CN107170890A - 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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CN107170890A
CN107170890A CN201710336423.4A CN201710336423A CN107170890A CN 107170890 A CN107170890 A CN 107170890A CN 201710336423 A CN201710336423 A CN 201710336423A CN 107170890 A CN107170890 A CN 107170890A
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nano wire
methylamine
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iodine
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CN107170890B (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.This method comprises the following steps：By the PbI that concentration is 0.167mol/L~0.271mol/L2Solution 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, iodate Pb Nanowires are obtained；Methylamine iodine powder is uniformly layered on culture dish, the parallel culture dish surface that is fixed on of spin coating back glass sheet is incubated 1.5 hours~2.5 hours in vacuum drying oven, obtains methylamine lead iodine nano wire at a distance of 0.8~1.1 centimeters with clip.Preparation technology of the present invention is simple, and cost is low；Prepare the CH of pure phase3NH3PbI3Nanowire length is dozens of micron even up to a hundred micron levels, it is possible to by changing PbI2DMF solution concentration and unit volume PbI2DMF solution in add 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 cell and field of photoelectric devices, it is related to a kind of organic inorganic hybridization perovskite structure first The preparation of amine lead iodine nano wire, belongs to technical field.
Background technology
In recent years, problem of energy crisis and environmental pollution were serious, promoted the material of perovskite structure and turned into study hotspot, Because its preparation technology is simple, excellent photoelectric properties so that methylamine lead iodine, methylamine lead bromine, methylamine lead chlorine and mixed type The research and application of perovskite structural material turn into upsurge.
At present, go out unconsciously about the preparation layer of methylamine lead iodine film, a step solwution method and two step solwution methods prepare methylamine Lead iodine film, or even the method for gas phase auxiliary liquid phase can also prepare methylamine lead iodine film, relevant methylamine lead iodine (CH3NH3PbI3) Preparing for nano wire is less, wherein the solvent of typically dissolving lead iodide is all organic solvent, is separated out herein using inorganic aqueous solvent The characteristics of lead iodide, prepares lead iodide (PbI2) nano wire, and prepare methylamine lead iodine nanometer using the method for gas evaporation Line.
The content of the invention
The purpose of the present invention is that provided herein is a kind of perovskite structure methylamine lead for defect of the prior art and deficiency The preparation method of iodine nano wire, and by changing PbI2The concentration of dimethylformamide (DMF) solution can obtain difference Length sum purpose PbI2Nano wire.This method is PbI using DMF2Good solvent, and water is PbI2Non-benign solvent, lead to Cross to PbI2DMF solution in add water, and then separate out from mixed solution PbI2Nano 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 add water amount to CH3NH3PbI3Nano wire carries out Effective Regulation.Preparation technology letter of the present invention Single, cost is low, is prepared available for large area, can apply to solar cell and field of photodetectors.
The technical scheme is that：
A kind of preparation method of controllable methylamine lead iodine nano wire, this method comprises the following steps：
The first step, configuration concentration is 0.167mol/L~0.271mol/L PbI2Solution, the solvent of solution is dimethyl Formamide；
Second step, by PbI2Solution is placed in container, and then temperature is stirring 0.5~0.75 hour at 70~80 DEG C；
3rd step, upward equipped with PbI2Deionized water, sealing and standing 10~11 hours are added in the container of solution；Its In, every milliliter of PbI2Solution adds 0.14~0.26 ml deionized water；
4th step, container of the upper step sealing after static is shaken, 2~5min is then stirred on magnetic stirrer, is obtained Dispersion liquid；
5th step, the dispersant liquid drop that upper step is obtained is added on the sheet glass after cleaning, is then placed on spin coating on spin coater 7s~15s, obtains iodate Pb Nanowires；Wherein, the μ L dispersion liquids of 100 μ L of dropwise addition every square centimeter~200；Spin coater rotating speed is 2000r/min~4000r/min；
6th step, methylamine iodine powder is uniformly layered on culture dish, and training is fixed on by spin coating back glass sheet is parallel with clip Support ware surface has PbI in 0.8~1.1 centimeters, sheet glass2One facing to methylamine iodine powder；Wherein, every square Centimetre paving spills 0.125g~0.5g methylamine iodine powder；
7th step, culture dish is placed on and has been warming up in 140 DEG C~160 DEG C of vacuum drying oven, keeps at this temperature 1.5 Hour~2.5 hours, obtain methylamine lead iodine nano wire.
