CN110176518B - Communication waveband infrared detector and preparation method thereof - Google Patents
Communication waveband infrared detector and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a communication waveband infrared detector and a preparation method thereof, wherein the infrared detector comprises Bi growing on a substrate2S3A nanoflake channel layer, an electrode layer grown on the channel layer, the electrode layer having an opening therein, a large-sized PbS quantum dot photoactive layer grown in the opening; the infrared detector of the invention contains Bi2S3the-PbS mixed system overcomes the interface Fermi level pinning effect existing in the prior mixed system and maintains Bi2S3Inherent high mobility and gate voltage controllability, large optical gain and low noise are realized; the infrared detector has wide wave spectrum, millisecond order fast response and high sensitivity, and can be widely applied to important fields of optical communication, medical imaging and the like; in addition, the preparation method has simple process, mature technology, operation at room temperature and low cost, and is very favorable for large-scale preparation and application.
Description
Technical Field
The invention relates to the field of detectors, in particular to a communication waveband outer detector and a preparation method thereof.
Background
The photoelectric detection technology is the core of a plurality of technologies influencing the modern life of human beings, and greatly enriches and facilitates the daily life of people; in particular, the infrared detector in the communication band (with the advantages of long working distance, strong penetration ability, good anti-interference performance, etc., has very wide and important application in the fields of military affairs, industry, medicine, security, etc. although the traditional film semiconductor (such as InGaAs, InSb, etc.) detector has mature process, it also faces the problems of difficult material preparation, complex process, low-temperature operation, high cost, etc. therefore, the development of new materials and new structures is urgently needed to meet the fast development demand of the infrared detection technology which is continuously improved
Recently, with the rapid development of low-dimensional materials (including two-dimensional atomic crystals and sol quantum dots), important advantages such as unique atomic/electronic structure, strong light-matter interaction, easy large-scale preparation, CMOS compatibility and the like are combined, especially two-dimensional-quantum dot mixed material system (such as graphene-quantum dot mixed material system)Dot, MoS2Quantum dots) have become a candidate material system for a new generation of low cost high performance infrared detectors. However, the mixed system developed in the past has the problems of fermi level pinning effect at the interface and the like, so that larger dark current and noise are easily caused, and the sensitivity and the response time of the device are reduced; meanwhile, the surface of the two-dimensional atomic crystal has no dangling bond, so that the quantum dots are simply stacked on the surface of the two-dimensional semiconductor, and the efficient charge transfer between the quantum dots and the two-dimensional semiconductor is seriously influenced.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention mainly aims to provide a communication waveband infrared detector and a preparation method thereof, and based on the purpose, the invention at least adopts the following technical scheme:
the preparation method of the communication waveband infrared detector comprises the following steps:
preparing Bi on the surface of a silicon oxide substrate2S3A nanoflake;
in the presence of Bi2S3Preparing an electrode layer on the surface of the nano sheet, wherein the electrode layer is provided with an opening;
preparing large-size PbS quantum dots, and preparing the large-size PbS quantum dots into a large-size PbS quantum dot solution with a specific concentration;
growing the large-size PbS quantum dot solution with the specific concentration layer by layer and spin-coating the solution into the opening;
and annealing in inert gas after the layer-by-layer growth is carried out, so as to obtain the communication waveband infrared detector.
Further, preparing Bi2S3In the step of preparing the nano-sheet, the physical vapor deposition method is adopted to prepare Bi2S3The deposition temperature of the nano-flake is 600-850 ℃, the deposition time is 5-10 minutes, and the Bi is2S3The thickness of the nano-flake is 20-30 nm.
Furthermore, in the step of preparing the electrode, laser direct writing and evaporation technology are adopted to prepare the Bi2S3Preparing electrode layers of 1-5nmTi layers and 40-80nmAu layers on the surface of the nano sheet in sequence, wherein the electrode layers are made of metal materialsAn opening is formed in the layer, the opening exposing the Bi2S3The length of the opening on the surface of the nano-flake is 2-20 μm, and the width of the opening is 5-30 μm.
Further, in the step of preparing the large-size PbS quantum dots, 0.4-5g of lead oxide is added into 4-50ml of oleic acid, stirred for 6-24 hours under the conditions of vacuum and 60-100 ℃, then 15-100ml of 1-octadecene is added, and the temperature is raised to 120-160 ℃; after reaching the specified temperature, adding 1-10mmol TMS; and finally, centrifugally cleaning for 2-5 times, and dissolving into toluene, wherein the concentration of the large-size PbS quantum dots in the toluene solution is 20-60 mg/ml.
