CN104498021A - Synthetic method for core-shell quantum dot which is capable of realizing emission of blue light to green light and possesses uniformly-alloyed core - Google Patents
Synthetic method for core-shell quantum dot which is capable of realizing emission of blue light to green light and possesses uniformly-alloyed core Download PDFInfo
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 76
- 238000010189 synthetic method Methods 0.000 title claims abstract description 16
- 239000011258 core-shell material Substances 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 22
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000011669 selenium Substances 0.000 claims abstract description 20
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 19
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 17
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 17
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 15
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 claims description 27
- PFRGXCVKLLPLIP-UHFFFAOYSA-N diallyl disulfide Chemical group C=CCSSCC=C PFRGXCVKLLPLIP-UHFFFAOYSA-N 0.000 claims description 22
- 239000005864 Sulphur Substances 0.000 claims description 18
- 239000000956 alloy Substances 0.000 claims description 18
- 229910045601 alloy Inorganic materials 0.000 claims description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000009413 insulation Methods 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 8
- 238000010792 warming Methods 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 238000001556 precipitation Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 125000004432 carbon atom Chemical group C* 0.000 claims description 6
- 229920006395 saturated elastomer Polymers 0.000 claims description 6
- 235000021122 unsaturated fatty acids Nutrition 0.000 claims description 6
- 150000004670 unsaturated fatty acids Chemical class 0.000 claims description 6
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 5
- 241001062009 Indigofera Species 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 150000001661 cadmium Chemical class 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 150000001336 alkenes Chemical class 0.000 claims description 3
- 238000002955 isolation Methods 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 2
- 150000001335 aliphatic alkanes Chemical group 0.000 claims description 2
- 238000009835 boiling Methods 0.000 claims description 2
- 229960004756 ethanol Drugs 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 235000003441 saturated fatty acids Nutrition 0.000 claims description 2
- 150000004671 saturated fatty acids Chemical class 0.000 claims description 2
- 239000000203 mixture Substances 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 2
- JLATXDOZXBEBJX-UHFFFAOYSA-N cadmium(2+);selenium(2-);sulfide Chemical compound [S-2].[Se-2].[Cd+2].[Cd+2] JLATXDOZXBEBJX-UHFFFAOYSA-N 0.000 abstract 1
- 239000003446 ligand Substances 0.000 abstract 1
- 229910052717 sulfur Inorganic materials 0.000 abstract 1
- 239000011593 sulfur Substances 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 11
- 239000007788 liquid Substances 0.000 description 7
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 6
- 238000005275 alloying Methods 0.000 description 6
- GWOWVOYJLHSRJJ-UHFFFAOYSA-L cadmium stearate Chemical compound [Cd+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O GWOWVOYJLHSRJJ-UHFFFAOYSA-L 0.000 description 6
- 238000005580 one pot reaction Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- -1 octadecylene Chemical group 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000006862 quantum yield reaction Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 3
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 3
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 3
- 239000005642 Oleic acid Substances 0.000 description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 3
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 2
- PFNQVRZLDWYSCW-UHFFFAOYSA-N (fluoren-9-ylideneamino) n-naphthalen-1-ylcarbamate Chemical compound C12=CC=CC=C2C2=CC=CC=C2C1=NOC(=O)NC1=CC=CC2=CC=CC=C12 PFNQVRZLDWYSCW-UHFFFAOYSA-N 0.000 description 1
- ZQRRBZZVXPVWRB-UHFFFAOYSA-N [S].[Se] Chemical compound [S].[Se] ZQRRBZZVXPVWRB-UHFFFAOYSA-N 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
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- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 238000011403 purification operation Methods 0.000 description 1
- JPJALAQPGMAKDF-UHFFFAOYSA-N selenium dioxide Chemical compound O=[Se]=O JPJALAQPGMAKDF-UHFFFAOYSA-N 0.000 description 1
- 125000003748 selenium group Chemical group *[Se]* 0.000 description 1
- VIDTVPHHDGRGAF-UHFFFAOYSA-N selenium sulfide Chemical compound [Se]=S VIDTVPHHDGRGAF-UHFFFAOYSA-N 0.000 description 1
- 229960005265 selenium sulfide Drugs 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Abstract
The invention discloses a synthetic method for a core-shell quantum dot which is capable of realizing emission of blue light to green light and possesses a uniformly-alloyed core. The core-shell quantum dot employs uniformly-alloyed cadmium selenide sulfide CdSexS1-x as a core and employs CdS as a shell, and the composition is shortly named CdSexS1-x/CdS, wherein x=0.05-0.60. By controlling the molar ratio of a sulfur source to a selenium source, the usage amount of a cadmium source and a ligand, and the reaction temperature and time in the synthesis process of the core-shell quantum dot, the emission peak wavelength of the core-shell quantum dot is continuously adjustable in the scope of 460-530 nm. The synthetic method has green and economic characteristics, the synthesis process and the product structure and performances are highly controllable, and the method is applicable to large-scale preparation of the quantum dot.
