CN107993923B - Preparation method of controllable quantum dot array based on photothermal effect - Google Patents
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Abstract
The invention discloses a method for preparing a controllable quantum dot array based on a photo-thermal effect, which takes a metal or alloy nanoparticle array as a template, controls the reaction condition of a quantum dot precursor by a local surface plasmon thermal effect initiated by a light source, and thereby controls the preparation site, the size and the nucleation density of the quantum dot precursor. The method can be combined with a semiconductor processing technology, and the prepared quantum dot array can be applied to processing and manufacturing of devices such as quantum dot lasers, single photon light sources, solar cells, efficient light emitting diodes and memories.
Description
Technical Field
The invention relates to the field of preparation of nano materials, in particular to a preparation method of a controllable quantum dot array based on a photothermal effect.
Background
Quantum dots are a nanoscale material that can exhibit different physical properties from the bulk material due to the effects of quantum size effects. The semiconductor quantum dots are generally composed of II-VI group or III-V group elements, the particle size of the semiconductor quantum dots is generally 1-10 nm, the semiconductor quantum dots are generally provided with discrete energy band structures due to the influence of electron hole quantum confinement effect, and the light-emitting wavelength can be regulated and controlled through the size. The growth of quantum dot arrays with precise control is the focus of research in many high-performance optical devices today. In various scientific research fields including quantum dot lasers, single photon light sources, efficient light emitting diodes, sensitized solar cells and flat panel display fields, extremely high performance requirements are provided for the density, nucleation position, size and shape uniformity of quantum dot arrays. At present, the preparation of highly uniform and ordered quantum dot arrays mainly depends on the mode of combining a patterned substrate template with an S-K growth mode and utilizes the epitaxial growth self-assembly preparation of molecular beam epitaxial growth or chemical vapor deposition. The technology is already applied to the preparation of quantum dot arrays of III-V semiconductor materials, but because the equipment needs ultra-high vacuum and a photoetching process, the preparation cannot take both the cost and the effect into consideration.
The chemical synthesis is a method for preparing the semiconductor quantum dots with low cost, the process flow is simple, the quantum dots can be prepared in a large area with extremely low cost, the defect of high epitaxial growth preparation cost is overcome, and the method is the quantum dot preparation method which is most suitable for large-scale industrialization. However, in the preparation of the quantum dot array, the chemical synthesis method has great difficulty in controlling the preparation sites and nucleation positions of the quantum dots, so that the preparation of the chemically synthesized quantum dots is greatly limited in practical application, and the method is also a challenging and urgent problem to be solved in controllable synthesis of the quantum dot array with large area and low cost.
Disclosure of Invention
In view of the problem of insufficient control of the preparation sites of the quantum dots in the prior art, the invention provides a controllable quantum dot array preparation method based on the photothermal effect, which realizes the control of the growth conditions of the quantum dots on the surface and further realizes the accurate control of the preparation sites and the nucleation positions of the quantum dot array. The method is suitable for large-scale preparation of the quantum dot array with accurate control on a semiconductor and an oxide substrate.
In order to achieve the purpose, the invention provides a preparation method of a controllable quantum dot array based on a photothermal effect. The specific technical scheme is as follows:
a preparation method of a controllable quantum dot array based on a photothermal effect comprises the following steps:
step one, pretreatment of the surface of a substrate: selecting and determining a substrate material, cleaning the surface of the substrate according to a standard surface cleaning process, and carrying out plasma cleaning pretreatment, wherein the substrate material is a semiconductor, an oxide or a high molecular polymer material.
Step two, depositing a surface metal film: the method comprises the steps of preparing a metal film by using a physical vapor deposition method, wherein the thickness of the metal film is 0.5-200 nm, the metal film comprises one or more of Au, Ag, Cu, Al, In, Pt and Pd, and the deposition In the physical vapor deposition method is any one of sputtering deposition, pulse laser deposition and evaporation deposition.
Step three, preparing a metal nanoparticle array: and annealing the metal film under a vacuum condition or a protective atmosphere to enable the metal film to grow into a nano particle array in a self-assembly manner, so as to prepare the metal nano particle array, wherein the metal nano particle array can be prepared by a photoetching method, and the annealing treatment is replaced, so that the particle size and the surface distribution are more uniform.
Step four, deposition of a protective layer: and depositing or oxidizing the metal nanoparticle array to grow a protective layer, wherein the protective layer is an oxide or a nitride, the thickness of the protective layer is 0.1-100 nm, and the protective layer can be unused in some cases of quantum dot arrays. The oxide protective layer can be obtained by performing oxidation treatment when the metal is an easily oxidizable metal such as Al or In. The oxide layer can be adjusted to be a semiconductor thin film layer, an organic layer or not deposited according to application requirements.
Step five, quantum dot growth: placing the substrate loaded with the metal nanoparticle array in a quantum dot precursor solution, and fixing or scanning and irradiating the metal nanoparticle array by using a light sourceThe power density is 0.1-5W/cm2The light source is pulse type or continuous type laser, the quantum dot precursor solution is in a flowing state, and a flowing design is adopted.
