CN113097321A - MoS2/SnSe2/H-TiO2Preparation method of heterojunction photoelectric detector - Google Patents

MoS2/SnSe2/H-TiO2Preparation method of heterojunction photoelectric detector Download PDF

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CN113097321A
CN113097321A CN202110345225.0A CN202110345225A CN113097321A CN 113097321 A CN113097321 A CN 113097321A CN 202110345225 A CN202110345225 A CN 202110345225A CN 113097321 A CN113097321 A CN 113097321A
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吕慧丹
王子良
刘勇平
班如静
王璇
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Guilin University of Technology
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Abstract

The invention provides a MoS2/SnSe2/H‑TiO2The preparation method of the heterojunction photoelectric detection device comprises the following steps: (1) preparation of TiO using anodic oxidation2A nanotube; (2) growing SnSe by using double-temperature-zone vacuum atmosphere tube furnace2Nanosheet to give SnSe2/H‑TiO2A heterojunction; (3) the obtained SnSe2/H‑TiO2The heterojunction is placed in a sputtering vacuum chamber and a target MoS is used2(purity 99.99%) under argon atmosphere at room temperature, adopting magnetron sputtering method to perform reaction on SnSe2/H‑TiO2Composite MoS on heterojunction2To obtain MoS2/SnSe2/H‑TiO2A heterojunction. MoS obtained by the method2/SnSe2/H‑TiO2The heterojunction photoelectric detector has larger optical response value and detectivity.

Description

MoS2/SnSe2/H-TiO2Preparation method of heterojunction photoelectric detector
Technical Field
The invention belongs to the technical field of heterojunction photoelectric detectors, and particularly relates to a MoS2/SnSe2/H-TiO2A heterojunction photoelectric detector and a preparation method thereof.
Background
The principle of the photoelectric detector is to convert the physical characteristics of the detected object into optical signals, detect the characteristics and changes of the optical signals, and then obtain various items of information of the detected object by processing the optical signal data. The key components of many devices used in our daily lives are made up of it. Silicon photodetectors are the most commonly used in life, with device miniaturization and scalability, but they suffer from reduced efficiency due to the limitations of silicon as a light absorbing material (the indirect bandgap of about 1.1eV limits absorption in the visible and near infrared portions of the electromagnetic spectrum), so that there is a need to develop novel nanoscale semiconductor materials to overcome the limitations of silicon photodetectors.
One-dimensional nanowire (tube)/two-dimensional heterostructure arrays have been widely studied and have made great progress in various fields such as photodetectors, catalysis and gas sensors. Due to the light trapping effect of the one-dimensional structure, the one-dimensional nanowire (tube) can effectively convert absorbed photons into electron-hole pairs, and the electron acceptor and the transporter in the one-dimensional nanowire (tube)/two-dimensional heterostructure can help the electron-hole pair separation to improve the response rate of the photoelectric device. The two-dimensional material can be subjected to band gap tuning through size change, intercalation, heterostructure, alloying and optical tuning, which are important for improving the performance of the array device and obtaining the optimal performance. Two-dimensional SnSe2、MoS2The nano material has large surface area and larger sensitivity to light, and can generate more free electrons under the combined action of illumination and bias voltage. TiO 22The detectable wavelength range of the nanotube ultraviolet detector is narrow, and MoS is prepared for increasing the detection range2/SnSe2/TiO2Heterojunction andas ultraviolet-visible photodetector material.
Disclosure of Invention
The invention aims to provide a MoS2/SnSe2/H-TiO2The preparation method of the heterojunction photoelectric detector solves the defects of low light responsivity and narrow detection range of the conventional photoelectric detector.
The purpose of the invention is realized by the following technical scheme:
MoS2/SnSe2/H-TiO2The preparation method of the heterojunction photoelectric detector comprises the following steps:
(1) preparing TiO by using titanium sheet as substrate and adopting anodic oxidation method2A nanotube;
(2) growing SnSe by using double-temperature-zone vacuum atmosphere tube furnace2Nanosheet: respectively using selenium powder and SnCl4·5H2O is taken as a Se source and a Sn source, and is added into TiO under the environment of mixed gas of argon and hydrogen2Growing SnSe on nanotubes2Nanosheet, and SnSe is obtained after the temperature of the tube furnace is reduced to room temperature2/H-TiO2A heterojunction;
(3) the obtained SnSe2/H-TiO2The heterojunction is placed in a sputtering vacuum chamber and a target MoS is used2(purity 99.99%) under the condition of room temperature and argon atmosphere, adopting magnetron sputtering method to make SnSe2/H-TiO2Composite MoS on heterojunction2To obtain MoS2/SnSe2/H-TiO2A heterojunction.
