CN109638091B - Construction method and regulation and control strategy of high-performance hybrid photoelectric detector - Google Patents
Construction method and regulation and control strategy of high-performance hybrid photoelectric detector Download PDFInfo
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Abstract
The invention belongs to the field of nano materials and devices, discloses a construction method of a high-performance mixed type photoelectric detector and a regulation and control strategy thereof, and particularly discloses a high-performance mixed type photoelectric detector based on all-inorganic lead-halogen perovskite nanocrystals, which comprises a single-layer MoS2Layer and CsPbX3(X ═ Cl, Br, I) perovskite nanocrystalline layers, single layer MoS2The layer being of 2D material, CsPbX3The nanocrystalline layer is a 0D material, and the nanocrystalline layer and the 0D material are compounded by constructing a Van der Waals heterojunction. The invention is used for matching single-layer MoS2The key materials for forming the heterojunction and different process steps adopted by characteristic factors of the key materials for forming the heterojunction are explored and improved, and the hybrid photoelectric detector with adjustable/optimized performance is realized. Essentially, this is due to the light trapping capability of the perovskite nanocrystal layer and the photogenerated carriers in 0D perovskite nanocrystals/2D single layer MoS2The exciton separation and charge transfer at the heterojunction interface are effectively regulated and controlled, so that the photoresponse performance of the hybrid photoelectric detector is directly influenced.
Description
Technical Field
The invention belongs to the field of nano materials and devices, and particularly relates to a construction method and a regulation and control strategy of a high-performance hybrid photoelectric detector, which can construct and obtain the high-performance hybrid photoelectric detector based on all-inorganic lead-halogen perovskite nano crystals.
Background
MoS2As a representative of transition metal chalcogenide (TMDs) semiconductor materials, the transition metal chalcogenide semiconductor material has high electron mobility and extremely high on-off ratio, and is a good channel material; the single layer of molybdenum sulfide (i.e., two layers of S atoms and one layer of Mo atoms arranged in the form of S-Mo-S) is a direct bandgap semiconductor with very high quantum efficiency. The photoelectric detector can convert optical signals into electric signals, is one of important electronic devices, and is widely applied to various fields of military affairs and national economy. The photoelectric detector takes a photosensitive material as a channel, ohmic electrodes with low impedance are built at two ends, and the response to light can be completed by forming a passage. The single-layer molybdenum sulfide is used as a two-dimensional semiconductor material, and has extremely high optical response and a wide spectral detection range. But for single-layer molybdenum sulfide, the light absorption capacity is greatly reduced due to the ultra-thin thickness and the narrow spectral absorption range. If the thickness of the material is increased, the dark current will increase accordingly, resulting in a transistor that is insensitive to gate voltage. The purposes of increasing the light absorption efficiency and widening the spectrum without losing other performances can be achieved by modifying the surface of the two-dimensional material. For example, Chen et al improves the light responsivity of the device by four times and shortens the response time by spin-coating Graphene Quantum Dots (GQDs) on the surface of a molybdenum sulfide phototransistor; for example, Huo et al uses HgTe quantum dots to modify molybdenum sulfide phototransistor and uses TiO2Packaging to make the responsivity of the photodetector reach 106A W-1。
Perovskite is used as a novel semiconductor material, and has many advantages, such as high absorption coefficient, high carrier mobility and long carrier diffusion distance, and the absorption wave band covers the whole visible light wave band; adjustable band gap, etc. If the photoelectric sensor can be integrated on a molybdenum sulfide photoelectric transistor, the defects of the molybdenum sulfide photoelectric detector can be effectively overcome. However, since all-inorganic perovskites are easily decomposed in water and oxygen, the conventional method of transferring molybdenum sulfide onto the perovskite thin film substrate is not suitable.
Disclosure of Invention
In view of the above defects or improvement needs of the prior art, the present invention aims to provide a construction method of a high-performance hybrid photodetector and a control strategy thereof, wherein the high-performance hybrid photodetector obtained by construction based on all-inorganic lead-halogen perovskite nanocrystals is used for matching with single-layer MoS2The key material for forming the heterojunction, the characteristic factors of the key material and different process steps adopted by the corresponding preparation method are explored and improved, and the hybrid photoelectric detector with adjustable/optimized performance is realized. The invention controls the key all-inorganic CsPbX in the mixed photoelectric detector3The microstructure and composition of the perovskite nanocrystalline layer are controlled, particularly the specific species and the adhesion amount of ligands attached to the surface of the perovskite nanocrystalline are controlled, and the all-inorganic CsPbX is prepared3CsPbX used for perovskite nanocrystalline layer3Concentration of nanocrystalline solution and all-inorganic CsPbX formed correspondingly3The thickness of the perovskite nanocrystalline layer can realize the performance regulation strategy of the device; correspondingly, the device preparation method can further control the type and content of the adopted nanocrystalline surface ligand and the concentration of the perovskite nanocrystalline solution, so that the photoelectric property of the hybrid photoelectric detector can be effectively regulated, controlled and optimized. Essentially, this is due to the light trapping capability of the perovskite nanocrystal layer and the photogenerated carriers in 0D perovskite nanocrystals/2D single layer MoS2The exciton separation and charge transfer at the heterojunction interface are effectively regulated and controlled, so that the photoresponse performance of the hybrid photoelectric detector is directly influenced.
