CN116206961A - Preparation method of two-dimensional thin film material device based on Van der Waals contact metal electrode - Google Patents
Preparation method of two-dimensional thin film material device based on Van der Waals contact metal electrode Download PDFInfo
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- H01L29/66409—Unipolar field-effect transistors
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- H01L29/42312—Gate electrodes for field effect devices
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- H01L29/42384—Gate electrodes for field effect devices for field-effect transistors with insulated gate for thin film field effect transistors, e.g. characterised by the thickness or the shape of the insulator or the dimensions, the shape or the lay-out of the conductor
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Abstract
The invention belongs to the field of photoelectron device manufacturing, and in particular relates to a preparation method of a two-dimensional thin film material device based on a van der Waals contact metal electrode, which comprises the following steps: spin coating photoresist on a substrate and baking; exposing and masking the substrate coated with the photoresist, and developing; carrying out metal electrode deposition on the developed substrate; spin-coating PMMA on a substrate on which a metal electrode is deposited in advance, and heating the PMMA into a film shape; removing the membranous PMMA with the metal electrode and transferring the membranous PMMA onto a slide glass with the PDMS spin coating; fixing a glass slide on a 3D transfer platform, aligning a metal film electrode micro-area by observing an image on an optical microscope, and growing to obtain a Van der Waals electrode transistor; and annealing and impurity removing treatment are carried out on the van der Waals electrode transistor. The metal electrode device prepared by the invention can effectively protect the metal/two-dimensional material interface of the electrode of the device, thereby having better device reliability and good electrical and photoelectric characteristics.
Description
Technical Field
The invention belongs to the field of manufacturing of optoelectronic devices, and particularly relates to a preparation method of a two-dimensional thin film material device based on a van der Waals contact metal electrode.
Background
Currently, research on new semiconductor two-dimensional thin film material devices is mainly focused on constructing transistors based on semiconductor two-dimensional thin film materials. How to use the good single crystal lattice structure and regular atomic arrangement of the semiconductor two-dimensional film material to improve the carrier mobility of the device, the switching ratio of the photoelectric device, the electrical and photoelectric properties such as light responsivity, light sensitivity and the like is the key point of the research of the two-dimensional material and the device.
The metal/semiconductor junction is an important component of a semiconductor two-dimensional material optoelectronic device. However, the traditional metal electrode is manufactured by methods such as exposure, thermal evaporation or plasma assisted sputtering, and the like, and the process has little influence on the semiconductor film material with thicker layer thickness (micron-sized); however, when the layer thickness of the semiconductor film material is reduced to an atomic scale (1 nanometer scale), the surface of the two-dimensional material is a body, and in the process, unavoidable pollution of chemical reagents to the two-dimensional film material exists due to optical exposure, meanwhile, higher process temperature exists during metal electrode deposition, and damage to the lattice structure of the two-dimensional material due to particle impact during high-energy particle bombardment is caused, so that a large number of defects are caused in the contact area of the metal electrode and the material, ideal metal semiconductor Schottky contact is difficult to realize, and the device performance is seriously reduced.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a two-dimensional thin film material device based on a van der Waals contact metal electrode, which comprises the following steps:
s1: will be cleanSi/SiO 2 Or Si is used as a substrate, photoresist is spin-coated on the prepared substrate through a spin coater and baking treatment is carried out;
s2: placing the substrate coated with the photoresist into a binary exposure machine for exposure, and masking the substrate by using a prefabricated electrode mask plate;
s3: developing the exposed substrate;
s4: performing metal electrode deposition on the developed substrate by adopting a magnetron sputtering method, and removing photoresist on the substrate;
s5: spin-coating 8wt% of PMMA on a substrate on which a metal electrode was previously deposited, and heating at 150℃for 30min to cure the PMMA into a film;
s6: removing the solidified membranous PMMA with the metal electrode from the substrate, transferring the membranous PMMA to a slide glass with PDMS attached in advance, and fixing the slide glass to a 3D transfer platform;
s7: after the metal film electrode micro-areas are aligned through observing images on an optical microscope, moving to a target area of a two-dimensional film material to be transferred, and growing on the two-dimensional film material to obtain a two-dimensional film material van der Waals electrode transistor with a PMMA film;
s8: and carrying out annealing treatment and impurity removal treatment on the two-dimensional film material van der Waals electrode transistor with the PMMA film to obtain the clean and flat two-dimensional film material van der Waals metal electrode device.
