CN103776856A - Representation method of small organic molecule single-crystal material and application of representation method - Google Patents
Representation method of small organic molecule single-crystal material and application of representation method Download PDFInfo
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Abstract
The invention provides a representation method of a small organic molecule single-crystal material and application of the representation method. The representation method comprises the following steps: 1), using a dielectric material and an organic semiconductor material to form a dielectric layer and an organic semiconductor nano-film on a grid in sequence, wherein the thickness of the organic semiconductor nano-film is 0.8-8 nm; 2) annealing the product obtained from the step 1) under the anhydrous and oxygen-free conditions to convert the organic semiconductor nano-film into an organic single-crystal nano material; 3) placing the product obtained from the step 2) under a transmission electron microscope for observation, and measuring the size, the surface roughness and the crystallinity of the organic single-crystal nano material. The method has the advantages that a nanocrystal is prepared under the conditions of lower temperature and normal pressure, the obtained product is generated in situ on the grid, a crystal retransfer step is not needed, crystal grains are not polluted or damaged during the single crystal forming process, and the method is directly used for electron microscopy observation and representation. The method especially facilitates analyzing different intermediate states during the nanocrystal forming process.
Description
Technical field
The present invention relates to Electronic Speculum characterizing method and the application of the method in research organic single-crystal nanometer material structure of a kind of characterizing method and application thereof of organic molecule monocrystal material, particularly nanoscale organic molecule monocrystal material.
Background technology
State of aggregation or the crystal structure of analyzing organic small molecule material can provide indispensable material foundation for further studying organic solid electronic transport property and preparing organic electro-optic device.This is because the crystal structure of organic molecule has directly reflected the mode of piling up of molecule, and molecular stuffing arrangement will directly have influence on density of electronic states (such as the non-local character of electronics in π key).In existing document and patent, the growing method of organic crystal has multiple, is divided into chemical method and Physical.Organic crystal poor stability, physical strength is low, so very easily destroy single crystal samples in transfer crystallization process, makes structure analysis become very difficulty.The standby crystal of applied physics legal system carries out Micro-Structure Analysis at present, while particularly nanocrystal being carried out to structure analysis, because crystal is combined with substrate firmly, and crystalline size is too small, make sample transfer process very difficult, cannot realize sample is intactly shifted and adhered on copper mesh, then put into sample for use in transmitted electron microscope chamber and carry out structure observation or electronic diffraction sign; Nanocrystal prepared by chemical method can structural integrity also adhere on copper mesh preferably, but crystal is attaching impurity effect structural characterization and analysis in solution.
Summary of the invention
The object of the invention is to propose a kind of simple characterizing method for tem study organic nano crystal structure.
The invention provides a kind of characterizing method and application thereof of organic molecule monocrystal material, it is characterized in that, the method comprises:
1) utilize dielectric material and organic semiconducting materials carrying online dielectric layer and the organic semiconductor nano thin-film of forming successively, the thickness of described organic semiconductor nano thin-film is 0.8-8nm;
2) product under anhydrous and oxygen-free condition, step 1) being obtained is annealed, and makes 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 and observes, and measure size, surfaceness and the crystallinity of organic single-crystal nano material.
The present invention is relative, and prior art tool has the following advantages:
What the present invention proposed is suitable for the organic molecule nano crystal, particularly pentacene nano crystal material that transmission electron microscope characterizes.Under lower temperature, condition of normal pressure, prepare nanocrystal, products therefrom is carrying online original position generation, and without crystal transfer step again, in crystal formation process, crystal grain can not be polluted or damage, and can be directly used in transmission electron microscope observation and sign.As required, can also help researcher to carry out careful analysis (can realize by controlling annealing temperature and/or time) to different intermediate states in nanocrystal forming process.The certain hour of annealing under inert gas shielding environment, can obtain required sign sample.In characterization, can keep crystal perfection, obtain complete nano crystal structure, can accurately reflect the structural information of required analytic sample, there is certain universality.Characterizing method of the present invention has solved and cannot obtain the complete pattern of organic nano crystal prepared by physical method and the shortcoming of structure, and also having avoided chemical method to prepare organic nanocrystal has the impact of foreign impurity because of preparation condition.
