CN109679645A - A kind of preparation method of high stability perovskite quantum dot - Google Patents
A kind of preparation method of high stability perovskite quantum dot Download PDFInfo
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Abstract
The present invention provides a kind of high stability, the synthetic method of high-quantum efficiency perovskite quantum dot.Perovskite quanta point material of the invention, it is by the suction-operated between montmorillonite and cation, react perovskite quantum dot between montmorillonite layer, it is separated between perovskite nanoparticle by lamellar structure, it can be effectively reduced the ion free exchange between perovskite quantum dot, lamellar structure plays the role of high prevention steam and oxygen simultaneously, greatly improves the stability of quantum dot.Specific steps are as follows: a. mixes CsX with water and ethyl alcohol, is sufficiently stirred until being completely dissolved；B. sheet montmorillonite is added in the solution of step a, Cs+ cation is attracted between montmorillonite layer；After the reaction was completed, centrifuge washing 3 times, are scattered in octadecylene after vacuum drying；C. lead source, organic long-chain acid, organic long-chain amine and solvent are mixed, form transparency liquid；D. the dispersion liquid in step b is injected into rapidly in the transparency liquid of step c.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, in particular to a kind of preparation side of perovskite quantum dot
Method.
Background technique
Quantum dot is the semiconductor nano with several nano-scales, and when the stimulation by light or electricity, quantum dot will
The light of certain wavelength is issued, launch wavelength is determined by the composition material and size shape of quantum dot.Relative to organic material, quantum
Point can provide outstanding excitation purity and thermal stability.These characteristics make quantum dot in illumination, display, solar energy and biology mark
The fields such as note have potential application and cause the extensive concern of people.
Nano-perovskite quantum dot possesses huge application potential in terms of photoelectric device.Nano-perovskite quantum dot has
By changing ingredient or size the accuracy controlling of emission wavelength may be implemented, tuning range can be light in very high luminous efficiency
It changes places and covers entire visible light region.Nano-perovskite quantum dot has very narrow 12 ~ 40 nm of the spectral line of emission, by perovskite
The LED colour gamut being prepared is up to 140%, considerably beyond commercialized Organic Light Emitting Diode.Just because of these
Charming characteristic so that nano-perovskite quantum dot shows huge application value in terms of next-generation display.
Although nano-perovskite quantum dot shows superior in terms of display, commercialization is realized, there are still very much
Problem.Different degrees of degradation occurs in light, heat, oxygen for nano-perovskite quantum dot, leads to serious fluorescent quenching, into
And lead to the reduction of device photoelectric transfer efficiency.
Summary of the invention
In view of the problems of the prior art, the present invention provides a kind of high stability, high-quantum efficiency perovskite
The synthetic method of quantum dot.The invention adopts the following technical scheme:
A. CsX is mixed with water and ethyl alcohol, is sufficiently stirred until being completely dissolved；
B. sheet montmorillonite is added in above-mentioned solution, moistens expansion, at 0-100 degrees Celsius, stirred 1-24 hours, Cs+ sun from
Son is attracted between montmorillonite layer；After the reaction was completed, centrifuge washing 3 times, are scattered in octadecylene after vacuum drying；
C. lead source, organic long-chain acid, organic long-chain amine and solvent are mixed, are heated to 50-250 degrees Celsius, are formed transparent
Liquid；
D. dispersion liquid in step b is injected into rapidly in the transparency liquid of step c, is reacted 1-60 minutes.
CsX in the step a is CsCl, CsBr, one or more of CsI.
The ratio of water and ethyl alcohol in the step a is arbitrary proportion.
The concentration of CsX in the step a is 0.01mol/L to 1mol/L.
Montmorillonite in the step b is laminated structure, piece thickness 1-100nm, length 10-1000nm, and montmorillonite can be with
Be it is natural, be also possible to artificial synthesized.
