CN108373918A - A kind of preparation method of CdSe/ZnS quantum dots - Google Patents
A kind of preparation method of CdSe/ZnS quantum dots Download PDFInfo
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- CN108373918A CN108373918A CN201810041319.7A CN201810041319A CN108373918A CN 108373918 A CN108373918 A CN 108373918A CN 201810041319 A CN201810041319 A CN 201810041319A CN 108373918 A CN108373918 A CN 108373918A
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- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical class [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000000243 solution Substances 0.000 claims abstract description 63
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 22
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 22
- 239000011259 mixed solution Substances 0.000 claims abstract description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 18
- SGJUCMOYVKXLDY-UHFFFAOYSA-N acetic acid;cadmium Chemical compound [Cd].CC(O)=O.CC(O)=O SGJUCMOYVKXLDY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000011669 selenium Substances 0.000 claims abstract description 15
- 239000000839 emulsion Substances 0.000 claims abstract description 14
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 14
- 239000012498 ultrapure water Substances 0.000 claims abstract description 14
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 11
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 11
- 239000004246 zinc acetate Substances 0.000 claims abstract description 11
- 235000019441 ethanol Nutrition 0.000 claims abstract description 10
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 9
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 9
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000005642 Oleic acid Substances 0.000 claims abstract description 9
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 claims abstract description 9
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 9
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 9
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 8
- 230000001681 protective effect Effects 0.000 claims abstract description 6
- 238000005119 centrifugation Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 2
- 239000007790 solid phase Substances 0.000 claims description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims 2
- 239000007789 gas Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 3
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 239000002096 quantum dot Substances 0.000 description 11
- 238000002156 mixing Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000002360 explosive Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 231100000331 toxic Toxicity 0.000 description 3
- 230000002588 toxic effect Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- 238000001215 fluorescent labelling Methods 0.000 description 1
- XUCNUKMRBVNAPB-UHFFFAOYSA-N fluoroethene Chemical compound FC=C XUCNUKMRBVNAPB-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000003550 marker Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004054 semiconductor nanocrystal Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
- 235000021419 vinegar Nutrition 0.000 description 1
Classifications
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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
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Optics & Photonics (AREA)
- Biophysics (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Composite Materials (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention belongs to Nano semiconductor luminescent material technical fields, and in particular to a kind of preparation method of CdSe/ZnS quantum dots.1) cadmium acetate is dissolved in ultra-pure water, obtains acetic acid cadmium solution, and carried out nitrogen and be bubbled protection；2) enuatrol, oleic acid, ethyl alcohol and enough selenium powders are added sequentially in acetic acid cadmium solution, are stirred at room temperature, obtain emulsion；3) emulsion is transferred in ptfe autoclave, isothermal reaction, cooled to room temperature after taking-up obtains the first solution；4) zinc acetate and sodium sulphate are dissolved in ultra-pure water successively, obtain the second solution, and carried out nitrogen and be bubbled protection；5) the second solution is added in the first solution and obtains mixed solution, mixed solution is stirred in the case where nitrogen is bubbled protective condition, mixed solution is transferred in ptfe autoclave again, isothermal reaction obtains reaction solution；6) it purifies and dry, obtains CdSe/ZnS quantum dots.This method mild condition, process safety is easy to implement, at low cost.
Description
Technical field
The invention belongs to Nano semiconductor luminescent material technical fields, and in particular to a kind of preparation of CdSe/ZnS quantum dots
Method.
Background technology
Quantum dot be a kind of radius be less than or close to glass exciton radii semiconductor nano crystal grain, due to having uniqueness
Fluorescence nano effect, excite spectrum width and continuously distributed, emission spectra is narrow and symmetrical, and launch wavelength can pass through and change grain size
Regulated and controled with composition, fluorescence intensity is strong, bleaching rate is slow, high sensitivity, is widely used in photocatalysis, photosensitive sensor, hair
The fields such as luminescent material, fluorescence probe label.The quantum dot (such as CdSe) of especially II B races and VI A races element composition, due to having
Special excellent visible and near infrared spectrum fluorescent emission property, in terms of biomedical fluorescence probe marker and sensor
There is important value.
Since there are surface states for quantum dot, the luminous efficiency of quantum dot is influenced, can be coated on bare quantum spot surface another
Nucleocapsid is made in the kind broader semi-conducting material of band-gap energy, to reduce the influence of bare quantum spot surface state, improves quantum dot
Yield and stability.Nucleocapsid CdSe/ZnS quantum dots usually select TOP/TOPO/HDA to do dicyandiamide solution, 300 DEG C with
At a high temperature of upper, the quantum dot of different-grain diameter and fluorescent emission is obtained.But solvent that this method uses is inflammable and explosive, price is high
It is expensive and be more toxic.
