CN108373919A - A kind of preparation method of CdSe quantum dot - Google Patents
A kind of preparation method of CdSe quantum dot Download PDFInfo
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- CN108373919A CN108373919A CN201810041810.XA CN201810041810A CN108373919A CN 108373919 A CN108373919 A CN 108373919A CN 201810041810 A CN201810041810 A CN 201810041810A CN 108373919 A CN108373919 A CN 108373919A
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- quantum dot
- cdse quantum
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- ethyl alcohol
- oleic acid
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
- C09K11/881—Chalcogenides
- C09K11/883—Chalcogenides with zinc or cadmium
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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
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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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
Abstract
The present invention relates to a kind of preparation methods of CdSe quantum dot, include the following steps：Cadmium acetate is dissolved in ultra-pure water, N2It is bubbled protection；Enuatrol, oleic acid, ethyl alcohol, Se powder are sequentially added in above-mentioned solution again, stirring a period of time, obtain certain density emulsion；Above-mentioned emulsion is transferred in ptfe autoclave, is put into baking oven, at a certain temperature isothermal reaction certain time；Reaction solution is purified, centrifuge washing, and dried in vacuum drying chamber, finally obtains CdSe quantum dot.Manufacture craft of the present invention is simple, and raw material is cheap, nontoxic, safe, is convenient for large-scale production.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, and in particular to a kind of preparation method of CdSe quantum dot.
Background technology
Quantum dot (Quantum dot, abbreviation QD) be a kind of radius be less than or close to Bohr's exciton radii semiconductor
Nanocrystal.Quantum dot is also known as semiconductor nano, and size is generally zero dimensional nanometer materials in 2~10nm, it is tieed up at three
Size on degree is all close with electron mean free path, has unique discrete energy levels system, therefore the artificial atom that is otherwise known as.
Quantum dot has the Spectral Properties such as exciting light spectrum width, emission spectrum are symmetrical and width is narrow, Color tunable, photochemical stability height
Sign.Since quantum dot has strong size-dependent, so, with the reduction of quantum dot size, the absorption of particle and fluorescence
Corresponding blue shift can occur for spectrum.Quantum dot has higher specific surface, has apparent shadow to its grain structure and optical property
It rings.Shell Materials by wrapping up broad-band gap can increase the inoxidizability of quantum dot, and can improve quantum yield, in recent years, core
The research and development of the quantum dot of shell mould have also obtained great development, such as CdSe/ZnS, CdSe/ZnSe, CdSe/CdS etc..As one
Kind visible light Illuminant nanometer material, early in 1994, the application on electro-optical device began to be concerned.
CdSe quantum dot is very suitable for visually observing since launch wavelength covers entire visible region range, thus close several
Nian Laiyi causes the concern of people, it can be used for the application in various fields, including luminescent device, photovoltaic device and biomedicine
The fields such as imaging.There are many approach for traditional CdSe quantum dot synthesis, and the CdSe quantum dot of high quality is organic by metal at present
Compound route synthesizes.This method usually selects TOP/TOPO/HDA to do dicyandiamide solution, by Se at a high temperature of 300 DEG C or more
Complex solution injects in Cd precursors, obtains the quantum dot of different-grain diameter and fluorescent emission.At high temperature due to thermodynamical equilibrium
There is deviation so that it is difficult to the reaction that Control granularity is evenly distributed.And various solvents that this method uses are inflammable, it is explosive and
Toxicity is stronger, and overall cost is high, is unfavorable for mass producing.
Invention content
Technical problem to be solved by the invention is to provide a kind of preparation method of CdSe quantum dot, this method materials safeties
Be easy to get, cheap, simple and safe operation, combined coefficient it is high, it can be achieved that quantum dot large-scale production.
The technical solution that the present invention solves above-mentioned technical problem is as follows：
A kind of preparation method of CdSe quantum dot, includes the following steps：
S1：Cadmium acetate is dissolved in ultra-pure water, the cadmium acetate solution of a concentration of 0.06~0.1mol/L, while N is made2
It is bubbled protection；
S2：Enuatrol, oleic acid, ethyl alcohol and Se powder are sequentially added in solution made from step S1, stirred, Se content is made
In the emulsion of 0.03~0.06mol/L；
S3：Emulsion obtained in step S2 is transferred in ptfe autoclave, is then placed in baking oven, constant temperature
Under the conditions of react a period of time；
S4：Reaction solution in S3 is purified, be separated by solid-liquid separation and obtained solid is washed, it is then dry in vacuum
It is dry in dry case.
