CN105543779B - A kind of TiOPc nanometer sheet and preparation method thereof - Google Patents
A kind of TiOPc nanometer sheet and preparation method thereof Download PDFInfo
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- CN105543779B CN105543779B CN201610030173.7A CN201610030173A CN105543779B CN 105543779 B CN105543779 B CN 105543779B CN 201610030173 A CN201610030173 A CN 201610030173A CN 105543779 B CN105543779 B CN 105543779B
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- tiopc
- nanometer sheet
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/12—Organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Composite Materials (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention discloses a kind of TiOPc nanometer sheet and preparation method thereof, the TiOPc nanometer sheet is in sheet of uniform size, and diameter is about 400 700nm, and thickness is 1 10nm.The TiOPc nanometer piece preparation method uses organic vapor phase deposition method, includes the following steps：A) heating region being put into TiOPc raw material to stove；B) under carrier gas atmosphere, heating TiOPc raw material makes TiOPc distil to 410 440 DEG C；C) by the carrier gas, the TiOPc of the distillation is guided to leave the heating region, until growth district, the temperature of the growth district is less than the temperature of the heating region；D) in growth district, TiOPc nanometer sheet is obtained.The TiOPc nanometer sheet of the present invention is new pattern, is had excellent performance, easy to operate, at low cost, pollution-free, can largely be prepared.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of TiOPc nanometer sheet and preparation method thereof.
Background technology
Phthalocyanine compound is that one kind uses extensive organic light-guide material.In many phthalocyanine compounds, TiOPc
It is had been favored by people with the photoelectric properties that its is outstanding.TiOPc has good low toxicity, thermal stability, good light stability and current-carrying
The advantages that sub- generation efficiency is high.
TiOPc is a kind of important charge generating material, is widely used in static dump/duplicating, photovoltaic device
And in the fields such as organic photoconductor.The morphology and size of nanometer TiOPc, has a great impact to its photoelectric properties.
Through having been reported that the synthetic method of TiOPc nano particle, but its method is complex, and product purity is not high, and grain size is uncontrollable,
And there is certain harm to environment.There is not the relevant report for preparing TiOPc nanometer sheet also at present.
Invention content
The first object of the present invention is to provide a kind of TiOPc nanometer sheet；The second object of the present invention is to provide one
Kind TiOPc nanometer piece preparation method.
What the first object of the present invention was realized in：The TiOPc nanometer sheet is new pattern, in the form of sheets, size
Uniformly, diameter 400-700nm, thickness 1-10nm.
What the second object of the present invention was realized in：The TiOPc nanometer piece preparation method uses organic vapors
Sedimentation includes the following steps：
A) heating region being evenly placed upon TiOPc raw material in stove；
B) it is passed through carrier gas, heating TiOPc raw material make TiOPc distil to 410 DEG C -440 DEG C；
C) carrier gas being passed through transports the TiOPc of distillation to growth district, and the temperature of the growth district is less than
Heating region temperature；
D) in growth district, TiOPc nanometer sheet is obtained.
Advantageous effect：The present invention is prepared for a kind of TiOPc nanometer sheet of new pattern.TiOPc provided by the invention
Preparation method：Vapour deposition process, product purity is higher, size tunable, several microns is generally arrived at tens nanometers, method is simple, right
It is environmental-friendly, it is to prepare the preferable method of monocrystalline.The factor that product is mainly influenced in preparation process includes temperature gradient, deposition
Time, flow rate of carrier gas, vacuum degree, underlayer temperature etc..Most of crystal of growth is one-dimensional column or two-dimensional sheet, specific shape
Dependent on the stack manner based on intermolecular weak interaction and its synergistic effect.
Description of the drawings
Fig. 1：The SEM of the TiOPc nanometer sheet of the present invention（1）Figure；
Fig. 2：The SEM of the TiOPc nanometer sheet of the present invention（2）Figure；
Fig. 3：The SEM of the TiOPc nanometer sheet of the present invention（3）Figure.
Specific implementation mode
With reference to embodiment and attached drawing, the present invention is further illustrated, but is not subject in any way to the present invention
Limitation, based on present invention teach that made by it is any transform or replace, all belong to the scope of protection of the present invention.
Experimental method used in following embodiments is conventional method unless otherwise specified.Institute in following embodiments
Material, reagent etc., are commercially available unless otherwise specified.
TiOPc nanometer sheet of the present invention is new pattern, and in the form of sheets, uniform in size, diameter 400-700nm is thick
Degree is 1-10nm.
A diameter of 400-500nm of the TiOPc nanometer sheet, thickness 1-5nm.
The preparation method of the TiOPc nanometer sheet is organic vapor phase deposition method.
The preparation process of the organic vapor phase deposition method is：A) heating region being put into TiOPc raw material to stove；
B) under carrier gas atmosphere, heating TiOPc raw material makes TiOPc distil to 410-440 DEG C；C) pass through the carrier gas, guiding
The TiOPc of the distillation leaves the heating region, until growth district, the temperature of the growth district is less than the heating region
Temperature；D) in growth district, TiOPc nanometer sheet is obtained.