Invention content
To solve the deficiencies in the prior art, the present invention provides a kind of preparation methods of CdSe/ZnS quantum dots.This method
Mild condition, process safety is easy to implement, at low cost.
Technical solution provided by the present invention is as follows：
A kind of preparation method of CdSe/ZnS quantum dots, includes the following steps：
1) cadmium acetate is dissolved in ultra-pure water, obtains acetic acid cadmium solution, and nitrogen drum is carried out to the acetic acid cadmium solution
Bubble protection；
2) enuatrol, oleic acid, ethyl alcohol and enough selenium powders are added sequentially in the acetic acid cadmium solution that step 1) obtains, room
Temperature stirring, obtains emulsion；
3) emulsion that step 2) obtains is transferred in ptfe autoclave, ptfe autoclave is put into
Into baking oven, isothermal reaction, after taking-up, cooled to room temperature obtains the first solution；
4) zinc acetate and sodium sulphate are dissolved in ultra-pure water successively, obtain the second solution, and to second solution into
Row nitrogen is bubbled protection；
5) second solution that step 4) obtains is added in first solution that step 3) obtains and is mixed
Solution is stirred the mixed solution in the case where nitrogen is bubbled protective condition, mixed solution is transferred to poly- four again after stirring
In vinyl fluoride reaction kettle, then ptfe autoclave is put into baking oven, isothermal reaction obtains reaction solution；
6) reaction solution that step 5) obtains is purified and is dried, obtain CdSe/ZnS quantum dots.
Based on the above-mentioned technical proposal, CdSe/ZnS quantum dots can be prepared.The preparation method mild condition, process peace
Entirely, easy to implement, it is at low cost.
Specifically, in step 1), cadmium acetate is dissolved in ultra-pure water, it is 0.05~0.1mol/L's to obtain molar concentration
Acetic acid cadmium solution.
Specifically, in step 2), by 1~2g enuatrols, 0.5~2mL oleic acid, 5~20mL ethyl alcohol and enough selenium powders according to
It is secondary to be added in the acetic acid cadmium solution that step 1) obtains, it is stirred at room temperature 2~4 hours, it is 0.03~0.06mol/L to obtain Se content
Emulsion.
Specifically, in step 3), isothermal reaction is to be reacted 3~6 hours at 150~200 DEG C.
Specifically, in step 4), in second solution：The molar concentration of zinc acetate is 0.1~0.3mol/L, sodium sulphate
Molar concentration be 0.1~0.3mol/L.
Specifically, in step 5), mixing time is 10~20 minutes；Isothermal reaction is that 3~6 are reacted at 150~200 DEG C
Hour.
Specifically, in step 6), the reaction solution that step 5) obtains is centrifuged, to the anhydrous second of isolated solid phase
Alcohol is washed, and is dried in vacuo again after washing, and CdSe/ZnS quantum dots are obtained.
Specifically, the rotating speed of centrifugation is 4000~8000r/min, the time of centrifugation is 10~30min；Absolute ethyl alcohol washs
Number be 2~3 times.
The beneficial effects of the invention are as follows：The preparation method of CdSe/ZnS quantum dots provided by the invention and existing method phase
Than the present invention has the characteristics that easy to operate and at low cost；Meanwhile the raw materials such as cadmium acetate, enuatrol, oleic acid, ethyl alcohol and Se powder
It is cheap, it is nontoxic, it is safe.The present invention raw material be easier to obtain, facilitate realization mass produce, can efficiently,
Inexpensively batch synthesis quantum dot, makes it be applied to the nano material of biological fluorescent labelling.
Description of the drawings
Fig. 1 is the flow chart of the preparation method of CdSe/ZnS quantum dots provided by the present invention.
Specific implementation mode
The principles and features of the present invention are described below, and illustrated embodiment is served only for explaining the present invention, is not intended to
Limit the scope of the present invention.
