CN103255374A - Method for preparing ordered one-dimensional organic nano wire array - Google Patents
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- CN103255374A CN103255374A CN2012103469708A CN201210346970A CN103255374A CN 103255374 A CN103255374 A CN 103255374A CN 2012103469708 A CN2012103469708 A CN 2012103469708A CN 201210346970 A CN201210346970 A CN 201210346970A CN 103255374 A CN103255374 A CN 103255374A
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Abstract
The invention discloses a method for preparing an ordered one-dimensional organic nano wire array, which comprises the following steps: carrying out a vapor plating on a clean silicon or silicon oxide substrate for forming a gold nanometer particle film by employing an electron beam deposition technology, wherein, the substrate for modifying gold nanometer particles is a growth substrate, and preparing an organic monocrystalline nano wire array by a physical vapour deposition method. The invention has the advantages of simple technology scheme and operation, and the preparation of large area one-dimensional organic semiconductor nano-material array on a gold plating substrate is realized by one step.
Description
Technical field
The present invention relates to organic nano linear array structure and preparation method thereof, be specifically related to a kind of method for preparing orderly one dimension organic nano linear array.
Background technology
As everyone knows, the performance of nano material and its appearance structure are closely bound up.Under specific pattern and structure, nano material can present excellent optics and electric property.Therefore, the researchist strives to find the nano material system that suitable method preparation has controllable appearance and structure.Nano-wire array is one of nano material integration system of greatest concern, and it has high-sequential, and good can be handling, and the set sunken photoeffect brought of effect and Laser emission etc.Existing result of study shows that nano-wire array material can be used as the important component part in the nano photoelectric devices such as transistor, feds, photovoltaic cell and chemical sensor.The preparation method of nano-wire array has self-assembly method, template, solvent-thermal method, gel method, electrochemical synthesis method, and chemical Vapor deposition process etc., but past people's research mainly concentrates on the inorganic nano linear array, and is then less for the research of organic nano linear array.
CuPc (CuPc) crystal is typical P type organic semiconductor material, is typical n type organic semiconductor material and fluoridize CuPc (F16 CuPc) crystal, and the both is important organic photoelectric semiconductor material.CuPc and molecular structure and the energy level characteristics thereof of fluoridizing CuPc have determined them to have a lot of excellent characteristic, as high temperature resistant, high conduction, therefore have broad application prospects at aspects such as photoconduction, photovoltaic, air-sensitive, thermoelectricity, electroluminescent and catalysis.CuPc and fluoridize the CuPc nanostructure and have excellent stability and good light electrical property makes it receive more and more concern.At present, the method for preparing the CuPc nano wire mainly contains vapour deposition process, template, aqueous phase synthesis method, hydro-thermal solvent-thermal method and electrochemical deposition method etc.The CuPc molecule usually along the direction oriented growth parallel with substrate surface, forms nano wire film when forming nanostructure, and to the report of the CuPc nano-wire array aspect of the angled ordering growth of substrate seldom.The successful example of part has: professor Chen Hongzheng that Zhejiang University's polymer science in 2005 and engineering science are utilizes electrodip process synthetic phthalocyanine copper nano-wire array on the AAO template; Chihaya professor Adachi of Japan utilized physical vaporous deposition to prepare nano wire and the nano belt array of CuPc in 2011, and utilized the CuPc nano-wire array of preparation to produce solar cell.Yet preceding a kind of method is subject to the size of AAO template, and output is less, and also must dissolve alumina formwork when further using, and the introducing of organic solvent unavoidably brings infringement to the crystal mass of organic nano line.Then a kind of method need deposit two-layer organic film in advance as crystal seed in substrate, and preparation process is more loaded down with trivial details, and is orientated relatively poorly, and the organic nano line of preparing is polycrystalline structure.Compare with aforesaid method, present method only needs sputter one deck golden film as thin as a wafer on growth substrate in advance, just can utilize physical vaporous deposition to prepare large-area organic nano linear array.At present with the report of noble metal nano particles catalytic growth organic nano line seldom, Germany scientist Helmut Dosch once reported at Nano Lett. and Chem. Mater. that gold nano grain can play the effect of inducing nucleation to phthalocyanines derivates, and grew the one-dimensional phthalocyanine nano wire with thermal evaporation at gold nano grain.But the preparation method of Helmut Dosch is quite time-consuming, and the CuPc nano wire orientational disorder that grows out, and homogeneity is relatively poor, is unfavorable for its application on functional device in the future.
