CN106567039B - A kind of MoS2/Ag/MoS2Semiconductor film material and preparation method thereof - Google Patents
A kind of MoS2/Ag/MoS2Semiconductor film material and preparation method thereof Download PDFInfo
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- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 126
- 229910052961 molybdenite Inorganic materials 0.000 title claims abstract description 119
- 239000000463 material Substances 0.000 title claims abstract description 66
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000010408 film Substances 0.000 claims abstract description 80
- 229910052751 metal Inorganic materials 0.000 claims abstract description 46
- 239000002184 metal Substances 0.000 claims abstract description 43
- 239000010409 thin film Substances 0.000 claims abstract description 42
- 239000004065 semiconductor Substances 0.000 claims abstract description 25
- 239000000758 substrate Substances 0.000 claims abstract description 23
- 238000004544 sputter deposition Methods 0.000 claims abstract description 21
- 238000005516 engineering process Methods 0.000 claims abstract description 7
- 238000009413 insulation Methods 0.000 claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 239000000919 ceramic Substances 0.000 claims description 12
- 238000010849 ion bombardment Methods 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 238000000151 deposition Methods 0.000 claims description 7
- 230000008021 deposition Effects 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000001465 metallisation Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 20
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 4
- 239000013077 target material Substances 0.000 abstract 1
- 238000009830 intercalation Methods 0.000 description 12
- 239000000047 product Substances 0.000 description 12
- 230000002687 intercalation Effects 0.000 description 11
- 230000000694 effects Effects 0.000 description 10
- 238000001755 magnetron sputter deposition Methods 0.000 description 9
- 108091006149 Electron carriers Proteins 0.000 description 4
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 239000003574 free electron Substances 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 230000007096 poisonous effect Effects 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 206010054949 Metaplasia Diseases 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 230000002463 transducing effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0623—Sulfides, selenides or tellurides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- 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
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
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- Inorganic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The present invention discloses a kind of MoS2/Ag/MoS2Semiconductor film material and preparation method thereof, the film are layer structure, from top to bottom successively include top layer MoS2Film layer, Ag metal layer, bottom MoS2Film layer and intrinsic insulation Si substrate.Preparation method is mainly used magnetically controlled DC sputtering technology, is successively bombarded different target material surfaces using high energy electron: using MoS first2Target deposits upper one layer of bottom MoS on Si substrate surface2Film layer；Then metal Ag target is used, in bottom MoS2One layer of Ag metal layer is deposited in film layer；Finally use MoS2Target deposits upper one layer of top layer MoS on Ag metal layer2Film layer.Relative to pure MoS2Film product, MoS of the invention2/Ag/MoS2Semiconductive thin film, resistivity reduce 4 orders of magnitude or more.Simple process of the invention, state modulator are easy；High yield rate, stable product quality and good reliability, and manufacturing cost is low, is suitable for industrialized production.
Description
Technical field
The present invention relates to a kind of semiconductor material and preparation method thereof more particularly to a kind of MoS2/Ag/MoS2Semiconductor film
Membrane material and preparation method thereof.
Background technique
Molybdenum disulfide itself is non-conductive, but has diamagnetism, can be used as linear photoconductor conductor and display p-type or N-type is conductive
The semiconductor of performance has the function of rectification and transducing.
Since molybdenum disulfide film material has typical layer structure, it is closely linked in layer with covalent bond, often
A Mo atom is surrounded by six S atoms, is in triangular prism column；It is then combined, is easy with weaker Van der Waals force between layers
It slips away.
The above structure feature of molybdenum disulfide leads to that its resistivity is very big, carrier transport performance is poor, makes it half
The application of conductor and devices field receives serious obstruction.