To achieve the above object, according to one aspect of the present invention, there is provided a hybrid photodetector based on all-inorganic lead-halogen perovskite nanocrystals, characterized in that the hybrid photodetector comprises a single-layer MoS2Layer and MoS located on the single layer2All-inorganic CsPbX on layer3Perovskite nanocrystalline layer, said single layer MoS2The layer comprises two layers of S atoms and one layer of Mo atoms, and X is at least one of Cl, Br and I; wherein the single layer MoS2The layer is made of 2D material, and the all-inorganic CsPbX3The perovskite nanocrystalline layer is made of 0D materials, and Van der Waals heterojunction is constructed between the perovskite nanocrystalline layer and the 0D materials, so that the hybrid photoelectric detector is obtained.
As a further preferred aspect of the present invention, the fully inorganic CsPbX is3The size of the perovskite nanocrystalline in the perovskite nanocrystalline layer is 5-20 nm, and a ligand is further attached to the surface of the perovskite nanocrystalline; preferably, the ligand is an oil, more preferably oleic acid and oleylamine.
As a further preferred aspect of the present invention, the single layer MoS2The thickness of the layer was 0.7 nm.
According to another aspect of the invention, the invention provides a method for preparing the above-mentioned mixed type photoelectric detector based on all-inorganic perovskite nanocrystals, which is characterized in that the method is firstly used for preparing single-layer MoS by an atmospheric pressure chemical vapor deposition method2A layer, and preparing perovskite nanocrystalline by ligand-assisted reprecipitation method, wherein the surface of the perovskite nanocrystalline is adhered with ligand, and the perovskite nanocrystalline is uniformly covered on the single-layer MoS by using spin coating method2Drying to form fully inorganic CsPbX3Perovskite nanocrystalline layer, thus get mixed type photoelectric detector.
As a further preference of the present invention, the ligand is an oil-like substance, preferably oleic acid and oleylamine;
the perovskite nano-crystal is prepared by ligand-assisted reprecipitation, preferably by reacting cesium halide CsX and lead halide PbX2Dissolving in dimethyl formamide solution to form CsPbX3Adding a certain amount of oil ligand into a precursor solution of the nanocrystal, and dripping the precursor solution into toluene to form CsPbX dispersed in toluene3A nanocrystal; then, the CsPbX dispersed in toluene was added3Centrifuging the nanocrystal at high speed by adopting acetonitrile, dispersing the obtained precipitate in toluene again for low-speed centrifugation, and obtaining supernatant fluid which is the purified CsPbX3And (4) nano crystal fine liquid.
In a further preferred embodiment of the present invention, the perovskite nanocrystal prepared by ligand-assisted reprecipitation is prepared by reacting the ligand with the CsPbX3NanocrystalThe ratio of the volume of the precursor solution to the volume of the CsPbX solution is 3:40, and the volume of the ligand to the CsPbX solution is3CsPbX correspondingly contained in precursor solution of nanocrystal3The ratio of the two substances of the nanocrystalline satisfies 3m L: 0.8mmol, and the oleic acid and the oleylamine in the ligand are preferably in a volume ratio of 2: 1;
carrying out centrifugal purification treatment on acetonitrile for 1-4 times; preferably, the number of times of centrifugal purification treatment with acetonitrile is 1;
the arbitrary centrifugal purification treatment by acetonitrile firstly adopts CsPbX3Dispersing the nano-crystal in toluene and acetonitrile according to the volume ratio of 3: 1 proportion of the mixed solution, and then carrying out centrifugal treatment for 5 minutes under the high-speed condition of 11000rpm, wherein the obtained precipitate is the processed CsPbX3A nanocrystal;
the purified CsPbX3A nanocrystalline fine liquid, in particular to CsPbX obtained by centrifugal purification treatment of acetonitrile3Dispersing the nanocrystals in toluene, centrifuging at low speed of 5000rpm for 3 min to obtain supernatant CsPbX3And (4) nano crystal fine liquid.