Summary of the invention
The objective of the invention is to overcome the above problem that prior art exists, a kind of method for preparing orderly one dimension organic nano linear array is provided.
For realizing above-mentioned technical purpose, reach above-mentioned technique effect, the present invention is achieved through the following technical solutions:
A kind of method for preparing orderly one dimension organic nano linear array may further comprise the steps:
Step 1) adopts electron beam deposition technology thick gold nano grain film of evaporation 5-8 nm on the silicon of cleaning or silicon oxide substrate;
Step 2) utilizes the substrate of modifying gold nano grain to be growth substrate, adopt physical vaporous deposition to prepare the organic single-crystal nano-wire array.
Further, described physical vaporous deposition (PVD) preparation organic single-crystal nano-wire array in the described step (2), concrete growth step is as follows: the presoma that will prepare described organic nano linear array according to the flow direction of air-flow places porcelain boat, and puts it into the center warm area of vacuum tube furnace; Get the cold zone that gold-plated substrate places described vacuum tube furnace, described substrate distance center warm area 10-2Ocm; Start vacuum pump, be evacuated to after pressure is lower than 1 Pa in the described furnace chamber, feeding inert protective gas argon gas to the pressure in the described furnace chamber in the furnace chamber is 4 * 10
4-6 * 10
4Pa is evacuated to again that pressure is lower than 1 Pa in the furnace chamber, after so repeating to guarantee that remnant oxygen is all taken away in the tube chamber 3 times, feeds argon gas toward silica tube in, and the maintenance gas flow rate is 30-60 sccm, and the chamber internal gas pressure is transferred to 220-260 Pa, the sealed vacuum pipe; Open heating unit, with 10-20 ℃/minute temperature rise rate, the center warm area of described vacuum tube furnace is heated to the vaporization temperature of described precursor, this moment, the temperature of center warm area was 380-420 ℃, and the temperature of growth substrates is 100-200 ℃; Keep and stop heating after above-mentioned vaporization temperature 10-60 minute, and make system naturally cool to room temperature, in described furnace chamber, feed argon gas to a normal atmosphere then, open furnace chamber, can obtain the one-dimensional phthalocyanine copper nano-wire array of large-area ordered crossed orientation growth in described growth substrates.
Further, the presoma for preparing described one dimension organic nano linear array is to can be used in the material that physical vaporous deposition carries out nanostructure growth, gold thin film on the described substrate in described step (1), (2) exists with the form of discontinuous nano-particular film, in the grown effect of catalysis nucleation of nano array structure.
Further, in the described step (2), when feeding non-oxidizing gas to normal atmosphere in the described furnace chamber, for the air flow that prevents from pouring in is suddenly destroyed the organic nano array structure, the flow of the non-oxidizing gas that feeds is not higher than 1O0sccm, and making temperature optimized temperature when the CuPc nano-wire array is grown of described vacuum tube furnace center warm area in the described step (2) is 415 ℃.
Further, used non-oxidized gas is nitrogen, argon gas or hydrogen argon (volume ratio 95: 5) mixed gas etc. among the described preparation method, and described one dimension organic nano linear array is classified CuPc nano-wire array, phthalocyanine cobalt nanowire array, Phthalocyanine Zinc nano-wire array, FePC nano-wire array as, fluoridizes the CuPc nano-wire array and fluoridized phthalocyanines derivates such as phthalocyanine cobalt nanowire array.