Other features and advantages of the present invention are described in detail the embodiment part subsequently.
Accompanying drawing explanation
Accompanying drawing is to be used to provide a further understanding of the present invention, and forms a part for instructions, is used from explanation the present invention, but is not construed as limiting the invention with embodiment one below.In the accompanying drawings:
Fig. 1 is material preparation tubular furnace structural representation;
Fig. 2 is pentacene thin film atomic force microscopy;
Fig. 3 is the stereoscan photograph of pentacene nanometer monocrystalline monocrystal material on the copper mesh of modifying;
Fig. 4 is the electronic transmission electromicroscopic photograph of pentacene nano crystal material;
Fig. 5 is pentacene nano crystal material electronics diffraction pattern photo;
Fig. 6 is the electronic transmission electromicroscopic photograph of the intermediateness in pentacene nano crystal material forming process;
Fig. 7 is the electron diffraction pattern photo of the intermediateness in pentacene nano crystal material forming process.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is elaborated.Should be understood that, embodiment described herein only, for description and interpretation the present invention, is not limited to the present invention.
The characterizing method that the invention provides a kind of organic molecule monocrystal material, is characterized in that, the method comprises:
1) utilize dielectric material and organic semiconducting materials carrying online dielectric layer and the organic semiconductor nano thin-film of forming successively, the thickness of described organic semiconductor nano thin-film is 0.8-8nm;
2) product under anhydrous and oxygen-free condition, step 1) being obtained is annealed, and makes 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 and observes, and measure size, surfaceness and the crystallinity of organic single-crystal nano material.
According to the present invention, described dielectric material can be various high molecular polymer or the inorganic material that can withstand high temperatures (at least can tolerate 140 ℃ of high temperature and indeformable) of this area routine, and under preferable case, described dielectric material is SiO
2, one in polycarbonate, polystyrene, polyimide and polymethylmethacrylate.
According to the present invention, described organic semiconducting materials can, for the conventional organic small molecule material with biphenyl structural in this area, be preferably pentacene.The present inventor's discovery, the inventive method can characterize the various features of pentacene nano crystal material especially preferably.
According to the present invention, described year net can be the conventional various years nets that use in this area, can be by commercially available, but under preferable case, described year net is the one in copper mesh, nickel screen, molybdenum net, golden net and nylon wire.
According to the present invention, be mainly the smooth surface in order to form low roughness carrying online formation dielectric layer, therefore, the method that forms described dielectric layer can be the method for various routines, preferably, the method that forms described dielectric layer is spin-coating method, magnetron sputtering method and self-assembling method.
The thickness of described dielectric layer can be selected in relative broad range, forms picture rich in detail as long as transmission electron microscope electron beam used can penetrate sample.
According to the present invention, the method that forms described organic semiconductor nano thin-film is preferably vacuum evaporatation.The condition of described vacuum vapor plating can be selected under wider condition, but under preferable case, the condition of described vacuum vapor plating comprises that sedimentation velocity is 0.001-0.05nm/s, and vacuum tightness is 1 × 10
-5-1 × 10
-7mbar, year residing temperature of net that is formed with dielectric layer when deposition is 20-30 ℃, sedimentation time is 30-300s.
According to the present invention, in described annealing process, there is migration in the molecule in described nano thin-film, the original molecule that forms nano thin-film is met again, thereby described nano thin-film to three-dimensional crystal structure transition, forms undersized crystal grain (whole process does not depart from dielectric layer surface) by the membrane structure of original two dimension.Therefore, described annealing can be carried out under wider condition, as long as can make described nano thin-film be converted into organic single-crystal nano material, under preferable case, described annealing is to be incubated 20-360min at 60-140 ℃ in anhydrous and oxygen-free condition and temperature, being preferably in anhydrous and oxygen-free condition and temperature is to be incubated 20-360min at 80-120 ℃, is to be more preferably incubated 60-120min at 100-120 ℃ in anhydrous and oxygen-free condition and temperature.The temperature that the present invention can anneal by control and/or time obtain the nano material recycling transmission electron microscope of different intermediate states and observe, this is very favourable to the different intermediate states in research nanocrystal forming process, not only do not need transfer step again, can also preserve complete crystal structure.Wherein, described anhydrous and oxygen-free refers to that liquid water content in reactor is below 0.5ppm, and oxygen content is below 0.05ppm, and the mode that realizes anhydrous and oxygen-free is well known to those skilled in the art, therefore repeat no more.
