CN109370578A - A kind of preparation method for the perovskite quanta point material that stratified material is compound - Google Patents
A kind of preparation method for the perovskite quanta point material that stratified material is compound Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of perovskite quanta point material that stratified material is compound, step includes: that stratified material is mixed with the mixed solution of Cs saline solution, the mixed solution of the DMF solution of MAX and water, the DMF solution of FAX and water respectively, centrifugation, washing, drying, respectively obtains Cs+Intercalation, MA intercalation, FA intercalation stratified material；Lead halide and/or tin halides are added in the mixed solution of octadecylene, oleic acid, oleyl amine, are vacuumized, heated under nitrogen atmosphere, clarified until solution becomes, precursor solution is made；Cs+ intercalation obtained, MA+ intercalation, FA+ intercalation stratified material is added separately in the mixed solution of octadecylene, oleic acid, oleyl amine, first ultrasound, it vacuumizes again, under nitrogen atmosphere after heat temperature raising under conditions of inert gas and stirring, it is added separately in precursor solution, ice-water bath, is centrifuged, it is washed with n-hexane.Environmental stability of the present invention is good；Can covering visible light range, preparation method is simple.
Description
Technical field
The present invention relates to the production method of perovskite quanta point material, in particular to a kind of perovskite that stratified material is compound
The preparation method of quanta point material.
Background technique
Class halogen perovskite quanta point material have high fluorescence quantum efficiency (up to 90%), wavelength of fluorescence is adjustable and
Entire visible light wave range, line width are covered, one of the research hotspot in semiconductor light emitting field is become, is expected to be applied to a new generation's amount
In son point display and lighting engineering.But class halogen perovskite quanta point material haves the shortcomings that stability is poor, perovskite quantum
Irreversible degradation can occur in light, heat, air for point, and then lead to serious fluorescent quenching, the serious ground resistance of this disadvantage
Its application in practice is hindered.
Summary of the invention
Goal of the invention: it is an object of the present invention to provide a kind of preparation sides of perovskite quanta point material that stratified material is compound
Method, the compound perovskite quanta point material environmental stability are good, it can be achieved that the entirely adjusting in visible-range.
Technical solution: the present invention provides a kind of preparation method of perovskite quanta point material that stratified material is compound, including
Following steps:
(1) stratified material and Cs saline solution are mixed, are centrifuged, washed, drying obtains Cs+The stratiform material of intercalation
Material, referred to as " Cs+Stratified material "；
The mixed solution of stratified material, the DMF solution of MAX and water is stirred, is centrifuged, is washed, drying obtains MA+It inserts
The stratified material of layer, referred to as " MA- stratified material "；
The mixed solution of stratified material, the DMF solution of FAX and water is stirred, is centrifuged, is washed, drying obtains FA+It inserts
The stratified material of layer, referred to as " FA- stratified material "；
(2) lead halide and/or tin halides are added in the mixed solution of octadecylene, oleic acid, oleyl amine, are vacuumized, in nitrogen
Atmosphere encloses lower heating, clarifies until solution becomes, precursor solution is made；
(3) by " Cs made from step (1)+Stratified material ", " MA- stratified material ", " FA- stratified material " are separately added into
To octadecylene, oleic acid, oleyl amine mixed solution in, first ultrasound, then vacuumizes, and is heated to 100-120 DEG C under nitrogen atmosphere, protects
Hold 10~20min, then be increased to 150~180 DEG C, keep 10~20min, inert gas and stirring under conditions of, respectively plus
Into step (2) precursor solution, ice-water bath, centrifugation is washed with n-hexane.
In above-mentioned technical proposal, based on inorganic lamellar material as carrier existing for quantum dot, Cs is allowed first+, MA or FA
Into in inorganic lamellar material, the halide of Pb or Sn are added, generates perovskite quantum dot in inorganic lamellar material interlayer, every
External world's water oxygen absolutely, protects unstable perovskite quantum dot, makes it have preferable environmental stability.
