CN117012812A - Method for etching two-dimensional tellurium alkene by combining wet method and dry method - Google Patents

Method for etching two-dimensional tellurium alkene by combining wet method and dry method Download PDF

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CN117012812A
CN117012812A CN202311284518.8A CN202311284518A CN117012812A CN 117012812 A CN117012812 A CN 117012812A CN 202311284518 A CN202311284518 A CN 202311284518A CN 117012812 A CN117012812 A CN 117012812A
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etching
dimensional
tellurium
alkene
dimensional tellurium
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CN117012812B (en
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王一休
杨青
张亮
李凌
付翔
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Zhejiang Lab
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L29/00Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
    • H01L29/02Semiconductor bodies ; Multistep manufacturing processes therefor
    • H01L29/12Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
    • H01L29/18Selenium or tellurium only, apart from doping materials or other impurities
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L29/00Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
    • H01L29/02Semiconductor bodies ; Multistep manufacturing processes therefor
    • H01L29/06Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions
    • H01L29/0657Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions characterised by the shape of the body
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L29/00Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
    • H01L29/02Semiconductor bodies ; Multistep manufacturing processes therefor
    • H01L29/06Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions
    • H01L29/10Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions with semiconductor regions connected to an electrode not carrying current to be rectified, amplified or switched and such electrode being part of a semiconductor device which comprises three or more electrodes
    • H01L29/1025Channel region of field-effect devices
    • H01L29/1029Channel region of field-effect devices of field-effect transistors
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L29/00Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
    • H01L29/66Types of semiconductor device ; Multistep manufacturing processes therefor
    • H01L29/66007Multistep manufacturing processes
    • H01L29/66969Multistep manufacturing processes of devices having semiconductor bodies not comprising group 14 or group 13/15 materials
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L29/00Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
    • H01L29/66Types of semiconductor device ; Multistep manufacturing processes therefor
    • H01L29/68Types of semiconductor device ; Multistep manufacturing processes therefor controllable by only the electric current supplied, or only the electric potential applied, to an electrode which does not carry the current to be rectified, amplified or switched
    • H01L29/76Unipolar devices, e.g. field effect transistors
    • H01L29/772Field effect transistors

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Abstract

The application discloses a method for etching two-dimensional tellurium alkene by combining a wet method and a dry method, which comprises the following steps: providing a single-crystal two-dimensional tellurium alkene; soaking the monocrystal two-dimensional tellurium alkene in hypochlorous acid solution, washing and drying for standby to obtain a first sample; the first sample was washed and etched under Ar atmosphere. The method of the application firstly adopts hypochlorous acid solution to activate the surface of the substrate, and then adopts an inductively coupled plasma machine to carry out the second step of etching. The atomic-level thickness two-dimensional tellurium alkene obtained by the method is flat in surface, and finally has no structural damage to the tellurium alkene.

Description

Method for etching two-dimensional tellurium alkene by combining wet method and dry method
Technical Field
The application relates to a plasma etching technology in the micro-nano processing field, in particular to a method for etching two-dimensional tellurium alkene by combining a wet method and a dry method.
Background
Conventional silicon-based semiconductor devices have begun to become miniaturized year by year in the information age, and such miniaturization is even approaching the physical limits of the materials themselves. However, when the three-dimensional material is continuously reduced, a plurality of problems such as great influence on the whole physical and chemical properties caused by dangling bonds on the surface of the three-dimensional material can occur; such as short channel effects; such as a tendency for mobility to drop sharply with decreasing thickness, etc. At present, the field effect transistor in the semiconductor industry has advanced to the size of a few nanometers, but a real three-terminal sub-5 nanometer short channel field effect transistor device is constructed to effectively avoid the short channel effect, and technical challenges still exist. The trend in this field is to find new materials and develop new technologies to further shrink the device size. Among many alternative new materials, two-dimensional materials represented by graphene stand out. In 2004, graphene was mechanically exfoliated, and then various semiconductors similar to van der waals structures appeared, which also showed better performance in the field of electronic devices. Because the surface of the material has no dangling bond, electrons are bound to move in a two-dimensional plane, so that the mobility of the material is theoretically higher, and the material can avoid the advantages of short channel effect and the like due to the structural characteristics of the material. The synthesis of two-dimensional materials is a hot topic. For mass production and high repeatability, gas phase and liquid phase methods are common synthetic methods, but most of the products are tens of nanometers thick, and for obtaining ideal atomic-level thickness, further etching methods become a very critical step in the synthetic link.
Compared with most two-dimensional materials, the tellurium is quite stable in air, and the tellurium field effect transistor has almost no change in performance when exposed to air for two months at room temperature. Thus, control of the tellurium alkene thickness has become a key ring in studying the material. The thickness of the tellurium alkene material directly synthesized by the hydrothermal method is about 20nm on average, and even through alkaline solution corrosion, the two-dimensional tellurium alkene with average thickness of several nanometers can be obtained. However, the corrosion is not easy to control, the surface of the obtained product is not smooth enough, and parameters are not controlled, even the atomic structure of the tellurium alkene is directly damaged, so that the performance of the device is affected.
Therefore, there is a need to propose a method for etching two-dimensional tellurium with high efficiency and controllability
Disclosure of Invention
Aiming at the defects of the prior art, the application provides a method for etching two-dimensional tellurium alkene by combining a wet method and a dry method.
According to a first aspect of an embodiment of the present application, there is provided a method for etching two-dimensional tellurium by combining a wet method and a dry method, the method comprising:
providing a single-crystal two-dimensional tellurium alkene;
soaking the monocrystal two-dimensional tellurium alkene in hypochlorous acid solution, washing and drying for standby to obtain a first sample;
and washing the first sample, and carrying out plasma etching on the first sample under the Ar atmosphere, wherein Ar gas is used as etching gas.