Description
One, technical field
The present invention relates to a kind of synthetic method of quantum dot, specifically a kind of indigo plant is to the synthetic method of the core-shell quanta dots of green emission, uniform alloy core.
Two, background technology
Quantum dot, owing to having the composition light emission performance relevant to size, is one of study hotspot of photoelectric material.Because quantum dot has good colour developing saturation ratio (half-peak width) and stability, in technique of display, there is good prospect of the application.In bluish-green red three primary colours display look unit, the research of ruddiness CdSe quantum dots is the most abundant, reaches good research level; Blue still insufficient relative to the research of ruddiness CdSe quantum dots with green light quantum point, still there are some problems.Blue emission is current to be realized primarily of CdS and ZnSe quantum dot, and CdS quantum dot is launched can reach 480nm, and ZnSe quantum dot emission can reach 445nm.But the radius of these quantum dots is close to the Bohr radius of material, and quantum confined effect dies down, their best quantum yield only can reach medium level.Although CdSe quantum dot also can launch blue light when reduced size, quantum dot poor stability under small size, synthesis difficulty is large.Current binary quantum dot realizes the blue efficient transmission to green glow (470-520nm) and is still a difficult point.But the green glow of the blue light of 470-480nm and 520-530nm is two colour developing primitives of total colouring, the quantum dot synthetic method that is efficient, economy developing this two section is the requirement of technique of display development.
Alloying is one of basic skills regulating (design) quantum dot emission, and the emission wavelength of ternary alloying quantum dot can regulate continuously between the wave band of two basic quantum dots, even owing to exceeding the wave band of basic quantum dot under nonlinear interaction.The CdSe of alloying
xs
1-xand Cd
xzn
1-xse is the quantum dot object launched to green section in indigo plant, existing more research, and achieves certain achievement.Existing synthetic method mainly contains hot note method and one pot of heating method, and the product structure of synthesis has uniform alloy structure and graded alloy structure.One pot of heating method has the advantages that operational stability is good, scaling-up is excellent, is more suitable for mass-producing synthesis.But the temperature reaction process characteristic of one pot of heating method synthesis, determines when carrying out alloying reaction to many components with reactive behavior difference, always produces graded alloy structure.The core-shell quanta dots structure of graded alloy is by multiple factors effect, and synthetic product structure poor repeatability, product property is unstable.Uniform alloy structure is the selected objective target of quantum dot alloying synthesis.To Cd
xzn
1-xse quantum dot is due to Cd
2+and Zn
2+reactive behavior difference is comparatively large, and cadmium selenide monomer generating rate is much bigger compared with zinc selenide, only has the high-temperature hot note method by more than 300 DEG C to synthesize and long period high temperature annealing aftertreatment (diffusion) reaches uniform alloy.CdSe
xs
1-xquantum dot is comparatively large due to elemental selenium and elemental sulfur reactive behavior difference, directly reacts with elemental selenium and elemental sulfur and cannot obtain uniform alloy product.With complexing selenium and sulphur such as TOP in current conventional synthetic technology, both activities difference is reduced; Or sulphur and selenium (selenium oxide) are reacted in advance generate selenium sulfide alloy, as sulphur selenium multiple sources, and adopt hot-fluid to note method synthesis.Existing alloying CdSe
xs
1-xand Cd
xzn
1-xthe feature of Se quantum dot synthetic method is: adopt hot note method, have the pyroreaction of phosphine system and more than 300 DEG C.There is following deficiency in existing synthetic method: 1, existing method is difficult to reach uniform alloy in more economical way, and mostly the quantum dot of synthesis is the structure with certain gradient composition; 2, hot note method is by the restriction of heat and mass transfer effect, is difficult to use in mass-producing synthesis; 3, the pyroreaction energy consumption of more than 300 DEG C is high, and it is larger that synthesis controls difficulty; 4, have that phosphine method cost is higher, tool environmental contamination.
Adopt without phosphine system one pot of heating method, at relatively low temperature, such as, lower than 240 DEG C, the CdSe of Reactive Synthesis uniform alloy
xs
1-xquantum dot, is not still successfully developed.
