CN107217303A - The adjustable CH of diameter3NH3PbI3The synthetic method of perovskite micro wire - Google Patents

The adjustable CH of diameter3NH3PbI3The synthetic method of perovskite micro wire Download PDF

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Publication number
CN107217303A
CN107217303A CN201710332494.7A CN201710332494A CN107217303A CN 107217303 A CN107217303 A CN 107217303A CN 201710332494 A CN201710332494 A CN 201710332494A CN 107217303 A CN107217303 A CN 107217303A
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pbi
substrate
micro wire
adjustable
perovskite
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史志锋
李森
李营
吉慧芳
李新建
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Zhengzhou University
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Zhengzhou University
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/54—Organic compounds
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution

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  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
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  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Catalysts (AREA)
  • Luminescent Compositions (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The present invention proposes a kind of adjustable CH of diameter3NH3PbI3The synthetic method of perovskite micro wire, solves the problem of production perovskite micro wire is relatively difficult in the prior art.The present invention is realized according to the following steps：Step（1）, cleaning substrate；Step（2）, prepare precursor solution；Step（3）, draw precursor solution and be added dropwise on substrate, and even application obtains sample；Step（4）, 30 ~ 60 ° of sample inclination is placed in sealing container and slowly dried, until substrate surface is covered with wire crystallization, and exist without liquid；Step（5）, take out crystallization after sample, made annealing treatment, obtain CH3NH3PbI3Perovskite micro wire.The present invention realizes one-dimensional CH at low ambient temperatures3NH3PbI3The controlledly synthesis of perovskite micro wire, technique is simple, with low cost, controllability strong, does not have dependence to substrate, and growth technique can be extended to CH3NH3PbBr3And CH3NH3PbCl3Deng material.