Further, immersing the single-crystal two-dimensional tellurium alkene in the hypochlorous acid solution comprises: the hypochlorous acid solution is 50-200ppm, and the soaking time is 4-6 hours.
Further, immersing the single-crystal two-dimensional tellurium alkene in the hypochlorous acid solution comprises: the hypochlorous acid solution was 200ppm and the soaking time was 5 hours.
Further, the washing includes: washing was performed with acetone and isopropanol.
Further, the first sample is etched under Ar atmosphere: the flow of Ar gas is more than or equal to 100mL/min, and the etching time is 5min.
According to a second aspect of the embodiment of the application, a two-dimensional tellurium thin film is provided, and the two-dimensional tellurium thin film is etched by the method of etching the two-dimensional tellurium by combining the wet method and the dry method.
According to a third aspect of an embodiment of the present application, there is provided a field effect transistor including: the substrate with the back gate is characterized in that a source electrode and a drain electrode are respectively arranged on two sides of the upper surface of the substrate, and the two-dimensional tellurium alkene thin films are further arranged on the upper surface of the substrate and in the middle of the source electrode and the drain electrode.
According to a fourth aspect of the embodiment of the present application, there is provided a chip, including a chip body and a field effect transistor as described above, wherein the field effect transistor is disposed on the chip body.
According to a fifth aspect of an embodiment of the present application, there is provided a circuit, including a circuit board main body and a chip as described above, wherein the chip is disposed on the circuit board main body.
According to a sixth aspect of embodiments of the present application, there is provided an apparatus comprising a housing and the circuit described above, wherein the circuit is disposed on the housing.
Compared with the prior art, the application has the following beneficial effects:
(1) The method utilizes the effect of hypochlorous acid solution on tellurium surface modification, so that the tellurium which cannot be directly etched by Ar gas can be controllably thinned to atomic-level thickness, and the smoothness of the surface and the stability of the structure are ensured.
(2) The method can etch the tellurium alkene channel material under the condition of protecting the structure of the tellurium alkene channel material, thereby achieving the effects of thinning the channel layer and reducing the size of the device. The performance of the field effect transistor comprising the two-dimensional tellurium alkene film prepared by the method is improved.
(3) The method has the advantages of simple and controllable process, short preparation period, safety, no pollution, low cost, high efficiency and convenience for industrialization. According to actual production requirements, the thickness control can be realized by flexibly modulating process parameters, and the method is an important exploration direction after the industrialization of the tellurium field effect transistor in the future.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort to a person skilled in the art.
FIG. 1 is a schematic flow chart of a method for etching two-dimensional tellurium by combining a wet method and a dry method provided by an embodiment of the application;
FIG. 2 is a photomicrograph of a two-dimensional tellurium alkene provided by an embodiment of the present application;
FIG. 3 is an XRD result pattern of a two-dimensional tellurium alkene provided by an embodiment of the present application;
FIG. 4 is a graph of the atomic force scanning electron microscope result of the two-dimensional tellurium alkene before etching, provided by the embodiment of the application;
FIG. 5 is a graph showing the results of an atomic force scanning electron microscope after etching in accordance with the preferred embodiment of the present application;
FIG. 6 is a graph showing the results of atomic force scanning surface roughness after etching in accordance with the preferred embodiment of the present application;
FIG. 7 is a graph of transfer characteristics of a two-dimensional tellurium-olefin field effect transistor obtained by a preferred embodiment of the present application;
FIG. 8 is a graph showing the results of an Atomic Force Scanning Electron Microscope (AFSEM) of the product before and after etching in example 2 of the present application;
FIG. 9 is a graph showing the results of an Atomic Force Scanning Electron Microscope (AFSEM) of the product before and after etching in example 3 of the present application;
FIG. 10 is a graph showing the results of an Atomic Force Scanning Electron Microscope (AFSEM) of the product before etching in accordance with example 4 of the present application;
FIG. 11 is a graph showing the results of an Atomic Force Scanning Electron Microscope (AFSEM) of the product after etching in example 4 of the present application.
Detailed Description
Reference will now be made in detail to exemplary embodiments, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, the same numbers in different drawings refer to the same or similar elements, unless otherwise indicated. The implementations described in the following exemplary examples do not represent all implementations consistent with the application. Rather, they are merely examples of apparatus and methods consistent with aspects of the application as detailed in the accompanying claims.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in this specification and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It should also be understood that the term "and/or" as used herein refers to and encompasses any or all possible combinations of one or more of the associated listed items.
It should be understood that although the terms first, second, third, etc. may be used herein to describe various information, these information should not be limited by these terms. These terms are only used to distinguish one type of information from another. For example, first information may also be referred to as second information, and similarly, second information may also be referred to as first information, without departing from the scope of the application. The word "if" as used herein may be interpreted as "at … …" or "at … …" or "responsive to a determination", depending on the context.
The present application will be described in detail with reference to the accompanying drawings. The features of the examples and embodiments described below may be combined with each other without conflict.
In the semiconductor industry, inductively Coupled Plasma (ICP) etching machines generate inductively coupled electric fields to coils via a radio frequency power supply, and under the action of the electric fields, etching gas glow discharge generates high density plasma. The method has stronger pertinence by etching the material by utilizing the plasma, and different etching samples need different etching gases and even pretreatment methods. As a new material, how to etch a two-dimensional thin film with ideal thickness and smooth surface by utilizing ICP (inductively coupled plasma) is a problem to be solved. The application provides a method for realizing etching by combining a wet method and a dry method. The method has the advantages that hypochlorous acid is utilized to pretreat the tellurium, ar gas is selected for ICP etching, the thickness of the obtained product is controllable, the surface is smooth, the structure is not damaged, and the two-dimensional tellurium thin film prepared by the method also shows excellent electrical performance in the field effect transistor.
