CN105885824A - Preparation method of ZnCdSe/ZnS quantum dots - Google Patents
Preparation method of ZnCdSe/ZnS quantum dots Download PDFInfo
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- CN105885824A CN105885824A CN201610371227.6A CN201610371227A CN105885824A CN 105885824 A CN105885824 A CN 105885824A CN 201610371227 A CN201610371227 A CN 201610371227A CN 105885824 A CN105885824 A CN 105885824A
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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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
Abstract
The invention provides a preparation method of ZnCdSe/ZnS quantum dots. The method comprises the following steps that 1, a zinc source, a cadmium source, organic acid and/or organic amine and an organic solvent are stirred and heated to be dissolved after shielding gas is introduced to obtain a zinc and cadmium mixed pro-solution; 2, the solution is heated to 200-350 DEG C, and then a selenium source is injected into the solution within 30 s; 3, a sulfur source or sulfur and zinc source mixed solution is added drop by drop; 4, the temperature of 200-350 DEG C is kept constant, then cooling is performed to reach the room temperature, and separation and purification are performed to obtain ZnCdSe/ZnS quantum dots. The preparation method of the ZnCdSe/ZnS quantum dots is safety to implement, simple, controllable, low in cost, and capable of achieving repetition and amplification; the obtained quantum dots are uniform and controllable in size and appearance, the monodipserity is good, the fluorescence quantum yield is high, and the good stability on the high-temperature, washing and water dissolution modification and other conditions is good.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, in particular to one simple and rapid " one kettle way " system
The method of standby ZnCdSe/ZnS quantum dot.
Background technology
Quantum dot, nanocrystalline also known as fluorescence semiconductor, because of its unique excellent optical property, it is widely used in biological doctor
Learn the research in the field such as detection and imaging, solar cell and photoelectric device.
Although there being at present much document reports about synthesis high-quality quantum dot, but mostly exist cost of material high,
Synthesis technique is complicated, compared with difficult control, time-consuming long, particle diameter compared with problems such as big, single yield little (generally less than 1g)；
And quantum dot quality that the simple and quick method of technique is often synthesized is not high enough, therefore, develops the conjunction of more green simplicity
It is the most necessary that one-tenth method prepares higher-quality quantum dot.
Photoluminescent property in view of quantum dot is one of its topmost character, and the fluorescence of quantum dot is mainly by the radiation of exciton
Compound generation, and exciton is combined and includes two kinds of mistakes of radiation recombination and non-radiative recombination (Auger is combined, phonon is combined)
Journey, if non-radiative recombination process can be effectively reduced, just can be greatly improved the rate of radiative recombination of exciton, also can significantly carry
The fluorescence quantum yield of high quantum dot；Non-radiative recombination is largely that internal by quantum dot and surface defect causes
, it addition, these defects also can affect the stability etc. of quantum dot, so it is the most necessary for trying every possible means to eliminate these defects
's.
A lattice misfit rate of about 14% is had between CdSe and ZnS body phase material, simple CdSe/ZnS core-shell type quantum point,
Defect between its nucleocapsid interface is difficult to avoid.And alloy type ZnCdSe/ZnS quantum dot can effectively reduce because of lattice
The defect that mispairing brings；Building-up process is not isolated, purifies, technological operation can be greatly simplified, be also beneficial to boundary
The formation of face alloy structure, these all will further improve the quality of quantum dot.
Summary of the invention
It is desirable to provide a kind of simple and quick method controllably preparing ZnCdSe/ZnS quantum dot, and the amount obtained
Half-peak breadth is narrow, fluorescence quantum yield is high, homogeneous adjustable, the good stability of particle diameter pattern for son point.
Realizing the technical scheme that above-mentioned purpose of the present invention used is:
The preparation method of a kind of ZnCdSe/ZnS quantum dot, comprises the following steps:
1) by zinc source, cadmium source, organic acid and/or organic amine, organic solvent under agitation, it is passed through protection gas, adds
Heat, to dissolving, obtains the mixing precursor solution of zinc and cadmium；
2) heat the solution to 200～350 DEG C, then within the time of 30 seconds, selenium source is injected in solution；
3) mixed liquor in sulphur source or sulphur source and zinc source is dropwise dripped；
4) it is incubated at 200～350 DEG C, is then cooled to room temperature, separate, obtain ZnCdSe/ZnS quantum dot after purification.
