CN106920855A - CdSe quantum dots and nanoporous carbon composite and preparation method thereof - Google Patents
CdSe quantum dots and nanoporous carbon composite and preparation method thereof Download PDFInfo
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- CN106920855A CN106920855A CN201710202017.9A CN201710202017A CN106920855A CN 106920855 A CN106920855 A CN 106920855A CN 201710202017 A CN201710202017 A CN 201710202017A CN 106920855 A CN106920855 A CN 106920855A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 148
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical class [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 title claims abstract description 144
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 142
- 239000002131 composite material Substances 0.000 title claims abstract description 77
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- -1 zeolite imidazoles esters Chemical class 0.000 claims abstract description 15
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 14
- 239000010457 zeolite Substances 0.000 claims abstract description 14
- 239000013256 coordination polymer Substances 0.000 claims abstract description 12
- 229920001795 coordination polymer Polymers 0.000 claims abstract description 12
- 239000011148 porous material Substances 0.000 claims abstract description 12
- 239000011261 inert gas Substances 0.000 claims abstract description 11
- 238000011065 in-situ storage Methods 0.000 claims abstract description 8
- 150000001661 cadmium Chemical class 0.000 claims description 27
- 239000007789 gas Substances 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 12
- 239000002096 quantum dot Substances 0.000 claims description 12
- 230000001186 cumulative effect Effects 0.000 claims description 11
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims description 9
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical group OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims description 9
- 229910000058 selane Inorganic materials 0.000 claims description 9
- 239000013154 zeolitic imidazolate framework-8 Substances 0.000 claims description 9
- MFLKDEMTKSVIBK-UHFFFAOYSA-N zinc;2-methylimidazol-3-ide Chemical group [Zn+2].CC1=NC=C[N-]1.CC1=NC=C[N-]1 MFLKDEMTKSVIBK-UHFFFAOYSA-N 0.000 claims description 9
- 229910052793 cadmium Inorganic materials 0.000 claims description 8
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 8
- 239000011669 selenium Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 229910052711 selenium Inorganic materials 0.000 claims description 6
- 239000012159 carrier gas Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000002242 deionisation method Methods 0.000 claims description 2
- 239000013158 zeolitic imidazolate framework-68 Substances 0.000 claims description 2
- 239000013159 zeolitic imidazolate framework-69 Substances 0.000 claims description 2
- 239000013160 zeolitic imidazolate framework-70 Substances 0.000 claims description 2
- 239000013163 zeolitic imidazolate framework-82 Substances 0.000 claims description 2
- 239000013162 zeolitic imidazolate framework-81 Substances 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 12
- 238000007146 photocatalysis Methods 0.000 abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 18
- 238000000034 method Methods 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- 229910052757 nitrogen Inorganic materials 0.000 description 9
- 239000000463 material Substances 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 206010013786 Dry skin Diseases 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000007654 immersion Methods 0.000 description 5
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 241000209094 Oryza Species 0.000 description 4
- 235000007164 Oryza sativa Nutrition 0.000 description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 229910021645 metal ion Inorganic materials 0.000 description 4
- 235000009566 rice Nutrition 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- 229910052725 zinc Inorganic materials 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 229910052738 indium Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000012621 metal-organic framework Substances 0.000 description 3
- SPVXKVOXSXTJOY-UHFFFAOYSA-N selane Chemical compound [SeH2] SPVXKVOXSXTJOY-UHFFFAOYSA-N 0.000 description 3
- 239000002023 wood Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000013153 zeolitic imidazolate framework Substances 0.000 description 2
- YBNMDCCMCLUHBL-UHFFFAOYSA-N (2,5-dioxopyrrolidin-1-yl) 4-pyren-1-ylbutanoate Chemical compound C=1C=C(C2=C34)C=CC3=CC=CC4=CC=C2C=1CCCC(=O)ON1C(=O)CCC1=O YBNMDCCMCLUHBL-UHFFFAOYSA-N 0.000 description 1