Description

The adjustable CH of diameter3NH3PbI3The synthetic method of perovskite micro wire
Technical field
The present invention relates to perovskite production field, particularly relate to that a kind of direction of growth is controllable, monodispersity is good, diameter is adjustable CH3NH3PbI3The synthetic method of perovskite micro wire.
Background technology
Nearly 2 years, hybrid perovskite material（CH3NH3PbX3, X=Cl/Br/I）In the latent of photodetection field Start to cause the extensive concern of people in application, this mainly has benefited from the larger absorption coefficient of light of the material, higher carrier The characteristic of transmission rate and its bandwidth continuously adjustabe.However, the photodetector based on perovskite material is in performance boost Bottleneck is encountered, the responsiveness of device is still relatively low.From the point of view of material, how to improve the crystallinity of material, ensure The continuity of material filming, reduces the defect that material internal is introduced because of crystal boundary, is to improve perovskite-based detector performance It is crucial.Meanwhile, the presence of a large amount of crystal boundaries also can substantially reduce the stability of material inside perovskite thin film, so as to have a strong impact on calcium The life-span of titanium ore detector in actual use.
Compared to the thin-film material of two dimension, the perovskite micro wire of one-dimentional structure has regular shape, structural integrity and knot The brilliant high advantage of degree, and material has low-down defect concentration in itself.Meanwhile, the direction of growth along perovskite micro wire With very high carrier mobility and diffusion length, this is very beneficial for the transmission of photo-generated carrier, to lifting photodetection The responsiveness and response speed of device are very favorable.Although, research of the existing part on one-dimensional perovskite material at present, More is to be confined to nanoscale, and is used more as luminescent material.In terms of one-dimensional perovskite micro wire, document " Aligned single-crystalline perovskite microwire arrays for high-performance flexible image sensors with long-term stability [J]. Adv. Mater. 28, 2201（2016）" report CH3NH3PbI3Application of the perovskite micro wire on photodetector, but because being limited to CH3NH3PbI3The poor crystallization of micro wire Degree and morphology controllable, the responsiveness of device is relatively low and the response time is longer.It is single from the point of view of device preparation The realization of the key indexs such as scattered, diameter micron dimension, length centimetres is lifting perovskite micro wire photodetection performance Key, therefore, development perovskite micro wire controlledly synthesis technology be device develop basis, its be successfully prepared also will for height Material foundation is established in the development of performance photodetector.
The content of the invention
The present invention proposes a kind of adjustable CH of diameter3NH3PbI3The synthetic method of perovskite micro wire, solves existing skill The problem of perovskite micro wire is relatively difficult is produced in art.
The technical proposal of the invention is realized in this way：A kind of direction of growth is controllable, monodispersity is good, diameter is adjustable CH3NH3PbI3The synthetic method of perovskite micro wire, is realized according to the following steps：
Step（1）, cleaning substrate；
Step（2）, by CH3NH3I and PbI2It is dissolved in dimethylformamide, compound concentration is 0.05 ~ 1.0 mol/L presoma Solution；
Step（3）, draw the μ L of precursor solution 10 ~ 30, dropwise addition obtained on cleaned substrate, and with slide even application Sample；
Step（4）, 30 ~ 60 ° of sample inclination is placed in sealing container and slowly dried, until substrate surface is covered with wire knot Crystalline substance, and exist without liquid；
Step（5）, take out crystallization after sample, be placed on warm table carry out 100 ~ 150 DEG C annealing, annealing time be 10 ~ 20 minutes, annealing atmosphere was high pure nitrogen, you can obtain CH3NH3PbI3Perovskite micro wire.
The step（4）It is room temperature condition.Or the step（4）30 DEG C are heated to sealing container
It is preferred that, step（1）Middle cleaning substrate is carried out in the following manner：By clean substrate successively in acetone, ethanol It is cleaned by ultrasonic 10 minutes with deionized water, is then dried up with high pure nitrogen.
It is preferred that, the step（1）Used in substrate be glass substrate, silicon substrate or Sapphire Substrate.
It is preferred that, step（2）Precursor solution in CH3NH3I and PbI2The ratio between the amount of material be 1:1.
The present invention utilizes simple solution phase methods, and one-dimensional CH is realized at low ambient temperatures3NH3PbI3Perovskite micro wire Controlledly synthesis.The preparation method technique is simple, with low cost, controllability strong, does not have dependence, and growth technique to substrate It can be extended to CH3NH3PbBr3And CH3NH3PbCl3Deng material.This is the photodetection for next carrying out one-dimensional perovskite micro wire Device development work has established material foundation.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing There is the accompanying drawing used required in technology description to be briefly described, it should be apparent that, drawings in the following description are only this Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can be with Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is CH in embodiment 13NH3PbI3The electron scanning micrograph of perovskite micro wire.
Fig. 2 is CH in embodiment 23NH3PbI3The electron scanning micrograph of perovskite micro wire.
Fig. 3 is CH in embodiment 33NH3PbI3The electron scanning micrograph of perovskite micro wire.
Fig. 4 is CH in embodiment 33NH3PbI3The X-ray diffractogram of perovskite micro wire.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.It is based on Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not paid Embodiment, belongs to the scope of protection of the invention.
