CN108359457A - A kind of room temperature synthetic method of ultrapure inorganic halogen perovskite blue light nanometer sheet - Google Patents
A kind of room temperature synthetic method of ultrapure inorganic halogen perovskite blue light nanometer sheet Download PDFInfo
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Abstract
The present invention provides a kind of room temperature synthetic methods of ultrapure inorganic halogen perovskite blue light nanometer sheet, include the following steps：Step 1：Configure oleyl amine：Oleic acid：The mixed liquor of toluene；Step 2：The presoma that lead bromide is first added in the mixed liquor of end is reacted into above-mentioned steps 1, after stirring evenly, adds the presoma of cesium bromide；The presoma of lead bromide is using dimethyl sulfoxide (DMSO) as solvent；The presoma of cesium bromide is using the hydrobromic acid solution of 40% weight ratio as solvent；Step 3：It is reacted into above-mentioned steps 2 after injecting butanol solution reaction fully in the mixed liquor of end, supernatant is collected by centrifugation；Step 4：It will again be centrifuged after supernatant microwave heating, the bottom sediment after centrifugation be scattered in toluene solution.Method provided by the invention is easy to operate efficiently, and the inorganic halogen perovskite blue light nanometer sheet luminescent properties of preparation are excellent, effectively compensate for the low unstable short slab of inorganic halogen perovskite blue light nanometer material luminous efficiency in the prior art.
Description
Technical field
The invention belongs to photoelectron material preparation fields, and in particular to a kind of ultrapure inorganic halogen perovskite blue light nanometer sheet
Room temperature synthetic method.
Background technology
Blue light significantly limits blue light and white light LEDs as the wave band lagged the most is developed in display and lighting area
Application, and short wavelength's blue light (400-450 nanometers) injures human eye retina very big, endangers eyeground health, induces eyes
Disease, therefore, developing efficient long wavelength's blue-ray LED material has important science and practical application meaning.
Ca-Ti ore type quantum dot or nano particle, such as Ca-Ti ore type Organic leadP halogen compound or full-inorganic Ca-Ti ore type lead
The advantages such as halide, since its synthesis cost is low, fluorescence efficiency is high, and luminous half-peak width and energy gap are adjustable, thus
There is potential application value in the fields such as solar cell, laser, optical detector, light emitting diode.
However the nanocrystalline luminous efficiency of perovskite blue light is low, and be mostly sky blue (475 nanometers -500 nanometers) or indigo plant
Purple (400 nanometers -450 nanometers), halfwidth are more than 20 nanometers, and chromatography is impure, and quantum yield is less than 60%, and in atmospheric environment
Under it is highly unstable, only have 2.6% based on the nanocrystalline LED component peak efficiency of perovskite blue light, it is green well below perovskite
Light, red light quantum point LED constrain the practical application space of perovskite material.
Invention content
Technical problem：In order to solve the defects of prior art, the present invention provides a kind of ultrapure inorganic halogen perovskite is blue
The room temperature synthetic method of light nanometer sheet.
Technical solution：The room temperature synthetic method of ultrapure inorganic halogen perovskite blue light nanometer sheet provided by the invention, including
Following steps：
Step 1：Configure oleyl amine：Oleic acid：Volume of toluene ratio is 1：1：10 mixed liquor, and stirred with the speed of 1000r/min
It mixes uniformly；
Step 2：The presoma that lead bromide is first added in the mixed liquor of end is reacted into above-mentioned steps 1, with 1000r/min
Rotating speed stir 1 minute after, add the presoma of cesium bromide, react 0.6-2 minutes；The presoma of the lead bromide is with diformazan
Base sulfoxide is solvent, a concentration of 0.125-0.8 moles every liter of lead bromide；The presoma of the cesium bromide is with the hydrogen of 40% weight ratio
Bromic acid solution is solvent, and cesium bromide or cesium carbonate solubility are 0.5-1.2 moles every liter；
Step 3：It is reacted into above-mentioned steps 2 and injects 0.25-3 milliliters of butanol solution reactions in the mixed liquor of end fully,
Supernatant is collected after being centrifuged 1-5 minutes with the speed of 8000-12000r/min；
Step 4：It is centrifuged again after the supernatant of above-mentioned collection is placed in 100-300W microwave heatings 0.5-5 minutes, it will be from
Bottom sediment after the heart is dissolved to obtain finished product with toluene solution.