- 229910000673 Indium arsenide Inorganic materials 0.000 description 1
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- AMULVJPCIVLXGR-UHFFFAOYSA-N cadmium(2+) ethanol dinitrate Chemical compound C(C)O.[N+](=O)([O-])[O-].[Cd+2].[N+](=O)([O-])[O-] AMULVJPCIVLXGR-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- RPQDHPTXJYYUPQ-UHFFFAOYSA-N indium arsenide Chemical compound [In]#[As] RPQDHPTXJYYUPQ-UHFFFAOYSA-N 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000320 mechanical mixture Substances 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 150000003342 selenium Chemical class 0.000 description 1
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0352—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their shape or by the shapes, relative sizes or disposition of the semiconductor regions
- H01L31/035209—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their shape or by the shapes, relative sizes or disposition of the semiconductor regions comprising a quantum structures
- H01L31/035218—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their shape or by the shapes, relative sizes or disposition of the semiconductor regions comprising a quantum structures the quantum structure being quantum dots
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/028—Inorganic materials including, apart from doping material or other impurities, only elements of Group IV of the Periodic Table
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/0296—Inorganic materials including, apart from doping material or other impurities, only AIIBVI compounds, e.g. CdS, ZnS, HgCdTe
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- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Electromagnetism (AREA)
- General Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Luminescent Compositions (AREA)
Abstract
The present invention provides a kind of CdSe quantum dots and nanoporous carbon composite and preparation method thereof.The CdSe quantum dots and nanoporous carbon composite are compounded to form by CdSe quantum dots and nanoporous carbon; the CdSe quantum dots growth in situ is obtained in the surface of the nanoporous carbon, the nanoporous carbon by the calcined zeolite imidazoles esters coordination polymer under inert gas shielding.Nanoporous carbon of the invention has the advantages that specific surface area is big, duct is uniform, pore size is big, the decentralization of CdSe quantum dots can be improved when composite is formed with CdSe quantum dots, control the crystallite dimension of CdSe quantum dots, reduce the generation of the CdSe quantum dots of small size, make the photocatalysis efficiency of composite and life-span be improved significantly.
Description
Technical field
The present invention relates to quantum dot synthetic method technical field, more particularly to a kind of CdSe quantum dots and nanoporous carbon
Composite and preparation method thereof.
Background technology
Direct conversion solar can be electric energy or chemical energy, or have important meaning using Driven by Solar Energy chemical reaction process
Justice, for example, can solve the problems, such as that fossil fuel faces exhaustion, and relatively for fossil fuel, solar energy is more cleaned.
In sunshine, ultraviolet light only account for sunshine gross energy~5%, it is seen that light account for sunshine gross energy~45%, due to purple
Outer smooth photon energy is higher, may destroy the structure of organic material, therefore it is mesh rationally efficiently to utilize the visible ray in sunshine
One of focus of preceding Photochemistry Study.
Quantum dot (QD, quantum dot), such as CdS, CdSe, ZnSe, ZnO, InP, InAs, PbSe etc., energy gap
Eg<3.2eV, there is absorption to visible ray, in addition due also to mature preparation process and price is relatively low, has in terms of using visible ray
Wide application prospect.The photoelectric properties of QD are related to the particle diameter of QD, but the group between the reduction of the particle diameter with QD, QD
Party increases, therefore need to introduce cap reagent, but the introduced inevitable light conversion efficiency on QD of cap reagent produces influence.
In addition, the reduction of the particle diameter with QD, the defect increase on QD surfaces, cause the non-radiative recombination of photo-generate electron-hole, so as to drop
Low photo-quantum efficiency (<10%).Additionally, also easily there is photoetch compared with the QD of small particle.Solving a method of this problem is
QD and other materials are constituted into composite, is improved electron injection and is improved photo-generate electron-hole separation, and then improve light quantum effect
Rate.
