CN112216751A - GaSe/MoS2Method for preparing heterojunction - Google Patents

GaSe/MoS2Method for preparing heterojunction Download PDF

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CN112216751A
CN112216751A CN201910624743.9A CN201910624743A CN112216751A CN 112216751 A CN112216751 A CN 112216751A CN 201910624743 A CN201910624743 A CN 201910624743A CN 112216751 A CN112216751 A CN 112216751A
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heterojunction
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何鹏
张墅野
胡平安
林铁松
张彦鑫
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Harbin Institute of Technology
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Abstract

The invention discloses GaSe/MoS2A preparation method of heterojunction belongs to the technical field of photoelectric devices. The invention aims to solve the problem of the existing preparation of GaSe/MoS2Hetero-junction MoS2Irregular shape of the nano-sheet, uncontrollable layer number and difficult accurate control. The invention adopts a chemical vapor deposition method to obtain single-layer MoS2Then, mechanically stripped GaSe and MoS are transferred by using PDMS as a transfer medium and using a transfer platform2Combined to obtain GaSe/MoS2A heterojunction. GaSe/MoS prepared by the invention2The heterojunction has good photoelectric propertiesCore components of a multi-optoelectronic device, such as ultraviolet photodetectors and the like.

Description

GaSe/MoS2Method for preparing heterojunction
Technical Field
The inventionBelongs to the technical field of photoelectric devices; in particular to GaSe/MoS2A heterojunction and a method of fabricating the same.
Background
In the semiconductor material, a homojunction can be formed by doping different semiconductor materials on two sides, and a heterojunction can be formed by depositing two or more layers of different semiconductor material films on the same substrate in sequence. Heterojunctions can be divided into two broad categories depending on the conductivity type of the semiconductor material forming the heterojunction. The conduction types of two sides of one type of heterojunction are the same, and the heterojunction is called as a homotype heterojunction; another type of heterojunction, which consists of semiconductor single-crystal materials of different conductivity types, i.e., P-type material and N-type material, is called an inversion heterojunction.
Preparation of GaSe/MoS2The heterojunction is essentially divided into two steps, the first being a single layer MoS2Depositing on a substrate; the second step is to mix GaSe and MoS2And (4) combining.
For the first step, the common preparation methods at present mainly comprise a mechanical stripping method, a lithium ion intercalation stripping method, a liquid phase stripping method and a laser thinning method. MoS prepared by these methods2The nano-sheets have irregular shapes and uncontrollable layer numbers.
For the second step, the common method today is to peel off a few layers of GaSe with Scotch tape and coat it with many single layers of MoS2The substrate is directly bonded, but the randomness of the method is large and the accurate control is difficult.
Disclosure of Invention
The invention aims to solve the problem of the existing preparation of GaSe/MoS2Hetero-junction MoS2The technical problems that the nano-sheets have irregular shapes, the layer number is not controllable and the precise control is difficult are solved, and the GaSe/MoS is provided2A method for fabricating a heterojunction.
GaSe/MoS in the invention2The preparation method of the heterojunction is completed by the following steps:
step one, MoO is used3And sulfur powder as raw material, and depositing single-layer MoS on the substrate by adopting double-temperature-zone chemical vapor deposition in nitrogen atmosphere2；
Step two, repeatedly sticking and tearing GaSe blocks by using a Scotch adhesive tape and sticking the GaSe blocks on a transfer medium, selecting GaSe with the size of 20 +/-5 mu m and the thickness of 20 nm-40 nm, cutting corresponding transfer medium areas together, and aligning the GaSe blocks to MoS on the substrate by using a transfer platform2GaSe is made to be in contact with the single layer MoS on the substrate by slow pressing2Tightly attaching, keeping for a period of time, and slowly lifting the transfer medium;
step three, repeating the step two until the MoS on the surface of the silicon wafer2Are all covered with GaSe, namely the GaSe/MoS is completed2And (4) preparing a heterojunction.