In a further preferred embodiment of the present invention, the perovskite nanocrystals are uniformly coated on the single layer MoS by spin coating2On the layer, CsPbX with perovskite nano-crystal concentration of 5mg/m L-40 mg/m L is adopted3A nanocrystalline solution, the CsPbX3The solvent in the nanocrystalline solution is toluene; preferably, the CsPbX is3The perovskite nanocrystal concentration of the nanocrystal solution is 5mg/m L, 10mg/m L, 20mg/m L or 40mg/m L, more preferably 40mg/m L.
As a further preferred of the present invention, the single layer MoS is prepared by an atmospheric pressure chemical vapor deposition method2The layer is characterized by comprising the following steps of respectively placing sulfur powder and molybdenum trioxide powder in two quartz boats, placing the quartz boat containing the sulfur powder at the upstream position of carrier gas airflow by using a multi-temperature-zone tube furnace capable of being filled with carrier gas, placing the quartz boat containing the molybdenum trioxide powder at the downstream position of the carrier gas airflow, and reversely arranging a substrate right above the molybdenum trioxide powder; the position of the quartz boat containing the sulfur powder is recorded as the first positionA temperature zone, wherein the position of the quartz boat containing the molybdenum trioxide powder is recorded as a second temperature zone, then, under the condition of continuously introducing carrier gas, the second temperature zone is heated to 780-800 ℃, the temperature of the first temperature zone affected by the heat radiation of the second temperature zone is not more than 75 ℃, then the first temperature zone and the second temperature zone are simultaneously heated, wherein the first temperature zone is heated to 180 ℃ within 5 minutes and then the heating is finished, the second temperature zone is continuously heated to 850 ℃ and is kept for 5 minutes and then the heating is finished, and the deposited MoS can be obtained on the substrate after cooling2A layer;
the carrier gas is argon.
More preferably, the sulfur powder is 100mg, the molybdenum trioxide powder is 10mg, the carrier gas is introduced so that the volume flow rate is stabilized at 100SCCM, and the substrate is SiO2a/Si substrate; preferably, the target deposition surface of the substrate is located at a vertical distance of 3mm directly above the molybdenum trioxide powder.
In a further preferred embodiment of the present invention, the perovskite nanocrystals are uniformly coated on the single layer MoS by the spin coating method2Before layering, the monolayer MoS2The surface of the layer is also prepared with a conductive electrode through photoetching treatment and electron beam thermal evaporation treatment.
In a further preferred embodiment of the present invention, the conductive electrode is at least one of a Cr electrode and an Au electrode.
Compared with the prior art, the technical scheme has the advantages that the cesium-lead halide-based perovskite nanocrystalline is matched with the single-layer molybdenum sulfide to form a heterojunction structure (the two are compounded by constructing a Van der Waals heterojunction in particular), the energy band matching is good, the perovskite nanocrystalline and the molybdenum sulfide have proper work function difference, the work function difference leads photogenerated carriers to be effectively separated under the action of an internal electric field after the two materials are contacted, and then a photocurrent signal is generated, so that the cesium-lead halide-based (CsPbX) is obtained3X ═ Cl, Br, I) perovskite nanocrystals/single layer molybdenum sulfide MoS2A high performance hybrid photodetector with (zero/two dimensional) heterojunctions. The invention is particularly realized by the solution concentration and the surface preparation of the perovskite nanocrystalThe further optimized regulation and control of the body content realizes the effective modulation and optimization of the photoelectric property of the hybrid photoelectric detector and provides a new strategy for regulating and controlling the performance of the device.
The method utilizes the performance advantage of the all-inorganic perovskite, and is more favorable for synthesizing an efficient hybrid detector. The invention adopts a mode of directly carrying the perovskite nanocrystalline solution on molybdenum sulfide through spin coating to construct a device, and can effectively avoid the decomposition of the all-inorganic perovskite. Taking X as Br as an example, the invention specifically comprises the following steps: preparation of CsPbBr by ligand-assisted reprecipitation3In the nanocrystalline solution, the ligand can be oil substances (such as oleic acid and oleylamine), and the regulation and control of the solution concentration and the surface ligand content are realized by changing the volume amount of the toluene solvent and the times of centrifugal purification treatment. CsPbBr under these different conditions3The nanocrystals are uniformly covered in the single-layer MoS grown by CVD2The surface of the material forms a composite film structure due to CsPbBr3The nanocrystalline has excellent light absorption characteristics, so that the hybrid device can generate a large number of photo-generated charge carrier pairs under the condition of light radiation, and efficient charge transfer is generated at an interface, so that the photocurrent is greatly increased. In addition, the centrifugal purification treatment of acetonitrile is adopted in the invention, and the centrifugal purification treatment of toluene and acetonitrile is preferably performed by using a solvent prepared by mixing toluene and acetonitrile in a volume ratio of 3: the mixed solution with the proportion of 1 can avoid the aggregation of the nanocrystalline easily caused by the overlarge proportion of the acetonitrile, and is not beneficial to the monodispersity and the quantum confinement effect of the nanocrystalline.