The invention has the beneficial effects that:
compared with the method for directly depositing the metal electrode on the two-dimensional film material by utilizing the traditional device electrode process, the method for preparing the metal electrode device by adopting the metal electrode transfer mode avoids the damage of the traditional electrode process to the metal and two-dimensional material interface caused by high temperature or high energy impact of metal atomic groups on the two-dimensional material, and can effectively protect the metal/two-dimensional material interface of the device electrode, thereby having better device reliability, and being suitable for preparing large-scale device arrays;
the van der Waals electrode device prepared by the method has good electrical and photoelectric characteristics, and has great potential in the application field of electrical and photoelectric devices of semiconductor two-dimensional film materials.
Drawings
FIG. 1 is a flow chart of a method of fabricating a two-dimensional thin film material device based on van der Waals contact metal electrodes of the present invention;
FIG. 2 is a schematic diagram of a metal electrode transfer process according to the present invention;
FIG. 3 is a schematic diagram of a two-dimensional thin film material device test prepared according to the present invention;
FIG. 4 shows WS prepared by the conventional micro-nano process of the present invention 2 Schematic of device testing.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
A preparation method of a two-dimensional thin film material device based on a Van der Waals contact metal electrode is shown in fig. 1, and comprises the following steps:
s1: to clean Si/SiO 2 Or Si is used as a substrate, photoresist is spin-coated on the prepared substrate through a spin coater and baking treatment is carried out;
s2: placing the substrate coated with the photoresist into a binary exposure machine for exposure, and masking the substrate by using a prefabricated electrode mask plate;
s3: developing the exposed substrate;
s4: performing metal electrode deposition on the developed substrate by adopting a magnetron sputtering method, and removing photoresist on the substrate;
s5: spin-coating 8wt% of PMMA on a substrate on which a metal electrode was previously deposited, and heating at 150℃for 30min to cure the PMMA into a film;
s6: removing the solidified membranous PMMA with the metal electrode from the substrate, transferring the membranous PMMA to a slide glass with PDMS attached in advance, and fixing the slide glass to a 3D transfer platform;
s7: after the metal film electrode micro-areas are aligned through observing images on an optical microscope, moving to a target area of a two-dimensional film material to be transferred, and growing on the two-dimensional film material to obtain a two-dimensional film material van der Waals electrode transistor with a PMMA film;
s8: and carrying out annealing treatment and impurity removal treatment on the two-dimensional film material van der Waals electrode transistor with the PMMA film to obtain the clean and flat two-dimensional film material van der Waals metal electrode device.
In this embodiment, the photoresist includes: s1805 photoresist and LOR photoresist.
Spin-coating photoresist on the prepared substrate by a spin coater and baking, comprising:
the method comprises the steps of firstly setting the rotating speed and time of a spin coater to 500r/min and 5S, then setting the rotating speed and time to 3500r/min and 35S, coating LOR photoresist on a substrate, then baking the substrate coated with the LOR photoresist at 170 ℃ for 10min, setting the rotating speed and time of the spin coater to 500r/min, 5S and 2000r/min and 35S, coating S1805 photoresist on the substrate coated with the LOR photoresist, and baking the substrate coated with the LOR photoresist at a temperature of 100 ℃ on a heating platform for 10min.
In this embodiment, the developing material is AZ300 developer.
The working principle of magnetron sputtering is that glow discharge is generated between a cathode and an anode in a relatively stable vacuum state, gas molecules between the cathode and the anode are ionized to generate charged charges, and electrons collide with argon atoms in the process of flying to a substrate under the action of an electric field E, so that Ar and new electrons are generated by ionization; the new electrons fly to the substrate, ar is accelerated to fly to the cathode target under the action of an electric field, and bombards the surface of the target with high energy, so that the target material is sputtered.
In this embodiment, the deposited metal electrode in S4 is Au, and the thickness is 50nm; other metals such as Ag, pt, pd, cu, etc. can also be deposited by the method.
The target two-dimensional thin film material comprises: by chemical vapour depositionBy Si/SiO 2 WS grown on substrate 2 A two-dimensional thin film material.
Growing on a target two-dimensional film material to obtain a two-dimensional film material van der Waals electrode transistor with a polymethyl methacrylate (PMMA) film, comprising:
after the metal thin film electrode micro-areas are aligned by observing the image on the optical microscope, the micro-areas with PDMS/PMMA/WS 2 The glass slide is heated at 100 degrees for 1min, the glass slide is slowly lifted, and a polymethyl methacrylate (PMMA) film with a metal electrode is aligned and transferred to a target material position, so that a two-dimensional film material van der Waals electrode transistor with the polymethyl methacrylate (PMMA) film is obtained.