Further, after the electrode layer preparation step and before the layer-by-layer growth spin coating step, annealing the electrode layer in inert gas at the annealing temperature of 80-150 ℃ for 0.5-2 hours; in the annealing after the layer-by-layer growth, the annealing temperature is 80-150 ℃, and the annealing time is 5-20 minutes.
Further, in the step of layer-by-layer growth spin coating, the number of growth layers is 1-10, and the process of growing 1 layer is specifically as follows: the substrate is placed on a rotating platform, the rotating speed is set to be 1000-3500rpm, and 1-5 drops of acetonitrile, 1-5 drops of toluene, 2-3 drops of 20-60mg/ml quantum dots, 1-2 drops of 2% EDT and 1-5 drops of acetonitrile are sequentially dropped on the surface of the substrate.
Further, the method also comprises the step of preparing Bi2S3Before the nano-sheet, sequentially performing ultrasonic treatment on the silicon oxide substrate by using soapy water, acetone and isopropanol for 10-30min respectively; then cleaning for 3-10min in ozone ultraviolet or oxygen plasma with oxygen flow of 30-80sccm and plasma power of 80-150W.
Communication wave band infrared detector, it includes:
a substrate;
bi grown on the substrate2S3A nanoflake channel layer;
an electrode layer grown on a side of the channel layer facing away from the substrate, the electrode layer having an opening therein, the opening exposing a surface of the channel layer;
and the large-size PbS quantum dot photosensitive layer is grown in the opening.
Further, said Bi2S3The thickness of the nano-thin sheet channel layer is 20-30 nm; the diameter of the large-size PbS quantum dot is 5-20 nm.
Further, the electrode layer is a double-layer structure with a bottom layer of 1-5nm Ti layer and a top layer of 40-80nm Au layer, the length of the opening is 2-20 μm, and the width is 5-30 μm; the substrate comprises a Si substrate and SiO on the Si substrate2And (3) layer structure.
Compared with the prior art, the invention has at least the following beneficial effects:
bi obtained by the method of the invention2S3The surface of the nano sheet is provided with a large number of sulfur vacancies which have a large number of surface dangling bonds, so that the effective crosslinking of PbS quantum dots is facilitated, and the more efficient charge transfer between the PbS quantum dots and the PbS quantum dots can be promoted; bi in the infrared detector of the invention2S3the-PbS mixed system overcomes the interface Fermi level pinning effect existing in the prior mixed system and maintains Bi2S3Inherent high mobility and gate voltage controllability, large optical gain and low noise are realized; the infrared detector of the invention has wide spectrum (1.8 μm), fast response (millisecond order), high sensitivity (response degree up to 10)4A/W, detectivity over 1011Jones), can be widely applied to important fields such as optical communication, medical imaging and the like; in addition, the preparation method has simple process, mature technology, operation at room temperature and low cost, and is very favorable for large-scale preparation and application.
Drawings
FIG. 1 shows a composition containing Bi2S3An infrared detector of a nanosheet, an optical microscopy image of the infrared detector of the present invention, and a schematic structural view of the infrared detector of the present invention.
FIG. 2 shows a composition containing Bi2S3The invention relates to an infrared detector of a nano sheet and a performance test chart of the infrared detector.
Detailed Description
The present invention will be described in further detail below.
In FIG. 1, a is a group containing Bi2S3The optical microscope picture of the infrared detector of the nanosheet, b is the optical microscope picture of the infrared detector of the present invention, and c is the structural schematic diagram of the infrared detector of the present invention. As shown in fig. 1, the infrared detector of the communication band of the present invention includes: a substrate comprising a Si substrate and SiO on the surface of the Si substrate2Layer of SiO2Bi on the surface of the layer2S3A nano-platelet channel layer in Bi2S3An electrode layer on the surface of the nano-sheet channel layer, the electrode layer having an opening therein, the opening exposing the Bi2S3The surface of the nano-sheet channel layer, and a large-size PbS quantum dot layer, Bi, grown in the opening2S3The surface of the nano sheet is beneficial to effective crosslinking of PbS quantum dots due to a large number of surface dangling bonds in an S space, and more efficient charge transfer between the PbS quantum dots and the PbS quantum dots is promoted; in addition, Bi2S3Bi is formed between the bismuth (III) and PbS2S3the-PbS mixed system overcomes the interface Fermi level pinning effect existing in the prior mixed system and maintains Bi2S3Inherent high mobility and gate voltage tunability, large optical gain and low noise are achieved.
