CN103147123B - A kind of micro-meter scale organic molecule monocrystal material and preparation method thereof - Google Patents
A kind of micro-meter scale organic molecule monocrystal material and preparation method thereof Download PDFInfo
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- CN103147123B CN103147123B CN201110404326.7A CN201110404326A CN103147123B CN 103147123 B CN103147123 B CN 103147123B CN 201110404326 A CN201110404326 A CN 201110404326A CN 103147123 B CN103147123 B CN 103147123B
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Abstract
The invention discloses a kind of preparation method of micro-meter scale organic molecule monocrystal material, the method comprises and utilizes organic semiconductor material to form organic semiconductor nanomembrane at dielectric material surface, and dielectric materials surface being formed organic semiconductor nanomembrane under anhydrous and oxygen-free condition is annealed, described nano thin-film is made to be converted into organic single-crystal nano material, recycling vapor growth method makes described organic single-crystal nano material grow, to form micro-meter scale organic molecule monocrystal material at dielectric material surface, wherein, the thickness of described nano thin-film is 0.1-10nm.The inventive method is at dielectric materials in-situ preparation product, and in single crystal growth process, crystal grain can not be polluted or damage, and technique is simple and easy to control, has certain universality; Obtained micro-meter scale organic molecule monocrystal material has the characteristics such as the two-dimentional yardstick of fabulous perfection of crystal, abundant macro morphology and certain distribution range.
Description
Technical field
The present invention relates to a kind of preparation method of micro-meter scale organic molecule monocrystal material, and micro-meter scale organic molecule monocrystal material obtained by this method.
Background technology
At present, received pay close attention to widely the research of organic single-crystal field effect transistor, this is not only because organic single-crystal can reflect the material characteristics that organic semiconductor is the most basic, is conducive to the research to electronic nature characteristic; Also because the crystal boundary of monocrystalline, charge trap density are reduced to minimum, thus likely reach the mobility higher than organic film FET.In addition, in actual applications, organic single-crystal field effect transistor has outstanding performance, and compared with organic film device, organic single-crystal field effect transistor has higher device performance.
In prior art, the method for growth organic single-crystal has solution method and physical vaporous deposition etc.But monocrystalline prepared by these methods all has respective limitation for device preparation.The organic single-crystal that solution method obtains is not easily separated, and there is a large amount of defect in crystal; In prior art, the operation steps of physical vaporous deposition is: substrate and evaporation source are placed in horizontal reactor (silica tube), under flowing carrier gas existent condition, on substrate, organic single-crystal is obtained by utilizing diamond heating evaporation source, organic single-crystal obtained like this needs to carry out monocrystalline transfer step and could be used for device after making monocrystalline be attached to dielectric materials, therefore bad with the contact of dielectric materials, interface quality is poor, and operation is more loaded down with trivial details, and single-crystal surface is coarse.
Summary of the invention
The object of the invention is the shortcoming overcoming prior art, a kind of method directly preparing micro-meter scale organic molecule monocrystal material at dielectric material surface is provided, thus obtained high-quality micro-meter scale organic molecule monocrystal material.
To achieve these goals, the invention provides a kind of micro-meter scale organic molecule monocrystal material and preparation method thereof, the method comprises and utilizes organic semiconductor material to form organic semiconductor nanomembrane at dielectric material surface, and dielectric materials surface being formed with organic semiconductor nano thin-film under anhydrous and oxygen-free condition is annealed, described nano thin-film is made to be converted into organic single-crystal nano material, recycling vapor growth method makes described organic single-crystal nano material grow, to form micro-meter scale organic molecule monocrystal material at dielectric material surface, wherein, the thickness of described nano thin-film is 0.1-10nm.
Preferably, the preparation method of described nano thin-film is vacuum evaporatation, and described organic semiconductor material is pentacene.