Commonsense method prepare activated carbon specific surface area is low, duct is uneven, constituting composite wood with CdSe quantum dots
During material, because the specific surface area of the activated carbon of commonsense method preparation is small, the decentralization of CdSe quantum dots is smaller, namely active sites
Point is few, causes the photocatalysis efficiency of composite low；The duct of the activated carbon prepared additionally, due to commonsense method is uneven also
The crystallite dimension of CdSe quantum dots is caused to be difficult to control to.Although super-active carbon specific surface area is big, in preparation process by
A large amount of micropores can be produced in super-active carbon in the presence of activator, when CdSe quantum dots and super-active carbon constitute composite wood
The CdSe quantum dots of substantial amounts of small particle size can be produced during material, due to CdSe quantum dots when particle diameter is smaller easily reunite and
Easily there is photoetch in light reaction procedure, therefore photocatalysis efficiency and the life-span of composite can be reduced.Additionally, super work
The uneven crystallite dimension for also resulting in CdSe quantum dots in duct of property carbon is difficult to control to.
The content of the invention
In view of problem present in background technology, more it is an object of the invention to provide a kind of CdSe quantum dots and nanometer
Hole carbon composite and preparation method thereof, it is excellent that the nanoporous carbon has that specific surface area is big, duct is uniform, pore size is big
Point, the decentralization of CdSe quantum dots can be improved when composite is formed with CdSe quantum dots, control CdSe quantum dots
Crystallite dimension, reduce small size CdSe quantum dots generation, obtain the photocatalysis efficiency of composite and life-span
It is obviously improved.
Another object of the present invention is to provide a kind of CdSe quantum dots and nanoporous carbon composite and its preparation
The preparation method raw material availability of method, the CdSe quantum dots and nanoporous carbon composite is high, process is simple.
In order to achieve the above object, in one aspect of the invention, the invention provides a kind of CdSe quantum dots and nanometer
Porous carbon composite, it is compounded to form by CdSe quantum dots and nanoporous carbon, the CdSe quantum dots growth in situ
In the surface of the nanoporous carbon, the nanoporous carbon is coordinated by the calcined zeolite imidazoles esters under inert gas shielding
Polymer is obtained.
In another aspect of this invention, the invention provides a kind of CdSe quantum dots and nanoporous carbon composite
Preparation method, for preparing CdSe quantum dots and nanoporous carbon composite described in one aspect of the present invention, including step：
At normal temperatures and pressures, cadmium salt soln is distributed to inside nanoporous carbon in equal volume, then passes to excessive make with inert gas
It is the hydrogen selenide gas of carrier gas, after reaction terminates, scrubbed, vacuum drying, obtains CdSe quantum dots and nanoporous carbon is multiple
Condensation material, wherein, the CdSe quantum dots growth in situ passes through in the surface of the nanoporous carbon, the nanoporous carbon
Calcined zeolite imidazoles esters coordination polymer is obtained under inert gas shielding.Isometric dispersion refers to the cadmium salt soln
Cumulative volume it is equal with the volume of the solvent for dissolving cadmium salt that the nanoporous carbon to be adsorbed.
Relative to prior art, beneficial effects of the present invention are：
In CdSe quantum dots of the invention and nanoporous carbon composite, nanoporous carbon is by inert gas
The lower calcined zeolite imidazoles esters coordination polymer of protection is obtained, with specific surface area it is big, that duct is uniform, pore size is big is excellent
Point, the decentralization of CdSe quantum dots can be improved when composite is formed with CdSe quantum dots, control CdSe quantum dots
Crystallite dimension, reduce small size CdSe quantum dots generation, obtain the photocatalysis efficiency of composite and life-span
It is obviously improved.
The preparation method raw material availability of CdSe quantum dots of the invention and nanoporous carbon composite is high, technique is simple
It is single.
The long lifespan of CdSe quantum dots of the invention and nanoporous carbon composite, can the structure several months be under light illumination
Change, it is adaptable to the hydrogen manufacturing of light splitting water, photocatalysis and light degradation.
Brief description of the drawings
Fig. 1 is X-ray diffraction (XRD) figure for the CdSe@NPC composites that embodiment 1 is obtained.
Fig. 2 is transmission electron microscope (TEM) figure for the CdSe@NPC composites that embodiment 1 is obtained.
Specific embodiment
The following detailed description of CdSe quantum dots of the invention and nanoporous carbon composite and preparation method thereof.
CdSe quantum dots and nanoporous carbon composite according to a first aspect of the present invention are illustrated first.
