CN107746072B - A kind of preparation method of perovskite micron ring array - Google Patents
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Abstract
The invention discloses a kind of preparation method of perovskite micron ring array, the perovskite micron ring array is full-inorganic CsPbX3Perovskite micron ring array or full-inorganic CsPb (BrnA1‑n)3Perovskite micron ring array, wherein X indicates one of Cl ion, Br ion or I ion, A indicates one of Cl ion or I ion, 0 < n < 3,1) preparation method is the following steps are included: prepare colloid monolayers template: polystyrene microsphere suspension is spin-coated in substrate, after water evaporation is complete, colloid monolayers template is obtained；2) prepare perovskite micron ring array: perovskite precursor solution be spin-coated in colloid monolayers template, it is to be dried after with toluene soak to remove polystyrene microsphere, it is finally heated to obtain perovskite micron ring array.This method is easy to operate, operating procedure difficulty is low, and the emission wavelength of the size of perovskite micron ring, calcium perovskite micron ring array is adjustable.
Description
Technical field
The present invention relates to a kind of preparation methods of perovskite micron ring array, belong to full-inorganic perovskite technical field.
Background technique
Micron cyclic structure also makes them by general in magnetics, optics, the unique performance of field of optoelectronic devices and application
Time concern.Full-inorganic perovskite is a kind of novel semiconductor nano material, since it possesses the fluorescence of high stability, superelevation
The emission wavelength that quantum yield, composition rely on can cover the excellent properties such as entire visible region and narrow linewidth, become close
The hot spot of research in several years.The CH prepared at present3NH3PbI3Perovskite hexagon micron chip arrays are to utilize to obtain in photoetching
To boron nitride single tier templates on chemical vapor deposition obtain, the device is complicated, operating procedure needed for this method disadvantage is
Difficulty is high, at high cost；Another colloid monolayers template etching method easy to operate and at low cost, can only prepare bowl-shape at present
With netted structure C H3NH3PbI3Perovskite；Compared to organic inorganic hybridization perovskite, full-inorganic perovskite not only has well
Optical characteristics, and have higher chemical stability.Therefore there is an urgent need to a kind of simple methods to prepare full-inorganic calcium titanium
Mine micron ring array.
Summary of the invention
Technical problem: the object of the present invention is to provide a kind of preparation method of perovskite micron ring array, the calcium titanium
Mine micron ring array is full-inorganic CsPbX3Perovskite micron ring array or full-inorganic CsPb (BrnA1-n)3Perovskite micron ring
Array, wherein X indicates that one of Cl ion, Br ion or I ion, A indicate one of Cl ion or I ion, 0 < n <
1, this method is easy to operate, operating procedure difficulty is low, and can size to the perovskite micron ring array of preparation and luminous wave
Length is regulated and controled.
Technical solution: the present invention provides a kind of preparation method of perovskite micron ring array, the perovskite micron
Ring array is full-inorganic CsPbX3Perovskite micron ring array or full-inorganic CsPb (BrnA1-n)3Perovskite micron ring array,
Middle X indicates that one of Cl ion, Br ion or I ion, A indicate one of Cl ion or I ion, 0 < n < 1, the preparation
Method the following steps are included:
1) it prepares colloid monolayers template: polystyrene microsphere suspension is spin-coated in substrate, after water evaporation is complete, obtain
Colloid monolayers template；
2) it prepares perovskite micron ring array: perovskite precursor solution is spin-coated in colloid monolayers template, it is to be dried
It is impregnated later with organic solvent containing benzene to remove polystyrene microsphere, it is finally heated to obtain perovskite micron ring array.
Wherein:
The step of colloid monolayers template is prepared described in step 1) are as follows: polystyrene microsphere suspension is spin-coated on substrate
On, after water evaporation is complete, 1~20h is heated under the conditions of 100~110 DEG C, room temperature is naturally cooled to and obtains colloid monolayers template,
And the time heated under the conditions of 100~110 DEG C is longer, the perovskite micron ring being finally prepared is bigger.
