CN104049022A - Molybdenum disulfide/silicon heterogeneous film component with hydrogen sensitivity effect as well as preparation method and application thereof - Google Patents
Molybdenum disulfide/silicon heterogeneous film component with hydrogen sensitivity effect as well as preparation method and application thereof Download PDFInfo
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- CN104049022A CN104049022A CN201410254110.0A CN201410254110A CN104049022A CN 104049022 A CN104049022 A CN 104049022A CN 201410254110 A CN201410254110 A CN 201410254110A CN 104049022 A CN104049022 A CN 104049022A
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Abstract
The invention discloses a molybdenum disulfide (MoS2)/silicon (Si) heterogeneous film component with a hydrogen sensitivity effect as well as a preparation method and application thereof. The MoS2/Si heterogeneous film component comprises a Si substrate and a MoS2 film layer which is deposited on the surface of the Si substrate by a direct current magnetron sputtering technology. According to the preparation method, by depositing the MoS2 film on the surface of the Si substrate, the MoS2/Si heterogeneous film component having an H2 sensitivity effect is prepared by virtue of H2 adsorption of the MoS2 film and electrical transport amplification action of a semiconductor heterogeneous interface. Test results show that under the condition of pure H2, when impressed voltage is -5V, the electric current of the MoS2/Si heterogeneous film component is reduced by two orders of magnitude; meanwhile, the heterogeneous film component shows obvious response to H2 concentration change. Compared with an existing semiconductor type H2 sensing component, the MoS2/Si heterogeneous film component has advantages of having obvious H2 response performance, and being good in repeatability, high in reliability and free of dependence on oxygen atmosphere condition and noble metal.
Description
Technical field
The invention belongs to nanometer semiconductor technology field, relate to semiconductor film film preparation and device fabrication technology, specifically relate to a kind of molybdenum disulfide/silicon heterofilm device with hydrogen sensitlzing effect and its preparation method and application.
Background technology
As a kind of reducibility gas and carrier gas, H
2the fields such as petrochemical industry, electronics, medical treatment, aviation have been widely used in.Meanwhile, H
2as new and effective clean energy resource, also attracted wide attention and large quantity research.But hydrogen molecule is very little, in production, transmission and use procedure, very easily leak.H in air
2when content reaches 5%～75%, under naked light condition, can there is heavy explosion.Therefore, the hydrogen content in air and specific environment is carried out in site measurement fast and accurately, there is great using value, also there is important academic significance simultaneously.Existing research shows, H
2the key of sensor development is research and the preparation of the quick material of hydrogen, and responsive response and the reappearance of the quick material of hydrogen are determining H
2the serviceability of sensor.In recent years, both at home and abroad to H
2the development of sensor mainly concentrates on the H such as semi-conductor type, electrothermic type, optical type, galvanochemistry type
2sensor.At various types of H
2in sensor, semi-conductor type H
2sensor (comprising MOS type and semiconductor Schottky type) has the plurality of advantages such as preparation technology is simple, the response time is short, reproducible, has now become the H being most widely used
2one of sensor.But existing semi-conductor type H of while
2sensor still exists the development that some shortcomings part is restricting it: MOS type H
2sensor need to be worked under aerobic conditions, and this has limited its usable range greatly; Schottky type H
2sensor needs noble metal (Pt, Pd etc.) carrier, and this causes its cost significantly to increase.For this reason, various novel semiconductor materials are constantly applied to novel H
2the development of sensor, wherein MoS
2material more merits attention.
MoS
2, be commonly called brightness molybdenum, at occurring in nature rich content.According to statistics, global molybdenum reserves are about 1,900 ten thousand tons, and the molybdenum ore resource of China is also quite abundant, and total reserves is about more than 800 ten thousand tons, is only second to the U.S. and occupies the 2nd, the world.MoS
2be typical layer structure, each unit is all " sandwich " structures of S-Mo-S.With weak Van der Waals force, combine between layers, there is larger space; In layer, with covalent bond, be closely linked, each Mo atom is surrounded by six S atoms, is triangular prism column, exposes a lot of Mo-S faceted pebbles, can be used as catalytic activity and gas adsorption site.Therefore, MoS
2in development of new gas sensor field, there is wide application prospect in material.The calculated results of having reported shows: MoS
2easily to H
2produce absorption, and cause its resistance generation significant change.This result of calculation shows, MoS
2can be used for developing H
2sensor, but the current report that there is no correlation test result at home and abroad.
