CN109734122A - A kind of preparation method preparing perovskite nanowire crystal based on ion exchange - Google Patents
A kind of preparation method preparing perovskite nanowire crystal based on ion exchange Download PDFInfo
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Abstract
The present invention proposes a kind of preparation method that perovskite nanowire crystal is prepared based on ion exchange, using the perovskite nano wire easily prepared as template, it is then immersed in different source of halide solution, 10~50 DEG C at a temperature of react 1~15 day, with the variation of ion-exchange reactions time, realize halide ion in protocalcium titanium ore with the halide ion in halogen source solution is different degrees of exchanges, to obtain the perovskite nano wire of different halogen components；The present invention is by controlling the swap time of perovskite nano wire and ion source, to conveniently compactly change halogenic ingredient in perovskite nano wire；The fluorescence radiation range of perovskite nano wire prepared by the present invention containing halogenic ingredient can cover entire visible light wave range；This preparation method raw material dosage is few, greatly reduces cost；Perovskite Nanowire Quality is high, and dispersibility is distributed on substrate, shifts without micro- manipulation, can carry out in-situ characterization and is prepared by device.
Description
Technical field
The present invention relates to photoelectricity information material technical fields, more particularly to a kind of ion exchange that is based on to prepare perovskite nanometer
The preparation method of line crystal.
Background technique
Perovskite refers to and CaTiO3There is the compound of similar crystal structure, which is referred to as perovskite, it
Chemical equation is ABX3, wherein A is mainly FA ((CH (NH)2)2 +)、MA(CH3NH3 +) and Cs+ etc., B is mainly Pb2+With Sn2+,
X is mainly chlorine (Cl-), bromine (Br-) and iodine (I-).In recent years, after the development of sensitizing dyestuff solar battery, inorganic/organic calcium
The light absorpting ability of titanium ore Yin Qigao and high photoelectric conversion efficiency become one of research hotspot.By the research of a few years,
The transfer efficiency of composite perofskite solar battery is from 22.7% in 3.81% to 2018 years of 2009.In addition to solar-electricity
Except pond, perovskite material also gradually development and application to electroluminescent (light emitting diode, LED), nano laser, photodetection
The fields such as (utilizing the Echo Wall WGM mode of high q-factor), bio-imaging.
Classical inorganic-organic hybridization perovskite (CH3NH3PbX3, X=I-, Br-, Cl-) and there is excellent light absorption energy
Power, these bipolar semiconductors due to simple process, that bandwidth is small, extinction coefficient is high, carrier lifetime is long, diffusion length is big etc. is excellent
Point causes very big concern.However these compounds are very sensitive to environment, including the oxygen in air, vapor, illumination, temperature
Degree etc., these factors easily cause the degradation of perovskite material, thus seriously limit its application.Therefore researchers adopt
Various measures have been taken to improve the stability of hydridization perovskite material and device, including using the reaction lower similar first of activity
Amidine cation or caesium inorganic atoms replacement methylamine etc..Due to full-inorganic CsPbX3Perovskite quantum dot it is excellent in terms of stability
Gesture so that it solar battery, LED, photodetector, in terms of have tremendous expansion.In addition, pure inorganic
CsPbX3Photoluminescence efficiency is very high, and quantum yield is up to 90% or more；Moreover, absorption and the centre of luminescence position of perovskite
It can be realized by adjusting the ratio of halogen, therefore its colour gamut is very wide, has reached the 130% of NTSC color standard.Therefore, one
Aspect Many researchers have made the LED based on perovskite quantum dot.On the other hand, the high-selenium corn based on perovskite, high quantum
Yield, high-gain can prepare nano laser in conjunction with the crystal surface properties that nanowire crystal is excellent.Either organic/inorganic
Composite material (MAPbX3), or CsPbX3It all has been reported that and produces laser emission, and control halogen ratio tuning can be passed through
Shoot laser wavelength.CsPbX3Nano wire has the advantages such as crystal quality is high, defect concentration is low, stability is high, the nanometer being made into
Laser has the characteristics such as high q-factor, Low threshold, high stability.Xiaoyang Zhu in 2015 et al. liquid phase method is prepared for
MAPbX3Nano wire, is successfully realized laser lasing, and laser threshold is 0.22 μ J/cm2, Q value is 3600.2016, Samuel
W.Eatona et al. reports liquid growth CsPbX3Nano wire, laser threshold are 5 μ J/cm2, Q value is 1009 ± 5.Kidong
Park et al. obtains nano wire by chemical gaseous phase conversion method, and laser threshold is 3 μ J/cm2, Q value is 1200-1400.
