CN105294706A - Iron phthalocyanine nanowire with new crystal structure and preparation method of iron phthalocyanine nanowire - Google Patents
Iron phthalocyanine nanowire with new crystal structure and preparation method of iron phthalocyanine nanowire Download PDFInfo
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- CN105294706A CN105294706A CN201510735830.3A CN201510735830A CN105294706A CN 105294706 A CN105294706 A CN 105294706A CN 201510735830 A CN201510735830 A CN 201510735830A CN 105294706 A CN105294706 A CN 105294706A
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- 239000002070 nanowire Substances 0.000 title claims abstract description 42
- KMHSUNDEGHRBNV-UHFFFAOYSA-N 2,4-dichloropyrimidine-5-carbonitrile Chemical compound ClC1=NC=C(C#N)C(Cl)=N1 KMHSUNDEGHRBNV-UHFFFAOYSA-N 0.000 title abstract 4
- 239000013078 crystal Substances 0.000 title description 15
- 238000002360 preparation method Methods 0.000 title description 8
- 238000002441 X-ray diffraction Methods 0.000 claims abstract description 5
- 238000012360 testing method Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 31
- 239000012159 carrier gas Substances 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 20
- 239000002994 raw material Substances 0.000 claims description 16
- 238000010792 warming Methods 0.000 claims description 14
- 239000011810 insulating material Substances 0.000 claims description 8
- 238000004821 distillation Methods 0.000 claims description 5
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000002329 infrared spectrum Methods 0.000 claims description 3
- 238000001228 spectrum Methods 0.000 abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 18
- 239000007789 gas Substances 0.000 description 13
- 239000000377 silicon dioxide Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical group N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 4
- 239000012535 impurity Substances 0.000 description 3
- 238000000859 sublimation Methods 0.000 description 3
- 230000008022 sublimation Effects 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- -1 Phthalocyanine compound Chemical class 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000001947 vapour-phase growth Methods 0.000 description 2
- 238000009423 ventilation Methods 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 206010034972 Photosensitivity reaction Diseases 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- PZZYQPZGQPZBDN-UHFFFAOYSA-N aluminium silicate Chemical compound O=[Al]O[Si](=O)O[Al]=O PZZYQPZGQPZBDN-UHFFFAOYSA-N 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 229930002875 chlorophyll Natural products 0.000 description 1
- 235000019804 chlorophyll Nutrition 0.000 description 1
- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical compound C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009415 formwork Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000002428 photodynamic therapy Methods 0.000 description 1
- 230000036211 photosensitivity Effects 0.000 description 1
- 150000004032 porphyrins Chemical class 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D487/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00
- C07D487/22—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00 in which the condensed system contains four or more hetero rings
-
- 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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- 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)
- Nitrogen Condensed Heterocyclic Rings (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses an iron phthalocyanine nanowire. An X-ray diffraction spectrum (test conditions: CuKalpha1, lambda =1.54056 angstrom, 0.02 degree/step/2s) of the iron phthalocyanine nanowire has characteristic peaks at following parts: at values of 2theta+/-0.10 DEG, wherein values of 2theta are 6.92 degrees, 8.70 degrees, 9.88 degrees, 15.67 degrees, 24.11 degrees and 26.06 degrees, and corresponds to the 2theta; the half-peak widths are 0.562, 0.515, 0.324, 0.502, 0.336 and 0.306 respectively and correspond to the 2theta respectively; the relative diffraction intensities are 100%, 6.5%, 4.7%, 18.2%, 4.4% and 8.7% respectively.
Description
Technical field
Embodiments of the invention relate to a kind of new crystalline structure FePC nano wire and preparation method thereof.
Background technology
Phthalocyanine ring is a large conjugate ring with 18 π-electrons, and structure is very similar to natural porphyrin, chlorophyll and protoheme.Phthalocyanine compound is formed after hydrogen atom in the middle of phthalocyanine ring is substituted by metallic element; Iron two hydrogen atoms of substituted phthalocyanine ring can form FePCs as the more metallic element of content on the earth.FePC is a kind of excellent functional materials, due to the catalytic activity of its uniqueness, photosensitivity, photoconductivity, light stability and the character such as non-linear, has been applied to the fields such as catalyzer, fuel cell, light-guide material and CD.