Montmorillonite in the step b can be unmodified, be also possible to modified.Wherein modified montmorillonoid includes K
+, Ca2+, Na+, Mg2+, Al3+, Mn2+, Zn2+, Fe3+, Co2+, Ni2+, Sn2+, Pb2+, Ag+, Cu2+ plasma modification one
Kind is several.It is furthermore preferred that metal ion and montmorillonite Inter layer adsorption be weaker than Cs+ ion and montmorillonite Inter layer adsorption from
Son, including be not limited to K+, Na+, Mg2+, Ca2+, Al3+ etc..
Preferably, CsX and the weight ratio of montmorillonite are 1:0.1-1:10；
Lead source in the step c is one or more of lead chloride, lead bromide, lead iodide.
The alkane or olefines that organic long-chain acid and organic long-chain amine in the step c are main chain containing 8-20 carbon are organic
Acid and organic amine cannot play the role of ligand lower than 8 since carbochain is shorter, and it is poor that carbochain is greater than 20 dissolubilities.
Beneficial effects of the present invention
By the suction-operated of montmorillonite layer and Cs+ cation, perovskite quantum dot is reacted between montmorillonite layer,
Perovskite nanoparticle montmorillonite is fixed and is separated by lamella, and the ion that can be effectively reduced between perovskite quantum dot is freely handed over
It changes, while lamellar structure plays the role of high prevention steam and oxygen, the resistance to water oxygen of quantum dot will be greatly improved, improve and stablize
Property.
Detailed description of the invention
Fig. 1 is synthesis step schematic diagram of the invention；
Fig. 2 is the perovskite quantum dot membrane structure figure of the embodiment of the present invention 11；
Fig. 3 is the high temperature and humidity stability diagram of the embodiment of the present invention 12；
Fig. 4 is the blue light stable figure of the embodiment of the present invention 13.
Specific embodiment
The present invention is described in more detail below with reference to accompanying drawings, which show the preferred embodiment of the present invention,
It should be understood that those skilled in the art can modify invention described herein and still realize advantageous effects of the invention.Cause
This, following description should be understood as the widely known of those skilled in the art, and be not intended as limitation of the present invention.
Embodiment 1
2.12g CsBr is taken to be dissolved in 1L water and alcohol mixed solution (volume ratio 1:1), mechanical stirring 1 hour, until completely molten
Solution.Form the A1 solution that concentration is 0.01mol/L.
Embodiment 2
168g CsCl is taken to be dissolved in 1L water, mechanical stirring 2 hours, until being completely dissolved.Formation precursor concentration is 1mol/L
A2 solution.
Embodiment 3
0.259g CsI is taken to be dissolved in 1L ethanol solution, mechanical stirring 3 hours, until being completely dissolved.Forming precursor concentration is
The A3 solution of 0.001mol/L.
The preparation of 4 Cs-M presoma of embodiment
1g sodium-based montmorillonite is weighed, is added in 1 precursor A 1 of embodiment, is stirred, 60 degrees Celsius is heated to and flows back 18 hours, make
Cs ion is sufficiently exchanged with Na ion.Suspended matter centrifugation after reaction is rinsed, centrifugation three times repeatedly, most with deionized water
It is dispersed in 20ml octadecylene after being dried in vacuo afterwards, forms solution C 1.
The preparation of 5 Cs-M presoma of embodiment
1g sodium-based montmorillonite is weighed, is added in 2 precursor A 2 of embodiment, is stirred, 100 degrees Celsius is heated to and flows back 1 hour, make
Cs ion is sufficiently exchanged with Na ion.Suspended matter centrifugation after reaction is rinsed, centrifugation three times repeatedly, most with deionized water
It is dispersed in 20ml octadecylene after being dried in vacuo afterwards, forms solution C 2.
The preparation of 6 Cs-M presoma of embodiment
3g calcium-base montmorillonite is weighed, is added in 3 precursor A 3 of embodiment, is stirred, 0 degree Celsius is stirred 24 hours, and Cs ion is made
It is sufficiently exchanged with Na ion.Suspended matter centrifugation after reaction is rinsed, centrifugation three times repeatedly, last vacuum with deionized water
It is dispersed in after drying in 20ml octadecylene, forms solution C 3.