The preparation method can realize single-layer MoS2Constructing a transistor, specifically preparing perovskite nanocrystalline by using a ligand-assisted reprecipitation method, wherein the perovskite nanocrystalline has good monodispersity and uniform size; single layer MoS2Is prepared by an atmospheric pressure chemical vapor deposition method (APCVD), and has excellent crystallinity; then the nano-crystals are uniformly covered on the MoS by a simple spin coating method2And obtaining the mixed type photoelectric detector on the transistor.
The invention further realizes the effective modulation and optimization of the photoelectric property of the mixed photoelectric detector by optimally regulating and controlling the solution concentration and the surface ligand content of the perovskite nanocrystalline. Specifically, the higher the concentration of the perovskite nanocrystals is, the stronger the light absorption capability of the formed perovskite thin film is, so that the hybrid device of the perovskite solution with high concentration has higher photocurrent; in this study, as the number of times of centrifugation increases, the number of surface defects of the nanocrystals gradually increases, and the recombination of holes and electrons is likely to occur on the surface of the nanocrystals, resulting in a decrease in photocurrent. This provides a new approach for regulating and optimizing the performance of the hybrid photodetector.
The invention provides a regulation strategy/means for the performance of the hybrid photoelectric detector. According to the all-inorganic perovskite nanocrystalline, the concentration of the solution is optimized, so that better light capture capacity can be obtained, and more photon-generated carriers can be effectively separated at a heterojunction interface; in addition, the organic ligand insulating layer on the surface of the nanocrystal has an important regulation and control function on the transfer efficiency of a photon-generated carrier and is also a key factor influencing the photoresponse performance of the photoelectric detector. The invention is based on CsPbBr3Nanocrystalline/single layer MoS2(0D/2D) heterojunction high-performance hybrid photodetector, and CsPbBr with the concentration of 5mg/m L-40 mg/m L (especially 5mg/m L, 10mg/m L, 20mg/m L and 40mg/m L) is respectively obtained by changing the volume amount of toluene solvent3A nanocrystalline solution; the content of the ligand on the surface of the nanocrystalline is regulated and controlled by regulating and controlling the centrifugal purification treatment times, so that the purpose of regulating and optimizing the performance of the mixed photoelectric detector is realized. The invention regulates and controls the content of the ligand on the surface of the nanocrystalline by regulating and controlling the centrifugal purification treatment times, thereby realizing the purpose of regulating and controlling and optimizing the performance of the mixed photoelectric detector.
In conclusion, the invention provides a new controllable and optimized strategy of the 0D/2D hybrid photoelectric detector, and has the characteristics of simplicity, feasibility, low cost and good stability.
Drawings
FIG. 1 is a MoS prepared by APCVD2Surface Scanning Electron Microscope (SEM) images of (a).
FIG. 2 is CsPbBr prepared by ligand-assisted reprecipitation3Transmission Electron Microscopy (TEM) images of the nanocrystals.
FIG. 3 is CsP prepared by ligand assisted reprecipitationbBr3A physical diagram of the nanocrystal. I, II, III and IV at the upper part of the figure 3 respectively show a real object diagram of the nanocrystalline solution after different times of centrifugal purification treatment under the radiation of a fluorescent lamp; the I, II, III and IV at the lower part of the figure 3 respectively show a real object diagram of the nanocrystalline solution after different times of centrifugal purification treatment under 365nm ultraviolet lamp radiation, and the green fluorescence of the solution gradually weakens from the I to the IV, which shows that the content of the ligand on the surface of the nanocrystalline gradually decreases with the increase of the times of purification treatment, and the fluorescence quenching phenomenon is more and more obvious.
FIG. 4 is based on CsPbBr3Nanocrystalline/single layer MoS2Device schematic diagram of heterojunction hybrid photodetector.
FIG. 5 is based on CsPbBr3Nanocrystalline/single layer MoS2The light responsivity of the heterojunction mixed type photoelectric detector changes with the concentration.
FIG. 6 is based on CsPbBr3Nanocrystalline/single layer MoS2The light responsivity of the heterojunction mixed type photoelectric detector is along with the trend chart of the centrifugal purification treatment times (namely the ligand content on the surface of the nanocrystalline is gradually reduced).