The electrode layer is of a double-layer structure comprising a Ti layer/Au layer, the thickness of the Ti layer is 1-5nm, and preferably, the thickness of the Ti layer is 2 nm; the thickness of the Au layer is 40-80nm, preferably 70nm, and the Ti layer contacts the Bi layer2S3A nanoflake channel layer having a thickness of 1-80nm, an opening in the electrode layer having a length of 2-20 μm and a width of 5-30 μm.
The following describes a method for manufacturing the infrared detector with the communication waveband in detail, and the method for manufacturing the infrared detector with the communication waveband comprises the following steps:
step 1, taking SiO2Cleaning of SiO on Si substrate2Si substrate: sequentially placing the substrate in soap water, acetone and isopropanol solution, and performing ultrasonic treatment for 20 min; then, the substrate is placed in ozone ultraviolet or oxygen plasma for cleaning for 5min, the oxygen flow is 50sccm, and the plasma power is 100W;
step 2: preparation of Bi by physical vapor deposition2S3Nano-flake: 50mg Bi2S3Putting the powder in a quartz boat, and putting the quartz boat in a middle heat preservation area of a quartz tube of a horizontal tube furnace; at a distance to contain Bi2S3Placing another quartz boat at the downstream end of 12cm of the powder quartz boat, and placing 2 SiO pieces2the/Si substrate is placed in a quartz boat with the right side facing upwards; introducing inert gas into the quartz tube at normal temperature for 20 minutes, completely exhausting the air in the tube, regulating the flow rate of gas to be less than 50sccm, heating the high-temperature tube furnace to 850 ℃, and growing for 10 minutes; and naturally cooling to room temperature after the reaction is completed, and taking out the sample to finish the preparation of the sample. The Bi2S3The growth thickness of the nano-flake is 20-30 nm.
And step 3: by adopting laser direct writing and evaporation process, in Bi2S3Preparing 1-5nmTi/40-80nmAu electrode layer on the surface of the nano-flake, preferably, the thickness of the Ti layer is 2nm, the thickness of the Au layer is 70nm, the electrode layer is formed with an opening, the length of the opening is 2-20 μm, the width of the opening is 5-30 μm, and the opening exposes Bi2S3A nanoflake surface; then annealing in inert gas of nitrogen and argon at 80-150 deg.C for 0.5-2 hr to improve the quality of electric contact, thereby obtaining a substrate with an open electrode.
And 4, step 4: preparing large-size PbS quantum dots, and preparing the large-size PbS quantum dots into a large-size PbS quantum dot solution with a specific concentration, wherein the specific process comprises the following steps: adding 0.45g of lead oxide (PbO) into 4.5ml of oleic acid, and stirring for 12 hours under vacuum at 85 ℃; then 15ml of 1-octadecene is added, and the temperature is raised to 120-160 ℃; after reaching the specified temperature, 1mmol of Tetramethylsilane (TMS) was added; and finally, centrifugally cleaning for 3 times by using methanol, dissolving the centrifugally cleaned product into toluene to obtain a large-size PbS quantum dot solution, wherein the concentration of the large-size PbS quantum dots in the solution is controlled to be 20-60mg/ml, and preferably, the concentration of the large-size PbS quantum dots in the solution is 40 mg/ml.
And 5: growing large-size PbS quantum dots on the surface of the substrate with the opening electrode layer by layer to prepare PbS quantum dots in step 4The obtained large-size PbS quantum dots are grown into the openings of the electrodes with the process: placing a substrate with an opening electrode on a rotating table, and setting the rotating speed to be 2500 rpm; dropping 2 drops of acetonitrile on the surface of the substrate in sequence to clean Bi2S3Surface → dropping 2 drops of toluene for washing → dropping 2 drops of 40mg/ml quantum dots → 1 drop of 2% EDT (ethylene dithiol) for ligand exchange → 2 drops of acetonitrile. The dropping sequence is the sequence of growing single layers, and 1-10 layers are grown layer by taking the sequence as a cycle.
Step 6: annealing in inert gas at 80-150 deg.c for 5-20 min to raise the performance of the detector and obtain stable and efficient infrared detector in communication waveband.
