CN105601637A - Preparation method of zinc tetraphenylporphyrin nano material with high spectrum absorption ability and high carrier mobility - Google Patents

Preparation method of zinc tetraphenylporphyrin nano material with high spectrum absorption ability and high carrier mobility Download PDF

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CN105601637A
CN105601637A CN201610030408.2A CN201610030408A CN105601637A CN 105601637 A CN105601637 A CN 105601637A CN 201610030408 A CN201610030408 A CN 201610030408A CN 105601637 A CN105601637 A CN 105601637A
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preparation
heating
tetraphenylporphyrin
nano material
tetraphenylporphyrin zinc
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CN105601637B (en
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王海
杨镒吉
张俊
赵建红
王晓燕
于雷鸣
刘颖
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Kunming University
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    • 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
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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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Abstract

The invention discloses a preparation method of zinc tetraphenylporphyrin nano material with high spectrum absorption ability and high carrier mobility. The preparation method includes: preprocessing, preparing materials, heating and growing, to be more specific, cleaning and drying a reaction platform, placing 5-30mg of zinc tetraphenylporphyrin in the sealed tube, located in a heating area, of a tube furnace, vacuumizing the wall of the sealed tube to remove impurities and moisture, feeding carrier gas according to the flow of 300-500sccm, heating the zinc tetraphenylporphyrin to 320-420 DEG C at the temperature-rising speed of 1-10 DEG/minute, keeping the temperature for 190-300 minutes after the temperature reaches the standard, using the carrier gas to guide the sublimated zinc tetraphenylporphyrin gas to a growing area from the heating area, and collecting the zinc tetraphenylporphyrin nano material in the growing area. The preparation method has the advantages that the method is simple and efficient, a large amount of uniform zinc tetraphenylporphyrin nano material with a special morphology structure can be prepared, the average diameter of the zinc tetraphenylporphyrin nano material is below 80 nanometers, fission and red shift of the ultraviolet-visible light absorption spectrum of the zinc tetraphenylporphyrin nano material occur, and the spectrum absorption ability and carrier mobility of the zinc tetraphenylporphyrin nano material are improved.

Description

The preparation method of the tetraphenylporphyrin zinc nano material that a kind of spectral absorption ability is strong, carrier mobility is high
Technical field
The invention belongs to nano material preparing technical field, be specifically related to that a kind of spectral absorption ability is strong, carrier mobilityThe preparation method of the tetraphenylporphyrin zinc nano material that rate is high.
Background technology
In field of molecular electronics, the organic molecule material of small scale and the combination of molecular device, construct, bring moreCarry out more opportunities and challenges. Especially at Organic Light Emitting Diode (OLED), gas sensor, OTFT(OTFT), the aspect such as organic solar batteries (OSC). Wherein, low-dimensional organic semiconductor nano material is due to its excellent opticsCharacter and stable chemical property are also more and more subject to people's attention.
Due to different preparation methods, what tetraphenylporphyrin zinc can implementation structure pattern regulates and controls, for its uniquenessStructural system and physical property have outstanding effect in nano science and bio-science field. The physics of porphyrin nano materialLearning character and its appearance structure feature has very large correlation, at present, has had mixed solvent method, surfactant to assist from groupDress (SAS), ion self assembly, evaporation and diffusion method etc., for the preparation of synthetic porphyrin nano material, show different morphologies knot simultaneouslyStructure, as: rhombus, rectangle, helical form and flakes etc.
Preparation and the assembling of and preparation method simple small size nano material special for pattern, regulate and control it and grewJourney is focus and the difficult point of Recent study nano material. And after all the most important nano material that is still in preparation processIn controllable growth and assembling, the structure that realizes nano material is controlled, thus realize low-dimension nano material is applied to device layerUltimate aim on face.
The present invention selects the organic semiconducting materials of this excellent performance of tetraphenylporphyrin zinc as analytic target, to its thingReason, chemical property are studied, and adopt organic vapor phase deposition equipment by regulation and control deposition parameter, little to simple a large amount of acquisitionsSize tetraphenylporphyrin zinc nano material, the preparation process of simplification tetraphenylporphyrin zinc nano material, reduces its production cost, thisApplication and Development for following nanoelectronic components and parts, chemical sensor and artificial photosynthesis's system is important by playing undoubtedlyFacilitation.