A kind of direction of growth is controllable, monodispersity is good, the adjustable CH of diameter3NH3PbI3The synthesis side of perovskite micro wire Method, is realized according to the following steps：
Step（1）, cleaning substrate；Selected substrate is glass substrate, silicon substrate or Sapphire Substrate.
Step（2）, by CH3NH3I and PbI2It is dissolved in dimethylformamide, compound concentration is before 0.05 ~ 1.0 mol/L Drive liquid solution；Wherein, CH3NH3I and PbI2The ratio between the amount of material be 1:1 or so.
Step（3）, draw the μ L of precursor solution solution 10 ~ 30, be added dropwise on cleaned substrate, and uniform with slide Coating obtains sample；
Step（4）, 30 ~ 60 ° of sample inclination is placed in sealing container and slowly dried, until substrate surface is covered with wire knot Crystalline substance, and exist without liquid；
Step（5）, take out crystallization after sample, be placed on warm table carry out 100 ~ 150 DEG C annealing, annealing time be 10 ~ 20 minutes, annealing atmosphere was high pure nitrogen, you can obtain CH3NH3PbI3Perovskite micro wire.
It is preferred that, the step（4）Be room temperature condition or to sealing container heating be 30 DEG C, can be carried when heating Rise CH3NH3PbI3The crystalline rate of perovskite micro wire, improves its crystalline quality.
It is preferred that, step（1）Middle cleaning substrate is carried out in the following manner：By substrate successively acetone, ethanol and It is cleaned by ultrasonic 10 minutes in deionized water, is then dried up with high pure nitrogen.
The present invention realizes CH3NH3PbI3The height of perovskite micro wire is single scattered, and linear diameter is from micron dimension to receiving Rice continuously adjustabe, line length reaches the controllable preparation of centimetres so that for high performance calcium titanium ore micro wire photodetector and Material foundation is established in the development of solar cell.
Embodiment 1：Step（1）Substrate is cleaned, the substrate used is common glass substrate.
Using glass as substrate, Chemical cleaning is carried out, cleaning step is：First, cleaning agent is placed the substrate in（It is vertical Person who is not a member of any political party's liquid detergent）Middle immersion 15 minutes, then rinsed well with deionized water；Then, substrate is put in acetone, ethanol and gone It is each in ionized water to be cleaned by ultrasonic 10 minutes；After dried up through high pure nitrogen after it is standby.
Step（2）：Configure precursor solution.
First, 0.158 gram of CH is weighed respectively with high Accuracy Electronic Balance3NH3I（Aladdin boards）With 0.464 gram PbI2（Aladdin boards）Powder；Then the two mixing is dissolved in 3mL dimethyl formamide solution；Then magnetic agitation is used Device is stirred 24 hours at 65 DEG C；Treat that temperature is down to room temperature and obtains precursor solution, the precursor solution configured is positioned over In the glove box of nitrogen gas protection.
According to needs are actually prepared, precursor solution concentration changes between 0.05 ~ 1.0 mol/L, such as its concentration can Think 0.05,0.3,0.5,0.8 or 1.0 mol/L.Reduced with concentration, linear diameter reduction, line distribution density can decline.
（3）Application of reactive precursor solution.
The μ L of precursor solution 10 configured are drawn with accurate sampler in glove box, are added dropwise in glass substrate surface； And then, with the clean above-mentioned solution of slide even application, the speed of coating is 100 micro- meter per seconds.
（4）Sample is sealed, slowly dried.
The sample after coating is positioned in clean air-tight bottle, is nitrogen environment in bottle, it is ensured that the ambient humidity of surrounding For 20 ~ 25%；Treat 10 hours or so, the surface of sample exists without obvious liquid.
（5）Sample is made annealing treatment.
Sample is taken out from air-tight bottle, is placed on warm table and is made annealing treatment, the annealing process is in nitrogen gas Carried out in the glove box of body protection；It is 10 minutes that annealing temperature, which is set as 100 DEG C, made annealing treatment,.Finally give CH3NH3PbI3 Perovskite micro wire.
Fig. 1 is the CH prepared using embodiment 13NH3PbI3The electron scanning micrograph of perovskite micro wire, micron The length of line is about 0.5 centimetre, and diameter is about 4 microns.
Embodiment 2：Using commercial silicon chip as substrate, because polished silicon slice has higher surface smoothness, it can be lifted The nucleation and crystalline rate of precursor solution in liquid phase reaction course, are conducive to obtaining the bigger one-dimensional CH of yardstick3NH3PbI3Calcium Titanium ore micro wire.Fig. 2 is the CH prepared using embodiment 23NH3PbI3The electron scanning micrograph of perovskite micro wire, it is micro- The diameter of rice noodles is about 8 microns, and length is close to 1 centimetre.The present embodiment other modes be the same as Example 1.
Embodiment 3：This example and embodiment 1 except that, after sample is positioned over clean air-tight bottle, sealing is held Device is heated, and heating-up temperature is 30 DEG C, and this method is in lifting CH3NH3PbI3The crystalline rate of perovskite micro wire is same When, it can also improve its crystalline quality.The present embodiment other modes be the same as Example 1.
Fig. 3 is to use CH manufactured in the present embodiment3NH3PbI3The electron scanning micrograph of perovskite micro wire, wire body With smooth, even curface, the presence of no significant defect.Fig. 4 is CH manufactured in the present embodiment3NH3PbI3Perovskite micro wire X-ray diffraction test result, two obvious diffraction maximums correspond to Tetragonal perovskite respectively（110）With（220）Diffraction maximum, With the good orientation of growth and crystallinity.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention God is with principle, and any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.

