CN107010653A - The cubical method of zinc blende-type cadmium sulfide nano is synthesized using cation exchange - Google Patents
The cubical method of zinc blende-type cadmium sulfide nano is synthesized using cation exchange Download PDFInfo
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- CN107010653A CN107010653A CN201710298022.4A CN201710298022A CN107010653A CN 107010653 A CN107010653 A CN 107010653A CN 201710298022 A CN201710298022 A CN 201710298022A CN 107010653 A CN107010653 A CN 107010653A
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- necked flask
- cadmium sulfide
- oleyl amine
- sulfide nano
- zinc blende
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G11/00—Compounds of cadmium
- C01G11/02—Sulfides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses one kind the cubical method of zinc blende-type cadmium sulfide nano is synthesized using cation exchange, sulphur powder and oleyl amine are first placed in ultrasonic disperse in conical flask, lead chloride and oleyl amine are placed in three-necked flask again, conical flask solution is injected in three-necked flask again, the colloidal solution of black vulcanized lead is formed, after colloidal solution cooling, centrifuge product and solvent, products therefrom is cleaned and centrifuged with ethanol, vacuum dried, obtains vulcanized lead nanocube；Again by vulcanized lead nanocube ultrasonic disperse in octadecylene, black liquor is formed；Cadmium acetate, oleic acid and oleyl amine dissolving are added in three-necked flask, argon gas is passed through, heats under magnetic stirring, then by black liquor injection wherein, progressively heats up, is cooled to room temperature, product is separated with solution centrifugal, obtain zinc blende-type cadmium sulfide nano cube.The present invention can keep cubical pattern, while (100) crystal face of exposure high energy, realizes the controlledly synthesis of high duplication.
Description
Technical field
The present invention is that, on semiconductor catalyst, more particularly to one kind synthesizes small size zincblende using cation exchange
The cubical method of type cadmium sulfide nano.
Background technology
In semiconductor catalyst, cadmium sulfide (CdS) material preferably absorbs and conduction band because it has to visible light wave range
Position is also applied for the fields such as photolysis water hydrogen and thin-film solar cells, thus it is of great interest, referring to Wu K,
Chen Z,Lv H,et al.Hole Removal Rate Limits Photodriven H 2Generation
Efficiency in CdS-Pt and CdSe/CdS-Pt Semiconductor Nanorod–Metal Tip
Heterostructures[J].Journal of the American Chemical Society,2014,136(21):
7708-7716。
The pattern of common vulcanization cadmium material has the quasi- spherical nanoparticles of Hydrothermal Synthesiss, nanometer rods, sea urchin shape, polypody shape
Deng.Referring to Yu J, Yu Y, Peng Z, et al.Morphology-dependent photocatalytic H 2-
production activity of CdS[J].Applied Catalysis B Environmental,2014,s 156–
157(2):184-191.Cadmium sulfide is in crystal growing process, and in order to reduce its surface energy, high energy crystal face can fade away, lead
The preparation of the nanocube of exposure high energy crystal face (100) is caused to there is obstacle.Referring to Shah S H, Azam A, Rafiq M
A.Atomistic Simulations of CdS Morphologies[J].Crystal Growth&Design,2015,15
(4):1792-1800。
Cadmium sulfide has two kinds of thing phases of buergerite and zincblende, it has been reported that although vulcanization cadmium material with different shapes
Looks, but the cadmium sulfide stability of wurtzite-type is higher, thus its thing synthesizes the zincblende of metastable phase based on wurtzite-type
Type cadmium sulfide nano cube difficulty is further increased.Referring to Bao N, Shen L, Takata T, et al.Facile Cd-
Thiourea Complex Thermolysis Synthesis of Phase-Controlled CdS Nanocrystals
for Photocatalytic Hydrogen Production under Visible Light[J].Journal of
Physical Chemistry C,2007,111(47):17527-17534。
The content of the invention
The purpose of the present invention, is to be difficult to prepare exposure (100) crystal face for existing process, and have zincblende thing phase
The cubical problem of small size cadmium sulfide nano utilizes hot injection method and subsequent ion exchange process controlledly synthesis 15nm there is provided one kind
The cubical method of the consistent appearance of left and right, the zinc blende-type cadmium sulfide nano of good dispersion and size uniformity.The present invention with from
Based on the method that son is exchanged, it is used as protection gas suppression chemical etching by adding inert gas, regulates and controls experiment parameter, it is final real
Now thoroughly ion exchange, obtains bright sulfur cadmium nanocube.Repeatability of the invention is strong, belongs to controlledly synthesis, can obtain
Pattern and Stability Analysis of Structures, small size and uniform product.
The present invention is achieved by following technical solution.