Pass through technique scheme, dielectric material surface directly obtains micro-meter scale organic molecule monocrystal material, thus largely solve organic single-crystal yardstick less than normal and with the contact problems of dielectric material surface, namely likely improve monocrystalline size and and dielectric material surface between interface quality, these are by the research of the preparation and device transmission performance that are conducive to high performance device.Micro-meter scale organic molecule monocrystal material prepared by the present invention has the characteristics such as the two-dimentional yardstick of fabulous perfection of crystal, abundant macro morphology and certain distribution range, as having two-dimentional yardstick in the bulk of 0.1-10 μm or sheet structure, or length is at the bar-shaped or zonal structure of 1-20 μm.In addition, by extending the vapor phase growth time, the size of micro-meter scale organic molecule monocrystal material can be increased further, thus provide high-quality monocrystal material for device preparation and material analysis characterize.
And the preparation method of micro-meter scale organic molecule monocrystal material provided by the invention can carry out under the condition of lesser temps, normal pressure, and preparation condition is simple; Products therefrom at the in-situ preparation of dielectric materials, without the need to crystal transfer step; In single crystal growth process, crystal grain can not be polluted or be damaged; Shape and the final size of controlling and adjustment monocrystal material can be come by the temperature and time controlling crystal growth, have the advantages that preparation technology is simple, be easy to control; And method of the present invention has certain universality.
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Accompanying drawing explanation
Accompanying drawing is used to provide a further understanding of the present invention, and forms a part for specification sheets, 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 the structural representation of tube furnace;
Fig. 2 is pentacene nano thin-film atomic force microscope (AFM) shape appearance figure;
Fig. 3 is pentacene monocrystal nano-material scanning electron microscope (SEM) shape appearance figure;
Fig. 4 is micro-meter scale pentacene monocrystal material scanning electron microscope (SEM) shape appearance figure;
Fig. 5 is micro-meter scale pentacene monocrystal material electronic transmission Electronic Speculum (TEM) shape appearance figure;
Fig. 6 is micro-meter scale pentacene monocrystal material electron diffraction pattern (SAED) figure.
Description of reference numerals
A represents the position that the product after annealing is placed;
B represents the position that evaporation source is placed.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
The invention provides a kind of preparation method of micro-meter scale organic molecule monocrystal material, it is characterized in that, the method comprises and utilizes organic semiconductor material to form organic semiconductor nanomembrane at dielectric material surface, and dielectric materials surface being formed with organic semiconductor nano thin-film under anhydrous and oxygen-free condition is annealed, described nano thin-film is made to be converted into organic single-crystal nano material, recycling vapor growth method makes described organic single-crystal nano material grow, to form micro-meter scale organic molecule monocrystal material at dielectric material surface, wherein, the thickness of described nano thin-film is 0.1-10nm, be preferably 0.8-3.2nm.
According to the present invention, described nano thin-film can be obtained, as vacuum evaporatation by method well-known to those skilled in the art.The present inventor finds, obtains nano thin-film can further improve micro-meter scale organic molecule monocrystal material quality by vacuum evaporatation.
Preferably, it is 0.001-0.01nm/s that the condition of described vacuum vapor plating comprises sedimentation velocity, and vacuum tightness is 1 × 10
-5-1 × 10
-7mbar, temperature during deposition residing for dielectric materials is 20-30 DEG C, and depositing time is 30-300s.
According to the present invention, in order to ensure described micro-meter scale organic molecule monocrystal material quality further, can also clean described dielectric materials before preparing nano thin-film, the purging method that the mode of cleaning can be well known to those skilled in the art, under preferable case, be that the ammonia soln of 5-29 % by weight carries out ultrasonic cleaning to dielectric materials by concentration.
According to the present invention, described dielectric materials can for this area routine can the high molecular polymer of withstand high temperatures (at least can tolerate 170 DEG C of high temperature and indeformable) or inorganic materials, under preferable case, described dielectric materials is SiO
2, polystyrene (PS), polyimide (PI), one in polymethylmethacrylate (PMMA).
Wherein, can determine the thickness of described dielectric materials according to the demand of device, generally, the thickness of described dielectric materials is 250-300nm.
According to the present invention, described dielectric materials can for forming the form of dielectric layer on substrate.Because the method preparing dielectric layer is well known to those skilled in the art, do not repeat them here.
