CN107416777B - A method of no phosphine synthesis tellurides is nanocrystalline - Google Patents
A method of no phosphine synthesis tellurides is nanocrystalline Download PDFInfo
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- CN107416777B CN107416777B CN201710635830.5A CN201710635830A CN107416777B CN 107416777 B CN107416777 B CN 107416777B CN 201710635830 A CN201710635830 A CN 201710635830A CN 107416777 B CN107416777 B CN 107416777B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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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
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- 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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- 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
A kind of nanocrystalline method of no phosphine synthesis tellurides of the invention belongs to technical field of nanometer material preparation, and using caddy or lead chloride and tellurium powder as raw material, oleyl amine and lauryl mercaptan are ligand and solvent, nanocrystalline using solvent structure CdTe and PbTe.Sample prepared by the present invention is mutually with high purity, sample crystallization is good, particle diameter distribution is uniform；Preparation method has many advantages, such as that process is simple, environmentally protective, generated time is short, at low cost, product is repeatable high.
Description
Technical field
The invention belongs to the technical field of nano material preparation, in particular to a kind of methods for preparing bielement nano crystalline substance.
Background technique
Semiconductor nano material has unique size-dependent, shows the optics different from body material, magnetics, electricity
With the properties such as calorifics, the extensive concern of domestic and international scientist is caused.Wherein, with the nanocrystalline telluride for representative of CdTe and PbTe
Object is nanocrystalline, because of its special optical property, thermal property, magnetic property, mechanical property, superconductivity, acoustical behavior etc., In
The fields such as solar battery, light emitting diode, thermoelectric material, biomarker and photo-thermal therapy show huge application prospect,
It is one of the research hotspot of current field of nanometer material technology.CdTe nanometer crystalline wide, direct energy band transition, exciton bind energy with band gap
The characteristics such as big, are important fluorescent emission, laser and nonlinear optical material.PbTe has relatively narrow band gap, direct band gap glimmering
The characteristics such as light emitting, the mirror symmetry of conduction band and valence band, lower auger recombination and thermal conductivity, in infrared optics and thermoelectric power
Source domain etc. has a good application prospect.With the foundation and development of concepts such as " Preen nono science ", scientific research personnel is being visited
Under the premise of the nanocrystalline type of rope tellurides as semiconductor and functional diversities, the green of synthetic method is gradually paid close attention to.At present
Until, it is nanocrystalline that researcher has developed a variety of synthetic method preparation CdTe and PbTe.Solvent thermal process has reaction temperature model
Enclose big, the reaction time is short, sample size uniformity and can reconcile morphology controllable the advantages that.It is molten utilizing due to the chemical property of tellurium
Agent thermal method prepare tellurides as semiconductor it is nanocrystalline when, frequently with tri octyl phosphine (TOP) dissolution tellurium as tellurium predecessor (TOP-Te)
(Nano Lett.,2008,8,2490–2496；J.Phys.Chem.B,2005,109,8538–8542；J.Am.Chem.Soc.,
2011,133,17590–17593；).Cause preparation process that there is pollution and at high cost however, TOP toxicity is big, price is high.Cause
This, the solvent-thermal method preparation CdTe and PbTe for needing to develop simply without phosphine is nanocrystalline, optimizes fluorescent emission and thermoelectricity of material etc.
Property.
Summary of the invention
The technical problem to be solved by the present invention is overcoming the problems, such as that background technique exists and defect, provides a kind of simple nothing
Phosphine solvent hot preparation CdTe and PbTe nanocrystalline method.
The present invention is using caddy, lead chloride and tellurium powder as raw material, and oleyl amine and lauryl mercaptan are ligand and solvent, using solvent
It is nanocrystalline that thermal method synthesizes CdTe and PbTe.Specific technical solution is as follows:
A method of no phosphine synthesis tellurides is nanocrystalline, be in Xi Laike (Schlenk) system under nitrogen protection into
Capable；Using the chloride of molar ratio 4:1 and tellurium powder as raw material, oleyl amine and lauryl mercaptan are ligand and solvent, the chloride
It is caddy or lead chloride；Firstly, tellurium powder and lauryl mercaptan are fitted into weighing bottle by mass volume ratio 0.0043g/mL, room temperature
Stirring 5 minutes is added the oleyl amine with lauryl mercaptan same volume, obtains uniform dark solution, be denoted as a solution；Again by caddy
It is fitted into a three-necked bottle with oleyl amine by mass volume ratio 0.0147g/mL, is stirred and heated to 120~140 DEG C, obtains colourless
Clear solution is denoted as b solution, and a solution is injected into b solution, reacts 5~20 minutes at 220~250 DEG C, obtains CdTe and receive
Meter Jing.
