CN107416777A - A kind of nanocrystalline method of no phosphine synthesis tellurides - Google Patents
A kind of nanocrystalline method of no phosphine synthesis tellurides Download PDFInfo
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- CN107416777A CN107416777A CN201710635830.5A CN201710635830A CN107416777A CN 107416777 A CN107416777 A CN 107416777A CN 201710635830 A CN201710635830 A CN 201710635830A CN 107416777 A CN107416777 A CN 107416777A
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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
- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
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Abstract
The method that a kind of no phosphine synthesis tellurides of the present invention is nanocrystalline 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 part and solvent, nanocrystalline using solvent structure CdTe and PbTe.Sample phase purity prepared by the present invention is high, sample crystallization is good, particle diameter distribution is uniform；Preparation method has the advantages that process is simple, green, generated time is short, cost is low, product is repeatable high.
Description
Technical field
It is more particularly to a kind of to prepare the brilliant method of bielement nano the invention belongs to technical field prepared by nano material.
Background technology
Semiconductor nano material has unique size-dependent, shows the optics different from body material, magnetics, electricity
With the property such as calorifics, the extensive concern of domestic and international scientist is caused.Wherein, with the nanocrystalline telluride for representative of CdTe and PbTe
Thing is nanocrystalline, because of its special optical property, thermal property, magnetic property, mechanical property, superconductivity, acoustical behavior etc.,
The fields such as solar cell, light emitting diode, thermoelectric material, biomarker and photo-thermal therapy show huge application prospect,
It is one of study hotspot of current field of nanometer material technology.CdTe nanometer crystalline have band gap it is wide, it is direct can band transition, exciton bind energy
The characteristic such as big, is important fluorescent emission, laser and nonlinear optical material.PbTe has narrower band gap, direct band gap glimmering
The characteristics such as mirror symmetry, relatively low auger recombination and the thermal conductivity of light transmitting, conduction band and valence band, 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 visiting
On the premise of the nanocrystalline species of rope tellurides as semiconductor and functional diversities, the green of synthetic method is gradually paid close attention to.At present
Untill, it is nanocrystalline that researcher has developed a variety of synthetic methods preparation CdTe and PbTe.Solvent thermal process has reaction temperature model
Enclose that big, the reaction time is short, sample size is homogeneous and can reconcile morphology controllable the advantages that.It is molten utilizing due to the chemical property of tellurium
The hot method of agent prepare tellurides as semiconductor it is nanocrystalline when, frequently with tri octyl phosphine (TOP) dissolve 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；).Preparation technology is caused to have contaminative and cost high however, TOP toxicity is big, price is high.Cause
, it is necessary to develop solvent-thermal method simply without phosphine, to prepare CdTe and PbTe nanocrystalline for this, optimizes fluorescent emission and thermoelectricity of material etc.
Property.
The content of the invention
The technical problem to be solved in the present invention is：The problem of overcoming background technology to exist and defect, there is provided a kind of simple nothing
Method nanocrystalline phosphine solvent hot preparation CdTe and PbTe.
The present invention is using caddy, lead chloride and tellurium powder as raw material, and oleyl amine and lauryl mercaptan are part and solvent, using solvent
Hot method synthesis CdTe and PbTe is nanocrystalline.Specific technical scheme is as follows：
A kind of nanocrystalline method of no phosphine synthesis tellurides, is to enter in Xi Laike (Schlenk) system under nitrogen protection
Capable；With mol ratio 4:1 chloride and tellurium powder is raw material, and oleyl amine and lauryl mercaptan are part and solvent, described chloride
It is caddy or lead chloride；First, tellurium powder and lauryl mercaptan are fitted into measuring cup by mass volume ratio 0.0043g/mL, room temperature
Stirring 5 minutes, the oleyl amine with lauryl mercaptan same volume is added, uniform dark solution is obtained, is designated as a solution；Again by caddy
It is fitted into oleyl amine by mass volume ratio 0.0147g/mL in a three-necked bottle, is stirred and heated to 120~140 DEG C, obtains colourless
Settled solution, b solution is designated as, a solution is injected into b solution, reacted 5~20 minutes at 220~250 DEG C, obtain CdTe and receive
Meter Jing.
In preparation process of the present invention, after a solution is injected into b solution, if described chloride is caddy, preferably exist
240 DEG C of reactions；If described chloride is lead chloride, preferably in 220 DEG C of reactions.
Beneficial effect：
The advantages of present invention preparation CdTe and PbTe nanometer crystal methods, 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 has, and process is simple, generated time is short, cost is low, product is repeatable
The advantages that high, with the nanocrystalline potentiality of large-scale production of CdTe and PbTe, and whole process participates in without TOP, building-up process green
Environmental protection.
Brief description of the drawings
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 pictures of the PbTe of the preparation of embodiment 2.
Fig. 5 is the nanocrystalline X-ray diffraction patterns of the PbTe of the preparation of embodiment 2.
