CN116124838A - WTE (wire train engine) 2 Electrode single-molecule test chip and preparation method thereof - Google Patents

WTE (wire train engine) 2 Electrode single-molecule test chip and preparation method thereof Download PDF

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CN116124838A
CN116124838A CN202310107993.1A CN202310107993A CN116124838A CN 116124838 A CN116124838 A CN 116124838A CN 202310107993 A CN202310107993 A CN 202310107993A CN 116124838 A CN116124838 A CN 116124838A
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electrode
wte
patterned
test chip
steps
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洪文晶
林荣健
刘俊扬
卢至行
郑珏婷
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Xiamen University
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Xiamen University
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
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    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65—Raman scattering
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention relates to a WTE 2 The electrode single molecule test chip and the preparation method thereof comprise the following steps: for the electricityPerforming magnetron sputtering on the electrode pattern to metal tungsten, enabling the metal tungsten to cover the electrode pattern to form a metal tungsten film, and washing off photoresist to obtain a metal tungsten electrode corresponding to the electrode pattern; performing high-temperature thermal oxidation on the metal tungsten electrode to generate electrode-patterned tungsten oxide, adding tellurium powder, and performing high Wen Dihua on the electrode-patterned tungsten oxide under the action of carrier gas and reducing gas to generate electrode-patterned 1T' -WTE 2 The method comprises the steps of carrying out a first treatment on the surface of the Cutting the middle position to form a pointed structure to obtain 1T' -WTE 2 An electrode; suspending the opposite tip structure to obtain electrode patterned 1T' -WTE 2 An electrode single molecule chip.

Description

WTE (wire train engine) 2 Electrode single-molecule test chip and preparation method thereof
Technical Field
The invention relates to the field of electrode single-molecule test chips, in particular to a WTE 2 An electrode single molecule test chip and a preparation method thereof.
Background
The molecular connection to the circuit via the electrode to construct molecular junction and realize the characterization of its electric property is the basic idea of molecular electronics. The molecular junction consists of three parts, namely an electrode/a molecule/an electrode, and the structure of the molecular junction is known that in the charge transport process of the molecular junction, charges are firstly injected into the molecule from one electrode and then collected by the other electrode, and the injection and collection of the charges occur at the interface of the molecule and the electrode, so that the interaction between the molecule and the electrode can greatly influence the electrical property of the molecular junction.
The electrode-molecule coupling affects the relative positions of the molecular front orbitals and the electrode fermi levels, determining the mechanism of charge transport in the molecular junction. Metal materials are commonly used as electrodes in current research reports, such as Au, ag, pt, cu and the like. The metal electrode is connected with the anchoring group of the molecule through covalent bond formation to realize the construction of a molecular junction, which can lead to the formation of strong coupling effect between the electrode and the molecule. However, the quenching effect caused by strong coupling can inhibit the expression of intrinsic properties of the molecules, such as fluorescence, optical switching, thermoelectric, and the like. Therefore, the coupling effect between the molecular electrodes is reduced, the intrinsic property of the molecules is more likely to be obtained, and the preparation of high-performance molecular devices is realized.
Meanwhile, if the electrode and the molecule are connected through van der Waals effect, the coupling between the electrode and the molecule is usually weak. For example, by adopting a nonmetallic electrode such as a single-wall carbon nanotube, graphene and the like to construct a molecular junction through van der Waals effect, the coupling between molecules and the electrode can be effectively reduced. However, such molecular junctions have a large contact resistance, which impedes the charge transport process, resulting in a lower molecular junction conductance.
In summary, how to balance the coupling and contact resistance is a difficulty in the prior art, and there is no method for the compatibility of motor materials and cracking technology in the art.
In order to solve the problems in the prior art, a WTE is designed 2 The electrode single molecule test chip and the preparation method thereof are the aim of the research of the invention.
Disclosure of Invention
In view of the above problems of the prior art, the present invention is to provide a WTE 2 The electrode single-molecule test chip and the preparation method thereof can effectively solve at least one problem existing in the prior art.
