CN106590665A - Preparation method of CdSe quantum dots with controllable spectrum - Google Patents
Preparation method of CdSe quantum dots with controllable spectrum Download PDFInfo
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- CN106590665A CN106590665A CN201710117670.5A CN201710117670A CN106590665A CN 106590665 A CN106590665 A CN 106590665A CN 201710117670 A CN201710117670 A CN 201710117670A CN 106590665 A CN106590665 A CN 106590665A
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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 invention discloses a preparation method of CdSe quantum dots with controllable spectrum. The preparation method comprises the following steps: step 1, a Se precursor is prepared through steps as follows: Se powder is added to tri-n-octylphosphine and heated to 100 DEG C, nitrogen is introduced for protection, a product is cooled to the room temperature after sufficient reaction, and a colorless and transparent liquid is taken; step 2, tetradecyl phosphoric acid, octadecylamine, tri-n-octylphosphine and cadmium oxide are taken and mixed, the mixture is heated with nitrogen introduction, vacuumized after the temperature reaches 100 DEG C and kept in the vacuum state, then nitrogen is introduced again, the mixture is heated to 330 DEG C, kept for 10 min and then cooled to 275 DEG C, the Se precursor obtained in the step 1 is added, and the CdSe quantum dots are separated and taken out within 4-80 s after addition of the Se precursor. The CdSe quantum dots with emission wavelength being 450 nm or smaller can be obtained with the method.
Description
Technical field
The present invention relates to a kind of CdSe quantum dot preparation method, the controllable CdSe quantum dot preparation side of particularly a kind of spectrum
Method, belongs to technical field of quantum dot preparation.
Background technology
Quantum dot is a kind of nano-particle elementary composition by II-VI group or iii-v.The particle diameter of quantum dot is typically situated between
Between 1～10nm, because electronics and hole are by quantum confinement, continuous band structure becomes the discrete energy with molecular characterization
Level structure, can launch fluorescence after being excited.Selenium powder is generally adopted in the preparation of CdSe quantum dot at present as selenium source, three n-octyls
Phosphine (TOP) prepares Se precursors as solvent, and CdO adds organic coating agent and cosolvent to obtain Cd precursors as cadmium source, mixes Se
CdSe quantum dot is obtained after precursor and Cd precursor reacting by heating certain hours.But the launch wavelength of the CdSe quantum dot for preparing is covered
Lid scope is 450 to 650nm, and existing preparation method all cannot stably obtain CdSe quantum of the launch wavelength less than 450nm
Point.
The content of the invention
For above-mentioned prior art defect, the task of the present invention is to provide a kind of controllable CdSe quantum dot of spectrum to prepare
Method, obtains CdSe quantum dot of the launch wavelength less than 450nm.
Technical scheme：The present invention provides technical scheme below：A kind of controllable CdSe quantum dot preparation method of spectrum, including
Step 1：Prepared by Se precursors, selenium powder addition tri-n-octyl phosphine is heated to into 100 DEG C is passed through after nitrogen protection fully reaction to be cooled to
Room temperature, takes colourless transparent liquid；Step 2：The mixing of myristyl phosphoric acid, 18-amine., trioctylphosphine and Aska-Rid. is taken, logical
Heated in the state of nitrogen, evacuation and vacuum state is kept after reaching 100 DEG C, nitrogen is passed through again and is heated to
330 DEG C maintain 10 minutes after be cooled to 275 DEG C, add Se precursors that step 1 obtains and in 4 to 80 seconds after Se precursors are added
Separate and take out CdSe quantum dot.
Preferably, the selenium powder and tri-n-octyl phosphine ratio are 456mg ︰ 10ml.
Preferably, the myristyl phosphoric acid, 18-amine., trioctylphosphine and Aska-Rid. mixing quality ratio are 56 ︰
The ︰ 14 of 350 ︰ 650.
Preferably, the taking-up CdSe quantum dot that separates is to add acetone in the solution for will add Se precursors, and waits molten
Liquid carries out centrifugal treating after further lowering the temperature.
Present invention advantage compared with prior art is：The method is added by control and take out after Se precursors CdSe quantum
The time of point controls its growth, obtains CdSe quantum dot of the launch wavelength less than 450nm.
Specific embodiment
The controllable CdSe quantum dot preparation method of spectrum includes,
Step 1：Weigh 114mg selenium powders and 2.5ml tri-n-octyl phosphines (TOP) are put into there-necked flask, stir at being heated to 100 DEG C
Mix and reacted.After being subsequently passed nitrogen and evacuation 3 times, lasting is passed through nitrogen.Stop heating after selenium powder is completely dissolved,
Continue to be passed through nitrogen until solution is down to room temperature, taking-up colourless transparent liquid.
Step 2：By 56mg myristyl phosphoric acid (TDPA), 0.35g 18-amine. (ODA), 0.65g trioctylphosphines
(TOPO) during, 14mg Aska-Rid .s (CdO) are put into there-necked flask, good seal flask simultaneously inserts thermometer.In the state of logical nitrogen
Under heated, solution is rendered as red troubled liquor and starts evacuation 30min after reaching 100 DEG C, and now liquid is in maroon.