As shown in fig. 1, the present application provides a method for etching two-dimensional tellurium alkene by combining a wet method and a dry method, the method comprising:
step S1, providing single-crystal two-dimensional tellurium alkene.
In the examples of the present application, two-dimensional tellurium was prepared using the procedure of Wang YIxiu, qia Gang, wang ruxing, et al, field-effect transistors made from solution-grown two-dimensional tellurene [ J ]. Nature Electronics, 2018, 1 (4): 228-236. Doi: 10.1038/s41928-018-0058-4 ]. Comprising the following steps:
0.1g of sodium tellurite and 0.5g of polyvinylpyrrolidone with molecular weight of 58000 are dissolved in 33mL of deionized water with electric conductivity of 18.2M omega cm, stirred for 30 minutes under a magnetic stirrer to form a solution A with concentration of 0.014mol/L, then 1.65mL of hydrazine hydrate and 3.3mL of ammonia water are mixed to form a solution B, the solution B is added into the solution A, the solution A is put into a hydrothermal reaction container, the solution B is reacted in a 160 ℃ oven for 30 hours after being sealed, product two-dimensional tellurium with width of about 15 micrometers and length of 80 micrometers and thickness of only tens of nanometers is obtained, the product two-dimensional tellurium is repeatedly washed for a plurality of times by acetone and isopropanol, and the product two-dimensional tellurium is transferred onto a substrate with concentration of 100 nm++ 2/Si P.
Further, the hydrothermal reaction container is selected from a reaction kettle, an electric pressure cooker, a soup pot or a beaker.
And S2, soaking the monocrystal two-dimensional tellurium alkene in hypochlorous acid solution, washing with acetone and isopropanol, and drying for later use to obtain a first sample.
Further, the hypochlorous acid solution is 50-200ppm, and the soaking time is 4-6 hours. If a hypochlorous acid solution with low concentration is selected, the soaking time is longer. In this example, the hypochlorous acid solution is preferably 200ppm and the soaking time is preferably 6 hours.
And S3, washing the first sample by using acetone and isopropanol, and performing plasma etching on the first sample under an Ar atmosphere, wherein Ar is used as etching gas.
Further, the flow rate of Ar gas is more than or equal to 100mL/min, and the etching time is 5min.
In this example, ICP-RIE is a physical etching technique in which argon is used as a carrier gasThe body and plasma components, these high energy ions can be used to remove atoms or molecules from the surface of the material. In this example, ar gas is taken as an etching gas, and tellurium without pretreatment cannot be etched by the gas. While other gases commonly used, e.g. O 2 ,SF 6 And the like, the direct etching of the tellurium alkene cannot be realized.
Meanwhile, the etching under the Ar atmosphere has the following beneficial effects:
(1) And (3) cooling gas: argon acts as a coolant during ICP etching, reducing the high temperature generated by the plasma. This helps to maintain a stable temperature within the reaction chamber and prevents overheating.
(2) Stabilizing the plasma: argon is used to stabilize the plasma. The plasma is composed of ionized gas molecules and ions, which are generated by exposure to a high energy radio frequency field. Argon maintains the stability of the plasma, ensures that it is continuously generated, and provides the required energy to etch the material.
(3) Removing etching products: argon may also be used to remove material residues generated during etching. It removes the product from the etched surface by means of physical purging to maintain the accuracy and repeatability of the etching.
(4) Control pressure: the flow and pressure of argon can be used to control the total gas pressure in the reaction chamber, an important parameter of the ICP etching process. By adjusting the argon flow, the etching rate and the etching quality can be controlled.
Example 1
Embodiment 1 is a preferred embodiment, and specifically includes the following steps:
step S1, providing single-crystal two-dimensional tellurium alkene.
The morphology of the single-crystal two-dimensional tellurium alkene product is shown in fig. 2, and the length is hundreds of micrometers, and the width is about 15 micrometers. The xrd results of fig. 3 confirm that the product is elemental tellurium. The atomic force scanning electron microscope results of the thickness and the morphology of the wafer are shown in fig. 4 before etching treatment.
Step S2: and (2) immersing the two-dimensional tellurium alkene obtained in the step (S1) in a hypochlorous acid solution with the concentration of 200ppm for 5 hours, taking out, washing with acetone and isopropanol, and drying for later use to obtain a first sample.
Step S3: the first sample obtained in S2 was repeatedly washed with acetone and isopropyl alcohol, and then placed in an Inductively Coupled Plasma (ICP) etcher, using an STS Multiplex etcher from STS company, with two paths of radio frequency power of 13.56MHz. The etching gas in the cavity is set to be Ar gas. In the cavity, the flow of Ar gas is set to be 100mL/min, the etching time is controlled to be about 5min, the longer the etching time is, the deeper the etching is, and the final etching depth also depends on the concentration and the time of the hypochlorous acid solution activated in the first step.
After etching, the material thickness was measured by an atomic force scanning electron microscope, and the result is shown in fig. 5. And the surface smoothness of the product obtained in example 1 was also scanned, and the results are shown in fig. 6, and fig. 6 shows a graph of atomic force microscope scanning results over an area of 1.5um in length and 1.5um in width.
As can be seen from the comparison of FIG. 4 and FIG. 5, the etching thinning effect is obvious by simultaneously acting on two-dimensional tellurium alkene through a dry method and a wet method, and the original 39.7nm is reduced to 6.2nm. As is clear from FIG. 6, the product obtained in example 1 had a very smooth surface with a roughness of about 0.2 nm.
