CN110194768A - The method that anti-solvent saturation vapor pressure method prepares high-sequential acid imide nano wire - Google Patents

The method that anti-solvent saturation vapor pressure method prepares high-sequential acid imide nano wire Download PDF

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Publication number
CN110194768A
CN110194768A CN201910491795.3A CN201910491795A CN110194768A CN 110194768 A CN110194768 A CN 110194768A CN 201910491795 A CN201910491795 A CN 201910491795A CN 110194768 A CN110194768 A CN 110194768A
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pdi
solvent
nano wire
vapor pressure
acid imide
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徐伟龙
郑敏
秦天
卞维柏
熊超
赵宇
陈海悦
陈磊
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Changzhou Institute of Technology
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Changzhou Institute of Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D471/00Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, at least one ring being a six-membered ring with one nitrogen atom, not provided for by groups C07D451/00 - C07D463/00
    • C07D471/02Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, at least one ring being a six-membered ring with one nitrogen atom, not provided for by groups C07D451/00 - C07D463/00 in which the condensed system contains two hetero rings
    • C07D471/06Peri-condensed systems

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention discloses a kind of method that anti-solvent saturation vapor pressure method prepares high-sequential acid imide (PDI) nano wire, include the following steps: 1) to dissolve PDI in a solvent;2) PDI solution is added dropwise on substrate, is subsequently placed in saturation anti-solvent acetonitrile (CAN) atmosphere;3) the self assembly effect for passing through molecule on substrate, forms the one-dimensional PDI nano wire of high-sequential.The present invention realizes PDI nanowire height ordering growth.PDI is dissolved in dichloro benzene solvent by the present invention, is then added dropwise on substrate, then as in saturation anti-solvent atmosphere, is finally passed through the self assembly effect of molecule on substrate, is formed the one-dimensional PDI nano wire of high-sequential.The present invention realizes the one-dimensional orderly homoepitaxial of PDI molecule, and shows good crystallization property.