One kind synthesizes the cubical method of zinc blende-type cadmium sulfide nano using cation exchange, with following steps：
(1) at room temperature, by sulphur powder and oleyl amine with 9:1 mass ratio is placed in ultrasonic disperse in conical flask, until forming equal
The oleyl amine solution of even sulphur powder；
(2) by lead chloride and oleyl amine with 140：3 mass ratio is placed in three-necked flask, wherein the quality of sulphur powder and lead chloride
Than about 1:10,220 DEG C are heated under magnetic stirring, are incubated 15 minutes；The oleyl amine solution for the sulphur powder that step (1) is prepared again is noted
Enter into the three-necked flask, be incubated 1h, eventually form the colloidal solution of black vulcanized lead；
(3) after the colloidal solution of step (2) is cooled down, by the liquid in three-necked flask under the rotating speed more than 10000rpm
Centrifuge 15min, separation product and solvent；Products therefrom is cleaned and centrifuged with ethanol, and it then is dried in vacuo into 6h at 60 DEG C,
Obtain vulcanized lead nanocube；
(4) by the dried vulcanized lead nanocube ultrasonic disperse of step (3) in octadecylene, concentration is 2.658g/
L, forms dispersed black liquor；
(5) 30mmol cadmium acetates are added in 500mL three-necked flasks, oleic acid and oleyl amine dissolving is added, its ratio is 3:2,
Argon gas is passed through as protection gas, 100 DEG C of insulation 15min are heated under magnetic stirring；Liquid obtained by step (4) is injected into
State in three-necked flask, heating-up temperature is progressively warming up to 300 DEG C, be incubated 30min；
(6) three-necked flask of step (5) is finally cooled to room temperature, product is separated with solution centrifugal, cleaned with ethanol
Centrifugation 2 times, obtains zinc blende-type cadmium sulfide nano cube.
The step (3) is cleaned and centrifuged with ethanol to products therefrom, is repeated 2 times.
It is difficult to obtain small size metastable phase and uniform regular cadmium sulfide nano cube instant invention overcomes prior art
The problem of, using vulcanized lead nanocube simple and easy to get as template, the cadmium sulfide nano cube for obtaining ion exchange
Body can keep cubical pattern, while (100) crystal face of exposure high energy.Whole building-up process need to only use common chemistry
Synthetic instrument, target product can be obtained by scaling up or reducing raw material dosage, realize the controlledly synthesis of high duplication.
Brief description of the drawings
Fig. 1 synthesizes the experimental provision schematic diagram of vulcanized lead nanocube for hot injection method of the invention；
Fig. 2 is that ion-exchange of the present invention prepares the cubical experimental provision schematic diagram of zinc blende-type cadmium sulfide nano；
Fig. 3 is the transmission electron microscope image of vulcanized lead nanocube；
(a) it is low power image, illustration is corresponding diffraction image；
(b) it is full resolution pricture；
Fig. 4 is the cubical low power transmission electron microscope image of zinc blende-type cadmium sulfide nano；
Fig. 5 is the cubical X-ray diffraction spectrogram of zinc blende-type cadmium sulfide nano.
Embodiment
The present invention is described further with accompanying drawing with reference to specific embodiment.
The cubical method of small size zinc blende-type cadmium sulfide nano is synthesized using cation exchange, with following steps：
(1) referring to Fig. 1, at room temperature, 54mg sulphur powder and 5mL oleyl amines are placed in ultrasonic disperse in 50mL conical flasks, directly
To the oleyl amine solution for forming uniform sulphur powder；
(2) by 0.56g lead chlorides (PbCl2) and 10mL oleyl amines be placed in 500mL three-necked flasks, heat under magnetic stirring
To 220 DEG C, 15 minutes are incubated；The oleyl amine solution for the sulphur powder that step (1) is prepared again is injected into the three-necked flask, is incubated 1h,
Eventually form black vulcanized lead (PbS) colloidal solution；Then cooling, obtained product is as shown in Figure 3.Fig. 3 is the PbS of monocrystalline
Nanocrystalline, product is size uniform, the regular cube of shape, and the electron diffraction diagram in (a) figure can draw PbS nano cubics
Body is Emission in Cubic, and the high resolution transmission electron microscopy photo of (b) figure shows that PbS nanocubes have good crystallinity.