And further limiting, the substrate in the step one is a silicon wafer or a silicon wafer with an oxidation layer with the thickness of 285nm, and the silicon wafer with the oxidation layer is prepared by heating the silicon wafer substrate by using a piranha solution to 83 ℃ and boiling for 30 minutes to enable the surface of the silicon wafer to be highly hydrophilic with a warp base. Then, sequentially carrying out ultrasonic oscillation on acetone, isopropanol and ethanol for 10 minutes to completely remove surface organic matters, and finally storing in ethanol for later use, wherein the piranha solution is a mixture of concentrated sulfuric acid and 30% (mass) of hydrogen peroxide in a volume ratio of 3: 2.
Further limiting, in the second step, Polydimethylsiloxane (PDMS) is used as a transfer medium.
Further, the dual-temperature zone chemical vapor deposition in the first step is carried out according to the following steps:
step 1, MoO3Placing the powder at one end of the quartz plate, placing the substrate at the other end of the quartz plate, placing in the high temperature region of a tube furnace, and placing MoO on the quartz plate3The end is placed close to the low-temperature area;
step 2, uniformly placing the sulfur powder in a porcelain boat, then placing the porcelain boat in a push-pull rod, then placing the porcelain boat in a position 12 +/-2 cm away from a low-temperature area in a tubular furnace, and sealing;
and 3, introducing argon to remove air in the tube furnace, simultaneously heating the high-temperature area and the low-temperature area, pushing the porcelain boat filled with the sulfur powder into the low-temperature area through a push-pull rod when the temperature of the high-temperature area and the low-temperature area reaches a set temperature, depositing (as shown in figure 1), withdrawing the porcelain boat filled with the sulfur powder from the low-temperature area through the push-pull rod when the temperature of the porcelain boat is reduced after the reaction is finished, slowly cooling the porcelain boat to room temperature along with the furnace, and taking out the porcelain boat and the growth substrate.
Further limited, MoO in step 13The powder dosage is 40mg, the sulfur powder dosage in the step 2 is 1g, and the mass ratio can be controlled so that MoO can be added3Fully vulcanized to obtain MoS2And the use of sulfur powder can be saved.
Further limited, MoO in step 13The distance between the substrate and the substrate is 3 cm-5 cm.
Further limiting, in the step 3, the set temperature of the high temperature region is 670 ℃, the set temperature of the low temperature region is 250 ℃, and the heating rates of the high temperature region and the low temperature region are both set to be 10 ℃/min-12 ℃/min.
Further defined, the flow rate of nitrogen gas during deposition in step 3 was controlled at 14 sccm.
Further limiting, the deposition time in the step 3 is 8 min-12 min.
The invention realizes MoS by controlling the reaction time, the reaction temperature and the gas flow of the chemical vapor deposition2And (4) controllable growth.
GaSe/MoS is obtained by the method2A vertical heterojunction.
Compared with MoS2Two-dimensional device, GaSe/MoS of the invention2The overall photoresponse value of the photoelectric detector is improved, and the ultraviolet (300-400 nm) effect is obvious. Wherein the optical power density is 0.008mW/cm2The optical response value of the heterojunction device is as high as 52.2A/W, and the detection value is as high as 1 multiplied by 1013Jones. In addition, the stability and the repeatability of the device are better, the response speed is greatly improved, and the light-dark corresponding ratio can reach 5.75.
The invention GaSe/MoS2The photovoltaic device has a rectification effect, has a certain photovoltaic effect under the irradiation of light (especially light in an ultraviolet band of 300-400 nm), has a filling factor of about 0.25 basically, and has an optical power density of 1.215mW/cm2Under the illumination of 350nm wavelength, the energy conversion efficiency reaches 0.0033 percent.
GaSe/MoS prepared by the method of the invention2The heterojunction has good photoelectric performance and is a core component of a plurality of photoelectric devicesSuch as a uv photodetector or the like.