Sixthly, cleaning and treating the substrate after: and after the fifth step is finished, carrying out ultrasonic cleaning on the substrate by using trichloromethane, and then carrying out ultrasonic cleaning on the substrate by using ethanol to prepare the controllable quantum dot array.
The preparation method disclosed by the invention is characterized in that a metal or alloy nanoparticle array is used as a template, and the synthesis sites, the size and the density of quantum dots are controlled by using the metal nanoparticle local surface plasmon photothermal effect initiated by laser or other light sources.
The preparation method of the quantum dot array disclosed by the invention is simple in process and can be integrated into a semiconductor processing flow. The method fully utilizes the local temperature regulation and control function of the photo-thermal effect of the metal nanoparticles, and has no damage to the substrate structure. Compared with other epitaxial growth processes, the method has the advantages of high synthesis rate, low cost, suitability for high-scale preparation, realization of preparation of large-scale quantum dot arrays and wide application prospect.
The invention has the following beneficial effects:
1. the preparation method disclosed by the invention is a large-area and low-cost quantum dot array preparation method based on regulation and control of photo-thermal effect of a metal nanoparticle array, the metal or alloy (one or more of Au, Ag, Cu, Al, Pt and Pd) nanoparticle array is used as a template, and the reaction condition of a quantum dot precursor is controlled by local surface plasmon thermal effect initiated by a light source, so that the preparation site, size and nucleation density of the quantum dot precursor are controlled, and the prepared quantum dot array is large in area and low in cost;
2. the preparation method disclosed by the invention can be combined with a semiconductor processing technology, and the prepared quantum dot array can be applied to processing and manufacturing of devices such as quantum dot lasers, single photon light sources, solar cells, efficient light emitting diodes, memories and the like.
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FIG. 1 is a flow chart of the steps of the disclosed manufacturing method.
Detailed Description
The invention is described in further detail below with reference to the figures and specific embodiments. It should be understood that the embodiments are illustrative of the invention and are not to be construed as limiting the scope of the invention in any way.
The preparation method comprises six steps of substrate surface pretreatment, surface metal film deposition, metal nanoparticle array preparation, protective layer deposition, quantum dot growth and substrate post-cleaning treatment.
Example 1:
step one, immersing the quartz glass substrate into acetone for ultrasonic cleaning for 15 minutes, and taking out after ethanol ultrasonic cleaning for 10 minutes to remove surface impurities. After rinsing with deionized water for 45 seconds, the residual moisture was dried with nitrogen. Putting the processed substrate into a plasma cleaning machine, and vacuumizing to 10 DEG-1Pa, introducing oxygen to 10Pa, cleaning for 5 minutes and taking out.
And step two, placing the cleaned substrate on a sample table of an ion sputtering device, and then placing an Au metal target on a target table. Closing the sputtering bin cover, vacuumizing to about 10Pa, setting ionization current of 3mA, applying voltage on an electrode of an ion sputtering device, and enabling Au to be in the form of Au after the current is stabilized
Is deposited on a quartz glass substrate. The Au deposition time was controlled to 50s to obtain a 10nm thick Au thin film.
Thirdly, the substrate deposited with the Au film is moved into an annealing furnace, and the chamber is vacuumized to 10 degrees after being sealed-1Pa below, and raising the temperature of the substrate to 750 ℃ at a temperature raising speed of 6 ℃/s, wherein the vacuum pump is continuously operated during the heating. After the temperature is kept for 450s, the heating is stopped, and after the temperature is cooled to 150 ℃ in vacuum, the heating chamber is filled with air to reduce the atmospheric pressure and is cooled to the room temperature.
Fourthly, the substrate loaded with the Au nanoparticle array is placed in a magnetron sputtering chamber, and the chamber is vacuumized to 10 DEG-4Introducing Ar gas below Pa to10Pa, deposition of SiO 20nm thick using a radio frequency power supply2And (5) a thin film protective layer.
And fifthly, adding the Cd source and the Se source into the 1-octadecene, heating and stirring until the mixture is clear, and obtaining a precursor solution of the CdSe quantum dots. And (3) placing the substrate loaded with the Au nanoparticle array in a CdSe quantum dot precursor solution, and integrally heating the solution to 160 ℃ in a nitrogen atmosphere. The intensity of the light source is 500mW, and the diameter of a light spot is 1cm2And a 635nm wavelength red laser, irradiating the substrate for 15 seconds, and carrying out photo-thermal growth on the CdSe quantum dot array with the diameter of about 5 nm.
And sixthly, cooling to room temperature, removing the nitrogen atmosphere, taking out the substrate, placing the substrate in chloroform for ultrasonic cleaning for 15min, performing ultrasonic cleaning for 10min by using an ethanol solution, taking out the substrate and drying to obtain the substrate loaded with the CdSe quantum dot array.
Example 2:
the method comprises the following steps: and (3) immersing the GaN (0001) substrate into acetone for ultrasonic cleaning for 15 minutes, and performing ultrasonic cleaning with ethanol for 10 minutes to remove surface impurities and then taking out. After rinsing with deionized water for 45 seconds, the residual moisture was dried with nitrogen. Putting the processed substrate into a plasma cleaning machine, and vacuumizing to 10 DEG-1Pa, introducing oxygen to 10Pa, cleaning for 5 minutes and taking out.