The preparation of 7 Cs-M presoma of embodiment
The fluorine-containing montmorillonite of the artificial synthesized magnesium-based of 2g is weighed, is added in 1 precursor A 1 of embodiment, stirs, is heated to 80 degrees Celsius
Reflux 12 hours, exchanges Cs ion sufficiently with Na ion.Suspended matter centrifugation after reaction, with deionized water rinse, from
It the heart three times repeatedly, is dispersed in 30ml octadecylene after being finally dried in vacuo, forms solution C 4.
The green perovskite quantum dot Cs-M method synthesis of embodiment 8
50ml octadecylene, 5ml oleic acid, 5ml oleyl amine, 0.14g lead bromide are weighed in the there-necked flask of 250ml, mechanical stirring, heating
It to after 100 DEG C, vacuumizes, removes the moisture in solution.170 degrees Celsius are continuously heating to, until solid is all molten in three empty bottles
Solution injects rapidly C1 solution 20ml, stops heating after reacting 3min, rapid ice bath is cooling.
Test: wavelength 521nm, half-peak breadth 19nm, quantum dot yield QY are 85%.
The red perovskite quantum dot Cs-M method synthesis of embodiment 9
80ml octadecylene, 4ml oleic acid, 6ml oleyl amine, 0.16g lead iodide are weighed in the there-necked flask of 250ml, mechanical stirring, heating
It to after 120 DEG C, vacuumizes, removes the moisture in solution.150 degrees Celsius are continuously heating to, until solid is all molten in three empty bottles
Solution injects rapidly C4 solution 20ml, stops heating after reacting 2min, rapid ice bath is cooling.
Test: wavelength 631nm, half-peak breadth 30nm, quantum dot yield QY are 80%.
The green perovskite quantum dot conventional method synthesis of embodiment 10
30ml octadecylene, 1ml oleic acid, 1ml oleyl amine, 0.07g lead iodide are weighed in the there-necked flask of 250ml, mechanical stirring, heating
It to after 100 DEG C, vacuumizes, removes the moisture in solution.120 degrees Celsius are continuously heating to, until solid is all molten in three empty bottles
Solution injects rapidly C2 solution 5ml, stops heating after reacting 20s, rapid ice bath is cooling.
Test: wavelength 518nm, half-peak breadth 19nm, quantum dot yield QY are 83%.
The preparation of 11 perovskite quantum dot film of embodiment
It is coated and cured at sandwich knot by 0.3% mass concentration in green perovskite quantum dot dissolution in acrylic Acid UV resin
The quantum dot film of structure, wherein quantum point protection is obstructed at two in the PET barrier film that grade is 10-1, as shown in Fig. 2, 1,3 are
PET barrier film, 2 be quantum dot resin layer.
12 perovskite quantum dot film high-temp. stability test of embodiment
Quantum dot film prepared by embodiment 11, is placed on 65 DEG C, in the hot and humid environment of 95%RH, tests at regular intervals
The brightness of quantum dot film.Such as Fig. 3, it will be apparent that the perovskite quantum dot high temperature and humidity stability of Cs-M method preparation is than conventional side
The perovskite quantum dot of method preparation is more stable.
The test of 13 perovskite quantum dot film blue light stable of embodiment
Quantum dot film prepared by embodiment 11, is placed on 3mW/cm2, in 447nm blue light illumination environment, tests at regular intervals
The brightness of quantum dot film.Such as Fig. 4, it will be apparent that the perovskite quantum dot blue light stable of Cs-M method preparation is than conventional method system
Standby perovskite quantum dot is more stable.
Of the invention is described in detail above by embodiment, but the content is only preferable implementation of the invention
Example, should not be considered as limiting the scope of the invention.It is all according to all the changes and improvements made by the present patent application range
Deng should still be within the scope of the patent of the present invention.