The invention has the beneficial effects as follows:
Adopt technical solution of the present invention, simple to operate, and realized preparing big area one dimension organic semiconductor nano material array in gold-plated substrate previous step.
Above-mentioned explanation only is the general introduction of technical solution of the present invention, for can clearer understanding technique means of the present invention, and can be implemented according to the content of specification sheets, below with preferred embodiment of the present invention and conjunction with figs. describe in detail as after.The specific embodiment of the present invention is provided in detail by following examples and accompanying drawing thereof.
Description of drawings
Accompanying drawing described herein is used to provide further understanding of the present invention, constitutes the application's a part, and illustrative examples of the present invention and explanation thereof are used for explaining the present invention, do not constitute improper restriction of the present invention.In the accompanying drawings:
Fig. 1 is the growth synoptic diagram of preparation one dimension organic nano linear array;
The optical photograph of CuPc nano-wire array on silicon base that Fig. 2 obtains for embodiment 1;
Scanning electronic microscope (SEM) photo of the CuPc nano-wire array that Fig. 3 obtains for embodiment 1 on silicon base;
Transmission electron microscope (TEM) photo of the CuPc nano wire that Fig. 4 obtains for embodiment 2;
The CuPc nano-wire array that Fig. 5 obtains for embodiment 2 is at the suprabasil scanning electronic microscope of SiO2 (SEM) photo;
What Fig. 6 obtained for embodiment 3 fluoridizes the CuPc nano-wire array at the suprabasil optical photograph of SiO2;
What Fig. 7 obtained for embodiment 3 fluoridizes the CuPc nano-wire array at the suprabasil scanning electronic microscope of SiO2 (SEM) photo.
Embodiment
Below with reference to the accompanying drawings and in conjunction with the embodiments, describe the present invention in detail.
Shown in figure, a kind of method for preparing orderly one dimension organic nano linear array may further comprise the steps:
Step 1) adopts electron beam deposition technology thick gold nano grain film of evaporation 5-8 nm on the silicon of cleaning or silicon oxide substrate;
Step 2) utilizes the substrate of modifying gold nano grain to be growth substrate, adopt physical vaporous deposition to prepare the organic single-crystal nano-wire array.
Further, described physical vaporous deposition (PVD) preparation organic single-crystal nano-wire array in the described step (2), concrete growth step is as follows: the presoma that will prepare described organic nano linear array according to the flow direction of air-flow places porcelain boat, and puts it into the center warm area of vacuum tube furnace; Get the cold zone that gold-plated substrate places described vacuum tube furnace, described substrate distance center warm area 10-2Ocm; Start vacuum pump, be evacuated to after pressure is lower than 1 Pa in the described furnace chamber, feeding inert protective gas argon gas to the pressure in the described furnace chamber in the furnace chamber is 4 * 104-6 * 104 Pa, be evacuated to the interior pressure of furnace chamber again and be lower than 1 Pa, after so repetition guarantees that remnant oxygen is all taken away in the tube chamber for 3 times, feed argon gas in silica tube, keeping gas flow rate is 30-60 sccm, and the chamber internal gas pressure transferred to 220-260 Pa, the sealed vacuum pipe; Open heating unit, with 10-20 ℃/minute temperature rise rate, the center warm area of described vacuum tube furnace is heated to the vaporization temperature of described precursor, this moment, the temperature of center warm area was 380-420 ℃, and the temperature of growth substrates is 100-200 ℃; Keep and stop heating after above-mentioned vaporization temperature 10-60 minute, and make system naturally cool to room temperature, in described furnace chamber, feed argon gas to a normal atmosphere then, open furnace chamber, can obtain the one-dimensional phthalocyanine copper nano-wire array of large-area ordered crossed orientation growth in described growth substrates.
Further, the presoma for preparing described one dimension organic nano linear array is to can be used in the material that physical vaporous deposition carries out nanostructure growth, gold thin film on the described substrate in described step (1), (2) exists with the form of discontinuous nano-particular film, in the grown effect of catalysis nucleation of nano array structure.