Summary of the invention
The object of the present invention is to provide the tetraphenylporphyrin zinc that a kind of spectral absorption ability is strong, carrier mobility is high to receiveThe preparation method of rice material.
The object of the present invention is achieved like this: the tetraphenyl porphin that described spectral absorption ability is strong, carrier mobility is highThe preparation method of quinoline zinc nano material, the operation that comprises pretreatment, gets the raw materials ready, heats and grow, specifically comprises:
A, pretreatment: clean and dry reaction platform, remove impurity and moisture;
B, get the raw materials ready: the sealed tube that tetraphenylporphyrin zinc source material 5 ~ 30mg is placed in to tube furnace and is arranged in heating region;
C, heating: introduce after tetraphenylporphyrin zinc source material, sealed tube body of wall is vacuumized, remove impurity and moisture; Then pressThe flow of 300 ~ 500sccm passes into carrier gas, in carrier gas environment, according to the programming rate of 1 ~ 10 DEG C/min, heats tetraphenylporphyrinZinc source material to 320 ~ 420 DEG C, are incubated 190 ~ 300min after reaching target temperature, and making the distillation of tetraphenylporphyrin zinc source material is gasBody;
D, growth: utilize the tetraphenylporphyrin zinc gas of the carrier gas guiding distillation passing into from heating region to growth district, insulationAfter end, in growth district, collect tetraphenylporphyrin zinc nano material.
The preparation method of nano material of the present invention compared with prior art has following advantages and effect:
(1) described preparation method is using the tetraphenylporphyrin zinc of the large ring of planar conjugate of stable chemical nature, symmetrical configuration as sourceMaterial, adopts organic vapor phase deposition technology to prepare tetraphenylporphyrin zinc nano material, for example, by regulation and control deposition parameter: sourceTemperature, gas flow, thermograde, backing material etc., acquisition small size tetraphenylporphyrin zinc nano material that can be a large amount of.
(2) described preparation method can obtain evenly, the tetraphenylporphyrin zinc nano material of a large amount of, specific morphology structure, straightFootpath is on average below 80nm, and the phenomenon of fission, red shift has occurred its ultraviolet-visible absorption spectra, improves and improved this nanometerSpectral absorption ability and the carrier mobility of material, can apply to nanoelectronic components and parts, chemical sensor, artificial light cooperationWith in field.
(3) the tetraphenylporphyrin zinc nano material physics, the stable chemical nature that adopt the method for the invention to prepare. MadeStandby nano material is preserved after time of 3 ~ 5 months at normal temperatures, and the SEM collection of illustrative plates retesting does not almost change, and sampleWater insoluble, non-hygroscopic.
(4) preparation process of described nano material need to be under vacuum, does not need pressurization yet, simple to operate, fastPrompt, efficiency is high, cost is low, equipment interoperability is good, easy to utilize.
Brief description of the drawings
Fig. 1 is the SEM collection of illustrative plates that adopts the tetraphenylporphyrin zinc nano material prepared of the method for the invention;
Fig. 2 is the FTIR collection of illustrative plates that adopts the tetraphenylporphyrin zinc nano material prepared of the method for the invention;
Fig. 3 is the XRD collection of illustrative plates that adopts the tetraphenylporphyrin zinc nano material prepared of the method for the invention;
Fig. 4 is the UV-vis collection of illustrative plates that adopts the tetraphenylporphyrin zinc nano material prepared of magic arts method of the present invention.
Detailed description of the invention
The present invention is further illustrated below, but never in any form the present invention is limited, based on the present inventionAny conversion or replacement that training centre is done, all belong to protection scope of the present invention.
