CN102206863B - Preparation method of metal phthalocyanine nanowires - Google Patents
Preparation method of metal phthalocyanine nanowires Download PDFInfo
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- CN102206863B CN102206863B CN2011100725483A CN201110072548A CN102206863B CN 102206863 B CN102206863 B CN 102206863B CN 2011100725483 A CN2011100725483 A CN 2011100725483A CN 201110072548 A CN201110072548 A CN 201110072548A CN 102206863 B CN102206863 B CN 102206863B
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Abstract
The invention discloses a preparation method of metal phthalocyanine nanowires which are monodispersed and are appressed on a substrate. The preparation method is characterized by comprising the following steps: I, mixing metal phthalocyanine and alumina according to a ratio by mass of 1:100 to form a mixture as raw material, taking out the raw material and putting the raw material together with a substrate into a container for heating growth; and II, filling inert protective gas of nitrogen or argon into the container, keeping a pressure intensity of 6*10<-2> Pa in the container, then heating the container to make the raw material grow at a constant temperature for a certain time, wherein the constant temperature is in a range of 450 to 500 DEG C and the growth time is in a range of 20 to 60 minutes, and then cooling the raw material together with the container to normal temperature to obtain metal phthalocyanine nanowires which grow on the substrate and are monodispersed and appressed on the substrate. The metal phthalocyanine nanowires provided by the preparation method have the advantages of simple and practicable processes, low cost and good contact with a substrate, and provide a possibility of further research of monocrystalline metal phthalocyanine nanowires.
Description
Technical field
The invention discloses a kind of organic semiconductor haplotype preparation of devices method, relate in particular to a kind of preparation method of metal phthalocyanine nano wire of grow single dispersion, smooth substrate, belong to the semiconductor growing preparation field.
Background technology
Organic single-crystal can not only disclose the intrinsic properties of material, also is one of optimal selection of constructing the high-performance optical electrical part simultaneously, gets more and more people's extensive concerning in recent years.Yet organic crystal is difficult to grow up usually, and most forms with the micro-nano crystalline substance exist.Therefore, if can directly on the basis of micro-nano crystalline substance, construct device, conduct a research; Can not only overcome the shortcoming that organic single-crystal is difficult to grow up; Realization also will promote the fusion of organic crystal and micro-nano opto-electronic device simultaneously to the efficient sign of material, promotes the development of nano molecular electronics.In order to explore the intrinsic properties of organic materials, at utmost improve the mobility of organic field effect tube, must adopt the organic semiconductor monocrystal device.Be preparation organic semiconductor haplotype device, the method for employing is usually, directly prepares a large amount of nano wires through physical gas-phase deposite method, through being dispersed in the organic solvent, is transferred on the silicon substrate then.The common more complicated of this preparation method, product yield are lower, mainly show contacting on the tightness degree of metal phthalocyanine nano wire and silicon substrate.
Summary of the invention
The objective of the invention is to propose a kind of preparation method of metal phthalocyanine nano wire of grow single dispersion, smooth substrate, to improve the metal phthalocyanine nano wire contacts the stability difference with silicon substrate problem.
Above-mentioned purpose of the present invention will be achieved through following technical scheme:
A kind of preparation method of metal phthalocyanine nano wire, said metal phthalocyanine nano wire be single disperse, smooth substrate, it is characterized in that comprising step:
I, press 1: 100 ground and mixed of mass ratio as raw material, said raw material is got material insert in the lump in the container in order to heat growth with silicon substrate with metal phthalocyanine and aluminium sesquioxide;
II, in container pressure 6 * 10 in filling inert protective gas nitrogen or argon gas and the holding chamber
-2Pa implements to heat to said container, makes raw material behind 450 ℃-500 ℃ following constant temperature growth 20min-60min, be cooled to normal temperature with container, and growth forms the metal phthalocyanine nano wire of single dispersion, smooth substrate on silicon substrate.
Further, the temperature of constant temperature growth is 450 ℃ in the Step II, and growth time is 40min; Perhaps the temperature of constant temperature growth is 480 ℃ in the Step II, and growth time is 30min; Or the temperature of constant temperature growth is 500 ℃ in the Step II, and growth time is 60min or 20min.
Further, said metal phthalocyanine comprises a kind of organic semiconductor in phthalocyanine cobalt, CuPc and the phthalocyanine nickel at least.
Use preparation method of the present invention; Its outstanding effect is: the present invention prepares single metal phthalocyanine nano wire that disperses smooth substrate; Simple for process, cost is low, the phthalocyanin nano line contacts with silicon substrate well, for the further field-effect characteristic of research single-crystal metal phthalocyanin nano line provides possibility.
