CN107170890B - A kind of preparation method of controllable methylamine lead iodine nano wire - Google Patents

A kind of preparation method of controllable methylamine lead iodine nano wire Download PDF

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CN107170890B
CN107170890B CN201710336423.4A CN201710336423A CN107170890B CN 107170890 B CN107170890 B CN 107170890B CN 201710336423 A CN201710336423 A CN 201710336423A CN 107170890 B CN107170890 B CN 107170890B
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iodine
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CN107170890A (en
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樊鹏凯
张新
任刚
陈秋颖
刘辉
郝秋艳
刘彩池
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Hebei University of Technology
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Abstract

The present invention is a kind of preparation method of controllable methylamine lead iodine nano wire.Method includes the following steps: the PbI for being 0.167mol/L~0.271mol/L by concentration2Solution is placed in container, and stirring is fitted with PbI backward2Deionized water is added in the container of solution, spin coating on sheet glass is then added dropwise, obtains iodate Pb Nanowires；Methylamine iodine powder is uniformly layered on culture dish, with clip spin coating back glass sheet culture dish surface is fixed at a distance of 0.8~1.1 centimeters in parallel, keeps the temperature 1.5 hours~2.5 hours in vacuum drying oven, obtain methylamine lead iodine nano wire.Preparation process of the present invention is simple, at low cost；Prepare the CH of pure phase3NH3PbI3Nanowire length is dozens of micron even a micron levels up to a hundred, and can be by changing PbI2DMF solution concentration and unit volume PbI2DMF solution in be added water amount being capable of Effective Regulation CH3NH3PbI3The length and quantity of nano wire.

Description

A kind of preparation method of controllable methylamine lead iodine nano wire
Technical field
The invention belongs to solar battery and field of photoelectric devices, are related to a kind of organic inorganic hybridization perovskite structure first The preparation of amine lead iodine nano wire, belongs to technical field.
Background technique
In recent years, problem of energy crisis and environmental pollution is serious promotes the material of perovskite structure to become research hotspot, Due to simple, the excellent photoelectric properties of its preparation process, so that methylamine lead iodine, methylamine lead bromine, methylamine lead chlorine and mixed type The research and application of perovskite structural material become upsurge.
Currently, the preparation layer in relation to methylamine lead iodine film goes out unconsciously, a step solwution method and two step solwution methods prepare methylamine The method of lead iodine film or even gas phase auxiliary liquid phase can also prepare methylamine lead iodine film, related methylamine lead iodine (CH3NH3PbI3) Preparing for nano wire is less, wherein the solvent of generally dissolution lead iodide is all organic solvent, is precipitated herein using inorganic aqueous solvent The characteristics of lead iodide, prepares lead iodide (PbI2) nano wire, and methylamine lead iodine nanometer is prepared using the method for gas evaporation Line.
Summary of the invention
It is an object of the present invention to for the defects in the prior art and insufficient, provided herein is a kind of perovskite structure methylamine lead The preparation method of iodine nano wire, and by changing PbI2Dimethylformamide (DMF) solution the available difference of concentration Length sum number purpose PbI2Nano wire.This method is PbI using DMF2Good solvent, and water is PbI2Non-benign solvent, lead to It crosses to PbI2DMF solution in water is added, and then PbI is precipitated from mixed solution2Nano wire, by evaporating methylamine iodine (CH3NH3I) method of powder prepares CH3NH3PbI3Nano wire, and can be by changing PbI2DMF solution concentration and list The PbI of position volume2DMF solution be added water amount to CH3NH3PbI3Nano wire carries out Effective Regulation.Preparation process letter of the present invention It is single, it is at low cost, it can be used for large area preparation, can be applied to solar battery and field of photodetectors.