Summary of the invention
The object of the present invention is to provide a kind of preparation method and application with molybdenum disulfide/silicon heterofilm device and this molybdenum disulfide/silicon heterofilm device of hydrogen sensitlzing effect.
The technology used in the present invention solution is:
Molybdenum disulfide/silicon heterofilm device with hydrogen sensitlzing effect, comprises Si substrate and MoS
2thin layer, MoS
2thin layer is arranged on Si substrate surface.
Preferably, described Si substrate is p-type Si single crystalline substrate, and resistivity is 1～10 Ω cm
-1; Described MoS
2thin layer thickness is 30～50nm.
Preferably, described Si substrate surface is also coated with mask sheet, and mask sheet is positioned at MoS
2between thin layer and Si substrate.
Preferably, described Si substrate and MoS
2on thin layer, be suppressed with metal electrode, metal electrode connects wire.
A preparation method with molybdenum disulfide/silicon heterofilm device of hydrogen sensitlzing effect, comprises the following steps:
(1) choose Si substrate, it is cleaned, then adopt chemical corrosion method to remove and clean rear Si substrate surface oxide layer;
(2) to removing the Si substrate of surface oxide layer, be dried, then coverage mask sheet;
(3) the Si substrate of coverage mask sheet is put into vacuum chamber, under Ar compression ring border, adopt magnetically controlled DC sputtering technology, utilize the Ions Bombardment MoS ionizing out
2target, at Si substrate surface deposition MoS
2thin layer, makes MoS
2/ Si heterofilm;
(4) respectively at MoS
2the MoS of/Si heterofilm
2on film and Si substrate, complete the compacting of metal electrode, and draw wire, make MoS
2/ Si heterofilm device.
Preferably, in step (1), described Si substrate is p-type Si single crystalline substrate, is of a size of 10 * 10mm, and resistivity is 1～10 Ω cm
-1; Cleaning process is as follows: by the repeated ultrasonic cleaning in high absolute alcohol and acetone soln successively of Si substrate, each time span of cleaning is 180s; , the removal process of described Si substrate surface oxide layer is as follows: Si substrate is soaked to 50～70s in hydrofluoric acid solution, and the mass concentration of hydrofluoric acid solution is 3～5%.
Preferably, described in step (2), Si substrate dry run is with drying nitrogen, substrate to be dried up, and nitrogen gas purity is 99.5%; Described mask sheet material is molybdenum, and thickness is 0.1mm, is of a size of 10 * 10mm, and aperture size is 5 * 5mm.
Preferably, in step (3), the back end vacuum tightness of described vacuum chamber is 5 * 10
-5pa, vacuum condition is jointly to be made by mechanical pump and molecular pump two-stage vacuum pump; Described MoS
2target is MoS
2pottery rake, target purity is 99.9%, and it is constant that described Ar gas air pressure maintains 1.0Pa, and target-substrate distance is 50mm, and the depositing temperature of film is 100 ℃, thin layer thickness is 30～50nm.
Preferably, in step (4), described metal electrode and conductor material are respectively In and Cu, and wherein the purity of In is 99.5%, and metal electrode diameter and thickness are 3mm, and Cu diameter of wire is 0.1mm.
Above-mentioned molybdenum disulfide/silicon heterofilm device with hydrogen sensitlzing effect can be at preparation H
2senser element aspect is applied.
Useful technique effect of the present invention is:
The present invention is by depositing MoS at Si substrate surface
2film, utilizes MoS
2film is to H
2suction-operated and the electronic transport amplification at heterogeneous semiconductor interface, develop and have H
2the MoS of sensitlzing effect
2/ Si heterofilm device.Test result shows: at pure H
2under condition, when impressed voltage be-during 5V, MoS
2the electric current of/Si heterofilm device reduces two orders of magnitude; Meanwhile, this heterofilm device is to H
2concentration change shows obvious response characteristic.With current existing semi-conductor type H
2senser element is compared, and the present invention has got rid of the dependence to oxygen atmosphere condition and noble metal, and has H
2response performance is remarkable, reproducible, high reliability, and preparation technology is simple, for preparing novel H
2senser element provides a kind of good semiconductor material and device architecture, at H
2field of detecting has more wide application prospect.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further illustrated:
Fig. 1 is prepared MoS
2the structural representation that/Si heterofilm device gas sensitization performance is measured.