The preparation method of perovskite nanowire crystal material is an important subject.There are mainly three types of methods at present
(1) it liquid phase method: using lead acetate or lead iodide as nanometer line template, is then immersed into the solution such as MAX/CsX/FAX
Carry out nano-material growth.(2) vapor phase method, by PbX2It is placed in vitreosil pipe and is heated at high temperature with CsX powder,
Nanowire is grown on silicon substrate except 10cm.(3) mixing method first prepares perovskite nano wire with liquid phase method, recycles
Vapor phase method grows the nano wire of other halogen component.Wherein, liquid phase method is the easiest, and vapor phase method energy consumption is high, and mixing method is more troublesome.
Above method prepares that the raw material needed when perovskite nano wire are more, and the nano wire prepared is wanted existing for cluster cluster
Characterization use is carried out to it, need to be shifted with micromechanics arm.One main mesh of perovskite nanowire crystal preparation at present
Mark is method simplicity, and raw material usage is few, and crystal quality is high, and covering colour gamut is wide, nano wire distribution dispersion.
Summary of the invention
It, should it is an object of the invention to propose a kind of preparation method for preparing perovskite nanowire crystal based on ion exchange
The perovskite nanowire crystal materials containing halogenic ingredient of method preparation are few, preparation is simple, crystal quality is high, covering colour gamut is wide
And nano wire distribution dispersion.
In order to achieve the above objectives, the present invention proposes a kind of preparation side that perovskite nanowire crystal is prepared based on ion exchange
Method, comprising the following steps:
Step 1: the perovskite nanowire crystal that preparation easily obtains；
Step 2: the perovskite nanowire crystal is immersed in the solution of source of halide；
Step 3: reacting one end time at a certain temperature, obtains the perovskite containing other halogenic ingredients with displacement
Nanowire crystal.
Preferably, the perovskite nanowire crystal is prepared by liquid phase method, vapor phase method or mixing method.
Preferably, the temperature is 10-50 DEG C.
Preferably, the time is 1-15 days.
Preferably, the molecular formula of the perovskite nanowire crystal of the halogenic ingredient is ABX3。
Preferably, the A is FA, MA or Cs；The B is Pb2+With Sn2+, X is halide ion.
Preferably, the FA is (CH (NH)2)2 +, MA CH3NH2 +And Cs+；The perovskite containing halogenic ingredient is received
Rice noodles crystal are as follows: CsPbCl3、CsPbBr3、CsPbI3、CsPbClxBr3-x、CsPbBrxI3-x、MAPbCl3、MAPbBr3、
MAPbI3、MAPbClxBr3-x、MAPbBrxI3-x、CsSnCl3、CsSnBr3、CsSnI3、CsSnClxBr3-x、CsSnBrxI3-x、FA
PbCl3、FA PbBr3、FAPbI3、FAClxBr3-xOr FABrxI3-x。
Preferably, the source of halide is to dissolve in a solvent, solution temperature 90- under surfactant hydrotropy
200℃；
The surfactant is oleic acid, oleyl amine or positive trioctylphosphine phosphorus.
Preferably, the source of halide is PbCl2、PbBr2、PbI2, OAmCl (chlorination oleyl amine), OAmBr (brominated oil
Amine), OAmI (iodate oleyl amine), MeMgCl (methyl-magnesium-chloride), MeMgBr (methyl chloride bromine) or MeMgI (methyl chloride
Iodine).
Preferably, as ion exchange obtain described in the perovskite nanowire crystal containing halogenic ingredient, original will not be changed
The size and shape of the perovskite nanowire crystal.
