YantingGao as photocatalysis medium, YaquanWang*andYuxiaoWang, PhotocatalyticHydrogenEvolutionfromWateronSiCunderVisibl eLightIrradiation, React.Kinet.Catal.Lett.Vol.91, 13-19 (2007)], by growing a layer graphene (several atomic layers thick) at SiC grain surface, form the SiC crystal grain of graphene coated or be called SiC crystal grain/Graphene hetero-junctions, the photocatalysis performance of SiC crystal grain can be improved further.Provided by the invention nanocrystalline/Graphene heterojunction structure and preparation method thereof, lay the foundation for SiC nanocrystal/Graphene hetero-junctions in the application of photocatalysis field.
Basic step of the present invention is:
1) utilize the screening technique (as sub-sieve etc.) of conventional general nanoparticle size, select the SiC nano-crystalline granule with close grain size.
2) adopt the conventional chemical cleaning method to semi-conducting material removal impurity (as adopted acetone, absolute ethyl alcohol) to the nanocrystalline organics removal of SiC, then adopt hydrochloric acid cleaning to remove metal impurities, finally use deionized water ultrasonic cleaning several times.
3) the SiC nano-crystalline granule after cleaning is dried in an oven.
4) the SiC nano-crystalline granule after oven dry is put into vacuum high-temperature heating furnace, carry out the high temperature anneal, annealing temperature 1100 DEG C-1600 DEG C, annealing time 10-60 minute.Then Temperature fall, SiC is nanocrystalline/and the growth of Graphene hetero-junctions terminates.
5) SiC taking out preparation from growth furnace is nanocrystalline/Graphene heterojunction material, pending various sign and photocatalysis experiment.
The SiC obtained by said method is nanocrystalline/and Graphene heterojunction material can adopt SEM (SEM), transmission electron microscope (TEM) and Raman scattering experiment technology test and verify, and its effect in photocatalytic applications is by testing to the degradation experiment of organic matter (as rhodamine B).
According to method provided by the invention, wherein utilizing the SiC nano-crystalline granule with close particle diameter yardstick of the method choice such as sub-sieve, may be single crystal form, also may be the mixing of several single crystal form.These single crystal forms may be 4H, 6H, 3C and other possible crystal formation.Further, its grain size is within the scope of 50nm-500 μm.
According to method provided by the invention, wherein, SiC nano-crystalline granule carries out the environment of the high temperature anneal, namely can be high vacuum, and also can be low vacuum environment, environmental pressure scope be between 1 × 10
-5between Pa and 1kPa, ambiance is vacuum or argon gas.
According to method provided by the invention, wherein, the temperature of SiC nano-crystalline granule high annealing can be 1000 DEG C-1600 DEG C, and lower than the growth temperature 50 DEG C-200 DEG C of epitaxial graphene in SiC wafer, preferred range is 1100 DEG C-1300 DEG C.
According to method provided by the invention, wherein, the time of SiC nano-crystalline granule high annealing can be 10 minutes-60 minutes, and preferable range is 20-30 minute.
According to method provided by the invention; under different high annealing environment (vacuum environment and argon shield environment); can by regulation and control annealing temperature and annealing time, prepare the Graphene with the different number of plies (1-10 layer) and the nanocrystalline heterojunction structure of SiC.
According to method provided by the invention, the SiC of preparation is nanocrystalline/Graphene heterojunction structure, there is the structural advantage of following uniqueness:
1) compared with SiC body material, SiC nano-crystalline granule size is little, and the surface area that compares is large, and surface reaction activity significantly improves;
2) SiC nano-crystalline granule outer surface, coated graphite alkene layer, SiC Particle surface charge transfer ability gets a promotion, and is conducive to the carrying out of surface-catalyzed reactions;
3) the external sheath Graphene number of plies is controlled, thus regulates and controls SiC nano-crystalline granule surface charge transfer ability further, contributes to the controllability etc. improving surface reaction speed.
Therefore, the SiC of preparation provided by the invention is nanocrystalline/method of Graphene heterojunction structure and the nano heterojunction material that obtains in photocatalysis field (comprising photocatalysis to degrade organic matter Sum decomposition water hydrogen manufacturing etc.), have a wide range of applications potential.