The beneficial effects of the invention are as follows：The preparation method of CdSe quantum dot provided by the invention compared with the existing methods,
The present invention has the characteristics that easy to operate and at low cost；Meanwhile the cost of material such as cadmium acetate, enuatrol, oleic acid, ethyl alcohol and Se powder
It is cheap, it is nontoxic, it is safe.The raw material of the present invention is easier to obtain, and realization is facilitated to mass produce.
Based on the above technical solution, the present invention can also be improved as follows.
Further, the usage ratio of enuatrol in the step S2, oleic acid, ethyl alcohol and Se powder is 4:1:2:0.5~1.
Further, mixing time is 2~4h in the step S2.
Further, reaction temperature is 150~200 DEG C in the step S3, and the reaction time is 3~6h.
Further, the method being separated by solid-liquid separation in the step S4 is to be handled using centrifuge, and the rotating speed of centrifuge is
The time of 4000~8000r/min, centrifugation are 10~30min.
Further, the washing in the step S4 refers to being washed 2~3 times with absolute ethyl alcohol.
Description of the drawings
Fig. 1 is the fabrication processing figure of the present invention.
Specific implementation mode
Principles and features of the present invention are described below in conjunction with drawings and the specific embodiments, example is served only for solving
The present invention is released, is not intended to limit the scope of the present invention.
Embodiment 1
As shown in Figure 1, the present embodiment provides a kind of preparation method of CdSe quantum dot, include the following steps：
S1：Cadmium acetate is dissolved in ultra-pure water, the cadmium acetate solution of a concentration of 0.07mol/L, while N is made2It is bubbled
Protection；
S2：1g enuatrols, 0.8mL oleic acid, 8mL ethyl alcohol and suitable 0.03mol Se powder are sequentially added into 1L step S1 systems
In the solution obtained, stir 2 hours at room temperature, the emulsion that obtained Se content is about 0.03mol/L；
S3：Emulsion obtained in step S2 is transferred in ptfe autoclave, is then placed in baking oven, 150
DEG C constant temperature under react 3.5h；
S4：Reaction solution in S3 is purified, the method being separated by solid-liquid separation herein is detached using centrifuge, centrifuge
10min is centrifuged under the rotating speed of 4000r/min to be separated by solid-liquid separation, and is obtained solid, then absolute ethyl alcohol is used to wash 2~3 times,
It is finally dry in vacuum drying chamber, obtain CdSe quantum dot.
Embodiment 2
As shown in Figure 1, the present embodiment provides a kind of preparation method of CdSe quantum dot, include the following steps：
S1：Cadmium acetate is dissolved in ultra-pure water, the cadmium acetate solution of a concentration of 0.08mol/L, while N is made2It is bubbled
Protection；
S2：Step is added in 1.5g enuatrols, 1.2mL oleic acid, 12mL ethyl alcohol and suitable 0.04mol Se powder successively 1L
In solution made from S1, stir 3 hours at room temperature, the emulsion that obtained Se content is about 0.04mol/L；
S3：Emulsion obtained in step S2 is transferred in ptfe autoclave, is then placed in baking oven, 175
DEG C constant temperature under react 4.5h；
S4：Reaction solution in S3 is purified, the method being separated by solid-liquid separation herein is detached using centrifuge, centrifuge
20min is centrifuged under the rotating speed of 6000r/min to be separated by solid-liquid separation, and is obtained solid, then absolute ethyl alcohol is used to wash 2~3 times,
It is finally dry in vacuum drying chamber, obtain CdSe quantum dot.
Embodiment 3
As shown in Figure 1, the present embodiment provides a kind of preparation method of CdSe quantum dot, include the following steps：
S1：Cadmium acetate is dissolved in ultra-pure water, the cadmium acetate solution of a concentration of 0.09mol/L, while N is made2It is bubbled
Protection；
S2：2g enuatrols, 1.6mL oleic acid, 16mL ethyl alcohol and suitable 0.06molSe powder are sequentially added into 1L step S1 systems
In the solution obtained, stir 4 hours at room temperature, the emulsion that obtained Se content is about 0.06mol/L；
S3：Emulsion obtained in step S2 is transferred in ptfe autoclave, is then placed in baking oven, 200
DEG C constant temperature under react 5.5h；
S4：Reaction solution in S3 is purified, the method being separated by solid-liquid separation herein is detached using centrifuge, centrifuge
30min is centrifuged under the rotating speed of 8000r/min to be separated by solid-liquid separation, and is obtained solid, then absolute ethyl alcohol is used to wash 2~3 times,
It is finally dry in vacuum drying chamber, obtain CdSe quantum dot.
