CN103776856B - The characterizing method of a kind of organic molecule monocrystal material and application thereof - Google Patents
The characterizing method of a kind of organic molecule monocrystal material and application thereof Download PDFInfo
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- CN103776856B CN103776856B CN201210410863.7A CN201210410863A CN103776856B CN 103776856 B CN103776856 B CN 103776856B CN 201210410863 A CN201210410863 A CN 201210410863A CN 103776856 B CN103776856 B CN 103776856B
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Abstract
The invention provides characterizing method and the application thereof of a kind of organic molecule monocrystal material, the method includes 1) utilize dielectric material and organic semiconducting materials to form dielectric layer and organic semiconductor nano thin-film successively in contained network, the thickness of described organic semiconductor nano thin-film is 0.8 8nm；2) under the conditions of anhydrous and oxygen-free, the product that step 1) obtains is annealed, make described organic semiconductor nano thin-film be converted into organic single-crystal nano material；3) by step 2) product that obtains is placed under transmission electron microscope observation, and measures the size of organic single-crystal nano material, surface roughness and crystallinity.The method of the present invention prepares nanocrystal under lower temperature, condition of normal pressure, and products therefrom is in-situ preparation in contained network, it is not necessary to crystal retransfers step, and during crystal formation, crystal grain will not be contaminated or damage, and can be directly used for electron microscopic observation and sign.The inventive method is also particularly conducive to the analysis to intermediate states different in nanocrystal forming process.
Description
Technical field
The characterizing method and the application, particularly nanoscale that the present invention relates to a kind of organic molecule monocrystal material are organic little
The Electronic Speculum characterizing method of molecule monocrystal material and the method application in research organic single-crystal nanometer material structure.
Background technology
Coherent condition or the crystal structure of analyzing organic small molecule material can be that research organic solid electronics passes further
Defeated character provides the material foundation of indispensability with preparing organic electro-optic device.This is because the crystal structure of organic molecule directly reflects
The mode of piling up of molecule, and molecular stuffing arrangement will directly influence the density of electronic states (non-locality of electronics in such as π key
Matter).In existing document and patent, the growing method of organic crystal has multiple, is divided into chemical method and Physical.Organic crystal is steady
Qualitative difference, mechanical strength is low, so being highly vulnerable to breakage single crystal samples in transfer crystallization process, making structural analysis become extremely and being stranded
Difficult.The crystal that at present prepared by Applied Physics method carries out Micro-Structure Analysis, when particularly nanocrystal being carried out structural analysis, by
It is firmly combined with substrate in crystal, and crystalline size is too small so that sample transfer process is extremely difficult, it is impossible to realize sample
Intactly transfer adheres on copper mesh, is then placed in sample for use in transmitted electron microscope room and carries out constructed observation or electronic diffraction sign；Chemistry
Nanocrystal prepared by method can adhere on copper mesh with structural integrity and preferably, but crystal attaches the impurity effect in solution
Structural characterization and analysis.
Summary of the invention
It is an object of the invention to propose a kind of simple for tem study organic nanocrystal
The characterizing method of structure.
The invention provides characterizing method and the application thereof of a kind of organic molecule monocrystal material, it is characterised in that the party
Method includes:
1) dielectric material and organic semiconducting materials is utilized to form dielectric layer and organic semiconductor nanometer successively in contained network
Thin film, the thickness of described organic semiconductor nano thin-film is 0.8-8nm；
2) under the conditions of anhydrous and oxygen-free, the product that step 1) obtains is annealed, make described organic semiconductor nano thin-film
It is converted into organic single-crystal nano material；
3) by step 2) product that obtains is placed under transmission electron microscope observation, and measures organic single-crystal nano material
Size, surface roughness and crystallinity.
The present invention has the advantage that relative to prior art
What the present invention proposed is suitable to the organic molecule nano crystal that transmission electron microscope characterizes, and particularly Benzo[b is received
Rice crystalline material.Preparing nanocrystal under lower temperature, condition of normal pressure, products therefrom is in-situ preparation in contained network, it is not necessary to
Crystal retransfers step, and during crystal formation, crystal grain will not be contaminated or damage, and can be directly used for transmission electron microscopy
Sem observation and sign.As required, it is also possible to help researcher that intermediate states different in nanocrystal forming process are carried out careful
Analyze (can realize) by controlling annealing temperature and/or time.Anneal certain time under inert gas shielding environment,
Obtain required sign sample.During sign, crystal perfection can be kept, obtain complete nano crystal structure, it is possible to accurately
The required structural information analyzing sample of reflection, has certain universality.The characterizing method of the present invention solves and cannot obtain physics
The complete pattern of organic nanocrystal prepared by method and the shortcoming of structure, it also avoid chemical method prepare organic nanocrystal because of
Preparation condition and have the impact of exogenous impurity.