The technical scheme of the invention is as follows:
WTE (wire train engine) 2 The preparation method of the electrode single-molecule test chip comprises the following steps:
taking a molybdenum sheet with polished double surfaces as a substrate, ultrasonically cleaning and drying;
growing a silicon oxide layer on the upper surface of the molybdenum sheet through plasma enhanced chemical vapor deposition;
spin-coating photoresist on the upper surface of the silicon oxide layer and drying;
carrying out mask photoetching and developing on the photoresist, so as to develop an electrode pattern corresponding to a mask template on the photoresist, wherein the mask template comprises conductive external circuit area templates which are arranged in a bilateral symmetry manner and lead templates connected between the conductive external circuit areas;
performing magnetron sputtering on the electrode pattern to metal tungsten, enabling the metal tungsten to cover the electrode pattern to form a metal tungsten film, and washing off photoresist to obtain a metal tungsten electrode corresponding to the electrode pattern;
performing high-temperature thermal oxidation on the metal tungsten electrode to generate electrode-patterned tungsten oxide, adding tellurium powder, and patterning the electrode-patterned tungsten oxide under the action of carrier gas and reducing gasHigh Wen Dihua electrode patterning 1T' -WTE 2 ；
Patterning of the electrode with FIB 1T' -WTe 2 Cutting the middle position of the wire template to form a sharp structure to obtain 1T' -WTE 2 An electrode;
suspending the opposite tip structure by wet etching the silicon oxide layer near the opposite tip structure to obtain electrode patterned 1T' -WTE 2 An electrode single molecule chip.
Further, siH 4 And O 2 And (3) performing plasma enhanced chemical vapor deposition to grow a silicon oxide layer as a reaction gas, and/or wherein the thickness of the silicon oxide layer is 1-3um.
Further, positive photoresist is adopted as the photoresist;
the mask photoetching and developing of the photoresist comprises the following steps:
performing first ultraviolet exposure on the positive photoresist according to the mask template, and performing photolysis reaction to generate carboxylic acid;
the carboxylic acid promotes the resin of the first ultraviolet exposure area in the positive photoresist to generate a crosslinking reaction at high temperature, so that the ultraviolet exposure area in the positive photoresist is insoluble in an alkaline developer;
and taking down the mask template to carry out second ultraviolet exposure, generating carboxylic acid in the area which is not subjected to the first ultraviolet exposure, and dissolving the carboxylic acid in an alkaline developer after developing to obtain the pattern identical to the mask template.
Further, the step of performing high-temperature thermal oxidation on the metal tungsten electrode to generate electrode-patterned tungsten oxide comprises the following steps:
placing the metal tungsten electrode in a tube furnace, and performing high-temperature thermal oxidation at 600-660 ℃.
Further, tellurium powder is added, and under the action of carrier gas and reducing gas, the electrode-patterned tungsten oxide is subjected to high Wen Dihua to generate electrode-patterned 1T' -WTE 2 Comprising the following steps:
sequentially placing tellurium powder and molybdenum sheets of tungsten oxide with the electrode patterns in the tube furnace according to a gas flow path;
heating to 600-660 ℃ by a tube furnace to sublimate tellurium powder, driving tellurium to contact with the electrode-patterned tungsten oxide by the carrier gas, and generating electrode-patterned 1T' -WTE by the reduction reaction of the reduction gas 2 。
Further, the carrier gas is Ar, and the reducing gas is H 2 Ar and H 2 Is 95:5 by volume.
Further, the tellurium powder is tellurium powder with a molecular sieve.
Further, electrode patterned 1T' -WTE is generated 2 Thereafter, execution is performed:
obtaining the electrode patterned 1T' -WTE 2 Determining the product as 1T' -WTE based on the Raman spectrum of the polymer and/or the electron diffraction pattern of the electrode patterning 2 。
WTE (wire train engine) 2 An electrode single molecule test chip comprising:
the upper surface of the substrate is provided with a silicon oxide layer, and the middle area of the silicon oxide layer is corroded by a wet method to form a groove;
1T'-WTe 2 the electrode comprises two conductive external circuit areas, a wire and a pair tip structure, wherein the number of the conductive external circuit areas is two, the two conductive external circuit areas are respectively arranged on the silicon oxide layer in a left-right mode, two ends of the wire respectively start from the conductive external circuit areas and extend to the middle area of the silicon oxide layer, the pair tip structure is arranged at the middle position of the wire, and the pair tip structure is suspended in the middle area of the silicon oxide layer.
