CN114724956A - Chemical vapor deposition preparation method of monolayer molybdenum disulfide and application of monolayer molybdenum disulfide in thin film transistor - Google Patents
Chemical vapor deposition preparation method of monolayer molybdenum disulfide and application of monolayer molybdenum disulfide in thin film transistor Download PDFInfo
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- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 83
- 239000002356 single layer Substances 0.000 title claims abstract description 50
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000010409 thin film Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000005229 chemical vapour deposition Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 38
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 29
- 239000000758 substrate Substances 0.000 claims abstract description 28
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 15
- 239000004065 semiconductor Substances 0.000 claims abstract description 8
- 238000012546 transfer Methods 0.000 claims abstract description 8
- 239000000376 reactant Substances 0.000 claims abstract description 5
- 229910052961 molybdenite Inorganic materials 0.000 claims description 39
- 239000010410 layer Substances 0.000 claims description 27
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- 238000007705 chemical test Methods 0.000 abstract 1
- 239000011593 sulfur Substances 0.000 abstract 1
- 229910052717 sulfur Inorganic materials 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 12
- 239000010453 quartz Substances 0.000 description 12
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- 230000007547 defect Effects 0.000 description 3
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- 125000004434 sulfur atom Chemical group 0.000 description 3
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- MZRVEZGGRBJDDB-UHFFFAOYSA-N N-Butyllithium Chemical compound [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
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- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
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- H01L21/02518—Deposited layers
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- H01L21/02568—Chalcogenide semiconducting materials not being oxides, e.g. ternary compounds
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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
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Abstract
The invention discloses a chemical vapor deposition preparation method of monolayer molybdenum disulfide and application thereof in a thin film transistor; according to the invention, molybdenum trioxide and sulfur are used as reactants, sodium hydroxide is added into molybdenum trioxide, and single-layer MoS with better quality is obtained through growth2The crystal domain is larger than 100 mu m, is not limited to one or more substrate materials, can stably grow on various single crystal and polycrystalline substrate materials, and the single-layer MoS prepared by the method2Applied to thin film field effect transistor and electrically connecting the thin film transistorPerforming chemical test to obtain transfer characteristic curve, and calculating mobility to 121cm2V‑1s‑1Prove that the single-layer MoS prepared by the method2The application requirements of the semiconductor device are met.
Description
Technical Field
The invention belongs to the technical field of two-dimensional nano material preparation, and particularly relates to a chemical vapor deposition preparation method of single-layer molybdenum disulfide and application of the single-layer molybdenum disulfide in a thin film transistor.
Background
Two-dimensional materials, which means that the material is far smaller than the other two dimensions in a certain dimension, electrons can move freely only in the other two dimensions to generate current, the discovery of the graphene in 2004 breaks through the idea that most people think that the two-dimensional materials cannot exist, the transition metal chalcogenide is a two-dimensional material with very rich and peculiar properties, and among the transition metal chalcogenide, Molybdenum Disulfide (MoS) is used2) MoS is a widely-focused product because it can be obtained directly from a large number of natural minerals in the nature, and its preparation cost is low2The graphene-like multilayer structure has a graphene-like layered structure, atoms in layers are closely connected in a S-Mo-S form by virtue of covalent bonds, and the layers are combined by mainly relying on Van der Waals force. More importantly, unlike zero band gap graphene, single-layer MoS2Has a direct band gap of about 1.9eV, so that it can be well embodied in a semiconductor device, and a high-performance thin film transistor and a photoelectric device can be manufactured. 2011 Kis et al first used mechanically stripped single layer MoS2The thin film field effect transistor with excellent electrical property and the carrier mobility of 15cm is prepared2V-1s-1(in a field effect transistor, mobility is an extremely important parameter, and the higher the mobility is, the faster the device operates, and the faster the operation speed of a circuit in which the device is located). In addition, according to the moore's law, each about 18-24 months, the size of the transistor is shortened to 0.7 times of the original size, and the current semiconductor industry is continuously advancing to smaller sizes, so that the chip manufacturing difficulty is high, the cost is high, and meanwhile, a plurality of new effects are brought, such as a short channel effect, a quantum tunneling effect and a single-layer MoS2Having a larger bandgap, ultra-thin dimensions, lower dielectric constant and larger electron effective mass, these problems are well overcome. Overall, single layer MoS2Is a powerful competitor of semiconductor materials in the post-silicon era and has important research value and application prospect in the fields of micro-nano electronics, flexible electronics, photoelectric detection, molecular detection and the like.