CdSe quantum dots and nanoporous carbon composite (being abbreviated as CdSe@NPC) according to a first aspect of the present invention
It is to be compounded to form by CdSe quantum dots and nanoporous carbon (NPC, Nanoporous Carbon), the CdSe quantum dots
, in the surface of the nanoporous carbon, the nanoporous carbon is by the calcined zeolite imidazoles under inert gas shielding for growth in situ
Esters coordination polymer (being abbreviated as ZIF) is obtained.
In the CdSe quantum dots described in first aspect present invention and nanoporous carbon composite, in the cadmium selenide
In quantum dot and nanoporous carbon composite, CdSe quantum dots and nanoporous carbon are not simple mechanical mixtures, but
CdSe quantum dots growth in situ is in the surface of the nanoporous carbon.
In the CdSe quantum dots described in first aspect present invention and nanoporous carbon composite, nanoporous carbon leads to
The calcined zeolite imidazoles esters coordination polymer under inert gas shielding is crossed to obtain, therefore the nanoporous carbon has specific surface
The big advantage of product, can improve the decentralization of CdSe quantum dots, and the duct of the nanoporous carbon is uniform, can control cadmium selenide amount
The crystallite dimension of son point, the pore size of the nanoporous carbon is big, can reduce the generation of the CdSe quantum dots of small size, makes
The photocatalysis efficiency of composite and life-span be improved significantly.
In CdSe quantum dots described according to a first aspect of the present invention and nanoporous carbon composite, metal is organic
Skeleton coordination polymer (MOF) material is the class for occurring in recent years by organic ligand and metal ion or metal ion cluster
A class high-crystallinity, the porous material of high-specific surface area for constituting.Wherein ZIF materials are by imidazoles or imdazole derivatives and gold
Category ion Zn2+/Co2+Constitute with zeolite structured MOF materials, its heat endurance high and change both with inorganic zeolite
Learn stability, and duct adjustability and big specific surface area with metal organic complex.
In CdSe quantum dots described according to a first aspect of the present invention and nanoporous carbon composite, it is preferable that
The zeolite imidazole esters coordination polymer is selected from ZIF-8, ZIF-67, ZIF-68, ZIF-69, ZIF-70, ZIF-79, ZIF-
81st, one or more in ZIF-82.ZIF-8 and ZIF-67 are the zeolite imidazole esters coordination polymers of typical SOD series,
It should be noted that ZIF-8 and ZIF-67 are homogeneous structures, difference is that the metal ion in ZIF-8 is Zn2+, in ZIF-67
Metal ion is Co2+。
In CdSe quantum dots described according to a first aspect of the present invention and nanoporous carbon composite, the selenizing
The BET specific surface area of cadmium quantum dot and nanoporous carbon composite is 300m2/ g~1200m2/g。
In CdSe quantum dots described according to a first aspect of the present invention and nanoporous carbon composite, in the selenium
In cadmium quantum dot and nanoporous carbon composite, the weight/mass percentage composition of CdSe quantum dots is 5%~30%.
In CdSe quantum dots described according to a first aspect of the present invention and nanoporous carbon composite, in the selenium
In cadmium quantum dot and nanoporous carbon composite, CdSe quantum dots are Emission in Cubic, the crystallite dimension of CdSe quantum dots
It is 15nm~30nm.Preferably, the crystallite dimension of CdSe quantum dots is 18nm~22nm.
In CdSe quantum dots described according to a first aspect of the present invention and nanoporous carbon composite, in the selenium
In cadmium quantum dot and nanoporous carbon composite, the BET specific surface area of the nanoporous carbon is 1300m2/ g~
1800m2/ g, the pore size of the nanoporous carbon is 3.5nm~4.5nm, it is preferable that the duct chi of the nanoporous carbon
Very little is 4nm.
In CdSe quantum dots described according to a first aspect of the present invention and nanoporous carbon composite, the inertia
Gas is selected from nitrogen or argon gas.
