CN110707177A - Gold nanorod-lead sulfide quantum dot light detector and preparation method thereof - Google Patents
Gold nanorod-lead sulfide quantum dot light detector and preparation method thereof Download PDFInfo
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- 229910052981 lead sulfide Inorganic materials 0.000 title claims abstract description 75
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- 238000006243 chemical reaction Methods 0.000 claims description 4
- HWSZZLVAJGOAAY-UHFFFAOYSA-L lead(II) chloride Chemical compound Cl[Pb]Cl HWSZZLVAJGOAAY-UHFFFAOYSA-L 0.000 claims description 4
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- 238000012935 Averaging Methods 0.000 description 1
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Images
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0352—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their shape or by the shapes, relative sizes or disposition of the semiconductor regions
- H01L31/035209—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their shape or by the shapes, relative sizes or disposition of the semiconductor regions comprising a quantum structures
- H01L31/035218—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their shape or by the shapes, relative sizes or disposition of the semiconductor regions comprising a quantum structures the quantum structure being quantum dots
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- H—ELECTRICITY
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- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
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- H01L31/08—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof in which radiation controls flow of current through the device, e.g. photoresistors
- H01L31/10—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof in which radiation controls flow of current through the device, e.g. photoresistors characterised by at least one potential-jump barrier or surface barrier, e.g. phototransistors
- H01L31/101—Devices sensitive to infrared, visible or ultraviolet radiation
- H01L31/112—Devices sensitive to infrared, visible or ultraviolet radiation characterised by field-effect operation, e.g. junction field-effect phototransistor
- H01L31/113—Devices sensitive to infrared, visible or ultraviolet radiation characterised by field-effect operation, e.g. junction field-effect phototransistor being of the conductor-insulator-semiconductor type, e.g. metal-insulator-semiconductor field-effect transistor
- H01L31/1136—Devices sensitive to infrared, visible or ultraviolet radiation characterised by field-effect operation, e.g. junction field-effect phototransistor being of the conductor-insulator-semiconductor type, e.g. metal-insulator-semiconductor field-effect transistor the device being a metal-insulator-semiconductor field-effect transistor
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Abstract
The invention provides a gold nanorod-lead sulfide quantum dot photodetector and a preparation method thereof, wherein the preparation method comprises the following steps: the invention discloses a preparation method of a lead sulfide quantum dot PbS QDs solution, a preparation method of a gold nanorod Au NRs solution and a preparation method of a gold nanorod-lead sulfide quantum dot light detector. The photodetector prepared by the method has greatly improved quantum efficiency, responsivity and detectivity compared with a pure lead sulfide photodetector, shows good photoelectric property, and can realize wide spectrum detection from visible light to near infrared light. The method has the characteristics of simplicity, low cost, rapidness, large-area production, strong practicability and the like.
Description
Technical Field
The invention belongs to the technical field of nano semiconductor devices, and particularly relates to a gold nanorod-lead sulfide quantum dot photodetector and a preparation method thereof.
Background
The colloidal lead sulfide quantum dot has the outstanding characteristics of size tunable band gap, multiple exciton effect, high fluorescence quantum yield and the like, and is regarded as one of the most promising photoelectric materials. The solution preparation is another advantage of the lead sulfide quantum dot, and the synthetic method is mature and can be divided into the preparation of lead precursor solution and the injection of sulfur source.
The gold nanorods have stable chemical properties, can be fully absorbed in a visible light region, can form plasmons on the surface under illumination, and have surface enhanced Raman scattering, biocompatibility and the like.
The colloidal lead sulfide quantum dots are widely applied to micro-nano optoelectronic devices such as photodetectors, solar cells, light emitting diodes and the like. The traditional photoelectric detector adopts single semiconductors such as silicon, gallium phosphide, gallium indium arsenide and the like as materials for response of the photoelectric detector, and the photoelectric detector is high in production cost and harsh in preparation conditions. The photosensitive layer of the light detector adopts a simple P-N structure, the absorption efficiency of light is low, the spectral response range is only limited to 0.4-0.76um, and the light detector generally cannot respond to ultraviolet light with the wavelength less than 0.4um and infrared light with the wavelength more than 0.76 um. The PbS quantum dot-based photodetector has a broad spectrum detection capability from visible light to near infrared. However, for photodetectors consisting of PbS quantum dots only, their relatively small light absorption cross-section and low carrier mobility limit their large-scale applications.