Claims (5)

1. a kind of direction of growth is controllable, monodispersity is good, the adjustable CH of diameter3NH3PbI3The synthetic method of perovskite micro wire, It is characterized in that being realized according to the following steps：
Step（1）, cleaning substrate；
Step（2）, by CH3NH3I and PbI2It is dissolved in dimethylformamide, compound concentration is 0.05 ~ 1.0 mol/L presoma Solution；
Step（3）, draw the μ L of precursor solution 10 ~ 30, dropwise addition obtained on cleaned substrate, and with slide even application Sample；
Step（4）, 30 ~ 60 ° of sample inclination is placed in sealing container and slowly dried, until substrate surface is covered with wire knot Crystalline substance, and exist without liquid；
Step（5）, take out crystallization after sample, be placed on warm table carry out 100 ~ 150 DEG C annealing, annealing time be 10 ~ 20 minutes, annealing atmosphere was high pure nitrogen, you can obtain CH3NH3PbI3Perovskite micro wire.
2. a kind of direction of growth according to claim 1 is controllable, monodispersity is good, the adjustable CH of diameter3NH3PbI3Calcium titanium The synthetic method of ore deposit micro wire, it is characterised in that：The step（4）It is room temperature condition.
3. a kind of direction of growth according to claim 1 is controllable, monodispersity is good, the adjustable CH of diameter3NH3PbI3Calcium titanium The synthetic method of ore deposit micro wire, it is characterised in that：The step（4）30 DEG C are heated to sealing container
A kind of direction of growth according to claim 1 or 2 or 3 is controllable, monodispersity is good, the adjustable CH of diameter3NH3PbI3 The synthetic method of perovskite micro wire, it is characterised in that step（1）Middle cleaning substrate is carried out in the following manner：Will be clean Substrate successively in acetone, ethanol and deionized water be cleaned by ultrasonic 10 minutes, then dried up with high pure nitrogen.
4. a kind of direction of growth according to claim 1 or 2 or 3 is controllable, monodispersity is good, diameter is adjustable CH3NH3PbI3The synthetic method of perovskite micro wire, it is characterised in that the step（1）Used in substrate be glass substrate, Silicon substrate or Sapphire Substrate.
5. a kind of direction of growth according to claim 1 or 2 or 3 is controllable, monodispersity is good, diameter is adjustable CH3NH3PbI3The synthetic method of perovskite micro wire, it is characterised in that：Step（2）Precursor solution in CH3NH3I and PbI2 The ratio between the amount of material be 1:1.
CN201710332494.7A 2017-05-12 2017-05-12 The adjustable CH of diameter3NH3PbI3The synthetic method of perovskite micro wire Pending CN107217303A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108539026A (en) * 2018-05-03 2018-09-14 河南科技大学 A kind of preparation method of the perovskite thin film with micrometer tube array structure
CN108878573A (en) * 2018-06-29 2018-11-23 合肥工业大学 A kind of photodetector of driving certainly and preparation method thereof based on the quasi- one-dimentional structure of methylamino lead iodide
CN110670139A (en) * 2019-09-16 2020-01-10 吉林师范大学 Preparation method of organic-inorganic hybrid lead halide perovskite nanocrystalline
CN110699745A (en) * 2019-10-31 2020-01-17 东南大学 Preparation method of perovskite single crystal
CN112397649A (en) * 2020-11-11 2021-02-23 北京大学 Preparation method of large-area perovskite semiconductor single crystal film

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* Cited by examiner, † Cited by third party
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CN104916783A (en) * 2015-06-11 2015-09-16 华中科技大学 Preparation and application of perovskite nanowires, photoelectric detector and solar cell
CN105280820A (en) * 2015-07-09 2016-01-27 中南大学 Preparation method of large-area perovskite micro-nano wire array and application thereof
CN105624771A (en) * 2016-01-18 2016-06-01 长安大学 Method for preparing perovskite structure CH3NH3PbBr3 nano-wire
US20170047530A1 (en) * 2015-08-13 2017-02-16 Florida State University Research Foundation, Inc. Polymer-Perovskite Films, Devices, and Methods

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104916783A (en) * 2015-06-11 2015-09-16 华中科技大学 Preparation and application of perovskite nanowires, photoelectric detector and solar cell
CN105280820A (en) * 2015-07-09 2016-01-27 中南大学 Preparation method of large-area perovskite micro-nano wire array and application thereof
US20170047530A1 (en) * 2015-08-13 2017-02-16 Florida State University Research Foundation, Inc. Polymer-Perovskite Films, Devices, and Methods
CN105624771A (en) * 2016-01-18 2016-06-01 长安大学 Method for preparing perovskite structure CH3NH3PbBr3 nano-wire

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108539026A (en) * 2018-05-03 2018-09-14 河南科技大学 A kind of preparation method of the perovskite thin film with micrometer tube array structure
CN108539026B (en) * 2018-05-03 2021-06-25 河南科技大学 Preparation method of perovskite thin film with micron tube array structure
CN108878573A (en) * 2018-06-29 2018-11-23 合肥工业大学 A kind of photodetector of driving certainly and preparation method thereof based on the quasi- one-dimentional structure of methylamino lead iodide
CN110670139A (en) * 2019-09-16 2020-01-10 吉林师范大学 Preparation method of organic-inorganic hybrid lead halide perovskite nanocrystalline
CN110699745A (en) * 2019-10-31 2020-01-17 东南大学 Preparation method of perovskite single crystal
CN110699745B (en) * 2019-10-31 2021-08-06 东南大学 Preparation method of perovskite single crystal
CN112397649A (en) * 2020-11-11 2021-02-23 北京大学 Preparation method of large-area perovskite semiconductor single crystal film

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Application publication date: 20170929