CN115295675B - Te/MoS based two-dimensional material 2 Preparation method of heterojunction photodetector - Google Patents
Te/MoS based two-dimensional material 2 Preparation method of heterojunction photodetector Download PDFInfo
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Abstract
The invention relates to a two-dimensional material based Te/MoS 2 The preparation method of the heterojunction photodetector comprises the following steps: fabrication of two-dimensional MoS-containing articles by mechanical lift-off or chemical vapor deposition 2 A first substrate; preparing a second substrate containing two-dimensional Te; transferring the two-dimensional Te to form a heterojunction; preparing a light detection device; carrying out high-pressure annealing treatment on the prepared optical detection device; by reducing Te/MoS during device fabrication 2 Te and MoS in heterojunctions 2 Inter-layer spacing of (2) to have a typical type I band arrangement structure of Te/MoS 2 The heterojunction is converted into a II-type energy band arrangement structure, and the Te/MoS based on a two-dimensional material is remarkably improved 2 The photodetection sensitivity of the heterojunction photodetector.
Description
Technical Field
The invention relates to the technical field of optical detection, in particular to a two-dimensional material-based Te/MoS 2 A method for fabricating a heterojunction photodetector.
Background
In traditional PN junction, because the diffusion of many son in p type and n type semiconductor material has produced the carrier depletion region, built-in electric field, on the light shines the PN junction, the photogenerated carrier in the material can pass the junction region through diffusion and drift process, arouse the increase of electric current, thereby realize photoelectric detection, but along with the increase of electronic chip integrated level, the required device is littleer and more, the technology is more and more complicated, traditional silicon-based CMOS size has reached the limit, need urgently that the optoelectronic device based on ultra-thin heterojunction appears and solve current problem, heterojunction optical detector based on two-dimensional material is satisfying such demand, another huge advantage of atom level two-dimensional material can carry out the modularization and pile up, the restriction to the mismatch of heterogeneous crystal lattice has been avoided effectively, can simply conveniently collocation different two-dimensional semiconductor material wantonly, prepare various van der Waals heterojunction.
Te alkene is used as a novel two-dimensional material, and has simple synthesis process, low cost and high mobility (700 cm) 2 V -1 s -2 ) The photoelectric detector based on the II-type heterojunction has the advantages that when light irradiates on the PN junction, the photo-generated electrons and the photo-generated holes in the material can be transferred to the material with a narrow band gap, the photo-generated electrons and the photo-generated holes in the material have great recombination probability, the service life of the photo-generated electrons and the photo-generated holes is short, the photoelectric detector with good performance is not easy to prepare, and when the light irradiates on the PN junction, the photo-generated electrons and the photo-generated holes in the material can be respectively transferred to different materials, so that the recombination probability of the photo-generated electrons and the photo-generated holes is greatly reduced, and the photocurrent is obviously higher than that of the I-type heterojunction.
Disclosure of Invention
The invention aims to provide a two-dimensional material based Te/MoS 2 A preparation method of a heterojunction photodetector is used for overcoming the defects in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
the application discloses a Te/MoS based two-dimensional material 2 The preparation method of the heterojunction photodetector specifically comprises the following steps:
s1, manufacturing the two-dimensional MoS by adopting mechanical stripping or chemical vapor deposition 2 A first substrate;
s2, preparing a second substrate containing two-dimensional Te: preparing single crystal two-dimensional Te by using sodium tellurite, polyvinylpyrrolidone, hydrazine hydrate and ammonia water as raw materials, and transferring the single crystal two-dimensional Te onto a second substrate;
s3, transferring the two-dimensional Te on the second substrate to the two-dimensional MoS on the first substrate 2 Position of (2) forming Te/MoS 2 A van der Waals heterojunction;
s4, preparing an optical detector: respectively at one side of two-dimensional Te and two-dimensional MoS 2 Preparing an electrode on one side of the substrate; the electrode adopts a double-layer structure; obtaining the Te/MoS based two-dimensional material 2 A photodetector prototype of a heterojunction;
s5, carrying out high-pressure annealing treatment on the photo-detector prototype in the step S4 to obtain a two-dimensional material-based Te/MoS 2 A heterojunction photodetector.
Preferably, the step S1 of preparing the two-dimensional MoS-containing material by chemical vapor deposition 2 Specifically, the substrate of (1) comprises the following substeps:
a11, selecting a single-side polished silicon oxide wafer as a growth substrate;
a12, in MoO 3 The powder and the S simple substance powder are used as reactants and are respectively arranged in two quartz boats;
a13, dicing the growth substrate of the step A11 so that the surface having the oxide layer faces downward, and placing the substrate in the step A12 with MoO 3 On a quartz boat of powder; placing two quartz boats in a quartz tube;
a14, introducing argon containing hydrogen into the quartz tube, and removing air in the quartz tube;
a15, heating the quartz tube to the growth temperature, and carrying out MoS 2 Growing; the growth temperature is 600-900 ℃; the growth time is 10 to 40 minutes;
a16, after the growth is finished, sampling to obtain the crystal boat containing the two-dimensional MoS after the quartz boat is cooled to room temperature 2 I.e. containing two-dimensional MoS 2 Substrate one.