Disclosure of Invention
Aiming at the technical problems, the invention provides a gold nanorod-lead sulfide quantum dot optical detector and a preparation method thereof, wherein the optical detector adopts a special sandwich structure, the gold nanostructure is doped in a photosensitive layer of a device, the local electromagnetic field enhancement caused by the plasmon resonance of the local surface of a metal nanoparticle is utilized to improve the optical absorption efficiency of a semiconductor, and the detection of near infrared light is realized by spin coating two layers of colloid lead sulfide quantum dots. The gold nanorod @ lead sulfide quantum dot (Au NRs @ PbS QDs) photodetector with the sandwich layered structure has greatly improved quantum efficiency, responsivity and detectivity compared with a pure lead sulfide photodetector, and shows good photoelectric property. The optical detection is more sensitive than the traditional optical detector, and the detection range is wider.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of a gold nanorod-lead sulfide quantum dot photodetector comprises the following steps:
preparing a lead sulfide quantum dot PbS QDs solution;
preparing a gold nanorod Au NRs solution: preparing gold seed solution and growth solution, adding the gold seed solution into the growth solution to prepare gold nanorod Au NRs solution;
preparing a gold nanorod-lead sulfide quantum dot photodetector: spin-coating the lead sulfide quantum dot PbS QDs solution on a back gate substrate, then carrying out surface ligand exchange on the quantum dots, spin-coating a gold nanorod Au NRs solution on the back gate substrate after the first quantum dot spin-coating and ligand exchange, and then placing the gold nanorod Au NRs solution in a vacuum drying oven for standing to obtain a gold nanorod Au NRs coating; and then carrying out secondary quantum dot spin coating and ligand exchange on the gold nanorod Au NRs coating by the same method, putting the gold nanorod Au NRs coating into a vacuum drying oven for standing after the secondary quantum dot spin coating and the ligand exchange are finished, and forming the gold nanorod-lead sulfide quantum dot light detector with the sandwich layered structure of the lead sulfide quantum dots PbS QDs-the gold nanorod AuNRs-lead sulfide quantum dots PbS QDs on the back gate substrate.
In the scheme, the preparation of the lead sulfide quantum dot PbS QDs solution specifically comprises the following steps:
preparing a cadmium sulfide quantum dot CdS QDs solution;
lead chloride PbCl is added2Mixing powder, oleylamine and oleic acid in a container, introducing high-purity argon, exhausting air, heating, cooling after the solution becomes clear, quickly injecting the cadmium sulfide quantum dot CdS QDs solution, continuously cooling, and adding n-hexane; continuously cooling, adding ethanol, centrifuging, removing supernatant, adding n-hexane, centrifuging, collecting upper black liquid, adding ethanol, centrifuging, removing supernatant to obtain black lead sulfide, oven drying, weighing, adding n-hexane, and making into 50mg.mL-1The lead sulfide quantum dot PbS QDs solution.
In the scheme, the preparation of the cadmium sulfide quantum dot CdS QDs solution specifically comprises the following steps:
adding reddish brown cadmium oxide powder CdO, oleic acid OA and octadecene ODE into a container, putting in a rotating magneton, introducing high-purity argon, exhausting air, heating to 260 ℃, removing a heat source after the solution becomes clear, and cooling; adding an ammonium sulfide solution into oleylamine, and uniformly mixing and stirring; when the temperature in the container is reduced to 30 ℃, quickly injecting the prepared ammonium sulfide solution into the flask, mixing uniformly, stopping stirring, and keeping the temperature; adding excessive ethanol to terminate the reaction, centrifuging, removing supernatant, drying the remaining lemon-yellow cadmium sulfide precipitate, weighing, adding n-hexane, and preparing into 100 mg/mL-1The cadmium sulfide quantum dot CdSQDs solution is reserved.
In the above scheme, the preparation of the gold seed solution specifically comprises:
the chloroauric acid tetrahydrate HAuCl4·4H2And adding the O solution into a CTAB solution of hexadecyl trimethyl ammonium bromide to obtain a mixed solution, and adding a newly prepared ice-cold sodium borohydride solution into the mixed solution to prepare a gold seed solution.
In the above scheme, the preparation of the growth liquid specifically comprises:
adding silver nitrate solution into cetyl trimethyl ammonium bromide CTAB solution, stirring, adding HAuCl4·4H2And (3) uniformly mixing the solution O, adding a hydrochloric acid solution, stirring, adding an ascorbic acid solution, and stirring to obtain a colorless solution, thereby obtaining the growth solution.
In the scheme, the preparation of the gold nanorod Au NRs solution specifically comprises the following steps:
adding the gold seed solution into the growth solution, stirring, standing, centrifuging the standing solution for 5 minutes at a rotating speed of 7500 rpm, removing supernatant, adding appropriate amount of distilled water, centrifuging for 3 minutes for the second time at a rotating speed of 6000 rpm; and re-dispersing the precipitate after the supernatant liquid is removed in distilled water to obtain a gold nanorod Au NRs solution.
In the above scheme, the surface ligand exchange specifically comprises:
the lead sulfide quantum dot PbS QDs solution is coated on a back gate substrate in a spinning mode to form a layer of thin film coated by long-chain ligands, then CTAB methanol solution is coated on the substrate in a spinning mode, the thin film is covered by the short-chain ligand solution and aired until the film layer presents oily organic matters, then the methanol solution is coated on the substrate in a spinning mode at the same rotating speed to wash away redundant CTAB, and ligand exchange is completed.