Preparation of Single-layer MoS2The methods of (a) are numerous and common methods such as a mechanical stripping method, a lithium ion intercalation method, a liquid phase ultrasonic stripping method, a magnetron sputtering method, a thermal decomposition method, a metal organic compound vapor deposition method, and a Chemical Vapor Deposition (CVD). Among them, the mechanical exfoliation method is simple and easy, but the yield is low, and the obtained single-layer MoS2Small size, poor repeatability, spontaneous combustion of n-butyl lithium used in lithium ion intercalation in air, high risk, and the biggest disadvantage of liquid phase ultrasonic stripping is separated MoS2Non-uniform thickness, single layer MoS2Low-yield MoS preparation by thermal decomposition method2More impurities are brought in the process, the gas precursor used by the metal organic compound vapor deposition method has high price and strong toxicity, and CVD is the most extensive monolayer MoS at present2The preparation method has the advantages of simple preparation method, low raw material price, high yield, stable process and low toxicity.
However, single layer MoS2The CVD growth of (i) is still subject to limitations, such as the growth of single-layer MoS2High defect density, single layer MoS2Small crystal domain and multi-layer MoS2Structures, all as a result of non-uniform aggregation and diffusion of Mo and S atoms on the substrate, nucleation sites of crystallites tend to be preferentially selected at impurities or defects on the substrate surface, so a single layer of MoS2The growth quality of the substrate has a great relationship with the state of the substrate surface, so that a relatively independent CVD growth mode which is less influenced by the state of the substrate surface needs to be found to obtain high-quality single-layer MoS2。
Disclosure of Invention
Single layer MoS growth for existing CVD2The invention provides a novel single-layer MoS2CVD growth preparation method ofMethod, single layer MoS grown by the method2The single-layer MoS prepared by the method has better quality, smaller density of S vacancies and defects, larger crystal domain (larger than 100 mu m), no limitation to one or more substrate materials, and stable growth on various single crystal and polycrystalline substrate materials2The method is applied to the thin film transistor, and the thin film transistor is electrically tested to obtain a transfer characteristic curve and calculate the mobility.
The purpose of the invention is realized by the following technical scheme: in one aspect, the present invention provides a chemical vapor deposition method for preparing monolayer molybdenum disulfide, comprising the following steps:
s1, substrate preparation: preparation of substrate Material with clean surface for MoS preparation2；
More preferably, the single-layer MoS prepared using S2 is used directly if desired2Preparing a thin film transistor, and selecting a conductive substrate with an insulating layer;
s2 single-layer MoS2Growing: with MoO3The powder and the S simple substance powder are used as reactants, and the MoS is prepared by adopting a CVD method2The reaction equation is as follows:
2MoO3+7S＝2MoS2+3SO2 (1)
in MoO3NaOH powder is added into the powder, NaOH can be ionized in the growth process, and-OH obtained by ionization can be in MoS2The S-Mo-S-OH double-layer structure is formed in the growth process, so that the MoS is formed2The surface forms a layer of-OH which is saturated and does not tend to bind new atoms, so that Mo and S atoms which reach the substrate later do not exist in MoS2The surface continues to stack, and is more prone to bond with Mo and S atoms on both sides, so that MoS2The growth of the silicon nitride is easier to be a large-area single-layer structure rather than a multi-layer structure;
more preferably, a single layer of MoS is grown2The adopted CVD is a low-pressure CVD mode;
more preferably, a single layer of MoS is grown2The temperature of the reaction kettle is 700-820 ℃;
more preferably, a single layer of Mo is grownS2The atmosphere of (a) is 100% argon or argon containing 5% hydrogen;
on the other hand, the invention provides an application of single-layer molybdenum disulfide in a thin film transistor based on preparation, and the MoS prepared by adopting a positive photoresist stripping process in a microelectronic process2Preparing a source electrode structure and a drain electrode structure; MoS2And (3) electrical testing of the thin film transistor: semiconductor analyzer for prepared MoS2The thin film transistor is electrically tested, mainly testing the modulation of a gate electrode to a source electrode and a drain electrode and a transfer characteristic curve, calculating the mobility according to the transfer characteristic curve, and calculating the mobility according to a formula shown in a formula (2);
wherein, IdsAnd VdsRespectively representing source and drain currents and voltages, VbgFor the gate voltage, L and W correspond to the channel length and width, CiIs the capacitance per unit area of the insulating layer.
