CN107140680A - Cadmium sulfide nano powder and preparation method thereof - Google Patents
Cadmium sulfide nano powder and preparation method thereof Download PDFInfo
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- CN107140680A CN107140680A CN201710545145.3A CN201710545145A CN107140680A CN 107140680 A CN107140680 A CN 107140680A CN 201710545145 A CN201710545145 A CN 201710545145A CN 107140680 A CN107140680 A CN 107140680A
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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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- 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
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- 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
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Abstract
The invention discloses a kind of cadmium sulfide nano powder and preparation method thereof, the preparation method includes：Cadmium salt, sodium diethyldithiocarbamate and water are mixed, presoma is obtained after ageing；Presoma progress calcination is obtained into cadmium sulfide nano powder.There is the problem of complicated step, too high cost or various pollutions that are being likely to result in environment in the preparation method for solving existing cadmium sulfide nanopowder.
Description
Technical field
The present invention relates to field of semiconductor materials, in particular it relates to a kind of cadmium sulfide nano powder and preparation method thereof.
Background technology
Semiconductor particle is due to having significant quantum size effect, therefore their photophysical property and chemical property
Rapidly become one of current most active research field, the supper-fast optical nonlinearity that wherein Nano semiconductor particles have
The characteristic such as response and (room temperature) luminescence generated by light extremely common people pay close attention to.Generally when semiconductor particle dimensional effect and its exciton Bohr half
When footpath is close, with the reduction of particle size, the Effective band gap increase of semiconductor particle, its corresponding absorption spectrum and fluorescence light
Blue shift occurs for spectrum, so that a series of discrete energy levels can be being formed in band.Nano semiconductor particles also have opto-electronic conversion simultaneously
Characteristic and electrology characteristic.
Especially noticeable 21st century will be wide application prospect that Nano semiconductor is shown.Although due to
Cost is too high, and commercialized photovoltaic cell is difficult to large-scale promotion application at present, but since Gratzel reports warp first
Since the excellent light transfer characteristic of the nanocrystalline photovoltaic cell of dye sensitization, scientists from all over the world are attracted by this, around nanometer
The research of brilliant photovoltaic cell is more and more hotter.This is due to that preparing for nanocrystalline photovoltaic cell is relatively simple, and with higher light
Photoelectric transformation efficiency.High-ratio surface high activity, the special characteristic of Nano semiconductor particles are made applied in terms of sensor
Most promising material.It is quite sensitive to environmental factors such as temperature, light, humidity.The change of external environment can draw rapidly
The change of surface or interface ion valence state electron transport is played, sensor can be made using the significant changes of its resistance, be characterized in
Fast response time, sensitivity are high, selectivity is excellent.CdS is the material that group Ⅱ-Ⅵ compound semiconductor is studied more, extensively
Applied to solar cell, photoelectron and photo-luminescent devices.
In recent years, CdS semi-conductor nano particles turn into the focus of research due to itself having excellent performance.Its system
Standby and performance study causes the broad interest of domestic and foreign scholars, and CdS is prepared at present mainly following methods：1. element is directly anti-
Ying Fa：Binary metal compound is prepared using elemental direct reaction, generally using high temperature gas phase/solid phase reaction mode, is such as used
Chemical vapour deposition technique (CVD) method, but the particle size that this method is obtained is larger, while the sulfur vapor produced in preparation process
Product is set to be difficult to keep its stoichiometric proportion.2. microemulsion method：Mealy structure pattern can be achieved effective control using this method,
But be due to form W/O microemulsions to use substantial amounts of surfactant, cost is too high, in microemulsion solubilization water very little, therefore
Yield is very low, so as to limit its commercial Application.3. hydro-thermal method：Hydrothermal system is a kind of untethered system, and researcher utilizes water
Thermal technology prepares spherical cube of β-CdS nanoparticle at a fairly low temperature, enclosed high pressure environment.4. pyrolytic reaction：Profit
With the precursor compound containing M-S keys in the decomposition of higher temperature, synthesis metal sulfide reaction.These above-mentioned preparation sides
Method often has that step complexity, cost are too high or that environment is likely to result in various.