Further, in the described step (2), when feeding non-oxidizing gas to normal atmosphere in the described furnace chamber, for the air flow that prevents from pouring in is suddenly destroyed the organic nano array structure, the flow of the non-oxidizing gas that feeds is not higher than 1O0sccm, and making temperature optimized temperature when the CuPc nano-wire array is grown of described vacuum tube furnace center warm area in the described step (2) is 415 ℃.
Further, used non-oxidized gas is nitrogen, argon gas or hydrogen argon (volume ratio 95: 5) mixed gas etc. among the described preparation method, and described one dimension organic nano linear array is classified CuPc nano-wire array, phthalocyanine cobalt nanowire array, Phthalocyanine Zinc nano-wire array, FePC nano-wire array as, fluoridizes the CuPc nano-wire array and fluoridized phthalocyanines derivates such as phthalocyanine cobalt nanowire array.
The present invention combines physical vaporous deposition (PVD) and catalyst inducement nano wire nucleating growth technology, a step large-area preparation high-sequential one dimension organic nano linear array.Silicon chip or the oxidized silicon chip that at first will be coated with the catalytic gold particle are growth substrates, because the gold nano catalysed particulate has high surface energy, can play the effect of inducing nucleating growth to the organic nano line in process of growth.Then, the method and the catalysed particulate fixed point catalytic growth technology that prepare material in conjunction with PVD, make the gold nano grain surface adsorption of precursor gaseous molecular on substrate assemble nucleation, extension forms one dimension Nano structure, finally forms organic one-dimensional nano-array structure of crossed orientation growth at gold-plated substrate.
Embodiments of the invention:
Employed vacuum tube furnace is produced by brilliant Materials Technology Ltd. of Hefei section among the embodiment, and the boiler tube of vacuum tube furnace is alundum tube, and used alundum tube is that internal diameter is that 37.44mm, external diameter are 44.3mm; Employed precursor CuPc powder is purchased in the lark waffle and is learned reagent company limited, CAS: 147-14-8; Fluoridize CuPc available from Sigma-aldrich, CAS: 14916-87-1; Silicon chip and oxidized silicon chip are purchased in sea, Zhejiang nano semiconductor company limited.
Embodiment one: at gold-plated silicon chip substrate preparation CuPc nano-wire array
Get 30-50 mg CuPc powder, place porcelain boat, porcelain boat is put in the high-temperature zone of vacuum tube furnace, get the silicon chip of 1 * 2cm plating 6nm gold, place it in airflow downstream apart from the low-temperature region of high temperature center 10-20cm, the sealing vacuum tube furnace; After being pumped in the furnace chamber pressure and being lower than the body pressure to the described furnace chamber of bleeding and being lower than 1 Pa, feeding non-oxidizable shielding gas to the pressure in the described furnace chamber in the furnace chamber is 4x1O
4Pa-6x1O
4Pa, the body pressure to the furnace chamber of bleeding again is lower than 1 Pa, so guarantees for 3 times repeatedly in the tube chamber with argon gas the pressure in the chamber to be charged to 220Pa, the sealed vacuum pipe for behind the state of anaerobic; Beginning is heated to 415 ℃ with 20 ℃/minute speed with the high-temperature zone of furnace chamber, and continues 30 minutes-60 minutes under 415 ℃ situation, and (intraluminal pressure change is very little in this whole process) naturally cools to room temperature; In furnace chamber, charge into argon gas (gas flow 60sccm-1OOsccm) to a normal atmosphere; Open furnace chamber, obtained blue vertical crossed orientation growth CuPc nano-wire array at the substrate basal plane of placing.Product is directly taken out from furnace chamber, can see from its optical photograph (see figure 2), the direction of falling along temperature obtains to the right of low temperature that larger area product and resulting product area only are subject to the size of vacuum chamber and in the difference of growth warm area temperature by the left side of high temperature.Resulting one-dimensional nano line array is observed under SEM (as Fig. 3 (a, b) shown in), be can be observed length and be the array that the CuPc nano wire epitaxy from the gold nano grain about 5 microns comes out to form; Scheme from TEM(such as Fig. 4 (a, b) shown in) that the nanowire surface pattern is smooth as can be seen, the crystals lattice fringe is high-visible, confirms that nano wire is the monocrystalline attitude.
