CN105552232A - Tree-shaped rubrene crystal thin film preparation method adopting high boiling point solvent to carry out regulation and control - Google Patents
Tree-shaped rubrene crystal thin film preparation method adopting high boiling point solvent to carry out regulation and control Download PDFInfo
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- CN105552232A CN105552232A CN201610030028.9A CN201610030028A CN105552232A CN 105552232 A CN105552232 A CN 105552232A CN 201610030028 A CN201610030028 A CN 201610030028A CN 105552232 A CN105552232 A CN 105552232A
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- rubrene
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- high boiling
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- YYMBJDOZVAITBP-UHFFFAOYSA-N rubrene Chemical compound C1=CC=CC=C1C(C1=C(C=2C=CC=CC=2)C2=CC=CC=C2C(C=2C=CC=CC=2)=C11)=C(C=CC=C2)C2=C1C1=CC=CC=C1 YYMBJDOZVAITBP-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 239000002904 solvent Substances 0.000 title claims abstract description 30
- 239000013078 crystal Substances 0.000 title claims abstract description 23
- 238000009835 boiling Methods 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000010409 thin film Substances 0.000 title abstract description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 9
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000758 substrate Substances 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 2
- 239000012153 distilled water Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 3
- 230000001276 controlling effect Effects 0.000 abstract 1
- 230000000979 retarding effect Effects 0.000 abstract 1
- 239000010408 film Substances 0.000 description 15
- 238000005516 engineering process Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- CUTSCJHLMGPBEJ-UHFFFAOYSA-N [N].CN(C)C=O Chemical compound [N].CN(C)C=O CUTSCJHLMGPBEJ-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000001548 drop coating Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
Classifications
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K10/00—Organic devices specially adapted for rectifying, amplifying, oscillating or switching; Organic capacitors or resistors having potential barriers
- H10K10/40—Organic transistors
- H10K10/46—Field-effect transistors, e.g. organic thin-film transistors [OTFT]
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K10/00—Organic devices specially adapted for rectifying, amplifying, oscillating or switching; Organic capacitors or resistors having potential barriers
- H10K10/80—Constructional details
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/80—Constructional details
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
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- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Electromagnetism (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Optics & Photonics (AREA)
- Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
Abstract
The invention relates to a tree-shaped rubrene crystal thin film preparation method adopting a high boiling point solvent to carry out regulation and control. Namely, growth of rubrene tree-shaped crystals is regulated and controlled by a DMF (Dimethyl Formamide) solvent, the DMF solvent with a volume ratio of 30 percent to 50 percent is added on the basis of an original chloroform solvent, a volatile speed is retarded by utilizing a solution dispensing method, the DMF solvent has a high boiling point, and the characteristic of further retarding the volatile speed enables rubrene molecules to have a sufficient driving force to sequentially complete the crystal growth process from a granular shape to a ribbon shape to a tree shape, thereby fulfilling the aim of regulating and controlling preparation of the tree-shaped rubrene crystals by the high boiling point solvent.
Description
Technical field
The present invention relates to the tree-shaped rubrene crystal film preparation method of a kind of high boiling solvent regulation and control, belong to organic optoelectronic technical field.
Background technology
In recent years, organic semiconductor, owing to having flexibility, cheapness, advantage that cost is low, has good application prospect in OTFT, organic solar batteries field.Rubrene (Rubrene, 5.6.11.12-tetraphenyl four benzene) a kind of polycyclic aromatic hydrocarbon of being made up of an aphthacene and four supporting rings, there is high mobility, long exciton diffusion length, can be applied to the fields such as light-emitting diode, field-effect transistor and solar cell, and the growth of rubrene crystal film is the primary condition realizing extensive use.
At present, the technology preparing film has epitaxial film deposition technology, ion sputtering, solution technique, physical gas phase deposition technology, chemical vapour deposition technique.Wherein solution technique advantage is that equipment is simple, with low cost, temperature requirement is low, can extensive deposition, and can directly at Grown crystal.Simultaneously, nitrogen dimethylformamide (N, N-Dimethylformamide, hereinafter referred to as DMF) be a kind of high boiling organic solvent, intermolecular force is large, can play and slow down solvent evaporates speed, for rubrene molecule provides the effect of sufficient actuating force, thus promote the spatial ordering and regularity of rubrene crystal film growth.
Therefore, the present invention is the tree-shaped rubrene crystal film preparation method of a kind of high boiling solvent regulation and control, namely by the growth of DMF solvent regulation and control rubrene tree, on the basis of original chloroform solvent, by adding the DMF solvent of volume ratio 30% ~ 50%, most rubrene molecule is made to have enough actuating forces to complete from granular successively, banded, to tree-shaped growth course, and, by changing the ratio of the DMF solvent added to change size and the regularity of tree-shaped rubrene crystal.
Summary of the invention
The present invention is the tree-shaped rubrene crystal film preparation method of a kind of high boiling solvent regulation and control, is intended to improve the cost occurred in current rubrene thin film preparation process high, complex process, the problem of film quality difference.The present invention adopts the method for molten drop-coated, utilizes high boiling solvent itself to have evaporation rate slow, is regulated and controled the growth of tree-shaped rubrene crystal film by DMF solvent.