Described annealing as long as carry out realizing object of the present invention under anhydrous and oxygen-free condition, consider that pure annealing conditions can further improve nanoscale organic molecule monocrystal material quality, under preferable case, in inert atmosphere, carry out annealing steps, wherein, described inert gas can be with above-mentioned to pass into inert gas in reactor identical (as Ar and/or N
2).
According to the present invention, for the method for observing under transmission electron microscope in step 3), because the method for transmission electron microscope is known in those skilled in the art, therefore utilize the method for operating that transmission electron microscope characterizes with reference to the instructions of Electronic Speculum, not repeat them here.
The present invention also provides the application of said method in research organic single-crystal nanometer material structure.The sign of utilizing method of the present invention to carry out organic molecule nano crystal material can obtain characterization result more accurately, for the structure analysis of organic nano monocrystal material provides better solution.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characterictic described in above-mentioned embodiment, in reconcilable situation, can combine by any suitable mode, for fear of unnecessary repetition, the present invention is to the explanation no longer separately of various possible array modes.
In addition, also can carry out combination in any between various embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Further describe the present invention below in conjunction with drawings and Examples.In following examples, pentacene be marketable material (powder, 97%, buy from Aldrich Chemical company); Copper mesh is the special copper mesh of commercially available Electronic Speculum (band Supported film); When spin coating, the concentration of polystyrene is 0.5 % by weight; The atomic force microscope for pattern (Nanoscope IIIa MultiMode, Veeco company) of film characterizes and obtains; The sign of nanocrystalline structure adopts transmission electron microscope (Tecnai G2F20U-TWIN, FEI Co.).
Fig. 1 is the schematic diagram of test tubular furnace used; The SK that the tubular furnace using in test is produced for Tianjin electric furnace factory
2-4-10A type, be equipped with a vacuum-pumping and be filled with the quartz ampoule of gas, its structural representation is as Fig. 1: quartz ampoule is positioned at resistance furnace inside, and resistance furnace temperature is controlled its temperature by temperature controller KSY-5-12A, evaporation source is put into resistance furnace central authorities, and the product after annealing is positioned over suitable temperature place; Blanket gas enters in quartz ampoule to the direction of annealing afterproduct along evaporation source.
Embodiment 1
(1) copper mesh is put into the organic solvents such as alcohol and left standstill, then take out in vacuum cavity and dry.After drying, modify one deck polystyrene by the mode of spin coating on copper mesh, thickness is 20nm, then puts into baking oven vacuum drying, and baking temperature is 80 ℃; Copper mesh after modification is put into evaporation instrument and is carried out vacuum vapor plating, and the temperature of controlling copper mesh place is 20 ℃, and pentacene powder thermal evaporation temperature is 122 ℃, and sedimentation velocity is 0.001nm/s, and vacuum tightness is 1 × 10
-7mbar, the pentacene thin film that deposit thickness is 0.8nm;
(2) copper mesh of having modified that deposits 0.8nm pentacene thin film is put into after quartz ampoule, quartz ampoule is sealed, be evacuated to below 10Pa with mechanical pump, then be filled with blanket gas (inert gas argon gas) to normal pressure, be evacuated to again below 10Pa, after be filled with blanket gas to normal pressure, so repeatedly, guarantee as much as possible no oxygen and water vapor in quartz ampoule; Be filled with for the last time after blanket gas, after quartz ampoule internal gas pressure is normal pressure, keep blanket gas (inert gas argon gas) to flow with the speed of 50sccm.By tubular furnace heat up, reach 120 ℃ after insulation.After insulation 20min, can obtain being formed at a year online pentacene monocrystal nano-material;
(3) pentacene thin film of acquisition and pentacene monocrystal nano-material are placed under transmission electron microscope and are observed, obtain Fig. 2 to Fig. 5.