Further, the lead halide of the step (2) is one of lead chloride, lead bromide and lead iodide or a variety of；Halogen
Change tin is one of stannic chloride, stannic bromide and stannic iodide or a variety of.Layered material is kaolin, montmorillonite or lithium soap
Stone.The Cs salt is respectively acetate or carbonate, and MAX is respectively one of MACl, MABr, MAI or a variety of, FAX difference
For one of FACl, FABr, FAI or a variety of.Wherein, molar concentration of the lead halide in octadecene solution is preferably
0.0376~0.04mol/L；The volume ratio of oleic acid and oleyl amine is preferably 1: 1~2: 1.The molar ratio of lead bromide and lead chloride is 0:
3~3: 0；In the mixture of lead bromide and lead iodide, the molar ratio of lead iodide and lead bromide is 0: 3~3: 0.The step (1)
Middle Cs saline solution Cs+Concentration be preferably 0.5mol/L；The amount ratio of stratified material and Cs salt, MA salt or FA salt is respectively 2g
:0.02mol.Intercalation " the Cs of the step (3)+The quality of stratified material " and the volume ratio of octadecylene are preferably 0.5g: 5mL；
Octadecylene, oleic acid, oleyl amine volume ratio be preferably 5: 1: 0.5ml；"Cs+The amount ratio of stratified material " and halide solution is excellent
It is selected as 0.5g: 5~7mL；The reagent of washing is n-hexane.
The utility model has the advantages that this hair has preferable environmental stability；The adjusting of fluorescence spectrum, covering visible light model can be achieved
It encloses, obtains wide color region；Synthesis process of the present invention does not need using any toxic solvent, does not need inert gas guarantor
Shield, preparation method are simple；The present invention can be used for the photoelectric functional materials such as white light LED part field.
Detailed description of the invention
Fig. 1 is the XRD diffracting spectrum of kaolin perovskite quantum dot composite material prepared by embodiment 1；
Fig. 2 is the fluorescent absorption spectrogram of kaolin perovskite quantum dot composite material prepared by embodiment 1；
Fig. 3 is the fluorescence emission spectrogram of compound of kaolin perovskite quantum dot composite material prepared by embodiment 5；
Fig. 4 is the fluorescence emission spectrogram of compound of kaolin perovskite quantum dot composite material prepared by embodiment 6.
Specific embodiment
Embodiment 1:CsPbBr3-K(CsPbBr3Kaolin composite material) composite material preparation method
(1) cesium acetate of 4g 20ml deionized water dissolving is taken, cesium acetate aqueous solution is obtained, the kaolin of 2g is added to
In cesium acetate aqueous solution, 70 DEG C of stirring in water bath 12h (revolving speed of stirring is 400r/min), (revolving speed of centrifugation is 5000r/ for centrifugation
Min) 7min takes lower layer's sample, and deionized water washes twice, and at 80 DEG C after dry 12h, obtaining intercalation has Cs+Height
Ridge soil Cs+Kaolin (Cs+-K)；
(2) by octadecylene (ODE) 5mL, oleic acid (OA) 1mL, oleyl amine (OAm) 1mL, lead bromide (PbBr2)0.0690g
(0.188mmol) is mixed in three-neck flask, and 30min, N are vacuumized after being heated to 120 DEG C2The lower 120 DEG C of stirrings of atmosphere be (stirring
Revolving speed is 200r/min) until solid is completely dissolved, obtain bromide solution；
(3) by 0.25g Cs+- K and 5mL octadecylene (ODE), 1ml oleic acid (OA), 0.5ml oleyl amine (OAm) are mixed in three necks
In flask, first ultrasound 1h, is then heated to 120 DEG C, vacuumizes 30min, N2160 DEG C are warming up under atmosphere, injection step (2)
Bromide solution, stirring 2min (after the revolving speed of stirring is 200r/min), ice-water bath is cooling, centrifugation (revolving speed 5000r/min,
Time is 7min), it takes lower layer's sample that the washing centrifugation of 4mL n-hexane is added and is repeated twice；60 DEG C of vacuum drying 12h, obtain
CsPbBr3- K composite luminescent material.