Drawings
FIG. 1 is a schematic view of chemical vapor deposition;
FIG. 2 is a MoS2Atomic force characterization and height profile, a) AFM characterization, b) height profile;
FIG. 3 is GaSe/MoS2Heterojunction Ophotograph 1-Single layer MoS2，2——GaSe；
FIG. 4 is GaSe/MoS2Heterojunction and single layer MoS2Ultraviolet absorption spectrum of (1);
FIG. 5 is GaSe/MoS2A model diagram of a photoelectric detector;
FIG. 6 shows MoS under 300-700nm wavelength light irradiation2Device and GaSe/MoS2Photodetector performance, a) photocurrent, b) photoresponse value, c) photodetection value.
Detailed Description
Example 1: GaSe/MoS in this example2The preparation method of the heterojunction is completed by the following steps:
step one, MoO is used3And sulfur powder as raw material, and depositing single-layer MoS on the substrate by adopting double-temperature-zone chemical vapor deposition in nitrogen atmosphere2；
The double-temperature-zone chemical vapor deposition in the first step is carried out according to the following steps:
step 1, heating a silicon wafer substrate to 83 ℃ by using a piranha solution, boiling for 30 minutes, and enabling the surface of the silicon wafer substrate to be highly hydrophilic due to the fact that the piranha solution is provided with channels. Then sequentially ultrasonically oscillating for 10 minutes by using acetone, isopropanol and ethanol to completely remove organic matters on the surface, and finally storing in ethanol for later use; a silicon wafer with an oxide layer with the thickness of 285nm as a substrate, wherein the piranha solution is a mixture of concentrated sulfuric acid and 30 percent (mass) of hydrogen peroxide in a volume ratio of 3:2,
mixing 40mgMoO3Placing the powder on one end of a quartz piece with a length of 8cm and a width of 2cm, placing the other end of the quartz piece on the substrate, and MoO3The right side is 4cm away from the left side of the substrate, then the substrate is placed in a high-temperature zone of a tube furnace, and MoO is placed on a quartz plate3The end is placed close to the low-temperature area;
step 2, uniformly placing 1g of sulfur powder in a porcelain boat, then placing the porcelain boat in a push-pull rod, then placing the porcelain boat in a position 12cm away from a low-temperature area in a tubular furnace, and sealing;
step 3, introducing argon of 200sccm for 20 minutes to discharge the air in the tubular furnace as far as possible, controlling the flow of the nitrogen at 14sccm, simultaneously heating the high-temperature area and the low-temperature area, setting the heating speed at 10 ℃/min, pushing the porcelain boat filled with the sulfur powder into the low-temperature area through a push-pull rod when the set temperature is reached, depositing (shown in figure 1), withdrawing the porcelain boat filled with the sulfur powder from the low-temperature area through the push-pull rod when the reaction is finished and the temperature is reduced, slowly cooling the porcelain boat to room temperature along with the furnace, and taking out the porcelain boat and the growth substrate, wherein the set temperature of the high-temperature area is 670 ℃, and the set temperature of the low-temperature area is 250 ℃;
step two, repeatedly sticking and tearing GaSe blocks by using a Scotch adhesive tape, sticking the GaSe blocks on transfer medium Polydimethylsiloxane (PDMS), selecting GaSe with the size of 20 +/-5 mu m and the thickness of 20 nm-40 nm, cutting corresponding PDMS areas together, and aligning the GaSe blocks to MoS on the substrate by using a transfer platform2GaSe is made to be in contact with the single layer MoS on the substrate by slow pressing2Tightly fitting, keeping for a period of time, and slowly lifting the transfer medium (as shown in fig. 3);
step three, repeating the step two until the MoS on the surface of the silicon wafer2Are all covered with GaSe, namely the GaSe/MoS is completed2And (4) preparing a heterojunction.