Preferably, the step S1 of preparing the two-dimensional MoS-containing material by mechanical stripping 2 Specifically, the substrate of (1) comprises the following substeps:
b1, selecting a single-side polished silicon oxide wafer as a growth substrate;
b2, moS using blue film adhesive tape to repeatedly dissociate blocks 2 Up to MoS on blue film tape 2 A very light transparent color is presented;
b3, moS on blue film 2 Pressing the region on the growth substrate of the step B1;
b4, moS will be attached 2 The growth substrate of (2) is placed on a heating plate and heated;
b5, after heating is finished, uncovering the blue film adhesive tape to obtain the adhesive tape containing two-dimensional MoS 2 I.e. containing two-dimensional MoS 2 Substrate one.
Preferably, step S2 specifically includes the following substeps:
s21, dissolving sodium tellurite and polyvinylpyrrolidone in deionized water, and uniformly stirring to obtain a solution A;
s22, mixing hydrazine hydrate and ammonia water to form a solution B;
s23, adding the solution B into the solution A, and carrying out hydrothermal reaction at the temperature of 160-200 ℃ for 20-40 hours;
s24, obtaining two-dimensional Te after the hydrothermal reaction is finished; and transferring the two-dimensional Te to PDMS to obtain a PDMS base containing the two-dimensional Te, namely a substrate II containing the two-dimensional Te.
Preferably, the dry transfer stage is adopted in step S3 to transfer the two-dimensional Te on the second substrate to the two-dimensional MoS on the first substrate 2 Position of (2) forming Te/MoS 2 Van der waals heterojunctions.
Preferably, in the step S4, the electrodes are prepared by a positive photoresist stripping technique in a microelectronic process, and all the electrodes adopt a double-layer electrode structure, wherein the electrodes in contact with the two-dimensional Te are a Pd contact layer and an Au conductive layer; and two-dimensional MoS 2 The contacted electrodes are a Ni contact layer and an Au conductive layer; the specific operation is as follows:
s41, laser direct writing pairing and two-dimensional MoS 2 Patterning the contacted electrode, and preparing the electrode by adopting magnetron sputtering, wherein the electrode comprises a two-dimensional MoS 2 A Ni contact layer in contact with the Au conductive layer attached above the Ni contact layer;
s42, patterning an electrode in contact with the two-dimensional Te by adopting laser direct writing, and preparing the electrode by adopting magnetron sputtering, wherein the electrode comprises a Pd contact layer in contact with the two-dimensional Te and an Au conductive layer attached above the Pd contact layer;
after the preparation of the electrodes in the steps S43, S41 and S42 is finished, the Te/MoS based two-dimensional material is obtained 2 A photodetector prototype of a heterojunction.
Preferably, in the step S5, the annealing temperature is 200-280 ℃, the annealing time is 2-4 hours, and N is used as inert gas 2 Or Ar, the inert gas pressure being maintained between 0.5 and 1.5MPa during the annealing.
The invention has the beneficial effects that:
the invention is based on a two-dimensional material Te/MoS 2 Preparation method of heterojunction optical detector, and prepared two-dimensional Te/MoS 2 The structure of the photodetector of the PN type heterojunction is optimized, and Te/MoS is reduced by annealing the photodetector of the heterojunction at high temperature and high pressure 2 Two layer spacing in the heterojunction, resulting in Te/MoS 2 Transition of energy band arrangement structure of heterojunction from type I to type II, te/MoS with type II energy band arrangement structure 2 The photogenerated electrons and the photogenerated holes in the heterojunction are respectively transferred to the two materials under the action of the built-in electric field, so that the recombination of photogenerated electron-hole pairs can be effectively inhibited, the service life of photogenerated carriers is prolonged, the size of photocurrent is improved, the improvement of the photo-detection capability is realized, and the photo-detection sensitivity of the photo-detector is improved.
The features and advantages of the present invention will be described in detail by embodiments in conjunction with the accompanying drawings.
Drawings
FIG. 1 shows a two-dimensional Te/MoS material prepared in example 1 of the present invention 2 Optical microscope photographs of van der waals heterojunctions;
FIG. 2 shows Te/MoS prepared in example 1 of the present invention 2 Raman spectra of van der waals heterojunctions;
FIG. 3 shows a two-dimensional Te/MoS material prepared in example 1 of the present invention 2 An optical microscope photograph of the heterojunction photodetector;
FIG. 4 is a schematic view ofTe/MoS prepared in example 1 of the invention 2 Transmission electron microscope photos of the van der waals heterojunction at the interface before and after high-temperature high-pressure annealing;
FIG. 5 shows a two-dimensional Te/MoS material prepared in example 1 of the present invention 2 IV curves corresponding to different energies of the heterojunction optical detector under the illumination of 532nm laser;
FIG. 6 shows a two-dimensional Te/MoS material prepared in example 1 of the present invention 2 The heterojunction optical detector is under the illumination of laser light with different wavelengths, and the light detection sensitivity relationship graphs corresponding to different energies are obtained;
FIG. 7 shows two-dimensional Te/MoS materials prepared in examples 1-5 of the present invention 2 The heterojunction optical detector has the photoelectric detection sensitivity of 1mW of incident energy under the illumination of 532nm laser;
FIG. 8 shows a two-dimensional Te/MoS-based material according to the present invention 2 A flow chart of a method of fabricating a heterojunction photodetector.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood, however, that the description herein of specific embodiments is only intended to illustrate the invention and not to limit the scope of the invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.