Step S4: and (3) continuously processing the ultrathin tellurium obtained in the step S3 through a standard micro-nano processing flow (spin coating, exposure, development and evaporation) to obtain the back electrode field effect transistor.
Step S5: the transfer characteristic curve of the field effect transistor was tested by standard semiconductor test with a probe station and a semiconductor tester, as shown in fig. 7, and the field effect transistor was found to exhibit better modulation performance, indicating that the tellurium structure was not destroyed.
As can be seen from FIG. 7, the field effect transistor prepared based on the ultrathin tellurium has good semiconductor field effect transistor performance, and the mobility can reach 694cm 2 /Vs。
Example 2
Step S1, providing single-crystal two-dimensional tellurium alkene.
Before the etching treatment, the atomic force scanning electron microscope result of the morphology of the single-crystal two-dimensional tellurium is shown in (a) of fig. 8, and the atomic force scanning electron microscope result of the thickness of the single-crystal two-dimensional tellurium is shown in (B) of fig. 8.
Step S2: the single-crystal two-dimensional tellurium alkene obtained in the step S1 was immersed in a hypochlorous acid solution with a concentration of 200ppm for 5 hours, taken out, dried and tested for thickness as shown in (C) of FIG. 8.
In this example 2, the dry method (i.e., etching in an Ar gas atmosphere) was omitted as a comparative example, and as is apparent from comparison of (B) in FIG. 8 and (C) in FIG. 8, the thickness of the tellurium is not substantially changed. It is explained that the etching thinning of the tellurium alkene cannot be realized by soaking the tellurium alkene in the hypochlorous acid solution alone.
Example 3
Step S1, providing single-crystal two-dimensional tellurium alkene.
Before the etching treatment, the atomic force scanning electron microscope result of the morphology of the single-crystal two-dimensional tellurium is shown in (a) of fig. 9, and the atomic force scanning electron microscope result of the thickness of the single-crystal two-dimensional tellurium is shown in (B) of fig. 9.
Step S2: repeatedly cleaning the monocrystal two-dimensional tellurium alkene obtained in the step S1 by using acetone and isopropanol, then placing the cleaned monocrystal two-dimensional tellurium alkene into an Inductively Coupled Plasma (ICP) etcher, and adopting an STS Multiplex etcher of STS company, wherein the two paths of radio frequency power are 13.56MHz. The etching gas in the cavity is set to be Ar gas. The flow rate of Ar gas in the cavity is set to be 100mL/min, the etching time is controlled to be about 5min, and after the etching is finished, an atomic force scanning electron microscope is used for testing the thickness of the material, and the result is shown in (C) of FIG. 9.
This example 3, as a comparative example, was free of the wet process (i.e., the pretreatment step of adding hypochlorous acid was omitted), and as can be seen from a comparison of (B) in fig. 9 and (C) in fig. 9, the inductively coupled plasma method alone failed to thin the two-dimensional tellurium.
Example 4
Step S1, providing single-crystal two-dimensional tellurium alkene.
Before the etching treatment, the atomic force scanning electron microscope result of the morphology of the single-crystal two-dimensional tellurium is shown in (a) of fig. 10, and the atomic force scanning electron microscope result of the thickness of the single-crystal two-dimensional tellurium is shown in (B) of fig. 10.
Step S2: and (2) soaking the monocrystal two-dimensional tellurium alkene obtained in the step (S1) in hypochlorous acid solution with the concentration of 200ppm for 3 hours, taking out, washing with acetone and isopropanol, and drying for later use to obtain a first sample.
Step S3: and (2) repeatedly cleaning the first sample obtained in the step (2) by using acetone and isopropanol, and then placing the cleaned sample into an Inductively Coupled Plasma (ICP) etcher, wherein two paths of radio frequency power are 13.56MHz by using an STS Multiplex etcher of STS company. The etching gas in the cavity is set to be Ar gas. In the cavity, the flow of Ar gas is set to be 100mL/min, and the etching time is controlled to be about 5min. After the completion, the morphology and thickness of the material were measured by an atomic force scanning electron microscope, the atomic force scanning electron microscope result of the morphology of the single-crystal two-dimensional tellurium is shown in fig. 11 (a), and the atomic force scanning electron microscope result of the thickness of the single-crystal two-dimensional tellurium is shown in fig. 11 (B).
In example 4, the hypochlorous acid treatment time was shortened, and as can be seen from comparison of fig. 10 and 11, the thinning speed was greatly slowed down. The length of the process time in this step thus affects the depth and etch rate after the final etch.
Example 5
Step S1, providing single-crystal two-dimensional tellurium alkene.
Step S2: and (2) soaking the monocrystal two-dimensional tellurium alkene obtained in the step (S1) in hypochlorous acid solution for 7 hours, taking out, washing with acetone and isopropanol, and drying for later use to obtain a first sample.
Step S3: and (2) repeatedly cleaning the first sample obtained in the step (2) by using acetone and isopropanol, and then placing the cleaned sample into an Inductively Coupled Plasma (ICP) etcher, wherein two paths of radio frequency power are 13.56MHz by using an STS Multiplex etcher of STS company. The etching gas in the cavity is set to be Ar gas. And setting the flow rate of Ar gas to be 100mL/min in the cavity, and controlling the etching time to be about 5min to obtain the ultrathin tellurium alkene.
Step S4: and (3) continuing to process the step S3 through a standard micro-nano processing flow (spin coating, exposure, development and evaporation) to obtain the ultrathin tellurium, thereby obtaining the back electrode field effect transistor.