Compared with prior art, of the invention to be advantageous in that: the present invention using the perovskite nano wire that easily prepares as
Template is then dipped in the solution in different ions source, by control swap time and temperature, available difference halogens at
The perovskite nano wire divided, we term it the perovskite nanowire crystal preparation methods based on ion exchange.According to different
Perovskite nano-material, selects suitable substrate, and substrate can be hydrophilic substrates, or hydrophilic substrates.Generally
For, when organic solvent is hydrophilic material, select hydrophilic substrates；When organic solvent is hydrophobic, selection is dredged
Aqueous substrate.
The perovskite nanowire crystal prepared by ion-exchange, halogenic ingredient can be with simple adjustment.According to reality
It is required that can satisfy the application requirements such as nano laser, detection.
The present invention is then dipped in the solution in different ions source using the perovskite nano wire easily prepared as template, is led to
The temperature and time for crossing control ion exchange, to obtain the perovskite nano wire of different halogen components.In the method, pass through
It controls ion-exchange time and changes halogenic ingredient ratio in perovskite nano wire, to realize nano wire emission wavelength to entirely may be used
The covering of light-exposed range；Material utilization amount is few, at low cost；Nanowire Quality is high, and dispersibility is distributed on substrate, can carry out original position
Measurement is prepared with device；And the halogenic ingredient in nano wire can be controlled by conditions such as ion-exchange time, temperature, root
According to actual requirement, the nanowire crystal of different sizes and halogenic ingredient can be prepared.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, technical solution of the present invention will be made below into
Illustrate to one step.
The present invention proposes a kind of preparation method that perovskite nanowire crystal is prepared based on ion exchange, including following step
It is rapid:
Step 1: perovskite is prepared so that perovskite nanowire crystal is prepared by liquid phase method, vapor phase method or mixing method
Nanowire crystal；
Step 2: perovskite nanowire crystal is immersed in the solution of source of halide；
Step 3: reacting 1-15 days under in the environment of temperature is 10-50 DEG C, obtains the calcium containing halogenic ingredient with displacement
Titanium ore nanowire crystal.
In the present embodiment, the molecular formula of the perovskite nanowire crystal of halogenic ingredient is ABX3。
In the present embodiment, A FA, MA or Cs；B is mainly Pb2+With Sn2+, X is halide ion, predominantly chlorine (Cl-)、
Bromine (Br-) and iodine (I-)。
In the present embodiment, the perovskite nanowire crystal of halogenic ingredient are as follows: CsPbCl3、CsPbBr3、CsPbI3、
CsPbClxBr3-x、CsPbBrxI3-x、MAPbCl3、MAPbBr3、MAPbI3、MAPbClxBr3-x、MAPbBrxI3-x、CsSnCl3、
CsSnBr3、CsSnI3、CsSnClxBr3-x、CsSnBrxI3-xOr FA PbCl3、FA PbBr3、FAPbI3、FAClxBr3-x、
FABrxI3-x。
In the present embodiment, source of halide is under surfactant hydrotropy, and in a solvent, solution temperature is for dissolution
90-200℃；
Surfactant is oleic acid, oleyl amine or positive trioctylphosphine phosphorus.
In the present embodiment, source of halide is mainly PbCl2、PbBr2、PbI2, OAmCl (chlorination oleyl amine), OAmBr (bromine
Carburetion amine), OAmI (iodate oleyl amine), MeMgCl (methyl-magnesium-chloride), MeMgBr (methyl chloride bromine) or MeMgI (methyl chloride
Change iodine).
In the present embodiment, the nanowire crystal obtained by ion exchange, will not change former nanowire crystal size and
Pattern.
Beneficial effects of the present invention will be made by five specific experiment schemes below further elucidated above:
Embodiment 1
The preparation of perovskite nanowire crystal.
