CN111394794A - Large-area organic semiconductor single crystal and preparation method and application thereof - Google Patents
Large-area organic semiconductor single crystal and preparation method and application thereof Download PDFInfo
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- CN111394794A CN111394794A CN201910002603.8A CN201910002603A CN111394794A CN 111394794 A CN111394794 A CN 111394794A CN 201910002603 A CN201910002603 A CN 201910002603A CN 111394794 A CN111394794 A CN 111394794A
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Abstract
The invention discloses a large-area organic semiconductor single crystal and a preparation method and application thereof, wherein the preparation method of the large-area organic semiconductor single crystal comprises the following steps of keeping a substrate at the temperature of 40-60 ℃, arranging a scraper on the upper surface of the substrate, enabling the distance between a blade at the bottom end of the scraper and the upper surface of the substrate to be 5-20 microns, dropwise adding an organic semiconductor solution with the concentration of 1-10 mg/m L between the scraper and the substrate, moving the scraper or the substrate at the speed of 0.01-0.4 mm/s to enable the substrate and the scraper to move relatively, and obtaining the large-area organic semiconductor single crystal on the substrate through which the blade passes.
Description
Technical Field
The invention belongs to the technical field of organic semiconductors, and particularly relates to a large-area organic semiconductor single crystal and a preparation method and application thereof.
Background
The two-dimensional organic semiconductor crystal effectively combines the advantages of long-range order of molecular arrangement in the organic single crystal, no crystal boundary, less impurities and defects, good flexibility of a two-dimensional material, high transparency and easiness in manufacturing a high-integration device, is an optimal choice for researching the relation between the structure and the performance of the material, disclosing the intrinsic performance of the organic semiconductor material, exploring a carrier transmission mode, constructing a high-performance transistor device and a large-scale flexible integrated circuit and attracts more and more people in recent years. The single crystal is an important material which is widely applied to semiconductor devices, solid laser devices, optical instruments, instruments and the like, and plays an important role in solid theory research. In practical application, people always want to obtain crystals with larger volume and higher quality, which needs to continuously explore the growth technology of the crystals, study the growth rule of the crystals and grow the crystals according to practical requirements. Compared with the corresponding three-dimensional bulk crystal, the ultrathin two-dimensional crystal not only has inherent flexibility, but also can show the intrinsic performance enhanced by the material, and can generate new properties which some bulk materials do not have due to the quantum local effect. The organic crystal is bonded by weak van der waals force, and the growth of the organic single crystal is very easily influenced by external conditions (solvent type, solution concentration, temperature, humidity and the like) due to the weak interaction, so that the organic single crystal mostly exists in a micro-nano crystal or polycrystal state. The growth of organic single crystals involves complex intermolecular interactions, including interactions between molecules of the same kind and between heterogeneous molecules, and how to understand, control and utilize these interactions to design an appropriate crystal growth method to prepare a two-dimensional organic semiconductor crystal meeting the demand is a difficult problem to be solved urgently.
At present, two-dimensional organic semiconductor crystals are different from inorganic crystals, and the research thereof has a prominent problem: and (4) controllable growth of the crystal. Unlike inorganic crystals, molecules in organic crystals are bound with weak van der waals forces, and factors affecting molecular crystallization are complicated. Meanwhile, compared with inorganic semiconductor materials, organic semiconductor molecules are in a wide variety, and new organic semiconductor molecules are continuously emerging under the continuous efforts of organic synthesizers. How to find suitable molecules from a large number of organic semiconductor molecules and design corresponding crystal growth techniques is a very big challenge for preparing two-dimensional organic semiconductor crystals. Conventional inorganic semiconductor materials and devices are currently manufactured using a top-down manufacturing process that involves multiple high temperature processing steps of several thousand degrees fahrenheit. One of the major challenges in the solution process for the preparation of organic semiconductors is the control of the film morphology during the printing/coating process, often with orders of magnitude differences in the device performance built from different film morphologies. Therefore, it is very important to control the morphology of the semiconductor thin film when organic semiconductors are processed in solution. The mainstream preparation methods of the organic semiconductor materials at present mainly comprise thermal evaporation, a pulling method and a solution epitaxy method. These cannot achieve precise control in the film formation process of the organic semiconductor.