Other features and advantages of the present invention will be described in detail in detailed description of the invention part subsequently.
Accompanying drawing explanation
Accompanying drawing is used to provide a further understanding of the present invention, and constitutes the part of description, with following tool
Body embodiment is used for explaining the present invention together, but is not intended that limitation of the present invention.In the accompanying drawings:
Fig. 1 is material preparation tube furnace structural representation；
Fig. 2 is pentacene thin film atomic force microscopy；
Fig. 3 is the stereoscan photograph of Benzo[b nanometer monocrystalline monocrystal material on the copper mesh modified；
Fig. 4 is the electronic transmission electromicroscopic photograph of Benzo[b nano crystal material；
Fig. 5 is Benzo[b nano crystal material electronics diffraction pattern photo；
Fig. 6 is the electronic transmission electromicroscopic photograph of the intermediateness in Benzo[b nano crystal material formation process；
Fig. 7 is the electron diffraction pattern photo of the intermediateness in Benzo[b nano crystal material formation process.
Detailed description of the invention
Below in conjunction with accompanying drawing, the detailed description of the invention of the present invention is described in detail.It should be appreciated that this place is retouched
The detailed description of the invention stated is merely to illustrate and explains the present invention, is not limited to the present invention.
The invention provides the characterizing method of a kind of organic molecule monocrystal material, it is characterised in that the method includes:
1) dielectric material and organic semiconducting materials is utilized to form dielectric layer and organic semiconductor nanometer successively in contained network
Thin film, the thickness of described organic semiconductor nano thin-film is 0.8-8nm；
2) under the conditions of anhydrous and oxygen-free, the product that step 1) obtains is annealed, make described organic semiconductor nano thin-film
It is converted into organic single-crystal nano material；
3) by step 2) product that obtains is placed under transmission electron microscope observation, and measures organic single-crystal nano material
Size, surface roughness and crystallinity.
According to the present invention, described dielectric material can be that the various high temperature that are resistant to of this area routine (are at least resistant to
140 DEG C of high temperature and indeformable) high molecular polymer or inorganic material, under preferable case, described dielectric material is SiO2, poly-carbon
One in acid esters, polystyrene, polyimides and polymethyl methacrylate.
According to the present invention, described organic semiconducting materials can be commonly used in the art organic little point with biphenyl structural
Sub-material, preferably Benzo[b.It was found by the inventors of the present invention that the inventive method is particular enable to preferably characterize Benzo[b nanometer
The various features of monocrystal material.
According to the present invention, described contained network can be various contained networks commonly used in the art, can pass through commercially available, but
Under preferable case, described contained network is the one in copper mesh, nickel screen, molybdenum net, gold net and nylon wire.
According to the present invention, contained network forms dielectric layer primarily to form the smooth surface of low roughness, therefore, shape
Becoming the method for described dielectric layer can be the method for various routine, it is preferable that the method forming described dielectric layer is spin-coating method, magnetic
Control sputtering method and self-assembling method.
The thickness of described dielectric layer can select in relative broad range, as long as transmission electron microscope electron beam used can penetrate sample
Product form picture rich in detail.
According to the present invention, the method forming described organic semiconductor nano thin-film is preferably vacuum evaporatation.Described
The condition of vacuum vapor plating can select under the conditions of wider, but under preferable case, the condition bag of described vacuum vapor plating
Including deposition velocity is 0.001-0.05nm/s, and vacuum is 1 × 10-5-1×10-7Mbar, is formed with the load of dielectric layer during deposition
Temperature residing for net is 20-30 DEG C, and sedimentation time is 30-300s.
According to the present invention, in described annealing process, the molecule in described nano thin-film there occurs migration, is i.e. originally defined
The molecule of nano thin-film is met again, thus described nano thin-film by the membrane structure of original two dimension to three-dimensional crystal structure
Change, form undersized crystal grain (whole process is without departing from dielectric layer surface).Therefore, described annealing can be wider
Under the conditions of carry out, as long as described nano thin-film can be made to be converted into organic single-crystal nano material, under preferable case, described in move back
Fire is incubated 20-360min at anhydrous and oxygen-free condition and temperature are 60-140 DEG C, in anhydrous and oxygen-free condition and temperature is preferably
It is incubated 20-360min at 80-120 DEG C, at anhydrous and oxygen-free condition and temperature are 100-120 DEG C, are more preferably incubated 60-120min.