Generally, the difference of preparation condition and method can obtain the FePC crystal of different crystal structure and different size, and the crystal of different structure and size is in character and the difference functionally having essence.Usually, the method preparing FePC have concentrated sulfuric acid solution recrystallization method, physical vaporous deposition, electrochemical deposition method, alumina formwork method, solution gradient falling temperature method FePC microwave method and in sealing system Solid-state pyrolyses method etc.These preparation methods can obtain the FePC crystal that crystal formation is α, β type usually, and these crystal are mainly needle-like, bar-shaped etc. on pattern.
Due to these patterns FePC crystal due to size thick, shortcomings such as solvent solubility is low, and can not effectively control its size and structure etc. in nanometer scale and limit the utilization of FePC.With this, based on the research of organic vapor phase deposition method in organic semiconductor nano material, pass through temperature by organic vapor phase deposition method, the regulation and control of the conditions such as the flow velocity of current-carrying gas can be prepared in a large number but be different from existing FePC structure, diameter is in nanometer scale, and nano wire bundle length reaches the high purity FePC nano wire of millimeter magnitude.And then, new phthalocyanine iron can be applied in nonlinear optics, electrochemistry, the different field such as photodynamic therapy, photoconductive material.
Summary of the invention
Embodiments of the invention relate to a kind of FePC nano wire, the x-ray diffraction pattern (test condition: Cu of described FePC nano wire
k α 1,
0.02 °/step/2s) at a following ° place, 2 θ ± 0.10, there is characteristic peak: 6.92 °, 8.70 °, 9.88 °, 15.67 °, 24.11 °, 26.06 °; And corresponding to above-mentioned 2 θ, peak width at half height is respectively 0.562,0.515,0.324,0.502,0.336,0.306; Correspond respectively to above-mentioned 2 θ, relative diffracted intensity is respectively 100%, 6.5%, 4.7%, 18.2%, 4.4%, 8.7%.
Optionally, described FePC nano wire has following fourier conversion infrared spectrum (FTIR) characteristic peak: 725cm
-1, 752cm
-1, 775cm
-1, 1080cm
-1, 1118cm
-1, 1165cm
-1, 1288cm
-1, 1330cm
-1, 1419cm
-1, 1493cm
-1, 1512cm
-1, 1612cm
-1.
Optionally, the mean diameter of described FePC nano wire is about 70nm.
Embodiments of the invention also provide a kind of method preparing FePC nano wire, comprise the following steps:
A) FePC raw material is placed in the heating region of tube furnace;
B) under carrier gas atmosphere, heating FePC raw material is extremely the highest 500 DEG C, the gaseous state FePC be elevated;
C) by this carrier gas, the gaseous state FePC of this distillation is guided to leave this heating region, to the temperature growth district that comparatively this heating region is low;
D) at this growth district, FePC nano wire is obtained.
Optionally, at described step b) in, heating FePC raw material is to the highest 490 DEG C, preferably the highest 460 DEG C.
Optionally, the temperature of described growth district, below 150 DEG C, preferably below 100 DEG C, more preferably below 50 DEG C, most preferably is room temperature.
Optionally, at described step b) in, heat in the mode of ladder-elevating temperature, be first preheated to 400 DEG C, and then staged is warming up to top temperature, the warming room that described staged heats up is divided into 1 DEG C-30 DEG C and temperature rise rate is 1 DEG C-5 DEG C/min.
Optionally, the flow velocity of described carrier gas in ingress is 0.2L/min-0.6L/min, and described carrier gas is being 0.2L/min-0.6L/min by flow velocity during described FePC raw material.
Optionally, the gap of 60-90mm is set between described heating region and described growth district; Wherein temperature insulating material is set in gap, and in temperature insulating material, ventilating pit is set.
Optionally, the flow velocity of described carrier gas in described ventilating pit is 1L/min-9L/min.
Accompanying drawing explanation
In order to be illustrated more clearly in the technical scheme of the embodiment of the present invention, be briefly described below by the accompanying drawing of embodiment, apparently, the accompanying drawing in the following describes only relates to some embodiments of the present invention, but not limitation of the present invention.
The FePC nano wire XRD figure spectrum that Fig. 1 provides for one embodiment of the invention;
Fig. 2 is α-FePC and β-FePC XRD figure spectrum
The FTIR collection of illustrative plates of the FePC raw material that Fig. 3 provides for an embodiment of the present invention and FePC nano wire;
The FePC nano wire SEM collection of illustrative plates that Fig. 4 provides for one embodiment of the invention.
Embodiment
For making the object of the embodiment of the present invention, technical scheme and advantage clearly, below in conjunction with the accompanying drawing of the embodiment of the present invention, the technical scheme of the embodiment of the present invention is clearly and completely described.Obviously, described embodiment is a part of embodiment of the present invention, instead of whole embodiments.Based on described embodiments of the invention, the every other embodiment that those of ordinary skill in the art obtain under without the need to the prerequisite of creative work, all belongs to the scope of protection of the invention.