Further, the WTE 2 The application method of the electrode single-molecule test chip comprises the following steps:
fixing the WTE 2 The left end and the right end of the electrode single-molecule test chip;
from the WTE by a stepper motor 2 The WTE is propped up right below the middle area of the electrode single-molecule test chip 2 The electrode single-molecule test chip is bent to drive the opposite tip structure to be broken by tensile force on two sides so as to form a nano gap;
and controlling the reciprocating motion of the stepping motor, and controlling the tip aligning structure to realize precise change of the size of the nano gap and the cracking process.
Accordingly, the present invention provides the following effects and/or advantages:
WTE is selected for use in the application 2 As the electrode material, WTE is advantageous 2 Is a typical layered TMDs material possessing a number of properties such as unsaturated magnetoresistive properties, ferroelectricity, topology, superconductivity, exor semi-metals, and the like. WTE in natural state 2 Is 1T' phase, is semi-metal, has high conductivity and is suitable for being used as electrode material of a molecular junction. In addition, 1T' -WTE 2 The surface of the material is provided with a suspension bond, so that an interface chemical bond is not introduced, and the contact resistance can be reduced; on the other hand 1T' -WTE 2 Can be connected with molecules through weak van der Waals interactions, so that the electrode-molecule interface is moderately coupled. Thus, 1T' -WTE is selected for use in the present application 2 Is very suitable for being used as an electrode material to construct a molecular junction.
The existing CVD method is to react the precursor with gasified tellurium at high temperature to generate gaseous tungsten telluride and deposit the gaseous tungsten telluride on the surface of a substrate to prepare the tungsten telluride, and the method cannot obtain a tungsten telluride film with a specific shape. The preparation method well solves the difficulty that patterning cannot be performed, and the patterned tungsten film can be obtained through photoetching and magnetron sputtering coating processes, and can be oxidized and in-situ telluride to obtain the tungsten telluride film with the required electrode pair shape.
The application realizes 1T' -WTE for the first time 2 And (3) preparing an electrode single-molecule test chip. The 1T' -WTE can be conveniently and rapidly prepared through two-step reaction of autonomous design 2 And the method can be combined with micro-nano processing technology to realize the preparation of chips. 1T' -WTE 2 The electrode single-molecule chip is connected with the molecules through van der Waals interaction, so that the molecules form weak coupling with the electrodes, and therefore quenching effect is not caused to inhibit the expression of the intrinsic property of the molecules. In addition, 1T' -WTE compared with other metal electrode materials 2 The material has a smaller work function, and is expected to reduce contact resistance so as to improve charge transport of a molecular junction.
The molecules studied in molecular electronics are typically below 5nm, while the nanogap in the center of the chip can be precisely sized to match the length of a single organic molecule to be tested.
It is to be understood that both the foregoing general description and the following detailed description of the present invention are exemplary and explanatory and are intended to provide further explanation of the invention as claimed.
Drawings
FIG. 1 is a flow chart of one embodiment of the present invention.
Fig. 2 is a schematic diagram of the result obtained in step S2 according to one embodiment of the present invention.
Fig. 3 is a schematic diagram of the result obtained in step S3 according to one embodiment of the present invention.
Fig. 4 is a schematic diagram of the result obtained in step S4 according to one embodiment of the present invention.
Fig. 5 is a schematic diagram of the result obtained in step S5 according to one embodiment of the present invention.
Fig. 6 is a schematic view of a reaction apparatus for a process of telluride tungsten oxide in step S6 according to one embodiment of the present invention.
Fig. 7 is a schematic diagram of the result obtained in step S6 according to one embodiment of the present invention.
FIG. 8 is a photograph of the chip obtained in the step S6, wherein (a) the chip is a photograph of the chip after thermal oxidation; (b) chip physical diagram after telluride reaction.
FIG. 9 is a diagram of 1T' -WTE generated in step S7 2 Schematic of the electrode.
FIG. 10 is a photograph of the real object obtained in steps S9-S10, wherein, (a) SEM represents a schematic view of the tip structure after FIB processing; (b) SEM (scanning electron microscope) characterization of suspended 1T' -WTE (wireless transmit-receive unit) after wet etching 2 Electrode pairs are schematically shown.