Temperature that the present invention can be annealed by control and/or time obtain the nano material recycling transmitted electron of different intermediate states
Microscope is observed, and this is highly beneficial to the different intermediate states in research nanocrystal forming process, not only need not turn again
Move one's steps rapid, additionally it is possible to preserve complete crystal structure.Wherein, described anhydrous and oxygen-free refers to that the water content in reactor is at 0.5ppm
Hereinafter, oxygen content is at below 0.05ppm, it is achieved the mode of anhydrous and oxygen-free is well known to those skilled in the art, therefore the most superfluous
State.
As long as described annealing carries out realizing the purpose of the present invention under the conditions of anhydrous and oxygen-free, it is contemplated that pure annealing
Condition can improve nanoscale organic molecule monocrystal material quality further, under preferable case, carries out in an inert atmosphere
Annealing steps, wherein, described noble gas can be identical (such as Ar and/or N with the above-mentioned noble gas being passed through in reactor2).
According to the present invention, for the method observed under transmission electron microscope in step 3), due to transmission electron microscope
Method be known in those skilled in the art, the operational approach carrying out characterizing hence with transmission electron microscope can be joined
According to the description of Electronic Speculum, do not repeat them here.
Present invention also offers said method application in research organic single-crystal nanometer material structure.Utilize the present invention's
Method carries out the sign of organic molecule nano crystal material and is obtained in that characterization result more accurately, for organic nano monocrystalline
The structural analysis of material provides preferred solution.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited in above-mentioned embodiment
Detail, in the technology concept of the present invention, technical scheme can be carried out multiple simple variant, this
A little simple variant belong to protection scope of the present invention.
It is further to note that each the concrete technical characteristic described in above-mentioned detailed description of the invention, at not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to various can
The compound mode of energy illustrates the most separately.
Additionally, combination in any can also be carried out between the various different embodiment of the present invention, as long as it is without prejudice to this
The thought of invention, it should be considered as content disclosed in this invention equally.
The present invention is further described below in conjunction with drawings and Examples.In following example, Benzo[b is marketable material (powder
End, 97%, buy from Aldrich Chemical company)；Copper mesh is the special copper mesh of commercially available Electronic Speculum (band Supported film)；During spin coating
The concentration of polystyrene is 0.5 weight %；The pattern of thin film with atomic force microscope (Nanoscope IIIa MultiMode,
Veeco company) characterize obtain；The sign of nanocrystalline structure use transmission electron microscope (Tecnai G2F20U-TWIN,
FEI Co.).
Fig. 1 is the schematic diagram of test tube furnace used；The tube furnace used in test is the SK that Tianjin electric furnace factory produces2-
4-10A type, is equipped with a vacuum-pumping and the quartz ampoule of insufflation gas, its structural representation such as Fig. 1: quartz ampoule is positioned at resistance furnace
Inside, resistance furnace temperature is controlled its temperature by temperature control instrument KSY-5-12A, and evaporation source puts into resistance furnace central authorities, the product after annealing
It is positioned at suitable temperature；Protective gas enters in quartz ampoule along evaporation source to the direction of annealing afterproduct.
Embodiment 1
(1) copper mesh is put in the organic solvents such as ethanol and stand, then take out and dry in vacuum cavity.After drying, use
The mode of spin coating modifies a strata styrene on copper mesh, and thickness is 20nm, places into baking oven vacuum drying, and baking temperature is 80
℃；Copper mesh after modification is put in evaporation instrument and is carried out vacuum vapor plating, and controlling the temperature at copper mesh is 20 DEG C, Benzo[b powder
End thermal evaporation temperature is 122 DEG C, and deposition velocity is 0.001nm/s, and vacuum is 1 × 10-7Mbar, deposit thickness is 0.8nm's
Pentacene thin film；
(2) after deposition having the copper mesh modified of 0.8nm pentacene thin film put into quartz ampoule, quartz ampoule is sealed, use
Mechanical pump is evacuated to below 10Pa, is then charged with protective gas (noble gas argon) to normal pressure, then be evacuated to 10Pa with
Under, after be filled with protective gas to normal pressure, the most repeatedly, ensure no oxygen and steam in quartz ampoule as far as possible；For the last time
After being filled with protective gas, after quartz ampoule internal gas pressure is normal pressure, keep protective gas (noble gas argon) with the speed of 50sccm
Rate flows.Tube furnace is heated up, is incubated after reaching 120 DEG C.After insulation 20min, i.e. can obtain the Benzo[b being formed in contained network
Monocrystal nano-material；
(3) pentacene thin film of acquisition and Benzo[b monocrystal nano-material are placed under transmission electron microscope observation,
To Fig. 2 to Fig. 5.