At high temperatures in enclosed spaces, MoO3Will react with sulfur vapor as follows; first stage, MoO3Is partially reduced into MoO by sulfur evaporation3-x(ii) a Second pole stage, MoO3-xWill be reduced by sulfur steam again to obtain MoS2In the invention, before the temperature reaches the reaction temperature of 670 ℃, MoO3And a small amount of sulfur vapor partially reduced MoO3-xAnd adsorbing diffusion nuclei on the surface of the substrate. After the reaction temperature reaches 670 ℃, sulfur powder is pushed in immediately, and MoS obtained through reaction2Lateral growth in the plane will occur.
For the MoS obtained in the step one2AFM characterization was performed and growth was performedThe thickness of the material is shown in FIG. 2a), and from the atomic force height chart in FIG. 2b), the surface height of the triangular topography is approximately 0.655nm higher than the substrate, which is exactly the same as MoS2The thicknesses of the single layers are identical, and in addition, the surface color of the triangular morphology is uniform and the roughness is small. The MoS with triangular morphology obtained2Has a single-layer structure and uniform growth.
Transfer of few-layer GaSe to single-layer MoS by mechanical stripping2Preparing GaSe/MoS on the surface2A vertical heterojunction.
In the preparation of GaSe/MoS2After heterojunction, the absorption capacity of the material under the irradiation of light with different wavelengths is tested, the Scotch adhesive tape is used for transferring the sheet layers with the bulk GaSe as much as possible onto PDMS, and the PDMS with more GaSe adhered thereon is attached to a substrate with MoS2Testing the ultraviolet absorption spectrum of the film on a quartz plate and comparing the film with MoS2The results of the films were compared. As shown in FIG. 4, the GaSe-coated MoS can still be seen in the above figure2Light absorption vs. MoS2The film is slightly improved, and the absorption capacity in an ultraviolet band is obviously improved.
In MoS2The electrodes are lapped by photolithography and vapor deposition, as shown in fig. 5. Exploring GaSe/MoS simultaneously2Photoelectric performance of heterojunction device compared with MoS2Variations of two-dimensional devices.
To accurately compare GaSe/MoS2The response condition of the photoelectric detector under different wavelengths is convenient to be matched with the single-layer MoS2The photo detectors compare the photocurrent and response values of the output voltage at 1V with the detection values, and the result is shown in fig. 6. As can be seen from FIG. 6, the GaSe/MoS values are either photocurrent, photoresponse or probe values2Photodetector compared to single layer MoS2The photoelectric detectors are improved to a certain extent, and are only improved a little in the range of 400-700 nm, and are improved to a larger extent in the wavelength range of 300-400 nm. Wherein, under the excitation light of 300nm, GaSe/MoS2The optical response value of the photoelectric detector reaches 42.6A/W, and the optical detection value reachesTo 8.17X 1012Jones, is MoS 23 times that of the photodetector. The improvement of photoelectric performance benefits from MoS2The composite material is compounded with a GaSe energy band structure, so that electrons and holes can be better separated, and effective recombination of electron and hole pairs can be prevented, so that the number of current carriers in a system is increased, and the photocurrent is effectively increased; on the other hand, the absorption characteristic of GaSe to ultraviolet band light enhances GaSe/MoS2The response of the photoelectric detector is within the range of 300-400 nm.
In addition, the light-dark corresponding ratio can reach 5.75 in a long-time corresponding process, and is higher than that of single-layer MoS2The photodetector has improved 72.15%.

Claims (10)

1.GaSe/MoS2A method for the preparation of a heterojunction, characterized in that the preparation method is completed by the following steps:
step one, MoO is used3And sulfur powder as raw material, and depositing single-layer MoS on the substrate by adopting double-temperature-zone chemical vapor deposition in nitrogen atmosphere2；
Step two, repeatedly sticking and tearing GaSe blocks by using a Scotch adhesive tape and sticking the GaSe blocks on a transfer medium, selecting GaSe with the size of 20 +/-5 mu m and the thickness of 20 nm-40 nm, cutting corresponding transfer medium areas together, and aligning the GaSe blocks to MoS on the substrate by using a transfer platform2GaSe is made to be in contact with the single layer MoS on the substrate by slow pressing2Tightly attaching, keeping for a period of time, and slowly lifting the transfer medium;
step three, repeating the step two until the MoS on the surface of the silicon wafer2Are all covered with GaSe, namely the GaSe/MoS is completed2And (4) preparing a heterojunction.
