CN105742191A - Preparation method for molybdenum disulfide nanometer film with preset patterns - Google Patents
Preparation method for molybdenum disulfide nanometer film with preset patterns Download PDFInfo
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- CN105742191A CN105742191A CN201410757571.XA CN201410757571A CN105742191A CN 105742191 A CN105742191 A CN 105742191A CN 201410757571 A CN201410757571 A CN 201410757571A CN 105742191 A CN105742191 A CN 105742191A
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Abstract
The invention belongs to the technical field of semiconducting material and especially relates to a preparation method for a molybdenum disulfide nanometer film with preset patterns. The method comprises following steps: (1) presetting patterns on a substrate; (2) depositing a molybdenum-source film on the substrate with preset patterns through a film deposition method; (3) removing photo-resist by use of ketone solvent; (4) preparing the molybdenum disulfide film with preset patterns by means of the chemical vapor deposition (CVD) method. By means of the method, a uniform molybdenum disulfide film with preset patterns is obtained, and the possibility that the film may be damaged or polluted due to later shape processing to the molybdenum disulfide film is reduced.
Description
Technical field
The invention belongs to technical field of semiconductor, particularly to the molybdenum disulfide nano membrane preparation method of a kind of presetting pattern.
Background technology
Molybdenum bisuphide has higher transmitance and theoretical mobility, has the band gap of a 1.2eV～1.8eV, uses molybdenum bisuphide as the FET theory on-off ratio of channel material up to 1010, have extremely wide application prospect in field of electronic devices.Application in sensor, the band gap of layer of molybdenum-disulfide can change along with the change of the factors such as the pH value of surrounding or humidity, therefore can use as sensor material；In flexible and transparent electronic device, molybdenum bisuphide can be used as transparent-channel material；Additionally, molybdenum bisuphide also has certain advantage in physical property, its Young's modulus is up to 0.33TPa ± 0.07TPa, it is ensured that the durability of molybdenum bisuphide device.
Molybdenum disulfide nano film grows with the form of triangle lamella in preparation process.But in the preparation of electronic device, particularly FET, shape and arrangement for channel material have certain requirement.Generally adopting the method that the molybdenum bisuphide film prepared carries out ion etching to obtain required shape when making molybdenum bisuphide device, this method wastes time and energy in the past, and molybdenum bisuphide film easily causes in etching process damage or pollutes.It is thus desirable to find a kind of can the method for preset molybdenum bisuphide shape so that molybdenum bisuphide can industrial applications.
Summary of the invention
It is an object of the invention to overcome deficiency of the prior art, it is provided that the molybdenum disulfide nano membrane preparation method of a kind of presetting pattern.Presetting pattern in the presoma set-up procedure of molybdenum bisuphide preparation technology, then uses the method for chemical vapour deposition (CVD) to carry out the preparation of molybdenum bisuphide, thus efficiently avoid the destruction of molybdenum bisuphide to having generated or pollution.
The molybdenum disulfide nano membrane preparation method of a kind of presetting pattern, comprises the steps:
(1) on substrate, presetting pattern is carried out；
(2) method deposited by film is at one layer of molybdenum source film of deposited on substrates of presetting pattern；
(3) ketones solvent is used to remove photoresist；
(4) chemical vapour deposition (CVD) (CVD) method is used to prepare the molybdenum bisuphide film of presetting pattern；
Described substrate is the bright and clean smooth resistant to elevated temperatures substrates of all surface such as silicon substrate, germanium substrate, silicon carbide substrates or Sapphire Substrate, primarily serves the supporting role to presoma and deuterogenic molybdenum bisuphide sample, and sample is transferred to any substrate after making.
Presetting pattern process adopts ultraviolet exposure technology, Ion Beam Lithography Technology, electron beam lithography or nanometer embossing etc..
Prepare the oxide that molybdenum source presoma is metal molybdenum or molybdenum of molybdenum source film.
Film deposition process adopts the metal film preparation methoies such as magnetron sputtering, electron beam evaporation or ald.
The thickness of described molybdenum source film is 0.25nm～10nm.
Described ketones solvent is acetone.
Described photoresist is one or both in ultraviolet photoresist and electron beam exposure glue, required depending on concrete technology.
Preparing the sulfur source presoma that molybdenum bisuphide film uses is sulfur simple substance or hydrogen sulfide gas.
The molybdenum disulfide nano membrane preparation method of a kind of presetting pattern, comprises the steps:
(1) substrate cleans；
(2) use sol evenning machine spin coating one layer photoetching glue on substrate, use the mask plate of respective graphical that the substrate scribbling photoresist is exposed, is developed, the photoresist at presetting pattern position is removed；
(3) at one layer of molybdenum source film of deposited on substrates；
(4) use ketones solvent to wash away the molybdenum source presoma outside photoresist and graphic limit, substrate leaves behind the molybdenum source presoma corresponding with required figure；
(5) method using chemical vapour deposition (CVD), generates the molybdenum disulfide nano film of presetting pattern when 700 DEG C～900 DEG C.