In CdSe quantum dots described according to a first aspect of the present invention and nanoporous carbon composite, the calcining
Temperature can be 800 DEG C~1000 DEG C.The preparation method of the nanoporous carbon is referred to：Hai-Long Jiang etal.,
From Metal-Organic Framework to Nanoporous Carbon:Toward a Very High Surface
Area and Hydrogen Uptake, J.Am.Chem.Soc., 2011,133,11854-11857 and Nagy L.Torad
etal.,Facile synthesis of nanoporous carbons with controlled particle sizes
by direct carbonization of monodispersed ZIF-8crystals,Chem.Commun.,2013,49,
2521-2523。
Secondly the preparation side of CdSe quantum dots and nanoporous carbon composite according to a second aspect of the present invention is illustrated
Method.
CdSe quantum dots according to a second aspect of the present invention and the preparation method of nanoporous carbon composite, for making
CdSe quantum dots and nanoporous carbon composite described in standby first aspect present invention, including step：At normal temperatures and pressures,
Cadmium salt soln is distributed to inside nanoporous carbon in equal volume, the excessive hydrogen selenide using inert gas as carrier gas is then passed to
Gas, after reaction terminates, scrubbed, vacuum drying obtains CdSe quantum dots and nanoporous carbon composite, wherein, institute
CdSe quantum dots growth in situ is stated in the surface of the nanoporous carbon, the nanoporous carbon is by inert gas shielding
Lower calcined zeolite imidazoles esters coordination polymer is obtained.It is described it is isometric dispersion refer to the cadmium salt soln cumulative volume with it is described
The volume of the nanoporous carbon solvent for dissolving cadmium salt to be adsorbed is equal.
In CdSe quantum dots described according to a second aspect of the present invention and the preparation method of nanoporous carbon composite
In, the CdSe quantum dots and the raw material availability of nanoporous carbon composite that are obtained by equi-volume process are high, process is simple.
Resulting CdSe quantum dots and nanoporous carbon composite long lifespan, can under light illumination the structure several months do not change,
Suitable for the hydrogen manufacturing of light splitting water, photocatalysis and light degradation.
In CdSe quantum dots described according to a second aspect of the present invention and the preparation method of nanoporous carbon composite
In, CdSe quantum dots and nanoporous carbon composite, the cumulative volume of the cadmium salt soln are prepared by isometric dispersion method
Volume with the solvent for dissolving cadmium salt that nanoporous carbon to be adsorbed is equal.If the totality of the cadmium salt soln for adding
Product is larger and quality of nanoporous carbon is relatively small, then formed CdSe quantum dots major part can be caused to remain in solution
In, cause the raw material availability of CdSe quantum dots to decline and the CdSe quantum dots for obtaining and nanoporous carbon composite wood can be made
Expecting to be separated with the CdSe quantum dots being formed in solution becomes difficult；If add cadmium salt soln cumulative volume it is smaller and
The relative mass of nanoporous carbon is larger, then the amount in the CdSe quantum dots of nanoporous supported on carbon surface can be caused to reduce,
Reduce the photocatalysis efficiency of CdSe quantum dots and nanoporous carbon composite, and due to the volume of cadmium salt soln for adding
Smaller, causing the nanoporous carbon of part cannot effectively contact with cadmium salt soln so that the CdSe quantum dots of growth are in nanometer
The skewness of porous carbon surface, can also influence the photocatalysis efficiency of CdSe quantum dots and nanoporous carbon composite.
In CdSe quantum dots described according to a second aspect of the present invention and the preparation method of nanoporous carbon composite
In, specifically, the cumulative volume of cadmium salt soln is 1ml with the ratio of the quality of nanoporous carbon：1g.I.e. per 1g nanoporous carbon certainly
Body can adsorb 1ml for dissolving the solvent (such as ethanol, deionized water or the mixed solution of the two) of cadmium salt, therefore, often add
Enter the cadmium salt soln that 1g nanoporous carbon needs correspondence to add cumulative volume for 1ml.
In CdSe quantum dots described according to a second aspect of the present invention and the preparation method of nanoporous carbon composite
In, in the cadmium salt soln, cadmium salt is selected from cadmium nitrate or caddy, and the solvent for dissolving cadmium salt is selected from ethanol, deionization
Water or the mixed solution of the two.