FIG. 2 is a performance test chart of the communication band infrared detector of the present invention, wherein a is a responsivity-intensity test chart of the communication band infrared detector of the present invention containing different quantum dot layer numbers (the optimal quantum dot layer number is 6 layers), and b is Bi2S3Nanosheet and Bi2S3The responsivity spectrum of the PbS mixed system, and c is a response time test chart of the communication waveband infrared detector under different grid pressures. From this, it can be seen that Bi of the present invention2S3The introduction of a PbS mixed system overcomes the interface Fermi level pinning effect existing in the prior mixed system and maintains Bi2S3The inherent high mobility and gate voltage controllability realize larger optical gain and lower noise, and the infrared detector of the invention has wide wave spectrum up to 1.8 mu m, fast response (millisecond order), high sensitivity (the responsivity reaches 10)4A/W, detectivity over 1011Jones), etc., can be widely applied to important fields of optical communication, medical imaging, etc.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. The preparation method of the communication waveband infrared detector is characterized by comprising the following steps of:
preparing Bi on the surface of a silicon oxide substrate2S3Nano-flakes, wherein Bi is produced by physical vapor deposition2S3A nanoflake;
in the presence of Bi2S3Preparing an electrode layer on the surface of the nano sheet, wherein the electrode layer is provided with an opening;
preparing large-size PbS quantum dots, and preparing the large-size PbS quantum dots into a large-size PbS quantum dot solution with a specific concentration;
growing the large-size PbS quantum dot solution with the specific concentration layer by layer and spin-coating the solution into the opening;
and annealing in inert gas after the layer-by-layer growth is carried out, so as to obtain the communication waveband infrared detector.
2. The method according to claim 1, wherein Bi is produced2S3In the step of nano-flake, preparing Bi by physical vapor deposition2S3When the nano-flake is prepared, the deposition temperature is 600-850 ℃, the deposition time is 5-10 minutes, and the Bi is2S3The thickness of the nano-flake is 20-30 nm.
3. The method according to claim 1, wherein in the step of preparing the electrode, the Bi is directly written by laser and evaporated by evaporation2S3Preparing an electrode layer of 1-5nmTi layer and 40-80nmAu layer on the surface of the nano sheet in sequence, wherein an opening is formed in the electrode layer, and the opening exposes the Bi2S3The length of the opening on the surface of the nano-flake is 2-20 μm, and the width of the opening is 5-30 μm.
4. The method as claimed in claim 1, wherein the step of preparing the large-sized PbS quantum dots and preparing the large-sized PbS quantum dot solution having a specific concentration comprises adding 0.4-5g of lead oxide to 4-50ml of oleic acid, stirring for 6-24 hours under vacuum at 60-100 ℃, adding 15-100ml of 1-octadecene, and raising the temperature to 120-160 ℃; after reaching the specified temperature, adding 1-10mmol TMS; and finally, centrifugally cleaning for 2-5 times, and dissolving into toluene, wherein the concentration of the large-size PbS quantum dots in the toluene solution is 20-60 mg/ml.
5. The preparation method according to claim 3, characterized in that, after the electrode layer preparation step and before the layer-by-layer growth spin coating step, the electrode layer is annealed in inert gas at 80-150 ℃ for 0.5-2 hours; in the annealing after the layer-by-layer growth, the annealing temperature is 80-150 ℃, and the annealing time is 5-20 minutes.
6. The preparation method according to claim 1, wherein in the step of layer-by-layer growth spin coating, the number of growth layers is 1-10, and the process of growing 1 layer is specifically as follows: the substrate is placed on a rotating platform, the rotating speed is set to be 1000-3500rpm, and 1-5 drops of acetonitrile, 1-5 drops of toluene, 2-3 drops of 20-60mg/ml quantum dots, 1-2 drops of 2% EDT and 1-5 drops of acetonitrile are sequentially dropped on the surface of the substrate.
7. The method according to claim 1, further comprising preparing Bi2S3Before the nano-sheet, sequentially performing ultrasonic treatment on the silicon oxide substrate by using soapy water, acetone and isopropanol for 10-30min respectively; then cleaning for 3-10min in ozone ultraviolet or oxygen plasma with oxygen flow of 30-80sccm and plasma power of 80-150W.
8. Communication wave band infrared detector, its characterized in that, it includes:
a substrate;
bi grown on the substrate2S3A nanoflake channel layer;
an electrode layer grown on a side of the channel layer facing away from the substrate, the electrode layer having an opening therein, the opening exposing a surface of the channel layer;
and the large-size PbS quantum dot photosensitive layer is grown in the opening.
9. The communications band infrared detector of claim 8, wherein said Bi is2S3The thickness of the nano-thin sheet channel layer is 20-30 nm; the diameter of the large-size PbS quantum dot is 5-20 nm.
10. The infrared detector of claim 8, wherein the electrode layer has a double-layer structure of a Ti layer with a bottom layer of 1-5nm and an Au layer with a top layer of 40-80nm, and the opening has a length of 2-20 μm and a width of 5-30 μm; the substrate comprises a Si substrate and SiO on the Si substrate2And (3) layer structure.
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