Fig. 2 is the AFM pattern of the 0.8nm pentacene thin film being deposited on the copper mesh surface using polymer dielectric layer to modify
Figure, prepared thin film is made up of discoid granule, and the thin film of this pattern is conducive to the formation of nanocrystal below.
Fig. 3 is the SEM shape appearance figure after the annealing of 0.8nm pentacene thin film, demonstrates that obtained nanocrystal shape is complete,
The sample of can be used in structural analysis is more.
Fig. 4, Fig. 5 are respectively TEM shape appearance figure and the SAED diffraction pattern figure of gained Benzo[b monocrystalline micro materials.TEM shape
Looks figure shows shape and the document (NorthrupJ.E. of the crystal grain for the sample analyzed;Tiago M.T.;Louie S.G.,
Phys.Rev.B 2002,66,121404 (R) (1-4) .) crystal grain in report is close, without damaged；SAED diffraction pattern figure is clear
Demonstrate the monocrystalline feature of crystal structure, free from admixture affects.
Result shows, use proposed by the invention first to commercially available copper mesh after polymer-modified, redeposited Benzo[b
Thin film, then carries out annealing and obtains nano material, and obtained nano material is characterized as and five through transmission electron microscope SAED
Benzene nano crystal, monocrystalline shape is identical with the equilibrium configuration of Benzo[b crystal in document report, it is possible to carry out size, table easily
Surface roughness and crystalline sign.
Embodiment 2
(1) copper mesh is put in the organic solvents such as ethanol and stand, then take out and dry in vacuum cavity.After drying, use
The mode of spin coating modifies a strata styrene on copper mesh, and thickness is 100nm, places into baking oven vacuum drying, and baking temperature is
80℃；Copper mesh after modification is put in evaporation instrument and is carried out vacuum vapor plating, and controlling the temperature at copper mesh is 30 DEG C, Benzo[b
Powder thermal evaporation temperature is 122 DEG C, and deposition velocity is 0.05nm/s, and vacuum is 1 × 10-5Mbar, deposit thickness be 8nm also
Pentaphene thin film；
(2), after deposition having the copper mesh modified of 8nm pentacene thin film put into quartz ampoule, quartz ampoule is sealed, uses machine
Tool pump is evacuated to below 10Pa, is then charged with protective gas (noble gas argon) to normal pressure, then is evacuated to below 10Pa,
After be filled with protective gas to normal pressure, the most repeatedly, ensure no oxygen and steam in quartz ampoule as far as possible；It is filled with for the last time
After protective gas, after quartz ampoule internal gas pressure is normal pressure, keep protective gas (noble gas argon) with the speed stream of 50sccm
Dynamic.Tube furnace is heated up, is incubated after reaching 80 DEG C.After insulation 360min, i.e. can obtain the Benzo[b monocrystalline being formed in contained network
Nano material；
(3) pentacene thin film and the Benzo[b monocrystal nano-material of acquisition are placed under transmission electron microscope observation, can
To observe the crystal of pattern and structural integrity.
Embodiment 3
(1) copper mesh is put in the organic solvents such as ethanol and stand, then take out and dry in vacuum cavity.After drying, use
The mode of spin coating modifies a strata styrene on copper mesh, and thickness is 50nm, places into baking oven vacuum drying, and baking temperature is 80
℃；Copper mesh after modification is put in evaporation instrument and is carried out vacuum vapor plating, and controlling the temperature at copper mesh is 25 DEG C, Benzo[b powder
End thermal evaporation temperature is 122 DEG C, and deposition velocity is 0.01nm/s, and vacuum is 1 × 10-7Mbar, deposit thickness be 1.2nm also
Pentaphene thin film；
(2) after deposition having the copper mesh modified of 0.8nm pentacene thin film put into quartz ampoule, quartz ampoule is sealed, use
Mechanical pump is evacuated to below 10Pa, is then charged with protective gas (noble gas argon) to normal pressure, then be evacuated to 10Pa with
Under, after be filled with protective gas to normal pressure, the most repeatedly, ensure no oxygen and steam in quartz ampoule as far as possible；For the last time
After being filled with protective gas, after quartz ampoule internal gas pressure is normal pressure, keep protective gas (noble gas argon) with the speed of 50sccm
Rate flows.Tube furnace is heated up, is incubated after reaching 100 DEG C.After insulation 60min, i.e. can obtain the Benzo[b being formed in contained network
Monocrystal nano-material；
(3) pentacene thin film and the Benzo[b monocrystal nano-material of acquisition are placed under transmission electron microscope observation, can
To observe the crystal of pattern and structural integrity.