Embodiment
The present invention is more specifically described in conjunction with the following example, unless otherwise specified, agents useful for same be it is commercially available can
The product of acquisition, purify not plus further and use.
Synthesis of the embodiment 1 without phosphine CdTe nanometer crystalline
Synthesizing CdTe nanometer crystalline is carried out in Xi Laike (Schlenk) system, and building-up process needs nitrogen to protect, specifically
Building-up process is as follows：In glove box under nitrogen protection, 0.0128g telluriums powder and 3mL lauryl mercaptans are fitted into measuring cup, room
Temperature stirring 5 minutes, adds 3mL oleyl amines, obtains uniform dark solution, be designated as a solution.By 0.0733g caddies and 5mL oleyl amines
It is fitted into three-necked bottle, afterwards clogs two side ports of three-necked bottle with plug, middle port is connected to Schlenk systems, by thermoelectricity
It is even to be inserted into from the side of three-necked bottle under liquid level, 120~140 DEG C are stirred and heated to, obtains colorless cleared solution, is designated as b solution.
A solution is injected into b solution, sample is extracted after being reacted 10 minutes at 240 DEG C.
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 prepared 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 is 550nm, and this shows
The present invention shows good fluorescent emission performance without phosphine synthesis CdTe nanometer crystalline.
Embodiment 2 is without synthesis nanocrystalline phosphine PbTe
It is nanocrystalline, which to synthesize PbTe, is carried out in Xi Laike (Schlenk) system, and building-up process needs nitrogen to protect, specifically
Building-up process is as follows：In glove box under nitrogen protection, 0.0128g telluriums powder and 3mL lauryl mercaptans are fitted into measuring cup, room
Temperature stirring 5 minutes, adds 3mL oleyl amines, obtains uniform dark solution, be designated as a solution.By 0.1112g lead chlorides and 5mL oleyl amines
It is fitted into three-necked bottle, afterwards clogs two side ports of three-necked bottle with plug, middle port is connected to Schlenk systems, by thermoelectricity
It is even to be inserted into from the side of three-necked bottle under liquid level, 120~140 DEG C are stirred and heated to, obtains white solution, is designated as b solution.By a
Solution is injected into b solution, and sample is extracted after being reacted 10 minutes at 220 DEG C.
The transmission electron microscope picture of the nanocrystalline samples of PbTe of preparation is as shown in figure 4, average grain diameter nanocrystalline PbTe is about
10nm.Fig. 5 is the nanocrystalline X-ray diffraction patterns of obtained PbTe, Fig. 5 show PbTe it is nanocrystalline be cube phase structure, and with good
Good crystallinity.
Claims (2)
1. a kind of nanocrystalline method of no phosphine synthesis tellurides, is carried out in Xi Laike systems under nitrogen protection；With mole
Than 4:1 chloride and tellurium powder is raw material, and oleyl amine and lauryl mercaptan are part and solvent, and described chloride is caddy or chlorine
Change lead；First, tellurium powder and lauryl mercaptan are fitted into measuring cup by mass volume ratio 0.0043g/mL, are stirred at room temperature 5 minutes, add
Enter the oleyl amine with lauryl mercaptan same volume, obtain uniform dark solution, be designated 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, obtains colorless cleared solution, is designated as
B solution, a solution is injected into b solution, is reacted 5~20 minutes at 220~250 DEG C, obtain CdTe nanometer crystalline.
2. the nanocrystalline method of a kind of no phosphine synthesis tellurides according to claim 1, it is characterised in that note a solution
Enter to after b solution, if described chloride is caddy, in 240 DEG C of reactions；If described chloride is lead chloride,
220 DEG C of reactions.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109534305A (en) * | 2019-01-23 | 2019-03-29 | 陕西科技大学 | A kind of method that solwution method prepares SnSe |
| 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 |
| CN110342475A (en) * | 2019-06-24 | 2019-10-18 | 吉林大学 | A kind of preparation method of the adjustable two telluride ferrum nano material of appearance 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 |
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 |
-
2017
- 2017-07-31 CN CN201710635830.5A patent/CN107416777B/en not_active Expired - Fee Related
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)
| Title |
|---|
| DONG YAO ET AL.: "Phosphine-Free Synthesis of Metal Chalcogenide Quantum Dots by Directly Dissolving Chalcogen Dioxides in Alkylthiol as the Precursor", 《ACS APPLIED MATERIALS & INTERFACES》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109534305A (en) * | 2019-01-23 | 2019-03-29 | 陕西科技大学 | A kind of method that solwution method prepares SnSe |
| 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 |
| CN110342475A (en) * | 2019-06-24 | 2019-10-18 | 吉林大学 | A kind of preparation method of the adjustable two telluride ferrum nano material of appearance and size |
| 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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| CN107416777B (en) | 2019-11-22 |
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Granted publication date: 20191122 Termination date: 20200731 |