Wherein, described method can also be included in utilize vapor growth method make described organic single-crystal nano material grow after carry out the step of substrate removal.
According to the present invention, described organic semiconductor material is pentacene.The present inventor finds, the pentacene micro-meter scale organic molecule monocrystal material quality using method of the present invention to obtain pentacene micro-meter scale organic molecule monocrystal material quality using pentacene as described organic semiconductor material more obtained than solution method and simple physical vaporous deposition is higher.
According to the present invention, in described annealing process, molecule in described nano thin-film there occurs migration, namely the original molecule forming nano thin-film is met again, thus described nano thin-film by the membrane structure of original two dimension to the crystal structure transition of three-dimensional, form undersized crystal grain (whole process does not depart from dielectric layer surface).Therefore, described annealing can be carried out under wider condition, as long as make described nano thin-film be converted into organic single-crystal nano material, under preferable case, described annealing is incubated 20-360min at anhydrous and oxygen-free condition and temperature are 60-160 DEG C, more preferably at anhydrous and oxygen-free condition and temperature are 100-120 DEG C, is incubated 60-120min.Wherein, described anhydrous and oxygen-free refers to that water-content in reactor is at below 0.5ppm, oxygen content at below 0.05ppm, can by repeatedly toward filling with inert gas in reactor (as Ar and/or N
2) vacuumize again to realize.
As long as described annealing is carried out realizing object of the present invention under anhydrous and oxygen-free condition, consider that pure annealing conditions can improve micro-meter scale organic molecule monocrystal material quality further, under preferable case, carry out annealing steps in an inert atmosphere, wherein, described rare gas element can be identical with the above-mentioned rare gas element passed in reactor (as Ar and/or N
2).
According to the present invention, as long as the product after described annealing is carried out together with evaporation source vapor phase growth step can obtain micro-meter scale organic molecule monocrystal material, described vapor growth method can carry out with reference to prior art, under preferable case, the mode utilizing vapor growth method that described organic single-crystal nano material is grown is included in carrier gas or under the air-proof condition of anhydrous and oxygen-free, the steam allowing evaporation source evaporate to obtain contacts organic single-crystal nano material is grown with the product after described annealing, and described evaporation source is identical with the material of described organic semiconductor nano thin-film.
In order to obtain the good micro-meter scale organic molecule monocrystal material of macro morphology, the sedimentation velocity of described vapor phase growth is preferably 1-10nm/s.Preferably, the temperature of described steam is 220-300 DEG C, and the temperature residing for the product after described annealing is 60-180 DEG C.Generally, be the reactor of 10mm relative to interior diameter, the speed of described carrier gas is 30-200sccm.
Wherein, described carrier gas is ultra-pure Ar and/or N
2.
The present invention also provides a kind of micro-meter scale organic molecule monocrystal material obtained by aforesaid method, and described micro-meter scale organic molecule monocrystal material has two-dimentional yardstick in the bulk of 0.1-10 μm or sheet structure or have two dimensional extent at the bar-shaped or zonal structure of 1-20 μm.
According to one of the present invention preferred embodiment, described vapor phase growth step can use the technical process shown in Fig. 1 to carry out, as shown in Figure 1, described vapor phase growth step can be carried out in the silica tube of tube furnace, product after described annealing is placed on the position A in silica tube, evaporation source is placed on the position B in silica tube, according to carrier gas stream to, position B is positioned at the front of position A, with mechanical pump, carrier gas is passed into from one end of silica tube, the other end is discharged, the flow direction of carrier gas as shown by arrows, start tube furnace and pump, the steam that evaporation source evaporation produces contacts with carrier gas and with the organic single-crystal nano material of position A, by temperature controller control temperature, make the temperature residing for organic single-crystal nano material lower, and lower than the temperature of steam, thus the steam of evaporation source is attached to organic single-crystal nano-material surface, organic single-crystal nano material is grown.