Embodiment 4
Prepare 0.8nm pentacene thin film according to the method for embodiment 3, except for the difference that, tube furnace is heated up, after reaching 60 DEG C
Insulation, the intermediate state sample during can obtaining from the film to monocrystalline, become by transmission electron microscope phenetic analysis structure
Change.Result as shown in Figure 6 and Figure 7, presents polycrystalline diffraction pattern.
Can be seen that the method for the present invention facilitates in particular also to characterize intermediate state sample.
The characterizing method of the present invention can carry out transmission electron microscope sign to crystalline material, during sign easily
Crystal preserves complete, and characterization result is true and reliable.
Claims (6)
1. the characterizing method of an organic molecule monocrystal material, it is characterised in that the method includes:
1) dielectric material and organic semiconducting materials is utilized to form dielectric layer and organic semiconductor nano thin-film successively in contained network,
The thickness of described organic semiconductor nano thin-film is 0.8-8nm, and the method forming described organic semiconductor nano thin-film is vacuum
Evaporation coating method, the condition of described vacuum vapor plating includes that deposition velocity is 0.001-0.05nm/s, and vacuum is 1 × 10-5-
1×10-7Mbar, is formed with the temperature residing for the contained network of dielectric layer and is 20-30 DEG C during deposition, sedimentation time is 30-300s；
2) by step 1 under the conditions of anhydrous and oxygen-free) product that obtains anneals, and makes described organic semiconductor nano thin-film convert
For organic single-crystal nano material, wherein, it is 20-360min with the time that the condition of described annealing includes that temperature is 60-140 DEG C；
3) by step 2) product that obtains is placed under transmission electron microscope observation, and measures the chi of organic single-crystal nano material
Very little, surface roughness and crystallinity.
Method the most according to claim 1, wherein, described dielectric material is SiO2, Merlon, polystyrene, polyamides sub-
One in amine and polymethyl methacrylate.
Method the most according to claim 1, wherein, described organic semiconducting materials is Benzo[b.
Method the most according to claim 1, wherein, described contained network is in copper mesh, nickel screen, molybdenum net, gold net and nylon wire
A kind of.
Method the most according to claim 1, wherein, formed the method for described dielectric layer be spin-coating method, magnetron sputtering method or
Self-assembling method.
6. method described in any one application in research organic single-crystal nanometer material structure in claim 1-5.
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| CN105951167B (en) * | 2016-05-05 | 2018-12-11 | 国家纳米科学中心 | Ultra-thin band-like micro-meter scale small organic molecule monocrystalline of one kind and its preparation method and application |
| CN113981541B (en) * | 2021-12-27 | 2022-04-12 | 天津大学 | Method and device for growing organic semiconductor single crystal |
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| WO2000023523A1 (en) * | 1998-10-22 | 2000-04-27 | Ube Nitto Kasei Co., Ltd. | Organic-inorganic composite graded material, method for preparation thereof and use thereof |
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| CN102067320A (en) * | 2009-05-19 | 2011-05-18 | 松下电器产业株式会社 | Method of producing flexible semiconductor device |
| EP2402982A1 (en) * | 2010-07-01 | 2012-01-04 | STMicroelectronics (Tours) SAS | Method for manufacturing thin film capacitor and thin film capacitor obtained by the same |
| CN102712558A (en) * | 2009-11-05 | 2012-10-03 | 出光兴产株式会社 | Asymmetric aromatic compound containing heterocyclic ring, compound for organic thin film transistor, and organic thin film transistor using same |
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| WO2000023523A1 (en) * | 1998-10-22 | 2000-04-27 | Ube Nitto Kasei Co., Ltd. | Organic-inorganic composite graded material, method for preparation thereof and use thereof |
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