FIG. 7 is based on CsPbBr3Nanocrystalline/single layer MoS2The current-time diagram of the heterojunction hybrid photodetector operating stably for 30 minutes.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1
The invention is based on CsPbBr3Nanocrystalline/single layer MoS2The preparation method of the heterojunction hybrid photoelectric detector mainly comprises the following steps:
(1) based on pure MoS2Preparation of a photodetector
1) First, a substrate, such as SiO2A (300nm)/Si substrate, the size of which can be 10mm × 13mm, is placed on a silicon wafer cleaning rack, ultrasonic treatment is carried out for 15 minutes respectively according to the sequence of acetone, alcohol, deionized water and alcohol, and then nitrogen is used for blow-drying for standby.
2) 10mg of MoO3The powder is uniformly scattered on a quartz boat, the cleaned substrate is placed on the quartz boat in an inverted and parallel mode, the quartz boat is placed in a quartz tube, 100mg of sulfur powder is poured into the quartz boat with two closed ends and placed in the quartz tube, the two quartz boats are respectively placed in the central areas of two temperature areas of a tube furnace (the tube furnace is at least provided with two temperature areas), the quartz boat for placing the sulfur powder is arranged at the upstream, and the other quartz boat is arranged at the downstream (namely, the two quartz boats containing 100mg of sulfur powder and 10mg of molybdenum trioxide powder are respectively placed in the middle positions of the two temperature areas at the upstream and the downstream of the tube furnace). The air pump was turned on to purge the gas for 5 minutes in order to evacuate the air so that the entire gas path was filled with high purity argon. After the gas washing is finished, the gas flow is adjusted to 100SCCM, the pressure is adjusted to normal pressure, then the temperature of the high-temperature region is raised firstly, when the temperature is raised from room temperature (20 ℃) to 790 ℃ (or raised to other temperature values within the range of 780-800 ℃), the temperature of the low-temperature region is raised, the temperature is raised from 75 ℃ for 5 minutes to 180 ℃, then the program is stopped, the temperature of the high-temperature region is raised to 850 ℃, the temperature is maintained for 5 minutes, the program is stopped, and the high-temperature region is naturally cooled to room temperature. Obtaining the single-layer triangular MoS with the thickness of about 0.7nm and uniform and compact distribution2. And (3) introducing 100SCCM argon gas in the whole process from the beginning of temperature rise treatment to the moment before the two temperature regions stop heating, and cooling the obtained product to room temperature along with the furnace after the reaction is stopped.
3) Dropping a proper amount of photoresist on a substrate on which a material is grown, wherein the rotation speed of a spin coater is 1000 revolutions per minute (rpm) for 10s, and then the rotation speed is rapidly increased to 4000rpm for 60 s.
4) And (3) heating the silicon wafer after glue homogenizing on a hot table at 95 ℃ for 5 minutes to remove solvent molecules in the glue and enable the glue to be firmly combined with the substrate.
5) The type of the used photoetching machine is Mask Aligner-MDA-400M, the power of a mercury lamp light source is 350W, the wavelength is 350 nm-450 nm, the exposure time is 4s, the Mask layout used in exposure can be in the shape of an insert finger, and the length of a channel in a unit area can be effectively increased. The channel width of the reticle interdigitated electrodes was 10 μm.
6) The photoresist used is a positive photoresist, i.e., the exposed portions will dissolve in the developer. The developing solution is tetramethylammonium hydroxide aqueous solution (can be 25% mass concentration), and the solution and water can be uniformly mixed according to the volume ratio of 1:7, then the exposed silicon wafer is immersed into the solution and gently shaken for 45s, so that the exposed part is dissolved. The developed pattern has clear boundary and no undissolved photoresist, which represents the success of the photoetching process and can be used for preparing the electrode film.
7) The electrode preparation is carried out by adopting an electron beam thermal evaporation mode, and the thicknesses of the electrode preparation are respectively Cr 10nm and Au 50 nm.
8) The step is to expose the channel material portion, i.e. the portion that is not dissolved in the developing process, so as to realize the separation of the source and drain electrodes. The silicon wafer bubble is heated in acetone at 60 ℃ for 30 minutes, and then the silicon wafer bubble is subjected to ultrasonic treatment in the acetone for about 20 seconds to complete the stripping. And finishing the preparation of the transistor after the stripping process.