The preparation side of the tetraphenylporphyrin zinc nano material that spectral absorption ability of the present invention is strong, carrier mobility is highMethod, the operation that comprises pretreatment, gets the raw materials ready, heats and grow, specifically comprises:
Described pretreatment process refers to: clean and dry reaction platform, remove impurity and moisture;
Described procedure for preparation refers to: the sealing that tetraphenylporphyrin zinc source material 5 ~ 30mg is placed in to tube furnace and is positioned at heating regionGuan Zhong;
Described heating process refers to: introduce after tetraphenylporphyrin zinc source material, sealed tube body of wall is vacuumized, remove impurity and waterPoint; Then pass into carrier gas by the flow of 300 ~ 500sccm, in carrier gas environment, according to the programming rate of 1 ~ 10 DEG C/min, heatTetraphenylporphyrin zinc source material to 320 ~ 420 DEG C, are incubated 190 ~ 300min after reaching target temperature, make tetraphenylporphyrin zinc source materialMaterial distillation is gas;
Described growth operation refers to: utilize the tetraphenylporphyrin zinc gas of the carrier gas guiding distillation passing into from heating region to growthTetraphenylporphyrin zinc nano material after insulation finishes, is collected in region in growth district.
Described tetraphenylporphyrin zinc molecular structure is as follows:
Described in pretreatment process, tube furnace can be level or vertically place, and described horizontal or vertical tube furnace can be singleAny in temperature section tube furnace or multiple temperature sections tube furnace, the furnace chamber of described tube furnace is wrapped with insulation material layer.
Described in pretreatment process, sealed tube can be any in quartz ampoule, stainless steel tube, glass tube or silicone tube; PreferablyQuartz ampoule. The inwall of preparing source material and be laid in described quartz ampoule and be positioned at heating region of described tetraphenylporphyrin zinc nano materialUpper, in this regional extent, place quartzy groove, described quartzy groove surrounding except two ground surface blockages is offered one or more littleHole.
Described in heating process, be before heating, sealed tube body of wall to be vacuumized to vacuumizing in sealed tube body of wall, make vacuumBe evacuated to and be less than 9Pa.
The effect vacuumizing is the effect of the impurity in body of wall and moisture being carried out an elimination before test heating, beBefore test heating, carry out.
Described in heating process, carrier gas can be N2Or any in Ar.
Described in heating process, heating refers to tetraphenylporphyrin zinc source material is warming up in the process of target temperature and is provided with temperatureDegree interlude, is respectively 310 DEG C, 330 DEG C, 350 DEG C, 355 DEG C, and each interlude is respectively incubated 20min.
Described in heating process, heating refers to tetraphenylporphyrin zinc source material is warming up in the process of target temperature and is provided with temperatureDegree interlude, be respectively 330 DEG C, 350 DEG C, 355 DEG C, 357 DEG C, 359 DEG C, each interlude be incubated successively 20min, 20min,10min、5min、2min。
Described in heating process, heating refers to tetraphenylporphyrin zinc source material is warming up in the process of target temperature and is provided with temperatureDegree interlude, temperature is 340 DEG C, insulation 190min.
Described in growth operation, heating region and growth district can directly be connected, or embed one or more transitional regions and carry outBe connected.
Described in growth operation, transitional region is filled with silicate heat-insulating heat-preserving material, and described silicate heat-insulating heat-preserving material canThink any in calcium silicates or alumina silicate.
Described in heating process and growth operation, passing into carrier gas comprises: before heating, pass into carrier gas, and before heating, keep logicalGas 30min; After insulation finishes, continue to keep ventilation 30min, regather tetraphenylporphyrin zinc nano material.