Implement 1
The preparation method of CdSe/ZnS quantum dots includes the following steps：
1) cadmium acetate is dissolved in ultra-pure water, obtains the acetic acid cadmium solution that molar concentration is 0.1mol/L, and nitrogen rouses
Bubble protection；
2) 1g enuatrols, 2mL oleic acid, 5mL ethyl alcohol and enough selenium powders are added sequentially to the cadmium acetate that step 1) obtains
It in solution, is stirred at room temperature 4 hours, obtains the emulsion that Se content is 0.03mol/L；
3) emulsion that step 2) obtains is transferred in ptfe autoclave, ptfe autoclave is put into baking
In case, isothermal reaction 3 hours at 200 DEG C, after taking-up, cooled to room temperature obtains the first solution；
4) zinc acetate and sodium sulphate are dissolved in ultra-pure water successively, obtain the second solution, and nitrogen is bubbled protection, it is described
In second solution：The molar concentration of zinc acetate is 0.3mol/L, and the molar concentration of sodium sulphate is 0.1/L；
5) second solution that step 4) obtains is added in the first solution that step 3) obtains and obtains mixed solution,
The mixed solution is stirred in the case where nitrogen is bubbled protective condition, mixing time is 20 minutes, then mixed solution is transferred to
In ptfe autoclave, ptfe autoclave is put into baking oven, isothermal reaction 6 hours at 150 DEG C, is obtained anti-
Answer liquid；
6) reaction solution that step 5) obtains is purified and is dried, obtain CdSe/ZnS quantum dots, purity 99.0%.
Implement 2
The preparation method of CdSe/ZnS quantum dots includes the following steps：
1) cadmium acetate is dissolved in ultra-pure water, obtains the acetic acid cadmium solution that molar concentration is 0.05mol/L, and nitrogen rouses
Bubble protection；
2) 2g enuatrols, 0.5mL oleic acid, 20mL ethyl alcohol and enough selenium powders are added sequentially to the acetic acid that step 1) obtains
It in cadmium solution, is stirred at room temperature 2 hours, obtains the emulsion that Se content is 0.06mol/L；
3) emulsion that step 2) obtains is transferred in ptfe autoclave, ptfe autoclave is put into baking
In case, isothermal reaction 6 hours at 150 DEG C, after taking-up, cooled to room temperature obtains the first solution；
4) zinc acetate and sodium sulphate are dissolved in ultra-pure water successively, obtain the second solution, and nitrogen is bubbled protection, it is described
In second solution：The molar concentration of zinc acetate is 0.1mol/L, and the molar concentration of sodium sulphate is 0.3mol/L；
5) second solution that step 4) obtains is added in the first solution that step 3) obtains and obtains mixed solution,
The mixed solution is stirred in the case where nitrogen is bubbled protective condition, mixing time is 10 minutes, then mixed solution is transferred to
In ptfe autoclave, ptfe autoclave is put into baking oven, isothermal reaction 3 hours at 200 DEG C, is obtained anti-
Answer liquid；
6) reaction solution that step 5) obtains is purified and is dried, obtain CdSe/ZnS quantum dots, purity 98.5%.
Implement 3
The preparation method of CdSe/ZnS quantum dots includes the following steps：
1) cadmium acetate is dissolved in ultra-pure water, obtains the acetic acid cadmium solution that molar concentration is 0.75mol/L, and nitrogen rouses
Bubble protection；
2) 1.5g enuatrols, 1.5mL oleic acid, 10mL ethyl alcohol and enough selenium powders are added sequentially to the vinegar that step 1) obtains
It in sour cadmium solution, is stirred at room temperature 3 hours, obtains the emulsion that Se content is 0.045mol/L；
3) emulsion that step 2) obtains is transferred in ptfe autoclave, ptfe autoclave is put into baking
In case, isothermal reaction 4.5 hours at 180 DEG C, after taking-up, cooled to room temperature obtains the first solution；
4) zinc acetate and sodium sulphate are dissolved in ultra-pure water successively, obtain the second solution, and nitrogen is bubbled protection, it is described
In second solution：The molar concentration of zinc acetate is 0.2mol/L, and the molar concentration of sodium sulphate is 0.2mol/L；
5) second solution that step 4) obtains is added in the first solution that step 3) obtains and obtains mixed solution,
The mixed solution is stirred in the case where nitrogen is bubbled protective condition, mixing time is 15 minutes, then mixed solution is transferred to
In ptfe autoclave, ptfe autoclave is put into baking oven, isothermal reaction 5 hours at 175 DEG C, is obtained anti-
Answer liquid；
6) reaction solution that step 5) obtains is purified and is dried, obtain CdSe/ZnS quantum dots, purity 99.2%.