Referring to FIG. 8, the present invention is based on two-dimensional Te/MoS material 2 The preparation method of the heterojunction photodetector specifically comprises the following steps:
s1, manufacturing two-dimensional MoS by adopting mechanical stripping or chemical vapor deposition 2 Substrate one;
s2, preparing a second substrate containing two-dimensional Te: preparing single crystal two-dimensional Te by using sodium tellurite, polyvinylpyrrolidone, hydrazine hydrate and ammonia water as raw materials, and transferring the single crystal two-dimensional Te onto a second substrate;
s3, transferring the two-dimensional Te on the second substrate to the two-dimensional MoS on the first substrate 2 Position of (2) to form Te/MoS 2 A van der waals heterojunction;
s4, preparing an optical detection device: respectively at one side of two-dimensional Te and two-dimensional MoS 2 Preparing an electrode on one side of the substrate; the electrode adopts a double-layer structure; obtaining the Te/MoS based two-dimensional material 2 A photodetector prototype of a heterojunction;
s5, carrying out high-pressure annealing treatment on the photo-detector prototype in the step S4 to obtain a two-dimensional material based Te/MoS 2 A heterojunction photodetector.
In one possible embodiment, the step S1 of manufacturing the two-dimensional MoS-containing material by chemical vapor deposition 2 Specifically, the substrate of (1) comprises the following substeps:
a11, selecting a single-side polished silicon oxide wafer as a growth substrate;
a12, in MoO 3 The powder and the S simple substance powder are used as reactants and are respectively arranged in two quartz boats;
a13, dicing the growth substrate of the step A11 so that the surface having the oxide layer faces downward, and placing the substrate in the step A12 with MoO 3 On a quartz boat of powder; placing two quartz boats in a quartz tube;
a14, introducing argon containing hydrogen into the quartz tube, and removing air in the quartz tube;
a15, heating the quartz tube to the growth temperature, and carrying out MoS 2 Growing; the growth temperature is 600-900 ℃; the growth time is 10 to 40 minutes;
a16, after the growth is finished, sampling to obtain the crystal boat containing the two-dimensional MoS after the quartz boat is cooled to room temperature 2 I.e. containing two-dimensional MoS 2 Substrate one.
In one possible embodiment, the step S1 of making the two-dimensional MoS-containing material by mechanical stripping 2 The substrate of (1) specifically comprises the following substeps:
b1, selecting a single-side polished silicon oxide wafer as a growth substrate;
b2, moS using blue film adhesive tape to repeatedly dissociate blocks 2 Up to MoS on blue film tape 2 A very light transparent color is presented;
b3, moS on blue film 2 Zone pressing in step B1A long substrate;
b4, moS to be attached 2 The growth substrate of (2) is placed on a heating plate and heated;
b5, after heating is finished, uncovering the blue film adhesive tape to obtain the product containing the two-dimensional MoS 2 I.e. containing two-dimensional MoS 2 Substrate one.
In a possible embodiment, step S2 specifically includes the following sub-steps:
s21, dissolving sodium tellurite and polyvinylpyrrolidone in deionized water, and uniformly stirring to obtain a solution A;
s22, mixing hydrazine hydrate and ammonia water to form a solution B;
s23, adding the solution B into the solution A, and carrying out hydrothermal reaction at the temperature of 160-200 ℃ for 20-40 hours;
s24, obtaining two-dimensional Te after the hydrothermal reaction is finished; and transferring the two-dimensional Te to PDMS to obtain a PDMS base containing the two-dimensional Te, namely a substrate II containing the two-dimensional Te.
In a possible embodiment, the dry transfer stage is used in step S3 to transfer the two-dimensional Te on the second substrate to the two-dimensional MoS on the first substrate 2 Position of (2) to form Te/MoS 2 Van der waals heterojunctions.
In a possible embodiment, step S4 is to prepare electrodes by positive photoresist stripping technology in microelectronic process, wherein the electrodes are both in a double-layer electrode structure, and the electrodes in contact with the two-dimensional Te are a Pd contact layer and an Au conductive layer; and two-dimensional MoS 2 The contacted electrodes are a Ni contact layer and an Au conductive layer; the specific operation is as follows:
s41, adopting laser direct writing pair and two-dimensional MoS 2 Patterning the contacted electrode, and preparing the electrode by adopting magnetron sputtering, wherein the electrode comprises a two-dimensional MoS 2 A Ni contact layer in contact with the Au conductive layer attached above the Ni contact layer;
s42, patterning an electrode in contact with the two-dimensional Te by adopting laser direct writing, and preparing the electrode by adopting magnetron sputtering, wherein the electrode comprises a Pd contact layer in contact with the two-dimensional Te and an Au conducting layer attached above the Pd contact layer;
after the preparation of the electrodes in the steps S43, S41 and S42 is finished, the Te/MoS based two-dimensional material is obtained 2 A photodetector prototype of a heterojunction.
In a practical embodiment, the annealing temperature is 200 to 280 ℃ and the annealing time is 2 to 4 hours in the step S5, and N is used as inert gas 2 Or Ar, the inert gas pressure being maintained between 0.5 and 1.5MPa during the annealing.