Unless otherwise defined, the technical term that uses of the disclosure or scientific terminology should be in field belonging to the present invention the ordinary meaning that the personage with general technical ability understands." first " " second " used in patent application specification of the present invention and claims and similar word do not represent any order, quantity or importance, and are only used to distinguish different integral parts.Equally, the similar word such as " " or " " does not represent quantity limitation yet, but represents to there is at least one." connection " or " being connected " etc. similar word be not defined in physics or the connection of machinery, no matter but can comprise electrical connection, be direct or indirectly.
In one embodiment of the invention, the x-ray diffraction pattern (test condition: Cu of FePC nano wire
k α 1,
0.02 °/step/2s) at a following ° place, 2 θ ± 0.10, there is characteristic peak: 6.92 °, 8.70 °, 9.88 °, 15.67 °, 24.11 °, 26.06; And correspond to above-mentioned 2 θ, peak width at half height is respectively 0.562,0.515,0.324,0.502,0.336/0.306; Correspond respectively to above-mentioned 2 θ, relative diffracted intensity is respectively 100%, 6.5%, 4.7%, 18.2%, 4.4%, 8.7%.
In one embodiment of the invention, FePC nano wire has following fourier conversion infrared spectrum (FTIR) characteristic peak: 725cm
-1, 752cm
-1, 775cm
-1, 1080cm
-1, 1118cm
-1, 1165cm
-1, 1288cm
-1, 1330cm
-1, 1419cm
-1, 1493cm
-1, 1512cm
-1, 1612cm
-1.
Fig. 1 shows the X-ray diffraction spectrogram of the FePC nano wire that one embodiment of the invention provides.The SEM of the FePC nano wire that one embodiment of the invention obtains as shown in Figure 4.
Embodiments of the invention additionally provide a kind of vapour deposition process preparing FePC nano wire, comprise the following steps:
A) FePC raw material is placed in the heating region of tube furnace;
B) under carrier gas atmosphere, heating FePC raw material is extremely the highest 500 DEG C, the gaseous state FePC be elevated;
C) by this carrier gas, the gaseous state FePC of this distillation is guided to leave this heating region, to the temperature growth district that comparatively this heating region is low;
D) at this growth district, FePC nano wire is obtained.
In preparation process, in above-mentioned steps a), first FePC is incorporated into the heating region in tube furnace.Optionally, FePC is placed in the sealed tube being arranged in tube furnace.Sealing pipe can be silica tube, and can be affect the pipe that crystalline other material any of FePC makes yet, and includes, but not limited in the pipe that the materials such as stainless steel, silicon, aluminum oxide, pottery, glass are formed.These materials also can be placed in sealed tube with the form of substrate, such as, in silica tube.
After adding FePC, pass into carrier gas toward heating region.This carrier gas can be such as nitrogen (N
2), argon gas (Ar) or helium (He).Under the existence of this carrier gas, heating FePC is to preset target temperature.But as long as it is the FePC that gas is unlikely to again to generate other crystal formation that the selection of temperature can make FePC raw material distil.Cause generating the FePC of other crystal formation for effectively preventing Heating temperature too high, such as, above-mentioned steps b) in, heating FePC raw material is to the highest 500 DEG C, preferably the highest 490 DEG C, preferably the highest 470 DEG C further, preferably the highest 460 DEG C further.
At described step b) in, such as can heat in the mode of ladder-elevating temperature.Such as, be first preheated to 400 DEG C, and then staged is warming up to target temperature, remains on this temperature certain hour.The warming room that described staged heats up every such as 1 DEG C-30 DEG C can be set to, preferably with the warming room of 1 DEG C, 2 DEG C, 5 DEG C, 8 DEG C, 10 DEG C, 15 DEG C, 20 DEG C, 25 DEG C or 30 DEG C every intensification, temperature rise rate such as can be set to 1 DEG C-5 DEG C/min.Warming room every implication be if such as warming room is divided into 1 DEG C, then raise held for some time after 1 DEG C, then continue to heat up.Adopt the effect of stage intensification to be that FePC can distil more reposefully, obtain FePC gas more stably, thus advantageously in the formation of new crystalline structure FePC nano wire.