In CdSe quantum dots described according to a second aspect of the present invention and the preparation method of nanoporous carbon composite
In, the mass percent concentration of the cadmium salt soln is 10%~40%.
In CdSe quantum dots described according to a second aspect of the present invention and the preparation method of nanoporous carbon composite
In, the hydrogen selenide gas may be from commercially available hydrogen selenide gas or the hydrogen selenide gas prepared using selenium salt.
With reference to embodiment, the application is expanded on further.It should be understood that these embodiments be merely to illustrate the application without
For limiting scope of the present application.
Embodiment 1
Under nitrogen protection, ZIF-8 and 4 times of KOH of mol ratio is calcined 3 hours at 1000 DEG C, is then lowered the temperature, product
Metallic zinc is removed through concentrated hydrochloric acid immersion, is washed three times, by black powder in 120 DEG C of dryings 12 hours, obtain nanoporous carbon, received
The BET specific surface area of rice porous carbon is 1800m2/ g, pore size is 3.7nm.
At normal temperatures and pressures, by cadmium nitrate aqueous dispersion receiving to 100mg that 0.1ml mass percent concentrations are 40%
In rice porous carbon, then nitrogen buffer gas are passed through excessive H2Se gases, after reaction terminates, are washed three times with ethanol, then 60
DEG C vacuum drying 8 hours, that is, obtain CdSe NPC composites.
CdSe@NPC composites through X-ray polycrystalline diffraction, show nanoporous carbon load CdSe quantum dots after
Structure does not change, and 2 θ show that the CdSe quantum dots of generation are Emission in Cubic (see figure in 25.3 °, 42 °, 49.7 ° of diffraction maximum
1).TEM (transmission electron microscope) gives the surface topography (see Fig. 2) of CdSe@NPC composites.Wherein, cadmium selenide quantum
The crystallite dimension of point is about 20nm.N under 77K2Isothermal adsorption test shows that the BET specific surface area of CdSe@NPC composites is
300m2/g.ICP-AES test results show that weight/mass percentage composition of the CdSe quantum dots in CdSe@NPC composites is
30%.
Embodiment 2
Under nitrogen protection, ZIF-8 and 4 times of KOH of mol ratio is calcined 3 hours at 900 DEG C, is then lowered the temperature, product
Metallic zinc is removed through concentrated hydrochloric acid immersion, is washed three times, by black powder in 120 DEG C of dryings 12 hours, obtain nanoporous carbon, received
The BET specific surface area of rice porous carbon is 1500m2/ g, pore size is 3.9nm.
At normal temperatures and pressures, by caddy aqueous dispersion receiving to 100mg that 0.1ml mass percent concentrations are 20%
In rice porous carbon, the then excessive H with argon gas as carrier gas is passed through2Se gases, after reaction terminates, are washed three times with ethanol, then 60
DEG C vacuum drying 8 hours, that is, obtain CdSe NPC composites.
CdSe@NPC composites are through X-ray polycrystalline diffraction, and structure is similar to Example 1.N under 77K2Isothermal adsorption
Test shows that the BET specific surface area of CdSe@NPC composites is 739m2/g.ICP-AES test results show, cadmium selenide amount
Son point weight/mass percentage composition in CdSe@NPC composites is 20%.In CdSe@NPC composites, CdSe quantum dots
Crystallite dimension be about 22nm.
Embodiment 3
Under nitrogen protection, ZIF-67 and 4 times of KOH of mol ratio is calcined 3 hours at 800 DEG C, is then lowered the temperature, product
Metallic cobalt is removed through concentrated hydrochloric acid immersion, is washed three times, black powder obtained nanoporous carbon, nanometer in 120 DEG C of dryings 12 hours
The BET specific surface area of porous carbon is 1300m2/ g, pore size is 4.3nm.