As shown in fig. 2, the alignment transfer of a polymethyl methacrylate (PMMA) film with a metal electrode to a target material location includes the steps of:
the first step: in SiO 2 Depositing a metal electrode to be transferred on the Si substrate;
and a second step of: spin-coating polymethyl methacrylate (PMMA) on a substrate, and then heating and curing to form a film;
and a third step of: polymethyl methacrylate (PMMA) with metal electrodes was peeled off the substrate and then transferred to a slide with Polydimethylsiloxane (PDMS);
fourth step: preparing a two-dimensional thin film material WS grown by CVD method 2 As a material to be transferred;
fifth step: transferring the metal electrode to a target material location;
sixth step: and heating the glass slide, finally transferring PMMA with the metal electrode to a target position, and removing the PMMA to obtain the clean, flat and well-contacted two-dimensional film material van der Waals metal electrode device.
Carrying out annealing treatment and impurity removal treatment on a two-dimensional film material van der Waals electrode transistor with a polymethyl methacrylate (PMMA) film, wherein the two-dimensional film material van der Waals electrode transistor comprises:
and (3) carrying out annealing treatment at the temperature of 250 ℃ for 10min on a two-dimensional film material van der Waals electrode transistor with a polymethyl methacrylate (PMMA) film under vacuum, putting the annealed two-dimensional film material van der Waals electrode transistor into an acetone solution for 10min to remove residual polymethyl methacrylate (PMMA), then sequentially putting into an alcohol solution and deionized water to remove residual acetone solution and alcohol solution, and finally drying by a nitrogen gun to obtain the clean and flat two-dimensional film material van der Waals metal electrode device.
As shown in FIG. 3, FIG. 3 (a) shows a monolayer of WS under 635nm laser irradiation at different optical power densities 2 I-V curve of Van der Waals electrode device; WS at-4V voltage 2 Van der Waals electrode device in darkness and different laser power density (2-181 mW/cm) 2 ) I-V curve under 635nm laser irradiation, illustrating that the current of the device increases significantly with increasing laser power when 635nm laser of different power densities is applied to the sample surface. FIG. 3 (b) WS under 635nm laser irradiation at source-drain voltage V=4V 2 The evolution rule of the light responsivity of the van der Waals electrode device along with the laser power density; according to formula R λ ＝I ph P.S (where P is the laser power density and S is the light effective area (1200 μm 2 ) Obtaining the light responsivity R under different laser power densities λ Values, shown in the figure, R λ Increasing with decreasing laser power density, when v=1v, the laser power density is 2mW/cm 2 When R is λ Maximum value of 2.5×10 5 mA/W, the Van der Waals electrode device has good light response. FIG. 3 (c) WS under 635nm laser irradiation at V=0.1V 2 The evolution rule of the external quantum efficiency EQE of the van der Waals electrode device along with the laser power density; according to the formula:
wherein e is electron charge, h is Planck constant, c is light speed, and lambda is laser wavelength;
the external quantum efficiency EQE increases with decreasing laser power density, when the source-drain voltage v=0.1v, the laser power density is 2mW/cm 2 The EQE maximum is 416%, indicating a higher external quantum efficiency for the van der Waals electrode device.
As shown in FIG. 4, (a) WS prepared by conventional micro-nano process 2 I-V curve of the device under dark and 635nm laser irradiation with different optical power densities; (b) WS prepared by traditional micro-nano technology 2 When V=1V, the light responsivity of the device under 635nm laser irradiation changes along with the evolution rule of the laser power density; (c) WS prepared by traditional micro-nano technology 2 When v=1v, the external quantum efficiency EQE of the device under 635nm laser irradiation follows the evolution rule of laser power density.
Comparing van der Waals metal electrodes WS in FIGS. 3 and 4 2 WS devices and methods of making same 2 The I-V characteristic curve of the device can find that the van der Waals electrode device has larger photocurrent than the traditional device and compared with the traditional WS 2 The device is about an order of magnitude larger because the high energy process in the conventional method may destroy the contact interface of the metal and the material, and increase the resistance to reduce the photocurrent.