In preparation process of the present invention, after a solution is injected into b solution, if the chloride is caddy, preferably exist
240 DEG C of reactions；If the chloride is lead chloride, preferably reacted at 220 DEG C.
The utility model has the advantages that
The present invention prepares the advantages of CdTe and PbTe nanometers of crystal method and is: the sample phase purity of preparation is very high, sample knot
Crystalline substance is good, particle diameter distribution is uniform；And this preparation method is with process is simple, generated time is short, at low cost, product is repeatable
The advantages that high, with the nanocrystalline potentiality of large-scale production of CdTe and PbTe, and whole process is participated in without TOP, synthesis process green
Environmental protection.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture of CdTe nanometer crystalline prepared by embodiment 1.
Fig. 2 is the X-ray diffraction pattern of CdTe nanometer crystalline prepared by embodiment 1.
Fig. 3 is the fluorescent emission figure of CdTe nanometer crystalline prepared by embodiment 1.
Fig. 4 is the nanocrystalline transmission electron microscope picture of the PbTe of the preparation of embodiment 2.
Fig. 5 is the nanocrystalline X-ray diffraction pattern of the PbTe of the preparation of embodiment 2.
Specific embodiment
The present invention is more specifically described now in conjunction with the following example, unless otherwise specified, agents useful for same be it is commercially available can
The product of acquisition is purified not plus further and is used.
Synthesis of the embodiment 1 without phosphine CdTe nanometer crystalline
Synthesizing CdTe nanometer crystalline is carried out in Xi Laike (Schlenk) system, and synthesis process needs nitrogen protection, specifically
Synthesis process is as follows: in glove box under nitrogen protection, 0.0128g tellurium powder and 3mL lauryl mercaptan being fitted into weighing bottle, room
Temperature stirring 5 minutes, is added 3mL oleyl amine, obtains uniform dark solution, be denoted as a solution.By 0.0733g caddy and 5mL oleyl amine
It is fitted into three-necked bottle, later clogs two side ports of three-necked bottle with rubber plug, middle port is connected to Schlenk system, by thermoelectricity
It is even to be inserted under liquid level from the side of three-necked bottle, 120~140 DEG C are stirred and heated to, colorless cleared solution is obtained, is denoted as b solution.
A solution is injected into b solution, extracts sample after ten minutes in 240 DEG C of reactions.
The transmission electron microscope picture of the CdTe nanometer crystalline sample of preparation is as shown in Figure 1, the average grain diameter of CdTe nanometer crystalline is about
12nm.The X-ray diffraction pattern of sample is as shown in Fig. 2, the CdTe nanometer crystalline of preparation is wurtzite structure, and has good crystallization
Property, Fig. 3 show the present embodiment synthesis CdTe nanometer crystalline fluorescent emission spectrogram, fluorescent emission peak position be 550nm, this shows
The present invention shows good fluorescent emission performance without phosphine synthesis CdTe nanometer crystalline.
The synthesis nanocrystalline without phosphine PbTe of embodiment 2
It is nanocrystalline, which to synthesize PbTe, is carried out in Xi Laike (Schlenk) system, and synthesis process needs nitrogen protection, specifically
Synthesis process is as follows: in glove box under nitrogen protection, 0.0128g tellurium powder and 3mL lauryl mercaptan being fitted into weighing bottle, room
Temperature stirring 5 minutes, is added 3mL oleyl amine, obtains uniform dark solution, be denoted as a solution.By 0.1112g lead chloride and 5mL oleyl amine
It is fitted into three-necked bottle, later clogs two side ports of three-necked bottle with rubber plug, middle port is connected to Schlenk system, by thermoelectricity
It is even to be inserted under liquid level from the side of three-necked bottle, 120~140 DEG C are stirred and heated to, white solution is obtained, is denoted as b solution.By a
Solution is injected into b solution, extracts sample after ten minutes in 220 DEG C of reactions.
The transmission electron microscope picture of the nanocrystalline sample of the PbTe of preparation is as shown in figure 4, PbTe nanocrystalline average grain diameter is about
10nm.Fig. 5 is the nanocrystalline X-ray diffraction pattern of PbTe obtained, and it is nanocrystalline for cube phase structure that Fig. 5 shows PbTe, and has good
Good crystallinity.