The content of the invention
It is an object of the invention to provide a kind of cadmium sulfide nano powder and preparation method thereof, solve existing cadmium sulfide and receive
There is the problem of complicated step, too high cost or various pollutions that are being likely to result in environment in the preparation method of ground rice.
To achieve these goals, the invention provides a kind of preparation method of cadmium sulfide nano powder, the preparation side
Method includes：
(1) cadmium salt, sodium diethyldithiocarbamate and water are mixed, presoma is obtained after ageing；
(2) presoma progress calcination is obtained into cadmium sulfide nano powder.
Present invention also offers a kind of cadmium sulfide nano powder, the cadmium sulfide nano powder is by above-mentioned preparation method system
.
It is described to prepare the invention provides a kind of cadmium sulfide nano powder and preparation method thereof according to above-mentioned technical proposal
Method includes：Cadmium salt, sodium diethyldithiocarbamate and water are mixed, presoma is obtained after ageing；Presoma is carried out
Calcination obtains cadmium sulfide nano powder.This method utilizes unimolecule presoma synthesis in solid state, compared to more some other liquid phase synthesis
Method, it is more cheap using raw material, and nontoxic pollution-free, simple production process, this method temperature control 300 DEG C with
Under, energy consumption is not only reduced, and products therefrom has wurtzite (hexagonal phase), the particle diameter of pure phase more uniform.
Other features and advantages of the present invention will be described in detail in subsequent embodiment part.
Brief description of the drawings
Accompanying drawing is, for providing a further understanding of the present invention, and to constitute a part for specification, with following tool
Body embodiment is used to explain the present invention together, but is not construed as limiting the invention.In the accompanying drawings：
Fig. 1 is the x-ray diffractogram of powder of the products therefrom of embodiment 1；
Fig. 2 is the fluorescence spectra of the products therefrom of embodiment 1；
Fig. 3 is the x-ray diffractogram of powder of the products therefrom of embodiment 2；
Fig. 4 is the transmission electron microscope picture of the products therefrom of embodiment 2；
Fig. 5 is the fluorescence spectra of the products therefrom of embodiment 2；
Fig. 6 is the x-ray diffractogram of powder of the products therefrom of embodiment 3；
Fig. 7 is the transmission electron microscope picture of the products therefrom of embodiment 3；
Fig. 8 is the fluorescence spectra of the products therefrom of embodiment 3.
Embodiment
The embodiment to the present invention is described in detail below.It should be appreciated that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to limit the invention.
The end points and any value of disclosed scope are not limited to the accurate scope or value herein, these scopes or
Value should be understood to comprising the value close to these scopes or value.For number range, between the endpoint value of each scope, respectively
It can be combined with each other between the endpoint value of individual scope and single point value, and individually between point value and obtain one or more
New number range, these number ranges should be considered as specific open herein.
The invention provides a kind of preparation method of cadmium sulfide nano powder, the preparation method includes：
(1) cadmium salt, sodium diethyldithiocarbamate and water are mixed, presoma is obtained after ageing；
(2) presoma progress calcination is obtained into cadmium sulfide nano powder.
The present invention it is a kind of preferred embodiment in, in order to which the wurtzite with pure phase is preferably made
Cadmium sulfide nano powder, the cadmium salt relative to 0.01/3mol, the consumption of the sodium diethyldithiocarbamate is 0.01-
0.03mol, the consumption of the water is 180-220mL.
The present invention it is a kind of preferred embodiment in, in order to which the wurtzite with pure phase is preferably made
Cadmium sulfide nano powder, one or more of the cadmium salt in cadmium sulfate, cadmium nitrate and caddy.
The present invention it is a kind of preferred embodiment in, in order to which the wurtzite with pure phase is preferably made
Cadmium sulfide nano powder, in step (2), the condition of calcination at least includes：The temperature of calcination be 250-280 DEG C, calcination when
Between be 5-12h.