Below will be described the present invention by embodiment.In following examples, pentacene is commercially available from Sigma-Aldrich company, and purity is 97%; The SK that the resistance furnace used is produced for Tianjin electric furnace factory
2-4-10A type tube furnace, be equipped with the silica tube (interior diameter of following silica tube used is 30mm) of a vacuum-pumping and insufflation gas, its structural representation is as Fig. 1, arrow represents the flow direction of rare gas element, silica tube is positioned at resistance furnace inside, product after annealing is positioned over suitable temp place (the A place in Fig. 1), evaporation source puts into silica tube central authorities (the B place of Fig. 1), resistance furnace is domestic (Tianjin Ma Fuer company) SK2-4-10A type tubular type retort furnace, uses KSY-5-12A type temperature controller to control its temperature; Rare gas element is Ar; Mechanical pump is domestic excellent one-tenth 4 liters of pumps; AFM is purchased from Veeco company, and model is NanoscopeIII type; SEM is Hitachi 4800 type; TEM is purchased from FEI Co., and model is TecnaiG2F20U-Twin type.
In following examples, the preparation method of nano thin-film is: at 1cm
2silicon substrate on prepare SiO
2, polystyrene or polymide dielectric layer (thickness is 250-300nm), be the ammonia soln ultrasonic cleaning dielectric layer of 3 % by weight by concentration, then be 1 × 10 in vacuum tightness
-5-1 × 10
-7under the vacuum condition of mbar, the method of vacuum vapor plating is adopted to deposit pentacene thin film at dielectric layer surface, temperature during deposition residing for dielectric materials is 20-30 DEG C, sedimentation velocity is 0.001-0.01nm/s, depositing time is 30-300s, the pentacene thin film thickness of deposition corresponds to 0.1-10nm, and Fig. 2 is the AFM shape appearance figure of the pentacene nano thin-film (thick 0.8nm) being deposited on dielectric layer surface.The thickness of nano thin-film and micro-meter scale pentacene monocrystal material is characterized by AFM and records; Two-dimentional yardstick/the length of micro-meter scale pentacene monocrystal material is characterized by SEM and records.
Embodiment 1
Pentacene thin film (thick 0.8nm) and SiO will be deposited
2the Si substrate of dielectric layer (thick 300nm) puts into silica tube, silica tube is placed in tube furnace rear enclosed silica tube, below 10Pa is evacuated to mechanical pump, then rare gas element is filled with to normal pressure, be evacuated to below 10Pa again, after be filled with rare gas element to normal pressure, repeatable operation like this 2 times, ensure that anaerobic is anhydrous in silica tube as far as possible; Being filled with rare gas element for the last time, is after normal pressure until silica tube internal gas pressure, keeps rare gas element to flow with the speed of 50sccm.Tube furnace is heated up, is incubated after reaching 80 DEG C.After insulation 60min, can obtain pentacene monocrystal nano-material, Fig. 3 is the SEM shape appearance figure after the annealing of 0.8nm pentacene thin film.
Separately getting 10mg pentacene is put in quartz crucible as evaporation source, and quartz crucible and pentacene monocrystal nano-material obtained above are placed in another silica tube as seed crystal, and seed crystal departs from quartz crucible and is about 12cm, then closed quartz tube.With preparing pentacene monocrystal nano-material process above, deoxygenation and water removal phase are carried out to the silica tube after closing, then tube furnace is heated up, after the temperature at quartz crucible place and pentacene monocrystal nano-material place reaches 225 DEG C and 125 DEG C respectively, continue insulation 600min and can obtain micro-meter scale pentacene monocrystal material, Fig. 4, Fig. 5 and Fig. 6 are respectively the SEM shape appearance figure of gained micro-meter scale pentacene monocrystal material, TEM shape appearance figure and SAED diffraction pattern figure.
Record micro-meter scale pentacene monocrystal material and there is the hexagon lumphy structure that length is 10 μm, thickness is 1 μm.As can be seen from the SEM shape appearance figure of pentacene monocrystal nano-material and micro-meter scale pentacene monocrystal material, the shape of pentacene bulk-shaped monocrystal nano material is identical with the shape of micro-meter scale pentacene monocrystal material.