(2) Perovskite nanocrystal preparation
Weighing cesium bromide and lead bromide powder with equal mole number (0.4mmol) and placing the cesium bromide and lead bromide powder into a beaker with the thickness of 100m L, adding 20m L dimethyl formamide (DMF) solution, and adding a certain amount of oleic acid and oleylamine as ligands (the volume of the ligands is equal to that of CsPbX) while continuously stirring3The volume ratio of the precursor solution is 3:40, oleic acid and oleylamine in the ligand are mixed according to the volume ratio of 2: 1), thus obtaining the nanocrystalline precursor solution after the ligand is applied, in addition, 10m L toluene solution is poured into a 25m L beaker and is placed on a stirring table for continuous stirring, then a liquid-transferring gun is used for slowly dripping 350 mu L precursor solution into the toluene solution, at the moment, the solution immediately turns into yellow green, after the solution is continuously stirred for a few minutes, the obtained solution is added into a certain amount of acetonitrile solution and then is centrifuged for 5 minutes at the rotating speed of 11000rpm (the volume of the acetonitrile solution is specifically one third of the volume of the obtained solution, namely 3.45m L acetonitrile solution is added), after the supernatant is removed, a certain amount of acetonitrile solution is added, and thenAnd (3) centrifuging the toluene solution for 3 minutes at the rotating speed of 5000rpm, and finally obtaining supernatant, namely the cesium lead bromoperovskite quantum dot solution.
CsPbBr with different characteristics is prepared by regulating and controlling the volume of toluene solvent and the centrifugal purification treatment frequency of acetonitrile solution3A nanocrystal solution comprising:
1) the purification treatment frequency is 1 time (namely, the prepared nanocrystalline solution is added with acetonitrile solution and then is centrifuged for 1 time at a high speed of 11000rpm, finally, the precipitate is dispersed in toluene and is centrifuged for 1 time at a low speed of 5000 rpm), and the concentration is 5mg/m L nanocrystalline solution;
2) 1 time of purification treatment, and the concentration is 10mg/m L nanocrystalline solution;
3) 1 time of purification treatment, and 20mg/m L of nanocrystalline solution;
4) the purification treatment times are 1 time, and the concentration is 40mg/m L nanocrystalline solution;
5) the concentration of the nanocrystalline solution is 20mg/m L, and the purification treatment time is 2 times (namely, the prepared nanocrystalline solution is added with acetonitrile solution and then is centrifuged for 2 times at a high speed of 11000rpm, finally, the precipitate is dispersed in toluene and is centrifuged for 1 time at a low speed of 5000 rpm);
6) the concentration of the nanocrystalline solution is 20mg/m L, and the purification treatment time is 3 times (namely, the prepared nanocrystalline solution is added with acetonitrile solution and then is centrifuged for 3 times at a high speed of 11000rpm, finally, the precipitate is dispersed in toluene and is centrifuged for 1 time at a low speed of 5000 rpm);
7) the concentration of the nanocrystal solution is 20mg/m L, and the purification treatment time is 4 times (i.e., the prepared nanocrystal solution is added with acetonitrile solution and then centrifuged at 11000rpm for 4 times at high speed, and finally the precipitate is dispersed in toluene and centrifuged at 5000rpm for 1 time).
And (3) carrying out centrifugal purification treatment on acetonitrile for different treatment times to obtain the nanocrystalline with different ligand contents. The arbitrary centrifugal purification treatment by acetonitrile is to make CsPbX3Dispersing the nano-crystal in a mixed solution of toluene and acetonitrile (volume ratio of 3: 1), centrifuging at 11000rpm for 5 min to obtain precipitateAre nanocrystals with different ligand contents. Finally, dispersing the sediment in a toluene solution, and carrying out centrifugal treatment for 3 minutes under the condition of low speed of 5000rpm, wherein the obtained supernatant is CsPbX3And (4) nano crystal fine liquid.
The perovskite nanocrystalline preparation process is carried out in the air, and moisture and oxygen in the air do not need to be isolated.
(3) Preparation of photoelectric detector based on all-inorganic perovskite quantum dot-single-layer molybdenum sulfide heterojunction
Take 50. mu. L CsPbBr with pipette3The nanocrystal solution was slowly dropped on the device, rotated on a spin coater at 1500rpm for 20 seconds, and then heated on a hot stage at a temperature of 80 ℃ for 1 minute to volatilize the toluene solvent, thereby obtaining the photodetector.
The change trends of the light responsivity of the device are shown in figures 5 and 6 (the structures of all the devices are similar and are all shown in figure 4), along with the increase of the concentration of the nanocrystals, the light responsivity of the device is gradually improved, along with the increment of the centrifugal purification treatment times (the ligand content on the surface of the nanocrystals is decreased), the light responsivity is gradually reduced, the change trends are closely related to the light trapping capacity of a perovskite layer and the charge transfer efficiency of a photogenerated carrier at a heterojunction interface, in addition, the mixed type photoelectric detector shows better work durability, and the CsPbBr of which the purification treatment times are 1 and the concentration is 20mg/m L is shown in figure 73As can be seen from FIG. 7, the mixed device constructed by the nanocrystalline solution has no obvious attenuation of photoresponse current after continuous operation for half an hour. Therefore, the all-inorganic perovskite has the advantages in performance, so that the all-inorganic perovskite is more beneficial to constructing an efficient hybrid detector.