To reduce MoS2The resistivity of thin-film material improves its electric conductivity, to meet MoS2Thin-film material is in semiconductor device
The use in part field.In the prior art, relatively successful way is, using metallic element to MoS2Be doped, with into
Row MoS2Material modification.Such as:
Wu Chen et al. (" micro-nano electronic technology ", 2014,08) disclose " Ag adulterate to MoS2The influence of film characteristics " is ground
Study carefully as a result, being prepared for Ag doping MoS on p-type electric-conducting Si substrate using chemical vapour deposition technique2Thin-film material；
Chinese patent ZL201510558994.3 discloses a kind of Pd-MoS2Heterojunction photovoltaic solar cell device and its
Preparation method, the technological means used are to carry out MoS using Pd metallic element2Doping treatment.
But this use metallic element is to MoS2It is doped, to carry out MoS2The method of material modification, principle are equal
It is to enter metallic element in molybdenum disulfide lattice, to replace molybdenum element original in molybdenum disulfide.Due to atomic radius, obtain
The difference of betatopic ability etc., this doping techniques necessarily form a large amount of defects in molybdenum disulfide, so as to cause product
Material structure and performance unstability.
In other words, using the technological means of doping, to carry out MoS2The modification of thin-film material, properties of product it is consistent
Property, stability are relatively poor, and the control difficulty of product quality is big.
More importantly the MoS for technical field of semiconductor device, after this kind of doping vario-property2Thin-film material,
Its resistivity is still higher, electric conductivity is still undesirable.
Summary of the invention
It is an object of the invention to provide a kind of MoS with excellent conductive performance2/Ag/MoS2Semiconductor film membrane material
Material.
Required technical problems to be solved are how MoS to be effectively reduced to the present invention to achieve the above object2Thin-film material
The technical issues of resistivity.
Present invention technical solution used for the above purpose is a kind of MoS2/Ag/MoS2Semiconductor film material,
It from top to bottom successively include top layer MoS it is characterized in that, being layer structure2Film layer, Ag metal layer, bottom MoS2Film layer and
Si substrate；Wherein:
The Si substrate is the intrinsic non-conductive monocrystal material of insulation, and single-sided polishing, burnishing surface is upper surface；
The MoS2Film layer, purity 99.9%；
The Ag metal layer, purity 99.99%；
The top layer MoS2Film layer, Ag metal layer, bottom MoS2The thickness of film layer be respectively 50nm, 3-10nm and
50nm。
The technical effect brought directely by the technical proposal is that in top layer MoS2Film layer and bottom MoS2Between film layer
It is inserted into one layer thin Ag metal layer, significantly reduces MoS2The resistivity value of thin-film material, significantly improves MoS2Thin-film material is led
Electrical property, and it is formed by MoS2/Ag/MoS2The stable structure of film, performance repeatability are strong.
Testing result shows MoS obtained by adopting the above technical scheme2/Ag/MoS2Thin-film material, electronic carrier are dense
Degree, electron mobility respectively reach 8.3 × 1022cm-3And 8.5cm2V-1s-1。
These performance parameters with have pure MoS2Thin-film material (pure MoS2Electron carrier density, the electronics of thin-film material move
Shifting rate and resistivity value are respectively 2.1 × 1017cm-3、0.1cm2V-1s-1) compare, 5 orders of magnitude and 1 are at least improved respectively
The order of magnitude.
In particular, the MoS obtained by by adopting the above technical scheme2/Ag/MoS2Thin-film material, resistivity value reaches 5.7 ×
10-2Ω cm, than single MoS2The resistivity value (1.1 × 10 of thin-film material3Ω cm) at least low 4 orders of magnitude.
Generally, the present invention is by by single MoS2Film layer changes into " sandwich of layers " structure type: using upper
Lower two layers of MoS2It is inserted into one layer of Ag thin metal layer this simple technological means between film layer, dexterously utilizes and be inserted into
Free electron in Ag thin metal layer is to MoS2The electron injection effect of film layer, the electronic carrier improved in thin-film material are dense
Degree and electron mobility, reaching significantly reduces MoS2The resistivity value of thin-film material improves MoS2The electric conductivity of thin-film material
Purpose.