CdSe/ZnS quantum dots preparation method synthesis condition provided by the invention requires relatively low, nucleocapsid CdSe/ZnS amounts
Son point usually selects TOP/TOPO/HDA to do dicyandiamide solution, at a high temperature of 300 DEG C or more, obtains different-grain diameter and fluorescent emission
Quantum dot.But solvent that this method uses is inflammable and explosive, expensive and be more toxic, and reacts the height at 300 DEG C or more
Se complex solutions are injected in Cd precursors under temperature, obtain the quantum dot of different-grain diameter and fluorescent emission, and it is provided by the invention
Synthetic method maximum 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；Together
When, TOP, TOPO solvent for using in above-mentioned tradition CdSe/ZnS quantum dot building-up processes there are it is inflammable, explosive, be more toxic,
The shortcomings of oxidizable, there are security risks, need to generally operate under vacuum, application range is obviously reduced.
CdSe/ZnS quantum dots preparation method provided by the invention, can effectively avoid and closed by metallo-organic compound route
At the uncontrollable situation of even particle size distribution reaction caused by CdSe/ZnS quantum dot high temperature, and reaction condition requirement is low,
Raw material is cheap to be easy to get, and 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 (8)
1. a kind of preparation method of CdSe/ZnS quantum dots, which is characterized in that include the following steps：
1) cadmium acetate is dissolved in ultra-pure water, obtains acetic acid cadmium solution, and nitrogen is carried out to the acetic acid cadmium solution and is bubbled guarantor
Shield；
2) enuatrol, oleic acid, ethyl alcohol and enough selenium powders are added sequentially in the acetic acid cadmium solution that step 1) obtains, room temperature is stirred
It mixes, obtains emulsion；
3) emulsion that step 2) obtains is transferred in ptfe autoclave, ptfe autoclave is put into baking
In case, isothermal reaction, after taking-up, cooled to room temperature obtains the first solution；
4) zinc acetate and sodium sulphate are dissolved in ultra-pure water successively, obtain the second solution, and nitrogen is carried out to second solution
Gas bell is protected；
5) second solution that step 4) obtains is added in first solution that step 3) obtains and obtains mixed solution,
The mixed solution is stirred in the case where nitrogen is bubbled protective condition, mixed solution is transferred to polytetrafluoroethylene (PTFE) again after stirring
In reaction kettle, then ptfe autoclave is put into baking oven, isothermal reaction obtains reaction solution；
6) reaction solution that step 5) obtains is purified and is dried, obtain CdSe/ZnS quantum dots.
2. the preparation method of CdSe/ZnS quantum dots according to claim 1, it is characterised in that：In step 1), by acetic acid
Cadmium is dissolved in ultra-pure water, obtains the acetic acid cadmium solution that molar concentration is 0.05~0.1mol/L.
3. the preparation method of CdSe/ZnS quantum dots according to claim 1, it is characterised in that：In step 2), by 1~2g
Enuatrol, 0.5~2mL oleic acid, 5~20mL ethyl alcohol and enough selenium powders are added sequentially to the acetic acid cadmium solution that step 1) obtains
In, it is stirred at room temperature 2~4 hours, obtains the emulsion that Se content is 0.03~0.06mol/L.
4. the preparation method of CdSe/ZnS quantum dots according to claim 1, it is characterised in that：In step 3), constant temperature is anti-
It should be and reacted 3~6 hours at 150~200 DEG C.
5. the preparation method of CdSe/ZnS quantum dots according to claim 1, which is characterized in that in step 4), described
In two solution：The molar concentration of zinc acetate is 0.1~0.3mol/L, and the molar concentration of sodium sulphate is 0.1~0.3mol/L.
6. the preparation method of CdSe/ZnS quantum dots according to claim 1, it is characterised in that：In step 5), when stirring
Between be 10~20 minutes；Isothermal reaction is to be reacted 3~6 hours at 150~200 DEG C.
7. the preparation method of CdSe/ZnS quantum dots according to any one of claims 1 to 6, it is characterised in that：In step 6),
The reaction solution that step 5) obtains is centrifuged, isolated solid phase is washed with absolute ethyl alcohol, vacuum again after washing
It is dry, obtain CdSe/ZnS quantum dots.
8. the preparation method of CdSe/ZnS quantum dots according to claim 7, it is characterised in that：The rotating speed of centrifugation is 4000
~8000r/min, centrifugation time be 10~30min；The number of absolute ethyl alcohol washing is 2~3 times.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050054004A1 (en) * | 2003-09-10 | 2005-03-10 | The Regents Of The University Of California | Graded core/shell semiconductor nanorods and nanorod barcodes |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050054004A1 (en) * | 2003-09-10 | 2005-03-10 | The Regents Of The University Of California | Graded core/shell semiconductor nanorods and nanorod barcodes |
Non-Patent Citations (2)
| Title |
|---|
| 杨保升等: "CdSe/ZnS量子点的合成及表征", 《成都电子机械高等专科学校学报》 * |
| 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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