In the scheme, the spin-coating rotating speed of the first quantum dot spin-coating and the second quantum dot spin-coating is not less than 2500 revolutions per minute, and the spin-coating time is not less than 15 seconds; after the first quantum dot spin coating and the second quantum dot spin coating, the device needs to be placed in a vacuum drying oven to stand for no less than 30 minutes.
In the scheme, the rotating speed of the surface ligand exchange is not less than 2500 revolutions per minute, the spin coating time is 10-15s, and the airing time is not less than 30 s.
A gold nanorod-lead sulfide quantum dot photodetector is prepared by using a preparation method of the gold nanorod-lead sulfide quantum dot photodetector.
Compared with the prior art, the invention has the beneficial effects that: the gold nanorod-lead sulfide quantum dot photodetector with the sandwich layered structure in the gold nanorod-lead sulfide quantum dot photodetector has greatly improved quantum efficiency, responsivity and detectivity compared with a pure lead sulfide photodetector. The preparation method can be used for simply, quickly and stably preparing the gold nanorod-lead sulfide quantum dot sandwich structure photodetector, and has the advantages of mild preparation conditions, controllable process parameters and high repeatability. The cost of optical detector preparation has been reduced, has realized simultaneously and has promoted at near infrared band detection performance, realizes the broad spectrum detection from visible light to near infrared light, and is more sensitive to the light signal, and the detectable scope is also wider.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a schematic diagram of a sandwich layered structure of a gold nanorod-lead sulfide quantum dot photodetector according to an embodiment of the invention;
FIG. 2 is an X-ray diffraction spectrum of lead sulfide quantum dots (black) and gold nanorods (gray) according to an embodiment of the present invention;
FIG. 3 is an electron microscope image of quantum dots and gold nanorods according to an embodiment of the present invention, FIG. 3(a) is a transmission electron microscope image of PbS QDs, FIG. 3(b) is a high-resolution transmission electron microscope image of PbS QDs, FIG. 3(c) is a fast Fourier transform image of PbS QDs, and FIG. 3(d) is a transmission electron microscope image of Au NRs;
FIG. 4 is a cross-sectional SEM image of a device according to an embodiment of the present invention, FIG. 4(a) is a field effect transistor of PbS QDs, and FIG. 4(b) is a field effect transistor of Au NRs @ PbS QDs;
FIG. 5 is a graph showing the output characteristic and transfer characteristic of the PbS QDs photodetector and the Au NRs @ PbS QDs photodetector according to an embodiment of the present invention, wherein FIGS. 5(a) and 5(b) are the output characteristic and transfer characteristic of the PbS QDs photodetector under different light power irradiation, respectively, and FIGS. 5(c) and 5(d) are the output characteristic and transfer characteristic of the Au NRs @ PbS QDs photodetector under different light power irradiation, respectively;
FIG. 6 shows responsivities of the PbS QDs photodetector and the Au NRs @ PbS QDs photodetector according to an embodiment of the present invention, wherein (a) shows responsivity spectra of the PbS QDs photodetector and the Au NRs @ PbS QDs photodetector, and FIG. 6(b) shows a responsivity enhancement ratio;
fig. 7 shows the detectivity of the photodetector according to an embodiment of the present invention, where fig. 7(a) shows the detectivity of the photodetector under the excitation of 808nm with different optical power densities, VG ═ VSD ═ 4V, and fig. 7(b) shows the detectivity spectra of the PbS QDs photodetector and the Au NRs @ PbS QDs photodetector;
fig. 8 is an external quantum efficiency of the photodetector according to an embodiment of the present invention, fig. 8(a) is an external quantum efficiency of the photodetector under the excitation of 808nm laser with different optical powers, VG ═ VSD ═ 4V, fig. 8(b) is an external quantum efficiency spectrum of the PbS QDs photodetector and the AuNRs @ PbS QDs photodetector, and fig. 8(c) is an external quantum efficiency enhancement ratio of the Au NRs @ PbS QDs photodetector;
in the figure, 1.Au source; 2, Au drain electrode; 3. a silicon dioxide gate insulating layer; an n-type heavily doped silicon wafer; 5. gold nanorod-lead sulfide quantum dot sandwich structure.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
The preparation method of the gold nanorod-lead sulfide quantum dot photodetector comprises the following steps:
preparing a lead sulfide quantum dot PbS QDs solution;
preparing a gold nanorod Au NRs solution: preparing gold seed solution and growth solution, adding the gold seed solution into the growth solution to prepare gold nanorod Au NRs solution;
preparing a gold nanorod-lead sulfide quantum dot photodetector: spin-coating the lead sulfide quantum dot PbS QDs solution on a back gate substrate, then carrying out surface ligand exchange on the quantum dots, spin-coating a gold nanorod Au NRs solution on the back gate substrate after the first quantum dot spin-coating and ligand exchange, and then placing the gold nanorod Au NRs solution in a vacuum drying oven for standing to obtain a gold nanorod Au NRs coating; and then carrying out secondary quantum dot spin coating and ligand exchange on the gold nanorod Au NRs coating by the same method, putting the gold nanorod Au NRs coating into a vacuum drying oven for standing after the secondary quantum dot spin coating and the ligand exchange are finished, and forming the gold nanorod-lead sulfide quantum dot light detector with the sandwich layered structure of the lead sulfide quantum dots PbS QDs-the gold nanorod AuNRs-lead sulfide quantum dots PbS QDs on the back gate substrate.