The technical solution of the present invention is as follows:
A kind of preparation method of controllable methylamine lead iodine nano wire, method includes the following steps:
The first step, configuration concentration are the PbI of 0.167mol/L~0.271mol/L2Solution, the solvent of solution are dimethyl Formamide；
Second step, by PbI2Solution is placed in container, and then temperature is to stir 0.5~0.75 hour at 70~80 DEG C；
Third step is upward equipped with PbI2It is added deionized water in the container of solution, sealing and standing 10~11 hours；Its In, every milliliter of PbI2Solution adds 0.14~0.26 ml deionized water；
4th step, by upper step seal it is static after container shake, then on magnetic stirrer stir 2~5min, obtain Dispersion liquid；
The dispersant liquid drop that upper step obtains is added on the sheet glass after cleaning, is then placed on spin coating on spin coater by the 5th step 7s~15s obtains iodate Pb Nanowires；Wherein, the 100 μ L dispersion liquids of μ L~200 of dropwise addition every square centimeter；Spin coater revolving speed is 2000r/min~4000r/min；
Methylamine iodine powder is uniformly layered on culture dish by the 6th step, and spin coating back glass sheet is fixed on training in parallel with clip Supporting ware surface has PbI in 0.8~1.1 centimeters, sheet glass2One facing towards methylamine iodine powder；Wherein, every square Centimetre paving spills 0.125g~0.5g methylamine iodine powder；
Culture dish is placed in the vacuum drying oven for being warming up to 140 DEG C~160 DEG C by the 7th step, keeps at this temperature 1.5 Hour~2.5 hours, obtain methylamine lead iodine nano wire.
In the preparation method of the methylamine lead iodine nano wire, obtained methylamine lead iodine nanowire length can pass through PbI2 Solution concentration regulation: work as PbI2The concentration of DMF solution when increasing within the scope of 0.167mol/L~0.271mol/L, and unit The PbI of volume2DMF solution volume when increasing within the scope of 0.14~0.26 times that deionized water is added, obtained methylamine lead Iodine nanowire length shows within the scope of 50um~300um successively decreases.
The cleaning of sheet glass in 5th step is successively to pass through deionized water, ethyl alcohol and acetone cleaning.
The atmosphere of vacuum oven in 7th step is nitrogen atmosphere.
The invention has the benefit that
Preparation process of the present invention is simple, at low cost；Prepare the CH of pure phase3NH3PbI3Nanowire length is dozens of micron Even a micron levels up to a hundred, and confirm by changing PbI2DMF solution concentration and unit volume PbI2Solution institute The amount of the deionized water of addition being capable of Effective Regulation CH3NH3PbI3The length and quantity of nano wire.Regulation can be passed through in this way CH3NH3PbI3The transmission path of the length control carrier of nano wire, carrier is less likely to occur compound, can further increase Electric current, so as to be applied to solar battery and field of photodetectors.
Detailed description of the invention
Fig. 1 is the XRD diffraction pattern of methylamine lead iodine nano wire obtained in embodiment 1.
Fig. 2 is the SEM figure of iodate Pb Nanowires obtained in embodiment 1.
Fig. 3 is the SEM figure of methylamine lead iodine nano wire obtained in embodiment 1.
Fig. 4 is the XRD diffraction pattern of methylamine lead iodine nano wire obtained in embodiment 2.
Fig. 5 is the SEM figure of iodate Pb Nanowires obtained in embodiment 2.
Fig. 6 is the SEM figure of methylamine lead iodine nano wire obtained in embodiment 2.
Fig. 7 is the XRD diffraction pattern of methylamine lead iodine nano wire obtained in embodiment 3.
Fig. 8 is the SEM figure of iodate Pb Nanowires obtained in embodiment 3.
Fig. 9 is the SEM figure of methylamine lead iodine nano wire obtained in embodiment 3.