Fig. 2 is without H
2with pure H
2prepared MoS under condition
2the I-V curve comparison of/Si heterofilm device.
Fig. 3 is prepared MoS
2/ Si heterofilm device is to pure H
2response performance.
Fig. 4 is prepared MoS
2/ Si heterofilm device is to variable concentrations H
2response performance.
Embodiment
The present invention utilizes magnetically controlled DC sputtering technology, in Si Semiconductor substrate, deposits MoS
2thin layer, thus MoS formed
2/ Si heterojunction.When being exposed to H
2in atmosphere, due to H
2produce absorption, MoS
2charge carrier and the Fermi level of film change, and this causes MoS
2the junction resistance generation significant change of/Si heterojunction, thus make prepared MoS
2/ Si heterojunction is to H
2show obvious response performance.
Below to MoS
2structure, preparation method and the application of/Si heterofilm device are elaborated.
MoS of the present invention
2/ Si heterofilm structure, comprises MoS
2semiconductor film layer and Si Semiconductor substrate, MoS
2thin layer is arranged on Si substrate surface.Si substrate is p-type Si single crystalline substrate, and resistivity is 1～10 Ω cm
-1, crystalline orientation is (100) orientation.Described MoS
2thin layer is to adopt magnetically controlled DC sputtering deposition techniques on Si substrate, and thickness is 30～50nm.
Say further, described Si substrate surface is also coated with mask sheet, and mask sheet is positioned at MoS
2between thin layer and Si substrate, mask sheet material therefor is molybdenum, and mask sheet thickness is 0.1mm, is of a size of 10 * 10mm, and aperture size is 5 * 5mm.
Further, at MoS
2the MoS of/Si heterofilm
2difference pressed metal electrode on thin layer and Si substrate, and draw wire, obtain MoS
2/ Si heterofilm device.
Above-mentioned MoS
2the preparation method of/Si heterofilm device, specifically comprises the following steps:
(1) choose Si substrate, it is cleaned, then adopt chemical corrosion method to remove and clean rear Si substrate surface oxide layer; Described Si substrate is p-type Si single crystalline substrate, is of a size of 10 * 10mm, and resistivity is 1～10 Ω cm
-1; Cleaning process is as follows: by the repeated ultrasonic cleaning in high absolute alcohol and acetone soln successively of Si substrate, each time span of cleaning is 180s; , the removal process of described Si substrate surface oxide layer is as follows: Si substrate is soaked to 50～70s in hydrofluoric acid solution, and preferred 60s, the mass concentration of hydrofluoric acid solution is 3～5%, as specifically can be 3%, 4% or 5%.
(2) to removing the Si substrate of surface oxide layer, be dried, then coverage mask sheet; Described Si substrate dry run is with drying nitrogen, substrate to be dried up, and nitrogen gas purity is 99.5%; Described mask sheet material is molybdenum, and thickness is 0.1mm, is of a size of 10 * 10mm, and aperture size is 5 * 5mm.
(3) the Si substrate of coverage mask sheet is put into vacuum chamber, under Ar compression ring border, adopt magnetically controlled DC sputtering technology, utilize the Ar Ions Bombardment MoS ionizing out
2target, at Si substrate surface deposition MoS
2thin layer, makes MoS
2/ Si heterofilm; The back end vacuum tightness of described vacuum chamber is 5 * 10
-5pa, vacuum condition is jointly to be made by mechanical pump and molecular pump two-stage vacuum pump; Described MoS
2target is MoS
2pottery rake, target purity is 99.9%, and it is constant that described Ar gas air pressure maintains 1.0Pa, and target-substrate distance is 50mm, and the depositing temperature of film is 100 ℃, thin layer thickness is 30～50nm.
(4) respectively at MoS
2the MoS of/Si heterofilm
2on film and Si substrate, complete the compacting of metal electrode, and draw wire, make MoS
2/ Si heterofilm device.Described metal electrode and conductor material are respectively In and Cu, and wherein the purity of In is 99.5%, and metal electrode diameter and thickness are 3mm, and Cu diameter of wire is 0.1mm.
Above-mentioned molybdenum disulfide/silicon heterofilm device with hydrogen sensitlzing effect can be at preparation H
2senser element aspect is applied.
Below in conjunction with performance measurement result, further illustrate effect of the present invention:
Fig. 1 is prepared MoS
2the structural representation that/Si heterofilm device gas sensitization performance is measured.