Description

The method that anti-solvent saturation vapor pressure method prepares high-sequential acid imide nano wire
Technical field
The present invention relates to a kind of methods for preparing high-sequential acid imide nano wire, belong to photoelectric material and device technology Field.
Background technique
In recent years, acid imide (PDI) because its thermostabilization and chemical stability it is good, it is cheap, high absorption efficiency and The features such as electron mobility, keeps it with important application prospects in organic electronic and opto-electronic device.However, PDI is easy to lead to The interaction for crossing pi-pi bond forms aggregation, is unfavorable for exciton dissociation in this way, while will increase non-bimolecular recombination losses, makes It is reduced at fluorescence efficiency.Monodimension nanometer material has big interfacial area, low defect state density can compared with thin-film material To realize the improvement of device performance and the diminution of size.During synthesizing PDI nano wire, need in dissolubility and molecular stacks Mode obtains balance, and the interaction of solvent and molecule equally will limit molecular self-assembling.It can using anti-solvent and steam annealing It to prepare one-dimensional PDI, however, nano wire is all usually distortion, mutually covers, this applies PDI in electronic device is Unfavorable.
The orderly PDI nano wire preparation of present level has the following problems:
(1) the intermolecular pi-pi bond of PDI stacks stronger, so that PDI is easy aggregation and forms cluster;
(2) when introducing other groups in PDI molecular structure, intermolecular interaction weakens, but is unfavorable for its ordered arrangement;
It (3) is usually to distort using PDI nano wire prepared by anti-solvent method and steam annealing method, this is to it in electronics device It is unfavorable for applying in part;
(4) high-sequential PDI nano wire Forming Mechanism is probed into relatively fewer.
In order to adapt to opto-electronic device fast development needs, research and development high-sequential PDI nano wire is particularly significant.
Summary of the invention
For the above-mentioned problems in the prior art, the present invention provides a kind of anti-solvent saturation vapor pressure method preparation height The method of orderly acid imide nano wire.
The present invention adopts the following technical scheme:
The method that anti-solvent saturation vapor pressure method prepares high-sequential acid imide nano wire, includes the following steps:
1) in a solvent by PDI dissolution;
2) PDI solution is added dropwise on substrate, is subsequently placed in saturation anti-solvent atmosphere;
3) the self assembly effect for passing through molecule on substrate, forms the one-dimensional PDI nano wire of high-sequential.
Further, the concentration of the PDI solution is 5 mg/mls.
Further, the solvent is dichloro-benzenes;The saturation anti-solvent is saturation acetonitrile steam.
Further, keep entire atmosphere closed in the step 3), stand.
Further, the purity of the PDI is greater than 98%.Further, the substrate material is silicon, and selection has The interdigital electrode of gold electrode, for depositing PDI nano wire, tests i-v curve as substrate.
Further, it at 24 hours, 48 hours, 72 hours and 96 hours, is taken from saturated vapor pressure atmosphere respectively Sample is observed out.
PDI nano wire prepared by the present invention has the following beneficial effects: compared with other techniques
(1) solution processing technology is used, method is simple, and parameter is easy to control;
(2) PDI nanowire structure is regular, and crystalline quality is high;
(3) electronics is easy to accomplish to go delocalized and migration in PDI nano wire one-dimensional square;
(4) long PDI nano wire and high current module be utilized it can in nano-device.
Detailed description of the invention
Fig. 1 is the molecular schematic diagram of PDI.
Fig. 2 is the schematic diagram of anti-solvent saturation vapor pressure method.
Fig. 3 is optical imagery, luminescent image and the scanning electron microscopy picture and carbon atom image of PDI nano wire.
Fig. 4 be in the different saturated vapor pressure periods, the optical imagery of PDI (on) and luminescent image (under).
Fig. 5 is intrinsic PDI, and anti-solvent handles the X-ray diffraction spectrum of the PDI of PDI and the processing of anti-solvent saturated vapor pressure.
Fig. 6 is intrinsic PDI, the i-v curve of the PDI of anti-solvent processing.
Fig. 7 is the i-v curve of the PDI of anti-solvent saturated vapor pressure processing.
Specific embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings.
High-sequential PDI nanowire preparation method of the invention, using anti-solvent saturation vapor pressure method, substrate material is Silicon prepares PDI nano wire by the enough saturated vapor pressure time, the specific steps are as follows:
(1) PDI is dissolved in dichlorobenzene solution, concentration is 5 mg/mls;
(2) PDI solution is added dropwise on substrate, is subsequently placed under saturation acetonitrile steam atmosphere;
(3) entire atmosphere is closed, stands, and PDI is allowed to carry out sufficient self assembly, forms PDI nano wire.
Chosen material is PDI, and purity is 98% or more, and the solvent of selection is dichloro-benzenes, and anti-solvent is acetonitrile, and silicon is substrate Material.The interdigital electrode with gold electrode is chosen as substrate for depositing PDI nano wire, tests i-v curve.
Embodiment 1: PDI is dissolved in dichlorobenzene solution, and configuration concentration is the PDI solution of 5 mg/mls;It is inhaled with suction pipe It takes a small amount of solution drop in substrate material, makes its natural drying, intrinsic PDI material is prepared with this;
Embodiment 2: acetonitrile solution is added in the dichlorobenzene solution dissolved with PDI as anti-solvent, volume ratio 5:1, 24 hours are stood, the solution with a small amount of precipitate is sucked out with suction pipe, is added dropwise on substrate material, makes its natural drying, this For anti-solvent facture;
Embodiment 3: the saturated vapor that substrate is placed in anti-solvent acetonitrile is depressed, PDI solution is added drop-wise to substrate with suction pipe On, it is closed, it stands, until PDI solution evaporation is complete.It is small 24 in order to study influence of the anti-solvent to PDI self assembling process When, 48 hours, 72 hours and 96 hours, respectively from taking-up sample carries out in saturated vapor pressure atmosphere.
Fig. 1-2 is the molecular schematic diagram of PDI and the schematic diagram of anti-solvent saturation vapor pressure method.
Fig. 3 is optical imagery, luminescent image and the scanning electron microscopy picture and carbon atom imaging of PDI nano wire.From In figure we can see that PDI be grown along one-dimensional square, and be it is straight, be bent it is less.Scanning electron microscope With higher resolution, it can be seen that the microstructure of Nano grade, we can see that the width of PDI nano wire is received for 200 Rice or so, what carbon atom imaging more illustrated to be formed is PDI nano wire.
Fig. 4 be in the different saturated vapor pressure periods, the optical imagery of PDI (on) and luminescent image (under).By not Optical imagery with the period is observed, it has been found that PDI within a short period of time, since anti-solvent and dichloro-benzenes act on, in local Over-saturation state is formed, so that the segregation of PDI, forms cluster structure, as the saturated vapor pressure time increases, anti-solvent is gradually It is slowly spread into dichloro-benzenes, limits the further aggregation of PDI, cluster gradually to fibre structure transition, ultimately forms one-dimensional Structure.
Fig. 5 is intrinsic PDI, and anti-solvent handles the X-ray diffraction spectrum of the PDI of PDI and the processing of anti-solvent saturated vapor pressure. From Fig. 4, it will be seen that the peak crystallization in X ray diffracting spectrum is bright after handling by anti-solvent saturated vapor pressure Aobvious, this shows that anti-solvent saturated vapor pressure handles advantageous PDI crystallization.
Fig. 6-7 is intrinsic PDI, and the Current Voltage that anti-solvent handles the PDI of PDI and the processing of anti-solvent saturated vapor pressure is bent Line.From in Fig. 6-7, it will be seen that in the PDI device handled by anti-solvent and anti-solvent saturation vapor pressure method, electric current It is all promoted, especially the PDI device of saturation vapor pressure method processing.This is because PDI intermolecular arrangements are orderly, be conducive to swash Going for son is delocalized, and under the action of applying outfield, charge can be transmitted effectively, lead to the promotion of electric current.
In conclusion the present invention is a kind of to utilize anti-solvent saturation vapor pressure method method, it is orderly to realize PDI nanowire height Growth.PDI is dissolved in dichloro benzene solvent, is then added dropwise on sinking to the bottom, then as in saturation anti-solvent atmosphere, is finally existed The self assembly effect for passing through molecule on substrate, forms the one-dimensional PDI nano wire of high-sequential.The present invention realizes PDI molecule One-dimensional orderly homoepitaxial, and show good crystallization property.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention.It is all in essence of the invention Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.