Comparative example 1
Getting 10mg pentacene is put in quartz crucible as evaporation source, will have SiO
2the Si substrate of dielectric layer (thick 300mm) puts into silica tube, closed quartz tube together with quartz crucible.Substrate is identical with embodiment 1 with the placement location of quartz crucible.Be evacuated to below 10Pa with mechanical pump, be then filled with rare gas element to normal pressure, then be evacuated to below 10Pa, after be filled with rare gas element to normal pressure, repeatable operation like this 2 times, ensure that anaerobic is anhydrous in silica tube as far as possible; Being filled with rare gas element for the last time, is after normal pressure until silica tube internal gas pressure, keeps rare gas element to flow with the speed of 50sccm.Then tube furnace is heated up, after the temperature at quartz crucible place and pentacene monocrystal nano-material place reaches 225 DEG C and 125 DEG C respectively, continue insulation 600min and can obtain micro-meter scale pentacene monocrystal material, observe its SEM, TEM and SAED diffraction pattern figure respectively, record micro-meter scale pentacene monocrystal material and there is the round porphyritic texture that diameter is 200-300nm.
Embodiment 2
The Si substrate depositing pentacene thin film (thick 6nm) and polystyrene dielectric layer (thick 10nm) is put into silica tube, silica tube is placed in tube furnace rear enclosed silica tube, below 10Pa is evacuated to mechanical pump, then rare gas element is filled with to normal pressure, be evacuated to below 10Pa again, after be filled with rare gas element to normal pressure, repeatable operation like this 2 times, ensure that anaerobic is anhydrous in silica tube as much as possible; Being filled with rare gas element for the last time, is after normal pressure until silica tube internal gas pressure, keeps rare gas element to flow with the speed of 50sccm.Tube furnace is heated up, is incubated after reaching 130 DEG C.After insulation 120min, pentacene monocrystal nano-material can be obtained.
Separately getting 10mg pentacene is that distillation raw material is put in quartz crucible, and be placed in another silica tube using quartz crucible and pentacene monocrystal nano-material obtained above as seed crystal, seed crystal departs from quartz crucible and is about 12cm, closed quartz tube.As prepared pentacene monocrystal nano-material process above, deoxygenation and water removal phase are carried out to the silica tube after closing, then tube furnace is heated up, after the temperature at crucible place and pentacene monocrystal nano-material place reaches 265 DEG C and 125 DEG C respectively, continue insulation 300min and can obtain micro-meter scale pentacene monocrystal material, observe its SEM, TEM and SAED diffraction pattern figure respectively, record micro-meter scale pentacene monocrystal material and there is the lumphy structure that length is 5 μm, thickness is 0.5 μm.
Embodiment 3
The Si substrate depositing pentacene thin film (thick 10nm) and polymide dielectric layer (thick 20nm) is put into silica tube, silica tube is placed in tube furnace rear enclosed silica tube, below 10Pa is evacuated to mechanical pump, then rare gas element is filled with to normal pressure, be evacuated to below 10Pa again, after be filled with rare gas element to normal pressure, repeatable operation like this 2 times, ensure that anaerobic is anhydrous in silica tube as much as possible; Being filled with rare gas element for the last time, is after normal pressure until silica tube internal gas pressure, keeps rare gas element to flow with the speed of 50sccm.Tube furnace is heated up, is incubated after reaching 160 DEG C.After insulation 120min, pentacene monocrystal nano-material can be obtained.
Separately getting 10mg pentacene is put in quartz crucible as evaporation source, and be placed in another silica tube using quartz crucible and pentacene monocrystal nano-material obtained above as seed crystal, seed crystal departs from quartz crucible and is about 12cm, closed quartz tube.As prepared pentacene monocrystal nano-material process above, deoxygenation and water removal phase are carried out to the silica tube after closing, then tube furnace is heated up, after the temperature at crucible place and pentacene monocrystal nano-material place reaches 285 DEG C and 180 DEG C respectively, continue insulation 300min and can obtain micro-meter scale pentacene monocrystal material, observe its SEM, TEM and SAED diffraction pattern figure respectively, record micro-meter scale pentacene monocrystal material and there is the lumphy structure that length is 2 μm, thickness is 0.2 μm.