Example 1:
s1, preparing two-dimensional MoS by adopting CVD method 2 : selecting a single-side polished silicon oxide wafer as MoS 2 The thickness of the silicon wafer is 0.5mm, and the surface of the polished surface is 300nmSiO 2 Oxide layer and silicon substrate are heavily doped with p-type dopant, and MoO is weighed 3 0.05g of powder and 0.5g of elemental powder of S were charged in two quartz boats, respectively, the substrate material was cut into a size of about 2cm in width and about 2cm in length, the substrate was turned over so that the side having the oxide layer was facing downward, and the substrate was placed in a chamber filled with MoO 3 Placing the quartz boat in a quartz tube, placing the quartz tube in a growth system (such as a chemical vapor deposition high-temperature furnace) and confirming the airtightness of the growth system, introducing 500sccm of argon gas containing 5% of hydrogen, opening a mechanical pump connected to an air outlet port and an air outlet port valve to exhaust air so as to exhaust air in the quartz tube, reducing the flow of the hydrogen and the argon gas to 20sccm before starting heating and raising the temperature, adjusting the size of the air outlet port valve to ensure that the air pressure in the quartz tube reaches 50mbar and stabilizes for about 20 minutes, setting the temperature to rise from room temperature to 750 ℃ at a constant speed for 20 minutes, and entering MoS after the temperature reaches the set temperature 2 The growth stage of (1) is that the growth time is 15 minutes, the heating is stopped after the growth is finished, the quartz tube is moved out of the furnace along the guide rail to be naturally cooled, the flow of argon is increased to 200sccm, the quartz boat is completely cooled to the room temperature, and then the sampling is carried out to obtain the grown two-dimensional MoS 2 Si/SiO of 2 A substrate;
s2, preparing two-dimensional Te by adopting a hydrothermal reaction method: dissolving 0.1g of sodium tellurite and 0.5g of polyvinylpyrrolidone with molecular weight in 33mL of deionized water, stirring for 30 minutes under a magnetic stirrer to form a solution A with the concentration of 0.014mol/L, then mixing 1.65mL of hydrazine hydrate and 3.3mL of ammonia water to form a solution B, adding the solution B into the solution A, placing the solution B into a hydrothermal reaction kettle, sealing, reacting in a 180 ℃ oven for 30 hours, taking out to obtain a product two-dimensional Te, transferring the product two-dimensional Te onto PDMS, and repeatedly washing with acetone and isopropanol for multiple times to obtain a PDMS substrate containing the two-dimensional Te;
s3, transferring the two-dimensional Te to form a heterojunction: transfer of two-dimensional Te on PDMS to target two-dimensional MoS Using Dry transfer stage 2 Thereby forming Te/MoS 2 Van der Waals heterojunction, FIG. 1 shows a prepared two-dimensional material Te/MoS 2 Optical microscope photograph of Van der Waals heterojunction, te/MoS prepared in FIG. 2 2 The Raman spectrogram of the Van der Waals heterojunction can clearly observe pure two-dimensional Te of 123cm -1 A (A) 1 Mode sum 140cm -1 At E 2 Characteristic peak of mode, pure MoS 2 Region E 12g Mode is at 382cm -1 A and A 1g The mode is 401cm -1 And no Te and MoS are found in the heterojunction region 2 Shift of characteristic peaks;
s4, preparing an optical detection device: the positive photoresist stripping technique in microelectronic process is adopted to prepare the electrode, and the problems of contact resistance, te and MoS are considered 2 Needs to be contacted with different electrode materials, so that the electrodes need to be prepared twice, and firstly, the laser direct writing pair and the MoS are adopted 2 Patterning the contacted electrode, preparing the electrode by adopting magnetron sputtering, wherein the electrode adopts a two-layer structure, the first layer is MoS 2 The second layer is an Au thin film conducting layer with the thickness of 60nm attached above the Ni thin film electrode, then laser direct writing is continuously adopted to carry out patterning on the electrode in contact with Te, magnetron sputtering is adopted to prepare the electrode, the electrode adopts a two-layer structure, the first layer is a 20nmPD thin film in contact with Te, the second layer is an Au thin film conducting layer with the thickness of 60nm attached above the Pd thin film electrode, and therefore the two-dimensional material Te/MoS is obtained 2 A heterojunction photodetector, FIG. 3 is a prepared two-dimensional material Te/MoS 2 An optical microscope photograph of the heterojunction photodetector;
s5, preparing the optical detectorCarrying out high-pressure annealing treatment on the workpiece: the prepared optical detector is placed in a high-pressure atmosphere annealing furnace, the annealing furnace is vacuumized, the oxygen in the air is mainly removed, the device is prevented from being oxidized during high-temperature annealing, and N is filled in the annealing furnace 2 The pressure in the annealing furnace was set to 1MPa, the annealing temperature was set at 200 ℃ and the annealing time was 4 hours, and FIG. 4 shows the prepared Te/MoS 2 Transmission electron microscope photographs of the van der Waals heterojunction at the interface before and after high-temperature high-pressure annealing can be observed, and Te and MoS before annealing 2 With a large space in the middle, mainly by preparing two-dimensional Te and two-dimensional MoS 2 Residues and oxides formed during the process, and the layer is significantly improved after annealing, te and MoS 2 The interlayer spacing of (a) is significantly reduced, on average less than 0.3nm.