The present invention it is a kind of preferred embodiment in, in order to which the wurtzite with pure phase is preferably made
Cadmium sulfide nano powder, in step (1), the time of ageing is 10-14h.
The present invention it is a kind of preferred embodiment in, in order to which the wurtzite with pure phase is preferably made
Cadmium sulfide nano powder, in step (2), the preparation method also includes：Presoma after ageing is subjected to suction filtration, by filter residue
After being washed with deionized 2-3 times, it is placed in 75-85 DEG C of environment and dries 1.5-2.5h.
Present invention also offers a kind of cadmium sulfide nano powder, the cadmium sulfide nano powder is by above-mentioned preparation method system
.
The present invention will be described in detail by way of examples below.
Embodiment 1
By 0.01/3mol cadmium sulfates (3CdSO4·8H2O), 0.02mol sodium diethyldithiocarbamates and 180mL water
Mixing, presoma is obtained after ageing (time of ageing is 10h)；Presoma is subjected to suction filtration, filter residue is washed with deionized 2
After secondary, be placed in 75 DEG C of environment dry 1.5h, afterwards by after processing by presoma carry out calcination (temperature of calcination be 250 DEG C,
The time of calcination is 5h) obtain cadmium sulfide nano powder.
Embodiment 2
By 0.01/3mol cadmium sulfates (3CdSO4·8H2O), sodium diethyldithiocarbamate and water mixing, are aged (old
The time of change be 14h) after obtain presoma；Presoma is subjected to suction filtration, filter residue is washed with deionized after 3 times, 85 are placed in
2.5h is dried in DEG C environment, (temperature of calcination is 280 DEG C, the time of calcination by presoma is carried out into calcination after processing afterwards
For 12h) obtain cadmium sulfide nano powder.
Embodiment 3
By 0.01/3mol cadmium sulfates (3CdSO4·8H2O), sodium diethyldithiocarbamate and water mixing, are aged (old
The time of change be 12h) after obtain presoma；Presoma is subjected to suction filtration, filter residue is washed with deionized after 3 times, 80 are placed in
2h is dried in DEG C environment, (temperature of calcination is 265 DEG C, and the time of calcination is by presoma is carried out into calcination after processing afterwards
8h) obtain cadmium sulfide nano powder.
Using Japanese Rigaku D/Max-3C x-ray powder diffraction instruments (Cu K α radiations, ) determine sulphur
The structure of cadmium nanometer powder；Using Dutch Philips company's Ts ecnai12 types transmission electron microscope (TEM, 120kV) to sulphur
The pattern of cadmium nanometer powder carries out observation test with size；Using Japanese Hitachi F-4500 XRFs to cadmium sulfide
The luminosity of nanometer powder is tested, and test result is shown in Fig. 1-Fig. 8.
Fig. 1：The x-ray diffractogram of powder of the products therefrom of the embodiment of the present invention 1.Its all X-ray diffraction peak is from left to right
Hexagonal phase CdS (100), (002), (101), (102), (110), (103), (112) crystal face is corresponded respectively to, no presoma
X diffraction maximums occur, and the product for illustrating the gained of embodiment 1 is the CdS of pure hexagonal phase.
Fig. 2：The fluorescence spectra of the products therefrom of the embodiment of the present invention 1.The excitation wavelength used is 350nm, and emission peak exists
At 396nm.
Fig. 3：The x-ray diffractogram of powder of the products therefrom of the embodiment of the present invention 2.Its all X-ray diffraction peak is from left to right
Hexagonal phase CdS (100), (002), (101), (102), (110), (103), (112) crystal face is corresponded respectively to, no presoma
X diffraction maximums occur, and the product for illustrating the gained of embodiment 1 is the CdS of pure hexagonal phase.
Fig. 4：The transmission electron microscope picture of the products therefrom of the embodiment of the present invention 2.Understand that product CdS powder is irregular from the figure
Particle, particle diameter is 20-40nm.