To more fully understand above-mentioned technical proposal, now it is described in detail from principle:
1, Ag metal intercalation is to MoS2There are three aspects for the attainable technical effect of thin-film material:
(1) a large amount of free electrons in Ag metal intercalation respectively enter top layer MoS by injection effect2Film layer and bottom
MoS2Upper and lower MoS has been respectively increased in film layer2Electron carrier density and electron mobility in film layer；
(2) by improving upper layer and lower layer MoS2Electron concentration and electron mobility in thin-film material, significantly reduce MoS2
The resistivity of thin-film material, substantially enhances MoS2The electric conductivity of thin-film material；
(3) continuity Characteristics of intermediate Ag metal intercalation, effectively enhance the stability of membrane structure, reduce in film
Portion's defects count, so that the stability of thin-film material performance and repeatability be made to be improved.
2, in above-mentioned technical proposal, the electronic work function of Ag metal layer is 4.2eV, is less than MoS2The work function of thin-film material
Value 4.5eV, to ensure that electronics can be injected into MoS by Ag metal layer2Film layer；
3, in above-mentioned technical proposal, Ag metal layer is located at two layers of MoS2Between material, it is conducive to electronics and passes through injection effect point
It Jin Ru not upper layer and lower layer MoS2Film layer improves the uniformity of Carrier Profile inside entire thin-film material；
4, in above-mentioned technical proposal, the thickness ultrathin of Ag metal layer is 3-10nm, on the one hand improves the equal of Ag metal layer
Even continuity；On the other hand also avoid film internal electron only using Ag metal layer as transfer passages, and without MoS2Film layer；
Meanwhile Ag metal layer can be upper layer and lower layer MoS2Film provides a large amount of free electrons.
It is demonstrated experimentally that the MoS of above-mentioned technical proposal2/Ag/MoS2Thin-film material has electron concentration height, electron mobility
Greatly, resistivity value is small, structure and steady performance.
Preferably, the bottom MoS2Film layer is deposited on the upper surface Si using DC magnetron sputtering method
's；
The Ag metal layer is to be deposited on the MoS using DC magnetron sputtering method2On film layer；
The top layer MoS2Film layer is deposited on the Ag metal layer using DC magnetron sputtering method.
The direct bring of the optimal technical scheme has the technical effect that preparation method is simple, technical process is easily controllable, product
Quality stability is more preferable with consistency.
The second purpose of the invention is to provide a kind of above-mentioned MoS2/Ag/MoS2The preparation method of semiconductor film material,
Its preparation process is simple, process is easily-controllable, high yield rate, and environmental friendly, is suitable for industrialized production.
Present invention technical solution used for the above purpose is a kind of above-mentioned MoS2/Ag/MoS2Thin-film material
Preparation method, which comprises the following steps:
The first step, silicon substrate surface cleaning step
The intrinsic non-conductive type Si monocrystal chip of insulation is chosen, is successively cleaned by ultrasonic in alcohol, acetone and deionized water
180s；
It takes out and is dried up with drying nitrogen；
Second step, bottom MoS2Thin-film surface deposition step
Si monocrystal chip substrate after cleaning is packed into pallet, is put into vacuum chamber, and vacuum chamber is taken out as high vacuum, in argon
Under compression ring border, the temperature of Si monocrystal chip is adjusted to the first temperature, ar pressure is adjusted to first pressure, using magnetically controlled DC sputtering
Technology utilizes the ion bombardment MoS ionized out under the conditions of constant 30W sputtering power2Ceramic target, in the Si substrate
Upper surface on, deposit one layer of MoS2Film layer；
Third step, Ag layer on surface of metal deposition step
By the pallet-changing equipped with sample to the surface of Ag metal targets；
The temperature of Si monocrystal chip is adjusted to second temperature, Ar air pressure is adjusted to second pressure, using magnetically controlled DC sputtering skill
Art, under the conditions of constant 30W sputtering power, using the ion bombardment Ag metal targets ionized out, in above-mentioned bottom MoS2It is thin
On the surface of film layer, redeposited one layer of Ag metal layer；
4th step, top layer MoS2Thin-film surface deposition step
Pallet equipped with sample is replaced again to MoS2The surface of ceramic target；
The temperature of Si monocrystal chip is adjusted to third temperature, Ar air pressure is adjusted to third pressure, using magnetically controlled DC sputtering skill
Art utilizes the ion bombardment MoS ionized out under the conditions of constant 30W sputtering power2Ceramic target, in above-mentioned Ag metal layer
Surface on, one layer of MoS of redeposition2Film layer to get.