Claims (10)
1. a kind of preparation method of high stability perovskite quantum dot, it is characterised in that include the following steps:
A. CsX is mixed with water and ethyl alcohol, is sufficiently stirred until being completely dissolved；
B. sheet montmorillonite is added in the solution of step a, moistens expansion；It at 0-100 degrees Celsius, stirs 1-24 hours, Cs+ sun
Ion is attracted between montmorillonite layer；After the reaction was completed, centrifuge washing 3 times, are scattered in octadecylene after vacuum drying；
C. lead source, organic long-chain acid, organic long-chain amine and solvent are mixed, are heated to 50-250 degrees Celsius, are formed transparent
Liquid；
D. the dispersion liquid in step b is injected into rapidly in the transparency liquid of step c, is reacted 1-60 minutes.
2. a kind of preparation method of high stability perovskite quantum dot as described in claim 1, it is characterised in that CsX in step a
For CsCl, CsBr, one or more of CsI.
3. a kind of preparation method of high stability perovskite quantum dot as described in claim 1, it is characterised in that in step a water and
The ratio of ethyl alcohol is arbitrary proportion.
4. a kind of preparation method of high stability perovskite quantum dot as described in claim 1, it is characterised in that CsX in step a
Concentration be 0.001mol/L to 1mol/L.
5. a kind of preparation method of high stability perovskite quantum dot as described in claim 1, it is characterised in that covered in step b de-
Soil is laminated structure, piece thickness 1-100nm, length 10-1000nm.
6. a kind of preparation method of high stability perovskite quantum dot as described in claim 1, it is characterised in that covered in step b de-
Soil can be unmodified, be also possible to modified；Wherein modified montmorillonoid include K+, Ca2+, Na+, Mg2+, Al3+, Mn2+,
Zn2+, Fe3+, Co2+, Ni2+, Sn2+, Pb2+, Ag+, Cu2+ ion modification are one or several kinds of.
7. a kind of preparation method of high stability perovskite quantum dot as claimed in claim 6, it is characterised in that metal ion with
Montmorillonite Inter layer adsorption is weaker than the ion of Cs+ ion Yu montmorillonite Inter layer adsorption, including be not limited to K+, Na+, Mg2+, Ca2+,
Al3+。
8. a kind of preparation method of high stability perovskite quantum dot as described in claim 1, it is characterised in that in step a and b
CsX and the weight ratio of montmorillonite are 1:0.1-1:10.
9. a kind of preparation method of high stability perovskite quantum dot as described in claim 1, it is characterised in that lead source in step c
For one or more of lead chloride, lead bromide, lead iodide.
10. a kind of preparation method of high stability perovskite quantum dot as described in claim 1, it is characterised in that have in step c
The alkane or olefines organic acid and organic amine that machine long chain acid and organic long-chain amine are main chain containing 8-20 carbon.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11807787B2 (en) | 2021-12-28 | 2023-11-07 | Industrial Technology Research Institute | Luminescence conversion material and fabrication method thereof |
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| CN105885846A (en) * | 2015-01-20 | 2016-08-24 | 北京化工大学 | Method for preparing CdTe quantum dot/layered material composite fluorescent powder |
| CN107129804A (en) * | 2017-06-22 | 2017-09-05 | 喻彦林 | A kind of preparation method of the carbon quantum dot montmorillonite-based nano composite powder shown for latent |
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- 2018-12-23 CN CN201811576833.7A patent/CN109679645A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105885846A (en) * | 2015-01-20 | 2016-08-24 | 北京化工大学 | Method for preparing CdTe quantum dot/layered material composite fluorescent powder |
| CN107129804A (en) * | 2017-06-22 | 2017-09-05 | 喻彦林 | A kind of preparation method of the carbon quantum dot montmorillonite-based nano composite powder shown for latent |
Non-Patent Citations (1)
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| JIA-YI SUN ET AL.: ""Facile Two-Step Synthesis of All-Inorganic Perovskite CsPbX3 (X = Cl, Br, and I) Zeolite-Y Composite Phosphors for Potential Backlight Display Application"", 《ADV. FUNCT. MATER.》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11807787B2 (en) | 2021-12-28 | 2023-11-07 | Industrial Technology Research Institute | Luminescence conversion material and fabrication method thereof |
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