Step S5: standard semiconductor tests were performed with the probe station and semiconductor tester to determine if the tellurium alkene was completely destroyed.
The time of hypochlorous acid was prolonged in example 5, and it was found that in the final product, there was a portion of the original thinner tellurium-alkene channel material, and the source-drain electrode was disconnected, indicating that too long a time would completely destroy some of the originally thinner two-dimensional crystals.
Example 6
Step S1, providing single-crystal two-dimensional tellurium alkene. And obtaining an atomic force scanning electron microscope result graph of the morphology and the thickness of the monocrystal two-dimensional tellurium alkene.
Step S2: and (2) immersing the two-dimensional tellurium alkene obtained in the step (S1) in a hypochlorous acid solution with the concentration of 50ppm for 6 hours, taking out, washing with acetone and isopropanol, and drying for later use to obtain a first sample.
Step S3: the first sample obtained in S2 was repeatedly washed with acetone and isopropyl alcohol, and then placed in an Inductively Coupled Plasma (ICP) etcher, using an STS Multiplex etcher from STS company, with two paths of radio frequency power of 13.56MHz. The etching gas in the cavity is set to be Ar gas. And setting the flow rate of Ar gas to be 105mL/min in the cavity, and etching for 5min.
And after etching, testing the appearance and thickness of the product by using an atomic force scanning electron microscope. The etching thinning effect of this embodiment 6 is obvious by comparing the morphology before and after etching and the thickness variation.
Step S4: and (3) continuously processing the ultrathin tellurium obtained in the step S3 through a standard micro-nano processing flow (spin coating, exposure, development and evaporation) to obtain the back electrode field effect transistor.
Step S5: the transfer characteristic curve of the field effect transistor is tested by using a probe station and a semiconductor tester to carry out standard semiconductor, and the field effect transistor is found to show better modulation performance, which indicates that the tellurium alkene structure is not destroyed.
Example 7
Step S1, providing single-crystal two-dimensional tellurium alkene. And obtaining an atomic force scanning electron microscope result graph of the morphology and the thickness of the monocrystal two-dimensional tellurium alkene.
Step S2: and (2) immersing the two-dimensional tellurium alkene obtained in the step (S1) in a hypochlorous acid solution with the concentration of 60ppm for 6 hours, taking out, washing with acetone and isopropanol, and drying for later use to obtain a first sample.
Step S3: the first sample obtained in S2 was repeatedly washed with acetone and isopropyl alcohol, and then placed in an Inductively Coupled Plasma (ICP) etcher, using an STS Multiplex etcher from STS company, with two paths of radio frequency power of 13.56MHz. The etching gas in the cavity is set to be Ar gas. And setting the flow rate of Ar gas to be 110mL/min in the cavity, and etching for 5min.
And after etching, testing the appearance and thickness of the product by using an atomic force scanning electron microscope. The etching thinning effect of this embodiment 7 is obvious by comparing the morphology before and after etching and the thickness variation.
Step S4: and (3) continuously processing the ultrathin tellurium obtained in the step S3 through a standard micro-nano processing flow (spin coating, exposure, development and evaporation) to obtain the back electrode field effect transistor.
Step S5: the transfer characteristic curve of the field effect transistor is tested by using a probe station and a semiconductor tester to carry out standard semiconductor, and the field effect transistor is found to show better modulation performance, which indicates that the tellurium alkene structure is not destroyed.
Example 8
Step S1, providing single-crystal two-dimensional tellurium alkene. And obtaining an atomic force scanning electron microscope result graph of the morphology and the thickness of the monocrystal two-dimensional tellurium alkene.
Step S2: and (2) immersing the two-dimensional tellurium alkene obtained in the step (S1) in a hypochlorous acid solution with the concentration of 80ppm for 6 hours, taking out, washing with acetone and isopropanol, and drying for later use to obtain a first sample.
Step S3: the first sample obtained in S2 was repeatedly washed with acetone and isopropyl alcohol, and then placed in an Inductively Coupled Plasma (ICP) etcher, using an STS Multiplex etcher from STS company, with two paths of radio frequency power of 13.56MHz. The etching gas in the cavity is set to be Ar gas. And setting the flow rate of Ar gas to be 110mL/min in the cavity, and etching for 5min.
And after etching, testing the appearance and thickness of the product by using an atomic force scanning electron microscope. The etching thinning effect of this embodiment 8 is obvious by comparing the morphology before and after etching and the thickness variation.
Step S4: and (3) continuously processing the ultrathin tellurium obtained in the step S3 through a standard micro-nano processing flow (spin coating, exposure, development and evaporation) to obtain the back electrode field effect transistor.
Step S5: the transfer characteristic curve of the field effect transistor is tested by using a probe station and a semiconductor tester to carry out standard semiconductor, and the field effect transistor is found to show better modulation performance, which indicates that the tellurium alkene structure is not destroyed.
Example 9
Step S1, providing single-crystal two-dimensional tellurium alkene. And obtaining an atomic force scanning electron microscope result graph of the morphology and the thickness of the monocrystal two-dimensional tellurium alkene.
Step S2: and (2) immersing the two-dimensional tellurium alkene obtained in the step (S1) in a hypochlorous acid solution with the concentration of 100ppm for 6 hours, taking out, washing with acetone and isopropanol, and drying for later use to obtain a first sample.
Step S3: the first sample obtained in S2 was repeatedly washed with acetone and isopropyl alcohol, and then placed in an Inductively Coupled Plasma (ICP) etcher, using an STS Multiplex etcher from STS company, with two paths of radio frequency power of 13.56MHz. The etching gas in the cavity is set to be Ar gas. And setting the flow rate of Ar gas to be 105mL/min in the cavity, and etching for 5min.