Step 1) described in zinc source be zinc powder, zinc chloride, zinc carbonate, zinc oxide, zinc oxalate, zinc acetate, stearic acid
One or more in zinc, zinc undecylenate and zinc diethyl dithiocarbamate；Described cadmium source is cadmium powder, chlorine
Cadmium, cadmium carbonate, cadmium oxide, cadmium oxalate, cadmium acetate, cadmium stearate, undecenoic acid cadmium and diethyl-dithio amino
One or more in formic acid cadmium；Described organic amine is in the saturated of carbon number >=8 or unsaturated fat amine
Plant or two or more；Described organic acid is one or more in the saturated of carbon number >=8 or unrighted acid；
Described organic solvent two or more for boiling point higher than 200 DEG C the tetradecane, hexadecane, octadecane, eicosane, 1-18
In alkene, phenylate, benzyl oxide, atoleine, cetylamine and octadecylamine one or more；Described protection gas be nitrogen,
One or more in argon gas, helium and neon.
Step 1) described in the total amount in zinc source and cadmium source be 1:2～1:50 with the mol ratio of organic acid and/or organic amine total amount.
Step 2) described in selenium source be inorganic selenium solution, organic selenium compounds solution and selenium organophosphite ligand polymer solution in
One or more；Wherein, described inorganic selenium includes that selenium powder, selenium dioxide, described Organic Selenium include selenol, selenium
Ether, selenazoles, selenophen, seleno acid esters, selenoprotein, two selenium compounds and selenium substituted acid amide, the organophosphite ligand compound of described selenium
Including tri-n-butyl phosphine selenium, tri-n-octyl phosphine selenium and diphenylphosphine selenium.
The concentration of selenium source is 0.01～10mol/L.
Step 3) described sulphur source is that the organophosphite ligand compound of the organic solution of inorganic sulfur, organosulfur compound solution and sulphur is molten
One or more in liquid；Wherein, the organic solution of described inorganic sulfur includes the 1-octadecylene solution of sulphur powder, sulphur powder
Atoleine solution, the saturated or unsaturated fat amine aqueous solution of carbon number >=8 of sulphur powder and carbon number >=8 of sulphur powder
Saturated or unsaturated fat acid solution, described organic sulfur includes mercaptan, thioether, sulphur azoles, thiocarbamide, thioester and sulphur
For acid amides etc., the organophosphite ligand compound of described sulphur includes tri-n-butyl phosphine sulphur, tri-n-octyl phosphine sulphur and diphenylphosphine sulphur.
The concentration in sulphur source is 0.01～10mol/L.
Step 4) described temperature retention time is 0.01～48h.
The preparation method operation of the ZnCdSe/ZnS quantum dot of the present invention is safe, the most controlled, it is only necessary to " note one ",
Low cost, it is easy to repeat and amplify；The quantum dot size of preparation, pattern are homogeneous controlled, and monodispersity is good, fluorescent quantum
Productivity is high, has good stability under the conditions of high temperature, washing and water-solubleization modification etc..Can be widely applied to phototube
Part, solar cell and the field such as biomedical detection and imaging.
Accompanying drawing explanation
The fluorescence spectrum figure of the ZnCdSe/ZnS quantum dot that Fig. 1 provides for the present invention；
The transmission electron microscope picture of the ZnCdSe/ZnS quantum dot that Fig. 2 provides for the present invention.
Detailed description of the invention
Below by specific embodiment, the invention will be further described, but should not be construed as limitation of the present invention.If not
Specified otherwise, the conventional means that technological means used by following example of the present invention is well known to the skilled person.
Embodiment 1
By 20mmol zinc oxide, 1mmol cadmium oxide, 2g tetradecylphosphonic acid, 10mL oleic acid and 90mL1-octadecylene
Join in the flask with thermometer and condenser pipe, under agitation, logical argon gas, it is heated to 260 DEG C；Treat completely
After dissolving, it is cooled to 150 DEG C, vacuumizes 30min；Stopping vacuumizes, and starts logical argon gas, is warming up to 280 DEG C, soon
Speed (in 30 seconds) injection 5mL selenium source；It is cooled to 260 DEG C, dropwise drips sulphur source 18mL with the speed of 0.2mL/min；
It is cooled to 220 DEG C after adding sulphur source, is incubated 30min；Being down to room temperature, add ethanol, 10000rpm/min is centrifuged 5min,
Supernatant discarded is precipitated, then passes sequentially through n-hexane, ethanol dissolving-deposition and purification.Products therefrom is dissolved in n-hexane,
Recording fluorescence spectrum with sepectrophotofluorometer, emission peak is positioned at 506nm.