Specific embodiment
Below in conjunction with the drawings and specific embodiments, the present invention will be described in detail:
Embodiment 1: the preparation process of pure phase methylamine lead iodine nano wire
The first step, configuration concentration is the PbI of 0.271mol/L in screw socket bottle2Solution, solvent DMF；
The sealing of screw socket bottle is placed in water-bath magnetic stirrer by second step, and temperature is 80 DEG C, keeps the temperature lower stirring 45min；
Third step, the deionized water of Xiang Shangshu solution 0.25 times of volume of addition, sealing and standing 11 hours；
4th step firmly shakes the screw socket bottle that above-mentioned solution is housed, is scattered in bottom precipitation in solution, in addition can be 2min is stirred on magnetic stirrer；
5th step prepares the clean sheet glass of 2cm*2cm, on the glass sheet by 600 μ L dispersant liquid drops, is placed on spin coater On, revolving speed 4000r/min rotates 10s, obtains PbI2Nano wire；
6th step, by 1.5gCH3NH3I powder is uniformly layered on clean culture dish, and extravagant area is 5cm2, with double The clip of face glue, which empties glass sheet sample, to be fixed in culture dish, makes have PbI on sheet glass2That facing towards CH3NH3I, and Guarantee is parallel with culture dish bottom not to be contacted, and keep at a distance general 1cm or so, and is covered on above with larger culture dish；
The culture dish for filling sample is placed in the vacuum drying oven for being warming up to 150 DEG C by the 7th step, and take out true Empty, inflated with nitrogen, is repeated twice, and guarantees to be nitrogen atmosphere in vacuum drying oven, pressure 0.02MPa, keeps 2 small at this temperature later When, obtain CH3NH3PbI3Nano wire.
Fig. 1 be pure phase methylamine lead iodine nano wire XRD diffraction pattern, it can be seen from the figure that 2 θ of diffraction maximum= It is corresponding with the diffraction maximum of methylamine lead iodine at 14.28 °, 24.48 °, 28.35 °, 31.82 ° and 40.79 °, and spreading out without other substances Peak is penetrated, illustrates that the methylamine lead iodine of preparation is the methylamine lead iodine of pure phase.
Fig. 2 is the SEM figure of iodate Pb Nanowires, from the figure we can see that, the length of iodate Pb Nanowires reaches 80um or so.The iodate Pb Nanowires that this method is prepared provide the foundation for the preparation of next step methylamine lead iodine nano wire.
Fig. 3 is the SEM figure that methylamine lead iodine nano wire is prepared under the above method, it can be seen from the figure that methylamine lead iodine nanometer The length of line can reach 80um or so.Iodate Pb Nanowires can be converted into methylamine lead iodine nano wire by the above method, Illustrate that the method is suitble to prepare methylamine lead iodine nano wire.And compared by Fig. 2 and Fig. 3: preparing methylamine lead iodine in lead iodide During, the length of nano wire is basically unchanged.
Embodiment 2: methylamine lead iodine nanowire size control process.
For embodiment 2 unlike implementation 1, the concentration of lead iodide and the volume of deionized water are different.
The first step, configuration concentration is the PbI of 0.2169mol/L in screw socket bottle2Solution, solvent DMF；
The sealing of screw socket bottle is placed in water-bath magnetic stirrer by second step, and temperature is 80 DEG C, keeps the temperature lower stirring 45min；
Third step, the deionized water of Xiang Shangshu solution 0.2 times of volume of addition, sealing and standing 11 hours；
4th step firmly shakes the screw socket bottle that above-mentioned solution is housed, is scattered in bottom precipitation in solution, in addition in magnetic force 2min is stirred on blender；
5th step prepares the clean sheet glass of 2cm*2cm, on the glass sheet by 600 μ L dispersant liquid drops, is placed on spin coater On, revolving speed 4000r/min rotates 10s, obtains PbI2Nano wire；
6th step, by 1.5gCH3NH3I powder is uniformly layered on clean culture dish, and extravagant area is 5cm2, with double The clip of face glue, which empties glass sheet sample, to be fixed in culture dish, makes have PbI on sheet glass2That facing towards CH3NH3I, and Guarantee is parallel with culture dish bottom not to be contacted, and keep at a distance general 1cm or so, and is covered on above with larger culture dish；
The culture dish for filling sample is placed in the vacuum drying oven for being warming up to 150 DEG C by the 7th step, and take out true Empty, inflated with nitrogen, is repeated twice, and guarantees to be nitrogen atmosphere in vacuum drying oven, pressure 0.02MPa, keeps 2 small at this temperature later When, obtain CH3NH3PbI3Nano wire.