The size of the film single crystal prepared by the method is in the micrometer or millimeter level, even if the same solution shearing method is adopted, the precision of the equipment is basically not as high as 5um, and the area of the prepared film single crystal is basically in the millimeter level.
Disclosure of Invention
In view of the shortcomings of the prior art, the invention aims to provide a preparation method of a large-area organic semiconductor single crystal.
Another object of the present invention is to provide a large-area organic semiconductor single crystal having an area of up to 3X 3cm at the maximum, obtained by the above-mentioned production method2。
Another object of the present invention is to provide the use of the above-mentioned field effect transistor formed of a large-area organic semiconductor single crystal for improving mobility and on-off ratio.
The purpose of the invention is realized by the following technical scheme.
A preparation method of a large-area organic semiconductor single crystal comprises the following steps of keeping a substrate at a temperature of 40-60 ℃, arranging a scraper on the upper surface of the substrate, enabling the distance between a blade at the bottom end of the scraper and the upper surface of the substrate to be 5-20 micrometers, dropwise adding an organic semiconductor solution with the concentration of 1-10 mg/m L between the scraper and the substrate, moving the scraper or the substrate at a speed of 0.01-0.4 mm/s to enable the substrate and the scraper to move relatively, and obtaining the large-area organic semiconductor single crystal on the substrate through which the blade passes.
In the above technical solution, the substrate is a silicon wafer.
In the technical scheme, the solute of the organic semiconductor solution is C6-DPA or C8-BTBT.
In the technical scheme, when the solute of the organic semiconductor solution is C8-BTBT, the concentration of the organic semiconductor solution is 5-10 mg/m L.
In the technical scheme, when the solute of the organic semiconductor solution is C6-DPA, the concentration of the organic semiconductor solution is 1-5 mg/m L.
In the technical scheme, the temperature for keeping the substrate is preferably 40-50 ℃.
In the technical scheme, the distance between the blade and the upper surface of the substrate is 5-10 micrometers, and preferably 5-8 micrometers.
In the above technical scheme, the solvent of the organic semiconductor solution is chlorobenzene.
In the technical scheme, the volume of the dropwise added organic semiconductor solution is 10-50 microliters.
In the technical scheme, the scraper inclines towards the spreading direction of the large-area organic semiconductor single crystal, and the inclined acute angle is 15-30 degrees.
The large-area organic semiconductor single crystal obtained by the preparation method.
In the technical scheme, the thickness of the large-area organic semiconductor single crystal is 5-42 nm.
In the above technical solution, the maximum energy of the large-area organic semiconductor single crystal reaches 3 × 3cm2。
The application of the field effect transistor constructed by the large-area organic semiconductor single crystal in improving the mobility and the on-off ratio.
In the technical scheme, when the solute of the organic semiconductor solution is C8-BTBT, the average mobility of the field effect transistor formed by the large-area organic semiconductor single crystal is 12.7cm2V-1s-1The maximum mobility is 17.7cm2V-1s-1Switches up to more than 1010。
In the technical scheme, when the solute of the organic semiconductor solution is C6-DPA, the hole mobility of the field effect transistor formed by the large-area organic semiconductor single crystal is 1.0cm on average2V-1s-1The highest mobility can reach 2cm2V-1s-1The switching ratio is up to 108。
Compared with the prior art, the invention has the following beneficial effects:
1. the preparation of the large-area organic semiconductor single crystal is carried out at the room temperature of 20-25 ℃, so that the influence of high temperature on the performance of an organic semiconductor is avoided.
2. The shear stress to which the molecules are subjected is greatly increased due to the reduction of the pitch, so that a large-area single crystal film is finally formed.
Drawings
FIG. 1 is a schematic diagram of shear stress gradients for different spacings between a top blade and a substrate;
FIG. 2 is a molecule of C6-DPA;
FIG. 3(a) is a polarization microscope photograph of a large-area organic semiconductor single crystal obtained in example 8 rotated by 0 °;
FIG. 3(b) is a polarization micrograph of the large-area organic semiconductor single crystal obtained in example 8 rotated by 45 °;
FIG. 4(a) is a transfer curve of a field effect transistor constructed of a large-area organic semiconductor single crystal obtained in example 8;
FIG. 4(b) is a graph showing an output curve of a field effect transistor constructed of a large-area organic semiconductor single crystal obtained in example 8;
FIG. 5 is a molecule of C8-BTBT;
FIG. 6(a) is a polarization microscope photograph of a large-area organic semiconductor single crystal obtained in example 2 rotated by 0 °;
FIG. 6(b) is a polarization microscope photograph of the large-area organic semiconductor single crystal obtained in example 2 rotated by 45 °;
FIG. 7(a) is a transfer curve of a field effect transistor constructed of a large-area organic semiconductor single crystal obtained in example 2;
FIG. 7(b) is a graph showing an output curve of a field effect transistor constructed by using the large-area organic semiconductor single crystal obtained in example 2;
FIG. 8 is a schematic structural diagram of the novel controllable organic crystal growth apparatus of the present invention.