Selenium source described in the present embodiment is prepared for using following methods: 80mg selenium powder and 5mL1-octadecylene are mixed,
Ultrasonic 30min, prepares the selenium source storing solution of 0.2mol/L.In the present embodiment, sulphur source is for using following methods to prepare:
Joining in there-necked flask by 320mg sulphur powder and 20mL1-octadecylene, logical argon gas, heating, at 150 DEG C, is incubated 10 points
Clock, obtains the sulphur source solution of 0.5mol/L.
Embodiment 2
By 20mmol zinc acetate, 1mmol cadmium oxalate, 1.4g octadecylphosphonic acid, 12mL oleic acid and 88mL liquid
Paraffin joins in the four-hole boiling flask with thermometer and condenser pipe, under agitation, logical argon gas, it is heated to 210 DEG C；
Until completely dissolved, it is cooled to 140 DEG C, vacuumizes 30min；Stopping vacuumizes, and starts logical argon gas, is warming up to 280
DEG C, fast injection 5mL selenium source；It is cooled to 260 DEG C, dropwise drips sulphur source 18mL with the speed of 0.3mL/min；Add
It is cooled to 240 DEG C after adding sulphur source, is incubated 20min；Being down to room temperature, add ethanol, 10000rpm/min is centrifuged 5min,
Supernatant discarded is precipitated, then passes sequentially through n-hexane, ethanol dissolving-deposition and purification.Products therefrom is dissolved in n-hexane,
Recording fluorescence spectrum with sepectrophotofluorometer, emission peak is positioned at 529nm.
Selenium source described in the present embodiment is prepared for using following methods: 80mg selenium powder and 5mL1-octadecylene are mixed,
Ultrasonic 30min, prepares the selenium source storing solution of 0.2mol/L.In the present embodiment, sulphur source is for using following methods to prepare:
320mg sulphur powder and 20mL tri-n-butyl phosphine are mixed, obtains the sulphur source solution of 0.5mol/L.
Embodiment 3
By 20mmol zinc acetate, 1mmol cadmium acetate, 1g octadecylphosphonic acid, 15mL oleic acid and 85mL liquid stone
Wax joins in the flask with thermometer and condenser pipe, under agitation, logical argon gas, it is heated to 260 DEG C；Treat
After CL, it is cooled to 150 DEG C, vacuumizes 30min；Stopping vacuumizes, and starts logical argon gas, is warming up to 290 DEG C,
Fast injection 5mL selenium source.It is cooled to 260 DEG C, dropwise drips sulphur source 10mL with the speed of 0.15mL/min；Add sulphur
It is cooled to 220 DEG C behind source, is incubated 120min；Being down to room temperature, add ethanol, 10000rpm/min is centrifuged 5min, abandons
Go supernatant to be precipitated, then pass sequentially through n-hexane, ethanol dissolving-deposition and purification.Products therefrom is dissolved in n-hexane, uses
Sepectrophotofluorometer records fluorescence spectrum, and emission peak is positioned at 541nm.
Selenium source described in the present embodiment is prepared for using following methods: 80mg selenium powder and 5mL tri-n-octyl phosphine are mixed,
Ultrasonic 10min, prepares the selenium source storing solution of 0.2mol/L.In the present embodiment, sulphur source is for using following methods to prepare:
4mL1-octyl mercaptan and 7.4mL atoleine are mixed, obtains the sulphur source solution of 2mol/L.
Embodiment 4
By 20mmol zinc stearate, 1mmol cadmium acetate, 0.1g hexadecyl phosphonic acid, 19mL oleic acid and 80mL liquid
Paraffin body joins in the flask with thermometer and condenser pipe, under agitation, logical argon gas, it is heated to 230 DEG C；
Until completely dissolved, it is cooled to 120 DEG C, vacuumizes 30min；Stopping vacuumizes, and starts logical argon gas, is warming up to 290
DEG C, fast injection 5mL selenium source.It is cooled to 260 DEG C, dropwise drips sulphur source 10mL with the speed of 0.15mL/min；Add
It is cooled to 220 DEG C after adding sulphur source, is incubated 120min；Being down to room temperature, add ethanol, 10000rpm/min is centrifuged 5min,
Supernatant discarded is precipitated, then passes sequentially through n-hexane, ethanol dissolving-deposition and purification.Products therefrom is dissolved in n-hexane,
Recording fluorescence spectrum with sepectrophotofluorometer, emission peak is positioned at 570nm.
Selenium source described in the present embodiment is prepared for using following methods: 80mg selenium powder and 5mL tri-n-octyl phosphine are mixed
Uniformly, the selenium source storing solution of 0.2mol/L is prepared.In the present embodiment, sulphur source is for using following methods to prepare: by 4mL1-
Octyl mercaptan and 7.4mL atoleine mix, and obtain the sulphur source solution of 2mol/L.