At a voltage of 1V, the laser power density was 2mW/cm 2 WS manufactured by the following traditional micro-nano process 2 The photoresponsivity of the device was 8mA/W, van der Waals electrode WS 2 The optical responsivity of the device is about 2.5×10 5 mA/W is far higher than the light responsivity of the traditional process device. WS made by traditional process 2 The device has a voltage of 1V and a laser power density of 2mW/cm 2 The maximum value of EQE is 1.5%. When v=0.1V, the laser power density was 2mW/cm 2 When the maximum EQE of the van der waals electrode device is 416%, 277 times the conventional method. The test result proves that the van der Waals device has excellent light responsivity and external quantum efficiency compared with the photoelectric device of the traditional process, and has great potential in the application fields of the electric and photoelectric devices of the semiconductor two-dimensional film material.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. The preparation method of the two-dimensional thin film material device based on the Van der Waals contact metal electrode is characterized by comprising the following steps of:
s1: to clean Si/SiO 2 Or Si is used as a substrate, photoresist is spin-coated on the prepared substrate through a spin coater and baking treatment is carried out;
s2: placing the substrate coated with the photoresist into a binary exposure machine for exposure, and masking the substrate by using a prefabricated electrode mask plate;
s3: developing the exposed substrate;
s4: performing metal electrode deposition on the developed substrate by adopting a magnetron sputtering method, and removing photoresist on the substrate;
s5: spin-coating 8wt% of PMMA on a substrate on which a metal electrode was previously deposited, and heating at 150℃for 30min to cure the PMMA into a film;
s6: removing the solidified membranous PMMA with the metal electrode from the substrate, transferring the membranous PMMA to a slide glass with PDMS attached in advance, and fixing the slide glass to a 3D transfer platform;
s7: after the metal film electrode micro-areas are aligned through observing images on an optical microscope, moving to a target area of a two-dimensional film material to be transferred, and growing on the two-dimensional film material to obtain a two-dimensional film material van der Waals electrode transistor with a PMMA film;
s8: and carrying out annealing treatment and impurity removal treatment on the two-dimensional film material van der Waals electrode transistor with the PMMA film to obtain the clean and flat two-dimensional film material van der Waals metal electrode device.
2. A method of fabricating a two-dimensional thin film material device based on van der waals contact metal electrodes as claimed in claim 1, wherein the photoresist comprises: s1805 photoresist and LOR photoresist.
3. The method for manufacturing a two-dimensional thin-film material device based on a van der waals contact metal electrode according to claim 1, wherein the photoresist is spin-coated on a prepared substrate by a spin coater and baked, comprising:
the method comprises the steps of firstly setting the rotating speed and time of a spin coater to 500r/min and 5S, then setting the rotating speed and time to 3500r/min and 35S, coating LOR photoresist on a substrate, then baking the substrate coated with the LOR photoresist at 170 ℃ for 10min, setting the rotating speed and time of the spin coater to 500r/min, 5S and 2000r/min and 35S, coating S1805 photoresist on the substrate coated with the LOR photoresist, and baking the substrate coated with the LOR photoresist at a temperature of 100 ℃ on a heating platform for 10min.
4. A method of fabricating a two-dimensional thin film material device based on van der waals contact metal electrodes as claimed in claim 1, wherein the developing material is AZ300 developing solution.
5. The method for manufacturing a two-dimensional thin-film material device based on van der waals contact metal electrodes according to claim 1, wherein the deposited metal electrode in S4 is Au, and the thickness is 50nm.
6. The method for preparing a two-dimensional thin-film material device based on a van der waals contact metal electrode according to claim 1, wherein the target two-dimensional thin-film material comprises: by chemical vapor deposition on Si/SiO 2 WS grown on substrate 2 A two-dimensional thin film material.
7. The method for preparing the two-dimensional thin film material device based on the van der Waals contact metal electrode according to claim 1, wherein the van der Waals electrode transistor with the PMMA thin film is grown on the target two-dimensional thin film material, and the method comprises the following steps:
after the metal thin film electrode micro-areas are aligned by observing the image on the optical microscope, the micro-areas with PDMS/PMMA/WS 2 Heating the glass slide at 100 deg.c for 1min to slow down the glass slideSlowly lifting, and aligning and transferring PMMA film with metal electrode to target material WS 2 To obtain WS with PMMA film 2 Van der waals electrode transistors.
8. The method for preparing a two-dimensional thin film material device based on a Van der Waals contact metal electrode according to claim 1, wherein the method comprises the steps of 2 The van der Waals electrode transistor is subjected to an annealing treatment and a impurity removal treatment, comprising:
for WS with PMMA film 2 Performing annealing treatment of Van der Waals electrode transistor under vacuum at 250 deg.C for 10min, and annealing the WS 2 Placing Van der Waals electrode transistor in acetone solution for 10min to remove residual PMMA, sequentially placing into alcohol solution and deionized water to remove residual acetone solution and alcohol solution, and blow-drying with nitrogen gun to obtain clean and flat WS 2 Van der waals metal electrode devices.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310153925.9A CN116206961A (en) | 2023-02-23 | 2023-02-23 | Preparation method of two-dimensional thin film material device based on Van der Waals contact metal electrode |
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| CN202310153925.9A CN116206961A (en) | 2023-02-23 | 2023-02-23 | Preparation method of two-dimensional thin film material device based on Van der Waals contact metal electrode |
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