Three, summary of the invention
The present invention aims to provide the synthetic method of a kind of indigo plant to the core-shell quanta dots of green emission, uniform alloy core, and core-shell quanta dots of the present invention is with the Se deposit quantum dot (CdSe of uniform alloy
xs
1-x) be shell for core, with CdS, be abbreviated as CdSe
xs
1-x/ CdS quantum dot, wherein x=0.05-0.60.
CdSe of the present invention
xs
1-xquantum dot and CdSe
xs
1-xthe emission peak wavelength of/CdS quantum dot between 460-530nm, continuously adjustabe; Sub-productive rate>=60% of quantum dot maximum amount.
The blue synthetic method to the core-shell quanta dots of green emission, uniform alloy core of the present invention comprises following process:
1, the synthesis of core quantum dot
At room temperature cadmium source, selenium source, sulphur source, part and synthetic medium are added in reactor, be warming up to 210-230 DEG C of more than insulation reaction 20min under nitrogen or argon, obtain Se deposit quantum dot.
Wherein the ratio of the integral molar quantity of sulphur source (in S) and selenium source, the molar weight in cadmium source and the molar weight of part is (0.85-1): 1:(1-6), in reaction system, cadmium concentration is 0.05-0.20mol/L.The mol ratio in selenium source and sulphur source is x:1-x, wherein x=0.05-0.60.
Described cadmium source is the cadmium salt of the saturated of carbonatoms 14-22 or unsaturated fatty acids.
Described selenium source is selenium powder.
Described sulphur source is diallyl disulphide.
Described part is the saturated or unsaturated fatty acids of the straight chain of carbonatoms 14-22.
Described synthetic medium is alkane or the alkene of boiling point >=240 DEG C.
Temperature rise rate >=15 when being warming up to 210-230 DEG C in step 1 DEG C/min.
2, original position involucrum
When the reaction solution of step 1 is cooled to below 100 DEG C, in reaction solution, add involucrum cadmium source and involucrum sulphur source, be warming up to 190-200 DEG C of insulation more than 20min under nitrogen or argon;
The mol ratio in described involucrum cadmium source and involucrum sulphur source (in S) is 1:(0.85-1), the molar weight in involucrum cadmium source is that step 1 adds the 0.5-1.0 of cadmium source molar weight doubly.
Described involucrum cadmium source is the cadmium salt of the saturated of carbonatoms 14-22 or unsaturated fatty acids.
Described involucrum sulphur source is diallyl disulphide.
Temperature rise rate when being warming up to 190-200 DEG C in step 2 is 5-10 DEG C/min.
3, the isolation and purification of quantum dot
When the reaction solution of step 2 is cooled to below 70 DEG C, by reaction solution impouring dehydrated alcohol, produce quantum dot precipitation, take cyclohexane as solvent, ethanol is non-solvent, with propyl carbinol and acetone for regulating solvent, precipitation, purifying quantum dot, obtain CdSe after drying
xs
1-x/ CdS quantum dot.
The invention provides the CdSe of uniform alloy core
xs
1-xthe synthetic method of/CdS nuclear shell structure quantum point.Quantum dot emission spike length provided by the invention is between 460-530nm, and continuously adjustabe, can meet the performance index requirement of technique of display blueness and green primitive well.
Synthetic method of the present invention is with highly active diallyl disulphide for sulphur source, and selenium powder is selenium source, adopts the Se deposit core quantum dot of one pot of heating method synthesis uniform alloy.By the selenium source in feed change simply and sulphur source ratio, realize the adjustment to core quantum dot composition and emission wavelength.
The present invention adopts in-situ reaction to carry out involucrum to core quantum dot, without the need to carrying out isolation and purification operation to core quantum dot, simplifying schedule of operation, decreasing the consumption of related solvents material.
The invention provides a kind of reliably easy and simple to handle, cost is lower, eco-friendly launches the blue core-shell quanta dots synthetic method to green glow.Present method controllability is good, is suitable for mass-producing preparation, has good Green Chemistry characteristic and economy, have larger value to quantum dot application development.
Four, accompanying drawing explanation
Fig. 1 is the CdSe of the 2-in-1 one-tenth of embodiment
0.3s
0.7uV and the PL figure of/CdS quantum dot.As can be seen from Figure 1, quantum dot UV absorption curve has good fine structure, and PL emission peak peak width at half height is about 33nm.
Fig. 2 is the UV figure of the quantum dot of embodiment 1-3 synthesis.As can be seen from Figure 2, increase with selenium amount in core, the continuous red shift of quantum dot UV absorption peak.