The present invention is the tree-shaped rubrene crystal film preparation method of a kind of high boiling solvent regulation and control.The present invention is achieved in that as shown in Figure 1, and rubrene molecular growth is final tree pattern.Solution drop-coating can play the effect slowing down solvent evaporates speed, for rubrene crystal growth provides sufficient actuating force, the DMF solvent added is due to the high feature of boiling point, solvent evaporates speed is slowed down further, thus makes rubrene crystal finally be grown to serve as the large scale tree film of compact structure.
Accompanying drawing explanation
Fig. 1 is the tree-shaped rubrene crystal film shape appearance figure of high boiling solvent regulation and control.
Fig. 2 is the tree-shaped rubrene crystal film growth schematic diagram of high boiling solvent regulation and control.
Embodiment
As shown in Figure 1, rubrene molecular growth is final tree pattern.
Specific implementation process: substrate is the SiO of 300nm by Si substrate and surface thickness
2insulating barrier forms; The order of substrate according to acetone, ethanol, distilled water is cleaned, puts into the baking oven heating, drying 20min of 60 DEG C; The configuration of rubrene solution 1, gets rubrene 1mg, and chloroform 0.5ml, DMF0.3ml(are hereinafter referred to as solution 1), volume ratio is 37.5%, and joining specification is successively in the reagent bottle of 5ml, and then carry out ultrasonic vibration under normal temperature, ultrasound intensity is 60%, and the time is 10min; Taken out from baking oven by substrate and be placed on the accurate electric hot plate of temperature digital display that model is HP-127, temperature is set as 60 DEG C; From solution 1, take out 100 μ l-120 μ l solution drip and be applied to substrate middle part, rubrene molecule carries out self assembly by the dispersity in solution, owing to dripping the evaporation rate being coated with and can slowing down solvent, the boiling point of adding DMF solvent is high, slow down solvent evaporates speed further, growth for rubrene crystal provides long motive force, after self assembly rubrene molecule assembles formation nucleus, rubrene molecule starts constantly to grow along nucleus direction, present band shape successively, tree-shaped rubrene crystal film shape, as shown in Figure 2.
Claims (1)
1. the present invention is the tree-shaped rubrene crystal film preparation method of a kind of high boiling solvent regulation and control, implementation procedure is: by substrate according to acetone, ethanol, the order of distilled water is cleaned, put into the baking oven heating, drying 20min of 60 DEG C, the configuration of rubrene solution 1: get rubrene 1mg, chloroform 0.5ml, add the DMF solvent that volume ratio is 30% ~ 50%, join successively (hereinafter referred to as solution 1) in the reagent bottle of 5ml, then ultrasonic vibration under normal temperature is carried out, ultrasound intensity is 60%, time is 10min, substrate is taken out from baking oven and is placed on the accurate electric hot plate of temperature, temperature is set as 60 DEG C, from solution 1, take out 100 μ l-120 μ l solution drip and be applied to substrate middle part, utilize the slow volatilization of solvent, realize the preparation of tree-shaped rubrene crystal film.
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CN201610030028.9A CN105552232A (en) | 2016-01-18 | 2016-01-18 | Tree-shaped rubrene crystal thin film preparation method adopting high boiling point solvent to carry out regulation and control |
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CN201610030028.9A CN105552232A (en) | 2016-01-18 | 2016-01-18 | Tree-shaped rubrene crystal thin film preparation method adopting high boiling point solvent to carry out regulation and control |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106025101A (en) * | 2016-07-23 | 2016-10-12 | 长春工业大学 | Method for regulating and controlling growth of spherical rubrene crystal thin film by cosolvent through polymer induction layer |
CN108417715A (en) * | 2018-03-05 | 2018-08-17 | 长春工业大学 | A kind of preparation method of the crystallinity Organic Thin Film Transistors of crystallinity solvent regulation and control |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101476103A (en) * | 2008-12-01 | 2009-07-08 | 苏州纳米技术与纳米仿生研究所 | Method for preparing organic semiconductor material rubrene micro-nano wire |
CN102154688A (en) * | 2011-03-25 | 2011-08-17 | 长春圣卓龙电子材料有限公司 | Rubrene weak epitaxial growth thin film and application thereof in organic thin-film transistor |
-
2016
- 2016-01-18 CN CN201610030028.9A patent/CN105552232A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101476103A (en) * | 2008-12-01 | 2009-07-08 | 苏州纳米技术与纳米仿生研究所 | Method for preparing organic semiconductor material rubrene micro-nano wire |
CN102154688A (en) * | 2011-03-25 | 2011-08-17 | 长春圣卓龙电子材料有限公司 | Rubrene weak epitaxial growth thin film and application thereof in organic thin-film transistor |
Non-Patent Citations (1)
Title |
---|
LIJUAN WANG,ET AL: "Insight into crystallization process of rubrene by binary solvent mixtures", 《RSC ADVANCES》 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106025101A (en) * | 2016-07-23 | 2016-10-12 | 长春工业大学 | Method for regulating and controlling growth of spherical rubrene crystal thin film by cosolvent through polymer induction layer |
CN108417715A (en) * | 2018-03-05 | 2018-08-17 | 长春工业大学 | A kind of preparation method of the crystallinity Organic Thin Film Transistors of crystallinity solvent regulation and control |
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Application publication date: 20160504 |