2. The GaSe/MoS of claim 12The preparation method of the heterojunction is characterized in that the substrate in the step one is a silicon wafer.
3. The GaSe/MoS of claim 12A method for preparing a heterojunction, characterized by the steps ofAnd step one, the substrate is a silicon wafer with an oxide layer with the thickness of 285nm, namely, the piranha solution is adopted to heat the substrate of the silicon wafer to 83 ℃ and boil for 30 minutes, so that the surface of the substrate is highly hydrophilic due to the fact that the piranha solution is provided with groups. Then, sequentially carrying out ultrasonic oscillation on acetone, isopropanol and ethanol for 10 minutes to completely remove surface organic matters, and finally storing in ethanol for later use, wherein the piranha solution is a mixture of concentrated sulfuric acid and 30% (mass) of hydrogen peroxide in a volume ratio of 3: 2.
4. The GaSe/MoS of claim 12The preparation method of the heterojunction is characterized in that Polydimethylsiloxane (PDMS) is used as a transfer medium in the second step.
5. GaSe/MoS according to any of claims 1 to 32The preparation method of the heterojunction is characterized in that the chemical vapor deposition of the double-temperature area in the step one is carried out according to the following steps:
step 1, MoO3Placing the powder at one end of the quartz plate, placing the substrate at the other end of the quartz plate, placing in the high temperature region of a tube furnace, and placing MoO on the quartz plate3The end is placed close to the low-temperature area;
step 2, uniformly placing the sulfur powder in a porcelain boat, then placing the porcelain boat in a push-pull rod, then placing the porcelain boat in a position 12 +/-2 cm away from a low-temperature area in a tubular furnace, and sealing;
and 3, introducing argon to remove air in the tube furnace, simultaneously heating the high-temperature area and the low-temperature area, pushing the porcelain boat filled with the sulfur powder into the low-temperature area through a push-pull rod when the temperature of the high-temperature area and the low-temperature area reaches a set temperature, depositing, withdrawing the porcelain boat filled with the sulfur powder from the low-temperature area through the push-pull rod when the temperature of the porcelain boat is reduced after the reaction is finished, slowly cooling the porcelain boat to room temperature along with the furnace, and taking out the porcelain boat and the growth substrate.
6. The GaSe/MoS of claim 42A preparation method of the heterojunction is characterized in that MoO in step 13The amount of the powder was 40mg, and the amount of the sulfur powder in step 2 was 1 g.
7. The GaSe/MoS of claim 42A preparation method of the heterojunction is characterized in that MoO in step 13The distance between the substrate and the substrate is 3 cm-5 cm.
8. The GaSe/MoS of claim 42The preparation method of the heterojunction is characterized in that in the step 3, the set temperature of the high-temperature region is 670 ℃, the set temperature of the low-temperature region is 250 ℃, and the heating rates of the high-temperature region and the low-temperature region are both set to be 10-12 ℃/min.
9. The GaSe/MoS of claim 42The preparation method of the heterojunction is characterized in that the flow rate of nitrogen gas in the deposition process in the step 3 is controlled to be 14 sccm.
10. The GaSe/MoS of claim 42The preparation method of the heterojunction is characterized in that the deposition time in the step 3 is 8-12 min.
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CN113035965A (en) * 2021-03-04 2021-06-25 电子科技大学 Preparation method of flexible photoelectric detector based on selenide/sulfide heterojunction
CN113097321A (en) * 2021-03-31 2021-07-09 桂林理工大学 MoS2/SnSe2/H-TiO2Preparation method of heterojunction photoelectric detector
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Application publication date: 20210112