Polystyrene microsphere particle size described in step 1) is 8~10um, polyphenyl second in polystyrene microsphere suspension
The emulsion solid content of alkene particle is 2.5~5.0wt%；The revolving speed of spin coating described in step 1) is 60~100rpm.
Substrate described in step 1) is treated quartz plate, glass slide or silicon wafer, treatment process are as follows: successively uses volume
Than the H for 7:3~3:12SO4/H2O2Mixed solution, acetone, isopropanol, ethyl alcohol and deionized water ultrasonic cleaning, nitrogen is blown later
It is dried for standby after dry.
Step 2) the perovskite precursor solution is to contain CsBr and PbBr2Dimethyl sulfoxide organic solution and CsBr
With PbBr2Molar ratio be 0.8~1.2, contain CsCl and PbCl2Dimethyl sulfoxide organic solution and CsCl and PbCl2Rub
You are than being 0.8~1.2, containing CsI and PbI2Dimethyl sulfoxide organic solution and CsI and PbI2Molar ratio be 0.8~1.2,
Contain CsBr, PbBr2And PbCl2Dimethyl sulfoxide organic solution and solution in Cs ion and Pb ion molar ratio be 0.8~
1.2 or contain CsBr, PbBr2And PbI2Dimethyl sulfoxide organic solution and solution in Cs ion and Pb ion molar ratio
It is 0.8~1.2.
The atomic ratio for adjusting Cl ion, Br ion and I ion in the perovskite precursor solution, obtains emission wavelength
Different perovskite micron ring arrays.
The perovskite precursor solution adjusts the atomic ratio of Cl ion therein, Br ion and I ion, is sent out
Optical wavelength range is the perovskite micron ring array of 470nm~550nm, wherein there was only the Br atomic time in precursor solution,
CsPbBr3The emission wavelength of perovskite micron ring array is 525nm；After Cl atom is added, CsPbBrnCl3-nPerovskite micron ring
The emission wavelength blue shift of array；After I atom is added, CsPbBrnI3-nThe emission wavelength red shift of perovskite micron ring array.
Organic solvent containing benzene described in step 2) is toluene, dimethylbenzene or chloroform.
Described in step 2) by perovskite precursor solution be spin-coated on the spin speed in colloid monolayers template be 4000~
5000rpm, spin-coating time are 30~60s, it is described it is to be dried after with toluene soak to remove polystyrene microsphere during
It is dry to refer to the drying in vacuum environment, and vacuum environment pressure is less than 20pa.
The temperature that heating described in step 2) obtains heating during perovskite micron ring array is 100~150 DEG C, heating
1~2h of Shi Changwei.
The utility model has the advantages that compared with prior art, present invention has the advantage that
1) preparation method of perovskite micron ring array proposed by the present invention is simple, operating procedure difficulty is low, and can be right
The size and emission wavelength of perovskite micron ring array are regulated and controled；
2) equipment needed for the preparation method of perovskite micron ring array proposed by the present invention is simple, reaction speed is fast, energy consumption
It is low, raw material is single, easy to operate, not dangerous, raw material supply is convenient, low in raw material price；
3) present invention be size and the controllable full-inorganic perovskite micron ring array of emission wavelength preparation and its in light
It learns and the application of field of optoelectronic devices is laid a good foundation；
Detailed description of the invention
Fig. 1 is the microscope figure of colloid monolayers template in embodiment 1；
Fig. 2 is CsPbBr in embodiment 13The microscope figure of perovskite micron ring array；
Fig. 3 is CsPbBr in embodiment 23The internal diameter and colloid monolayers template heating treatment time of perovskite micron ring array
Between relational graph；
Fig. 4 is to prepare when Cl ion, Br ion and I ion different mol ratio in perovskite precursor solution in embodiment 3
Perovskite micron ring array photoluminescence spectra spectral line.