And after etching, testing the appearance and thickness of the product by using an atomic force scanning electron microscope. The etching thinning effect of this embodiment 9 is obvious by comparing the morphology before and after etching and the thickness variation.
Step S4: and (3) continuously processing the ultrathin tellurium obtained in the step S3 through a standard micro-nano processing flow (spin coating, exposure, development and evaporation) to obtain the back electrode field effect transistor.
Step S5: the transfer characteristic curve of the field effect transistor is tested by using a probe station and a semiconductor tester to carry out standard semiconductor, and the field effect transistor is found to show better modulation performance, which indicates that the tellurium alkene structure is not destroyed.
Example 10
Step S1, providing single-crystal two-dimensional tellurium alkene. And obtaining an atomic force scanning electron microscope result graph of the morphology and the thickness of the monocrystal two-dimensional tellurium alkene.
Step S2: and (2) immersing the two-dimensional tellurium alkene obtained in the step (S1) in a hypochlorous acid solution with the concentration of 120ppm for 5.5 hours, taking out, washing with acetone and isopropanol, and drying for later use to obtain a first sample.
Step S3: the first sample obtained in S2 was repeatedly washed with acetone and isopropyl alcohol, and then placed in an Inductively Coupled Plasma (ICP) etcher, using an STS Multiplex etcher from STS company, with two paths of radio frequency power of 13.56MHz. The etching gas in the cavity is set to be Ar gas. And setting the flow rate of Ar gas to be 105mL/min in the cavity, and etching for 5min.
And after etching, testing the appearance and thickness of the product by using an atomic force scanning electron microscope. The etching thinning effect of this embodiment 10 is obvious by comparing the morphology before and after etching and the thickness variation.
Step S4: and (3) continuously processing the ultrathin tellurium obtained in the step S3 through a standard micro-nano processing flow (spin coating, exposure, development and evaporation) to obtain the back electrode field effect transistor.
Step S5: the transfer characteristic curve of the field effect transistor is tested by using a probe station and a semiconductor tester to carry out standard semiconductor, and the field effect transistor is found to show better modulation performance, which indicates that the tellurium alkene structure is not destroyed.
Example 11
Step S1, providing single-crystal two-dimensional tellurium alkene. And obtaining an atomic force scanning electron microscope result graph of the morphology and the thickness of the monocrystal two-dimensional tellurium alkene.
Step S2: and (2) immersing the two-dimensional tellurium alkene obtained in the step (S1) in a hypochlorous acid solution with the concentration of 135ppm for 5.5 hours, taking out, washing with acetone and isopropanol, and drying for later use to obtain a first sample.
Step S3: the first sample obtained in S2 was repeatedly washed with acetone and isopropyl alcohol, and then placed in an Inductively Coupled Plasma (ICP) etcher, using an STS Multiplex etcher from STS company, with two paths of radio frequency power of 13.56MHz. The etching gas in the cavity is set to be Ar gas. And setting the flow rate of Ar gas to be 105mL/min in the cavity, and etching for 5min.
And after etching, testing the appearance and thickness of the product by using an atomic force scanning electron microscope. The etching thinning effect of this embodiment 11 is obvious by comparing the morphology before and after etching and the thickness variation.
Step S4: and (3) continuously processing the ultrathin tellurium obtained in the step S3 through a standard micro-nano processing flow (spin coating, exposure, development and evaporation) to obtain the back electrode field effect transistor.
Step S5: the transfer characteristic curve of the field effect transistor is tested by using a probe station and a semiconductor tester to carry out standard semiconductor, and the field effect transistor is found to show better modulation performance, which indicates that the tellurium alkene structure is not destroyed.
Example 12
Step S1, providing single-crystal two-dimensional tellurium alkene. And obtaining an atomic force scanning electron microscope result graph of the morphology and the thickness of the monocrystal two-dimensional tellurium alkene.
Step S2: and (2) immersing the two-dimensional tellurium alkene obtained in the step (S1) in a hypochlorous acid solution with the concentration of 140ppm for 5 hours, taking out, washing with acetone and isopropanol, and drying for later use to obtain a first sample.
Step S3: the first sample obtained in S2 was repeatedly washed with acetone and isopropyl alcohol, and then placed in an Inductively Coupled Plasma (ICP) etcher, using an STS Multiplex etcher from STS company, with two paths of radio frequency power of 13.56MHz. The etching gas in the cavity is set to be Ar gas. And setting the flow rate of Ar gas to be 105mL/min in the cavity, and etching for 5min.
And after etching, testing the appearance and thickness of the product by using an atomic force scanning electron microscope. The etching thinning effect of this embodiment 12 is obvious by comparing the morphology before and after etching and the thickness variation.
Step S4: and (3) continuously processing the ultrathin tellurium obtained in the step S3 through a standard micro-nano processing flow (spin coating, exposure, development and evaporation) to obtain the back electrode field effect transistor.
Step S5: the transfer characteristic curve of the field effect transistor is tested by using a probe station and a semiconductor tester to carry out standard semiconductor, and the field effect transistor is found to show better modulation performance, which indicates that the tellurium alkene structure is not destroyed.
Example 13
Step S1, providing single-crystal two-dimensional tellurium alkene. And obtaining an atomic force scanning electron microscope result graph of the morphology and the thickness of the monocrystal two-dimensional tellurium alkene.
Step S2: and (2) immersing the two-dimensional tellurium alkene obtained in the step (S1) in a hypochlorous acid solution with the concentration of 160ppm for 5 hours, taking out, washing with acetone and isopropanol, and drying for later use to obtain a first sample.