FIG. 11 shows a step S8 of one embodiment of the present invention to obtain electrode patterned 1T' -WTE 2 Schematic of electrode single molecule chip.
FIG. 12 is a graph of experimental data for one embodiment of the present invention, wherein (a) the sample has a Raman spectrum and (b) the sample has an electron diffraction pattern.
FIG. 13 shows a WTE provided by the present invention 2 The structure of the electrode single-molecule test chip is schematically shown.
FIG. 14 shows a WTE provided by the present invention 2 Schematic diagram of the use state of the electrode single-molecule test chip.
Detailed Description
For the convenience of understanding by those skilled in the art, the structure of the present invention will now be described in further detail with reference to the accompanying drawings:
referring to FIG. 1, a WTE 2 The preparation method of the electrode single-molecule test chip comprises the following steps:
s1, taking a molybdenum sheet with double-sided polishing as a substrate, and drying after ultrasonic cleaning;
in the step, a double-sided polished molybdenum sheet with the diameter of 4inch is adopted as a substrate, and is dried in an oven for 2 hours after ultrasonic cleaning by using acetone and ethanol. Wherein the area of the 4inch double-sided polished molybdenum sheet is larger, so that a plurality of WTE can be prepared on the 4inch double-sided polished molybdenum sheet at one time through the subsequent steps 2 The electrodes are cut to obtain a plurality of WTE simultaneously 2 And an electrode single molecule test chip. And, each WTE 2 The electrode single molecule test chip may contain one or more WTE 2 An electrode. And are not limited herein.
In the embodiment, the molybdenum sheet is used as a substrate for the first time in the field, and the chemical property of molybdenum is relatively stable. The chemical nature of molybdenum in air or water is stable at normal or not too high a temperature.
S2, growing a silicon oxide layer on the upper surface of the molybdenum sheet through plasma enhanced chemical vapor deposition;
in this step, the method of Plasma Enhanced Chemical Vapor Deposition (PECVD) is a direct application of the prior art. Further, siH 4 And O 2 And (3) performing plasma enhanced chemical vapor deposition to grow a silicon oxide layer as a reaction gas, and/or wherein the thickness of the silicon oxide layer is 1-3um. The thickness of the silicon oxide layer is 1-3um, which can provide enough thickness space when wet etching is carried out in the subsequent steps, and provide corresponding structural foundation in the subsequent using methodThe motor is convenient for the precise change of the size of the reciprocating motion regulation gap. In addition, the silicon oxide layer also plays an insulating role as an insulating layer. Because the molybdenum substrate is metallic and can conduct electricity, if not insulated by silicon oxide, the substrate is insulated from WTE 2 The electrodes will short. Resulting in a substrate for growing a silicon oxide layer as shown in fig. 2.
S3, spin-coating photoresist on the upper surface of the silicon oxide layer and drying;
in the step, the steps of spin coating photoresist and drying are the prior art. The baking process volatilizes the organic solvent in the photoresist film layer. A substrate coated with a photoresist film layer as shown in fig. 3 was obtained.
S4, carrying out mask photoetching and developing on the photoresist, so as to develop an electrode pattern corresponding to a mask template on the photoresist, wherein the mask template comprises conductive external circuit area templates which are arranged in a bilateral symmetry manner and a wire template connected between the conductive external circuit areas;
before this step, a mask template may be prepared in advance, where the mask template includes a conductive external circuit region template that is arranged symmetrically left and right, and a wire template that is connected between the conductive external circuit regions. The electrode pattern corresponding to the mask template can be generated in the subsequent preparation process through the mask template.
Mask lithography and development of the photoresist are also straightforward in the prior art. This step results in a photoresist film layer with exposed electrode patterns as shown in fig. 4.
S5, performing magnetron sputtering on the electrode pattern to metal tungsten, enabling the metal tungsten to cover the electrode pattern to form a metal tungsten film, and washing off photoresist to obtain a metal tungsten electrode corresponding to the electrode pattern;
this step is the core improvement step of the present application. The metal tungsten is plated through magnetron sputtering, so that the patterning technical effect of the metal dock is realized. Then the substrate was put in an acetone solution and swelled and peeled off (Lift-off), and then a metal tungsten electrode corresponding to the electrode pattern shown in FIG. 5 was obtained. If a large-sized substrate is used in step S1, a molybdenum sheet may be diced using a laser dicing saw according to dicing marks in this step to obtain a plurality of small unit chips of 10mm by 30 mm.