The technical effect brought directely by the technical proposal is that preparation process is simple, high yield rate, it is suitable for industrial metaplasia
It produces, and above-mentioned preparation method is used without poisonous and harmful raw material, without poisonous and harmful waste generation or exhaust gas discharge, entire technique stream
Journey is environmentally protective, pollution-free；
Uniform in quality obtained by above-mentioned technical proposal is stable, each film layer adhesion-tight, thickness are uniform and stable and
It is easily controllable.
Preferably, the purity of above-mentioned argon gas is 99.999% or more；The high pure nitrogen refers to that purity is 99.95% or more
Drying nitrogen；The MoS2Ceramic target, purity 99.9%；The Ag metal targets, purity 99.99%；Institute
State MoS2The target-substrate distance of the target-substrate distance of target and the Ag target is 50mm.
The direct bring of the optimal technical scheme has the technical effect that, the distance be both able to satisfy ion during the motion with work
Make gas and sufficiently collide reduction kinetic energy, and can guarantee that ion has enough adhesive force in film forming procedure.
Further preferably, above-mentioned first temperature is 20-400 DEG C, and the first pressure is 1-10Pa；
The second temperature is 20-30 DEG C, and the second pressure is 1-5Pa；
The third temperature is 20-400 DEG C, and the third pressure is 1-10Pa.
The direct bring of the optimal technical scheme has the technical effect that, both can guarantee and has obtained good molybdenum disulfide film and silver
The crystal quality of metallic diaphragm, and be able to satisfy needed for ion film forming procedure, enough adhesive force, while can also be easier
Control film forming thickness.
In conclusion the present invention compared with the existing technology, has the advantages that
1, MoS of the invention2/Ag/MoS2Semiconductor film material has very significant low-resistivity (in room temperature condition
Under, electron carrier density, electron mobility and resistivity value are respectively 8.3 × 1022cm-3、8.5cm2V-1s-1With 5.7 × 10-2
Ωcm.With single pure MoS2Thin-film material compares, and carrier concentration at least improves 5 orders of magnitude, and electron mobility is at least
1 order of magnitude is improved, and resistivity value at least reduces 4 orders of magnitude).
2, MoS of the invention2/Ag/MoS2The preparation method of semiconductor film material has simple process, state modulator letter
Just；And its high yield rate, manufacturing cost are low, stable product quality and good reliability, are suitable for industrialized production.
Detailed description of the invention
Fig. 1 is MoS of the invention2/Ag/MoS2The structural schematic diagram of semiconductor film material；
Fig. 2 is MoS obtained by embodiment 12/Ag/MoS2The Raman spectrogram of semiconductor film material；
Fig. 3 is MoS of the invention2/Ag/MoS2The electron carrier density and mobility value of semiconductor film material are distinguished
With the variation rule curve figure of Ag layer thickness variation；
Fig. 4 is MoS of the invention2/Ag/MoS2The resistivity value of semiconductor film material with Ag layer thickness variation variation
Law curve figure.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is described in detail.