As a kind of prioritization scheme：Mixing time is 1min in step 1.
As advanced optimizing scheme：After butanol solution being injected in step 3, reaction time 1min.
As advanced optimizing scheme：The bottom sediment after centrifugation used containing polymethyl methacrylate in step 4 or
The toluene solution of person's polystyrene dissolves.
As advanced optimizing scheme：After the bottom sediment after centrifugation is dissolved with toluene solution in step 4, then with
The rotating speed of 6000-10000r/min centrifuges 1-10 minutes, collects supernatant and obtains finished product.
Advantageous effect：Method provided by the invention is easy to operate efficiently, the inorganic halogen perovskite blue light nanometer sheet of preparation
Luminescent properties are excellent, and building-up process is completed at room temperature, are not necessarily to inert gas shielding, effectively compensate for inorganic in the prior art
The low unstable short slab of halogen perovskite blue light nanometer material luminous efficiency.
Description of the drawings
Fig. 1 is the nanometer sheet PL schematic diagrames that embodiment 1-3 is obtained；
Fig. 2 is the PL pictorial diagrams of the nanometer sheet solution that the method for the present invention obtains and film under the excitation of 365nm ultraviolet lamps；
Fig. 3 is PL schematic diagram of the obtained film of the method for the present invention under the excitation of 365nm ultraviolet lamps；
Fig. 4 is obtained nanometer sheet PL schematic diagrames after different microwave time-triggered protocols.
Specific implementation mode
In the following with reference to the drawings and specific embodiments, the present invention is furture elucidated, it should be understood that these embodiments are merely to illustrate
It the present invention rather than limits the scope of the invention, after having read the present invention, those skilled in the art are to of the invention each
The modification of kind equivalent form falls within the application range as defined in the appended claims.
Embodiment 1
It weighs 367 milligrams of lead bromides to be dissolved in 2 milliliters of dimethyl sulfoxide (DMSO)s (DMSO), configures the presoma of lead bromide, claim
Take 212 milligrams of cesium bromides be dissolved in 1 milliliter of 40% weight by weight than hydrobromic acid solution in, configure the presoma of cesium bromide.
It measures 5 milliliters of toluene, 0.5 milliliter of oleyl amine, 0.5 milliliter of oleic acid and is stirred 1 minute at 1000r/min.By 100 microlitres of lead bromides
Presoma inject in above-mentioned toluene solution, the presoma of 100 microlitres of cesium bromides is injected after 1 minute, again by 0.5 after 1 minute
Milliliter butanol injection.Reaction centrifuged solution 1 minute in 8000r/min after one minute, collected clear liquid.The perovskite blue light of preparation
Nanometer sheet emission wavelength is 461 nanometers, and halfwidth is 14 nanometers.
Embodiment 2
It weighs 367 milligrams of lead bromides to be dissolved in 2 milliliters of dimethyl sulfoxide (DMSO)s (DMSO), configures the presoma of lead bromide, claim
It takes 212 milligrams of cesium bromides to be dissolved in the hydrobromic acid solution of 1 milliliter of 40% weight ratio, configures the presoma of cesium bromide.Measure 5 millis
It rises toluene, 0.5 milliliter of oleyl amine, 0.5 milliliter of oleic acid and is stirred 1 minute at 1000r/min.By the forerunner of 100 microlitres of lead bromides
Body injects in above-mentioned toluene solution, injects the presoma of 100 microlitres of cesium bromides after 1 minute, again by 0.5 milliliter of fourth after 1 minute
Alcohol injects.Reaction centrifuged solution 1 minute in 8000r/min after one minute, after collection clear liquid that clear liquid is fast in 100 watts of microwaves
Fast annealing 2 minutes.Solution is collected into precipitation after 8000r/min is centrifuged 4 minutes, is dispersed in 2 milliliters of toluene.The calcium titanium of preparation
Mineral blue light nanometer sheet emission wavelength is 462 nanometers, and halfwidth is 13 nanometers.