S6, performing high-temperature thermal oxidation on the metal tungsten electrode to generate electrode-patterned tungsten oxide, adding tellurium powder, and performing high Wen Dihua on the electrode-patterned tungsten oxide under the action of carrier gas and reducing gas to generate electrode-patterned 1T' -WTE 2 ；
This step is the core improvement step of the present application. The step adopts a two-step method to generate 1T' -WTE 2 The 1T' -WTE is realized by taking metal tungsten and tellurium powder as raw materials and adopting a two-step method 2 Is prepared by the following steps. Compared with the traditional method, the method designed by the embodiment can conveniently and quickly realize the 1T' -WTE of the specific pattern 2 Is convenient for realizing WTE by combining with micro-nano processing technology 2 And (3) preparing an electrode single-molecule chip.
The two-step process is as follows:
the first step is a thermal oxidation process of tungsten, and the step is to put a tungsten film obtained by magnetron sputtering into a high-temperature atmosphere of a tube furnace to cause the tungsten film to undergo oxidation reaction to generate tungsten oxide.
The second step is the process of telluride of tungsten oxide, the device is shown in figure 6, tellurium powder and tungsten oxide obtained in the first step are respectively arranged at the left end and the right end of a porcelain boat, the porcelain boat is arranged in a quartz tube and is aligned with the central heat source area of a tube furnace, and then the telluride reaction is carried out at high temperature and in the atmosphere of carrier gas and reducing gas to generate 1T' -WTE 2 . Tellurium powder sublimates at high temperature, the gas in the atmosphere is used as carrier gas, gasified tellurium is carried to the surface of the chip at a certain flow rate, and the reduction gas participates in the reduction reaction to react to generate tungsten telluride to generate 1T' -WTE 2 As shown in fig. 7. The physical photograph produced by the two-step method is shown in figure 8.
By this two-step process, this step produces electrode patterned 1T' -WTE 2 Realize 1T' -WTE 2 The preparation of the electrode can conveniently and rapidly prepare the 1T' -WTE through two-step reaction of autonomous design 2 And the method can be combined with micro-nano processing technology to realize the preparation of chips. The method can directly oxidize tungsten into tungsten oxideThe bit telluride generates tungsten telluride, and single crystal 1T' -WTE can be obtained 2 . Tungsten telluride can be generated in situ, so that the tungsten film can be patterned in advance, and finally the tungsten telluride with a specific shape is obtained.
S7, patterning the electrode by using FIB to form 1T' -WTE 2 Cutting the middle position of the wire template to form a sharp structure to obtain 1T' -WTE 2 An electrode;
the step utilizes FIB pairs to generate 1T' -WTE 2 Cutting the small cell chip to obtain a bowtie structure, wherein the bowtie structure is also a pair-tip structure. The opposite tips of the opposite tip structure are in a connected state to obtain 1T' -WTE as shown in FIG. 9 2 An electrode. Fig. 10 (a) is a photograph of the real object obtained in this step.
S8, suspending the opposite-tip structure by wet etching the silicon oxide layer near the opposite-tip structure to obtain the electrode patterned 1T' -WTE 2 An electrode single molecule chip.
Finally, wet etching is carried out by hydrofluoric acid to obtain 1T' -WTE with suspended central area 2 An electrode single molecule chip is shown in FIG. 11. Fig. 10 (b) is a photograph of the real object obtained in this step.
Further, positive photoresist is adopted as the photoresist;
in this embodiment, AZ5214E positive photoresist is selected, and post-baking inversion can be performed according to the characteristics of AZ5214E photoresist, where the photoresist is positive photoresist.
Specifically, the mask photoetching and developing of the photoresist comprises the following steps:
performing first ultraviolet exposure on the positive photoresist according to the mask template, and performing photolysis reaction to generate carboxylic acid;
the carboxylic acid promotes the resin of the first ultraviolet exposure area in the positive photoresist to generate a crosslinking reaction at high temperature, so that the ultraviolet exposure area in the positive photoresist is insoluble in an alkaline developer;
and taking down the mask template to carry out second ultraviolet exposure, generating carboxylic acid in the area which is not subjected to the first ultraviolet exposure, and dissolving the carboxylic acid in an alkaline developer after developing to obtain the pattern identical to the mask template.