Embodiment 1
The preparation method is as follows:
The first step, silicon substrate surface cleaning step
The intrinsic non-conductive type Si monocrystal chip of insulation is chosen, is successively cleaned by ultrasonic in alcohol, acetone and deionized water
180s；
It takes out and is dried up with drying nitrogen；
Second step, bottom MoS2Thin-film surface deposition step
Si monocrystal chip substrate after cleaning is packed into pallet, is put into vacuum chamber, and vacuum chamber is taken out as high vacuum, in argon
Under compression ring border, the temperature of Si monocrystal chip is adjusted to 200 DEG C of the first temperature, ar pressure is adjusted to first pressure 3Pa, using direct current
Magnetron sputtering technique utilizes the ion bombardment MoS ionized out under the conditions of constant 30W sputtering power2Ceramic target, in institute
On the upper surface for stating Si substrate, the MoS that a layer thickness is 50nm is deposited2Film layer；
Third step, Ag layer on surface of metal deposition step
By the pallet-changing equipped with sample to the surface of Ag metal targets；
The temperature of Si monocrystal chip is adjusted to 20-25 DEG C of second temperature, Ar air pressure is adjusted to second pressure 5Pa, using direct current
Magnetron sputtering technique, under the conditions of constant 30W sputtering power, using the ion bombardment Ag metal targets ionized out, above-mentioned
Bottom MoS2On the surface of film layer, redeposited a layer thickness is the Ag metal layer of 10nm；
4th step, top layer MoS2Thin-film surface deposition step
Pallet equipped with sample is replaced again to MoS2The surface of ceramic target；
The temperature of Si monocrystal chip is adjusted to 200 DEG C of third temperature, Ar air pressure is adjusted to third pressure 3Pa, using DC magnetic
Control sputtering technology utilizes the ion bombardment MoS ionized out under the conditions of constant 30W sputtering power2Ceramic target, above-mentioned
On the surface of Ag metal layer, redeposited a layer thickness is the MoS of 50nm2Film layer to get.
Properties of product testing result:
Through detecting, under the conditions of room temperature (20-25 DEG C), obtained MoS2/Ag/MoS2The electronics of semiconductor film material
Carrier concentration, electron mobility and resistivity value are respectively 8.3 × 1022cm-3、8.5cm2V-1s-1With 5.7 × 10-2Ωcm。
Illustrate: pure MoS2Electron carrier density, electron mobility and the resistivity value of thin-film material be respectively 2.1 ×
1017cm-3、 0.1cm2V-1s-1With 1.1 × 103Ω cm (referring to comparative example: the testing result of embodiment 2).
Embodiment 2
Illustrate: the embodiment is comparative example, and target product is pure MoS2Thin-film material, without intermediate Ag intercalation.
The preparation method is as follows:
The first step, silicon substrate surface cleaning step
The intrinsic non-conductive type Si monocrystal chip of insulation is chosen, is successively cleaned by ultrasonic in alcohol, acetone and deionized water
180s；
It takes out and is dried up with drying nitrogen；
Second step, bottom MoS2Thin-film surface deposition step
Si monocrystal chip substrate after cleaning is packed into pallet, is put into vacuum chamber, and vacuum chamber is taken out as high vacuum, in argon
Under compression ring border, the temperature of Si monocrystal chip is adjusted to 200 DEG C of the first temperature, ar pressure is adjusted to first pressure 3Pa, using direct current
Magnetron sputtering technique utilizes the ion bombardment MoS ionized out under the conditions of constant 30W sputtering power2Ceramic target, in institute
On the upper surface for stating Si substrate, the MoS that a layer thickness is 100nm is deposited2Film layer；To obtain the final product.
Properties of product testing result:
Through detecting, under the conditions of room temperature (20-25 DEG C), obtained MoS2Electron carrier density, the electricity of thin-film material
Transport factor and resistivity value are respectively 2.1 × 1017cm-3、0.1cm2V-1s-1With 1.1 × 103Ωcm。
Embodiment 3
Only in the third step, by adjusting sputtering time, intercalation thickness among Ag is adjusted to 3nm；Remaining, with implementation
Example 1.