The thickness of the perovskite nanocrystalline layer can be adjusted by CsPbX with different perovskite nanocrystalline concentrations3Adjusted by a nanocrystalline solution (e.g., CsPbX in the above-described embodiment)3The concentration of perovskite nano-crystal in the nano-crystal solution is 5mg/m L-40 mg/m L), and the concentration is equal to thatThe resulting fully inorganic CsPbX3The thickness of the perovskite nanocrystalline layer is in direct proportion; as shown in FIG. 5, in the embodiment of the present invention, CsPbX3The concentration of the perovskite nanocrystals in the nanocrystal solution is optimally 40mg/m L, which shows that the light capture capacity is continuously improved along with the increase of the concentration of the nanocrystals (namely, the thickness of the nanocrystal layer). the perovskite nanocrystals obtained in the above embodiment have an average size of about 10nm and a size fluctuation within a range of 5-20 nm.
The number of times of centrifugal purification treatment affects the amount of ligand on the surface of the nanocrystal, and the amount of ligand on the surface of the nanocrystal gradually decreases with the increase of the number of times of treatment. In addition to the optimal centrifugal purification treatment times given in the above embodiments, the centrifugal purification times corresponding to the optimal performance of the device can be flexibly adjusted according to actual conditions; for example, when the initial ligand is sufficiently large (in this case, when the perovskite nanocrystal is prepared by the ligand-assisted reprecipitation method, the amounts of the ligand oleic acid and oleylamine are also sufficiently large), the optimum number of centrifugal purifications may be two or three. The optimum number of centrifugal cleaning treatments for the above example was 1, and also illustrates the ligand volume used during perovskite nanocrystal preparation and the raw CsPbX without added ligand3The volume ratio of the precursor solution is 3:40, the volume of the ligand and CsPbX3Nominal CsPbX correspondingly contained in precursor solution of nano crystal3The ratio of the two substances of the nanocrystalline meets 3m L: 0.8mmol, and the oleic acid and the oleylamine in the ligand are proportioned according to the volume ratio of 2:1, so that the amount of the initial ligand attached to the surface of the nanocrystalline is moderate.
In addition to cesium lead bromoperovskite nanocrystals, other halogen-corresponding cesium lead halides (CsPbX) may also be employed3X ═ Cl, Br, I) perovskite nanocrystals.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (19)
1. Mixed light based on all-inorganic lead-halogen perovskite nanocrystallineAn electrical detector, wherein the hybrid photodetector comprises a single layer MoS2Layer and MoS located on the single layer2All-inorganic CsPbX on layer3Perovskite nanocrystalline layer, said single layer MoS2The layer comprises two layers of S atoms and one layer of Mo atoms, and X is at least one of Cl, Br and I; wherein the single layer MoS2The layer is made of 2D material, and the all-inorganic CsPbX3The perovskite nanocrystalline layer is made of 0D materials, and Van der Waals heterojunction is constructed between the perovskite nanocrystalline layer and the 0D materials, so that the hybrid photoelectric detector is obtained.
2. The hybrid photodetector based on all-inorganic lead-halogen perovskite nanocrystals as claimed in claim 1, wherein the all-inorganic CsPbX3The size of the perovskite nanocrystalline in the perovskite nanocrystalline layer is 5-20 nm, and a ligand is further attached to the surface of the perovskite nanocrystalline.
3. The hybrid photodetector based on all-inorganic lead-halogen perovskite nanocrystals as claimed in claim 2, wherein the ligand is an oil substance.
4. The hybrid photodetector based on all-inorganic lead-halogen perovskite nanocrystals as claimed in claim 3, wherein the ligands are oleic acid and oleylamine.
5. The hybrid photodetector based on all-inorganic lead-halogen perovskite nanocrystals as claimed in claim 1, wherein the single layer MoS is2The thickness of the layer was 0.7 nm.
6. The method for preparing the hybrid photodetector based on all-inorganic lead-halogen perovskite nanocrystals according to any one of claims 1 to 5, wherein the method comprises preparing a single-layer MoS by atmospheric pressure chemical vapor deposition2A layer, and preparing perovskite nanocrystalline by ligand-assisted reprecipitation method, wherein the surface of the perovskite nanocrystalline is adhered with ligand, and the perovskite nanocrystalline is uniformly covered on the single-layer MoS by using spin coating method2Drying to form fully inorganic CsPbX3Perovskite nanocrystalline layer, thus get mixed type photoelectric detector.