The AZ5214 photoresist mainly comprises 3 parts of photosensitive components, resin and solvent.
When the mask is exposed, the photosensitive component of the exposed area is converted into carboxylic acid, and the carboxylic acid after being baked again promotes the resin of the exposed area to generate a crosslinking reaction, so that the exposed area is insoluble in an alkaline developing solution, the step is also called glue inversion baking, then the mask is subjected to one-step flood exposure, namely maskless exposure, the carboxylic acid is generated in the area which is not exposed for the first time, and the carboxylic acid is dissolved in the alkaline developing solution after being developed to obtain the pattern which is the same as the mask.
The photoetching is carried out by two ultraviolet exposures, so that the inverted trapezoid glue appearance can be obtained, and the stripping of the rear magnetron sputtering tungsten plating film is facilitated. The atomic kinetic energy sputtered by the magnetron sputtering coating is high, so that the coating and the substrate have good adhesion, and the required electrode pattern can be well stripped by the inverted trapezoid adhesive morphology.
Further, the step of performing high-temperature thermal oxidation on the metal tungsten electrode to generate electrode-patterned tungsten oxide comprises the following steps:
placing the metal tungsten electrode in a tube furnace, and performing high-temperature thermal oxidation at 600-660 ℃.
Further, tellurium powder is added, and under the action of carrier gas and reducing gas, the electrode-patterned tungsten oxide is subjected to high Wen Dihua to generate electrode-patterned 1T' -WTE 2 Comprising the following steps:
sequentially placing tellurium powder and molybdenum sheets of tungsten oxide with the electrode patterns in the tube furnace according to a gas flow path;
heating to 600-660 ℃ by a tube furnace to sublimate tellurium powder, driving tellurium to contact with the electrode-patterned tungsten oxide by the carrier gas, and generating electrode-patterned 1T' -WTE by the reduction reaction of the reduction gas 2 。
Further, the carrier gas is Ar, and the reducing gas is H 2 Ar and H 2 Is 95:5 by volume.
Further, the tellurium powder is tellurium powder with a molecular sieve.
In the step, tellurium powder with molecular sieve is selected because the molecular sieve can slow down release of tellurium after sublimation, thereby controlling and obtaining the required reaction speed.
Further, electrode patterned 1T' -WTE is generated 2 Thereafter, execution is performed:
obtaining the electrode patterned 1T' -WTE 2 Determining the product as 1T' -WTE based on the Raman spectrum of the polymer and/or the electron diffraction pattern of the electrode patterning 2 。
As shown in FIG. 12, the characteristic peaks are located at 87cm, respectively, from the Raman spectrum of the sample -1 、117cm -1 、130cm -1 、160cm -1 、208cm -1 Compared with the prior art 1T' -WTE 2 Corresponds exactly to the raman spectrum of (c). The verification method of the electrode-patterned electron diffraction pattern is similar. The reaction product was determined to be 1T' -WTE by this step 2 。
WTE (wire train engine) 2 Electrode single molecule test chip can be realized by the WTE 2 The electrode single molecule test chip is prepared by a method, referring to fig. 13, comprising:
a substrate 1, wherein a silicon oxide layer 2 grows on the upper surface of the substrate 1, and a groove 4 is etched in the middle area of the silicon oxide layer 2 by a wet method;
1T'-WTe 2 the electrode 3 comprises two conductive external circuit areas, a wire and a pair tip structure 301, wherein the number of the conductive external circuit areas is two, the two conductive external circuit areas are respectively arranged on the silicon oxide layer 2 left and right, two ends of the wire respectively start from the conductive external circuit areas and extend to the middle area of the silicon oxide layer 2, the pair tip structure 301 is arranged at the middle position of the wire, and the pair tip structure 301 is suspended in the middle area of the silicon oxide layer 2.