More preferably, the electrodes of the source and drain electrodes have a double-layer structure, a Cr thin film as a contact layer and an adhesion layer, and an Au thin film as a conductive layer.
The invention has the beneficial effects that:
the invention utilizes CVD to grow single-layer MoS2By MoO in the reactants3Adding NaOH powder into the powder, and utilizing-OH ionized by NaOH in the growth process to ensure that MoS2The method is easier to grow into a large-area single-layer structure instead of a multi-layer structure, is not influenced by the substrate material and the state, and can prepare the single-layer MoS2The method is applied to a thin film field effect transistor, the electrical characteristics of the thin film field effect transistor are tested, and the single-layer MoS prepared by the method is proved through the obtained modulation and transfer characteristic curve of the gate electrode to the source and drain2The application requirements of the semiconductor device are met.
Drawings
FIG. 1 is a single layer MoS prepared according to the present invention2A Scanning Electron Microscope (SEM) photograph of (a).
FIG. 2 is a single layer MoS prepared in accordance with the present invention2The results of the raman spectroscopy test.
FIG. 3 shows MoS prepared according to the present invention2Metallographic microscope pictures of samples of thin film transistor examples.
FIG. 4 shows MoS when the gate voltage is set to-10V to-40V according to the present invention2Source drain IV curves for samples of thin film transistor embodiments.
FIG. 5 shows the source-drain voltage (V) of the present inventionds) MoS set to-0.05V2Transfer characteristics of samples of thin film transistor embodiments.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood, however, that the description herein of specific embodiments is only intended to illustrate the invention and not to limit the scope of the invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.
The invention provides a chemical vapor deposition preparation method of monolayer molybdenum disulfide and application of the monolayer molybdenum disulfide in a thin film transistor, which comprises the following steps:
s1, substrate preparation: selecting a single-side polished silicon oxide wafer as MoS2The thickness of the silicon wafer is 0.5mm, and the surface of the polished surface is 300nm SiO2The oxide layer and the non-polished surface have no oxide layer, the silicon substrate adopts p-type heavy doping, and MoS grown by adopting a CVD method2The deposition position on the substrate has uncertainty, and subsequent laser direct-write overlay MoS2Alignment mark positioning is needed when the source electrode and the drain electrode of the thin film transistor are positioned, so that an alignment mark pattern is prepared on the surface of a substrate by adopting a positive photoresist stripping process in a microelectronic process, the alignment mark adopts a double-layer thin film structure, Ti 20nm is used as an adhesion layer, then a 60nm Au thin film is deposited on the surface of the Ti thin film, and the alignment mark does not influence MoS2And can tolerate MoS2The growth temperature of (a);
s2, preparation of reactants: weighing MoO30.05g of powder and 0.5g of elemental S powder are respectively filled in two quartz boats, the width of each quartz boat is about 1.5cm, the length of each quartz boat is about 10cm, 0.015g of NaOH powder is weighed and placed in a container filled with MoO3In the quartz boat, the substrate material was cut into a size of about 2cm in width and about 2cm in length, the substrate was turned over so that the side having the oxide layer faced downward, and the substrate was placed in a chamber filled with MoO3Powder and NaOH powder on a quartz boat;
s3, placing precursors: moving the quartz tube to a proper position, loosening the sealing ring at the air inlet end of the quartz tube, dismounting the plug, and filling MoO3The porcelain boat containing the powder, the NaOH powder and the substrate is placed into a heating area at the middle position of the heating furnace from the air inlet end, and then the porcelain boat containing the S elemental powder is placed into the heating area at intervals containing MoO3The positions of the powder, NaOH powder and the ceramic boat of the substrate are 30 cm;
s4, preparing reaction atmosphere: installing a plug and a sealing ring of an air inlet port, introducing 500sccm of argon gas containing 5% of hydrogen after confirming the air tightness of a growth system, opening a mechanical pump connected to the air outlet port and an air outlet port valve to perform air suction for about 20 minutes to remove air in a quartz tube, reducing the flow of the hydrogen gas and the argon gas to 20sccm before starting heating and raising the temperature, adjusting the size of the valve of the air outlet port to ensure that the air pressure in the quartz tube reaches 50mbar, and stabilizing for about 20 minutes;