Below in conjunction with specific embodiment, the present invention is described in further detail, the specific embodiment provided only in order to illustrate the present invention, instead of in order to limit the scope of the invention.
Embodiment 1:
The present embodiment for illustration of SiC nanocrystalline/preparation method of Graphene hetero-junctions.
1) utilize sub-sieve technology, adopt 80 mesh standard sieve nets, select the 6H-SiC nano-crystalline granule of particle diameter yardstick within the scope of 150 μm-300 μm.
2) acetone, absolute ethyl alcohol ultrasonic cleaning 6H-SiC nano-crystalline granule is adopted successively, and clean by washed with de-ionized water; Then with hydrochloric ultrasonic wave cleaning 6H-SiC nano-crystalline granule, and clean by washed with de-ionized water.
3) the SiC nano-crystalline granule after cleaning is dried in an oven.
4) the 6H-SiC nano-crystalline granule after drying is put into high-temperature heater, utilize mechanical pump and molecular pump to bleed process to furnace chamber, make vacuum in chamber reach 5 × 10
-3below Pa.While maintenance molecular pump continues to bleed to furnace chamber, be warming up to 1400 DEG C, and this temperature 10 minutes, then close heating power supply, and inject argon gas to 10kpa in furnace chamber, Temperature fall was to room temperature.
5) SiC taking out preparation from growth furnace is nanocrystalline/Graphene heterojunction material, and pending various photocatalysis experiment.
The SiC that embodiment 1 obtains is nanocrystalline/the SEM image of Graphene heterojunction material as shown in Figure 1.Its Raman spectrum clearly can see characteristic peak: G peak is (at 1582cm
-1) and 2D peak (at 2700cm
-1), and 2D peak is the unimodal of symmetry, as Fig. 5 (a)., and SiC characteristic peak (1516cm further
-1) compare, G peak intensity is comparatively strong, and show that thicker in the number of plies of the Graphene of SiC nano-crystalline granule outer cladding is 5-10 layer, quality is better.
Embodiment 2:
The present embodiment for illustration of SiC nanocrystalline-preparation method of Graphene heterojunction structure.
1) utilize sub-sieve technology, adopt 200 mesh standard sieve nets, select the 6H-SiC nano-crystalline granule of particle diameter yardstick within the scope of 50 μm-100 μm.
2) acetone, absolute ethyl alcohol ultrasonic cleaning 6H-SiC nano-crystalline granule is adopted successively, and clean by washed with de-ionized water; Then with hydrochloric ultrasonic wave cleaning 6H-SiC nano-crystalline granule, and clean by washed with de-ionized water.
3) the SiC nano-crystalline granule after cleaning is dried in an oven.
4) the 6H-SiC nano-crystalline granule after drying is put into high-temperature heater, utilize mechanical pump and molecular pump to bleed process to furnace chamber, make vacuum in chamber reach 5 × 10
-3below Pa.While maintenance molecular pump continues to bleed to furnace chamber, be warming up to 1200 DEG C, and this temperature 15 minutes, then close heating power supply, and inject argon gas to 10kPa in furnace chamber, Temperature fall was to room temperature.
5) SiC taking out preparation from growth furnace is nanocrystalline/Graphene heterojunction material, and pending various photocatalysis experiment.
According to the characterizing method similar to embodiment 1, adopt SEM to SiC nanocrystalline/Graphene hetero-junctions characterizes, as shown in Figure 2.Meanwhile, its Raman spectrum clearly can see characteristic peak: G peak is (at 1582cm
-1) and 2D peak (at 2700cm
-1), and 2D peak is the unimodal of symmetry, as Fig. 5 (b)., and SiC characteristic peak (1516cm further
-1) compare, G peak intensity is more weak, and show that thinner in the number of plies of the Graphene of SiC nano-crystalline granule outer cladding is 1-3 layer, quality is better.
Embodiment 3:
The present embodiment for illustration of SiC nanocrystalline-preparation method of Graphene heterojunction structure.
1) utilize sub-sieve technology, select the SiC nano-crystalline granule of the mixing crystal formation of particle diameter yardstick within the scope of 50nm-100nm.