Specific embodiment
The present invention is done below with reference to embodiment and attached drawing and is further explained, the following example is merely to illustrate this hair
It is bright, but be not used to limit practical range of the invention.
The concentrated sulfuric acid used in following embodiment, hydrogen peroxide, acetone, isopropanol, toluene, dehydrated alcohol, cesium bromide, bromination
The raw materials such as lead, lead iodide, lead chloride, dimethyl sulfoxide are analytical reagents；Glass apparatus used in experimentation uses
It is dry after preceding use deionized water rinse three times；Polystyrene microsphere turbid liquid used is purchased from Shanghai Aladdin biochemical technology share
Co., Ltd.
Embodiment 1
Internal diameter is the full-inorganic CsPbBr of 2.5um3The preparation of perovskite micron ring array
1) H for being successively 3:1 with volume ratio by substrate of glass2SO4/H2O2It mixed solution, acetone, isopropanol, ethyl alcohol and goes
Ionized water ultrasonic cleaning；It is dried for standby again with being dried with nitrogen to be placed in baking oven, polystyrene microsphere hanging drop is being cleaned
Substrate of glass on, with the speed spin coating of 80rpm, to water evaporation after, obtain colloid monolayers template, wherein polystyrene is micro-
Ball particle size is 8um, and the emulsion solid content of ps particle is 5.0wt% in polystyrene microsphere suspension；
2) by 1mmolCsBr and 1mmolPbBr2It is dissolved in 10mL dimethyl sulfoxide, obtains the precursor solution of perovskite；
3) perovskite precursor solution is spin-coated in colloid monolayers template with the spin speed of 4500rpm, spin-coating time
For 30s, be placed on it is dry in vacuum environment of the pressure less than 20pa, to after completely with toluene soak to remove polystyrene
Microballoon is finally placed in 150 DEG C of heating 2h on warm table, obtains the CsPbBr that internal diameter is 2.5um3Perovskite micron ring array.
Fig. 1 be the present embodiment in colloid monolayers template micrograph, as shown in Figure 1, polystyrene microsphere size it is uniform and
Marshalling, microsphere diameter 8um；
Fig. 2 is CsPbBr in the present embodiment3The micrograph of perovskite micron ring array, as shown in Fig. 2, full-inorganic CsPbBr3
Perovskite micron ring size is uniform, and micron ring array marshalling, the outer diameter of ring is about 4.3um, and internal diameter is about 2.5um.
Embodiment 2
Internal diameter is the full-inorganic CsPbBr of 6um3The preparation method of perovskite micron ring array, includes the following steps:
1) H for being successively 7:3 with volume ratio by substrate of glass2SO4/H2O2Mixed solution, acetone, isopropanol and are gone ethyl alcohol
Ionized water ultrasonic cleaning；It is dried for standby again with being dried with nitrogen to be placed in baking oven.Polystyrene microsphere hanging drop is being cleaned
Substrate of glass on, with the speed spin coating of 60rpm, finished to water evaporation and be placed on warm table 100 DEG C and heat 20h or 110 DEG C
1h is heated, room temperature is naturally cooled to, obtains colloid monolayers template, wherein polystyrene microsphere particle size is 10um, polyphenyl second
The emulsion solid content of ps particle is 2.5wt% in alkene microsphere suspension liquid；
2) by 0.8mmolCsBr and 1mmolPbBr2It is dissolved in 10mL dimethyl sulfoxide, obtains perovskite precursor solution；
3) with the spin speed of 4000rpm, perovskite precursor solution is spin-coated on colloid monolayers mould for 60s by spin-coating time
On plate, then it is placed in drying in vacuum environment of the pressure less than 20pa, to completely micro- to remove polystyrene with toluene soak later
Ball is finally placed in 100 DEG C of heating 1h on warm table, obtains the CsPbBr that internal diameter is 6um3Perovskite micron ring array.