Description of drawings
Fig. 1 is single field emission scanning electron microscope (SEM) photo that disperses the phthalocyanine cobalt nanowire of smooth substrate that the present invention makes;
Fig. 2 is single AFM (AFM) photo that disperses the phthalocyanine cobalt nanowire of smooth substrate that the present invention makes.
Fig. 3 is single field emission scanning electron microscope (SEM) photo that disperses the CuPc nano wire of smooth substrate that the present invention makes;
Fig. 4 is single field emission scanning electron microscope (SEM) photo that disperses the phthalocyanine nickel nano wire of smooth substrate that the present invention makes.
Embodiment
Contact stability for improving the metal phthalocyanine nano wire with silicon substrate, the invention provides a kind of preparation method of metal phthalocyanine nano wire of on substrate, grow single dispersion, smooth substrate.Simply:
I, press 1: 100 ground and mixed of mass ratio as raw material, said raw material is got material insert in the lump in the container in order to heat growth with silicon substrate with metal phthalocyanine and aluminium sesquioxide;
II, in container pressure 6 * 10 in filling inert protective gas nitrogen or argon gas and the holding chamber
-2Pa implements heating to said container, makes raw material behind 450 ℃-500 ℃ following constant temperature growth 20min-60min, be cooled to normal temperature with container, and growth forms the metal phthalocyanine nano wire of monodispersed smooth substrate on silicon substrate.
Following examples are used to explain the present invention, but are not to be used for limiting scope of the present invention.
Embodiment 1:
0.01 gram phthalocyanine cobalt and 1 is restrained aluminium sesquioxide mix in the adding agate mortar, after fully grinding, in quartzy bateau special in the starting material transfer.Raw-material quartzy bateau will be housed, place the center position of horizontal pipe furnace warm area, place silicon substrate at air flow line; Tube furnace is evacuated to 6 * 10 in advance
-2Pa, logical subsequently protection gas nitrogen vacuumized 1 hour; The adjusting air-flow is 100sccm, and is heated to 500 ℃; Constant temperature 20min under nitrogen atmosphere cools to normal temperature with the furnace under nitrogen atmosphere, take out silicon substrate, can obtain single phthalocyanine cobalt nanowire that disperses smooth substrate, wide about 80nm.Fig. 1 is single field emission scanning electron microscope (SEM) photo that disperses the phthalocyanine cobalt nanowire of smooth substrate that the present invention makes.
Embodiment 2:
0.01 gram phthalocyanine cobalt and 1 is restrained aluminium sesquioxide mix in the adding agate mortar, after fully grinding, in quartzy bateau special in the starting material transfer.Raw-material quartzy bateau will be housed, place the center position of horizontal pipe furnace warm area, place silicon substrate at air flow line; Tube furnace is evacuated to 6 * 10 in advance
-2Pa, logical subsequently protection gas nitrogen vacuumized 1 hour; The adjusting air-flow is 100sccm, and is heated to 500 ℃; Constant temperature 60min under nitrogen atmosphere cools to normal temperature with the furnace under nitrogen atmosphere, take out silicon substrate, can obtain single phthalocyanine cobalt nanowire that disperses smooth substrate.Fig. 2 is single AFM (AFM) photo that disperses the phthalocyanine cobalt nanowire of smooth substrate that the present invention makes
Embodiment 3:
0.01 gram CuPc and 1 is restrained aluminium sesquioxide mix in the adding agate mortar, after fully grinding, in quartzy bateau special in the starting material transfer.Raw-material quartzy bateau will be housed, place the center position of horizontal pipe furnace warm area, place silicon substrate at air flow line; Tube furnace is evacuated to 6 * 10 in advance
-2Pa, logical subsequently protection gas nitrogen vacuumized 1 hour; The adjusting air-flow is 100sccm, and is heated to 480 ℃; Constant temperature 30min under nitrogen atmosphere cools to normal temperature with the furnace under nitrogen atmosphere, take out silicon substrate, can obtain single CuPc nano wire that disperses smooth substrate.Fig. 3 is single field emission scanning electron microscope (SEM) photo that disperses the CuPc nano wire of smooth substrate that the present invention makes;
Embodiment 4:
0.01 gram phthalocyanine nickel and 1 is restrained aluminium sesquioxide mix in the adding agate mortar, after fully grinding, in quartzy bateau special in the starting material transfer.Raw-material quartzy bateau will be housed, place the center position of horizontal pipe furnace warm area, place silicon substrate at air flow line; Tube furnace is evacuated to 6 * 10 in advance
-2Pa, logical subsequently protection gas nitrogen vacuumized 1 hour; The adjusting air-flow is 100sccm, and is heated to 450 ℃; Constant temperature 40min under nitrogen atmosphere cools to normal temperature with the furnace under nitrogen atmosphere, take out silicon substrate, can obtain single phthalocyanine nickel nano wire that disperses smooth substrate.Fig. 4 is single field emission scanning electron microscope (SEM) photo that disperses the phthalocyanine nickel nano wire of smooth substrate that the present invention makes.