Fig. 3 is the PL figure of the quantum dot of embodiment 1-3 synthesis.As can be seen from Figure 3, increase with selenium amount in core, the continuous red shift of quantum dot PL emission peak.
Fig. 4 is the CdSe that embodiment 3 is synthesized
0.4s
0.6tEM and the HRTEM figure of/CdS quantum dot.As can be seen from Figure 4, quantum dot has good monodispersity.
Fig. 5 is the CdSe that embodiment 3 is synthesized
0.4s
0.6the XRD figure of/CdS quantum dot.As can be seen from Figure 5, quantum dot has cubic structure.
Five, embodiment
Embodiment 1: synthesize CdSe in octadecylene medium
0.2s
0.8/ CdS quantum dot
Cadmium stearate 0.200mmol is added, selenium powder 0.040mmol, diallyl disulphide 0.160mmol (taking S as metering primitive), oleic acid 0.20mmol, octadecylene 9.60 grams in reaction flask.Pass into argon purge 5min under room temperature, then be heated to 210 DEG C with 20 DEG C/min speed, insulation 20min, stops heating; When reacting liquid temperature drops under 100 DEG C, cadmium stearate 0.200mmol and diallyl disulphide 0.180mmol is added in reaction flask, be heated to 195 DEG C with 7 DEG C/min speed, insulation 30min, stops heating, when reacting liquid temperature drops under 70 DEG C, reaction solution is poured in 50mL dehydrated alcohol, quantum dot Precipitation, then be non-solvent with dehydrated alcohol, cyclohexane is solvent, dissolve and precipitate quantum dot three times, after drying, obtaining CdSe
0.2s
0.8/ CdS quantum dot dry powder.
The CdSe that the present embodiment is obtained
0.2s
0.8/ CdS quantum dot emission peak wavelength is 472nm, quantum yield 36%.
Embodiment 2: synthesize CdSe in liquid olefin medium
0.3s
0.7/ CdS quantum dot
Cadmium stearate 0.200mmol is added, selenium powder 0.060mmol, diallyl disulphide 0.140mmol (taking S as metering primitive), oleic acid 0.20mmol, whiteruss 9.60 grams in reaction flask.Pass into argon purge 5min under room temperature, then be heated to 210 DEG C with 20 DEG C/min speed, insulation 20min, stops heating; When reacting liquid temperature drops under 100 DEG C, cadmium stearate 0.200mmol and diallyl disulphide 0.190mmol is added in reaction flask, 195 DEG C are heated to 7 DEG C/min speed, insulation 30min, stop heating, when reacting liquid temperature drops under 70 DEG C, reaction solution is poured in 50mL dehydrated alcohol and acetone mixture (volume ratio 3:1), quantum dot Precipitation, be non-solvent again with dehydrated alcohol, cyclohexane is solvent, dissolve and precipitate quantum dot three times, after drying, obtaining CdSe
0.3s
0.7/ CdS quantum dot dry powder.
The CdSe that the present embodiment is obtained
0.3s
0.7/ CdS quantum dot emission peak wavelength is 493nm, quantum yield 44%.
Embodiment 3: synthesize CdSe in octadecylene medium
0.4s
0.6/ CdS quantum dot
Cadmium stearate 0.200mmol is added, selenium powder 0.080mmol, diallyl disulphide 0.120mmol (taking S as metering primitive), oleic acid 0.20mmol, octadecylene 9.60 grams in reaction flask.Pass into argon purge 5min under room temperature, then be heated to 210 DEG C with 20 DEG C/min speed, insulation 20min, stops heating; When reacting liquid temperature drops under 100 DEG C, cadmium stearate 0.200mmol and diallyl disulphide 0.190mmol is added in reaction flask, be heated to 195 DEG C with 7 DEG C/min speed, insulation 30min, stops heating, when reacting liquid temperature drops under 70 DEG C, reaction solution is poured in 50mL dehydrated alcohol, quantum dot Precipitation, then be non-solvent with dehydrated alcohol, cyclohexane is solvent, dissolve and precipitate quantum dot three times, after drying, obtaining CdSe
0.4s
0.6/ CdS quantum dot dry powder.
The CdSe that the present embodiment is obtained
0.4s
0.6/ CdS quantum dot emission peak wavelength is 521nm, quantum yield 62%.