7. The method of claim 6, wherein the ligand is an oil-like substance;
the perovskite nano-crystal is prepared by ligand-assisted reprecipitation method through mixing cesium halide CsX and lead halide PbX2Dissolving in dimethyl formamide solution to form CsPbX3Adding a certain amount of oil ligand into a precursor solution of the nanocrystal, and dripping the precursor solution into toluene to form CsPbX dispersed in toluene3A nanocrystal; then, the CsPbX dispersed in toluene was added3Centrifuging the nanocrystal at high speed by adopting acetonitrile, dispersing the obtained precipitate in toluene again for low-speed centrifugation, and obtaining supernatant fluid which is the purified CsPbX3And (4) nano crystal fine liquid.
8. The method of claim 7, wherein said ligand and said CsPbX are used to produce perovskite nanocrystals by ligand-assisted reprecipitation3The volume ratio of the precursor solution of the nanocrystal to the precursor solution of the nanocrystal is 3:40, and the volume of the ligand to the CsPbX3CsPbX correspondingly contained in precursor solution of nanocrystal3The ratio of the two amounts of the substances of the nanocrystalline satisfies 3m L: 0.8 mmol;
carrying out centrifugal purification treatment on acetonitrile for 1-4 times;
the arbitrary centrifugal purification treatment by acetonitrile firstly adopts CsPbX3Dispersing the nano-crystal in toluene and acetonitrile according to the volume ratio of 3: 1 proportion of the mixed solution, and then carrying out centrifugal treatment for 5 minutes under the high-speed condition of 11000rpm, wherein the obtained precipitate is the processed CsPbX3A nanocrystal;
the purified CsPbX3A nanocrystalline fine liquid, in particular to CsPbX obtained by centrifugal purification treatment of acetonitrile3Dispersing the nanocrystals in toluene, centrifuging at low speed of 5000rpm for 3 min to obtain supernatant CsPbX3NanocrystalAnd (5) fine liquid.
9. The method of claim 8, wherein the number of centrifugal purification treatments with acetonitrile is 1.
10. The method of claim 8, wherein the ligands are oleic acid and oleylamine.
11. The method of claim 10, wherein said oleic acid and said oleylamine of said ligand are present in a 2:1 ratio by volume.
12. The method according to claim 6, wherein the perovskite nanocrystals are uniformly coated on the single layer MoS by spin coating2On the layer, CsPbX with perovskite nano-crystal concentration of 5mg/m L-40 mg/m L is adopted3A nanocrystalline solution, the CsPbX3The solvent in the nanocrystal solution is toluene.
13. The method of claim 12, wherein the CsPbX3The perovskite nanocrystal concentration of the nanocrystal solution is 5mg/m L, 10mg/m L, 20mg/m L or 40mg/m L.
14. The method of claim 12, wherein the CsPbX3The perovskite nanocrystal concentration of the nanocrystal solution is 40mg/m L.
15. The method of claim 6, wherein the single layer MoS is prepared by atmospheric pressure chemical vapor deposition2The layer is characterized by comprising the following steps of respectively placing sulfur powder and molybdenum trioxide powder in two quartz boats, placing the quartz boat containing the sulfur powder at the upstream position of carrier gas airflow by using a multi-temperature-zone tube furnace capable of being filled with carrier gas, placing the quartz boat containing the molybdenum trioxide powder at the downstream position of the carrier gas airflow, and reversely arranging a substrate right above the molybdenum trioxide powder; recording the position of the quartz boat containing the sulfur powder as a first temperature zone, and recording the positions of the quartz boat containing the sulfur powder as three temperature zonesThe method comprises the steps of arranging a quartz boat of molybdenum oxide powder in a second temperature zone, heating the second temperature zone to 780-800 ℃ under the condition of continuously introducing carrier gas, enabling the temperature of the first temperature zone not to exceed 75 ℃ under the influence of heat radiation of the second temperature zone, simultaneously heating the first temperature zone and the second temperature zone, heating the first temperature zone to 180 ℃ within 5 minutes, finishing heating, continuously heating the second temperature zone to 850 ℃ and finishing heating after heat preservation for 5 minutes, and obtaining deposited MoS on a substrate after cooling2A layer;
the carrier gas is argon.
16. The method of claim 15, wherein the sulfur powder is 100mg, the molybdenum trioxide powder is 10mg, the carrier gas is introduced at a volume flow rate of 100SCCM, and the substrate is SiO2a/Si substrate.
17. The method of claim 16, wherein the target deposition surface of the substrate is located a vertical distance of 3mm directly above the molybdenum trioxide powder.
18. The method according to claim 6, wherein the perovskite nanocrystals are uniformly coated on the single layer MoS by spin coating2Before layering, the monolayer MoS2The surface of the layer is also prepared with a conductive electrode through photoetching treatment and electron beam thermal evaporation treatment.
19. The method of claim 18, wherein the conductive electrode is at least one of a Cr electrode and an Au electrode.
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