FIG. 9(a) is a transfer curve of a field effect transistor constructed of a large-area organic semiconductor single crystal obtained in example 1;
FIG. 9(b) is a graph showing an output curve of a field effect transistor constructed of a large-area organic semiconductor single crystal obtained in example 1;
FIG. 10(a) is a transfer curve of a field effect transistor constructed of a large-area organic semiconductor single crystal obtained in example 3;
FIG. 10(b) is a graph showing an output curve of a field effect transistor constructed of a large-area organic semiconductor single crystal obtained in example 3;
FIG. 11(a) is a transfer curve of a field effect transistor constructed of a large-area organic semiconductor single crystal obtained in example 4;
FIG. 11(b) is a graph showing an output curve of a field effect transistor constructed of a large-area organic semiconductor single crystal obtained in example 4;
FIG. 12(a) is a transfer curve of a field effect transistor constructed of a large-area organic semiconductor single crystal obtained in example 5;
FIG. 12(b) is a graph showing the output curve of a field effect transistor constructed using a large-area organic semiconductor single crystal obtained in example 5.
Wherein: 1: base plate, 2: electric translation stage, 3: elevating platform, 4: pitching table, 5: a scraping arm, 6: scraper, 7: heat dissipation base, 8: semiconductor refrigeration piece, 9: thermally conductive sheet, 10: and (3) a silicon wafer.
Detailed Description
The apparatus referred to in the following examples is as follows:
polarizing microscope (POM) Nikon EC L IPSE Ci-PO L polarizing optical microscope;
electrical property curve test instrument: keithley 4200-SCS machine quasi-probe station;
thickness test (AFM atomic force microscope): bruker Dimension Icon atomic force microscope;
the drug purchase sources referred to in the following examples are as follows:
C8-BTBT:Sigma-Aldrich
C6-DPA Taiwan L umtec
The technical scheme of the invention is further explained by combining specific examples.
A method for preparing a large-area organic semiconductor single crystal comprises the following steps:
preparing a silicon wafer as a substrate, keeping the substrate at a temperature of T ℃, arranging a scraper on the upper surface of the substrate, setting a distance between a blade edge positioned at the bottom end of the scraper and the upper surface of the substrate to be D micrometers, dripping an organic semiconductor solution with a volume of Y microliter and a concentration of C mg/m L between the scraper and the substrate, wherein a solvent of the organic semiconductor solution is chlorobenzene, moving the substrate at a speed of V mm/S to enable the substrate and the scraper to move relatively, obtaining a large-area organic semiconductor single crystal on the substrate through which the blade edge passes, wherein the scraper inclines towards the spreading direction of the large-area organic semiconductor single crystal, the acute angle of the inclination is 15 degrees, the thickness of the large-area organic semiconductor single crystal is T, and the area of the large-area organic semiconductor.
The solutes, T, V, T, D, Y and C of the above organic semiconductor solution are specified in Table 1.
TABLE 1
Fig. 1 is a schematic diagram of shear stress gradients for different spacings between a top blade and a substrate.
FIG. 2 is a molecule of C6-DPA.
FIGS. 3(a) and 3(b) are polarization micrographs of a large-area organic semiconductor single crystal obtained in example 8, in which FIG. 3(a) is a polarization micrograph of a large-area organic semiconductor single crystal rotated by 0 ℃ and FIG. 3(b) is a polarization micrograph of a large-area organic semiconductor single crystal rotated by 45 ℃ and it is clear that the entire region undergoes a significant change in brightness, demonstrating that the alignment is uniform throughout.