Embodiment 3
It weighs 367 milligrams of lead bromides to be dissolved in 2 milliliters of dimethyl sulfoxide (DMSO)s (DMSO), configures the presoma of lead bromide, claim
It takes 212 milligrams of cesium bromides to be dissolved in the hydrobromic acid solution of 1 milliliter of 40% weight ratio, configures the presoma of cesium bromide.Measure 5 millis
It rises toluene, 0.5 milliliter of oleyl amine, 0.5 milliliter of oleic acid and is stirred 1 minute at 1000r/min.By the forerunner of 100 microlitres of lead bromides
Body injects in above-mentioned toluene solution, injects the presoma of 100 microlitres of cesium bromides after 1 minute, again by 0.5 milliliter of fourth after 1 minute
Alcohol injects.Reaction centrifuged solution 1 minute in 8000r/min after one minute, after collection clear liquid that clear liquid is fast in 100 watts of microwaves
Fast annealing 2.5 minutes.Solution is collected into precipitation after 8000r/min is centrifuged 4 minutes, is dispersed in 0.3 milligram of every milliliter of oleyl amine bromine
Toluene solution in.The perovskite blue light nanometer sheet emission wavelength of preparation is 462 nanometers, and halfwidth is 11 nanometers.
Embodiment 4
It weighs 367 milligrams of lead bromides to be dissolved in 2 milliliters of dimethyl sulfoxide (DMSO)s (DMSO), configures the presoma of lead bromide, claim
It takes 212 milligrams of cesium bromides to be dissolved in the hydrobromic acid solution of 1 milliliter of 40% weight ratio, configures the presoma of cesium bromide.Measure 5 millis
It rises toluene, 0.5 milliliter of oleyl amine, 0.5 milliliter of oleic acid and is stirred 1 minute at 1000r/min.By the forerunner of 100 microlitres of lead bromides
Body injects in above-mentioned toluene solution, injects the presoma of 100 microlitres of cesium bromides after 1 minute, again by 0.5 milliliter of fourth after 1 minute
Alcohol injects.Reaction centrifuged solution 1 minute in 8000r/min after one minute, after collection clear liquid that clear liquid is fast in 300 watts of microwaves
Fast annealing 1 minute.Solution is collected into precipitation after 8000r/min is centrifuged 4 minutes, is dispersed in 2 milliliters of toluene.The calcium titanium of preparation
It is respectively 462 nanometers, 479 nanometers and 505 nanometers that mine nanometer sheet solution, which has multiple glow peaks, emission wavelength,.
Embodiment 5
It weighs 367 milligrams of lead bromides to be dissolved in 2 milliliters of dimethyl sulfoxide (DMSO)s (DMSO), configures the presoma of lead bromide, claim
It takes 212 milligrams of cesium bromides to be dissolved in the hydrobromic acid solution of 1 milliliter of 40% weight ratio, configures the presoma of cesium bromide.Measure 5 millis
It rises toluene, 0.5 milliliter of oleyl amine, 0.5 milliliter of oleic acid and is stirred 1 minute at 1000r/min.By the forerunner of 100 microlitres of lead bromides
Body injects in above-mentioned toluene solution, injects the presoma of 100 microlitres of cesium bromides after 1 minute, again by 0.5 milliliter of fourth after 1 minute
Alcohol injects.Reaction centrifuged solution 1 minute in 8000r/min after one minute, after collection clear liquid that clear liquid is fast in 100 watts of microwaves
Fast annealing 1 minute.Solution is collected into precipitation after 8000r/min is centrifuged 4 minutes, is dispersed in 2 milliliters of toluene.Measure 10 microlitres
The perovskite blue light nanometer sheet solution of preparation is dispersed in 4 milliliters of toluene, and the emission wavelength for measuring sample is 462 nanometers, and half is high
Width is 13 nanometers, integrated intensity 604.