It takes 0.814g cesium carbonate and 2.5mL oleic acid to be mixed into be dissolved in 40mL octadecylene, 120 DEG C of dry 1h, in nitrogen ring
150 DEG C are heated under border, until reaction generates oleic acid caesium completely；0.069g lead bromide is taken to be added in 5mL octadecylene, 120 DEG C
Dry 30min；0.5mL oleyl amine and 0.5mL oleic acid hydrotropy is added, oil bath pan is heated to 180 DEG C, after lead bromide is completely dissolved,
It is taken out after oleic acid caesium 0.4mL reaction 5s is added, immerses in ice water and be quickly cooled to room temperature, obtain CsPbBr3Perovskite nanometer
Grain.Then it is centrifuged 15min with 12000rpm, removes supernatant liquor, is dispersed with toluene, 12000rpm is centrifuged 15min again, repeats
3 times.The perovskite nanometer powder that centrifugation obtains is dissolved in spare in 20mL methanol.The hydrophilic substrate handled well is placed in 130 DEG C
Heating plate on, take the above-mentioned solution of a drop to be added drop-wise on substrate, methanol can volatilize rapidly, and perovskite nano particle is dispersed in
On substrate.Then, which is placed in the culture dish of room temperature, and 5 drop methanol is added dropwise in culture dish, form the full of methanol
And steam, it cultivates 5 days, obtains CsPbBr3Perovskite linear crystal material.
Take 0.13mmol PbCl2Be mixed into octadecylene, 120 DEG C of dry 1h, be added 0.5mL oleic acid, 0.5mL oleyl amine, with
And the positive trioctylphosphine phosphorus hydrotropy of 1mL, wait PbCl2After being completely dissolved, temperature is down to 40 DEG C, as ion source.
Then by CsPbBr obtained3Nano wire immerses in ion source, and 40 DEG C are cultivated 1 day, obtains CsPbBrxCl3-xNanometer
Line.
This method replaces the halide ion of perovskite nanowire crystal, uses fluorescence microscope, discovery afterwards
Nano wire has apparent color change, and color is partially blue.
Embodiment 2
The preparation of perovskite nanowire crystal.
It takes 0.814g cesium carbonate and 2.5mL oleic acid to be mixed into be dissolved in 40mL octadecylene, 120 DEG C of dry 1h, in nitrogen ring
150 DEG C are heated under border, until reaction generates oleic acid caesium completely；0.069g lead bromide is taken to be added in 5mL octadecylene, 120 DEG C
Dry 30min；0.5mL oleyl amine and 0.5mL oleic acid hydrotropy is added, oil bath pan is heated to 180 DEG C, after lead bromide is completely dissolved,
It is taken out after oleic acid caesium 0.4mL reaction 5s is added, immerses in ice water and be quickly cooled to room temperature, obtain CsPbBr3Perovskite nanometer
Grain.Then it is centrifuged 15min with 12000rpm, removes supernatant liquor, is dispersed with toluene, 12000rpm is centrifuged 15min again, repeats
3 times.The perovskite nanometer powder that centrifugation obtains is dissolved in spare in 20mL methanol.The hydrophilic substrate handled well is placed in 130 DEG C
Heating plate on, take the above-mentioned solution of a drop to be added drop-wise on substrate, methanol can volatilize rapidly, and perovskite nano particle is dispersed in
On substrate.Then, which is placed in the culture dish of room temperature, and 5 drop methanol is added dropwise in culture dish, form the full of methanol
And steam, it cultivates 5 days, obtains CsPbBr3Perovskite linear crystal material.
Take 0.13mmol PbCl2Be mixed into octadecylene, 120 DEG C of dry 1h, be added 0.5mL oleic acid, 0.5mL oleyl amine, with
And the positive trioctylphosphine phosphorus hydrotropy of 1mL, wait PbCl2After being completely dissolved, temperature is down to 40 DEG C, as ion source.
Then by CsPbBr obtained3Nano wire immerses in ion source, and 40 DEG C are cultivated 2 days, obtains CsPbCl3Nano wire.
This method prepare when the halide ion of perovskite nanowire crystal is replaced, after seen with fluorescence microscope
It examines, discovery nano wire has apparent color change, and color is partially purple.
Embodiment 3
The preparation of perovskite nanowire crystal.