Carrying out logical nitrogen again after evacuation is completed carries out being heated to 330 DEG C.After treating that target temperature reaches, continuous heating
10min, in the process liquid is gradually transparent in orange-yellow.Stopping heating after it is changed into clarifying carries out cooling to 275 DEG C,
The Se precursors prepared before addition, solution now is rendered as brown.Different time takes in 4 to 80 seconds after Se precursors are added
Go out centrifugal treating after solution adds acetone to be cooled down and obtain CdSe quantum dot, the CdSe quantum dot transmitted wave that different time takes out
Long such as following table.
The useable linear curve description over time of quantum dot light emitting wavelength：λ=433.23+0.15883*t, its medium wavelength
The unit in form is taken with the time.
Claims (4)
1. the controllable CdSe quantum dot preparation method of a kind of spectrum, it is characterised in that including step 1：Prepared by Se precursors, by selenium powder
Add tri-n-octyl phosphine to be heated to 100 DEG C and be passed through after nitrogen protection fully reaction to be cooled to room temperature, take colourless transparent liquid；Step
2：The mixing of myristyl phosphoric acid, 18-amine., trioctylphosphine and Aska-Rid. is taken, is heated in the state of logical nitrogen, reached
Evacuation and keep vacuum state to after 100 DEG C, be passed through again nitrogen carry out being heated to 330 DEG C maintain 10 minutes after be cooled to
275 DEG C, add the Se precursors of step 1 acquisition and separate in 4 to 80 seconds after Se precursors are added and take out CdSe quantum dot.
2. the controllable CdSe quantum dot preparation method of spectrum according to claim 1, it is characterised in that the selenium powder and three
N-octyl phosphine ratio is 456mg ︰ 10ml.
3. the controllable CdSe quantum dot preparation method of spectrum according to claim 1, it is characterised in that the myristyl
Phosphoric acid, 18-amine., trioctylphosphine and Aska-Rid. mixing quality ratio are the ︰ 14 of 56 ︰, 350 ︰ 650.
4. the controllable CdSe quantum dot preparation method of spectrum according to claim 1, it is characterised in that the separation is taken out
CdSe quantum dot is that acetone is added in the solution for will add Se precursors, and waits solution to carry out centrifugal treating after lowering the temperature.
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| CN201710117670.5A CN106590665B (en) | 2017-03-01 | 2017-03-01 | A kind of CdSe quantum dot preparation method that spectrum is controllable |
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| CN201710117670.5A CN106590665B (en) | 2017-03-01 | 2017-03-01 | A kind of CdSe quantum dot preparation method that spectrum is controllable |
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| CN106590665A true CN106590665A (en) | 2017-04-26 |
| CN106590665B CN106590665B (en) | 2019-03-01 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111718709A (en) * | 2020-07-01 | 2020-09-29 | 合肥福纳科技有限公司 | Post-processing method and preparation method of quantum dots, prepared quantum dots and application |
| CN113122265A (en) * | 2019-12-31 | 2021-07-16 | Tcl集团股份有限公司 | Composite material, preparation method thereof and quantum dot light-emitting diode |
| CN113528140A (en) * | 2021-08-25 | 2021-10-22 | 合肥福纳科技有限公司 | Method for removing impurity peak in quantum dot emission spectrum |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1743361A (en) * | 2005-09-22 | 2006-03-08 | 复旦大学 | Inorganic semiconductor nanocrystal and conjugated polymer hybrid material and its preparing method |
| CN101130693A (en) * | 2007-09-27 | 2008-02-27 | 上海交通大学 | Method of producing three fundamental quantum dot CdZnSe |
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2017
- 2017-03-01 CN CN201710117670.5A patent/CN106590665B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1743361A (en) * | 2005-09-22 | 2006-03-08 | 复旦大学 | Inorganic semiconductor nanocrystal and conjugated polymer hybrid material and its preparing method |
| CN101130693A (en) * | 2007-09-27 | 2008-02-27 | 上海交通大学 | Method of producing three fundamental quantum dot CdZnSe |
Non-Patent Citations (1)
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| 安利民,: "《含镉量子点的荧光性质》", 30 September 2015 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113122265A (en) * | 2019-12-31 | 2021-07-16 | Tcl集团股份有限公司 | Composite material, preparation method thereof and quantum dot light-emitting diode |
| CN111718709A (en) * | 2020-07-01 | 2020-09-29 | 合肥福纳科技有限公司 | Post-processing method and preparation method of quantum dots, prepared quantum dots and application |
| CN113528140A (en) * | 2021-08-25 | 2021-10-22 | 合肥福纳科技有限公司 | Method for removing impurity peak in quantum dot emission spectrum |
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| CN106590665B (en) | 2019-03-01 |
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Effective date of registration: 20210804 Address after: 215513 Building 1, No. 7, research institute road, Changshu Economic and Technological Development Zone, Suzhou, Jiangsu Patentee after: Suzhou kundao New Material Technology Co.,Ltd. Address before: 215500 Changshou City South Three Ring Road No. 99, Suzhou, Jiangsu Patentee before: CHANGSHU INSTITUTE OF TECHNOLOGY |