Embodiment 1
First, clean and dry reaction platform is the quartz ampoule in experiment porch and horizontal pipe furnace, removes impurity and moisture, adoptsWith PU1065 flexible pipe be gas path pipe, be connected and installed after consersion unit, tetraphenylporphyrin zinc source material 15mg is placed in and can be compiledIn the multiple temperature sections open-close type horizontal pipe furnace of program control temperature, be arranged in the quartz ampoule of heating region. Introduce tetraphenylporphyrin zinc source materialAfter, quartz ampoule body of wall is vacuumized, until being evacuated to, vacuum is less than 9Pa, further remove impurity and moisture. Then pressThe flow of 500sccm passes into N2As carrier gas, before startup heating, keep ventilation 30min, then at N2In compression ring border according to 1 ~ 10DEG C/programming rate of min, heating tetraphenylporphyrin zinc source material to 350 DEG C, is incubated 190min after reaching target temperature, makes fourThe distillation of phenyl zinc porphyrin source material is gas, and in preparation process, quartz ampoule cavity need keep normal pressure. The carrier gas that utilization passes into is drawnLead the tetraphenylporphyrin zinc gas of distillation from heating region to growth district, after insulation finishes, stop heating, continue to keep logicalGas 30min collects tetraphenylporphyrin zinc nano material in growth district.
Embodiment 2
First, clean and dry reaction platform is the quartz ampoule in experiment porch and horizontal pipe furnace, removes impurity and moisture, adoptsWith PU1065 flexible pipe be gas path pipe, be connected and installed after consersion unit, tetraphenylporphyrin zinc source material 20mg is placed in and can be compiledIn the multiple temperature sections open-close type horizontal pipe furnace of program control temperature, be arranged in the quartz ampoule of heating region. Introduce tetraphenylporphyrin zinc source materialAfter, quartz ampoule body of wall is vacuumized, until being evacuated to, vacuum is less than 9Pa, further remove impurity and moisture. Then pressThe flow of 500sccm passes into N2As carrier gas, before startup heating, keep ventilation 30min, then at N2In compression ring border according to 2 ~ 6 DEG C/The programming rate of min, heating tetraphenylporphyrin zinc source material to 360 DEG C is provided with temperature in the process that is warming up to target temperatureInterlude, is respectively 310 DEG C, 330 DEG C, 350 DEG C, 355 DEG C, and each interlude is respectively incubated 20min, is incubated after reaching target temperature190min, makes the distillation of tetraphenylporphyrin zinc source material for gas, and in preparation process, quartz ampoule cavity need keep normal pressure. Utilize logicalThe tetraphenylporphyrin zinc gas of the carrier gas guiding distillation entering, from heating region to growth district, stops heating after insulation finishes,Continue to keep ventilation 30min, in growth district, collect tetraphenylporphyrin zinc nano material.
Embodiment 3
First, clean and dry reaction platform is the quartz ampoule in experiment porch and horizontal pipe furnace, removes impurity and moisture, adoptsWith PU1065 flexible pipe be gas path pipe, be connected and installed after consersion unit, tetraphenylporphyrin zinc source material 10mg is placed in and can be compiledIn the multiple temperature sections open-close type horizontal pipe furnace of program control temperature, be arranged in the quartz ampoule of heating region. Introduce tetraphenylporphyrin zinc source materialAfter, quartz ampoule body of wall is vacuumized, until being evacuated to, vacuum is less than 9Pa, further remove impurity and moisture. Then pressThe flow of 500sccm passes into N2As carrier gas, before startup heating, keep ventilation 30min, then at N2In compression ring border according to 1 ~ 5 DEG C/The programming rate of min, heating tetraphenylporphyrin zinc source material to 360 DEG C is provided with temperature in the process that is warming up to target temperatureInterlude, is respectively 330 DEG C, 350 DEG C, 355 DEG C, 357 DEG C, 359 DEG C, each interlude be incubated successively 20min, 20min,10min, 5min, 2min, be incubated 190min after reaching target temperature, and making the distillation of tetraphenylporphyrin zinc source material is gas, in systemIn standby process, quartz ampoule cavity need keep normal pressure. The tetraphenylporphyrin zinc gas of the carrier gas guiding distillation that utilization passes into is from the thermal treatment zoneTerritory, to growth district, stops heating after insulation finishes, and continues to keep ventilation 30min, collects tetraphenyl porphin in growth districtQuinoline zinc nano material.