Example 2:
s1, preparing two-dimensional MoS by adopting mechanical stripping 2 : selecting a single-side polished silicon oxide wafer as MoS 2 The thickness of the silicon wafer is 0.5mm, and the surface of the polished surface is 300nmSiO 2 An oxide layer, a silicon substrate adopting p-type heavy doping, and MoS using blue film adhesive tape to repeatedly dissociate blocks 2 Up to MoS on blue film tape 2 The MoS on the blue film appears very light transparent 2 Region pressing on the substrate to attach MoS 2 The substrate is placed on a heating plate at 80 ℃ to be heated for 30min, and then the blue film adhesive tape is uncovered, so that the two-dimensional MoS 2 A substrate of (a);
s2, preparing two-dimensional Te by adopting a hydrothermal reaction method: dissolving 0.1g of sodium tellurite and 0.5g of polyvinylpyrrolidone with molecular weight in 33mL of deionized water, stirring for 30 minutes under a magnetic stirrer to form a solution A with the concentration of 0.014mol/L, then mixing 1.65mL of hydrazine hydrate and 3.3mL of ammonia water to form a solution B, adding the solution B into the solution A, placing the solution B into a hydrothermal reaction kettle, sealing, reacting in an oven at 200 ℃ for 20 hours, taking out the solution to obtain a product two-dimensional Te, transferring the product two-dimensional Te onto PDMS, and repeatedly washing the product two-dimensional Te with acetone and isopropanol for multiple times to obtain a PDMS substrate containing the two-dimensional Te;
s3, transferring the two-dimensional Te to form a heterojunction: transfer of two-dimensional Te on PDMS to target Using Dry transfer stageStandard two-dimensional MoS 2 Thereby forming Te/MoS 2 A van der waals heterojunction;
s4, preparing an optical detector: the method comprises preparing electrodes by positive photoresist stripping technique in microelectronic process, and first using laser direct writing pair and MoS 2 Patterning the contacted electrode, preparing the electrode by adopting magnetron sputtering, wherein the electrode adopts a two-layer structure, the first layer is MoS 2 The second layer is an Au thin film conducting layer with the thickness of 80nm attached above the Ni thin film electrode, then the electrode in contact with Te is patterned by continuously adopting laser direct writing, the electrode is prepared by adopting magnetron sputtering, the electrode adopts a two-layer structure, the first layer is a 5nmPD thin film in contact with Te, the second layer is an Au thin film conducting layer with the thickness of 80nm attached above the Pd thin film electrode, and therefore the two-dimensional material Te/MoS is obtained 2 A heterojunction photodetector;
s5, carrying out high-pressure annealing treatment on the prepared optical detection device: the prepared optical detector is placed in a high-pressure atmosphere annealing furnace, the annealing furnace is vacuumized, ar is filled in the annealing furnace, the air pressure in the annealing furnace reaches 1MPa, the annealing temperature is set to be 200 ℃, and the annealing time is 4 hours.
Example 3:
s1, preparing two-dimensional MoS by adopting CVD method 2 : selecting a single-side polished silicon oxide wafer as MoS 2 The thickness of the silicon wafer is 0.5mm, and the surface of the polished surface is 300nmSiO 2 Oxide layer and silicon substrate are heavily doped with p-type dopant, and MoO is weighed 3 0.05g of powder and 0.5g of elemental powder of S were charged in two quartz boats, respectively, the substrate material was cut into a size of about 2cm in width and about 2cm in length, the substrate was turned over so that the side having the oxide layer was facing downward, and the substrate was placed in a chamber filled with MoO 3 Placing the quartz boat in a quartz tube, placing the quartz tube in a growth system (such as a chemical vapor deposition high-temperature furnace) and confirming the airtightness of the growth system, introducing 500sccm of argon gas containing 5% of hydrogen gas, opening a mechanical pump and an outlet port valve connected to an outlet port to exhaust the air in the quartz tube, reducing the flow of the hydrogen gas and the argon gas to 20sccm before heating and raising the temperature, and adjusting the valve of the outlet portThe size of the gate is adjusted to ensure that the air pressure in the quartz tube reaches 50mbar and is stabilized for about 20 minutes, the temperature is set for 30 minutes and is uniformly increased from room temperature to 900 ℃, and MoS is carried out after the set temperature is reached 2 The growth stage of (1) is that the growth time is 10 minutes, the heating is stopped after the growth is finished, the quartz tube is moved to the outside of the furnace along the guide rail to be naturally cooled, the flow of argon is increased to 200sccm, and the quartz boat is completely cooled to the room temperature and then sampled to obtain the grown two-dimensional MoS 2 Si/SiO of 2 A substrate;
s2, preparing two-dimensional Te by adopting a hydrothermal reaction method: dissolving 0.1g of sodium tellurite and 0.5g of polyvinylpyrrolidone with molecular weight in 33mL of deionized water, stirring for 30 minutes under a magnetic stirrer to form a solution A with the concentration of 0.014mol/L, then mixing 1.65mL of hydrazine hydrate and 3.3mL of ammonia water to form a solution B, adding the solution B into the solution A, placing the solution B into a hydrothermal reaction kettle, sealing, reacting in an oven at 160 ℃ for 40 hours, taking out to obtain a product two-dimensional Te, transferring the product two-dimensional Te onto PDMS, and repeatedly washing with acetone and isopropanol for many times to obtain a PDMS substrate containing the two-dimensional Te;
s3, transferring the two-dimensional Te to form a heterojunction: two-dimensional Te on PDMS is transferred to target two-dimensional MoS by using dry transfer table 2 Thereby forming Te/MoS 2 A van der waals heterojunction;
s4, preparing an optical detection device: the positive photoresist stripping technology in microelectronic process is adopted to prepare electrodes, and laser direct writing pairing and MoS are adopted firstly 2 Patterning the contacted electrode, preparing the electrode by adopting magnetron sputtering, wherein the electrode adopts a two-layer structure, the first layer is MoS 2 A contact 20nmNi film, a second layer is an Au film conducting layer with the thickness of 80nm attached above the Ni film electrode, then the electrode in contact with Te is patterned by continuously adopting laser direct writing, the electrode is prepared by adopting magnetron sputtering, the electrode adopts a two-layer structure, the first layer is a 20nmPD film in contact with Te, the second layer is an Au film conducting layer with the thickness of 80nm attached above the Pd film electrode, and thus the two-dimensional material Te/MoS is obtained 2 A heterojunction photodetector;
s5, carrying out high-pressure annealing treatment on the prepared optical detection device: the prepared optical detector is placed in a high-pressure atmosphere annealing furnace, the annealing furnace is vacuumized, ar is filled in the annealing furnace, the air pressure in the annealing furnace reaches 0.5MPa, the annealing temperature is set to be 280 ℃, and the annealing time is 2 hours.