Fig. 4 be pure phase methylamine lead iodine nano wire XRD diffraction pattern, it can be seen from the figure that 2 θ of diffraction maximum= It is corresponding with the diffraction maximum of methylamine lead iodine at 14.30 °, 24.38 °, 28.25 °, 31.72 ° and 40.80 °, and spreading out without other substances Peak is penetrated, illustrates that the methylamine lead iodine of preparation is the methylamine lead iodine of pure phase, while illustrating the lead iodide under above-mentioned concentration and corresponding addition The amount of deionized water can prepare the methylamine lead iodine of pure phase.
Fig. 5 is the SEM figure of lead iodide under above-mentioned concentration, it can be seen from the figure that lead iodide nanowire length reaches 120um Left and right.By that can obtain with Fig. 2 comparison: the amount of the iodate lead solution addition deionized water of the concentration and unit volume of lead iodide subtracts Small, the nanowire length of lead iodide is elongated, illustrates the PbI of iodate lead concentration and unit volume2The amount of solution addition deionized water It can influence the pattern of final iodate Pb Nanowires；In addition, PbI2Number significantly reduce.
Fig. 6 is the SEM figure of the methylamine lead iodine nano wire prepared under the above method, it can be seen from the figure that iodate lead concentration Reduce, methylamine lead iodine nanowire length reaches 120um or so, and is compared by Fig. 5 and Fig. 6: preparing methylamine in lead iodide During lead iodine, the length of nano wire is basically unchanged.It can be obtained by comparison diagram 3: PbI2Concentration and unit volume PbI2It is molten The reduction of the amount of deionized water is added in liquid, and the nanowire length of lead iodide is elongated, illustrates the concentration and unit volume of lead iodide PbI2The variation that the amount of deionized water is added in solution influences the pattern of methylamine lead iodine nano wire；Furthermore the number of methylamine lead iodine is also bright It is aobvious to reduce.
Embodiment 3: methylamine lead iodine nanowire size control process.
For embodiment 3 unlike implementation 1, the concentration of lead iodide and the volume of deionized water are different.
The first step, the PbI of configuration concentration 0.1808mol/L in screw socket bottle2Solution, solvent DMF；
The sealing of screw socket bottle is placed in water-bath magnetic stirrer by second step, and temperature is 80 DEG C, keeps the temperature lower stirring 45min；
Third step, the deionized water of Xiang Shangshu solution 0.167 times of volume of addition, sealing and standing 11 hours；
4th step firmly shakes the screw socket bottle that above-mentioned solution is housed, is scattered in bottom precipitation in solution, in addition in magnetic force 2min is stirred on blender；
5th step prepares the clean sheet glass of 2cm*2cm, on the glass sheet by 600 μ L dispersant liquid drops, is placed on spin coater On, revolving speed 4000r/min rotates 10s, obtains PbI2Nano wire；
6th step, by 1.5gCH3NH3I powder is uniformly layered on clean culture dish, and extravagant area is 5cm2, with double The clip of face glue, which empties glass sheet sample, to be fixed in culture dish, makes have PbI on sheet glass2That facing towards CH3NH3I, and Guarantee is parallel with culture dish bottom not to be contacted, and keep at a distance general 1cm or so, and is covered on above with larger culture dish；
The culture dish for filling sample is placed in the vacuum drying oven for being warming up to 150 DEG C by the 7th step, and take out true Empty, inflated with nitrogen, is repeated twice, and guarantees to be nitrogen atmosphere in vacuum drying oven, pressure 0.02MPa, keeps 2 small at this temperature later When, obtain CH3NH3PbI3Nano wire.