Embodiment 2:CsPbCl3- K composite material (CsPbCl3Kaolin composite material) preparation method
(1) cesium carbonate of 4g 20ml deionized water dissolving is taken, cesium carbonate aqueous solution is obtained, the kaolin of 2g is added to
In cesium carbonate aqueous solution, 70 DEG C of stirring in water bath 12h (revolving speed of stirring is 400r/min), (revolving speed of centrifugation is 5000r/ for centrifugation
Min) 7min takes lower layer's sample, and deionized water washes twice, and at 80 DEG C after dry 12h, obtaining intercalation has Cs+Height
Ridge soil Cs+Kaolin (Cs+-K)；
(2) by octadecylene (ODE) 5mL, oleic acid (OA) 1mL, oleyl amine (OAm) 1mL, lead chloride (PbCl2) 0.0523g
(0.188mmol) is mixed in three-neck flask, and 30min, N are vacuumized after being heated to 100 DEG C2The lower 120 DEG C of stirrings of atmosphere be (stirring
Revolving speed is 200r/min) until solid is completely dissolved, obtain bromide solution；
(3) by 0.25g Cs+- K and 5mL octadecylene (ODE), 1ml oleic acid (OA), 0.5ml oleyl amine (OAm) are mixed in three necks
In flask, first ultrasound 1h, is then heated to 120 DEG C, vacuumizes 30min, N2160 DEG C are warming up under atmosphere, injection step (2)
Bromide solution, stirring 2min (after the revolving speed of stirring is 200r/min), ice-water bath is cooling, centrifugation (revolving speed 5000r/min,
Time is 7min), it takes lower layer's sample that the washing centrifugation of 4mL n-hexane is added and is repeated twice；60 DEG C of vacuum drying 12h, obtain
CsPbCl3- K composite luminescent material.
Embodiment 3:CsPbCl1.5Br1.5-M(CsPbCl1.5Br1.5Montmorillonite composite material) composite material preparation method
(1) cesium acetate of 4g 20ml deionized water dissolving is taken, cesium acetate aqueous solution is obtained, the montmorillonite of 2g is added to cesium acetate water
In solution, 70 DEG C of stirring in water bath 12h (revolving speed of stirring is 400r/min), centrifugation (revolving speed of centrifugation is 5000r/min) 7min,
Lower layer's sample is taken, deionized water washes twice, and at 80 DEG C after dry 12h, obtaining intercalation has Cs+Kaolin Cs+It covers
De- stone (Cs+-M)；
(2) by octadecylene (ODE) 5mL, oleic acid (OA) 1mL, oleyl amine (OAm) 1mL, lead chloride (PbCl2) 0.0261g
(0.094mmol), lead bromide (PbBr2) 0.0345g (0.094mmol) is mixed in three-neck flask, it is heated to take out at 120 DEG C true
Empty 30min, N2The lower 120 DEG C of stirrings of atmosphere (revolving speed of stirring is 200r/min) obtain halide until solid is completely dissolved
Mixed solution；
(3) by 0.25g Cs+- M and 5mL octadecylene (ODE), lml oleic acid (OA), 0.5ml oleyl amine (OAm) are mixed in three necks
In flask, first ultrasound lh, is then heated to 120 DEG C, vacuumizes 30min, N2150 DEG C are warming up under atmosphere, injection step (2)
Halide mixed solution, (after the revolving speed of stirring is 200r/min), ice-water bath is cooling, is centrifuged (revolving speed 5000r/ by stirring 2min
Min, time 7min), it takes lower layer's sample that the washing centrifugation of 4mL n-hexane is added and is repeated twice；60 DEG C of vacuum drying 12h, obtain
CsPbCl1.5Br1.5- M composite luminescent material.