At above-mentioned steps c) in, the temperature of described growth district, below 150 DEG C, preferably below 100 DEG C, more preferably below 50 DEG C, most preferably is room temperature.The temperature of growth district is lower than the temperature of heating region, thus the FePC gas of distillation can be solidified as FePC crystal at growth district.The temperature of growth district is unsuitable too high.Too high, FePC gas crystallization can generate other crystalline structure, such as beta crystal.
In step c) in, the FePC gas that obtains of distilling by carrier gas by fast transportation to FePC nanowire growth region.In transportation, fast turn-around FePC sublimation gases, avoids FePC nano wire at other crystal formation FePC of outgrowth of growth district.Optionally, growth district adjoins heating region.Or growth district also can away from heating region.Optionally, between growth district and heating region, there is certain interval, the gap of such as 40-100mm, or the gap of 50-95mm, or the gap of 60-90mm.Temperature insulating material can be filled in the gap.Temperature insulating material includes, but not limited to Calucium Silicate powder, pure aluminium silicate, Teflon (Teflon) or urethane.Providing holes in this temperature insulating material, to make to guide the carrier gas of FePC gas to pass through.The number in hole and diameter can be arranged as required.Such as, the number in hole is 1-12; The diameter in hole is 3-8mm.The setting of passing hole, makes carrier gas being compared by the flow velocity (L/min) during above described holes be greatly improved with by the flow velocity (L/min) during FePC raw material.Thus, delivery FePC sublimation gases is made can to arrive growth district fast.The FePC crystal of the embodiment of the present invention, such as lower than 150 DEG C, or lower than 100 DEG C, or lower than the growth district growth of 50 DEG C, or grows in room temperature region.
In the process preparing FePC nano wire, can carry out at ambient pressure.This prepares FePC nano wire process, also can as required, in vacuum or add pressure and carry out.In the whole process of preparation, the flow of carrier gas needs to keep stable.Carrier gas is generally 0.1L/min-1L/min at the flow velocity of ingress, or 0.2L/min-0.5L/min.When passing through the hole in above-mentioned temperature insulating material, the flow velocity (speed) of described carrier gas can be 1L/min-20L/min, or the flow velocity of carrier gas is 1L/min-9L/min, or the flow velocity of carrier gas is 2L/min-6L/min, or the flow velocity of carrier gas is 3L/min-5L/min.Carrier gas guides FePC sublimation gases quickly through each warm area, reduces the region growing crystal outside growth district.
Method of the present invention is cleaned the step of this silica tube, is included, but are not limited to before being also included in and introducing FePC:
(1) with an organic solvent acetone, dehydrated alcohol, washed with de-ionized water silica tube and substrate, the impurity on removing silica tube and substrate;
(2) high pure nitrogen gas is used to dry up impurity remaining on silica tube and substrate and water;
(3) vacuum system is used to vacuumize silica tube cavity before preparation, to remove the impurity such as air in silica tube.
The above-mentioned FePC nano wire that the embodiment of the present invention provides is after long-time preservation, and its physicochemical property keep stable.
Illustrate implementation of the present invention by the following examples.
Embodiment 1:
Adopt the list temperature section open tubular furnace of temperature control able to programme.FePC raw material is placed in the middle position of this tube furnace high temperature section.Carrier gas N
2flow set be 0.4L/min.Logical 30min minute N
2after gas, to FePC heating raw materials.First be heated to 400 DEG C, after reaching 400 DEG C, be warming up to 420 DEG C with the speed of 4 DEG C/min.After reaching 420 DEG C, insulation 20min, is then warming up to 440 DEG C with the speed of 4 DEG C/min.After reaching 440 DEG C, insulation 20min, is then warming up to 460 DEG C with the speed of 2 DEG C/min.Reach 460 DEG C and be incubated 180min.Distillation FePC gas is transported to growth district by carrier gas.After being incubated, stop heating, continue logical N
230min, obtains FePC nano wire.
Embodiment 2:
On the basis of embodiment 1, adopt the list temperature section open tubular furnace of temperature control able to programme, regulation and control N
2the flow of ingress is 0.6L/min, in the ladder-elevating temperature mode of 400 DEG C, 440 DEG C, 460 DEG C, 480 DEG C, 490 DEG C, 500 DEG C, is warming up to 500 DEG C, insulation 300min.This growth district is connected with the silica tube that an internal diameter is 5mm with heating region.By small-bore pipe, the flow velocity of carrier gas is increased to 3.6L/min.After heating terminates, continue ventilation 30min, then stop ventilation, FePC nano wire grows in room temperature section.