Fig. 7 be pure phase methylamine lead iodine nano wire XRD diffraction pattern, it can be seen from the figure that 2 θ of diffraction maximum= It is corresponding with the diffraction maximum of methylamine lead iodine at 14.30 °, 24.38 °, 28.25 °, 31.72 ° and 40.80 °, and spreading out without other substances Peak is penetrated, illustrates that the methylamine lead iodine of preparation is the methylamine lead iodine of pure phase, while illustrating the lead iodide under above-mentioned concentration and corresponding addition The amount of deionized water can prepare the methylamine lead iodine of pure phase.
Fig. 8 is the SEM figure of lead iodide under above-mentioned concentration, it can be seen from the figure that lead iodide nanowire length reaches 200um Left and right.By that can obtain with Fig. 5 comparison: the amount of the iodate lead solution addition deionized water of the concentration and unit volume of lead iodide reduces When, the nanowire length of lead iodide is elongated, illustrates that deionized water is added in the iodate lead solution of iodate lead concentration and unit volume Amount can influence the pattern of final iodate Pb Nanowires；In addition, PbI2Number significantly reduce.
Fig. 9 is the SEM figure of the methylamine lead iodine nano wire prepared under the above method, it can be seen from the figure that iodate lead concentration When the amount that deionized water is added with the iodate lead solution of unit volume reduces, methylamine lead iodine nanowire length reaches 200um or so, And compared by Fig. 8 and Fig. 9: during lead iodide prepares methylamine lead iodine, the length of nano wire is basically unchanged.Pass through Comparison diagram 6 can obtain: PbI2Concentration and unit volume PbI2When the amount that deionized water is added in solution reduces, the nano wire of lead iodide Length illustrates that the variation of the amount of deionized water added by the concentration of lead iodide and the iodate lead solution of unit volume influences methylamine The pattern of lead iodine nano wire；In addition, the number of methylamine lead iodine also significantly reduces.
Embodiment 4
Other steps are changed to 0.167mol/L, deionized water volume by 0.271mol/L with embodiment 1, difference concentration 0.154 times is changed to by 0.25 times.It with the naked eye can be observed there is a small amount of precipitating to generate in screw socket bottle, it can under Olympus microscope Observe PbI2Nano wire.
Embodiment 5
Other steps are changed to 0.155mol/L, deionized water volume by 0.271mol/L with embodiment 1, difference concentration 0.143 times is changed to by 0.25 times.It with the naked eye can be observed to generate in screw socket bottle without precipitating, in addition show and received under mirror in Olympus PbI is not observed2Nano wire.
Embodiment 6
Other steps are changed to 0.282mol/L, deionized water volume by 0.271mol/L with embodiment 1, difference concentration 0.26 times is changed to by 0.25 times.It is with the naked eye considerable to clip when deionized water is added in the DMF solution to lead iodide, have at once big Amount precipitating generates, and deposit buildup is together.In addition in the aobvious microscopic observation of receiving of Olympus less than PbI2Nano wire.