It takes 0.814g cesium carbonate and 2.5mL oleic acid to be mixed into be dissolved in 40mL octadecylene, 120 DEG C of dry 1h, in nitrogen ring
150 DEG C are heated under border, until reaction generates oleic acid caesium completely；0.069g lead bromide is taken to be added in 5mL octadecylene, 120 DEG C
Dry 30min；0.5mL oleyl amine and 0.5mL oleic acid hydrotropy is added, oil bath pan is heated to 180 DEG C, after lead bromide is completely dissolved,
It is taken out after oleic acid caesium 0.4mL reaction 5s is added, immerses in ice water and be quickly cooled to room temperature, obtain CsPbBr3Perovskite nanometer
Grain.Then it is centrifuged 15min with 12000rpm, removes supernatant liquor, is dispersed with toluene, 12000rpm is centrifuged 15min again, repeats
3 times.The perovskite nanometer powder that centrifugation obtains is dissolved in spare in 20mL methanol.The hydrophilic substrate handled well is placed in 130 DEG C
Heating plate on, take the above-mentioned solution of a drop to be added drop-wise on substrate, methanol can volatilize rapidly, and perovskite nano particle is dispersed in
On substrate.Then, which is placed in the culture dish of room temperature, and 5 drop methanol is added dropwise in culture dish, form the full of methanol
And steam, it cultivates 5 days, obtains CsPbBr3Perovskite linear crystal material.
0.038mol oleyl amine and 100 ethyl alcohol are blended in three-neck flask, and ice water water-bath is then slowly added into 0.076mol
HX reacts a whole night, and vacuum evaporation obtains OAmX, and then with ether mostly with cleaning, OAmX is heated to 80 DEG C in a vacuum, heating
A whole night.
0.026mmol OAmCl is taken to be mixed into octadecylene, 0.5mL oleic acid is added in 120 DEG C of dry 1h, 0.5mL oleyl amine helps
Molten, after waiting OAmCl to be completely dissolved, temperature is down to 40 DEG C, as ion source.
Then by CsPbBr obtained3Nano wire immerses in ion source, and 40 DEG C are cultivated 2 days, obtains CsPbCl3Nano wire.
This method prepare when the halide ion of perovskite nanowire crystal is replaced, after seen with fluorescence microscope
It examines, discovery nano wire has apparent color change, and color is partially purple.
Embodiment 4
The preparation of perovskite nanowire crystal.
Take the PbI of 460mg2In the molten anhydrous dimethyl formamide (DMF) to 1mL, one is stirred on 70 DEG C of warm table
It is stand-by whole night, take the DMF solution of PbI2 to be added drop-wise to spin coating on clean glass substrate, revolving speed 1000rpm rotates 120s, with
The PbI that spin coating is good afterwards2Sample, which is placed on 100 DEG C of warm table, heats 15min, forms PbI2Film.The film is immersed in
In the methanol solution of the CsBr of 8mg/mL, PbI2Film upward, grows 12h in the environment of 50 DEG C.Sample is taken out with anhydrous different
Propyl alcohol rinses 30s, is subsequently placed on 50 DEG C of warm table and heats 5min, obtains CsPbBr3Nano wire.
Take 0.13mmol PbI2Be mixed into octadecylene, 120 DEG C drying one hour, be added 0.5mL oleic acid, 0.5mL oleyl amine
Hydrotropy waits PbBr2After being completely dissolved, temperature is down to 40 DEG C, as ion source.
Then by CsPbBr obtained3Nano wire immerses in ion source, and 40 DEG C are cultivated 2 days, obtains CsPbI3Nano wire.
This method replaces the halide ion of perovskite nano wire when preparing, and uses fluorescence microscope, hair afterwards
Existing nano wire has apparent color change, and color reddens.
Embodiment 5
The preparation of perovskite nanowire crystal.
Prepare the PbAc of 100mg/mL2Methanol solution, then by PbAc2Methanol solution be coated onto 65 DEG C of glass substrate
Upper (the quality of painting about 1mg/cm2), 30min then is heated on 65 DEG C of warm table, PbAc is made2Film.The film is immersed
To the CH of the 5mg/ml of 1mL3NH3In the aqueous isopropanol of Br, down, 20h is reacted at room temperature.Then take out sample isopropyl
Alcohol cleans 5s, obtains CH3NH3PbBr3Nano wire.