Fig. 3 is CsPbBr in embodiment 23The pre- place of internal diameter and polystyrene microsphere single tier templates heating of perovskite micron ring
The relationship between the time is managed, passes through the time different to 100 DEG C of heat pre-treatments of polystyrene microsphere single tier templates as shown in Figure 3
Available perovskite micron ring array of different sizes, the time of heating is longer, and the internal diameter of obtained ring is bigger.
Embodiment 3
Internal diameter is the full-inorganic CsPb (Cl of 2.5um0.3Br0.7)3The preparation of perovskite micron ring array
1) H for being successively 8:3 with volume ratio by substrate of glass2SO4/H2O2Mixed solution, acetone, isopropanol and are gone ethyl alcohol
Ionized water ultrasonic cleaning；It is dried for standby again with being dried with nitrogen to be placed in baking oven.Polystyrene microsphere hanging drop is being cleaned
Substrate of glass on, with the speed spin coating of 80rpm, after water evaporation finish be placed on warm table it is naturally cold after 110 DEG C of heating 1h
But to room temperature, colloid monolayers template is obtained；Wherein polystyrene microsphere particle size is 9um, in polystyrene microsphere suspension
The emulsion solid content of ps particle is 3.5wt%；
2) by 1mmolCsBr, 0.7mmolPbBr2And 0.3mmolPbCl2It is dissolved in 10mL dimethyl sulfoxide, obtains after mixing
To the perovskite precursor solution of the ion containing Cl；
3) with the spin speed of 5000rpm, perovskite precursor solution is spin-coated on colloid monolayers mould for 40s by spin-coating time
On plate, then it is placed in drying in vacuum environment of the pressure less than 20pa, to completely micro- to remove polystyrene with toluene soak later
Ball is finally placed in 120 DEG C of heating 1.5h on warm table, obtains CsPb (Cl0.3Br0.7)3Perovskite micron ring array.
Embodiment 4
Internal diameter is the full-inorganic CsPb (Br of 2.5um0.8I0.2)3The preparation of perovskite micron ring array
1) H for being successively 3:1 with volume ratio by substrate of glass2SO4/H2O2Mixed solution, acetone, isopropanol and are gone ethyl alcohol
Ionized water ultrasonic cleaning；It is dried for standby again with being dried with nitrogen to be placed in baking oven.Polystyrene microsphere hanging drop is being cleaned
Substrate of glass on, with the speed spin coating of 100rpm, after water evaporation finish be placed on warm table it is naturally cold after 105 DEG C of heating 2h
But to room temperature, colloid monolayers template is obtained；Wherein polystyrene microsphere particle size is 8um, in polystyrene microsphere suspension
The emulsion solid content of ps particle is 4.5wt%；
2) by 1mmolCsBr, 0.8mmolPbBr2And 0.4mmolPbI2It is dissolved in 10mL dimethyl sulfoxide, obtains after mixing
The perovskite precursor solution of the ion containing I；
3) with the spin speed of 4500rpm, perovskite precursor solution is spin-coated on colloid monolayers mould for 50s by spin-coating time
On plate, then it is placed in drying in vacuum environment of the pressure less than 20pa, to completely micro- to remove polystyrene with toluene soak later
Ball is finally placed in 140 DEG C of heating 2h on warm table, obtains CsPb (Br0.8I0.2)3Perovskite micron ring array.
Fig. 4 is CsPb (Br in embodiment 3 and embodiment 4nA1-n)3The micron prepared when perovskite difference halogen atom ratio
The PL spectral line of ring array, as shown in figure 4, there was only CsBr and PbBr in precursor solution2When obtained micron ring emission wavelength be
PbCl is added in 525nm2It can make emission wavelength blue shift, PbI is added2It can make emission wavelength red shift.