2) the SiC nano-crystalline granule of acetone, absolute ethyl alcohol ultrasonic cleaning mixing crystal formation is adopted successively, and clean by washed with de-ionized water; Then nano-crystalline granule is cleaned with hydrochloric ultrasonic wave, and clean by washed with de-ionized water.
3) the SiC nano-crystalline granule after cleaning is dried in an oven.
4) the SiC nano-crystalline granule after drying is put into high-temperature heater, utilize mechanical pump and molecular pump to bleed process to furnace chamber, make vacuum in chamber reach 5 × 10
-3below Pa.While maintenance molecular pump continues to bleed to furnace chamber, be warming up to 1000 DEG C, and this temperature 30 minutes, then close heating power supply, and inject argon gas to 10kPa in furnace chamber, Temperature fall was to room temperature.
5) SiC taking out preparation from growth furnace is nanocrystalline/Graphene heterojunction material, and pending various photocatalysis experiment.
The SiC of mixing crystal formation that embodiment 2 obtains is nanocrystalline/the TEM picture of Graphene heterojunction material as shown in Figure 4.
Embodiment 4:
The present embodiment for illustration of SiC nanocrystalline/Graphene heterojunction structure improving the application potential of SiC nano-crystalline granule surface catalysis aspect of performance.
1) for the SiC particle of 50 μm-100 μm, according to method described in this paper, SiC Graphene heterojunction material is prepared.
2) by the SiC particle of identical weight 0.3 gram and SiC nanocrystalline/Graphene hetero-junctions particle is dispersed in (its concentration is 0.02mM) in the organic dyestuff rhodamine B solution of 100 milliliters respectively.
3) under the same conditions, with ultraviolet mercury lamp from the corresponding solution of vertical irradiation above, the solution taking out 3 milliliters every certain time interval (being generally 30 minutes) carries out organic dyestuff measurement of concetration, and concrete test result is as Fig. 6.
As can be seen from Figure 6 adopt SiC nanocrystalline/Graphene heterojunction material as catalyst when, the efficiency of photocatalytically degradating organic dye doubles than the simple degradation efficiency of SiC particle that adopts.Prove the SiC of preparation provided by the invention nanocrystalline/material that obtains of the method for Graphene hetero-junctions has obvious effect improving in photocatalysis usefulness.
Claims (2)
1. a SiC nanocrystalline/application of Graphene nucleocapsid structure hetero-junctions granular materials in photocatalysis field;
This SiC is nanocrystalline/and Graphene nucleocapsid structure hetero-junctions granular materials prepared by the following method:
By SiC nano-crystalline granule in a vacuum, carry out annealing in process in 1000 DEG C-1600 DEG C, obtain SiC nanocrystalline/Graphene nucleocapsid structure hetero-junctions;
Wherein, the crystal formation of this SiC nano-crystalline granule is the single crystal form of 4H, 6H, 3C or the mixture of these crystal formations, and the grain size of this SiC nano-crystalline granule is within the scope of 50nm-500 μm;
Vacuum pressure is 1 × 10
-5between Pa-1kPa;
The annealing in process time is 10-60 minute;
The SiC prepared is nanocrystalline/Graphene nucleocapsid structure hetero-junctions granular materials in, the number of plies of Graphene controls the number of plies of Graphene between 1-10 layer by regulating annealing temperature, annealing time and ambiance.
2. application according to claim 1, wherein, the SiC of preparation is nanocrystalline/and Graphene nucleocapsid structure hetero-junctions particle is applied to light degradation organic matter, photocatalysis hydrogen production and sensitization solar battery.
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| CN110354879B (en) * | 2018-04-10 | 2022-03-01 | Tcl科技集团股份有限公司 | Composite material and preparation method thereof |
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| CN110028070B (en) * | 2019-05-09 | 2020-10-23 | 清芯未来(北京)科技有限公司 | Single crystal silicon carbide/graphene core-shell structure nanofiber and preparation method and application thereof |
| CN115106106B (en) * | 2022-06-23 | 2023-03-14 | 广东工业大学 | Graphene-loaded silicon carbide photocatalyst for hydrogen production by visible light and preparation method thereof |
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