Embodiment 5
20mmol zinc acetate, 1mmol cadmium carbonate, 22mL oleic acid and 78mL atoleine are joined with temperature
In the flask of meter and condenser pipe, under agitation, logical argon gas, it is heated to 260 DEG C；Until completely dissolved, it is cooled to
130 DEG C, vacuumize 30min；Stopping vacuumizes, and starts logical argon gas, is warming up to 290 DEG C, fast injection 5mL selenium source.
It is cooled to 260 DEG C, dropwise drips sulphur source 10mL with the speed of 0.15mL/min；It is cooled to 230 DEG C after adding sulphur source,
Insulation 120min；Being down to room temperature, add ethanol, 10000rpm/min is centrifuged 5min, and supernatant discarded is precipitated, then
Pass sequentially through n-hexane, ethanol dissolving-deposition and purification.Products therefrom is dissolved in n-hexane, records with sepectrophotofluorometer
Fluorescence spectrum, emission peak is positioned at 585nm.
Selenium source described in the present embodiment is prepared for using following methods: 120mg selenium powder and 5mL atoleine are mixed,
Ultrasonic 10min, prepares the selenium source storing solution of 0.3mol/L.In the present embodiment, sulphur source is for using following methods to prepare:
5mL1-lauryl mercaptan and 5.5mL atoleine are mixed, obtains the sulphur source solution of 2mol/L.
Embodiment 6
20mmol zinc stearate, 1mmol cadmium stearate, 25mL oleic acid and 75mL atoleine are joined with
In the flask of thermometer and condenser pipe, under agitation, logical argon gas, it is heated to 260 DEG C；Until completely dissolved, fall
Temperature, to 150 DEG C, vacuumizes 30min；Stopping vacuumizes, and starts logical argon gas, is warming up to 280 DEG C, fast injection 5mL
Selenium source.It is cooled to 260 DEG C, dropwise drips sulphur source 19mL with the speed of 0.3mL/min；It is cooled to 220 after adding sulphur source
DEG C, it is incubated 120min；Being down to room temperature, add ethanol, 10000rpm/min is centrifuged 5min, and supernatant discarded is precipitated,
Pass sequentially through n-hexane, ethanol dissolving-deposition and purification again.Products therefrom is dissolved in n-hexane, surveys with sepectrophotofluorometer
Obtaining fluorescence spectrum, emission peak is positioned at 612nm.
Selenium source described in the present embodiment is prepared for using following methods: 160mg selenium powder and 5mL tri-n-butyl phosphine are mixed
Close uniform, to prepare 0.4mol/L selenium source storing solution.In the present embodiment, sulphur source is for using following methods to prepare: will
4mL1-octyl mercaptan and 18.8mL1-octadecylene mix, and obtain the sulphur source solution of 1mol/L.
The fluorescence spectrum figure of product prepared in above example of the present invention is as it is shown in figure 1, embodiment 1 gained in Fig. 1
The emission peak of product is positioned at 506nm, and the emission peak of embodiment 2 products therefrom is positioned at 529nm, embodiment 3 products therefrom
Emission peak be positioned at 541nm, the emission peak of embodiment 4 products therefrom is positioned at 570nm, embodiment 5 products therefrom send out
Penetrating peak and be positioned at 585nm, the emission peak of embodiment 6 products therefrom is positioned at 612nm.
The transmission electron microscope picture of the above embodiment of the present invention 2, embodiment 4 and the product obtained by embodiment 6 as in figure 2 it is shown,
As can be seen from Figure 2 obtained quantum dot size, pattern are homogeneous, and monodispersity is good.
Claims (8)
1. the preparation method of a ZnCdSe/ZnS quantum dot, it is characterised in that comprise the following steps:
1) by zinc source, cadmium source, organic acid and/or organic amine, organic solvent under agitation, it is passed through protection gas, adds
Heat, to dissolving, obtains the mixing precursor solution of zinc and cadmium；
2) heat the solution to 200～350 DEG C, then within the time of 30 seconds, selenium source is injected in solution；
3) mixed liquor in sulphur source or sulphur source and zinc source is dropwise dripped；
4) it is incubated at 200～350 DEG C, is then cooled to room temperature, separate, obtain ZnCdSe/ZnS quantum dot after purification.