Embodiment 6
It weighs 367 milligrams of lead bromides to be dissolved in 2 milliliters of dimethyl sulfoxide (DMSO)s (DMSO), configures the presoma of lead bromide, claim
It takes 212 milligrams of cesium bromides to be dissolved in the hydrobromic acid solution of 1 milliliter of 40% weight ratio, configures the presoma of cesium bromide.Measure 5 millis
It rises toluene, 0.5 milliliter of oleyl amine, 0.5 milliliter of oleic acid and is stirred 1 minute at 1000r/min.By the forerunner of 100 microlitres of lead bromides
Body injects in above-mentioned toluene solution, injects the presoma of 100 microlitres of cesium bromides after 1 minute, again by 0.5 milliliter of fourth after 1 minute
Alcohol injects.Reaction centrifuged solution 1 minute in 8000r/min after one minute, after collection clear liquid that clear liquid is fast in 100 watts of microwaves
Fast annealing 1.5 minutes.Solution is collected into precipitation after 8000r/min is centrifuged 4 minutes, is dispersed in 2 milliliters of toluene.It is micro- to measure 10
It rises the perovskite blue light nanometer sheet solution prepared to be dispersed in 4 milliliters of toluene, the emission wavelength for measuring sample is 462 nanometers, partly
High width is 13 nanometers, integrated intensity 615.
Embodiment 7
It weighs 367 milligrams of lead bromides to be dissolved in 2 milliliters of dimethyl sulfoxide (DMSO)s (DMSO), configures the presoma of lead bromide, claim
It takes 212 milligrams of cesium bromides to be dissolved in the hydrobromic acid solution of 1 milliliter of 40% weight ratio, configures the presoma of cesium bromide.Measure 5 millis
It rises toluene, 0.5 milliliter of oleyl amine, 0.5 milliliter of oleic acid and is stirred 1 minute at 1000r/min.By the forerunner of 100 microlitres of lead bromides
Body injects in above-mentioned toluene solution, injects the presoma of 100 microlitres of cesium bromides after 1 minute, again by 0.5 milliliter of fourth after 1 minute
Alcohol injects.Reaction centrifuged solution 1 minute in 8000r/min after one minute, after collection clear liquid that clear liquid is fast in 100 watts of microwaves
Fast annealing 2 minutes.Solution is collected into precipitation after 8000r/min is centrifuged 4 minutes, is dispersed in 2 milliliters of toluene.Measure 10 microlitres
The perovskite blue light nanometer sheet solution of preparation is dispersed in 4 milliliters of toluene, and the emission wavelength for measuring sample is 462 nanometers, and half is high
Width is 13 nanometers, integrated intensity 6040.
Embodiment 8
It weighs 367 milligrams of lead bromides to be dissolved in 2 milliliters of dimethyl sulfoxide (DMSO)s (DMSO), configures the presoma of lead bromide, claim
It takes 212 milligrams of cesium bromides to be dissolved in the hydrobromic acid solution of 1 milliliter of 40% weight ratio, configures the presoma of cesium bromide.Measure 5 millis
It rises toluene, 0.5 milliliter of oleyl amine, 0.5 milliliter of oleic acid and is stirred 1 minute at 1000r/min.By the forerunner of 100 microlitres of lead bromides
Body injects in above-mentioned toluene solution, injects the presoma of 100 microlitres of cesium bromides after 1 minute, again by 0.5 milliliter of fourth after 1 minute
Alcohol injects.Reaction centrifuged solution 1 minute in 8000r/min after one minute, after collection clear liquid that clear liquid is fast in 100 watts of microwaves
Fast annealing 2.5 minutes.Solution is collected into precipitation after 8000r/min is centrifuged 4 minutes, is dispersed in 2 milliliters of toluene.It is micro- to measure 10
It rises the perovskite blue light nanometer sheet solution prepared to be dispersed in 4 milliliters of toluene, the emission wavelength for measuring sample is 462 nanometers, partly
High width is 13 nanometers, integrated intensity 7927.