Embodiment 4
First, clean and dry reaction platform is the quartz ampoule in experiment porch and horizontal pipe furnace, removes impurity and moisture, adoptsWith PU1065 flexible pipe be gas path pipe, be connected and installed after consersion unit, tetraphenylporphyrin zinc source material 20mg is placed in and can be compiledIn the multiple temperature sections open-close type horizontal pipe furnace of program control temperature, be arranged in the quartz ampoule of heating region. Introduce tetraphenylporphyrin zinc source materialAfter, quartz ampoule body of wall is vacuumized, until being evacuated to, vacuum is less than 9Pa, further remove impurity and moisture. Then pressThe flow of 500sccm passes into N2As carrier gas, before startup heating, keep ventilation 30min, then at N2In compression ring border according to 1 ~ 10DEG C/programming rate of min, heating tetraphenylporphyrin zinc source material to 400 DEG C, is incubated 300min after reaching target temperature, makes fourThe distillation of phenyl zinc porphyrin source material is gas, and in preparation process, quartz ampoule cavity need keep normal pressure. The carrier gas that utilization passes into is drawnLead the tetraphenylporphyrin zinc gas of distillation from heating region to growth district, after insulation finishes, stop heating, continue to keep logicalGas 30min collects tetraphenylporphyrin zinc nano material in growth district.
Embodiment 5
First, clean and dry reaction platform is the quartz ampoule in experiment porch and horizontal pipe furnace, removes impurity and moisture, adoptsWith PU1065 flexible pipe be gas path pipe, be connected and installed after consersion unit, tetraphenylporphyrin zinc source material 20mg is placed in and can be compiledIn single temperature section open-close type horizontal pipe furnace of program control temperature, be arranged in the quartz ampoule of heating region. Introduce tetraphenylporphyrin zinc source materialAfter, quartz ampoule body of wall is vacuumized, until being evacuated to, vacuum is less than 9Pa, further remove impurity and moisture. Then pressThe flow of 400sccm passes into N2As carrier gas, before startup heating, keep ventilation 30min, then at N2In compression ring border according to 5 ~ 10DEG C/programming rate of min, heating tetraphenylporphyrin zinc source material to 350 DEG C, is incubated 210min after reaching target temperature, makes fourThe distillation of phenyl zinc porphyrin source material is gas, and in preparation process, quartz ampoule cavity need keep normal pressure. The carrier gas that utilization passes into is drawnLead the tetraphenylporphyrin zinc gas of distillation from heating region to growth district, after insulation finishes, stop heating, continue to keep logicalGas 30min collects tetraphenylporphyrin zinc nano material in growth district.
Embodiment 6
First, clean and dry reaction platform is the glass tube in experiment porch and horizontal pipe furnace, removes impurity and moisture, adoptsWith PU1065 flexible pipe be gas path pipe, be connected and installed after consersion unit, tetraphenylporphyrin zinc source material 5mg is placed in able to programmeIn the multiple temperature sections open-close type horizontal pipe furnace of temperature control, be arranged in the glass tube of heating region. Introduce tetraphenylporphyrin zinc source materialAfter, glass tube body of wall is vacuumized, until being evacuated to, vacuum is less than 9Pa, further remove impurity and moisture. Then pressThe flow of 460sccm passes into Ar as carrier gas, start heating before keep ventilate 30min, then in Ar compression ring border according to 2 ~ 7DEG C/programming rate of min, heating tetraphenylporphyrin zinc source material to 370 DEG C, is incubated 240min after reaching target temperature, makes fourThe distillation of phenyl zinc porphyrin source material is gas, and in preparation process, glass tube cavity need keep normal pressure. The carrier gas that utilization passes into is drawnLead the tetraphenylporphyrin zinc gas of distillation from heating region to growth district, after insulation finishes, stop heating, continue to keep logicalGas 30min collects tetraphenylporphyrin zinc nano material in growth district.