Preparation method the most according to claim 1, it is characterised in that: step 1) described in zinc source be zinc powder, chlorine
Change zinc, zinc carbonate, zinc oxide, zinc oxalate, zinc acetate, zinc stearate, zinc undecylenate and diethyl-dithio amino
One or more in zinc formate；Described cadmium source is cadmium powder, caddy, cadmium carbonate, cadmium oxide, cadmium oxalate, vinegar
One or more in acid cadmium, cadmium stearate, undecenoic acid cadmium and cadmium diethyl dithiocarbamate；Described have
Machine amine is one or more in the saturated of carbon number >=8 or unsaturated fat amine；Described organic acid is carbon atom
Number >=8 saturated or unrighted acid in one or more；Described organic solvent is two or more to be higher than for boiling point
The tetradecane of 200 DEG C, hexadecane, octadecane, eicosane, 1-octadecylene, phenylate, benzyl oxide, atoleine, 16
In amine and octadecylamine one or more；Described protection gas is one or both in nitrogen, argon gas, helium and neon
Above.
Preparation method the most according to claim 1, it is characterised in that: step 1) described in zinc source and cadmium source total
Amount is 1:2～1:50 with the mol ratio of organic acid and/or organic amine total amount.
Preparation method the most according to claim 1, it is characterised in that: step 2) described in selenium source be that inorganic selenium is molten
One or more in the organophosphite ligand polymer solution of liquid, organic selenium compounds solution and selenium；Wherein, described inorganic
Selenium include selenium powder, selenium dioxide, described Organic Selenium include selenol, selenide, selenazoles, selenophen, seleno acid esters, selenoprotein,
Two selenium compounds and selenium substituted acid amide, the organophosphite ligand compound of described selenium includes tri-n-butyl phosphine selenium, tri-n-octyl phosphine selenium and two
Phenylphosphine selenium.
5. according to the preparation method described in claim 1 or 4, it is characterised in that: the concentration of selenium source is 0.01～10mol/L.
Preparation method the most according to claim 1, it is characterised in that: step 3) described sulphur source is having of inorganic sulfur
One or more in the organophosphite ligand polymer solution of machine solution, organosulfur compound solution and sulphur；Wherein, described
The organic solution of inorganic sulfur include the 1-octadecylene solution of sulphur powder, the atoleine solution of sulphur powder, sulphur powder carbon number >=
Saturated or the unsaturated fat acid solution of carbon number >=8 of saturated or unsaturated fat amine aqueous solution and the sulphur powder of 8, described
Organic sulfur includes mercaptan, thioether, sulphur azoles, thiocarbamide, thioester and thioamides etc., the organophosphite ligand compound of described sulphur
Including tri-n-butyl phosphine sulphur, tri-n-octyl phosphine sulphur and diphenylphosphine sulphur.
7. according to the preparation method described in claim 1 or 6, it is characterised in that: the concentration in sulphur source is 0.01～10mol/L.
Preparation method the most according to claim 1, it is characterised in that: step 4) described temperature retention time is 0.01～48h.
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| CN107686731A (en) * | 2017-09-20 | 2018-02-13 | 天津市中环量子科技有限公司 | A kind of alloy quantum dot and preparation method thereof |
| CN108163818A (en) * | 2018-01-11 | 2018-06-15 | 武汉华思创新科技有限公司 | A kind of preparation method of PbSe quantum dots |
| CN109575300A (en) * | 2018-11-15 | 2019-04-05 | 三明学院 | A kind of synthetic method of conductive metal organic framework materials |
| CN109817921A (en) * | 2019-01-22 | 2019-05-28 | 五邑大学 | A kind of sulfur doping MXene negative electrode material and its preparation method and application |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106566553A (en) * | 2016-10-20 | 2017-04-19 | 深圳天吉新创科技有限公司 | Methods for synthesizing ZnxCd1-xSe, ZnxCd1-xSe/ZnS and ZnxCd1-xSe/ZnS/ZnS alloy quantum dots |
| CN107686731A (en) * | 2017-09-20 | 2018-02-13 | 天津市中环量子科技有限公司 | A kind of alloy quantum dot and preparation method thereof |
| CN107686731B (en) * | 2017-09-20 | 2021-04-09 | 天津市中环量子科技有限公司 | Alloy quantum dot and preparation method thereof |
| CN108163818A (en) * | 2018-01-11 | 2018-06-15 | 武汉华思创新科技有限公司 | A kind of preparation method of PbSe quantum dots |
| CN109575300A (en) * | 2018-11-15 | 2019-04-05 | 三明学院 | A kind of synthetic method of conductive metal organic framework materials |
| CN109817921A (en) * | 2019-01-22 | 2019-05-28 | 五邑大学 | A kind of sulfur doping MXene negative electrode material and its preparation method and application |
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Application publication date: 20160824 |