The method of the invention oxidizes the titanium sheet into TiO by an anodic oxidation method2Nanotube arrays, then in TiO in a dual temperature zone tube furnace2SnSe growth on nanotube array substrate material2Nanosheet, and finally performing magnetron sputtering on SnSe2/H-TiO2Composite MoS on heterojunction2Obtaining new MoS2/SnSe2/H-TiO2A heterojunction material.
The preparation method of the invention can be further improved as follows:
selenium powder and SnCl in step (2)4·5H2The mass ratio of O is 0.3-0.5: 0.2-0.4.
SnSe is carried out in the step (2) in a double-temperature-zone vacuum atmosphere tube furnace2The growth of the nano-sheets comprises the following specific operations: placing selenium powder into a quartz boat positioned in an upstream central heating zone, and adding SnCl4·5H2The O solid is placed in another quartz boat positioned in a downstream central heating area of the double-temperature-area tube furnace, and the quartz boat is placed at the upper end of the downstream heating area and is 5cm away from the downstream heating center; TiO obtained in the step (1)2The nanotubes were placed at the end of the downstream zone, 7cm from the downstream heating center.
Further, the upstream of the dual-temperature-zone vacuum atmosphere tube furnace is heated to the temperature of 300-500 ℃, the heating rate is 6-8 ℃/min, the downstream is heated to the temperature of 400-600 ℃, the two sides are simultaneously heated to the set temperature, and the heat preservation time is 10-30 min.
Further, the operation of introducing argon to remove air is as follows: before the heating process, introducing argon for 30 min; the argon flow of the gas path system in the temperature rise process is set to be 80s.c.c.m, the mixed gas of argon and hydrogen is introduced in the heat preservation stage, the argon flow is switched to be 60s.c.c.m, the hydrogen flow is switched to be 20s.c.c.m, only argon is introduced in the temperature reduction stage, and the flow is 80s.c.c.m.
In the step (3), the magnetron sputtering power is 300W, and the pressure is 1 Pa.
Compared with the prior art, the invention has the following beneficial effects:
(1) MoS of the invention2/SnSe2/H-TiO2Method for preparing heterojunction photoelectric detector on TiO2Chemical vapor deposition of SnSe on nanotube arrays2Nanosheet, and then SnSe by magnetron sputtering method2/H-TiO2Heterojunction surface recombination MoS2Obtaining MoS2/SnSe2/H-TiO2The heterojunction material has higher photoelectric response performance and enlarges the detection range of the device,
(2) the preparation method is simple, low in cost and easy to control reaction conditions.
Drawings
FIG. 1 shows the MoS obtained in example 4 of the present invention2/SnSe2/H-TiO2XRD pattern of heterojunction photodetector.
FIG. 2 shows the MoS obtained in example 4 of the present invention2/SnSe2/H-TiO2SEM image of heterojunction photodetector.
FIG. 3 shows the MoS obtained in example 4 of the present invention2/SnSe2/H-TiO2Ultraviolet-visible absorption spectrum of heterojunction photodetectors.
FIG. 4 shows the MoS obtained in example 4 of the present invention2/SnSe2/H-TiO2I-V plot of heterojunction photodetectors.
FIG. 5 shows the MoS obtained in example 4 of the present invention2/SnSe2/H-TiO2I-T plot of heterojunction photodetectors.
Detailed Description
The present invention is further described below in conjunction with specific examples to better understand and implement the technical solutions of the present invention for those skilled in the art.
Example 1
MoS2/SnSe2/H-TiO2The preparation method of the heterojunction photoelectric detector comprises the following steps:
(1) preparation of TiO by anodic oxidation2An array of nanotubes.
(2) The samples were synthesized using a dual-temperature zone vacuum atmosphere tube furnace. During synthesis, 0.4g of selenium powder was placed in a quartz boat located in the upstream central heating zone. 0.2g of SnCl4·5H2The O solid is placed in another quartz boat positioned in a central heating zone at the downstream of the two-temperature zone tube furnace, and the quartz boat is placed at the upper end of the downstream heating zone and is 5cm away from the downstream heating center. TiO obtained in the step (1)2The nanotubes were placed at the end of the downstream zone, 7cm from the downstream heating center. The CVD system was vented with high purity argon (99.99%) for 30min to remove air and reduce contamination of the experiment with other gases after the sample was placed in the tube furnace and before the heating process. The downstream central heating zone was then heated to a temperature of 450 c at atmospheric pressure while the upstream central heating zone was heated to a temperature of 350 c. The gas path system is set to be argon gas for 80s.c.c.m. When the temperature reaches a set value, the gas circuit system is switched to a mixed gas containing 60s.c.c.m. argon and 20s.c.c.m. hydrogen. The entire hydrogen passage time lasted 15 min. Because the flow velocity of the gas flow has great influence on CVD, the argon gas flow is rapidly converted into 80s.c.c.m. after the introduction of the hydrogen is finished so as to ensure the stability of the flow velocity of the whole gas flow, thereby ensuring the stability of SnSe2And (4) growing and depositing the nanosheets. Obtaining SnSe after the temperature of the tube furnace is reduced to room temperature2/H-TiO2A heterojunction.