Fig. 2 is the AFM shape appearance figure that is deposited on the 0.8nm pentacene thin film on the copper mesh surface that adopts polymer dielectric layer modification, and prepared film is made up of discoid particle, and the 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 obtained nanocrystal shape complete, and the sample of the structure analysis that can be used in is more.
Fig. 4, Fig. 5 are respectively TEM shape appearance figure and the SAED diffraction pattern figure of gained pentacene monocrystalline micro materials.TEM shape appearance figure shows shape and the document (NorthrupJ.E. of the crystal grain of the sample for analyzing; Tiago M.T.; Louie S.G., Phys.Rev.B 2002,66,121404 (R) is (1-4) .) and crystal grain in report is close, without damaged; SAED diffraction pattern figure clearly demonstrates the monocrystalline feature of crystal structure, inclusion-free impact.
Result shows, adopt proposed by the invention first to commercially available copper mesh after polymer-modified, deposit again pentacene thin film, then anneal and obtain nano material, the nano material obtaining is characterized by pentacene nano crystal through transmission electron microscope SAED, monocrystalline shape is identical with the equilibrium configuration of pentacene crystal in bibliographical information, can carry out easily size, surfaceness and crystalline sign.
Embodiment 2
(1) copper mesh is put into the organic solvents such as alcohol and left standstill, then take out in vacuum cavity and dry.After drying, modify one deck polystyrene by the mode of spin coating on copper mesh, thickness is 100nm, then puts into baking oven vacuum drying, and baking temperature is 80 ℃; Copper mesh after modification is put into evaporation instrument and is carried out vacuum vapor plating, and the temperature of controlling copper mesh place is 30 ℃, and pentacene powder thermal evaporation temperature is 122 ℃, and sedimentation velocity is 0.05nm/s, and vacuum tightness is 1 × 10
-5mbar, the pentacene thin film that deposit thickness is 8nm;
(2) copper mesh of having modified that deposits 8nm pentacene thin film is put into after quartz ampoule, quartz ampoule is sealed, be evacuated to below 10Pa with mechanical pump, then be filled with blanket gas (inert gas argon gas) to normal pressure, be evacuated to again below 10Pa, after be filled with blanket gas to normal pressure, so repeatedly, guarantee as much as possible no oxygen and water vapor in quartz ampoule; Be filled with for the last time after blanket gas, after quartz ampoule internal gas pressure is normal pressure, keep blanket gas (inert gas argon gas) to flow with the speed of 50sccm.By tubular furnace heat up, reach 80 ℃ after insulation.After insulation 360min, can obtain being formed at a year online pentacene monocrystal nano-material;
(3) pentacene thin film of acquisition and pentacene monocrystal nano-material are placed under transmission electron microscope and are observed, can observe the crystal of pattern and structural integrity.
Embodiment 3
(1) copper mesh is put into the organic solvents such as alcohol and left standstill, then take out in vacuum cavity and dry.After drying, modify one deck polystyrene by the mode of spin coating on copper mesh, thickness is 50nm, then puts into baking oven vacuum drying, and baking temperature is 80 ℃; Copper mesh after modification is put into evaporation instrument and is carried out vacuum vapor plating, and the temperature of controlling copper mesh place is 25 ℃, and pentacene powder thermal evaporation temperature is 122 ℃, and sedimentation velocity is 0.01nm/s, and vacuum tightness is 1 × 10
-7mbar, the pentacene thin film that deposit thickness is 1.2nm;
(2) copper mesh of having modified that deposits 0.8nm pentacene thin film is put into after quartz ampoule, quartz ampoule is sealed, be evacuated to below 10Pa with mechanical pump, then be filled with blanket gas (inert gas argon gas) to normal pressure, be evacuated to again below 10Pa, after be filled with blanket gas to normal pressure, so repeatedly, guarantee as much as possible no oxygen and water vapor in quartz ampoule; Be filled with for the last time after blanket gas, after quartz ampoule internal gas pressure is normal pressure, keep blanket gas (inert gas argon gas) to flow with the speed of 50sccm.By tubular furnace heat up, reach 100 ℃ after insulation.After insulation 60min, can obtain being formed at a year online pentacene monocrystal nano-material;
(3) pentacene thin film of acquisition and pentacene monocrystal nano-material are placed under transmission electron microscope and are observed, can observe the crystal of pattern and structural integrity.