Example 4:
s1, preparing two-dimensional MoS by adopting CVD method 2 : selecting a single-side polished silicon oxide wafer as MoS 2 The thickness of the silicon wafer is 0.5mm, and the surface of the polished surface is 300nmSiO 2 Oxide layer and silicon substrate are heavily doped with p-type dopant, and MoO is weighed 3 0.05g of powder and 0.5g of elemental powder of S were charged in two quartz boats, respectively, the substrate material was cut into a size of about 2cm in width and about 2cm in length, the substrate was turned over so that the side having the oxide layer was facing downward, and the substrate was placed in a chamber filled with MoO 3 Placing the quartz boat in a quartz tube, placing the quartz tube in a growth system (such as a chemical vapor deposition high-temperature furnace) and confirming the airtightness of the growth system, introducing 500sccm argon gas containing 5% of hydrogen, opening a mechanical pump connected to an air outlet port and an air outlet port valve to exhaust air so as to remove air in the quartz tube, reducing the flow of the hydrogen and the argon gas to 20sccm before heating and warming up, adjusting the valve size of the air outlet port to ensure that the air pressure in the quartz tube reaches 50mbar and is stabilized for about 20 minutes, setting the temperature to rise from room temperature to 600 ℃ at a constant speed for 15 minutes, and entering MoS after the set temperature is reached 2 The growth stage of (1) is that the growth time is 40 minutes, the heating is stopped after the growth is finished, the quartz tube is moved to the outside of the furnace along the guide rail to be naturally cooled, the flow of argon is increased to 200sccm, and the quartz boat is completely cooled to the room temperature and then sampled to obtain the grown two-dimensional MoS 2 Si/SiO of 2 A substrate;
s2, preparing two-dimensional Te by adopting a hydrothermal reaction method: dissolving 0.1g of sodium tellurite and 0.5g of polyvinylpyrrolidone with molecular weight in 33mL of deionized water, stirring for 30 minutes under a magnetic stirrer to form a solution A with the concentration of 0.014mol/L, then mixing 1.65mL of hydrazine hydrate and 3.3mL of ammonia water to form a solution B, adding the solution B into the solution A, placing the solution B into a hydrothermal reaction kettle, sealing, reacting in an oven at 180 ℃ for 30 hours, taking out the solution A to obtain a product two-dimensional Te, transferring the product two-dimensional Te onto PDMS, and repeatedly washing the product two-dimensional Te with acetone and isopropanol for multiple times to obtain a PDMS substrate containing the two-dimensional Te;
s3, transferring the two-dimensional Te to form a heterojunction: transfer of two-dimensional Te on PDMS to target two-dimensional MoS Using Dry transfer stage 2 Thereby forming Te/MoS 2 A van der waals heterojunction;
s4, preparing an optical detection device: the method comprises preparing electrodes by positive photoresist stripping technique in microelectronic process, and first using laser direct writing pair and MoS 2 Patterning the contacted electrode, preparing the electrode by adopting magnetron sputtering, wherein the electrode adopts a two-layer structure, the first layer is MoS 2 The second layer is an Au thin film conducting layer with the thickness of 60nm attached above the Ni thin film electrode, then the electrode in contact with Te is patterned by continuously adopting laser direct writing, the electrode is prepared by adopting magnetron sputtering, the electrode adopts a two-layer structure, the first layer is a 20nmPD thin film in contact with Te, the second layer is an Au thin film conducting layer with the thickness of 60nm attached above the Pd thin film electrode, and therefore the two-dimensional material Te/MoS is obtained 2 A heterojunction photodetector;
s5, carrying out high-pressure annealing treatment on the prepared optical detection device: placing the prepared optical detector in a high-pressure atmosphere annealing furnace, vacuumizing the annealing furnace, and filling N into the annealing furnace 2 The air pressure in the annealing furnace is up to 1.5MPa, the annealing temperature is set to 280 ℃, and the annealing time is 2 hours.