CdSe quantum dot synthetic method synthesis condition provided by the invention requires relatively low, traditional metal organic solvent hydrothermal method
Synthesis CdSe quantum dot usually selects TOP/TOPO/HDA to do dicyandiamide solution, and reaction coordinates Se at a high temperature of 300 DEG C or more
Object solution injects in Cd precursors, the quantum dot of acquisition different-grain diameter and fluorescent emission, and synthetic method highest provided by the invention
Temperature only needs 200 DEG C, hence it is evident that less than 300 DEG C in above-mentioned prior synthesizing method, production cost reduces；Meanwhile above-mentioned tradition
TOP, TOPO solvent used in CdSe quantum dot building-up process there are it is inflammable, explosive, be more toxic, it is oxidizable the shortcomings of, deposit
In security risk, need to generally operate under vacuum, application range is obviously reduced.
CdSe quantum dot synthetic method provided by the invention, can effectively avoid and synthesized by metallo-organic compound route
The uncontrollable situation of even particle size distribution reaction caused by CdSe quantum dot high temperature, and reaction condition requirement is low, raw material is low
Honest and clean to be easy to get, production cost reduces, and safety coefficient significantly improves, and is conducive to large-scale production.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of preparation method of CdSe quantum dot, which is characterized in that include the following steps：
S1：Cadmium acetate is dissolved in ultra-pure water, the cadmium acetate solution of a concentration of 0.06~0.1mol/L, while N is made2It is bubbled
Protection；
S2：Enuatrol, oleic acid, ethyl alcohol and Se powder are sequentially added in solution made from step S1, stirred, Se content is made and exists
The emulsion of 0.03~0.06mol/L；
S3：Emulsion obtained in step S2 is transferred in ptfe autoclave, is then placed in baking oven, constant temperature
Lower reaction a period of time；
S4：Reaction solution in S3 is purified, be separated by solid-liquid separation and obtained solid is washed, then in vacuum drying chamber
Interior drying.
2. a kind of preparation method of CdSe quantum dot according to claim 1, it is characterised in that：Oleic acid in the step S2
Sodium, oleic acid, ethyl alcohol and Se powder usage ratio be 4:1:2:0.5~1.
3. a kind of preparation method of CdSe quantum dot according to claim 1, it is characterised in that：It is stirred in the step S2
Time is 2~4h.
4. a kind of preparation method of CdSe quantum dot according to claim 1, it is characterised in that：It is reacted in the step S3
Temperature is 150~200 DEG C, and the reaction time is 3~6h.
5. a kind of preparation method of CdSe quantum dot according to claim 1, it is characterised in that：Solid-liquid in the step S4
The method of separation is to be handled using centrifuge, and the rotating speed of centrifuge is 4000~8000r/min, time of centrifugation is 10~
30min。
6. a kind of preparation method of CdSe quantum dot according to claim 1, it is characterised in that：Washing in the step S4
Wash refers to being washed 2~3 times with absolute ethyl alcohol.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810041810.XA CN108373919A (en) | 2018-01-16 | 2018-01-16 | A kind of preparation method of CdSe quantum dot |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103506139A (en) * | 2013-03-14 | 2014-01-15 | 江苏大学 | Preparation method and application of hydrothermal synthesized CdSe quantum dot photocatalyst |
| JP2017160072A (en) * | 2016-03-09 | 2017-09-14 | 三菱マテリアル株式会社 | Method for producing CdSe colloidal particles |
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- 2018-01-16 CN CN201810041810.XA patent/CN108373919A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103506139A (en) * | 2013-03-14 | 2014-01-15 | 江苏大学 | Preparation method and application of hydrothermal synthesized CdSe quantum dot photocatalyst |
| JP2017160072A (en) * | 2016-03-09 | 2017-09-14 | 三菱マテリアル株式会社 | Method for producing CdSe colloidal particles |
Non-Patent Citations (1)
| Title |
|---|
| 连雪茹等: "CdSe/CdS核壳型量子点的合成及性质研究", 《化工时刊》 * |
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Application publication date: 20180807 |