Properties of product testing result:
Through detecting, under the conditions of room temperature (20-25 DEG C), obtained MoS2/Ag/MoS2The electronic carrier of thin-film material
Concentration, electron mobility and resistivity value are respectively 1.8 × 1020cm-3、1.2cm2V-1s-1With 9.8 Ω cm.
Embodiment 4
Only in the third step, by adjusting sputtering time, intercalation thickness among Ag is adjusted to 8nm；Remaining, with implementation
Example 1.
Properties of product testing result:
Through detecting, under the conditions of room temperature (20-25 DEG C), obtained MoS2/Ag/MoS2The electronics of semiconductor film material
Carrier concentration, electron mobility and resistivity value are respectively 8.8 × 1021cm-3、2.3cm2V-1s-1With 1.1 Ω cm.
Embodiment 5
Only in the third step, by adjusting sputtering time, intercalation thickness among Ag is adjusted to 10nm；Remaining, with real
Apply example 1.
Properties of product testing result:
Through detecting, under the conditions of room temperature (20-25 DEG C), obtained MoS2/Ag/MoS2The electronics of semiconductor film material
Carrier concentration, electron mobility and resistivity value are respectively 6.0 × 1022cm-3、5.7cm2V-1s-1With 0.12 Ω cm.
Technical characterstic for a better understanding of the invention, with reference to the accompanying drawing, to the performance of product obtained by the present invention
Detection method and testing result are described in detail.
Fig. 1 is MoS of the invention2/Ag/MoS2The structural schematic diagram of semiconductor film material.
As shown in Figure 1, MoS of the invention2/Ag/MoS2Semiconductor film material is layer structure, from top to bottom successively
Including top layer MoS2Film layer, Ag metal layer, bottom MoS2Film layer and Si substrate；Wherein:
Above-mentioned Si substrate is the intrinsic non-conductive monocrystal material of insulation, and single-sided polishing, burnishing surface is upper surface；
Above-mentioned MoS2Film layer, purity 99.9%；
Above-mentioned Ag metal layer, purity 99.99%；
Above-mentioned top layer MoS2Film layer, Ag metal layer, bottom MoS2The thickness of film layer be respectively 50nm, 3-10nm and
50nm；
Above-mentioned bottom MoS2Film layer is deposited on the above-mentioned upper surface Si using DC magnetron sputtering method；
Above-mentioned Ag metal layer is to be deposited on above-mentioned MoS using DC magnetron sputtering method2On film layer；
Above-mentioned top layer MoS2Film layer is deposited on above-mentioned Ag metal layer using DC magnetron sputtering method.
Fig. 2 is MoS obtained by embodiment 12/Ag/MoS2The Raman spectrum analysis figure of semiconductor film material.
As shown in Fig. 2, 382cm-1And 407cm-1Respectively MoS2The typical in plane vibration mode (E of film1 2g) and face outside shake
Dynamic model formula (A1g).Show that obtained film material is MoS2。
Fig. 3 is MoS of the invention2/Ag/MoS2The electron carrier density and mobility value of semiconductor film material are with Ag
The variation rule curve figure of layer thickness variation.
From figure 3, it can be seen that with the increase of intercalation thickness among Ag, MoS2/Ag/MoS2The electronics of thin-film material carries
It flows sub- concentration and mobility value is gradually increased.As it can be seen that with the increase of thickness, the uniform continuity enhancing of intercalation among Ag is
Ag layers internal to MoS2Injected electrons number and effect enhancing in film, so as to cause the carrier concentration and electricity of entire film
Transport factor significantly improves.
Fig. 4 is MoS of the invention2/Ag/MoS2The resistivity value of semiconductor film material with Ag layer thickness variation variation
Law curve figure.