TiOPc molecular structure is as follows：
Embodiment 1：
Empirically step cleans quartz ampoule and substrate successively, and installs experimental facilities, after being passed through nitrogen 30 minutes, starts
390 DEG C are heated to, 440 DEG C of target temperature is then warming up to the velocity step ladder of 1-8 DEG C/min again and keeps the temperature 180min.Nitrogen will
TiOPc after distillation is transported from heating region to growth district, the temperature near room temperature of the growth district.After the completion of heat preservation
Stop heating, the preparation of Continuous aeration 30min, TiOPc nano material terminate.
The TiOPc nanometer sheet is in the form of sheets, uniform in size, and diameter is about 400-700nm, thickness 1-10nm.
Embodiment 2：
On the basis of embodiment 1, change experiment condition：Target temperature is set as 420 DEG C, with the speed of 8-15 DEG C/min
It is warming up to target temperature, and keeps the temperature 300min.TiOPc nanometer sheet is obtained in growth district.
The TiOPc nanometer sheet is in the form of sheets, uniform in size, and diameter is about 400-500nm, thickness 1-5nm.
Embodiment 3：
On the basis of embodiment 1, change experiment condition：Target temperature is set as 410 DEG C, with the speed liter of 1-8 DEG C/min
Temperature keeps the temperature 300min to target temperature.TiOPc nanometer sheet is obtained in growth district.
The TiOPc nanometer sheet is in the form of sheets, uniform in size, and diameter is about 500-700nm, thickness 1-10nm.
Claims (2)
1. a kind of TiOPc nanometer piece preparation method, it is characterised in that a diameter of 400- of the TiOPc nanometer sheet
700nm, thickness 1-10nm, preparation method are：Quartz ampoule and substrate are cleaned successively and installs equipment, are passed through nitrogen 30 minutes
After begin heat to 390 DEG C, then be warming up to 440 DEG C with the velocity step ladder of 1-8 DEG C/min and keep the temperature 180min；After nitrogen will distil
TiOPc transported from heating region to growth district, the temperature near room temperature of growth district；Stop heating after the completion of heat preservation,
Maintaining nitrogen purge 30min, preparation terminate；Prepared TiOPc nanometer sheet is in the form of sheets, uniform in size, a diameter of 400-700nm,
Thickness is 1-10nm.
2. a kind of TiOPc nanometer piece preparation method, it is characterised in that a diameter of 400- of the TiOPc nanometer sheet
500nm, thickness 1-5nm, preparation method are：Quartz ampoule and substrate are cleaned successively and installs equipment, are passed through nitrogen 30 minutes
After begin heat to 390 DEG C, then be warming up to 420 DEG C with the velocity step ladder of 8-15 DEG C/min and keep the temperature 300min；Nitrogen will distil
TiOPc afterwards is transported from heating region to growth district, the temperature near room temperature of growth district；Stop adding after the completion of heat preservation
Heat, maintaining nitrogen purge 30min, preparation terminate；Prepared TiOPc nanometer sheet is in the form of sheets, uniform in size, a diameter of 400-
500nm, thickness 1-5nm.
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| CN201610030173.7A CN105543779B (en) | 2016-01-18 | 2016-01-18 | A kind of TiOPc nanometer sheet and preparation method thereof |
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| CN201610030173.7A CN105543779B (en) | 2016-01-18 | 2016-01-18 | A kind of TiOPc nanometer sheet and preparation method thereof |
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| CN105543779A CN105543779A (en) | 2016-05-04 |
| CN105543779B true CN105543779B (en) | 2018-07-13 |
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| CN113135926A (en) * | 2021-04-23 | 2021-07-20 | 昆明学院 | Novel crystal structure indium phthalocyanine nanowire and preparation method thereof |
| CN113956261A (en) * | 2021-09-16 | 2022-01-21 | 昆明学院 | Novel crystal structure chlorinated gallium phthalocyanine nanobelt and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1952223A (en) * | 2005-10-17 | 2007-04-25 | 中国科学院化学研究所 | Condensed aromatic organic semiconductor single-crystal micro/nano materials and their preparation method and application |
| CN101210347A (en) * | 2006-12-29 | 2008-07-02 | 中国科学院化学研究所 | Method for preparing organic compound single-crystal nano structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH05113585A (en) * | 1991-10-21 | 1993-05-07 | Nippon Telegr & Teleph Corp <Ntt> | Material for organic nonlinear optical element and organic nonlinear optical thin film using the same |
| JP2000174277A (en) * | 1998-12-01 | 2000-06-23 | Hitachi Ltd | Thin film transistor and its manufacture |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1952223A (en) * | 2005-10-17 | 2007-04-25 | 中国科学院化学研究所 | Condensed aromatic organic semiconductor single-crystal micro/nano materials and their preparation method and application |
| CN101210347A (en) * | 2006-12-29 | 2008-07-02 | 中国科学院化学研究所 | Method for preparing organic compound single-crystal nano structure |
Non-Patent Citations (1)
| Title |
|---|
| "Fabrication of Various Ordered Films of Oxotitanium(IV) Phthalocyanine by Vacuum Deposition and Their Spectroscopic Behavior";Hisatomo Yonehara et al;《Chem. Mater》;20011231;第13卷;第1015-1022页 * |
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