Claims (2)
1. a kind of method that no phosphine synthesis tellurides is nanocrystalline, is carried out under nitrogen protection in Xi Laike system；With mole
Chloride and tellurium powder than 4:1 are raw material, and oleyl amine and lauryl mercaptan are ligand and solvent, and the chloride is caddy or chlorine
Change lead；Firstly, tellurium powder and lauryl mercaptan are fitted into weighing bottle by mass volume ratio 0.0043g/mL, it is stirred at room temperature 5 minutes, adds
Enter the oleyl amine with lauryl mercaptan same volume, obtain uniform dark solution, is denoted as a solution；Caddy and oleyl amine are pressed into quality again
Volume ratio 0.0147g/mL is fitted into a three-necked bottle, is stirred and heated to 120~140 DEG C, is obtained colorless cleared solution, is denoted as
B solution, or lead chloride and oleyl amine are fitted into a three-necked bottle by mass volume ratio 0.0222g/mL, it is stirred and heated to 120
~140 DEG C, white solution is obtained, is denoted as b solution, a solution is injected into b solution, reacts 5~20 points at 220~250 DEG C
Clock obtains CdTe nanometer crystalline.
2. a kind of nanocrystalline method of no phosphine synthesis tellurides according to claim 1, which is characterized in that infuse a solution
Enter to after b solution, if the chloride is caddy, is reacted at 240 DEG C；If the chloride is lead chloride, In
220 DEG C of reactions.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109534305B (en) * | 2019-01-23 | 2022-12-20 | 陕西科技大学 | Method for preparing SnSe by solution method |
| CN110203891A (en) * | 2019-03-27 | 2019-09-06 | 吉林建筑大学 | A kind of new method of two telluride manganese nano material of green syt |
| CN110342475B (en) * | 2019-06-24 | 2022-07-19 | 吉林大学 | Preparation method of iron ditelluride nano material with adjustable shape and size |
| CN115285945A (en) * | 2022-08-04 | 2022-11-04 | 安徽工程大学 | Antimony-silver ditelluride nanocrystal and phosphine-free liquid phase synthesis method and application thereof |
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|---|---|---|---|---|
| CN101074493A (en) * | 2007-04-09 | 2007-11-21 | 吉林大学 | Method for synthesizing supefine CdSe and CdTe nano-crystal |
| CN102583262A (en) * | 2012-01-04 | 2012-07-18 | 吉林大学 | Method for preparing oil soluble semiconductor nanocrystalline without phosphine |
| CN105174235A (en) * | 2015-08-24 | 2015-12-23 | 中国科学技术大学 | Liquid-phase preparation method of cubic phase Cu2SnTe3 nanometer crystal |
| CN106635022A (en) * | 2016-09-23 | 2017-05-10 | 吉林大学 | Method for preparing oil-soluble selenium or telluride semiconductor quantum dot without phosphine through dissolving chalcogenide oxide by alkanethiol |
| CN106967422A (en) * | 2017-05-11 | 2017-07-21 | 吉林大学 | A kind of preparation method of the Cd Cu Fe S quaternary nanocrystals with photoluminescent property |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101074493A (en) * | 2007-04-09 | 2007-11-21 | 吉林大学 | Method for synthesizing supefine CdSe and CdTe nano-crystal |
| CN102583262A (en) * | 2012-01-04 | 2012-07-18 | 吉林大学 | Method for preparing oil soluble semiconductor nanocrystalline without phosphine |
| CN105174235A (en) * | 2015-08-24 | 2015-12-23 | 中国科学技术大学 | Liquid-phase preparation method of cubic phase Cu2SnTe3 nanometer crystal |
| CN106635022A (en) * | 2016-09-23 | 2017-05-10 | 吉林大学 | Method for preparing oil-soluble selenium or telluride semiconductor quantum dot without phosphine through dissolving chalcogenide oxide by alkanethiol |
| CN106967422A (en) * | 2017-05-11 | 2017-07-21 | 吉林大学 | A kind of preparation method of the Cd Cu Fe S quaternary nanocrystals with photoluminescent property |
Non-Patent Citations (1)
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| Phosphine-Free Synthesis of Metal Chalcogenide Quantum Dots by Directly Dissolving Chalcogen Dioxides in Alkylthiol as the Precursor;Dong Yao et al.;《ACS Applied Materials & Interfaces》;20170302;第9卷;第9840-9848页 * |
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