As shown in figure 4, the pure MoS without Ag metal intercalation (when corresponding in figure with a thickness of 0)2The electronics of thin-film material carries
Flowing sub- concentration, electron mobility and resistivity value is respectively 2.1 × 1017cm-3、0.1cm2V-1s-1With 1.1 × 103Ωcm。
Figure 4, it is seen that with the increase of intercalation thickness among Ag, MoS2/Ag/MoS2The resistivity of thin-film material
Value is gradually reduced.
Under the conditions of room temperature (20-25 DEG C), the obtained MoS with 10nm Ag metal intercalation2/Ag/MoS2Semiconductor
Electron carrier density, electron mobility and the resistivity value of thin-film material are respectively 8.3 × 1022cm-3、8.5cm2V-1s-1With
5.7×10-2Ωcm。
It is more than 5 orders of magnitude that data comparison, which can be seen that carrier concentration increase rate, and electron mobility increase rate is super
1 order of magnitude is crossed, and it is more than 4 orders of magnitude that resistivity value, which reduces amplitude, electric conductivity improvement amplitude is huge, effect is very aobvious
It writes.
Claims (1)
1. a kind of MoS2/Ag/MoS2The preparation method of semiconductor film material, which comprises the following steps:
The first step, silicon substrate surface cleaning step
The intrinsic non-conductive type Si monocrystal chip of insulation is chosen, is successively cleaned by ultrasonic 180s in alcohol, acetone and deionized water；
It takes out and is dried up with drying nitrogen；
Second step, bottom MoS2Thin-film surface deposition step
Si monocrystal chip substrate after cleaning is packed into pallet, is put into vacuum chamber, and vacuum chamber is taken out as high vacuum, in argon gas ring
Under border, the temperature of Si monocrystal chip is adjusted to the first temperature, ar pressure is adjusted to first pressure, using magnetically controlled DC sputtering skill
Art utilizes the ion bombardment MoS ionized out under the conditions of constant 30W sputtering power2Ceramic target, in the Si substrate
On upper surface, one layer of MoS is deposited2Film layer；
Third step, Ag layer on surface of metal deposition step
By the pallet-changing equipped with sample to the surface of Ag metal targets；
The temperature of Si monocrystal chip is adjusted to second temperature, Ar air pressure is adjusted to second pressure, using magnetically controlled DC sputtering technology,
Under the conditions of constant 30W sputtering power, using the ion bombardment Ag metal targets ionized out, in above-mentioned bottom MoS2Film layer
On surface, redeposited one layer of Ag metal layer；
4th step, top layer MoS2Thin-film surface deposition step
Pallet equipped with sample is replaced again to MoS2The surface of ceramic target；
The temperature of Si monocrystal chip is adjusted to third temperature, Ar air pressure is adjusted to third pressure, using magnetically controlled DC sputtering technology,
Under the conditions of constant 30W sputtering power, the ion bombardment MoS ionized out is utilized2Ceramic target, on the surface of above-mentioned Ag metal layer
On, one layer of MoS of redeposition2Film layer to get；
In above-mentioned steps, the purity of the argon gas is 99.999% or more；
The nitrogen refers to that purity is 99.95% or more drying nitrogen；
The MoS2Ceramic target, purity 99.9%；
The Ag metal targets, purity 99.99%；
The MoS2The target-substrate distance of the target-substrate distance of target and the Ag target is 50mm；
First temperature is 20-400 DEG C, and the first pressure is 1-10Pa；
The second temperature is 20-30 DEG C, and the second pressure is 1-5Pa；
The third temperature is 20-400 DEG C, and the third pressure is 1-10Pa.
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| CN111455318A (en) * | 2020-06-01 | 2020-07-28 | 中国科学院兰州化学物理研究所 | Molybdenum nitride/molybdenum disulfide/silver ternary composite high-temperature solid lubricating film and preparation method thereof |
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