Claims (7)

1. the method that anti-solvent saturation vapor pressure method prepares high-sequential acid imide nano wire, which is characterized in that including as follows Step:
1) in a solvent by PDI dissolution;
2) PDI solution is added dropwise on substrate, is subsequently placed in saturation anti-solvent atmosphere;
3) the self assembly effect for passing through molecule on substrate, forms the one-dimensional PDI nano wire of high-sequential.
2. the method that anti-solvent saturation vapor pressure method according to claim 1 prepares high-sequential acid imide nano wire, It is characterized in that, the concentration of the PDI solution is 5 mg/mls.
3. the method that anti-solvent saturation vapor pressure method according to claim 1 prepares high-sequential acid imide nano wire, It is characterized in that, the solvent is dichloro-benzenes;The saturation anti-solvent is saturation acetonitrile steam.
4. the method that anti-solvent saturation vapor pressure method according to claim 1 prepares high-sequential acid imide nano wire, It is characterized in that, making entire atmosphere closed in the step 3), stand.
5. the method that anti-solvent saturation vapor pressure method according to claim 1 prepares high-sequential acid imide nano wire, It is characterized in that, the purity of the PDI is greater than 98%.
6. the method that anti-solvent saturation vapor pressure method according to claim 1 prepares high-sequential acid imide nano wire, It is characterized in that, the substrate material is silicon, the interdigital electrode with gold electrode is chosen as substrate for depositing PDI nanometers Line tests i-v curve.
7. the method that anti-solvent saturation vapor pressure method according to claim 1 prepares high-sequential acid imide nano wire, It is characterized in that, at 24 hours, 48 hours, 72 hours and 96 hours, taken out from saturated vapor pressure atmosphere respectively sample into Row observation.
CN201910491795.3A 2019-06-06 2019-06-06 The method that anti-solvent saturation vapor pressure method prepares high-sequential acid imide nano wire Withdrawn CN110194768A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110724141A (en) * 2019-10-22 2020-01-24 南京大学 Method for preparing EP-PDI micron line
CN110818711A (en) * 2019-11-01 2020-02-21 河北科技大学 Preparation method of organic heterojunction nanowire

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110724141A (en) * 2019-10-22 2020-01-24 南京大学 Method for preparing EP-PDI micron line
CN110818711A (en) * 2019-11-01 2020-02-21 河北科技大学 Preparation method of organic heterojunction nanowire

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