Embodiment two: at gold-plated oxidized silicon chip substrate preparation CuPc nano-wire array
Get 30-50 mg CuPc powder, place porcelain boat, porcelain boat is put in the high-temperature zone of vacuum tube furnace, get the oxidized silicon chip of 1 * 2cm plating 6nm gold, place it in airflow downstream apart from the low-temperature region of high temperature center 10-20cm, the sealing vacuum tube furnace; After being pumped in the furnace chamber pressure and being lower than the body pressure to the described furnace chamber of bleeding and being lower than 1 Pa, feeding non-oxidizable shielding gas to the pressure in the described furnace chamber in the furnace chamber is 4x1O
4Pa-6x1O
4Pa, the body pressure to the furnace chamber of bleeding again is lower than 1 Pa, so guarantees for 3 times repeatedly in the tube chamber with argon gas the pressure in the chamber to be charged to 220Pa, the sealed vacuum pipe for behind the state of anaerobic; Beginning is heated to 415 ℃ with 20 ℃/minute speed with the high-temperature zone of furnace chamber, and continues 5 minutes-10 minutes under 415 ℃ situation, naturally cools to room temperature; In furnace chamber, charge into argon gas (gas flow 60sccm-1OOsccm) to a normal atmosphere; Open furnace chamber, obtained blue vertical crossed orientation growth of one-dimensional CuPc nano-wire array at the substrate basal plane of placing.
Product is directly taken out from furnace chamber, can see that from its electron micrograph (see figure 5) resulting one-dimensional nano line is perpendicular to the substrate that is coated with gold nano grain.
Embodiment three: fluoridize the CuPc nano-wire array in gold-plated silicon base preparation
Fluoridize the CuPc nano-wire array according to the preparation of the method for embodiment 2 perpendicular to gold-plated silicon substrate.Difference is: the used precursor of present embodiment is for fluoridizing CuPc, and the amount of presoma is 30mg-50mg; Be put in the high-temperature zone of vacuum tube furnace with the porcelain boat of fluoridizing the CuPc presoma is housed, get the oxidized silicon chip of 1 * 2cm plating 6nm gold, place it in airflow downstream apart from the low-temperature region of high temperature center 10-20cm, the sealing vacuum tube furnace; After being pumped in the furnace chamber pressure and being lower than the body pressure to the described furnace chamber of bleeding and being lower than 1 Pa, feeding non-oxidizable shielding gas to the pressure in the described furnace chamber in the furnace chamber is 4x1O
4Pa-6x1O
4Pa, the body pressure to the furnace chamber of bleeding again is lower than 1 Pa, so guarantees for 3 times repeatedly in the tube chamber with argon gas the pressure in the chamber to be charged to 220Pa, the sealed vacuum pipe for behind the state of anaerobic; Beginning is heated to 415 ℃ with 20 ℃/minute speed with the high-temperature zone of furnace chamber, and continues 10 minutes-30 minutes under 415 ℃ situation.
Product is directly taken out from furnace chamber, (as Fig. 6) can be observed the direction of falling along temperature from its optical photograph, be 3cm by the right of high temperature to the length of the resultant product in the left side of low temperature, bigger and its area of the product area that obtains only is subject to the size of vacuum chamber and growth warm area.Resulting 1-dimention nano linear array is observed under SEM.Shown in Fig. 7 (a), can be observed length be about 10 microns fluoridize CuPc nano-wire array structure perpendicular to metal base.