Embodiment 4:CsPbBr1.5I1.5- L composite material (CsPbBr1.5I1.5Lithium soap stone composite material) preparation method
(1) cesium acetate of 4g 20ml deionized water dissolving is taken, cesium acetate aqueous solution is obtained, the hectorite of 2g is added to
In cesium acetate aqueous solution, 70 DEG C of stirring in water bath 12h (revolving speed of stirring is 400r/min), (revolving speed of centrifugation is 5000r/ for centrifugation
Min) 7min takes lower layer's sample, and deionized water washes twice, and at 80 DEG C after dry 12h, obtaining intercalation has Cs+Height
Ridge soil Cs+Hectorite (Cs+-L)；
(2) by octadecylene (ODE) 5mL, oleic acid (OA) 1mL, oleyl amine (OAm) 1mL, lead bromide (PbBr2)0.0345g
(0.094mmol), lead iodide (PbI2) 0.0433g (0.094mmol) is mixed in three-neck flask, it is heated to take out at 120 DEG C true
Empty 30min, N2The lower 120 DEG C of stirrings of atmosphere (revolving speed of stirring is 200r/min) obtain halide until solid is completely dissolved
Mixed solution；
(3) by 0.25g Cs+- L and 5mL octadecylene (ODE), 1ml oleic acid (OA), 0.5ml oleyl amine (OAm) are mixed in three necks
In flask, first ultrasound 1h, is then heated to 120 DEG C, vacuumizes 30min, N2180 DEG C are warming up under atmosphere, injection step (2)
Halide mixed solution, (after the revolving speed of stirring is 200r/min), ice-water bath is cooling, is centrifuged (revolving speed 5000r/ by stirring 2min
Min, time 7min), it takes lower layer's sample that the washing centrifugation of 4mL n-hexane is added and is repeated twice；60 DEG C of vacuum drying 12h, obtain
CsPbBr1.5I1.5- L composite luminescent material.
Embodiment 5:CsPbI3- K composite material (CsPbI3Kaolin composite material) preparation method
(1) cesium acetate of 4g 20ml deionized water dissolving is taken, cesium acetate aqueous solution is obtained, the kaolin of 2g is added to
In cesium acetate aqueous solution, 70 DEG C of stirring in water bath 12h (revolving speed of stirring is 400r/min), (revolving speed of centrifugation is 5000r/ for centrifugation
Min) 7min takes lower layer's sample, and deionized water washes twice, and at 80 DEG C after dry 12h, obtaining intercalation has Cs+Height
Ridge soil Cs+Kaolin (Cs+-K)；
(2) by octadecylene (ODE) 5mL, oleic acid (OA) 1mL, oleyl amine (OAm) 1mL, lead iodide (PbI2)0.0867g
(0.188mmol) is mixed in three-neck flask, is heated to vacuumize 30min, N at 120 DEG C2The lower 120 DEG C of stirrings of atmosphere be (stirring
Revolving speed is 200r/min) until solid is completely dissolved, obtain iodide solution；
(3) by 0.25g Cs+- K and 5mL octadecylene (ODE), 1ml oleic acid (OA), 0.5ml oleyl amine (OAm) are mixed in three necks
In flask, first ultrasound 1h, is then heated to 120 DEG C, vacuumizes 30min, N2160 DEG C are warming up under atmosphere, injection step (2)
Iodide solution, stirring 2min (after the revolving speed of stirring is 200r/min), ice-water bath is cooling, centrifugation (revolving speed 5000r/min,
Time is 7min), it takes lower layer's sample that the washing centrifugation of 4mL n-hexane is added and is repeated twice；60 DEG C of vacuum drying 12h, obtain
CsPbI3- K composite luminescent material.
Embodiment 6: CsPbBr is synthesized with precipitation at room temperature method3- K composite material (CsPbBr3Kaolin composite material) system
Preparation Method
(1) lead bromide (PbBr is weighed2) 0.0587g (0.16mmol), cesium bromide (CsBr) 0.0340g (0.16mmol) be molten
200 μ l oleic acid are added in 2mlDMF or DMSO in solution, and 100 μ l oleyl amines form precursor solution；
(2) kaolin powder of 0.1g is dispersed in the organic solvents such as 5ml toluene or n-hexane, carries out 1~2h of ultrasound；
(3) 500 μ l precursor solutions are taken, instills be dispersed in kaolinic toluene or n-hexane with vigorous stirring, 2000
~5000rpm centrifugation, 60 DEG C of vacuum drying 12h obtain CsPbBr3- K composite luminescent material.