In the preparation method of described methylamine lead iodine nano wire, obtained methylamine lead iodine nanowire length can be by PbI2 Solution concentration regulates and controls：Work as PbI2The concentration of DMF solution when increasing in the range of 0.167mol/L~0.271mol/L, and unit The PbI of volume2DMF solution add the volume of deionized water when increasing in the range of 0.14~0.26 times, obtained methylamine lead Iodine nanowire length shows in the range of 50um~300um successively decreases.
The cleaning of sheet glass in the 5th described step is sequentially passes through deionized water, and ethanol and acetone are cleaned.
The atmosphere of vacuum drying chamber in the 7th described step is nitrogen atmosphere.
Beneficial effects of the present invention are：
Preparation technology of the present invention is simple, and cost is low；Prepare the CH of pure phase3NH3PbI3Nanowire length is dozens of micron Even up to a hundred micron levels, and confirming by changing PbI2DMF solution concentration and the PbI of unit volume2Solution institute The amount of the deionized water of addition being capable of Effective Regulation CH3NH3PbI3The length and quantity of nano wire.Regulation and control can so be passed through CH3NH3PbI3The length of nano wire controls the transmission path of carrier, makes carrier be less likely to occur to be combined, can further increase Electric current, so as to applied to solar cell and field of photodetectors.
Brief description of the drawings
Fig. 1 is the XRD diffraction patterns of the methylamine lead iodine nano wire obtained in embodiment 1.
Fig. 2 is the SEM figures of the iodate Pb Nanowires obtained in embodiment 1.
Fig. 3 is the SEM figures of the methylamine lead iodine nano wire obtained in embodiment 1.
Fig. 4 is the XRD diffraction patterns of the methylamine lead iodine nano wire obtained in embodiment 2.
Fig. 5 is the SEM figures of the iodate Pb Nanowires obtained in embodiment 2.
Fig. 6 is the SEM figures of the methylamine lead iodine nano wire obtained in embodiment 2.
Fig. 7 is the XRD diffraction patterns of the methylamine lead iodine nano wire obtained in embodiment 3.
Fig. 8 is the SEM figures of the iodate Pb Nanowires obtained in embodiment 3.
Fig. 9 is the SEM figures of the methylamine lead iodine nano wire obtained in embodiment 3.
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, the PbI that configuration concentration is 0.271mol/L in screw socket bottle2Solution, solvent is DMF；
Second step, screw socket bottle sealing is placed in water-bath magnetic stirrer, temperature is 80 DEG C, the lower stirring 45min of insulation；
3rd step, the deionized water of 0.25 times of volume, sealing and standing 11 hours are added to above-mentioned solution；
4th step, firmly rocks the screw socket bottle equipped with above-mentioned solution, bottom precipitation is scattered in solution, in addition can be 2min is stirred on magnetic stirrer；
5th step, prepares 2cm*2cm clean sheet glass, is placed on spin coater by 600 μ L dispersant liquid drops on the glass sheet On, rotating speed is 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 soars glass sheet sample, to be fixed in culture dish, makes have PbI on sheet glass2That facing to 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；
7th step, the culture dish for filling sample is placed on and has been warming up in 150 DEG C of vacuum drying oven, and carries out taking out true Empty, inflated with nitrogen, is repeated twice, it is ensured that be nitrogen atmosphere in vacuum drying oven, pressure is 0.02MPa, keeps 2 small at this temperature afterwards When, obtain CH3NH3PbI3Nano wire.