s5, heating: setting the temperature to rise from room temperature to 750 ℃ at a constant speed for 20 minutes, and MoO3Has a melting point of 795 ℃, but at a temperature below the melting point, MoO3Has remarkable sublimation phenomenon and generates MoO3Steam, wherein the boiling point of the S simple substance is only 444 ℃, the S simple substance is firstly melted in the temperature rising process, and then S steam is formed;
S6、MoS2and (3) growing the material: upon reaching the set temperature, MoO3Both steam and S steam have formed, now into MoS2The constant temperature duration time is the growth time, and the growth time is 15 minutes;
s7, cooling, sampling and cleaning: stopping heating after finishing growth, moving the quartz tube to the outside of the furnace along the guide rail to naturally cool the quartz tube, increasing the flow of argon to 200sccm, and finishing the quartz boatAfter the mixture is fully cooled to room temperature, sampling is carried out, argon is turned off, a mechanical pump is turned off, a sealing ring and a plug at the gas inlet end are disassembled, the substrate is taken out, and the prepared single-layer MoS is shown in figure 12The side length of the triangular crystal domain is larger than 100 μm according to the measurement result of the crystal domain, and MoS can be observed according to the measurement of the thickness by an Atomic Force Microscope (AFM)2Is 0.689nm, and the prepared MoS was confirmed2Is a single-layer structure, FIG. 2 is a single-layer MoS prepared2The Raman spectrum of (1) shows that E is1 2gAnd A1gCharacteristic peaks are respectively 383cm-1And 403cm-1Completely conforms to single-layer MoS2The vibration mode of (1);
S8、MoS2preparing a thin film transistor device: prepared MoS by adopting metallographic microscope2Image acquisition was performed using Klayout software at the selected MoS based on the acquired images2Designing and drawing source and drain electrode pattern, MoS2The width of the channel is designed to be 3 mu m, the source electrode and the drain electrode are subjected to alignment by adopting a positive photoresist stripping process in a microelectronic process, wherein an alignment mark made by S1 is used when an alignment pattern is directly written by laser, a double-layer electrode structure is prepared by magnetron sputtering, Cr 20nm is a contact layer and an adhesion layer, Au 60nm is a conductive layer, and FIG. 3 is the prepared MoS2A metallographic microscope photograph of the thin film transistor;
S9、MoS2electrical testing of the thin film transistor device: MoS using Agilent B1500A semiconductor device Analyzer2The thin film transistor was electrically tested, and FIG. 4 shows MoS when the gate voltage was set to-10V to-40V2The source-drain IV curve of the sample of the thin film transistor embodiment, i.e. the modulation curve of the gate electrode to the source-drain, can be observed from the figure that the gate voltage has an obvious modulation effect on the source-drain, and fig. 5 is the source-drain voltage (V)ds) MoS set to-0.05V2The transfer characteristic curve of the transistor was calculated by the formula (2) to obtain a mobility of 121cm2V-1s-1。
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (4)
1. A chemical vapor deposition preparation method of monolayer molybdenum disulfide is characterized by comprising the following steps:
s1, substrate preparation: preparation of substrate Material with clean surface for MoS preparation2；
S2 single-layer MoS2Growing: with MoO3The powder and the S simple substance powder are used as reactants, and the chemical vapor deposition method is adopted to prepare MoS2In MoO3Adding NaOH powder into the powder, and ionizing during growth to obtain-OH in MoS2An S-Mo-S-OH structure is formed in the growth process.
2. The use of the single-layer molybdenum disulfide prepared according to claim 1 in a thin film transistor, wherein the MoS prepared by the positive photoresist stripping process in the microelectronic process is used2Preparing a source electrode structure and a drain electrode structure; semiconductor analyzer for prepared MoS2And electrically testing the thin film transistor, and testing the modulation and transfer characteristic curve of the gate electrode to the source and the drain.
3. The method according to claim 1, wherein in step S1, the substrate material is selected from a conductive substrate with an insulating layer.
4. Use according to claim 2, characterized in that MoS is a mobile phone2The electrodes of a source electrode and a drain electrode in the preparation of the thin film transistor adopt a double-layer structure, a Cr thin film is used as a contact layer and an adhesion layer, and an Au thin film is used as a conductive layer.
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