The monocrystalline yardstick of the micro-meter scale organic molecule monocrystal material prepared as can be seen from embodiment 1-3 and comparative example 1 and shape, use method of the present invention to prepare crystalline size that micro-meter scale organic molecule monocrystal material substantially improves organic single-crystal; The micro-meter scale organic molecule monocrystal material that the present invention obtains has the characteristics such as the two-dimentional yardstick of fabulous crystallographic, good macro morphology and certain distribution range; And the present invention is at dielectric materials in-situ preparation micro-meter scale organic molecule monocrystal material, can be directly used in device without the need to crystal transfer step, simple to operate.
Below the preferred embodiment of the present invention is described in detail by reference to the accompanying drawings; 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 the concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode.In order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out arbitrary combination between various different 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.
Claims (4)
1. the preparation method of a micro-meter scale organic molecule monocrystal material, it is characterized in that, the method comprises and utilizes organic semiconductor material to form organic semiconductor nanomembrane at dielectric material surface, and dielectric materials surface being formed with organic semiconductor nano thin-film under anhydrous and oxygen-free condition is annealed, described nano thin-film is made to be converted into organic single-crystal nano material, recycling vapor growth method makes described organic single-crystal nano material grow, to form micro-meter scale organic molecule monocrystal material at dielectric material surface, wherein, the thickness of described nano thin-film is 0.1-10nm, described organic semiconductor material is pentacene, the preparation method of described nano thin-film is vacuum evaporatation, it is 0.001-0.01nm/s that the condition of described vacuum vapor plating comprises sedimentation velocity, vacuum tightness is 1 × 10
-5-1 × 10
-7mbar, temperature during deposition residing for dielectric materials is 20-30 DEG C, depositing time is 30-300s, described dielectric materials is for can tolerate 170 DEG C and indeformable high molecular polymer or inorganic materials, it be 60-160 DEG C and time is 20-360min that the condition of described annealing comprises temperature, the described mode utilizing vapor growth method that described organic single-crystal nano material is grown comprises: under carrier gas or the air-proof condition at anhydrous and oxygen-free, the steam allowing evaporation source evaporate to obtain contacts organic single-crystal nano material is grown with the product after described annealing, described evaporation source is identical with the material of described organic semiconductor nano thin-film, the sedimentation velocity of described vapor phase growth is 1-10nm/s.
2. method according to claim 1, wherein, the thickness of described nano thin-film is 0.8-3.2nm.
3. method according to claim 1, wherein, described dielectric materials is SiO
2, polystyrene, one in polyimide and polymethylmethacrylate.
4. method according to claim 1, wherein, the temperature of described steam is 220-300 DEG C, and the temperature residing for the product after described annealing is 60-180 DEG C.
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| CN103436949B (en) * | 2013-09-04 | 2016-08-17 | 清华大学 | A kind of monocrystal thin films of organic semiconductor compound and preparation method and application |
| CN104022221A (en) * | 2014-06-20 | 2014-09-03 | 国家纳米科学中心 | Method for preparing ultra-thin and large organic small molecule single crystal wafer layer and high-quality bottom grid top contact field effect transistor of ultra-thin and large organic small molecule single crystal wafer layer |
| CN105586641B (en) * | 2016-01-12 | 2018-02-09 | 山东大学 | Methylamine lead halide phosphate compounds monocrystalline micro flakes growing method and grower |
| 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 |
| CN110085738B (en) * | 2018-01-26 | 2021-11-02 | 中国科学院化学研究所 | Organic single crystal spin valve and preparation method and application thereof |
| CN114622271A (en) * | 2022-02-10 | 2022-06-14 | 合肥科晶材料技术有限公司 | Water-removing and oxygen-removing system of small-sized tube furnace |
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