The preparation method of the lead sulfide quantum dot PbS QDs solution specifically comprises the following steps:
preparing a cadmium sulfide quantum dot CdS QDs solution;
lead chloride PbCl is added2Mixing powder, oleylamine and oleic acid in a container, introducing high-purity argon, exhausting air, heating, cooling after the solution becomes clear, and injecting into the container rapidlyThe solution of the cadmium sulfide quantum dots CdS QDs is changed into black, the temperature is continuously reduced, and normal hexane is added; continuously cooling, adding ethanol, centrifuging, removing supernatant, adding n-hexane, centrifuging, collecting upper black liquid, adding ethanol, centrifuging, removing supernatant to obtain black lead sulfide, oven drying, weighing, adding n-hexane, and making into 50mg.mL-1The lead sulfide quantum dot PbS QDs solution.
The preparation of the cadmium sulfide quantum dot CdS QDs solution specifically comprises the following steps:
adding reddish brown cadmium oxide powder CdO, oleic acid OA and octadecene ODE into a container, putting in a rotating magneton, introducing high-purity argon, exhausting air, heating to 260 ℃, removing a heat source after the solution becomes clear, and cooling; adding an ammonium sulfide solution into oleylamine, and uniformly mixing and stirring; when the temperature in the container is reduced to 30 ℃, quickly injecting the prepared ammonium sulfide solution into the flask, mixing uniformly, stopping stirring, and keeping the temperature; adding excessive ethanol to terminate the reaction, centrifuging, removing supernatant, oven drying the remaining lemon-yellow cadmium sulfide precipitate, weighing, adding n-hexane, and making into 100 mg/mL-1The cadmium sulfide quantum dot CdSQDs solution is reserved.
The preparation method of the gold seed solution comprises the following specific steps:
the chloroauric acid tetrahydrate HAuCl4·4H2And adding the O solution into a CTAB solution of hexadecyl trimethyl ammonium bromide to obtain a mixed solution, and adding a newly prepared ice-cold sodium borohydride solution into the mixed solution to prepare a gold seed solution.
The preparation of the growth liquid comprises the following specific steps:
adding silver nitrate solution into cetyl trimethyl ammonium bromide CTAB solution, stirring, adding HAuCl4·4H2And (3) uniformly mixing the solution O, adding a hydrochloric acid solution, stirring, adding an ascorbic acid solution, and stirring to obtain a colorless solution, thereby obtaining the growth solution.
The preparation method of the gold nanorod Au NRs solution comprises the following steps:
adding the gold seed solution into the growth solution, stirring, standing, centrifuging the standing solution for 5 minutes at a rotating speed of 7500 rpm, removing supernatant, adding appropriate amount of distilled water, centrifuging for 3 minutes for the second time at a rotating speed of 6000 rpm; and re-dispersing the precipitate after the supernatant liquid is removed in distilled water to obtain a gold nanorod Au NRs solution.
The surface ligand exchange is specifically as follows:
the lead sulfide quantum dot PbS QDs solution is coated on a back gate substrate in a spinning mode to form a layer of thin film coated by long-chain ligands, then CTAB methanol solution is coated on the substrate in a spinning mode, the thin film is covered by the short-chain ligand solution and aired until the film layer presents oily organic matters, then the methanol solution is coated on the substrate in a spinning mode at the same rotating speed to wash away redundant CTAB, and ligand exchange is completed.
The spin-coating rotating speed of the first quantum dot spin-coating and the second quantum dot spin-coating is not less than 2500 revolutions per minute, and the spin-coating time is not less than 15 seconds; after the first quantum dot spin coating and the second quantum dot spin coating, the device needs to be placed in a vacuum drying oven to stand for no less than 30 minutes.
The rotating speed of the surface ligand exchange is not less than 2500 revolutions per minute, the spin coating time is 10-15s, and the airing time is not less than 30 s.
Fig. 1 shows an embodiment of the gold nanorod-lead sulfide quantum dot photodetector according to the present invention, which is prepared by using the method for preparing the gold nanorod-lead sulfide quantum dot photodetector. The gold nanorod-lead sulfide quantum dot light detector comprises an Au source electrode 1, an Au drain electrode 2, a silicon dioxide gate insulating layer 3, an n-type heavily doped silicon chip 4 and a gold nanorod-lead sulfide quantum dot sandwich structure 5; the silicon dioxide gate insulating layer 3 is positioned on the n-type heavily doped silicon chip 4, the Au source electrode 1 and the Au drain electrode 2 are positioned on the silicon dioxide gate insulating layer 3 to form a back gate substrate, and the gold nanorod-lead sulfide quantum dot sandwich structure 5 is spin-coated on the back gate substrate and positioned between the Au source electrode 1 and the Au drain electrode 2; the gold nanorod-lead sulfide quantum dot sandwich structure 5 is a structure that a layer of gold nanorod Au NRs is sandwiched between two layers of lead sulfide quantum dots PbS QDs.