Step S3: the first sample obtained in S2 was repeatedly washed with acetone and isopropyl alcohol, and then placed in an Inductively Coupled Plasma (ICP) etcher, using an STS Multiplex etcher from STS company, with two paths of radio frequency power of 13.56MHz. The etching gas in the cavity is set to be Ar gas. In the cavity, the flow of Ar gas is set to be 100mL/min, and the etching time is 5min.
And after etching, testing the appearance and thickness of the product by using an atomic force scanning electron microscope. The etching thinning effect of this embodiment 13 is obvious by comparing the morphology before and after etching and the thickness variation.
Step S4: and (3) continuously processing the ultrathin tellurium obtained in the step S3 through a standard micro-nano processing flow (spin coating, exposure, development and evaporation) to obtain the back electrode field effect transistor.
Step S5: the transfer characteristic curve of the field effect transistor is tested by using a probe station and a semiconductor tester to carry out standard semiconductor, and the field effect transistor is found to show better modulation performance, which indicates that the tellurium alkene structure is not destroyed.
Example 14
Step S1, providing single-crystal two-dimensional tellurium alkene. And obtaining an atomic force scanning electron microscope result graph of the morphology and the thickness of the monocrystal two-dimensional tellurium alkene.
Step S2: and (2) immersing the two-dimensional tellurium alkene obtained in the step (S1) in a hypochlorous acid solution with the concentration of 170ppm for 4.5 hours, taking out, washing with acetone and isopropanol, and drying for later use to obtain a first sample.
Step S3: the first sample obtained in S2 was repeatedly washed with acetone and isopropyl alcohol, and then placed in an Inductively Coupled Plasma (ICP) etcher, using an STS Multiplex etcher from STS company, with two paths of radio frequency power of 13.56MHz. The etching gas in the cavity is set to be Ar gas. In the cavity, the flow of Ar gas is set to be 100mL/min, and the etching time is 5min.
And after etching, testing the appearance and thickness of the product by using an atomic force scanning electron microscope. The etching thinning effect of this embodiment 14 is obvious by comparing the morphology before and after etching and the thickness variation.
Step S4: and (3) continuously processing the ultrathin tellurium obtained in the step S3 through a standard micro-nano processing flow (spin coating, exposure, development and evaporation) to obtain the back electrode field effect transistor.
Step S5: the transfer characteristic curve of the field effect transistor is tested by using a probe station and a semiconductor tester to carry out standard semiconductor, and the field effect transistor is found to show better modulation performance, which indicates that the tellurium alkene structure is not destroyed.
Example 15
Step S1, providing single-crystal two-dimensional tellurium alkene. And obtaining an atomic force scanning electron microscope result graph of the morphology and the thickness of the monocrystal two-dimensional tellurium alkene.
Step S2: and (2) immersing the two-dimensional tellurium alkene obtained in the step (S1) in a hypochlorous acid solution with the concentration of 180ppm for 4 hours, taking out, washing with acetone and isopropanol, and drying for later use to obtain a first sample.
Step S3: the first sample obtained in S2 was repeatedly washed with acetone and isopropyl alcohol, and then placed in an Inductively Coupled Plasma (ICP) etcher, using an STS Multiplex etcher from STS company, with two paths of radio frequency power of 13.56MHz. The etching gas in the cavity is set to be Ar gas. In the cavity, the flow of Ar gas is set to be 100mL/min, and the etching time is 5min.
And after etching, testing the appearance and thickness of the product by using an atomic force scanning electron microscope. The etching thinning effect of this embodiment 15 is obvious by comparing the morphology before and after etching and the thickness variation.
Step S4: and (3) continuously processing the ultrathin tellurium obtained in the step S3 through a standard micro-nano processing flow (spin coating, exposure, development and evaporation) to obtain the back electrode field effect transistor.
Step S5: the transfer characteristic curve of the field effect transistor is tested by using a probe station and a semiconductor tester to carry out standard semiconductor, and the field effect transistor is found to show better modulation performance, which indicates that the tellurium alkene structure is not destroyed.
Example 16
Step S1, providing single-crystal two-dimensional tellurium alkene. And obtaining an atomic force scanning electron microscope result graph of the morphology and the thickness of the monocrystal two-dimensional tellurium alkene.
Step S2: and (2) immersing the two-dimensional tellurium alkene obtained in the step (S1) in a hypochlorous acid solution with the concentration of 190ppm for 4 hours, taking out, washing with acetone and isopropanol, and drying for later use to obtain a first sample.
Step S3: the first sample obtained in S2 was repeatedly washed with acetone and isopropyl alcohol, and then placed in an Inductively Coupled Plasma (ICP) etcher, using an STS Multiplex etcher from STS company, with two paths of radio frequency power of 13.56MHz. The etching gas in the cavity is set to be Ar gas. In the cavity, the flow of Ar gas is set to be 100mL/min, and the etching time is 5min.
And after etching, testing the appearance and thickness of the product by using an atomic force scanning electron microscope. The etching thinning effect of this embodiment 16 is obvious by comparing the morphology before and after etching and the thickness variation.
Step S4: and (3) continuously processing the ultrathin tellurium obtained in the step S3 through a standard micro-nano processing flow (spin coating, exposure, development and evaporation) to obtain the back electrode field effect transistor.
Step S5: the transfer characteristic curve of the field effect transistor is tested by using a probe station and a semiconductor tester to carry out standard semiconductor, and the field effect transistor is found to show better modulation performance, which indicates that the tellurium alkene structure is not destroyed.
It is worth mentioning that the embodiment of the application also provides a two-dimensional tellurium alkene film which is etched by the method for etching the two-dimensional tellurium alkene by combining the wet method and the dry method.