FIGS. 4(a) and 4(b) are graphs showing the transfer curve and output curve of a field-effect transistor constructed from a large-area organic semiconductor single crystal obtained in example 8, and it is understood from these graphs that the hole mobility of the C6-DPA field-effect transistor is 1.0cm on average2V-1s-1Up to 2cm2V-1s-1Switching ratio of up to 108。IDIs the drain current. FIG. 5 is a molecule of C8-BTBT.
FIG. 6(a) is a polarization microscope photograph of the large-area organic semiconductor single crystal obtained in example 2 rotated by 0 ℃ and FIG. 6(b) is a polarization microscope photograph of the large-area organic semiconductor single crystal obtained in example 2 rotated by 45 ℃, and it is clear that the entire region is clearly changed in brightness, which proves that the whole is aligned in the same orientation.
FIGS. 7(a) and 7(b) are graphs showing the transfer curve and output curve of a field effect transistor constructed from the large-area organic semiconductor single crystal obtained in example 2, and the average mobility of the field effect transistor having the large-area organic semiconductor single crystal produced in example 2 was 12.7cm2V-1s-1The maximum mobility is 17.7cm2V-1s-1Switches up to more than 1010。
FIGS. 9(a) and 9(b) are a transfer curve and an output curve of a field effect transistor constructed of a large-area organic semiconductor single crystal obtained in example 1; the average mobility of the field effect transistor for producing a large-area organic semiconductor single crystal from example 1 was 10cm2V-1s-1Maximum mobility of 12.7cm2V-1s-1Switches up to more than 1010。
FIGS. 10(a) and 10(b) are a transfer curve and an output curve of a field effect transistor constructed of a large-area organic semiconductor single crystal obtained in example 3; the average mobility of the field effect transistor for producing a large-area organic semiconductor single crystal from example 3 was 8cm2V-1s-1Maximum mobility of 11cm2V-1s-1Switches up to more than 1010。
FIGS. 11(a) and 11(b) are a transfer curve and an output curve of a field effect transistor constructed of a large-area organic semiconductor single crystal obtained in example 4; the average mobility of the field effect transistor for producing a large-area organic semiconductor single crystal from example 4 was 6.7cm2V-1s-1The maximum mobility is 8.5cm2V-1s-1Switches up to more than 1010。
FIGS. 12(a) and 12(b) are a transfer curve and an output curve of a field effect transistor constructed of a large-area organic semiconductor single crystal obtained in example 5; the average mobility of the field effect transistor for producing a large-area organic semiconductor single crystal from example 5 was 4.5cm2V-1s-1Maximum mobility of 6.3cm2V-1s-1Switches up to more than 109。
The average mobility of the field effect transistor for producing a large-area organic semiconductor single crystal from example 6 was 0.4cm2V- 1s-1Maximum mobility of 0.9cm2V-1s-1Switches up to more than 107。
The average mobility of the field effect transistor for producing a large-area organic semiconductor single crystal from example 7 was 0.7cm2V-1s-1Maximum mobility of 1.3cm2V-1s-1Switches up to more than 108。
Average mobility of field effect transistor for producing large-area organic semiconductor single crystal from example 9 was 1cm2V-1s-1Maximum mobility of 1.8cm2V-1s-1Switches up to more than 108。
The average mobility of the field effect transistor for producing a large-area organic semiconductor single crystal from example 10 was 0.3cm2V-1s-1Maximum mobility of 0.8cm2V-1s-1Switches up to more than 107。
The above embodiment can be prepared by using a novel controllable organic crystal growth device, which is shown in fig. 8 and comprises a base plate 1, an electric translation table 2, a lifting table 3, a pitching table 4, a scraping arm 5, a scraper 6, a heat dissipation base 7, a semiconductor refrigeration piece 8 and a heat conduction piece 9.
The elevating platform 3 is positioned at one side of the electric translation platform 2 and fixed on the base plate 1, the pitching platform 4 is installed on the elevating platform 3, one end of the scraping arm 5 is fixedly installed on the action table of the pitching platform 4, and the other end of the scraping arm is provided with the scraper 6. The height of the scraper is adjusted through the lifting platform, and the pitching angle of the scraper is adjusted through the pitching platform.
Furthermore, the heat conducting strip 9 is a copper strip, a mounting hole for mounting the thermal resistance probe is formed in the copper strip, and the thermal resistance probe is embedded into the mounting hole and used for collecting real-time temperature data of the heat conducting strip.