Example 5:
s1, preparing two-dimensional MoS by adopting CVD method 2 : selecting a single-side polished silicon oxide wafer as MoS 2 The thickness of the silicon wafer is 0.5mm, and the surface of the polished surface is 300nmSiO 2 Oxide layer and silicon substrate are heavily doped with p-type dopant, and MoO is weighed 3 0.05g of powder and 0.5g of elemental powder of S were charged in two quartz boats, respectively, the substrate material was cut into a size of about 2cm in width and about 2cm in length, the substrate was turned over so that the side having the oxide layer was facing downward, and the substrate was placed in a chamber filled with MoO 3 Placing the quartz boat in a quartz tube, placing the quartz tube in a growth system (such as a chemical vapor deposition high temperature furnace) and confirming the gas tightness of the growth systemThen, argon gas with the hydrogen content of 5 percent is introduced into the quartz tube by 500sccm, a mechanical pump connected to an air outlet port and an air outlet port valve are opened to exhaust air so as to remove air in the quartz tube, the flow of the hydrogen and the argon gas is reduced to 20sccm before heating and temperature rising are started, the valve size of the air outlet port is adjusted to ensure that the air pressure in the quartz tube reaches 50mbar and is stabilized for about 20 minutes, the temperature is set for 20 minutes, the temperature is uniformly raised from the room temperature to 750 ℃ at a constant speed, and after the set temperature is reached, moS is carried out 2 The growth stage of (1) is that the growth time is 15 minutes, the heating is stopped after the growth is finished, the quartz tube is moved out of the furnace along the guide rail to be naturally cooled, the flow of argon is increased to 200sccm, the quartz boat is completely cooled to the room temperature, and then the sampling is carried out to obtain the grown two-dimensional MoS 2 Si/SiO of 2 A substrate;
s2, preparing two-dimensional Te by adopting a hydrothermal reaction method: dissolving 0.1g of sodium tellurite and 0.5g of polyvinylpyrrolidone with molecular weight in 33mL of deionized water, stirring for 30 minutes under a magnetic stirrer to form a solution A with the concentration of 0.014mol/L, then mixing 1.65mL of hydrazine hydrate and 3.3mL of ammonia water to form a solution B, adding the solution B into the solution A, placing the solution B into a hydrothermal reaction kettle, sealing, reacting in an oven at 180 ℃ for 30 hours, taking out the solution A to obtain a product two-dimensional Te, transferring the product two-dimensional Te onto PDMS, and repeatedly washing the product two-dimensional Te with acetone and isopropanol for multiple times to obtain a PDMS substrate containing the two-dimensional Te;
s3, transferring the two-dimensional Te to form a heterojunction: transfer of two-dimensional Te on PDMS to target two-dimensional MoS Using Dry transfer stage 2 Thereby forming Te/MoS 2 A van der waals heterojunction;
s4, preparing an optical detection device: the method comprises preparing electrodes by positive photoresist stripping technique in microelectronic process, and first using laser direct writing pair and MoS 2 Patterning the contacted electrode, preparing the electrode by adopting magnetron sputtering, wherein the electrode adopts a two-layer structure, the first layer is MoS 2 The second layer is an Au thin film conducting layer with the thickness of 60nm attached above the Ni thin film electrode, then the electrode in contact with Te is patterned by continuously adopting laser direct writing, the electrode is prepared by adopting magnetron sputtering, the electrode adopts a two-layer structure, the first layer is a 20nmPD thin film in contact with TeThe second layer is an Au thin film conductive layer with the thickness of 60nm attached above the Pd thin film electrode, thereby obtaining a two-dimensional material Te/MoS 2 A heterojunction photodetector;
s5, carrying out high-pressure annealing treatment on the prepared optical detection device: placing the prepared photodetector in a high-pressure annealing furnace, vacuumizing the annealing furnace, and charging into the annealing furnace to a concentration of 50% N 2 And 50% of Ar, by weight, in such a manner that the gas pressure in the annealing furnace becomes 1MPa, the annealing temperature is set at 240 ℃ and the annealing time is 3 hours.
The photodetection devices prepared in examples 1 to 5 were subjected to a photodetection test: firstly, a laser with the wavelength of 532nm is adopted to carry out a photoelectric detection test on a prepared optical detection device, the incident energy of the laser is adjusted from 1mW to 6mW, FIG. 5 is an IV curve corresponding to different energies of the optical detector in the embodiment 1 under the illumination of 532nm laser, secondly, lasers with the wavelengths of 633nm, 808nm and 1550nm are adopted to carry out the photoelectric detection test on the prepared optical detection device, and FIG. 6 is a photo-sensitivity relation graph corresponding to different energies of the optical detector in the embodiment 1 under the illumination of different wavelengths laser, so that whether in a visible light range or a near infrared range, compared with a two-dimensional material Te/MoS before high-temperature high-pressure annealing and after annealing, the two-dimensional material Te/MoS is obtained after annealing in a high-temperature high-pressure annealing process 2 The photoelectric detection sensitivity of the heterojunction optical detector is obviously improved. Examples 1-5 two-dimensional materials Te/MoS 2 The photoelectric detection sensitivity of the heterojunction photodetector with incident energy of 1mW under 532nm laser illumination is shown in figure 7, and the comparison result shows that the two-dimensional material Te/MoS prepared in the experimental condition range given by the patent of the invention 2 The heterojunction optical detector has small performance difference, and can effectively improve the photoelectric detection sensitivity.