Fig. 2 is without H
2with pure H
2prepared MoS under condition
2the I-V curve comparison of/Si heterofilm device.As shown in the figure, prepared MoS
2the I-V curve table of/Si heterofilm device reveals obvious asymmetric feature.At pure H
2under condition, when voltage be-during 5V, the electric current of heterofilm is 4.1 * 10
-3mA, this is than without H
2electric current (4.5 * 10 under condition
-1mA) reduce two orders of magnitude.Above-mentioned feature shows: prepared MoS
2/ Si heterofilm device shows obvious H
2sensitive property.
Fig. 3 is prepared MoS
2/ Si heterofilm device is to pure H
2response performance.As shown in the figure, by changing its residing atmospheric condition, prepared MoS
2/ Si heterofilm device shows good H
2response performance, has in stable condition, repeated advantages of higher.
Fig. 4 is prepared MoS
2/ Si heterofilm device is to variable concentrations H
2response performance.As shown in the figure, prepared MoS
2/ Si heterofilm device is to different low concentration H
2all shown obvious response performance.Work as H
2when concentration occurs to change a little, prepared MoS
2the inverse current of/Si heterofilm device changes fast.This further illustrates such heterofilm device and can be used to development of new H
2senser element.
Claims (10)
1. molybdenum disulfide/silicon heterofilm device with hydrogen sensitlzing effect, is characterized in that: comprise Si substrate and MoS
2thin layer, MoS
2thin layer is arranged on Si substrate surface.
2. a kind of molybdenum disulfide/silicon heterofilm device with hydrogen sensitlzing effect according to claim 1, is characterized in that: described Si substrate is p-type Si single crystalline substrate, and resistivity is 1～10 Ω cm
-1; Described MoS
2thin layer thickness is 30～50nm.
3. a kind of molybdenum disulfide/silicon heterofilm device with hydrogen sensitlzing effect according to claim 1, is characterized in that: described Si substrate surface is also coated with mask sheet, and mask sheet is positioned at MoS
2between thin layer and Si substrate.
4. a kind of molybdenum disulfide/silicon heterofilm device with hydrogen sensitlzing effect according to claim 1, is characterized in that: described Si substrate and MoS
2on thin layer, be suppressed with metal electrode, metal electrode connects wire.
5. a preparation method with molybdenum disulfide/silicon heterofilm device of hydrogen sensitlzing effect, is characterized in that comprising the following steps:
(1) choose Si substrate, it is cleaned, then adopt chemical corrosion method to remove and clean rear Si substrate surface oxide layer;
(2) to removing the Si substrate of surface oxide layer, be dried, then coverage mask sheet;
(3) the Si substrate of coverage mask sheet is put into vacuum chamber, under Ar compression ring border, adopt magnetically controlled DC sputtering technology, utilize the Ions Bombardment MoS ionizing out
2target, at Si substrate surface deposition MoS
2thin layer, makes MoS
2/ Si heterofilm;
(4) respectively at MoS
2the MoS of/Si heterofilm
2on film and Si substrate, complete the compacting of metal electrode, and draw wire, make MoS
2/ Si heterofilm device.
6. a kind of preparation method with molybdenum disulfide/silicon heterofilm device of hydrogen sensitlzing effect according to claim 5, it is characterized in that: in step (1), described Si substrate is p-type Si single crystalline substrate, is of a size of 10 * 10mm, and resistivity is 1～10 Ω cm
-1; Cleaning process is as follows: by the repeated ultrasonic cleaning in high absolute alcohol and acetone soln successively of Si substrate, each time span of cleaning is 180s; , the removal process of described Si substrate surface oxide layer is as follows: Si substrate is soaked to 50～70s in hydrofluoric acid solution, and the mass concentration of hydrofluoric acid solution is 3～5%.
7. a kind of preparation method with molybdenum disulfide/silicon heterofilm device of hydrogen sensitlzing effect according to claim 5, it is characterized in that: described in step (2), Si substrate dry run is with drying nitrogen, substrate to be dried up, nitrogen gas purity is 99.5%; Described mask sheet material is molybdenum, and thickness is 0.1mm, is of a size of 10 * 10mm, and aperture size is 5 * 5mm.