Claims (5)
1. the preparation method of a metal phthalocyanine nano wire, said metal phthalocyanine nano wire be singly disperse, smooth substrate, it is characterized in that comprising step:
I, press 1: 100 ground and mixed of mass ratio as raw material, said raw material is got material insert in the lump in the container in order to heat growth with silicon substrate with metal phthalocyanine and aluminium sesquioxide;
II, in container pressure 6 * 10 in filling inert protective gas nitrogen or argon gas and the holding chamber
-2Pa implements to heat to said container, makes raw material behind 450 ℃-500 ℃ following constant temperature growth 20min-60min, be cooled to normal temperature with container, and growth forms the metal phthalocyanine nano wire of single dispersion, smooth substrate on silicon substrate.
2. the preparation method of a kind of metal phthalocyanine nano wire according to claim 1 is characterized in that: the temperature of constant temperature growth is 450 ℃ in the Step II, and growth time is 40min.
3. the preparation method of a kind of metal phthalocyanine nano wire according to claim 1 is characterized in that: the temperature of constant temperature growth is 480 ℃ in the Step II, and growth time is 30min.
4. the preparation method of a kind of metal phthalocyanine nano wire according to claim 1 is characterized in that: the temperature of constant temperature growth is 500 ℃ in the Step II, and growth time is 60min or 20min.
5. the preparation method of a kind of metal phthalocyanine nano wire according to claim 1 is characterized in that: said metal phthalocyanine comprises the phthalocyanine cobalt at least, a kind of organic semiconductor in CuPc and the phthalocyanine nickel.
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CN102505144B (en) * | 2011-11-03 | 2014-12-10 | 苏州大学 | Preparation method for directional growth of organic micro/nano structure |
CN103788101B (en) * | 2012-10-31 | 2017-02-01 | 中国科学院苏州纳米技术与纳米仿生研究所 | Cross-linked metalloporphyrin nanocrystal and preparation method thereof, and manufacturing method for optical detector |
CN104086555B (en) * | 2014-06-20 | 2016-08-17 | 昆明学院 | New crystal structure Cobalt Phthalocyanine (J-CoPc) nano wire and preparation method thereof |
CN104610269B (en) * | 2015-01-23 | 2017-08-15 | 昆明学院 | New crystal structure Nickel Phthalocyanine(ω‑NiPc)Nano wire and preparation method thereof |
CN104557952A (en) * | 2015-01-23 | 2015-04-29 | 昆明学院 | New crystalline structural zinc phthalocyanine (iota-ZnPc) nanowire and preparation method thereof |
KR102243520B1 (en) * | 2019-11-20 | 2021-04-21 | 포항공과대학교 산학협력단 | Novel phthalocyanine nanowire and use thereof |
CN113956261A (en) * | 2021-09-16 | 2022-01-21 | 昆明学院 | Novel crystal structure chlorinated gallium phthalocyanine nanobelt and preparation method thereof |
CN114427104B (en) * | 2021-12-13 | 2023-03-21 | 深圳先进技术研究院 | Copper phthalocyanine polymer @ copper nanowire core-shell nano material as well as preparation method and application thereof |
Citations (1)
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CN1150261A (en) * | 1995-11-01 | 1997-05-21 | 中国科学院化学研究所 | nm-class phthalocyanines organic light-guide material and preparing process and use thereof |
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CN1150261A (en) * | 1995-11-01 | 1997-05-21 | 中国科学院化学研究所 | nm-class phthalocyanines organic light-guide material and preparing process and use thereof |
Non-Patent Citations (3)
Title |
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Ana Borras et. al..Synthesis of supported single-crystalline organic Nanowires by Physical Vapor Deposition.<<Chem.Mater>>.2008,第20卷7371-7373. * |
Feng-Xia Wang et. al..Vapor growth and photoconductivity of single-crystal nickel-phthalocyanine nanorods.<<Materials letters>>.2010,第65卷933-936. * |
W.Y.Tong et.al..Synthesis and properties of copper phthalocyanine nanowires.<<Thin solid films>>.2007,第515卷5270-5274. * |
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