Embodiment 7
First, clean and dry reaction platform is the silicone tube in experiment porch and horizontal pipe furnace, removes impurity and moisture, adoptsPU1065 flexible pipe is gas path pipe, has been connected and installed after consersion unit, and tetraphenylporphyrin zinc source material 30mg is placed in able to programmeIn single temperature section open-close type horizontal pipe furnace of temperature control, be arranged in the silicone tube of heating region. Introduce after tetraphenylporphyrin zinc source material,Silicone tube body of wall is vacuumized, be less than 9Pa until vacuum is evacuated to, further remove impurity and moisture. Then press the stream of 350sccmAmount pass into Ar as carrier gas, start heating before keep ventilate 30min, then in Ar compression ring border according to the intensification of 4 ~ 9 DEG C/minSpeed, heating tetraphenylporphyrin zinc source material to 380 DEG C, is incubated 240min after reaching target temperature, makes tetraphenylporphyrin zinc sourceMaterial distillation is gas, and in preparation process, silicone tube cavity need keep normal pressure. The tetraphenyl of the carrier gas guiding distillation that utilization passes intoZinc porphyrin gas, from heating region to growth district, stops heating after insulation finishes, and continues to keep ventilation 30min, in growthIn region, collect tetraphenylporphyrin zinc nano material.

Claims (10)

1. a preparation method for the tetraphenylporphyrin zinc nano material that spectral absorption ability is strong, carrier mobility is high, its spyLevy the operation that is to comprise pretreatment, gets the raw materials ready, heats and grows, specifically comprise:
A, pretreatment: clean and dry reaction platform, remove impurity and moisture;
B, get the raw materials ready: the sealed tube that tetraphenylporphyrin zinc source material 5 ~ 30mg is placed in to tube furnace and is arranged in heating region;
C, heating: introduce after tetraphenylporphyrin zinc source material, sealed tube body of wall is vacuumized, remove impurity and moisture; Then pressThe flow of 300 ~ 500sccm passes into carrier gas, in carrier gas environment, according to the programming rate of 1 ~ 10 DEG C/min, heats tetraphenylporphyrinZinc source material to 320 ~ 420 DEG C, are incubated 190 ~ 300min after reaching target temperature, and making the distillation of tetraphenylporphyrin zinc source material is gasBody;
D, growth: utilize the tetraphenylporphyrin zinc gas of the carrier gas guiding distillation passing into from heating region to growth district, insulationAfter end, in growth district, collect tetraphenylporphyrin zinc nano material.
2. preparation method according to claim 1, is characterized in that sealed tube can be quartz ampoule, stainless described in operation AAny in steel pipe, glass tube or silicone tube.
3. preparation method according to claim 1, it is characterized in that described in operation C in sealed tube body of wall, vacuumize beBefore heating, sealed tube body of wall is vacuumized, vacuum is evacuated to and is less than 9Pa.
4. preparation method according to claim 1, is characterized in that carrier gas can be N described in operation C2Or arbitrary in ArKind.
5. preparation method according to claim 1, is characterized in that heating and referring to tetraphenylporphyrin zinc source described in operation CMaterial is warming up in the process of target temperature and is provided with temperature interlude, is respectively 310 DEG C, 330 DEG C, 350 DEG C, 355 DEG C, Mei GezhongBetween the each insulation of section 20min.
6. preparation method according to claim 1, is characterized in that heating and referring to tetraphenylporphyrin zinc source described in operation CMaterial is warming up in the process of target temperature and is provided with temperature interlude, is respectively 330 DEG C, 350 DEG C, 355 DEG C, 357 DEG C, 359 DEG C,Each interlude is incubated 20min, 20min, 10min, 5min, 2min successively.
7. preparation method according to claim 1, is characterized in that heating and referring to tetraphenylporphyrin zinc source described in operation CMaterial is warming up in the process of target temperature and is provided with temperature interlude, and temperature is 340 DEG C, insulation 190min.
8. preparation method according to claim 1, is characterized in that described in step D that heating region and growth district can be directBe connected, or embed one or more transitional regions and be connected.
9. preparation method according to claim 8, is characterized in that described in step D that transitional region is filled with silicate heat insulationInsulation material.
10. preparation method according to claim 1, is characterized in that passing into carrier gas described in operation C and step D comprises:Before heating, pass into carrier gas, and before heating, keep ventilation 30min; After insulation finishes, continue to keep ventilation 30min, regather fourPhenyl zinc porphyrin nano material.
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