8. a kind of preparation method with molybdenum disulfide/silicon heterofilm device of hydrogen sensitlzing effect according to claim 5, is characterized in that: in step (3), the back end vacuum tightness of described vacuum chamber is 5 * 10
-5pa, vacuum condition is jointly to be made by mechanical pump and molecular pump two-stage vacuum pump; Described MoS
2target is MoS
2pottery rake, target purity is 99.9%, and it is constant that described Ar gas air pressure maintains 1.0Pa, and target-substrate distance is 50mm, and the depositing temperature of film is 100 ℃, thin layer thickness is 30～50nm.
9. a kind of preparation method with molybdenum disulfide/silicon heterofilm device of hydrogen sensitlzing effect according to claim 5, it is characterized in that: in step (4), described metal electrode and conductor material are respectively In and Cu, wherein the purity of In is 99.5%, metal electrode diameter and thickness are 3mm, and Cu diameter of wire is 0.1mm.
10. a kind of molybdenum disulfide/silicon heterofilm device with hydrogen sensitlzing effect as claimed in claim 1 is at preparation H
2the application of senser element aspect.
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| CN104465844A (en) * | 2014-11-27 | 2015-03-25 | 中国石油大学(华东) | MoS2/Si p-n junction solar cell device and preparation method thereof |
| CN104614403A (en) * | 2015-01-22 | 2015-05-13 | 江西师范大学 | Sensor, forming method of sensor, and method for defecting gas |
| CN104792830A (en) * | 2015-05-15 | 2015-07-22 | 哈尔滨工业大学 | Graphene/molybdenum disulfide compounding-based gas sensitive material and preparation method thereof |
| CN105021683A (en) * | 2015-06-05 | 2015-11-04 | 东南大学 | Manufacturing method for molybdenum disulfide field effect transistor for biomolecular detection |
| CN105158306A (en) * | 2015-07-09 | 2015-12-16 | 济南大学 | Preparation method of gas sensor for volatile organic matter detection |
| CN105928986A (en) * | 2016-04-11 | 2016-09-07 | 温州大学 | Silicon carbon based high temperature hydrogen sensor and preparation method thereof |
| CN109682863A (en) * | 2018-12-10 | 2019-04-26 | 华中科技大学 | Gas sensor and preparation method thereof based on TMDCs-SFOI hetero-junctions |
| CN109935654A (en) * | 2019-03-21 | 2019-06-25 | 电子科技大学 | A kind of silicon substrate molybdenum disulfide heterojunction photovoltaic sensor and preparation method |
| CN113644138A (en) * | 2021-06-21 | 2021-11-12 | 西安电子科技大学 | Single layer MoS2-Si-based tunneling diode and preparation method thereof |
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| CN104465844A (en) * | 2014-11-27 | 2015-03-25 | 中国石油大学(华东) | MoS2/Si p-n junction solar cell device and preparation method thereof |
| CN104614403B (en) * | 2015-01-22 | 2017-05-24 | 江西师范大学 | Sensor, forming method of sensor, and method for defecting gas |
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| CN104792830A (en) * | 2015-05-15 | 2015-07-22 | 哈尔滨工业大学 | Graphene/molybdenum disulfide compounding-based gas sensitive material and preparation method thereof |
| CN104792830B (en) * | 2015-05-15 | 2017-06-16 | 哈尔滨工业大学 | The preparation method of the gas sensitive material being combined based on Graphene/molybdenum bisuphide |
| CN105021683B (en) * | 2015-06-05 | 2017-09-15 | 东南大学 | Towards the preparation method of the molybdenum disulfide field-effect transistor of biomolecule detection |
| CN105021683A (en) * | 2015-06-05 | 2015-11-04 | 东南大学 | Manufacturing method for molybdenum disulfide field effect transistor for biomolecular detection |
| CN105158306B (en) * | 2015-07-09 | 2016-06-22 | 济南大学 | A kind of preparation method of the gas sensor for volatile organic matter detection |
| CN105158306A (en) * | 2015-07-09 | 2015-12-16 | 济南大学 | Preparation method of gas sensor for volatile organic matter detection |
| CN105928986A (en) * | 2016-04-11 | 2016-09-07 | 温州大学 | Silicon carbon based high temperature hydrogen sensor and preparation method thereof |
| CN105928986B (en) * | 2016-04-11 | 2018-08-31 | 温州大学 | A kind of Si carbon-base high-temperature hydrogen sensor and preparation method thereof |
| CN109682863A (en) * | 2018-12-10 | 2019-04-26 | 华中科技大学 | Gas sensor and preparation method thereof based on TMDCs-SFOI hetero-junctions |
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Application publication date: 20140917 |