Fig. 1 for pure phase methylamine lead iodine nano wire XRD diffraction patterns, it can be seen that the θ of diffraction maximum 2= Diffraction maximum at 14.28 °, 24.48 °, 28.35 °, 31.82 ° and 40.79 ° with methylamine lead iodine is corresponding, and spreading out without other materials Peak is penetrated, it is the methylamine lead iodine of pure phase to illustrate the methylamine lead iodine prepared.
Fig. 2 schemes for the SEM of iodate Pb Nanowires, it will be seen that the length of iodate Pb Nanowires reaches from figure 80um or so.The iodate Pb Nanowires that this method is prepared, are that the preparation of next step methylamine lead iodine nano wire provides the foundation.
Fig. 3 is prepares the SEM figures of methylamine lead iodine nano wire under the above method, it can be seen 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 adapted to prepare methylamine lead iodine nano wire.And contrasted by Fig. 2 and Fig. 3：Methylamine lead iodine is prepared in lead iodide During, the length of nano wire is basically unchanged.
Embodiment 2：Methylamine lead iodine nanowire size control process.
Embodiment 2 is from implementing unlike 1, and the concentration of lead iodide is different with the volume of deionized water.
The first step, the PbI that configuration concentration is 0.2169mol/L in screw socket bottle2Solution, solvent is DMF；
Second step, screw socket bottle sealing is placed in water-bath magnetic stirrer, temperature is 80 DEG C, the lower stirring 45min of insulation；
3rd step, the deionized water of 0.2 times of volume, sealing and standing 11 hours are added to above-mentioned solution；
4th step, firmly rocks the screw socket bottle equipped with above-mentioned solution, bottom precipitation is scattered in solution, in addition in magnetic force 2min is stirred on mixer；
5th step, prepares 2cm*2cm clean sheet glass, is placed on spin coater by 600 μ L dispersant liquid drops on the glass sheet On, rotating speed is 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 soars glass sheet sample, to be fixed in culture dish, makes have PbI on sheet glass2That facing to 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；
7th step, the culture dish for filling sample is placed on and has been warming up in 150 DEG C of vacuum drying oven, and carries out taking out true Empty, inflated with nitrogen, is repeated twice, it is ensured that be nitrogen atmosphere in vacuum drying oven, pressure is 0.02MPa, keeps 2 small at this temperature afterwards When, obtain CH3NH3PbI3Nano wire.
Fig. 4 for pure phase methylamine lead iodine nano wire XRD diffraction patterns, it can be seen that the θ of diffraction maximum 2= Diffraction maximum at 14.30 °, 24.38 °, 28.25 °, 31.72 ° and 40.80 ° with methylamine lead iodine is corresponding, and spreading out without other materials Peak is penetrated, illustrates that the methylamine lead iodine prepared is the methylamine lead iodine of pure phase, while illustrating that lead iodide and correspondence under above-mentioned concentration are added The amount of deionized water can prepare the methylamine lead iodine of pure phase.
Fig. 5 is the SEM figures of lead iodide under above-mentioned concentration, it can be seen that lead iodide nanowire length reaches 120um Left and right.By that can be obtained with Fig. 2 contrasts：The concentration of lead iodide and the iodate lead solution of unit volume add subtracting for the amount of deionized water Small, the nanowire length of lead iodide is elongated, illustrates iodate lead concentration and the PbI of unit volume2Solution adds the amount of deionized water The pattern of final iodate Pb Nanowires can be influenceed；In addition, PbI2Number significantly reduce.
Fig. 6 is the SEM figures of the methylamine lead iodine nano wire prepared under the above method, it can be seen that iodate lead concentration Reduce, methylamine lead iodine nanowire length reaches 120um or so, and is contrasted by Fig. 5 and Fig. 6：Methylamine is prepared 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 Liquid adds the reduction of the amount of deionized water, the nanowire length of lead iodide is elongated, illustrates the concentration and unit volume of lead iodide PbI2Solution adds the pattern of the change influence methylamine lead iodine nano wire of the amount of deionized water；In addition the number of methylamine lead iodine is also bright It is aobvious to reduce.