Embodiment 9
It weighs 367 milligrams of lead bromides to be dissolved in 2 milliliters of dimethyl sulfoxide (DMSO)s (DMSO), configures the presoma of lead bromide, claim
It takes 212 milligrams of cesium bromides to be dissolved in the hydrobromic acid solution of 1 milliliter of 40% weight ratio, configures the presoma of cesium bromide.Measure 5 millis
It rises toluene, 0.5 milliliter of oleyl amine, 0.5 milliliter of oleic acid and is stirred 1 minute at 1000r/min.By the forerunner of 100 microlitres of lead bromides
Body injects in above-mentioned toluene solution, injects the presoma of 100 microlitres of cesium bromides after 1 minute, again by 0.5 milliliter of fourth after 1 minute
Alcohol injects.Reaction centrifuged solution 1 minute in 8000r/min after one minute, after collection clear liquid that clear liquid is fast in 100 watts of microwaves
Fast annealing 3 minutes.Solution is collected into precipitation after 8000r/min is centrifuged 4 minutes, is dispersed in 2 milliliters of toluene.Measure 10 microlitres
The perovskite blue light nanometer sheet solution of preparation is dispersed in 4 milliliters of toluene, and the emission wavelength for measuring sample is 462 nanometers, and half is high
Width is 13 nanometers, integrated intensity 6488.
Embodiment 10
It weighs 91.75 milligrams of lead bromides to be dissolved in 2 milliliters of dimethyl sulfoxide (DMSO)s (DMSO), configures the presoma of lead bromide,
It weighs 106.4 milligrams of cesium bromides to be dissolved in the hydrobromic acid solution of 1 milliliter of 40% weight ratio, configures the presoma of cesium bromide.Amount
It takes 5 milliliters of toluene, 0.5 milliliter of oleyl amine, 0.5 milliliter of oleic acid and is stirred 1 minute at 1000r/min.By 100 microlitres of lead bromides
Presoma inject in above-mentioned toluene solution, the presoma of 100 microlitres of cesium bromides is injected after 1 minute, again will after 0.6 minute
0.25 milliliter of butanol injection.Reaction centrifuged solution 3 minutes in 10000r/min after one minute, and clear liquid exists after collecting clear liquid
Short annealing 0.5 minute in 200 watts of microwaves.Solution is collected into precipitation after 8000r/min is centrifuged 4 minutes, 2 milliliters is dispersed in and contains
Have in the toluene solution of polymethyl methacrylate, the solution is then centrifuged into 1min with the rotating speed of 6000r/min again, so
After collect supernatant.The perovskite blue light nanometer sheet emission wavelength of preparation is 462 nanometers, and halfwidth is 13 nanometers.
Embodiment 11
It weighs 5872 milligrams of lead bromides to be dissolved in 2 milliliters of dimethyl sulfoxide (DMSO)s (DMSO), configures the presoma of lead bromide, claim
It takes 255.37 milligrams of cesium bromides to be dissolved in the hydrobromic acid solution of 1 milliliter of 40% weight ratio, configures the presoma of cesium bromide.It measures
5 milliliters of toluene, 0.5 milliliter of oleyl amine, 0.5 milliliter of oleic acid simultaneously stir 1 minute at 1000r/min.By 100 microlitres of lead bromides
Presoma injects in above-mentioned toluene solution, injects the presoma of 100 microlitres of cesium bromides after 1 minute, again by 3 milliliters after 2 minutes
Butanol injects.Reaction centrifuged solution 5 minutes in 12000r/min after one minute, by clear liquid in 200 watts of microwaves after collection clear liquid
Middle short annealing 5 minutes.Solution is collected into precipitation after 8000r/min is centrifuged 4 minutes, is dispersed in the toluene containing polystyrene
In solution, the solution is then centrifuged into 10min with the rotating speed of 10000r/min again, then collects supernatant.The calcium titanium of preparation
Mineral blue light nanometer sheet emission wavelength is 462 nanometers, and halfwidth is 11 nanometers.
Claims (5)
1. a kind of room temperature synthetic method of ultrapure inorganic halogen perovskite blue light nanometer sheet, it is characterised in that：Include the following steps：
Step 1：Configure oleyl amine：Oleic acid：Volume of toluene ratio is 1：1：10 mixed liquor, and it is equal with the stirring of the speed of 1000r/min
It is even；
Step 2：The presoma that lead bromide is first added in the mixed liquor of end is reacted into above-mentioned steps 1, with turning for 1000r/min
After speed stirring 1 minute, the presoma of cesium bromide is added, is reacted 0.6-2 minutes；The presoma of the lead bromide is with dimethyl Asia
Sulfone is solvent, a concentration of 0.125-0.8 moles every liter of lead bromide；The presoma of the cesium bromide is with the hydrobromic acid of 40% weight ratio
Solution is solvent, and cesium bromide or cesium carbonate solubility are 0.5-1.2 moles every liter；
Step 3：It is reacted into above-mentioned steps 2 and injects 0.25-3 milliliters of butanol solution reactions in the mixed liquor of end fully, with
The speed of 8000-12000r/min collects supernatant after centrifuging 1-5 minutes；
Step 4：It is centrifuged again after the supernatant of above-mentioned collection is placed in 100-300W microwave heatings 0.5-5 minutes, after centrifugation
Bottom sediment dissolved to obtain finished product with toluene solution.