The semiconductor refrigeration piece is externally connected with a direct current power supply, the direct current power supply for supplying power to the semiconductor refrigeration piece adopts a programmable direct current power supply which is connected with a PC (personal computer) and adopts a Henghui P L D-3605M model, the PC is connected with the thermal resistance probe through a data collector (the signal output end of the thermal resistance probe is connected with the data collector, the data collector is of a MPS-150601 model, the data collector is connected with a PC serial port and sends the collected temperature data to the PC), and the PC is programmed through labview and adopts a PID (proportion integration differentiation) algorithm to realize high-precision temperature control of the thermal conduction piece.
Further, the scraper is cube shaped with one top edge of the cube serving as the cutting edge.
Furthermore, the electric translation stage is a direct-drive linear translation stage DDSM100 with the type of Thorlabs, the direct-drive linear translation stage DDSM100 provides a stroke with the precision of 0.5um, the translation stage is suitable for being used in a high-precision control occasion, a servo drive motor of the electric translation stage is connected with a PC, and various parameters of the electric translation stage are controlled through Kinesis software.
The model of the lifting platform is GCM-162. The type of the pitching platform is GCM-190, the pitching angle is +/-3 degrees, and the thread is 10 mm.
The method for preparing a large-area organic semiconductor single crystal using the novel controllable organic crystal growth apparatus of the above embodiment is as follows:
firstly preparing organic semiconductor solution, then placing a cleaned silicon wafer 10 on a heat conducting fin 9, adjusting a lifting table 3 and a pitching table 4, keeping a scraper horizontally arranged, adjusting the distance between the cutting edge of the scraper and a substrate (a microscope can be arranged beside an electric translation table, and the distance between the cutting edge and the silicon wafer is observed by using the microscope in the adjusting process), setting the temperature of the heat conducting fin with the precision of +/-0.1 ℃, after the temperature is stabilized, dripping the organic semiconductor solution on the substrate through a liquid transfer gun, keeping the electric translation table 2 at a certain moving speed, waiting for the scraper 6 to completely move through the substrate, and obtaining large-area organic semiconductor single crystals on the silicon wafer.
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (10)
1. The preparation method of the large-area organic semiconductor single crystal is characterized by comprising the following steps of keeping a substrate at the temperature of 40-60 ℃, arranging a scraper on the upper surface of the substrate, enabling the distance between a blade at the bottom end of the scraper and the upper surface of the substrate to be 5-20 micrometers, dropwise adding an organic semiconductor solution with the concentration of 1-10 mg/m L between the scraper and the substrate, moving the scraper or the substrate at the speed of 0.01-0.4 mm/s, enabling the substrate and the scraper to move relatively, and obtaining the large-area organic semiconductor single crystal on the substrate through which the blade passes.
2. The method of claim 1, wherein the substrate is a silicon wafer.
3. The method according to claim 2, wherein the organic semiconductor solution has a solute of C6-DPA or C8-BTBT.
4. The production method according to claim 3, wherein the solvent of the organic semiconductor solution is chlorobenzene.
5. The method according to claim 4, wherein the volume of the organic semiconductor solution to be added dropwise is 10 to 50. mu.l.
6. The production method according to claim 5, wherein the doctor blade is inclined toward the direction of spreading the large-area organic semiconductor single crystal at an acute angle of 15 to 30 °.
7. A large-area organic semiconductor single crystal obtained by the production method according to any one of claims 1 to 6.
8. The large area organic semiconductor single crystal according to claim 7, wherein the thickness of the large area organic semiconductor single crystal is 5 to 42nm, and the maximum energy of the large area organic semiconductor single crystal is 3 x 3cm2。
9. Use of a large area organic semiconductor single crystal according to claim 8 for improving mobility and on-off ratio after construction of a field effect transistor.
10. The use according to claim 9, wherein the average mobility of the large area organic semiconductor single crystal forming a field effect transistor is 12.7cm when the solute of the organic semiconductor solution is C8-BTBT2V-1s-1The maximum mobility is 17.7cm2V-1s-1Switches up to more than 1010；
When the solute of the organic semiconductor solution is C6-DPA, the hole mobility of the field effect transistor formed by the large-area organic semiconductor single crystal is 1.0cm on average2V-1s-1The highest mobility can reach 2cm2V-1s-1The switching ratio is up to 108。
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Application publication date: 20200710 |