Embodiment 7: FAPbBr is synthesized with precipitation at room temperature method3M composite (FAPbBr3Montmorillonite composite material) system
Preparation Method
(1) carbonamidine bromine (FABr) 0.0200g (0.16mmol), lead bromide (PbBr are weighed2) 0.0587g (0.16mmol) is molten
200 μ l oleic acid are added in 2ml DMF or DMSO in solution, and 100 μ l oleyl amines form precursor solution；
(2) the montmorillonite powder of 0.1g is dispersed in the organic solvents such as 5ml toluene or n-hexane, carries out 1~2h of ultrasound；
(3) 500 μ l precursor solutions are taken, instills be dispersed in kaolinic toluene or n-hexane with vigorous stirring, 2000
~5000rpm centrifugation, 60 DEG C of vacuum drying 12h obtain FAPbBr3- M composite luminescent material.
Embodiment 8:MAPbBr3- K composite material (MAPbBr3Kaolin composite material) preparation method
(1) take the methylamine bromine (MABr) of 2g with 2ml DMF dissolve, then plus 20ml water, the kaolin of 2g is added to mixing
In solution, 70 DEG C of stirring in water bath 12h (revolving speed of stirring is 400r/min), centrifugation (revolving speed of centrifugation is 5000r/min) 7min,
Lower layer's sample is taken, deionized water washes twice, and obtains the kaolin MA- kaolinite that intercalation has MA after dry 12h at 80 DEG C
Native (MA-K)；
(2) by octadecylene (ODE) 5mL, oleic acid (OA) 1mL, oleyl amine (OAm) 1mL, lead bromide (PbBr2)0.0690g
(0.188mmol) is mixed in three-neck flask, and 30min, N are vacuumized after being heated to 120 DEG C2The lower 120 DEG C of stirrings of atmosphere be (stirring
Revolving speed is 200r/min) until solid is completely dissolved, obtain bromide solution；
(3) by 0.25g MA+- K and 5mL octadecylene (ODE), 1ml oleic acid (OA), 0.5ml oleyl amine (OAm) are mixed in three necks
In flask, first ultrasound 1h, is then heated to 120 DEG C, vacuumizes 30min, N2160 DEG C are warming up under atmosphere, injection step (2)
Iodide solution, stirring 2min (after the revolving speed of stirring is 200r/min), ice-water bath is cooling, centrifugation (revolving speed 5000r/min,
Time is 7min), it takes lower layer's sample that the washing centrifugation of 4mL n-hexane is added and is repeated twice；60 DEG C of vacuum drying 12h, obtain
MAPbBr3- K composite luminescent material.
Embodiment 9:CsSnBr3- K composite material (CsSnBr3Kaolin composite material) preparation method
(1) cesium acetate of 4g 20ml deionized water dissolving is taken, cesium acetate aqueous solution is obtained, the kaolin of 2g is added to
In cesium acetate aqueous solution, 70 DEG C of stirring in water bath 12h (revolving speed of stirring is 400r/min), (revolving speed of centrifugation is 5000r/ for centrifugation
Min) 7min takes lower layer's sample, and deionized water washes twice, and at 80 DEG C after dry 12h, obtaining intercalation has Cs+Height
Ridge soil Cs+Kaolin (Cs+-K)；
(2) by octadecylene (ODE) 5mL, oleic acid (OA) 1mL, oleyl amine (OAm) 1mL, stannous bromide (SnBr2)0.0524g
(0.188mmol) is mixed in three-neck flask, and 30min, N are vacuumized after being heated to 120 DEG C2The lower 120 DEG C of stirrings of atmosphere be (stirring
Revolving speed is 200r/min) until solid is completely dissolved, obtain bromide solution；
(3) by 0.25g Cs+- K and 5mL octadecylene (ODE), 1ml oleic acid (OA), 0.5ml oleyl amine (OAm) are mixed in three necks
In flask, first ultrasound 1h, is then heated to 120 DEG C, vacuumizes 30min, N2160 DEG C are warming up under atmosphere, injection step (2)
Bromide solution, stirring 2min (after the revolving speed of stirring is 200r/min), ice-water bath is cooling, centrifugation (revolving speed 5000r/min,
Time is 7min), it takes lower layer's sample that the washing centrifugation of 4mL n-hexane is added and is repeated twice；60 DEG C of vacuum drying 12h, obtain
CsSnBr3- K composite luminescent material.