The invention have the benefit that
Molybdenum disulfide nano membrane crystallization uniform quality prepared by the inventive method is consistent, and electron mobility can reach to use the phase same level of other CVD method.Can ensure that avoid rete on molybdenum disulfide nano film pattern basis accurately is subject to undermine the probability of pollution in later stage etching process simultaneously.
Accompanying drawing explanation
Fig. 1 is the process chart of the molybdenum disulfide nano membrane preparation method of presetting pattern of the present invention；
Fig. 2 is CVD system apparatus structure schematic diagram used in the present invention；
Number in the figure: 106-SiO2Or Si substrate, 107-photoresist, 201-high purity quartz pipe, 202-surface deposition have the SiO of molybdenum film2Or Si substrate.
Detailed description of the invention
The invention provides the molybdenum disulfide nano membrane preparation method of a kind of presetting pattern, below in conjunction with the drawings and specific embodiments, the present invention will be further described.
Fig. 1 is the flow process of presetting pattern molybdenum bisuphide membrane preparation method of the present invention, including:
Step 101: substrate cleans, and substrate can be silicon substrate, germanium substrate, silicon carbide substrates, Sapphire Substrate etc., primarily serves the supporting role to presoma and deuterogenic molybdenum bisuphide sample；
Step 102: using sol evenning machine spin coating one layer photoetching glue on substrate (can be ultraviolet exposure glue, ion beam exposure and electron beam exposure glue etc., depending on concrete technology requirement), the substrate scribbling photoresist is exposed, develops by the mask plate using respective graphical, is removed by the photoresist at presetting pattern position；
Step 103: the method utilizing magnetron sputtering technique, electron beam evaporation or ald, at the oxidation film of deposited on substrates layer of metal molybdenum film or molybdenum, thicknesses of layers is determined by required molybdenum bisuphide thickness；
Step 104: use ketones solvent to wash away the molybdenum source presoma outside photoresist and graphic limit, substrate leaves behind the molybdenum source presoma corresponding with required figure；
Step 105: the method using chemical vapour deposition (CVD), using elemental sulfur or hydrogen sulfide gas as sulfur source, the molybdenum source being loaded with substrate, the molybdenum disulfide nano film of presetting pattern is generated when 700 DEG C～900 DEG C；
Fig. 2 is CVD system apparatus structure schematic diagram used in the present invention.
Embodiment 1
A kind of can the molybdenum bisuphide CVD preparation method of presetting pattern, comprise the following specific steps that:
Step 101: substrate cleans, and substrate is thermal oxidation silicon substrate, primarily serves the supporting role to presoma and deuterogenic molybdenum bisuphide sample.
Step 102: using sol evenning machine spin coating one positive glue of layer photoetching on the silicon substrate of cleaning, use mask plate that the sample processed through front baking is exposed, sample is developed after processing by after bake；
Step 103: use magnetron sputtering apparatus to deposit layer of metal molybdenum in sample substrate as presoma.The technological parameter used in sputter procedure to be argon flow amount be 20sccm, sputtering pressure are 2.0Pa, sputtering power be 10W, sputtering time is 1min.Obtained molybdenum film thickness is about 5nm；
Step 104: the sample being coated with molybdenum film is soaked 20s in acetone solvent, dries.Molybdenum film outside presetting pattern is together removed with photoresist, and substrate leaves behind the molybdenum film of presetting pattern.
Step 105: the quartz boat being loaded with substrate is placed in the heating region of tubular heater, the quartz boat being loaded with sulfur simple substance is placed in the windward region of tubular heater, pass into the nitrogen of 20sccm, tube furnace temperature is set as 750 DEG C, rise to maintenance 10min after target temperature until furnace temperature.In cooling back substrate, namely deposition has the molybdenum disulfide nano film consistent with required figure of a layer.
Claims (10)
1. the molybdenum disulfide nano membrane preparation method of a presetting pattern, it is characterised in that comprise the steps:
(1) on substrate, presetting pattern is carried out；
(2) method deposited by film is at one layer of molybdenum source film of deposited on substrates of presetting pattern；
(3) ketones solvent is used to remove photoresist；
(4) chemical vapour deposition technique is used to prepare the molybdenum bisuphide film of presetting pattern.
2. the molybdenum disulfide nano membrane preparation method of a kind of presetting pattern according to claim 1, it is characterised in that described substrate is silicon substrate, germanium substrate, silicon carbide substrates or Sapphire Substrate.
3. the molybdenum disulfide nano membrane preparation method of a kind of presetting pattern according to claim 1, it is characterised in that presetting pattern process adopts ultraviolet exposure technology, Ion Beam Lithography Technology, electron beam lithography or nanometer embossing.