Claims (8)
1. indigo plant is to a synthetic method for the core-shell quanta dots of green emission, uniform alloy core, comprises the following steps:
1) synthesis of core quantum dot
At room temperature cadmium source, selenium source, sulphur source, part and synthetic medium are added in reactor, be warming up to 210-230 DEG C of more than insulation reaction 20min under nitrogen or argon, obtain Se deposit quantum dot;
2) original position involucrum
Until step 1) reaction solution in reaction solution, add involucrum cadmium source and involucrum sulphur source when being cooled to below 100 DEG C, be warming up to 190-200 DEG C of insulation more than 20min under nitrogen or argon;
3) isolation and purification of quantum dot
Until step 2) reaction solution when being cooled to below 70 DEG C, by reaction solution impouring dehydrated alcohol, produce quantum dot precipitation, take cyclohexane as solvent, ethanol is non-solvent, with propyl carbinol and acetone for regulating solvent, precipitation, purifying quantum dot, obtain CdSe after drying
xs
1-x/ CdS quantum dot, x=0.05-0.60.
2. method according to claim 1, is characterized in that:
Step 1) in the ratio of the integral molar quantity of sulphur source and selenium source, the molar weight in cadmium source and the molar weight of part be (0.85-1): 1:(1-6), in reaction system, cadmium concentration is 0.05-0.20mol/L.
3. method according to claim 1 and 2, is characterized in that:
The mol ratio in selenium source and sulphur source is x:(1-x), wherein x=0.05-0.60.
4. method according to claim 1 and 2, is characterized in that:
Described cadmium source is the cadmium salt of the saturated of carbonatoms 14-22 or unsaturated fatty acids;
Described selenium source is selenium powder;
Described sulphur source is diallyl disulphide;
Described part is the saturated or unsaturated fatty acids of the straight chain of carbonatoms 14-22;
Described synthetic medium is alkane or the alkene of boiling point >=240 DEG C.
5. method according to claim 1, is characterized in that:
Step 1) in temperature rise rate >=15 when being warming up to 210-230 DEG C DEG C/min.
6. method according to claim 1, is characterized in that:
Step 2) in the mol ratio in involucrum cadmium source and involucrum sulphur source be 1:(0.85-1), the molar weight in involucrum cadmium source is step 1) add the 0.5-1.0 of cadmium source molar weight doubly.
7. the method according to claim 1 or 6, is characterized in that:
Described involucrum cadmium source is the cadmium salt of the saturated of carbonatoms 14-22 or unsaturated fatty acids;
Described involucrum sulphur source is diallyl disulphide.
8. method according to claim 1, is characterized in that:
Step 2) in temperature rise rate when being warming up to 190-200 DEG C be 5-10 DEG C/min.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106647037A (en) * | 2017-02-06 | 2017-05-10 | 苏州星烁纳米科技有限公司 | Quantum dots backlight module and liquid crystal display device |
| CN108715762A (en) * | 2017-03-15 | 2018-10-30 | 东亚碳技术股份公司 | The preparation method of quantum dot and the quantum dot thus prepared |
| WO2020224439A1 (en) * | 2019-05-07 | 2020-11-12 | 纳晶科技股份有限公司 | Core-shell quantum dot and preparation method therefor, and quantum dot photoelectric device |
| WO2021196789A1 (en) * | 2020-03-30 | 2021-10-07 | 京东方科技集团股份有限公司 | Quantum dot structure and manufacturing method therefor, and quantum dot light-emitting device |
| US20220064530A1 (en) * | 2016-12-30 | 2022-03-03 | Tcl Technology Group Corporation | Quantum dot composite material, preparation method, and semiconductor device |
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| US20220064530A1 (en) * | 2016-12-30 | 2022-03-03 | Tcl Technology Group Corporation | Quantum dot composite material, preparation method, and semiconductor device |
| US11746293B2 (en) * | 2016-12-30 | 2023-09-05 | Tcl Technology Group Corporation | Quantum dot composite material, preparation method, and semiconductor device |
| CN106647037A (en) * | 2017-02-06 | 2017-05-10 | 苏州星烁纳米科技有限公司 | Quantum dots backlight module and liquid crystal display device |
| CN108715762A (en) * | 2017-03-15 | 2018-10-30 | 东亚碳技术股份公司 | The preparation method of quantum dot and the quantum dot thus prepared |
| WO2020224439A1 (en) * | 2019-05-07 | 2020-11-12 | 纳晶科技股份有限公司 | Core-shell quantum dot and preparation method therefor, and quantum dot photoelectric device |
| WO2021196789A1 (en) * | 2020-03-30 | 2021-10-07 | 京东方科技集团股份有限公司 | Quantum dot structure and manufacturing method therefor, and quantum dot light-emitting device |
| US11795393B2 (en) | 2020-03-30 | 2023-10-24 | Boe Technology Group Co., Ltd. | Quantum dot structure, manufacturing method thereof, and quantum dot light-emitting device |
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