Claims (5)
1. a kind of preparation method for the perovskite quanta point material that stratified material is compound, characterized by the following steps:
(1) stratified material and Cs saline solution are mixed, are centrifuged, washed, drying obtains Cs+The stratified material of intercalation；
The mixed solution of stratified material, the DMF solution of MAX and water is stirred, is centrifuged, is washed, drying obtains the layer of MA intercalation
Shape material；
The mixed solution of stratified material, the DMF solution of FAX and water is stirred, is centrifuged, is washed, drying obtains the layer of FA intercalation
Shape material；
(2) lead halide and/or tin halides are added in the mixed solution of octadecylene, oleic acid, oleyl amine, are vacuumized, in nitrogen atmosphere
Lower heating is enclosed, is clarified until solution becomes, precursor solution is made；
(3) by Cs made from step (1)+The stratified material difference of the stratified material of intercalation, the stratified material of MA intercalation, FA intercalation
It is added in the mixed solution of octadecylene, oleic acid, oleyl amine, first ultrasound, then vacuumizes, be heated to 100-120 under nitrogen atmosphere
DEG C, 10~20min is kept, then be increased to 150~180 DEG C, keeps 10~20min, under conditions of inert gas and stirring, point
It is not added in step (2) precursor solution, ice-water bath, is centrifuged, is washed with n-hexane.
2. the preparation method of the compound perovskite quanta point material of stratified material according to claim 1, it is characterised in that:
The lead halide of the step (2) is one of lead chloride, lead bromide and lead iodide or a variety of.
3. the preparation method of the compound perovskite quanta point material of stratified material according to claim 1, it is characterised in that:
The tin halides of the step (2) are one of stannic chloride, stannic bromide and stannic iodide or a variety of.
4. the preparation method of the compound perovskite quanta point material of stratified material according to claim 1, it is characterised in that:
Layered material is kaolin, montmorillonite or hectorite.
5. the preparation method of the compound perovskite quanta point material of stratified material according to claim 1, it is characterised in that:
The Cs salt is respectively acetate or carbonate, and MAX is respectively one of MACl, MABr, MAI or a variety of, and FAX is respectively
One of FACl, FABr, FAI or a variety of.
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| CN110317607A (en) * | 2019-06-04 | 2019-10-11 | 华南理工大学 | A kind of perovskite quantum dot and low-dimensional-oxide composite luminescent material and preparation and application |
| CN110938432A (en) * | 2019-12-17 | 2020-03-31 | 南京邮电大学 | Preparation method of perovskite quantum dot material |
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| CN108841387A (en) * | 2018-07-18 | 2018-11-20 | 深圳扑浪创新科技有限公司 | A kind of quantum nanoparticles crystalline substance compound and preparation method thereof |
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| SUN, JIA-YI;等: "Facile Two-Step Synthesis of All-Inorganic Perovskite CsPbX3 (X = Cl, Br, and I) Zeolite-Y Composite Phosphors for Potential Backlight Display Application", 《ADVANCED FUNCTIONAL MATERIALS》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110317607A (en) * | 2019-06-04 | 2019-10-11 | 华南理工大学 | A kind of perovskite quantum dot and low-dimensional-oxide composite luminescent material and preparation and application |
| CN110317607B (en) * | 2019-06-04 | 2021-05-14 | 华南理工大学 | Perovskite quantum dot and low-dimensional oxide composite luminescent material and preparation and application thereof |
| CN110938432A (en) * | 2019-12-17 | 2020-03-31 | 南京邮电大学 | Preparation method of perovskite quantum dot material |
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