The above only for the preferred embodiment of invention, is not limited to the present invention, and for a person skilled in the art, the present invention can have various changes and variation.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. method for preparing orderly one dimension organic nano linear array may further comprise the steps:
Step 1) adopts electron beam deposition technology thick gold nano grain film of evaporation 5-8 nm on the silicon of cleaning or silicon oxide substrate;
Step 2) utilizes the substrate of modifying gold nano grain to be growth substrate, adopt physical vaporous deposition to prepare the organic single-crystal nano-wire array.
2. the method for the orderly one dimension organic nano of preparation according to claim 1 linear array, it is characterized in that, described physical vaporous deposition (PVD) preparation organic single-crystal nano-wire array in the described step (2), concrete growth step is as follows: the presoma that will prepare described organic nano linear array according to the flow direction of air-flow places porcelain boat, and puts it into the center warm area of vacuum tube furnace; Get the cold zone that gold-plated substrate places described vacuum tube furnace, described substrate distance center warm area 10-2Ocm; Start vacuum pump, be evacuated to after pressure is lower than 1 Pa in the described furnace chamber, feeding inert protective gas argon gas to the pressure in the described furnace chamber in the furnace chamber is 4 * 10
4-6 * 10
4Pa is evacuated to again that pressure is lower than 1 Pa in the furnace chamber, after so repeating to guarantee that remnant oxygen is all taken away in the tube chamber 3 times, feeds argon gas toward silica tube in, and the maintenance gas flow rate is 30-60 sccm, and the chamber internal gas pressure is transferred to 220-260 Pa, the sealed vacuum pipe; Open heating unit, with 10-20 ℃/minute temperature rise rate, the center warm area of described vacuum tube furnace is heated to the vaporization temperature of described precursor, this moment, the temperature of center warm area was 380-420 ℃, and the temperature of growth substrates is 100-200 ℃; Keep and stop heating after above-mentioned vaporization temperature 10-60 minute, and make system naturally cool to room temperature, in described furnace chamber, feed argon gas to a normal atmosphere then, open furnace chamber, can obtain the one dimension organic nano linear array of large-area ordered crossed orientation growth in described growth substrates.
3. according to the method for claim 1, the orderly one dimension organic nano of 2 described preparations linear array, it is characterized in that, the presoma for preparing described one dimension organic nano linear array is to can be used in the material that physical vaporous deposition carries out nanostructure growth, gold thin film on the described substrate in described step (1), (2) exists with the form of discontinuous nano-particular film, in the grown effect of catalysis nucleation of nano array structure.
4. the method for the orderly one dimension organic nano of preparation according to claim 1 linear array, it is characterized in that, in the described step (2), when feeding non-oxidizing gas to normal atmosphere in the described furnace chamber, for the air flow that prevents from pouring in is suddenly destroyed the organic nano array structure, the flow of the non-oxidizing gas that feeds is not higher than 1O0sccm, and making temperature optimized temperature when the CuPc nano-wire array is grown of described vacuum tube furnace center warm area in the described step (2) is 415 ℃.
5. according to the method for claim 1, the orderly one dimension organic nano of 2 described preparations linear array, it is characterized in that, used non-oxidized gas is nitrogen, argon gas or hydrogen argon (volume ratio 95: 5) mixed gas etc. among the described preparation method, and described one dimension organic nano linear array is classified CuPc nano-wire array, phthalocyanine cobalt nanowire array, Phthalocyanine Zinc nano-wire array, FePC nano-wire array as, fluoridizes the CuPc nano-wire array and fluoridized phthalocyanines derivates such as phthalocyanine cobalt nanowire array.
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| CN116463627A (en) * | 2023-04-18 | 2023-07-21 | 陕西科技大学 | Indium phosphide nanowire and preparation method thereof |
| CN116463627B (en) * | 2023-04-18 | 2024-03-15 | 陕西科技大学 | Indium phosphide nanowire and preparation method thereof |
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