2. a kind of room temperature synthetic method of ultrapure inorganic halogen perovskite blue light nanometer sheet according to claim 1, special
Sign is：Mixing time is 1min in step 1.
3. a kind of room temperature synthetic method of ultrapure inorganic halogen perovskite blue light nanometer sheet according to claim 1, special
Sign is：After butanol solution being injected in step 3, reaction time 1min.
4. a kind of room temperature synthetic method of ultrapure inorganic halogen perovskite blue light nanometer sheet according to claim 1, special
Sign is：By toluene solution of the bottom sediment after centrifugation containing polymethyl methacrylate or polystyrene in step 4
Dissolving.
5. a kind of room temperature synthetic method of ultrapure inorganic halogen perovskite blue light nanometer sheet according to claim 1, special
Sign is：After the bottom sediment after centrifugation is dissolved with toluene solution in step 4, then with the rotating speed of 6000-10000r/min from
Heart 1-10 minutes collects supernatant and obtains finished product.
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| CN109385268A (en) * | 2018-10-18 | 2019-02-26 | 天津大学 | A kind of synthetic method of organic inorganic hybridization perovskite quantum dot |
| CN110117024A (en) * | 2019-06-25 | 2019-08-13 | 重庆大学 | A kind of unleaded caesium copper iodine perovskite blue light of zero dimension is nanocrystalline and preparation method thereof |
| CN111189811A (en) * | 2020-01-13 | 2020-05-22 | 云南大学 | Synthesis method of water-soluble cesium lead perovskite and application of water-soluble cesium lead perovskite in copper and mercury ion analysis |
| CN114671458A (en) * | 2022-03-18 | 2022-06-28 | 江苏理工学院 | Preparation method and application of perovskite material |
| CN114873635A (en) * | 2022-05-09 | 2022-08-09 | 复旦大学 | Controllable antimony-doped high-luminous-efficiency blue-light perovskite nanosheet and preparation method thereof |
| CN116478689A (en) * | 2023-02-08 | 2023-07-25 | 宿迁学院产业技术研究院 | Preparation method of cesium-lead-bromine perovskite nanosheets capable of emitting ultra-pure green light |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109385268A (en) * | 2018-10-18 | 2019-02-26 | 天津大学 | A kind of synthetic method of organic inorganic hybridization perovskite quantum dot |
| CN110117024A (en) * | 2019-06-25 | 2019-08-13 | 重庆大学 | A kind of unleaded caesium copper iodine perovskite blue light of zero dimension is nanocrystalline and preparation method thereof |
| CN110117024B (en) * | 2019-06-25 | 2021-11-26 | 重庆大学 | Zero-dimensional lead-free cesium copper iodoperovskite blue light nanocrystal and preparation method thereof |
| CN111189811A (en) * | 2020-01-13 | 2020-05-22 | 云南大学 | Synthesis method of water-soluble cesium lead perovskite and application of water-soluble cesium lead perovskite in copper and mercury ion analysis |
| CN114671458A (en) * | 2022-03-18 | 2022-06-28 | 江苏理工学院 | Preparation method and application of perovskite material |
| CN114873635A (en) * | 2022-05-09 | 2022-08-09 | 复旦大学 | Controllable antimony-doped high-luminous-efficiency blue-light perovskite nanosheet and preparation method thereof |
| CN116478689A (en) * | 2023-02-08 | 2023-07-25 | 宿迁学院产业技术研究院 | Preparation method of cesium-lead-bromine perovskite nanosheets capable of emitting ultra-pure green light |
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Application publication date: 20180803 |