Further, the WTE 2 The application method of the electrode single-molecule test chip comprises the following steps:
referring to fig. 14, the WTe is fixed 2 The left end and the right end of the electrode single-molecule test chip;
from the WTe by means of a stepper motor 5 2 Electrode single molecule measurementJacking the WTE right below the middle area of the test chip 2 The electrode single-molecule test chip is bent to drive the opposite tip structure to be broken by tensile force on two sides so as to form a nano gap;
and controlling the reciprocating motion of the stepping motor 5, and controlling the tip aligning structure to realize precise change of the size of the nano gap and the cracking process.
In this embodiment, WTE is selected 2 Single molecule materials with the advantage of WTE 2 Is a typical layered TMDs material possessing a number of properties such as unsaturated magnetoresistive properties, ferroelectricity, topology, superconductivity, exor semi-metals, and the like. WTE in natural state 2 Is 1T' phase, is semi-metal, has high conductivity and is suitable for being used as electrode material of a molecular junction. In addition, 1T' -WTE 2 The surface of the material is provided with a suspension bond, so that an interface chemical bond is not introduced, and the contact resistance can be reduced; on the other hand 1T' -WTE 2 Can be connected with molecules through weak van der Waals interactions, so that the electrode-molecule interface is moderately coupled. Thus, 1T' -WTE is selected for use in the present application 2 Can be used as electrode material to construct molecular junction.
The existing CVD method is to react the precursor with gasified tellurium at high temperature to generate gaseous tungsten telluride and deposit the gaseous tungsten telluride on the surface of a substrate to prepare the tungsten telluride, and the method cannot obtain a tungsten telluride film with a specific shape. The preparation method well solves the difficulty that patterning cannot be performed, and the patterned tungsten film can be obtained through photoetching and magnetron sputtering coating processes, and can be oxidized and in-situ telluride to obtain the tungsten telluride film with the required electrode pair shape.
It should be noted that in the claims, any reference signs placed between parentheses shall not be construed as limiting the claim. The word "comprising" does not exclude the presence of elements or steps not listed in a claim. The word "a" or "an" preceding an element does not exclude the presence of a plurality of such elements. The invention may be implemented by means of hardware comprising several distinct elements, and by means of a suitably programmed computer. In the unit claims enumerating several means, several of these means may be embodied by one and the same item of hardware. The use of the words first, second, third, etc. do not denote any order. These words may be interpreted as names.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
In the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communicated with the inside of two elements or the interaction relationship of the two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms should not be understood as necessarily being directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.

Claims (10)

1. WTE (wire train engine) 2 The preparation method of the electrode single-molecule test chip is characterized by comprising the following steps of: the method comprises the following steps:
taking a molybdenum sheet with polished double surfaces as a substrate, ultrasonically cleaning and drying;
growing a silicon oxide layer on the upper surface of the molybdenum sheet through plasma enhanced chemical vapor deposition;
spin-coating photoresist on the upper surface of the silicon oxide layer and drying;
carrying out mask photoetching and developing on the photoresist, so as to develop an electrode pattern corresponding to a mask template on the photoresist, wherein the mask template comprises conductive external circuit area templates which are arranged in a bilateral symmetry manner and lead templates connected between the conductive external circuit areas;
performing magnetron sputtering on the electrode pattern to metal tungsten, enabling the metal tungsten to cover the electrode pattern to form a metal tungsten film, and washing off photoresist to obtain a metal tungsten electrode corresponding to the electrode pattern;
performing high-temperature thermal oxidation on the metal tungsten electrode to generate electrode-patterned tungsten oxide, adding tellurium powder, and performing high Wen Dihua on the electrode-patterned tungsten oxide under the action of carrier gas and reducing gas to generate electrode-patterned 1T' -WTE 2 ；
Patterning of the electrode with FIB 1T' -WTe 2 Cutting the middle position of the wire template to form a sharp structure to obtain 1T' -WTE 2 An electrode;
suspending the opposite tip structure by wet etching the silicon oxide layer near the opposite tip structure to obtain electrode patterned 1T' -WTE 2 An electrode single molecule chip.
2. A WTe according to claim 1 2 The preparation method of the electrode single-molecule test chip is characterized by comprising the following steps of: siH (SiH) 4 And O 2 And (3) performing plasma enhanced chemical vapor deposition to grow a silicon oxide layer as a reaction gas, and/or wherein the thickness of the silicon oxide layer is 1-3um.