Embodiment 3：Methylamine lead iodine nanowire size control process.
Embodiment 3 is from implementing unlike 1, and the concentration of lead iodide is different with the volume of deionized water.
The first step, the configuration concentration 0.1808mol/L PbI in screw socket bottle2Solution, solvent is DMF；
Second step, screw socket bottle sealing is placed in water-bath magnetic stirrer, temperature is 80 DEG C, the lower stirring 45min of insulation；
3rd step, the deionized water of 0.167 times of volume, sealing and standing 11 hours are added to above-mentioned solution；
4th step, firmly rocks the screw socket bottle equipped with above-mentioned solution, bottom precipitation is scattered in solution, in addition in magnetic force 2min is stirred on mixer；
5th step, prepares 2cm*2cm clean sheet glass, is placed on spin coater by 600 μ L dispersant liquid drops on the glass sheet On, rotating speed is 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 soars glass sheet sample, to be fixed in culture dish, makes have PbI on sheet glass2That facing to 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；
7th step, the culture dish for filling sample is placed on and has been warming up in 150 DEG C of vacuum drying oven, and carries out taking out true Empty, inflated with nitrogen, is repeated twice, it is ensured that be nitrogen atmosphere in vacuum drying oven, pressure is 0.02MPa, keeps 2 small at this temperature afterwards When, obtain CH3NH3PbI3Nano wire.
Fig. 7 for pure phase methylamine lead iodine nano wire XRD diffraction patterns, it can be seen that the θ of diffraction maximum 2= Diffraction maximum at 14.30 °, 24.38 °, 28.25 °, 31.72 ° and 40.80 ° with methylamine lead iodine is corresponding, and spreading out without other materials Peak is penetrated, illustrates that the methylamine lead iodine prepared is the methylamine lead iodine of pure phase, while illustrating that lead iodide and correspondence under above-mentioned concentration are added The amount of deionized water can prepare the methylamine lead iodine of pure phase.
Fig. 8 is the SEM figures of lead iodide under above-mentioned concentration, it can be seen that lead iodide nanowire length reaches 200um Left and right.By that can be obtained with Fig. 5 contrasts：The amount that the concentration of lead iodide and the iodate lead solution of unit volume add deionized water reduces When, the nanowire length of lead iodide is elongated, illustrates that the iodate lead solution of iodate lead concentration and unit volume adds deionized water Amount can influence the pattern of final iodate Pb Nanowires；In addition, PbI2Number significantly reduce.
Fig. 9 is the SEM figures of the methylamine lead iodine nano wire prepared under the above method, it can be seen that iodate lead concentration When the amount for adding deionized water with the iodate lead solution of unit volume reduces, methylamine lead iodine nanowire length reaches 200um or so, And contrasted 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 be obtained:PbI2Concentration and unit volume PbI2When the amount that solution adds deionized water reduces, the nano wire of lead iodide Length, illustrates the change influence methylamine of the amount of deionized water added by the concentration of lead iodide and the iodate lead solution of unit volume The pattern of lead iodine nano wire；In addition, the number of methylamine lead iodine is also significantly reduced.
Embodiment 4
Other step be the same as Examples 1, difference concentration is changed to 0.167mol/L, deionized water volume by 0.271mol/L 0.154 times is changed to by 0.25 times.It with the naked eye can be observed there is a small amount of precipitation to produce in screw socket bottle, can under Olympus microscope It was observed that PbI2Nano wire.
Embodiment 5
Other step be the same as Examples 1, difference concentration is changed to 0.155mol/L, deionized water volume by 0.271mol/L 0.143 times is changed to by 0.25 times.It with the naked eye can be observed to produce without precipitation in screw socket bottle, show in Olympus receive under mirror in addition PbI is not observed2Nano wire.