(3) The obtained SnSe2/H-TiO2The heterojunction is placed in a sputtering vacuum chamber and a target MoS is used2(purity 99.99%) under room temperature, power 300W, pressure 1Pa, sputtering gas atmosphere argon sputtering for 15min, obtained MoS2/SnSe2/H-TiO2A heterojunction.
Example 2
MoS2/SnSe2/H-TiO2The preparation method of the heterojunction photoelectric detector comprises the following steps:
(1) preparation of TiO by anodic oxidation2An array of nanotubes.
(2) The samples were synthesized using a dual temperature controlled vacuum atmosphere tube furnace. During the synthesis, 2.0g of NaH2PO2·H2O and 20mg of sulfur powder were placed in the heating zone upstream of the tube furnace. Placing the tungsten trioxide nanosheet array material obtained in the step (1) in a central heating zone at the downstream of a two-temperature-zone tubular furnace, and ventilating the tubular furnace with high-purity argon (99.99%) for 30min to remove air and reduce the pollution of other gases to the experiment before the heating process. Then, the downstream central heating zone was heated to 550 ℃ at a rate of 5 ℃/min at atmospheric pressure while the upstream central heating zone was heated to 350 ℃, and the gas circuit system was set to 80s.c.c.m. argon. When the temperature reaches a set value, the gas circuit system is switched to a mixed gas containing 60s.c.c.m. argon and 20s.c.c.m. hydrogen. The entire hydrogen passage time lasted 15 min. Because the flow velocity of the gas flow has great influence on CVD, the argon gas flow is rapidly converted into 80s.c.c.m. after the introduction of the hydrogen is finished so as to ensure the stability of the flow velocity of the whole gas flow, thereby ensuring the stability of SnSe2Growth of nanosheets andand (6) depositing. Obtaining SnSe after the temperature of the tube furnace is reduced to room temperature2/H-TiO2A heterojunction.
(3) The obtained SnSe2/H-TiO2The heterojunction is placed in a sputtering vacuum chamber and a target MoS is used2(purity 99.99%) under room temperature, power 300W, pressure 1Pa, sputtering gas atmosphere argon sputtering for 20min, obtained MoS2/SnSe2/H-TiO2A heterojunction.
Example 3
MoS2/SnSe2/H-TiO2The preparation method of the heterojunction photoelectric detector comprises the following steps:
(1) preparation of TiO by anodic oxidation2An array of nanotubes.
(2) The samples were synthesized using a dual-temperature zone vacuum atmosphere tube furnace. During synthesis, 0.4g of selenium powder was placed in a quartz boat located in the upstream central heating zone. 0.2g of SnCl4·5H2The O solid is placed in another quartz boat positioned in a central heating zone at the downstream of the two-temperature zone tube furnace, and the quartz boat is placed at the upper end of the downstream heating zone and is 5cm away from the downstream heating center. TiO obtained in the step (1)2The nanotubes were placed at the end of the downstream zone, 7cm from the downstream heating center. The CVD system was vented with high purity argon (99.99%) for 30min to remove air and reduce contamination of the experiment with other gases after the sample was placed in the tube furnace and before the heating process. The downstream central heating zone was then heated to a temperature of 650 c at atmospheric pressure while the upstream central heating zone was heated to a temperature of 450 c. The gas path system at this time is set to be argon gas 80s.c.c.m. When the temperature reaches a set value, the gas circuit system is switched to a mixed gas containing 60s.c.c.m. argon and 20s.c.c.m. hydrogen. The entire hydrogen passage time lasted 15 min. Because the flow velocity of the gas flow has great influence on CVD, the argon gas flow is rapidly converted into 80s.c.c.m. after the introduction of the hydrogen is finished so as to ensure the stability of the flow velocity of the whole gas flow, thereby ensuring the stability of SnSe2And (4) growing and depositing the nanosheets. Obtaining SnSe after the temperature of the tube furnace is reduced to room temperature2/H-TiO2A heterojunction.