The invention discloses a preparation method for preparing a gold nanorod-lead sulfide quantum dot sandwich-layer structured photodetector by adopting a low-cost liquid phase spin coating technology and a ligand exchange technology. Lead sulfide quantum dots PbS QDs with good dispersibility are prepared by a cation replacement method and a thermal injection method, and gold nanorods Au NRs with uniform size are prepared by a seed method. The sandwich layer structure field effect optical transistor type optical detector is prepared by adopting a method of layered spin coating on a back gate substrate. The photodetector prepared by the method has greatly improved quantum efficiency, responsivity and detectivity compared with a pure lead sulfide photodetector, shows good photoelectric property, and can realize wide spectrum detection from visible light to near infrared light. The method has the characteristics of simplicity, low cost, rapidness, large-area production, strong practicability and the like.
The specific embodiment is as follows:
a preparation method of a gold nanorod-lead sulfide quantum dot photodetector comprises the following steps:
50 mg/mL of the solution was prepared-1The preparation of the lead sulfide quantum dot PbS QDs solution specifically comprises the following steps:
preparing a cadmium sulfide quantum dot CdS QDs solution: adding 0.28g of reddish brown cadmium oxide powder CdO, 1.5 mL of oleic acid OA and 18mL of octadecene ODE into a three-neck flask, putting a rotating magneton, introducing high-purity argon, exhausting air, heating to 260 ℃, keeping the temperature for 20 minutes, removing a heat source after the solution becomes clear, and naturally cooling. 360ul of ammonium sulfide solution is taken by a liquid transfer gun and added into 10mL of oleylamine, and the mixture is mixed and stirred uniformly. When the temperature in the flask is reduced to 30 ℃, quickly injecting the prepared ammonium sulfide solution into the flask, mixing uniformly, stopping stirring, and keeping the temperature for 1 hour. Adding excessive ethanol to terminate the reaction, centrifuging, removing supernatant, oven drying the remaining lemon-yellow cadmium sulfide precipitate, weighing, adding 10mL n-hexane, and making into 100 mg/mL-1The cadmium sulfide quantum dot CdS QDs solution is reserved.
0.834g of lead chloride PbCl2Mixing powder, 10mL of oleylamine and 2mL of oleic acid in a clean three-neck flask, introducing high-purity argon, exhausting air, heating to 150 ℃, continuing for 30 minutes, naturally cooling to 120 ℃ after the solution becomes clear, and quickly injecting 3mL of cadmium sulfide quantum dot CdS QDs solution into the solutionTurning black with a molar ratio of lead to sulfur of about 3/2. Continuously cooling to 75 ℃, and adding 10mL of n-hexane; cooling to 40 deg.C, adding not less than 10ml ethanol, centrifuging, and removing supernatant; adding n-hexane, centrifuging, and placing the upper black liquid into a new centrifugal tube; adding 10mL ethanol, centrifuging, removing supernatant, oven drying black lead sulfide, weighing, adding 10mL n-hexane, and making into 50mg. mL-1PbS QDs solution of (1).
The preparation method of the gold nanorod Au NRs solution specifically comprises the following steps:
synthesizing a gold seed solution: 10mL of 0.5mM chloroauric acid tetrahydrate HAuCl4The 4H2O solution was added to 10mL of 0.2M CTAB cetyltrimethylammonium bromide solution, stirred gently and mixed well. 1.2mL of a freshly prepared 0.01M ice-cold sodium borohydride solution was added thereto, the solution turned pale brown, stirred for 30 seconds, and then allowed to stand at room temperature for 30 minutes. And (4) synthesizing the gold seed solution.
Synthesizing a growth solution: 12L of 0.1M silver nitrate solution was added to 6mL of 0.2M CTAB solution, and after gentle stirring, 1.2mL of 5mM HAuCl was added44H2O solution, mix well. Then 12L of 2.0M hydrochloric acid solution was added thereto, and the mixture was stirred gently, and 66L of 0.1M ascorbic acid solution was added thereto, and the solution became colorless after stirring, to synthesize a growth liquid.
Growth of gold nanorods Au NRs: 15L of the seed solution was added to the growth liquid, gently stirred for 10 seconds, and allowed to stand at normal temperature for 10 hours. And centrifuging the Au nanorod solution for 5 minutes at the rotating speed of 7500 rpm, removing supernatant, adding a proper amount of distilled water, and centrifuging for 3 minutes for the second time at the rotating speed of 6000 rpm. After the supernatant was removed, the solution was redispersed in 3mL of distilled water for further use to obtain a gold nanorod Au NRs solution.