At normal temperatures and pressures, the cadmium nitrate ethanol solution that 0.1ml mass percent concentrations are 10% is distributed to 100mg's
In nanoporous carbon, the then excessive H with argon gas as carrier gas is passed through2Se gases, after reaction terminates, are washed three times with ethanol, then
60 DEG C are vacuum dried 8 hours, that is, obtain CdSe NPC composites.
CdSe@NPC composites are through X-ray polycrystalline diffraction, and structure is similar to Example 1.N under 77K2Isothermal adsorption
Test shows that the BET specific surface area of CdSe@NPC composites is 1200m2/g.ICP-AES test results show, cadmium selenide amount
Son point weight/mass percentage composition in CdSe@NPC composites is 5%.In CdSe@NPC composites, CdSe quantum dots
Crystallite dimension is about 18nm.
Comparative example 1
Under nitrogen protection, ZIF-8 and 4 times of KOH of mol ratio is calcined 3 hours at 1000 DEG C, is then lowered the temperature, product
Metallic zinc is removed through concentrated hydrochloric acid immersion, is washed three times, black powder obtained nanoporous carbon, nanometer in 120 DEG C of dryings 12 hours
The BET specific surface area of porous carbon is 1800m2/ g, pore size is 3.7nm.
At normal temperatures and pressures, by cadmium nitrate aqueous dispersion that 10.0ml mass percent concentrations are 40% to 100mg's
In nanoporous carbon, then nitrogen buffer gas are passed through excessive H2Se gases, after reaction terminates, are washed three times with ethanol, then
60 DEG C are vacuum dried 8 hours, that is, obtain CdSe NPC composites.
N under 77K2Isothermal adsorption test shows that the BET specific surface area of CdSe@NPC composites is 350m2/g。ICP-AES
Test result shows that weight/mass percentage composition of the CdSe quantum dots in CdSe@NPC composites is 29.3%.
Because the cumulative volume of the cadmium nitrate aqueous solution for adding is larger and quality of nanoporous carbon is relatively small, cause institute's shape
Into the most of residual of CdSe quantum dots in the solution, cause the raw material availability of CdSe quantum dots to decline and can make to obtain
CdSe@NPC composites separated with the CdSe quantum dots being formed in solution and become difficult, reduce production efficiency.
Comparative example 2
Under nitrogen protection, ZIF-8 and 4 times of KOH of mol ratio is calcined 3 hours at 1000 DEG C, is then lowered the temperature, product
Metallic zinc is removed through concentrated hydrochloric acid immersion, is washed three times, black powder obtained nanoporous carbon, nanometer in 120 DEG C of dryings 12 hours
The BET specific surface area of porous carbon is 1800m2/ g, pore size is 3.7nm.
At normal temperatures and pressures, by cadmium nitrate aqueous dispersion that 0.05ml mass percent concentrations are 40% to 100mg's
In nanoporous carbon, then nitrogen buffer gas are passed through excessive H2Se gases, after reaction terminates, are washed three times with ethanol, then
60 DEG C are vacuum dried 8 hours, that is, obtain CdSe NPC composites.
N under 77K2Isothermal adsorption test shows that the BET specific surface area of CdSe@NPC composites is 750m2/g。ICP-AES
Test result shows that weight/mass percentage composition of the CdSe quantum dots in CdSe@NPC composites is 15.4%.In CdSe@
In NPC composites, the crystallite dimension of CdSe quantum dots is about 20nm.
Because the cumulative volume of the cadmium nitrate aqueous solution is smaller, nanoporous carbon relative mass is larger, causes in nanoporous
The amount of the CdSe quantum dots of load is reduced in carbon, reduces the photocatalysis efficiency of CdSe@NPC composites, and due to adding
The cadmium nitrate aqueous solution cumulative volume it is smaller, causing the nanoporous carbon of part cannot effectively contact with the cadmium nitrate aqueous solution, make
Distribution of the CdSe quantum dots that must be formed on nanoporous carbon surface is also uneven, can also influence CdSe@NPC composites
Photocatalysis efficiency.
Claims (10)
1. a kind of CdSe quantum dots and nanoporous carbon composite, it is characterised in that the composite is by cadmium selenide amount
Son point and nanoporous carbon are compounded to form, and the CdSe quantum dots growth in situ is described in the surface of the nanoporous carbon
Nanoporous carbon is obtained by the calcined zeolite imidazoles esters coordination polymer under inert gas shielding.