(3) The obtained SnSe2/H-TiO2Heterogeneous natureThe junction was placed in a sputtering vacuum chamber using a target material MoS2(purity 99.99%) under room temperature, power 300W, pressure 1Pa, sputtering gas atmosphere argon sputtering for 25min, obtained MoS2/SnSe2/H-TiO2A heterojunction.
Example 4
MoS2/SnSe2/H-TiO2The preparation method of the heterojunction photoelectric detector comprises the following steps:
(1) preparation of TiO by anodic oxidation2An array of nanotubes.
(2) The samples were synthesized using a dual-temperature zone vacuum atmosphere tube furnace. During synthesis, 0.4g of selenium powder was placed in a quartz boat located in the upstream central heating zone. 0.2g of SnCl4·5H2The O solid is placed in another quartz boat positioned in a central heating zone at the downstream of the two-temperature zone tube furnace, and the quartz boat is placed at the upper end of the downstream heating zone and is 5cm away from the downstream heating center. TiO obtained in the step (1)2The nanotubes were placed at the end of the downstream zone, 7cm from the downstream heating center. The CVD system was vented with high purity argon (99.99%) for 30min to remove air and reduce contamination of the experiment with other gases after the sample was placed in the tube furnace and before the heating process. The downstream central heating zone was then heated to a temperature of 550 c at atmospheric pressure while the upstream central heating zone was heated to a temperature of 450 c. The gas path system at this time is set to be argon gas 80s.c.c.m. When the temperature reaches a set value, the gas circuit system is switched to a mixed gas containing 60s.c.c.m. argon and 20s.c.c.m. hydrogen. The entire hydrogen passage time lasted 15 min. Because the flow velocity of the gas flow has great influence on CVD, the argon gas flow is rapidly converted into 80s.c.c.m. after the introduction of the hydrogen is finished so as to ensure the stability of the flow velocity of the whole gas flow, thereby ensuring the stability of SnSe2And (4) growing and depositing the nanosheets. Obtaining SnSe after the temperature of the tube furnace is reduced to room temperature2/H-TiO2A heterojunction.
(3) The obtained SnSe2/H-TiO2The heterojunction is placed in a sputtering vacuum chamber and a target MoS is used2(purity 99.99%) under room temperature, power 300W, pressure 1Pa, sputtering gas atmosphere argon sputtering for 20min, obtained MoS2/SnSe2/H-TiO2A heterojunction.
And (3) electrochemical performance testing: the materials prepared in the examples were fabricated into devices, respectively. In the growth of MoS2/SnSe2/H-TiO2And (3) dispensing silver paste on the spot and adhering copper foil to the spot to serve as an electrode at one end, dispensing silver paste on the ground titanium sheet substrate at the other end and adhering copper foil to serve as an electrode at the other end, and preparing the vertical photoelectric detection device. The prepared photoelectric device is subjected to I-V curve test under-1-1V bias voltage and 520nm wavelength of 370 and T curve test under 0.5V bias voltage.
As shown in fig. 1, which is an XRD pattern of the electrode material prepared in example 4. For MoS in the figure2Characteristic peaks appear at 2 θ ═ 14.2 °, 32.94 °, 43.52 ° and 58.13 °, which match standard card JCPDS No.74-0932, and correspond to crystal planes (003), (101), (009), and (110), respectively. For H-TiO2An array of nanotubes having diffraction peaks at 25.18 °, 36.93 °, 37.92 °, 47.87 °, 53.93 ° and 70.37 ° 2 θ, respectively. H-TiO2The diffraction peak of the nanotube (JCPDF 21-1272) array matches well with anatase, and its crystallinity is high. For SnSe in heterojunction2The characteristic diffraction peaks of the nanosheets appear at 14.4 °, 26.99 °, 30.73 °, 40.07 °, 47.69 and 50.08 ° 2 θ respectively, corresponding to SnSe2The diffraction peaks of the (001), (100), (011), (012), (110) and (111) crystal planes in the standard card of hexagonal crystal structure (JCPDS PDF No. 089-3197). In MoS2/SnSe2/H-TiO2No diffraction peak of other impurities is detected in the XRD pattern of (1), which indicates that MoS2/SnSe2/H-TiO2Heterojunctions were synthesized and samples were prepared with high purity and high crystallinity.
As shown in fig. 2, is an SEM image of the electrode material prepared in example 4. From the figure, MoS can be seen2Attached to SnSe2/H-TiO2The upper part is plush-shaped, and the appearance has larger surface area, thereby increasing the absorption of light.