3. A WTe according to claim 1 2 The preparation method of the electrode single-molecule test chip is characterized by comprising the following steps of: the saidThe photoresist is positive photoresist;
the mask photoetching and developing of the photoresist comprises the following steps:
performing first ultraviolet exposure on the positive photoresist according to the mask template, and performing photolysis reaction to generate carboxylic acid;
the carboxylic acid promotes the resin of the first ultraviolet exposure area in the positive photoresist to generate a crosslinking reaction at high temperature, so that the ultraviolet exposure area in the positive photoresist is insoluble in an alkaline developer;
and taking down the mask template to carry out second ultraviolet exposure, generating carboxylic acid in the area which is not subjected to the first ultraviolet exposure, and dissolving the carboxylic acid in an alkaline developer after developing to obtain the pattern identical to the mask template.
4. A WTe according to claim 1 2 The preparation method of the electrode single-molecule test chip is characterized by comprising the following steps of: the tungsten oxide patterned by high-temperature thermal oxidation of the metal tungsten electrode comprises the following components:
placing the metal tungsten electrode in a tube furnace, and performing high-temperature thermal oxidation at 600-660 ℃.
5. A WTe according to claim 4 2 The preparation method of the electrode single-molecule test chip is characterized by comprising the following steps of: adding tellurium powder, and carrying out high Wen Dihua on the electrode-patterned tungsten oxide under the action of carrier gas and reducing gas to generate electrode-patterned 1T' -WTE 2 Comprising the following steps:
sequentially placing tellurium powder and molybdenum sheets of tungsten oxide with the electrode patterns in the tube furnace according to a gas flow path;
heating to 600-660 ℃ by a tube furnace to sublimate tellurium powder, driving tellurium to contact with the electrode-patterned tungsten oxide by the carrier gas, and generating electrode-patterned 1T' -WTE by the reduction reaction of the reduction gas 2 。
6. A WTe according to claim 1 or 5 2 Electrode single molecule testingThe preparation method of the chip is characterized in that: the carrier gas is Ar, and the reducing gas is H 2 Ar and H 2 Is 95:5 by volume.
7. A WTe according to claim 1 or 5 2 The preparation method of the electrode single-molecule test chip is characterized by comprising the following steps of: the tellurium powder is tellurium powder with molecular sieve.
8. A WTe according to claim 1 2 The preparation method of the electrode single-molecule test chip is characterized by comprising the following steps of: generating electrode patterned 1T' -WTE 2 Thereafter, execution is performed:
obtaining the electrode patterned 1T' -WTE 2 Determining the product as 1T' -WTE based on the Raman spectrum of the polymer and/or the electron diffraction pattern of the electrode patterning 2 。
9. WTE (wire train engine) 2 The electrode single molecule test chip is characterized in that: comprising the following steps:
the upper surface of the substrate is provided with a silicon oxide layer, and the middle area of the silicon oxide layer is corroded by a wet method to form a groove;
1T'-WTe 2 the electrode comprises two conductive external circuit areas, a wire and a pair tip structure, wherein the number of the conductive external circuit areas is two, the two conductive external circuit areas are respectively arranged on the silicon oxide layer in a left-right mode, two ends of the wire respectively start from the conductive external circuit areas and extend to the middle area of the silicon oxide layer, the pair tip structure is arranged at the middle position of the wire, and the pair tip structure is suspended in the middle area of the silicon oxide layer.
10. A WTe according to claim 9 2 The electrode single molecule test chip is characterized in that: the WTE (WTE) 2 The application method of the electrode single-molecule test chip comprises the following steps:
fixing the WTE 2 The left end and the right end of the electrode single-molecule test chip;
from the WTE by a stepper motor 2 The WTE is propped up right below the middle area of the electrode single-molecule test chip 2 The electrode single-molecule test chip is bent to drive the opposite tip structure to be broken by tensile force on two sides so as to form a nano gap;
and controlling the reciprocating motion of the stepping motor, and controlling the tip aligning structure to realize precise change of the size of the nano gap and the cracking process.
CN202310107993.1A 2023-03-27 2023-03-27 WTE (wire train engine) 2 Electrode single-molecule test chip and preparation method thereof Pending CN116124838A (en)

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