2. CdSe quantum dots according to claim 1 and nanoporous carbon composite, it is characterised in that the zeolite
Imidazoles esters coordination polymer is selected from ZIF-8, ZIF-67, ZIF-68, ZIF-69, ZIF-70, ZIF-79, ZIF-81, ZIF-82
In one or more.
3. CdSe quantum dots according to claim 1 and nanoporous carbon composite, it is characterised in that the selenizing
The BET specific surface area of cadmium quantum dot and nanoporous carbon composite is 300m2/ g~1200m2/g。
4. CdSe quantum dots according to claim 1 and nanoporous carbon composite, it is characterised in that in the selenium
In cadmium quantum dot and nanoporous carbon composite, the weight/mass percentage composition of CdSe quantum dots is 5%~30%.
5. CdSe quantum dots according to claim 1 and nanoporous carbon composite, it is characterised in that in the selenium
In cadmium quantum dot and nanoporous carbon composite, CdSe quantum dots are Emission in Cubic, the crystallite dimension of CdSe quantum dots
It is 15nm~30nm, it is preferable that the crystallite dimension of CdSe quantum dots is 18nm~22nm.
6. CdSe quantum dots according to claim 1 and nanoporous carbon composite, it is characterised in that in the selenium
In cadmium quantum dot and nanoporous carbon composite, the BET specific surface area of the nanoporous carbon is 1300m2/ g~
1800m2/ g, the pore size of the nanoporous carbon is 3.5nm~4.5nm, it is preferable that the duct chi of the nanoporous carbon
Very little is 4nm.
7. the preparation method of a kind of CdSe quantum dots and nanoporous carbon composite, appoint in claim 1-6 for preparing
CdSe quantum dots and nanoporous carbon composite described in one, it is characterised in that including step：
At normal temperatures and pressures, cadmium salt soln is distributed to inside nanoporous carbon in equal volume, is then passed to excessive with indifferent gas
Body is reacted after terminating as the hydrogen selenide gas of carrier gas, scrubbed, vacuum drying, obtains CdSe quantum dots and nanoporous
Carbon composite, wherein, the CdSe quantum dots growth in situ is in the surface of the nanoporous carbon, the nanoporous carbon
Obtained by the calcined zeolite imidazoles esters coordination polymer under inert gas shielding；
Wherein, isometric dispersion refers to the cumulative volume and the use to be adsorbed of nanoporous carbon of the cadmium salt soln
It is equal in the volume of the solvent of dissolving cadmium salt.
8. the preparation method of CdSe quantum dots according to claim 7 and nanoporous carbon composite, cadmium salt soln
The ratio of quality of cumulative volume and nanoporous carbon be 1ml：1g.
9. the preparation method of CdSe quantum dots according to claim 8 and nanoporous carbon composite, its feature exists
In in the cadmium salt soln, cadmium salt is selected from cadmium nitrate or caddy, and the solvent for dissolving cadmium salt is selected from ethanol, deionization
Water or the mixed solution of the two.
10. the preparation method of CdSe quantum dots according to claim 7 and nanoporous carbon composite, its feature exists
In the mass percent concentration of the cadmium salt soln is 10%~40%.
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| CN101884620A (en) * | 2010-05-28 | 2010-11-17 | 同济大学 | Activated carbon granule of load quantum dots as well as preparation method and application thereof |
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| CN106252676A (en) * | 2016-07-28 | 2016-12-21 | 青岛大学 | A kind of quantum dot modified metal organic backbone embeds the preparation of carbon nano-tube material |
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| CN101884620A (en) * | 2010-05-28 | 2010-11-17 | 同济大学 | Activated carbon granule of load quantum dots as well as preparation method and application thereof |
| CN104201385A (en) * | 2014-08-14 | 2014-12-10 | 中国科学技术大学 | Preparation method of high-nitrogen-doped graphene nanoparticles and application of high-nitrogen-doped graphene nanoparticles as negative material of lithium ion battery |
| US20160144348A1 (en) * | 2014-11-20 | 2016-05-26 | Korea Institute Of Science And Technology | Photocatalyst using semiconductor-carbon nanomaterial core-shell composite quantum dot and method for preparing the same |
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