4. the molybdenum disulfide nano membrane preparation method of a kind of presetting pattern according to claim 1, it is characterised in that prepare the oxide that molybdenum source presoma is metal molybdenum or molybdenum of molybdenum source film.
5. the molybdenum disulfide nano membrane preparation method of a kind of presetting pattern according to claim 1, it is characterised in that film deposition process adopts magnetron sputtering, electron beam evaporation or Atomic layer deposition method.
6. the molybdenum disulfide nano membrane preparation method of a kind of presetting pattern according to claim 1, it is characterised in that the thickness of described molybdenum source film is 0.25nm～10nm.
7. the molybdenum disulfide nano membrane preparation method of a kind of presetting pattern according to claim 1, it is characterised in that described ketones solvent is acetone.
8. the molybdenum disulfide nano membrane preparation method of a kind of presetting pattern according to claim 1, it is characterised in that described photoresist is one or both in ultraviolet photoresist and electron beam exposure glue.
9. the molybdenum disulfide nano membrane preparation method of a kind of presetting pattern according to claim 1, it is characterised in that preparing the sulfur source presoma that molybdenum bisuphide film uses is sulfur simple substance or hydrogen sulfide gas.
10. the molybdenum disulfide nano membrane preparation method of a kind of presetting pattern according to claim 1～9 any one claim, it is characterised in that comprise the steps:
(1) substrate cleans；
(2) use sol evenning machine spin coating one layer photoetching glue on substrate, use the mask plate of respective graphical that the substrate scribbling photoresist is exposed, is developed, the photoresist at presetting pattern position is removed；
(3) at one layer of molybdenum source film of deposited on substrates；
(4) use ketones solvent to wash away the molybdenum source presoma outside photoresist and graphic limit, substrate leaves behind the molybdenum source presoma corresponding with required figure；
(5) method using chemical vapour deposition (CVD), generates the molybdenum disulfide nano film of presetting pattern when 700 DEG C～900 DEG C.
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| CN109378267A (en) * | 2018-09-27 | 2019-02-22 | 华中科技大学 | A kind of vulcanization molybdenum film and preparation method thereof |
| CN109881176A (en) * | 2019-03-08 | 2019-06-14 | 华南农业大学 | A kind of petal-like molybdenum disulfide two dimensional crystal material and its preparation method and application |
| CN111307911A (en) * | 2018-12-11 | 2020-06-19 | 有研工程技术研究院有限公司 | pH sensor and preparation method thereof |
| CN111542641A (en) * | 2017-11-07 | 2020-08-14 | 阿卜杜拉国王科技大学 | Method for growing transition metal dichalcogenide layer, transition metal dichalcogenide growth device, and method for forming semiconductor device |
| CN112853290A (en) * | 2021-01-05 | 2021-05-28 | 南昌大学 | Preparation method of large-area molybdenum disulfide film |
| CN115231616A (en) * | 2022-07-19 | 2022-10-25 | 南京大学 | Method for preparing molybdenum disulfide micropore pattern without mask |
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| CN111542641A (en) * | 2017-11-07 | 2020-08-14 | 阿卜杜拉国王科技大学 | Method for growing transition metal dichalcogenide layer, transition metal dichalcogenide growth device, and method for forming semiconductor device |
| CN111542641B (en) * | 2017-11-07 | 2022-08-16 | 阿卜杜拉国王科技大学 | Method for growing transition metal dichalcogenide layer, growth device and method for forming semiconductor device |
| US11538682B2 (en) | 2017-11-07 | 2022-12-27 | King Abdullah University Of Science And Technology | Method for growing a transition metal dichalcogenide layer, transition metal dichalcogenide growth device, and method for forming a semiconductor device |
| CN109378267A (en) * | 2018-09-27 | 2019-02-22 | 华中科技大学 | A kind of vulcanization molybdenum film and preparation method thereof |
| CN109378267B (en) * | 2018-09-27 | 2021-03-26 | 华中科技大学 | Molybdenum sulfide film and preparation method thereof |
| CN111307911A (en) * | 2018-12-11 | 2020-06-19 | 有研工程技术研究院有限公司 | pH sensor and preparation method thereof |
| CN111307911B (en) * | 2018-12-11 | 2024-01-09 | 有研工程技术研究院有限公司 | PH sensor and preparation method thereof |
| CN109881176A (en) * | 2019-03-08 | 2019-06-14 | 华南农业大学 | A kind of petal-like molybdenum disulfide two dimensional crystal material and its preparation method and application |
| CN112853290A (en) * | 2021-01-05 | 2021-05-28 | 南昌大学 | Preparation method of large-area molybdenum disulfide film |
| CN115231616A (en) * | 2022-07-19 | 2022-10-25 | 南京大学 | Method for preparing molybdenum disulfide micropore pattern without mask |
| CN115231616B (en) * | 2022-07-19 | 2023-06-16 | 南京大学 | Method for preparing molybdenum disulfide micropore pattern without mask |
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Application publication date: 20160706 |