The experimental result is shown in fig. 2, wherein the black curve is lead sulfide quantum dots, and the gray curve is gold nanorods. The peak positions of the black curves are consistent with those of lead sulfide of a bulk cubic structure of JCPDS NO.650346, and the peak positions of the (111), (200) and (220) planes are more prominent, and the diffraction angles thereof are 25.645 °, 29.772 ° and 42.617 °, respectively, according to the Debyscherrer equation:
wherein D is the particle diameter, R is the Scherrer constant, is
The half-height peak width is the diffraction angle corresponding to the diffraction peak. The diameter of the quantum dot can be finally calculated to be about 3.4nm by calculating the D values of different diffraction peaks and then averaging. In the XRD spectrum of the gold nanorod, the crystal faces of (111), (200), (220) and (311) have obvious diffraction peaks, and are consistent with the gold crystal with the standard card of JCPDS NO.4784 face-centered cubic structure.
Preparing a gold nanorod-lead sulfide quantum dot photodetector device: and spin-coating the prepared lead sulfide quantum dot PbS QDs solution on a back gate substrate at the rotating speed of 2500 rpm, wherein the spin-coating time is 15 seconds. Then, surface ligand exchange is carried out on the lead sulfide quantum dots PbS QDs, and 10mg.ml is prepared-1Spin coating two drops of CTAB methanol solution on the substrate, spin coating for 10 seconds, air standing for 30 seconds, and spin coating 3 drops of methanol on the substrate to clean off the excessive CTAB. The processes of spin coating and ligand exchange of the lead sulfide quantum dots PbS QDs are carried out twice in total. The preparation process of the Au NRs @ PbS QDs photodetector comprises the steps of spin-coating a drop of gold nanorod solution after the first quantum dot spin-coating and ligand exchange, placing the device into a vacuum drying oven to stand for 30 minutes, then carrying out the second quantum dot spin-coating and ligand exchange, and placing the device into the vacuum drying oven to stand for 30 minutes after the device spin-coating is completed, so that the residual solvent is volatilized, and the performance of the device is improved.
As shown in FIG. 3(a), which is a transmission electron microscope image of PbS QDs, it can be seen that the PbS QDs prepared by the cation exchange method have good monodispersity and uniform size of about 3.4nm, which is consistent with the calculation result of XRD data. As shown in FIGS. 3(b), (c), the high resolution TEM image and the corresponding FFT image of PbS QDs shows better crystallinity. FIG. 3(d) is a transmission electron micrograph of Au NRs, wherein the average length of the Au NRs is 51.3nm, the average diameter is 19.5nm, and the length-diameter ratio is about 2.63.
As shown in fig. 4, a cross-sectional scanning electron microscope image of a field effect transistor of a spin-coated sample shows that the structure of stacking layers is very obvious, and the structure is an n-type heavily doped silicon wafer (4), a silicon dioxide gate insulating layer (3) and a gold nanorod-lead sulfide quantum dot sandwich structure (5) of a photosensitive layer from bottom to top. FIG. 4(a) shows the thickness of the photosensitive layer of the field effect transistor PbS QDs is about 275nm, and FIG. 4(b) shows the thickness of the photosensitive layer of the Au NRs @ PbS QDs field effect transistor Au NRs @ PbS QDs is about 281nm, so that the light absorption efficiency of the Au NRs @ PbS QDs field effect transistor Au NRs @ PbS QDs is high.
As shown in FIG. 5, (a) and (b) are respectively the output characteristic and transfer characteristic curves of the PbS QDs photodetector under different light power irradiation, and the intersecting curve with the vertical coordinate in FIG. 5(a) is dark,5mW/cm2,137.5mW/cm2,455mW/cm2,827mW/cm2The curve, which is the vertical intersection curve of 5mW/cm, in FIG. 5(b) is dark,5mW/cm2,137.5mW/cm2,455mW/cm2,827mW/cm2The curve, in FIG. 5(c), the intersecting curve of the vertical coordinates is dark,5mW/cm from bottom to top2,137.5mW/cm2,455mW/cm2,827mW/cm2The curve, in FIG. 5(d), the vertical coordinate intersection curve is, from bottom to top, dark,5mW/cm2,137.5mW/cm2,455mW/cm2,827mW/cm2Curve line. FIGS. 5(c) and (d) are graphs of output characteristics and transfer characteristics of Au NRs @ PbS QDs photodetector under different light power irradiation, respectively. Fig. 5(a), (c) show that under the illumination condition, both photocurrent is generated, and the photocurrent is gradually increased along with the increase of the optical power, which indicates that more photons are incident, so that the photosensitive layer of the device generates more carriers, and particularly, for the device of PbS QDs introduced with gold nanorods, the photocurrent generated by the device under the same condition is 2.6 times higher than that of a photodetector without metal, which is due to the enhancement of the electromagnetic field caused by the local near-field surface plasmon resonance of the metal, so that the optical absorption of the semiconductor is enhanced to generate more photocarriers. FIGS. 5(b), (d) show that for the PbS QDs photodetectors, the hole mobility and electron mobility are about 0.23cm, respectively2V-1s-1And 0.14cm2V-1s-1(ii) a The hole mobility and the electron mobility of the Au NRs @ PbS QDs photodetector reach about 0.41cm2V-1s-1And 0.34cm2V-1s-1Respectively increased by 1.7 times and 2.4 times.