The invention selects mature two-dimensional n-type wide bandgap semiconductor material MoS 2 Forming Van der Waals heterojunction with tellurine, preparing optical detector, and making Te/MoS contact with two-dimensional materials 2 The Van der Waals heterojunction is a typical I-type energy band arrangement structure, but analysis shows that the interlayer spacing of two layers of the heterojunction can influence the type of the heterojunction, and the narrower the spacing is, the more complete the conversion is easierChanging into II type energy band arrangement structure, and calculating according to first principle when Te/MoS 2 Te/MoS when the interlayer spacing of the Van der Waals heterojunction is less than-0.28 nm 2 The van der waals heterojunction will form a type II band aligned structure. In the present invention, two-dimensional Te and MoS will be prepared separately 2 Materials, formation of Te/MoS by dry transfer method 2 Van der Waals heterojunction and preparation of photodetector, and for Te/MoS 2 The interlayer spacing of the Van der Waals heterojunction is optimized, and the Te/MoS of the two-dimensional material is improved by changing the energy band arrangement structure of the heterojunction 2 Heterojunction light detection sensitivity.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (6)
1. Te/MoS based two-dimensional material 2 The preparation method of the heterojunction photodetector is characterized by comprising the following steps:
s1, manufacturing two-dimensional MoS by adopting mechanical stripping or chemical vapor deposition 2 A first substrate;
s2, preparing a second substrate containing two-dimensional Te: preparing single crystal two-dimensional Te by using sodium tellurite, polyvinylpyrrolidone, hydrazine hydrate and ammonia water as raw materials, and transferring the single crystal two-dimensional Te onto a second substrate;
s3, transferring the two-dimensional Te on the second substrate to the two-dimensional MoS on the first substrate 2 Position of (2) to form Te/MoS 2 A van der waals heterojunction;
s4, preparing an optical detection device: respectively on one side of Te and MoS 2 Preparing an electrode on one side of the substrate; the electrode adopts a double-layer structure; obtaining the Te/MoS based two-dimensional material 2 A photodetector prototype of a heterojunction;
s5, carrying out high-pressure annealing treatment on the photo-detector prototype in the S4 to obtain a two-dimensional material-based Te/MoS 2 A heterojunction photodetector; in the step S5, the annealing temperature is 200-280 ℃, the annealing time is 2-4 hours, and the inert gas adopts N 2 Or in ArOne or more, the inert gas pressure is maintained at 0.5-1.5MPa during annealing.
2. Two-dimensional material based Te/MoS as claimed in claim 1 2 The preparation method of the heterojunction photodetector is characterized in that in the step S1, the two-dimensional MoS is prepared by adopting chemical vapor deposition 2 The substrate of (1) specifically comprises the following substeps:
a11, selecting a single-side polished silicon oxide wafer as a growth substrate;
a12, in MoO 3 The powder and the S simple substance powder are used as reactants and are respectively arranged in two quartz boats;
a13, dicing the growth substrate of A11 so that the surface having the oxide layer faces downward, placing in A12 with MoO 3 On a quartz boat of powder; placing two quartz boats in a quartz tube;
a14, introducing argon containing hydrogen into the quartz tube, and removing air in the quartz tube;
a15, heating the quartz tube to the growth temperature, and carrying out MoS 2 Growing; the growth temperature is 600-900 ℃; the growth time is 10 to 40 minutes;
a16, after the growth is finished, sampling to obtain the crystal boat containing the two-dimensional MoS after the quartz boat is cooled to room temperature 2 I.e. containing two-dimensional MoS 2 Substrate one.
3. Two-dimensional material based Te/MoS as claimed in claim 1 2 The preparation method of the heterojunction photodetector is characterized in that mechanical stripping is adopted in the step S1 to manufacture the photodetector containing two-dimensional MoS 2 Specifically, the substrate of (1) comprises the following substeps:
b1, selecting a single-side polished silicon oxide wafer as a growth substrate;
b2, moS using blue film adhesive tape to repeatedly dissociate blocks 2 Up to MoS on blue film tape 2 The transparent color is presented;
b3, moS on blue film 2 The area is pressed on the growth substrate of B1;
b4, attaching MoS 2 The growth substrate is placed on a heating plate and heated;
b5, after heating is finished, uncovering the blue film adhesive tape to obtain the product containing the two-dimensional MoS 2 I.e. containing two-dimensional MoS 2 Substrate one.
4. Two-dimensional material based Te/MoS as claimed in claim 1 2 The preparation method of the heterojunction photodetector is characterized in that the step S2 specifically comprises the following substeps:
s21, dissolving sodium tellurite and polyvinylpyrrolidone in deionized water, and uniformly stirring to obtain a solution A;
s22, mixing hydrazine hydrate and ammonia water to form a solution B;
s23, adding the solution B into the solution A, and carrying out hydrothermal reaction at the temperature of 160-200 ℃ for 20-40 hours;
s24, obtaining two-dimensional Te after the hydrothermal reaction is finished; and transferring the two-dimensional Te to PDMS to obtain a PDMS substrate containing the two-dimensional Te, namely a substrate II containing the two-dimensional Te.
5. Two-dimensional material based Te/MoS as claimed in claim 1 2 The preparation method of the heterojunction photodetector is characterized in that: step S3, a dry transfer table is adopted to transfer the two-dimensional Te on the second substrate to the two-dimensional MoS on the first substrate 2 Position of (2) to form Te/MoS 2 Van der waals heterojunctions.
6. Two-dimensional material based Te/MoS as claimed in claim 1 2 The preparation method of the heterojunction photodetector is characterized in that S4, electrodes are prepared by adopting a positive photoresist stripping technology in a microelectronic process, the electrodes all adopt a double-layer electrode structure, and the electrodes in contact with Te are a Pd contact layer and an Au conductive layer; and MoS 2 The contacted electrodes are a Ni contact layer and an Au conductive layer; the specific operation is as follows:
s41, adopting laser direct writing pair and MoS 2 Patterning the contacted electrode, and preparing the electrode by magnetron sputtering, wherein the electrode comprisesAnd MoS 2 A Ni contact layer in contact with the Au conductive layer and attached above the Ni contact layer;
s42, patterning an electrode in contact with Te by adopting laser direct writing, and preparing the electrode by adopting magnetron sputtering, wherein the electrode comprises a Pd contact layer in contact with Te and an Au conducting layer attached above the Pd contact layer;
after the preparation of the electrodes in S43, S41 and S42 is finished, the Te/MoS based two-dimensional material is obtained 2 A photodetector prototype of a heterojunction.
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