Embodiment 6
Other step be the same as Examples 1, difference concentration is changed to 0.282mol/L, deionized water volume by 0.271mol/L 0.26 times is changed to by 0.25 times.It is with the naked eye considerable to clip when adding deionized water in the DMF solution to lead iodide, have big at once Amount precipitation is produced, and deposit buildup is together.Show in addition in Olympus and receive Microscopic observation 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 to add deionized water volume2DMF solution volume when, according to above step operation can obtain PbI2Nano wire and with the increase of the amount of deionized water added by concentration and unit liquor capacity, it is observed that in solution The precipitation capacity increase of the iodate Pb Nanowires of precipitation, can be observed under mirror in Olympus aobvious receive：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 deionized water volume, when being 0.154 times of liquor capacity, nanowire length is 230um or so；When concentration is increased 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 deionized water volume, when being 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 deionized water volume, when being 0.25 times of liquor capacity, the length of nano wire is decreased to 80um or so.So drawing summing-up rule：PbI2DMF solution concentration be 0.167mol/L~0.271mol/L, and add It is 0.14~0.26 times of PbI to enter deionized water volume2DMF 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 shows decline trend, length model Enclose substantially between 50um~300um.Because 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 add 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, above institute Only presently preferred embodiments of the present invention is stated, is not intended to limit the invention, within the spirit and principles of the invention institute Any modifications, equivalent substitutions and improvements made etc., should be included in the scope of the protection.
Unaccomplished matter of the present invention is known technology.

Claims (4)

1. a kind of preparation method of controllable methylamine lead iodine nano wire, it is characterized in that this method comprises the following steps：
The first step, configuration concentration is 0.167mol/L~0.271mol/L PbI2Solution, the solvent of solution is dimethyl formyl Amine；
Second step, by PbI2Solution is placed in container, and then temperature is stirring 0.5~0.75 hour at 70~80 DEG C；
3rd step, upward equipped with PbI2Deionized water, sealing and standing 10~11 hours are added in the container of solution；Wherein, per milli Rise PbI2Solution adds 0.14~0.26 ml deionized water；
4th step, container of the upper step sealing after static is shaken, 2~5min is then stirred on magnetic stirrer, is disperseed Liquid；
5th step, the dispersant liquid drop that upper step is obtained 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 μ L dispersion liquids of 100 μ L of dropwise addition every square centimeter~200；Spin coater rotating speed is 2000r/ Min~4000r/min；
6th step, methylamine iodine powder is uniformly layered on culture dish, and culture dish is fixed on by spin coating back glass sheet is parallel with clip There is PbI surface in 0.8~1.1 centimeters, sheet glass2One facing to methylamine iodine powder；Wherein, it is every square centimeter Paving spills 0.125g~0.5g methylamine iodine powder；
7th step, culture dish is placed on and has been warming up in 140 DEG C~160 DEG C of vacuum drying oven, 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 claimed in claim 1, it is characterized in that described methylamine lead iodine is received In the preparation method of rice noodles, obtained methylamine lead iodine nanowire length can be by PbI2Solution concentration regulates and controls：Work as PbI2DMF The concentration of solution increases in the range of 0.167mol/L~0.271mol/L, and the PbI of unit volume2DMF solution add go When the volume of ionized water increases in the range of 0.14~0.26 times, obtained methylamine lead iodine nanowire length is in 50um~300um In the range of show and successively decrease.
3. the preparation method of controllable methylamine lead iodine nano wire as claimed in claim 1, it is characterized in that in the 5th described step The cleaning of sheet glass is sequentially passes through deionized water, and ethanol and acetone are cleaned.
4. the preparation method of controllable methylamine lead iodine nano wire as claimed in claim 1, it is characterized in that in the 7th described step The atmosphere of vacuum drying chamber is nitrogen atmosphere.
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