Take 0.13mmol PbI2It is mixed into octadecylene, 120 DEG C of dry 1h, 0.5mL oleic acid is added, 0.5mL oleyl amine helps
It is molten, wait PbI2After being completely dissolved, temperature is down to 40 DEG C, as ion source.
Then by CH obtained3NH3PbBr3Nano wire immerses in ion source, and 40 DEG C are cultivated 2 days, obtains CH3NH3PbI3It receives
Rice noodles.
This method prepare when the halide ion of perovskite nanowire crystal is replaced, after seen with fluorescence microscope
It examines, discovery nano wire has apparent color change, and color reddens.
The above is only a preferred embodiment of the present invention, does not play the role of any restrictions to the present invention.Belonging to any
Those skilled in the art, in the range of not departing from technical solution of the present invention, to the invention discloses technical solution and
Technology contents make the variation such as any type of equivalent replacement or modification, belong to the content without departing from technical solution of the present invention, still
Within belonging to the scope of protection of the present invention.
Claims (10)
1. a kind of preparation method for preparing perovskite nanowire crystal based on ion exchange, which comprises the following steps:
Step 1: the perovskite nanowire crystal being easy to get is prepared；
Step 2: the perovskite nanowire crystal is immersed in the solution of source of halide；
Step 3: reacting one end time at a certain temperature, obtains the perovskite nanometer containing other halogenic ingredients with displacement
Line crystal.
2. the preparation method according to claim 1 for being prepared perovskite nanowire crystal based on ion exchange, feature are existed
In the perovskite nanowire crystal is prepared by liquid phase method, vapor phase method or mixing method.
3. the preparation method according to claim 1 for being prepared perovskite nanowire crystal based on ion exchange, feature are existed
In the temperature is 10-50 DEG C.
4. the preparation method according to claim 1 for being prepared perovskite nanowire crystal based on ion exchange, feature are existed
In the time is 1-15 days.
5. the preparation method according to claim 1 for being prepared perovskite nanowire crystal based on ion exchange, feature are existed
In the molecular formula of the perovskite nanowire crystal containing halogenic ingredient is ABX3。
6. the preparation method according to claim 5 for being prepared perovskite nanowire crystal based on ion exchange, feature are existed
In the A is FA, MA or Cs；The B is Pb2+With Sn2+, X is halide ion.
7. the preparation method according to claim 1 for being prepared perovskite nanowire crystal based on ion exchange, feature are existed
In the FA is (CH (NH)2)2+, MA CH3NH2+And Cs+；The perovskite nanowire crystal containing halogenic ingredient are as follows:
CsPbCl3、CsPbBr3、CsPbI3、CsPbClxBr3-x、CsPbBrxI3-x、MAPbCl3、MAPbBr3、MAPbI3、
MAPbClxBr3-x、MAPbBrxI3-x、CsSnCl3、CsSnBr3、CsSnI3、CsSnClxBr3-x、CsSnBrxI3-x、FAPbCl3、
FAPbBr3、FAPbI3、FAClxBr3-xOr FABrxI3-x。
8. according to the preparation method described in claim 1 for preparing perovskite nanowire crystal based on ion exchange, which is characterized in that
The source of halide is under surfactant hydrotropy, and in a solvent, solution temperature is 90-200 DEG C for dissolution；
The surfactant is oleic acid, oleyl amine or positive trioctylphosphine phosphorus.
9. according to the preparation method described in claim 1 for preparing perovskite nanowire crystal based on ion exchange, which is characterized in that
The source of halide is PbCl2、PbBr2、PbI2, OAmCl, OAmBr, OAmI, MeMgCl, MeMgBr or MeMgI.
10. according to the preparation method described in claim 1 for preparing perovskite nanowire crystal based on ion exchange, feature exists
In, as ion exchange obtain described in the perovskite nanowire crystal containing halogenic ingredient, the former perovskite will not be changed and received
The size and shape of rice noodles crystal.
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| CN113004745A (en) * | 2021-03-02 | 2021-06-22 | 苏州大学 | High-viscosity perovskite quantum dot conductive ink and preparation method thereof |
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Application publication date: 20190510 |