Embodiment 4
Prepare 0.8nm pentacene thin film according to the method for embodiment 3, different, tubular furnace is heated up, reach 60 ℃ after insulation, the intermediate state sample can obtaining from film to monocrystalline process, by the structural change of transmission electron microscope phenetic analysis.Result as shown in Figure 6 and Figure 7, presents polycrystalline diffraction pattern.
Can find out that method of the present invention also contributes to characterize intermediate state sample especially.
Characterizing method of the present invention can carry out transmission electron microscope sign to crystalline material easily, and in characterization, crystal is preserved completely, and characterization result is true and reliable.
Claims (8)
1. a characterizing method for organic molecule monocrystal material, is characterized in that, the method comprises:
1) utilize dielectric material and organic semiconducting materials carrying online dielectric layer and the organic semiconductor nano thin-film of forming successively, the thickness of described organic semiconductor nano thin-film is 0.8-8nm;
2) product under anhydrous and oxygen-free condition, step 1) being obtained is annealed, and makes 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 and observes, and measure size, surfaceness and the crystallinity of organic single-crystal nano material.
2. method according to claim 1, wherein, described dielectric material is SiO
2, one in polycarbonate, polystyrene, polyimide and polymethylmethacrylate.
3. method according to claim 1, wherein, described organic semiconducting materials is pentacene.
4. method according to claim 1, wherein, described year net is the one in copper mesh, nickel screen, molybdenum net, golden net and nylon wire.
5. method according to claim 1, wherein, the method that forms described dielectric layer is spin-coating method, magnetron sputtering method and self-assembling method.
6. method according to claim 1, wherein, the method that forms described organic semiconductor nano thin-film is vacuum evaporatation, and the condition of described vacuum vapor plating comprises that sedimentation velocity is 0.001-0.05nm/s, and vacuum tightness is 1 × 10
-5-1 × 10
-7mbar, year residing temperature of net that is formed with dielectric layer when deposition is 20-30 ℃, sedimentation time is 30-300s.
7. method according to claim 1, wherein, the condition of described annealing comprises that it is 20-360min with the time that temperature is 60-140 ℃.
8. the application of the method described in any one in research organic single-crystal nanometer material structure in claim 1-7.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105951167A (en) * | 2016-05-05 | 2016-09-21 | 国家纳米科学中心 | Ultrathin banded micrometer-scale organic small molecule single crystal, preparation method and application thereof |
| CN113981541A (en) * | 2021-12-27 | 2022-01-28 | 天津大学 | Method and device for growing organic semiconductor single crystal |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101230149A (en) * | 2007-12-29 | 2008-07-30 | 中国科学院化学研究所 | Two-dimensional ordered organic semiconductor composite nano membrane as well as special substrate and preparation method thereof |
| CN101838792A (en) * | 2009-03-19 | 2010-09-22 | 国家纳米科学中心 | Vacuum thermal evaporation device for preparing large-area membrane for flexible substrate |
| 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 |
-
2012
- 2012-10-24 CN CN201210410863.7A patent/CN103776856B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101230149A (en) * | 2007-12-29 | 2008-07-30 | 中国科学院化学研究所 | Two-dimensional ordered organic semiconductor composite nano membrane as well as special substrate and preparation method thereof |
| CN101838792A (en) * | 2009-03-19 | 2010-09-22 | 国家纳米科学中心 | Vacuum thermal evaporation device for preparing large-area membrane for flexible substrate |
| CN102067320A (en) * | 2009-05-19 | 2011-05-18 | 松下电器产业株式会社 | Method of producing flexible semiconductor device |
| 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 |
| 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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105951167A (en) * | 2016-05-05 | 2016-09-21 | 国家纳米科学中心 | Ultrathin banded micrometer-scale organic small molecule single crystal, preparation method and application thereof |
| 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 |
| CN113981541A (en) * | 2021-12-27 | 2022-01-28 | 天津大学 | Method and device for growing organic semiconductor single crystal |
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