Embodiment 3:
On the basis of embodiment 2, adopt the list temperature section open tubular furnace of temperature control able to programme, regulation and control N
2the flow of ingress is 0.6L/min, in the ladder-elevating temperature mode of 400 DEG C, 420 DEG C, 450 DEG C, 460 DEG C, is warming up to 460 DEG C, insulation 300min.Obtain FePC nano wire.
Embodiment 4:
Change experiment condition: substrate material is simple glass, temperature and type of heating repeat embodiment 1, and temperature stops heating after reaching 460 DEG C of maintenance 180min, and FePC the fabricate of nanowires terminates, and collects FePC nano wire.
The above is only exemplary embodiment of the present invention, but not for limiting the scope of the invention, protection scope of the present invention is determined by appended claim.
Claims (10)
1. a FePC nano wire, is characterized in that the x-ray diffraction pattern (test condition: Cu of described FePC nano wire
k α 1,
0.02 °/step/2s) at a following ° place, 2 θ ± 0.10, there is characteristic peak: 6.92 °, 8.70 °, 9.88 °, 15.67 °, 24.11 °, 26.06 °; And corresponding to above-mentioned 2 θ, peak width at half height is respectively 0.562,0.515,0.324,0.502,0.336,0.306; Correspond respectively to above-mentioned 2 θ, relative diffracted intensity is respectively 100%, 6.5%, 4.7%, 18.2%, 4.4%, 8.7%.
2. FePC nano wire according to claim 1, is characterized in that described FePC nano wire has following fourier conversion infrared spectrum (FTIR) characteristic peak: 725cm
-1, 752cm
-1, 775cm
-1, 1080cm
-1, 1118cm
-1, 1165cm
-1, 1288cm
-1, 1330cm
-1, 1419cm
-1, 1493cm
-1, 1512cm
-1, 1612cm
-1.
3. FePC nano wire according to claim 1 and 2, is characterized in that the mean diameter of described FePC nano wire is for about 70nm.
4. prepare a method for FePC nano wire, comprise the following steps:
A) FePC raw material is placed in the heating region of tube furnace;
B) under carrier gas atmosphere, heating FePC raw material is extremely the highest 500 DEG C, the gaseous state FePC be elevated;
C) by this carrier gas, the gaseous state FePC of this distillation is guided to leave this heating region, to the temperature growth district that comparatively this heating region is low;
D) at this growth district, FePC nano wire is obtained.
5. method according to claim 4, is characterized in that described step b) in, heating FePC raw material is to the highest 490 DEG C, preferably the highest 460 DEG C.
6. method according to claim 4, is characterized in that the temperature of described growth district is below 150 DEG C, preferably below 100 DEG C, more preferably below 50 DEG C, most preferably is room temperature.
7. the method according to any one of claim 4-6, it is characterized in that at described step b) in, heat in the mode of ladder-elevating temperature, first be preheated to 400 DEG C, and then staged is warming up to top temperature, the warming room that described staged heats up is divided into 1 DEG C-30 DEG C and temperature rise rate is 1 DEG C-5 DEG C/min.
8. the method according to any one of claim 4-6, is characterized in that, the flow velocity of described carrier gas in ingress is 0.2L/min-0.6L/min, and described carrier gas is being 0.2L/min-0.6L/min by flow velocity during described FePC raw material.
9. method according to claim 8, is characterized in that, arranges the gap of 60-90mm between described heating region and described growth district; Wherein temperature insulating material is set in gap, and in temperature insulating material, ventilating pit is set.
10. method according to claim 9, is characterized in that, the flow velocity of described carrier gas in described ventilating pit is 1L/min-9L/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510735830.3A CN105294706B (en) | 2015-11-03 | 2015-11-03 | New crystal structure phthalocyanine Fe nanowire and preparation method thereof |
Applications Claiming Priority (1)
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Cited By (2)
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| CN110034232A (en) * | 2019-04-05 | 2019-07-19 | 东北师范大学 | Using FePC as the preparation method and application of the field effect transistor of raw material |
| CN113956261A (en) * | 2021-09-16 | 2022-01-21 | 昆明学院 | Novel crystal structure chlorinated gallium phthalocyanine nanobelt and preparation method thereof |
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| CN110034232A (en) * | 2019-04-05 | 2019-07-19 | 东北师范大学 | Using FePC as the preparation method and application of the field effect transistor of raw material |
| CN113956261A (en) * | 2021-09-16 | 2022-01-21 | 昆明学院 | Novel crystal structure chlorinated gallium phthalocyanine nanobelt and preparation method thereof |
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