Fig. 6(a) shows the responsivity spectrum of the device, and the photodetector based on the lead sulfide quantum dots can realize wide-spectrum photodetection, but the responsivity is relatively low in the near infrared band. It can be seen from the spectrum that after the gold nanorods are introduced into the PbS QDs photodetector, the responsivity of the device is improved in the near infrared band. FIG. 6(b) is the responsivity enhancement ratio, the responsivity of the Au NRs @ PbS QDs photodetector is 2.7 compared with the responsivity of the PbS QDs photodetector, the enhancement ratio is up to 1020nm, and the responsivity of the photodetector in the near infrared band is enhanced by introducing the gold nanorods.
As shown in FIG. 7, VGAnd VSDBoth are 4V, and under the excitation of a power-adjustable 808nm laser, the detection rate of the optical detector and the power density of the light source are linearly reduced. Under the same condition, the detection rate of the Au NRs @ PbS QDs photodetector is higher than that of the PbS QDs photodetector, and the power density is 5mW cm-2The responsivity of the two devices reaches a maximum value of 6.31010Jones, 4.81010Jones, respectively. FIG. 7(b) is the detectivity spectrum of the device, at a wavelength of 1000 nm, for a PbS QDs photodetector with a detectivity of 0.14X 1011The detection rate of the Jones, Au NRs @ PbS QDs photodetector is 0.26 multiplied by 1011Jones, both have a detection rate that is improved by about 1.85 times compared to Au NRs @ PbS QDs photodetectors.
As shown in FIG. 8(a), the power density was 5mW cm-2Under the irradiation of a 808nm laser, the EQE of the two devices reaches the maximum, the PbS QDs photodetector is 767%, and the Au NRs @ PbS QDs photodetector is 1251%. Through the calculation of quantum efficiency, the multi-exciton effect of the quantum dot is very obvious. FIG. 8(b) is a plot of EQE versus wavelength for two devices, showing that the external quantum efficiency peaks near 590nm and a lower peak near 1020nm, which is related to the amount of lead sulfideThe first exciton absorption characteristics of the sub-dots coincide. As shown in fig. 8(c), the external quantum efficiency of the AuNRs @ PbS QDs photodetector in the near infrared band is higher, which is improved by about 2.7 times.
The invention prepares PbS QDs with better dispersibility by cation replacement and a thermal injection method, and prepares Au NRs with uniform size by adopting a seed method. Then a PbS QDs photodetector and an Au NRs @ PbS QDs photodetector based on a field effect phototransistor are prepared, the electrical property of the device under the condition of no illumination is tested, and the characteristic of bidirectional conduction is presented; under the excitation of 808nm laser, the hole photocurrent of the Au NRs @ PbS QDs photodetector is stronger than the electron photocurrent, and the optical power density is 5mW/cm-2When the source-drain voltage and the grid voltage are-4V, the responsivity of the PbS QDs photodetector reaches 4.9AW-1The detection degree reaches 4.81010Jones, the quantum efficiency reaches 767%, and the responsivity of the Au NRs @ PbS QDs photodetector reaches 8.2AW-1The detection degree reaches 6.31010Jones, and the quantum efficiency reaches 1251%. The responsivity spectrum and the EQE spectrum prove that the gold nanorod-lead sulfide quantum dot light detector with the sandwich layered structure of the lead sulfide quantum dots PbS QDs-gold nanorod Au NRs-lead sulfide quantum dots PbS QDs enhances the performance of the light detector in a near-red band.
It should be understood that although the present description has been described in terms of various embodiments, not every embodiment includes only a single embodiment, and such description is for clarity purposes only, and those skilled in the art will recognize that the embodiments described herein may be combined as suitable to form other embodiments, as will be appreciated by those skilled in the art.
The above-listed detailed description is only a specific description of a possible embodiment of the present invention, and they are not intended to limit the scope of the present invention, and equivalent embodiments or modifications made without departing from the technical spirit of the present invention should be included in the scope of the present invention.
Claims (10)
1.A preparation method of a gold nanorod-lead sulfide quantum dot photodetector is characterized by comprising the following steps:
preparing a lead sulfide quantum dot PbS QDs solution;
preparing a gold nanorod Au NRs solution: preparing gold seed solution and growth solution, adding the gold seed solution into the growth solution to prepare gold nanorod Au NRs solution;
preparing a gold nanorod-lead sulfide quantum dot photodetector: spin-coating the lead sulfide quantum dot PbS QDs solution on a back gate substrate, then performing surface ligand exchange on the quantum dots, spin-coating a gold nanorod Au NRs solution on the back gate substrate after the first quantum dot spin coating and ligand exchange, and then placing the back gate substrate in a vacuum drying oven for standing to obtain a gold nanorod Au NRs coating; and then carrying out secondary quantum dot spin coating and ligand exchange on the gold nanorod Au NRs coating by the same method, putting the gold nanorod Au NRs coating into a vacuum drying oven to stand after the secondary quantum dot spin coating and the ligand exchange are finished, and forming the gold nanorod-lead sulfide quantum dot light detector with the lead sulfide quantum dot PbS QDs-gold nanorod Au NRs-lead sulfide quantum dot PbS QDs sandwich layered structure on the back gate substrate.