The embodiment of the application also provides a field effect transistor, which comprises: the substrate with the back gate is characterized in that a source electrode and a drain electrode are respectively arranged on two sides of the upper surface of the substrate, and the two-dimensional tellurium alkene thin films are further arranged on the upper surface of the substrate and in the middle of the source electrode and the drain electrode.
It should be noted that the embodiment of the present application also provides a chip, which may include a chip body and the field effect transistor in the above embodiment, where the field effect transistor is disposed on the chip body.
The embodiment of the application also provides a circuit which can comprise a circuit board main body and the chip in the embodiment, wherein the circuit is arranged on the circuit board main body.
The embodiment of the application also provides a device, and the integrated storage device can comprise a shell and the circuit in the embodiment, wherein the circuit is arranged on the shell.
In conclusion, the method utilizes the effect of hypochlorous acid solution on tellurium surface modification, so that the tellurium which cannot be directly etched by Ar gas can be controllably thinned to atomic-level thickness, and the smoothness of the surface and the stability of the structure are ensured. The method can etch the tellurium alkene channel material under the condition of protecting the structure of the tellurium alkene channel material, thereby achieving the effects of thinning the channel layer and reducing the size of the device. The performance of the field effect transistor comprising the two-dimensional tellurium alkene film prepared by the method is improved. The method has the advantages of simple and controllable process, short preparation period, safety, no pollution, low cost, high efficiency and convenience for industrialization. According to actual production requirements, the thickness control can be realized by flexibly modulating process parameters, and the method is an important exploration direction after the industrialization of the tellurium field effect transistor in the future.
Other embodiments of the application will be apparent to those skilled in the art from consideration of the specification and practice of the disclosure herein. This application is intended to cover any variations, uses, or adaptations of the application following, in general, the principles of the application and including such departures from the present disclosure as come within known or customary practice within the art to which the application pertains. The specification and examples are to be regarded in an illustrative manner only.
It is to be understood that the application is not limited to the precise arrangements and instrumentalities shown in the drawings, which have been described above, and that various modifications and changes may be effected without departing from the scope thereof.

Claims (10)

1. A method for etching two-dimensional tellurium by combining a wet method and a dry method, which is characterized by comprising the following steps:
providing a single-crystal two-dimensional tellurium alkene;
soaking the monocrystal two-dimensional tellurium alkene in hypochlorous acid solution, washing and drying for standby to obtain a first sample;
and washing the first sample, and carrying out plasma etching on the first sample under the Ar atmosphere, wherein Ar gas is used as etching gas.
2. The method for etching two-dimensional tellurium by combining a wet process and a dry process as claimed in claim 1, wherein immersing the single crystal two-dimensional tellurium in hypochlorous acid solution comprises: the hypochlorous acid solution is 50-200ppm, and the soaking time is 4-6 hours.
3. The method for etching two-dimensional tellurium by combining a wet process and a dry process as claimed in claim 2, wherein immersing the single-crystal two-dimensional tellurium in hypochlorous acid solution comprises: the hypochlorous acid solution was 200ppm and the soaking time was 5 hours.
4. A method of etching a two-dimensional tellurium alkene by a combination of wet and dry processes as claimed in claim 1, wherein the washing comprises: washing was performed with acetone and isopropanol.
5. The method for etching two-dimensional tellurium alkene by combining a wet method and a dry method according to claim 1, wherein the first sample is etched under Ar atmosphere: the flow of Ar gas is more than or equal to 100mL/min, and the etching time is 5min.
6. A two-dimensional tellurium thin film, which is etched by the method of etching two-dimensional tellurium by combining the wet method and the dry method as claimed in any one of claims 1 to 5.
7. A field effect transistor, comprising: a substrate with a back gate, wherein a source electrode and a drain electrode are respectively arranged on two sides of the upper surface of the substrate, and the two-dimensional tellurium alkene thin film as claimed in claim 6 is further arranged on the upper surface of the substrate and in the middle of the source electrode and the drain electrode.
8. A chip comprising a chip body and the field effect transistor of claim 7, wherein the field effect transistor is disposed on the chip body.
9. A circuit comprising a circuit board body and the chip of claim 8, wherein the chip is disposed on the circuit board body.
10. An apparatus comprising a housing and the circuit of claim 9, wherein the circuit is disposed on the housing.
CN202311284518.8A 2023-10-07 2023-10-07 Method for etching two-dimensional tellurium alkene by combining wet method and dry method Active CN117012812B (en)

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Publication number Priority date Publication date Assignee Title
CN112537796A (en) * 2020-12-08 2021-03-23 南京大学 Low-energy light-excited material nondestructive thinning method
CN113421826A (en) * 2021-06-18 2021-09-21 南京大学 Atomic-level precision lossless layer-by-layer etching method for two-dimensional layered material
CN115101404A (en) * 2022-06-10 2022-09-23 香港理工大学深圳研究院 Two-dimensional tellurine local thinning method
CN116314260A (en) * 2023-02-08 2023-06-23 南京航空航天大学 Manufacturing method of two-dimensional material field effect transistor

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112537796A (en) * 2020-12-08 2021-03-23 南京大学 Low-energy light-excited material nondestructive thinning method
CN113421826A (en) * 2021-06-18 2021-09-21 南京大学 Atomic-level precision lossless layer-by-layer etching method for two-dimensional layered material
CN115101404A (en) * 2022-06-10 2022-09-23 香港理工大学深圳研究院 Two-dimensional tellurine local thinning method
CN116314260A (en) * 2023-02-08 2023-06-23 南京航空航天大学 Manufacturing method of two-dimensional material field effect transistor

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