(3) by after the colloidal solution cooling of step (2), the liquid in three-necked flask is centrifuged under 12000rpm rotating speed
15min, separation product and solvent；Products therefrom is cleaned and centrifuged with ethanol, is repeated 2 times, and cleans up solvent and unreacted
Presoma, contributes to the progress of subsequent reactions, and it then is dried in vacuo into 6h at 60 DEG C, vulcanized lead nanocube is obtained；
(4) by the dried vulcanized lead nanocube ultrasonic disperse of step (3) in 25mL octadecylene, concentration is
2.658g/L, forms dispersed black liquor (time is about 10min)；It is placed on afterwards in the syringe shown in Fig. 2；
(5) 30mmol cadmium acetates (Cd (Ac) is added in 500mL three-necked flasks2.3H2O), 45mL oleic acid (OA) and 30mL
Oleyl amine (ODE), is passed through argon gas as protection gas, and 100 DEG C of insulation 15min are heated under magnetic stirring；By liquid obtained by step (4)
Body is injected into above-mentioned 500mL three-necked flasks, and heating-up temperature is progressively warming up to 300 DEG C, is incubated 30min；
(6) three-necked flask of step (5) is finally cooled to room temperature, product is separated with solution centrifugal, cleaned with ethanol
Centrifugation 2 times, obtains zinc blende-type cadmium sulfide nano cube.
The cubical cube pattern of zinc blende-type cadmium sulfide nano is as shown in figure 4, the crystal structure of its zinc blende-type can
Characterized by Fig. 5 X ray diffracting spectrum, lower section vertical line is the standard spectrogram (PDF#10-0454) in PDF cards, contrast is understood
Obtained cadmium sulfide cube is zincblende crystal formation.
Claims (2)
1. one kind synthesizes the cubical method of zinc blende-type cadmium sulfide nano using cation exchange, with following steps：
(1) at room temperature, by sulphur powder and oleyl amine with 9:1 mass ratio is placed in ultrasonic disperse in conical flask, until forming uniform
The oleyl amine solution of sulphur powder；
(2) by lead chloride and oleyl amine with 140：3 mass ratio is placed in three-necked flask, and wherein the mass ratio of sulphur powder and lead chloride is about
1:10,220 DEG C are heated under magnetic stirring, are incubated 15 minutes；The oleyl amine solution for the sulphur powder that step (1) is prepared again is injected into
In the three-necked flask, 1h is incubated, the colloidal solution of black vulcanized lead is eventually formed；
(3) by after the colloidal solution cooling of step (2), the liquid in three-necked flask is centrifuged under the rotating speed more than 10000rpm
15min, separation product and solvent；Products therefrom is cleaned and centrifuged with ethanol, and it then is dried in vacuo into 6h at 60 DEG C, obtained
Vulcanized lead nanocube.
(4) by the dried vulcanized lead nanocube ultrasonic disperse of step (3) in octadecylene, the concentration of vulcanized lead is
2.658g/L, forms dispersed black liquor；
(5) 30mmol cadmium acetates are added in three-necked flask, oleic acid and oleyl amine dissolving is added, its ratio is 3:2, it is passed through argon gas work
For protection gas, 100 DEG C of insulation 15min are heated under magnetic stirring；Black liquor obtained by step (4) is injected into above-mentioned three mouthfuls
In flask, heating-up temperature is progressively warming up to 300 DEG C, 30min is incubated；
(6) three-necked flask of step (5) is finally cooled to room temperature, product is separated with solution centrifugal, centrifugation 2 is cleaned with ethanol
It is secondary, obtain zinc blende-type cadmium sulfide nano cube.
2. utilization cation exchange according to claim 1 synthesizes the cubical method of zinc blende-type cadmium sulfide nano, its
It is characterised by, the step (3) is cleaned and centrifuged with ethanol to products therefrom, is repeated 2 times.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101475148A (en) * | 2009-01-22 | 2009-07-08 | 中国科学院上海硅酸盐研究所 | Method for preparing CdS or CdSe nano-tube with KCdCl3 nanowire as template |
| CN101866960A (en) * | 2010-02-10 | 2010-10-20 | 中国科学院上海硅酸盐研究所 | Method for preparing CdS-Bi2S3 composite nanocrystalline by utilizing partial cation exchange reaction |
| CN104229870A (en) * | 2014-09-01 | 2014-12-24 | 浙江师范大学 | Method for preparing ZnxCd1-xS nano hollow brick |
-
2017
- 2017-04-29 CN CN201710298022.4A patent/CN107010653A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101475148A (en) * | 2009-01-22 | 2009-07-08 | 中国科学院上海硅酸盐研究所 | Method for preparing CdS or CdSe nano-tube with KCdCl3 nanowire as template |
| CN101866960A (en) * | 2010-02-10 | 2010-10-20 | 中国科学院上海硅酸盐研究所 | Method for preparing CdS-Bi2S3 composite nanocrystalline by utilizing partial cation exchange reaction |
| CN104229870A (en) * | 2014-09-01 | 2014-12-24 | 浙江师范大学 | Method for preparing ZnxCd1-xS nano hollow brick |
Non-Patent Citations (1)
| Title |
|---|
| YANGYANG ZHANG ET AL.: "Zinc-Blende CdS Nanocubes with Coordinated Facets for Photocatalytic Water Splitting", 《ACS CATAL.》 * |
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Application publication date: 20170804 |