2. The method for preparing a gold nanorod-lead sulfide quantum dot photodetector as claimed in claim 1, wherein the preparation of the lead sulfide quantum dot PbS QDs solution specifically comprises the following steps:
preparing a cadmium sulfide quantum dot CdS QDs solution;
lead chloride PbCl is added2Mixing powder, oleylamine and oleic acid in a container, introducing high-purity argon, exhausting air, heating, cooling after the solution becomes clear, quickly injecting the cadmium sulfide quantum dot CdS QDs solution, continuously cooling after the solution becomes black, and adding n-hexane; continuously cooling, adding ethanol, centrifuging, removing supernatant, adding n-hexane, centrifuging, collecting upper black liquid, adding ethanol, centrifuging, removing supernatant to obtain black lead sulfide, oven drying, weighing, adding n-hexane, and making into 50mg.mL-1The lead sulfide quantum dot PbS QDs solution.
3. The method for preparing a gold nanorod-lead sulfide quantum dot photodetector as claimed in claim 1, wherein the preparation of the cadmium sulfide quantum dot CdS QDs solution specifically comprises:
adding reddish brown cadmium oxide powder CdO, oleic acid OA and octadecene ODE into a container, putting in a rotating magneton, introducing high-purity argon, exhausting air, heating to 260 ℃, removing a heat source after the solution becomes clear, and cooling; adding an ammonium sulfide solution into oleylamine, and uniformly mixing and stirring; when the temperature in the container is reduced to 30 ℃, quickly injecting the prepared ammonium sulfide solution into the flask, mixing uniformly, stopping stirring, and keeping the temperature; adding excessive ethanol to terminate the reaction, centrifuging, removing supernatant, drying the remaining lemon-yellow cadmium sulfide precipitate, weighing, adding n-hexane, and preparing into 100mg.mL-1The cadmium sulfide quantum dot CdS QDs solution is reserved.
4. The method for preparing a gold nanorod-lead sulfide quantum dot photodetector as claimed in claim 1, wherein the preparation of the gold seed solution specifically comprises:
the chloroauric acid tetrahydrate HAuCl4·4H2And adding the O solution into a CTAB solution of cetyl trimethyl ammonium bromide to obtain a mixed solution, and adding a newly prepared ice-cold sodium borohydride solution into the mixed solution to prepare a gold seed solution.
5. The method for preparing a gold nanorod-lead sulfide quantum dot photodetector as claimed in claim 1, wherein the growth solution is prepared by:
adding silver nitrate solution into cetyl trimethyl ammonium bromide CTAB solution, stirring, adding HAuCl4·4H2And (3) uniformly mixing the solution O, adding a hydrochloric acid solution, stirring, adding an ascorbic acid solution, and stirring to obtain a colorless solution, thereby obtaining the growth solution.
6. The method for preparing a gold nanorod-lead sulfide quantum dot photodetector as claimed in claim 1, wherein the preparation of the gold nanorod Au NRs solution specifically comprises:
adding the gold seed solution into the growth solution, stirring, standing, centrifuging the standing solution for 5 minutes at a rotating speed of 7500 rpm, removing supernatant, adding appropriate amount of distilled water, centrifuging for 3 minutes for the second time at a rotating speed of 6000 rpm; and re-dispersing the precipitate after the supernatant liquid is removed in distilled water to obtain a gold nanorod Au NRs solution.
7. The method for preparing a gold nanorod-lead sulfide quantum dot photodetector as claimed in claim 1, wherein the surface ligand exchange is specifically:
the lead sulfide quantum dot PbS QDs solution is coated on a back gate substrate in a spinning mode to form a long-chain ligand coated film, then a CTAB methanol solution is coated on the substrate in a spinning mode, the short-chain ligand solution covers the film and is aired until the film layer presents oily organic matters, then the methanol solution is coated on the substrate in a spinning mode at the same rotating speed to wash away redundant CTAB, and ligand exchange is completed.
8. The method for preparing a gold nanorod-lead sulfide quantum dot photodetector as claimed in claim 1, wherein the spin-coating rotation speed of the first quantum dot spin-coating and the second quantum dot spin-coating is not less than 2500 revolutions per minute, and the spin-coating time is not less than 15 seconds; after the first quantum dot spin coating and the second quantum dot spin coating, the device needs to be placed in a vacuum drying oven to stand for no less than 30 minutes.
9. The method for preparing a gold nanorod-lead sulfide quantum dot photodetector as claimed in claim 7, wherein the surface ligand exchange rotation speed is not less than 2500 rpm, the spin coating time is 10-15s, and the air-drying time is not less than 30 s.
10. A gold nanorod-lead sulfide quantum dot photodetector, characterized in that the gold nanorod-lead sulfide quantum dot photodetector is prepared by the method of any one of claims 1 to 9.
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