As shown in fig. 3, the ultraviolet-visible light absorption spectrum of the electrode material prepared in example 4 is shown. It can be seen from the figure thatSnSe2/H-TiO2The absorption range of the heterojunction is 300-450nm, and the MoS2/SnSe2/H-TiO2The absorption range of (2) is extended to a wavelength range of 500 nm. Thus, MoS2/SnSe2/H-TiO2The heterojunction can detect most ultraviolet and visible light, and the device can be applied to equipment for detecting UV light.
As shown in fig. 4, which is an I-V plot of the electrode material prepared in example 4. The curves are seen to have a non-linear relationship, indicating that silver electrodes are associated with MoS2/SnSe2/H-TiO2Ohmic contact is formed between the semiconductor materials, and non-ohmic contact is formed between the semiconductor materials. The change of illumination from visible to ultraviolet shows that the device has better photoresponse capability in the visible light region and has maximum photocurrent of 45mA/cm at the wavelength of 450nm2The high optical responsivity was 7.12A/W.
As shown in fig. 5, is an I-T plot of the electrode material prepared in example 4. It can be seen from the figure that the stability of the material at the wavelengths of 520nm and 450nm was found to be good by a linear voltammetric scan of 100s, and was most stable at 450 nm.
The above embodiments are described in detail, but the embodiments of the invention are not limited thereto, and those skilled in the art can achieve the object of the invention based on the disclosure of the present invention, and any modifications and variations based on the concept of the present invention fall within the protection scope of the present invention, which is defined by the claims.

Claims (6)

1. MoS2/SnSe2/H-TiO2The heterojunction photoelectric detector and the preparation method thereof comprise the following steps:
(1) preparing TiO by using titanium sheet as substrate and adopting anodic oxidation method2A nanotube;
(2) growing SnSe by using double-temperature-zone vacuum atmosphere tube furnace2Nanosheet: respectively taking selenium powder and SnCl4 & 5H2O as Se source and Sn source, and reacting in the presence of mixed gas of argon and hydrogen in TiO atmosphere2On the nanotubeGrowing SnSe2Nanosheet, and SnSe is obtained after the temperature of the tube furnace is reduced to room temperature2/H-TiO2A heterojunction;
(3) the obtained SnSe2/H-TiO2The heterojunction is placed in a sputtering vacuum chamber and a target MoS is used2(purity 99.99%) under the condition of room temperature and argon atmosphere, adopting magnetron sputtering method to make SnSe2/H-TiO2Composite MoS on heterojunction2To obtain MoS2/SnSe2/H-TiO2A heterojunction.
2. The MoS of claim 12/SnSe2/H-TiO2The preparation method of the heterojunction photoelectric detector is characterized in that the mass ratio of the selenium powder to the SnCl4 & 5H2O in the step (2) is 0.3-0.5: 0.2-0.4.
3. The MoS of claim 12/SnSe2/H-TiO2The preparation method of the heterojunction photoelectric detector is characterized in that in the step (2), SnSe is carried out in a double-temperature-zone vacuum atmosphere tube furnace2The growth of the nano-sheets comprises the following specific operations: placing selenium powder into a quartz boat positioned in an upstream central heating zone, and adding SnCl4·5H2The O solid is placed in another quartz boat positioned in a downstream central heating area of the double-temperature-area tube furnace, and the quartz boat is placed at the upper end of the downstream heating area and is 5cm away from the downstream heating center; TiO obtained in the step (1)2The nanotubes were placed at the end of the downstream zone, 7cm from the downstream heating center.
4. The MoS of claim 32/SnSe2/H-TiO2The preparation method of the heterojunction photoelectric detector is characterized in that the upstream of the dual-temperature-zone vacuum atmosphere tube furnace is heated to the temperature of 300-500 ℃, the heating rate is 6-8 ℃/min, the downstream is heated to the temperature of 400-600 ℃, the temperature of the two sides is simultaneously raised to the set temperature, and the heat preservation time is 10-30 min.
5. The MoS of claim 42/SnSe2/H-TiO2The preparation method of the heterojunction photoelectric detector is characterized in that argon is introduced to remove air, and the operation is as follows: before the heating process, introducing argon for 30 min; and in the temperature rise process, the argon flow of the gas path system is set to be 80s.c.c.m, the mixed gas of argon and hydrogen is introduced in the heat preservation stage, the argon flow is switched to be 60s.c.c.m, and the hydrogen flow is switched to be 20s.c.c.m. And in the cooling stage, only argon is introduced, and the flow rate is 80s.c.c.m.
6. The MoS of claim 12/SnSe2/H-TiO2The preparation method of the heterojunction photoelectric detector is characterized in that in the step (3), the magnetron sputtering power is 300W, and the pressure is 1 Pa.
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