Fig. 5：The fluorescence spectra of the products therefrom of the embodiment of the present invention 2.The excitation wavelength used is 350nm, and emission peak exists
At 382nm.
Fig. 6：The x-ray diffractogram of powder of the products therefrom of the embodiment of the present invention 3.Its all X-ray diffraction peak is from left to right
Hexagonal phase CdS (100), (002), (101), (102), (110), (103), (112) crystal face is corresponded respectively to, no presoma
X diffraction maximums occur, and the product for illustrating the gained of embodiment 1 is the CdS of pure hexagonal phase.
Fig. 7：The transmission electron microscope picture of the products therefrom of the embodiment of the present invention 3.Understand that product CdS powder is irregular from the figure
Particle, is easier to reunite, particle diameter is 20-40nm.
Fig. 8：The fluorescence spectra of the products therefrom of the embodiment of the present invention 3.The excitation wavelength used is 350nm, and emission peak exists
At 400nm.
The preferred embodiment of the present invention is described in detail above in association with accompanying drawing, still, the present invention is not limited to above-mentioned reality
The detail in mode is applied, in the range of the technology design of the present invention, a variety of letters can be carried out to technical scheme
Monotropic type, these simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should equally be considered as content disclosed in this invention.
Claims (7)
1. a kind of preparation method of cadmium sulfide nano powder, it is characterised in that the preparation method includes：
(1) cadmium salt, sodium diethyldithiocarbamate and water are mixed, presoma is obtained after ageing；
(2) presoma progress calcination is obtained into cadmium sulfide nano powder.
2. preparation method according to claim 1, wherein, the cadmium salt relative to 0.01/3mol, the diethyl-dithio
The consumption of carbamic acid sodium is 0.01-0.03mol, and the consumption of the water is 180-220mL.
3. preparation method according to claim 1 or 2, wherein, the cadmium salt is in cadmium sulfate, cadmium nitrate and caddy
One or more.
4. preparation method according to claim 1 or 2, wherein, in step (2), the condition of calcination at least includes：Calcination
Temperature be 250-280 DEG C, time of calcination is 5-12h.
5. preparation method according to claim 1 or 2, wherein, in step (1), the time of ageing is 10-14h.
6. preparation method according to claim 1 or 2, wherein, in step (2), the preparation method also includes：Will be old
The presoma obtained after change carries out suction filtration, after filter residue is washed with deionized 2-3 times, is placed in 75-85 DEG C of environment and dries
1.5-2.5h。
7. a kind of cadmium sulfide nano powder, it is characterised in that cadmium sulfide nano powder any one in claim 1-6
Described preparation method is made.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710545145.3A CN107140680A (en) | 2017-07-06 | 2017-07-06 | Cadmium sulfide nano powder and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710545145.3A CN107140680A (en) | 2017-07-06 | 2017-07-06 | Cadmium sulfide nano powder and preparation method thereof |
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| CN107140680A true CN107140680A (en) | 2017-09-08 |
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| CN201710545145.3A Pending CN107140680A (en) | 2017-07-06 | 2017-07-06 | Cadmium sulfide nano powder and preparation method thereof |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104689835A (en) * | 2015-03-18 | 2015-06-10 | 湖南大学 | CeO2 (Cerium Oxide) nano-particle/CdS (Cadmium Sulfide) nano-rod composite photo-catalyst as well as preparation method and application thereof |
-
2017
- 2017-07-06 CN CN201710545145.3A patent/CN107140680A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104689835A (en) * | 2015-03-18 | 2015-06-10 | 湖南大学 | CeO2 (Cerium Oxide) nano-particle/CdS (Cadmium Sulfide) nano-rod composite photo-catalyst as well as preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| YONG CAI ZHANG ET AL.: "In air synthesis of hexagonal Cd1 − xZnxS nanoparticles from single-source molecular precursors", 《MATERIALS LETTERS》 * |
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