Claims (7)
1. a kind of preparation method of perovskite micron ring array, it is characterised in that: the perovskite micron ring array be completely without
Machine CsPbX3Perovskite micron ring array or full-inorganic CsPb (BrnA1-n)3Perovskite micron ring array, wherein X indicate Cl from
One of son, Br ion or I ion, A indicate one of Cl ion or I ion, 0 < n < 1, the preparation method include with
Lower step:
1) it prepares colloid monolayers template: polystyrene microsphere suspension is spin-coated in substrate, after water evaporation is complete, obtain colloid
Single tier templates；
2) it prepares perovskite micron ring array: perovskite precursor solution being spin-coated in colloid monolayers template, after to be dried
It is impregnated with organic solvent containing benzene to remove polystyrene microsphere, it is finally heated to obtain perovskite micron ring array；
Polystyrene microsphere particle size described in step 1) is 8~10um, and polystyrene is micro- in polystyrene microsphere suspension
The emulsion solid content of grain is 2.5~5.0wt%；The revolving speed of spin coating described in step 1) is 60~100rpm.
2. a kind of preparation method of perovskite micron ring array as described in claim 1, it is characterised in that: described in step 1)
The step of preparing colloid monolayers template are as follows: polystyrene microsphere suspension is spin-coated in substrate, after water evaporation is complete, 100
1~20h is heated under the conditions of~110 DEG C, is naturally cooled to room temperature and is obtained colloid monolayers template, is used to prepare various sizes of ring.
3. a kind of preparation method of perovskite micron ring array as claimed in claim 2, it is characterised in that: described 100
The time heated under the conditions of~110 DEG C is longer, and the perovskite micron ring being finally prepared is bigger.
4. a kind of preparation method of perovskite micron ring array as described in claim 1, it is characterised in that: described in step 2)
It is 4000~5000rpm, spin-coating time 30 that perovskite precursor solution, which is spin-coated on the spin speed in colloid monolayers template,
~60s.
5. a kind of preparation method of perovskite micron ring array as described in claim 1, it is characterised in that: perovskite presoma
The concentration of solution is 0.2~0.4M.
6. a kind of preparation method of perovskite micron ring array as described in claim 1, it is characterised in that: described in step 2)
It is impregnated after to be dried with organic solvent containing benzene to remove drying during polystyrene microsphere and refer to the drying in vacuum environment,
And vacuum environment pressure needs to be less than 20pa.
7. a kind of preparation method of perovskite micron ring array as described in claim 1, it is characterised in that: described in step 2)
The finally heated temperature heated during perovskite micron ring array that obtains is 100~150 DEG C, when heating a length of 1~2h, be used for
Obtain the better perovskite of crystalline quality.
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| CN109300805A (en) * | 2018-08-31 | 2019-02-01 | 华南师范大学 | Vacuum control CsPbIxBr3-xThe method and photovoltaic device of perovskite growth |
| CN110079302B (en) * | 2019-04-24 | 2022-05-13 | 东南大学 | Preparation method of manganese-doped perovskite microstructure ring/rod |
| CN111908417B (en) * | 2019-05-10 | 2023-11-28 | 中国科学院化学研究所 | Perovskite single crystal nano ring and preparation method and application thereof |
| CN111952463B (en) * | 2020-08-26 | 2023-04-07 | 合肥工业大学 | Preparation method of large-area perovskite nanowire array |
| CN112608403B (en) * | 2020-11-20 | 2022-02-22 | 西安交通大学 | Preparation method and application of high-stability polymer microsphere @ all-inorganic lead-halogen perovskite quantum dot |
| CN114874764B (en) * | 2022-05-12 | 2023-06-02 | 东南大学 | Preparation method of perovskite film with enhanced luminescence performance |
| CN114890460A (en) * | 2022-05-17 | 2022-08-12 | 山东建筑大学 | Method for preparing perovskite nano material based on elliptic paraboloid-shaped aluminum oxide template |
| CN116948642A (en) * | 2023-07-25 | 2023-10-27 | 东南大学 | Nano structure for enhancing nonlinear luminescence performance of perovskite and preparation method thereof |
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