It can be seen from above-described embodiment that working as PbI2DMF solution concentration be 0.167mol/L~0.271mol/L, And it is 0.14~0.26 times of PbI that deionized water volume, which is added,2DMF solution volume when, according to above step operate it is available PbI2The increase of nano wire and the amount with deionized water added by concentration and unit liquor capacity, it can be observed that in solution The precipitation capacity of the iodate Pb Nanowires of precipitation increases, and can observe in the case where Olympus shows and receives mirror: when concentration is 0.155mol/ L, and deionized water volume be 0.143 times of liquor capacity when, without PbI2Nano wire is formed；When concentration increases to 0.167mol/ L, and when deionized water volume is 0.154 times of liquor capacity, nanowire length is 230um or so；When concentration increases to 0.1808mol/L, and deionized water volume be 0.167 times of liquor capacity when, nanowire length reduces to 200um or so；Work as concentration Increase to 0.2169mol/L, and when deionized water volume is 0.2 times of liquor capacity, nanowire length reduces to 120um or so；It is dense Degree continues to increase to 0.271mol/L, and when deionized water volume is 0.25 times of liquor capacity, the length of nano wire is decreased to 80um or so.So obtaining summing-up rule: PbI2DMF solution concentration be 0.167mol/L~0.271mol/L, and add Entering deionized water volume is 0.14~0.26 times of PbI2DMF solution volume when, with PbI2DMF solution concentration and unit it is molten The increase of the amount for the deionized water that liquid product is added, the length of iodate Pb Nanowires generally show decline trend, length model It encloses substantially between 50um~300um.Since obtained methylamine lead iodine nano wire is directly to be transformed by iodate Pb Nanowires, Therefore the length and PbI of methylamine lead iodine nano wire2DMF solution concentration and unit volume iodate lead solution be added deionized water The relation character of amount close and state summary.
As it will be easily appreciated by one skilled in the art that those of ordinary skill in the art can implement to specifications, the above institute Only presently preferred embodiments of the present invention is stated, is not intended to limit the invention, all within the spirits and principles of the present invention institute Any modifications, equivalent replacements, and improvements etc. of work, should all be included in the protection scope of the present invention.
Unaccomplished matter of the present invention is well-known technique.

Claims (4)

1. a kind of preparation method of controllable methylamine lead iodine nano wire, it is characterized in that method includes the following steps:
The first step, configuration concentration are the PbI of 0.167mol/L~0.271mol/L2Solution, the solvent of solution are dimethyl formyl Amine；
Second step, by PbI2Solution is placed in container, and then temperature is to stir 0.5~0.75 hour at 70~80 DEG C；
Third step is upward equipped with PbI2It is added deionized water in the container of solution, sealing and standing 10~11 hours；Wherein, every milli Rise PbI2Solution adds 0.14~0.26 ml deionized water；
4th step shakes the container after upper step sealing and standing, and 2~5min is then stirred on magnetic stirrer, is dispersed Liquid；
5th step, by the dispersant liquid drop that upper step obtains be added to cleaning after sheet glass on, be then placed on spin coating 7s on spin coater~ 15s obtains iodate Pb Nanowires；Wherein, the 100 μ L dispersion liquids of μ L~200 of dropwise addition every square centimeter；Spin coater revolving speed is 2000r/ Min~4000r/min；
Methylamine iodine powder is uniformly layered on culture dish by the 6th step, and spin coating back glass sheet is fixed on culture dish in parallel with clip There is PbI in surface in 0.8~1.1 centimeters, sheet glass2One facing towards methylamine iodine powder；Wherein, every square centimeter Paving spills 0.125g~0.5g methylamine iodine powder；
Culture dish is placed in the vacuum drying oven for being warming up to 140 DEG C~160 DEG C by the 7th step, is kept for 1.5 hours at this temperature ~2.5 hours, obtain methylamine lead iodine nano wire.
2. the preparation method of controllable methylamine lead iodine nano wire as described in claim 1, it is characterized in that the methylamine lead iodine is received In the preparation method of rice noodles, obtained methylamine lead iodine nanowire length can pass through PbI2Solution concentration regulation: work as PbI2DMF The concentration of solution increases within the scope of 0.167mol/L~0.271mol/L, and the PbI of unit volume2DMF solution addition go When the volume of ionized water increases within the scope of 0.14~0.26 times, obtained methylamine lead iodine nanowire length is in 50um~300um It shows and successively decreases in range.
3. the preparation method of controllable methylamine lead iodine nano wire as described in claim 1, it is characterized in that in the 5th step The cleaning of sheet glass is successively to pass through deionized water, ethyl alcohol and acetone cleaning.
4. the preparation method of controllable methylamine lead iodine nano wire as described in claim 1, it is characterized in that in the 7th step The atmosphere of vacuum oven is nitrogen atmosphere.
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