Step two: the cleaned substrate is placed on a sample table of an ion sputtering device, and then an Ag metal target is placed on a target table (cathode). Closing the sputtering bin cover, vacuumizing to about 10Pa, setting ionization current of 3mA, applying voltage on the electrode of the ion sputtering device, and enabling Ag to react with Ag after the current is stabilized
Is deposited on a GaN (0001) substrate. The deposition time of Ag is controlled to be 20s, and an Ag film with the thickness of 5nm is obtained. The target material is replaced by metal Pt, the deposition operation is repeated, and a Pt film with the thickness of 5nm is deposited on the Ag film.
Step three: transferring the substrate deposited with Ag-Pt film into annealing furnace, sealing, and vacuumizing the chamber to 10%-1Introducing nitrogen to atmospheric pressure below Pa, and heating the substrate to 650 ℃ at a heating rate of 6 ℃/s. After incubation for 450s, heating was stoppedAnd cooling to room temperature and taking out.
Step four: placing the substrate loaded with the Ag-Pt nano particle array in a magnetron sputtering chamber, and vacuumizing the chamber to 10 DEG-4And introducing Ar gas below Pa to 10Pa, and depositing a 20 nm-thick silicon dioxide protective layer by using a radio frequency power supply.
Step five: adding a Cd source and a Se source into 1-octadecene, heating and stirring until the mixture is clear to obtain a precursor solution of the CdSe quantum dots, placing the substrate loaded with the Ag-Pt nanoparticle array in the precursor solution of the CdSe quantum dots, and integrally heating the solution to 160 ℃ in a nitrogen atmosphere. The intensity of the light source is 500mW, and the diameter of a light spot is 1cm2And a green laser with the wavelength of 532nm irradiates the substrate for 10 seconds to photo-thermally grow the CdSe quantum dot array with the diameter of about 6 nm.
Step six: and cooling to room temperature, removing nitrogen atmosphere, taking out the substrate, placing the substrate in chloroform for ultrasonic cleaning for 15min, performing ultrasonic cleaning for 10min by using an ethanol solution, taking out the substrate and drying to obtain the substrate loaded with the CdSe quantum dot array.
Example 3:
the method comprises the following steps: and immersing the Si substrate into acetone for ultrasonic cleaning for 15 minutes, and performing ultrasonic cleaning with ethanol for 10 minutes to remove surface impurities and then taking out. After rinsing with deionized water for 45 seconds, the residual moisture was dried with nitrogen. Putting the processed substrate into a plasma cleaning machine, and vacuumizing to 10 DEG-1Pa, introducing oxygen to 10Pa, cleaning for 5 minutes and taking out.
Step two: and placing the cleaned substrate on a sample table of an ion sputtering device, and then placing an Al metal target on a target table. The sputtering chamber lid was closed and the vacuum was pulled to about 10 deg.f-4Pa, introducing Ar gas to 10Pa, setting the ionization current to 4mA, applying voltage on an electrode of an ion sputtering device, and enabling Al to react with Al after the current is stabilized
Is deposited on the substrate. Controlling the Al deposition time to be 100s to obtain an Al film with the thickness of 20 nm.
Step three: the Al thin film was etched into a nanostructure array with a diameter of 150nm using photolithography.
Step four: the substrate loaded with the Al nano-structure array is moved into an annealing furnace, and after the substrate is sealed, the chamber is vacuumized to 10 DEG-1Introducing nitrogen to atmospheric pressure below Pa, and raising the substrate temperature to 800 ℃ at a temperature raising speed of 6 ℃/s. After the heat preservation for 1200s, the heating is stopped, the substrate is cooled to 150 ℃ under the nitrogen atmosphere, and the chamber of the annealing furnace is vacuumized to 10 DEG-4Introducing oxygen to atmospheric pressure below Pa, heating the substrate to 800 ℃ at the heating rate of 6 ℃/s, and keeping the temperature for 1800s to form an aluminum oxide protective layer on the surface of the aluminum nano-particles.
Step five: adding a Cd source and a Te source into 1-octadecene, heating and stirring until the mixture is clear to obtain a precursor solution of CdTe quantum dots, placing a substrate loaded with an Al nanoparticle array in the precursor solution of CdTe quantum dots, and heating the whole solution to 160 ℃ in a nitrogen atmosphere. The intensity of the light spot is 150mW, and the diameter of the light spot is 1cm2And a purple laser with the wavelength of 405nm irradiates the substrate for 10 seconds, and repeats three times of photo-thermal growth for CdTe quantum dot array with the diameter of about 8nm in the interval of 20 seconds.
Step six: and cooling to room temperature, removing nitrogen atmosphere, taking out the substrate, placing the substrate in chloroform for ultrasonic cleaning for 15min, performing ultrasonic cleaning for 10min by using an ethanol solution, taking out the substrate and drying to obtain the substrate loaded with the CdTe quantum dot array.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (6)
1. A preparation method of a controllable quantum dot array based on a photothermal effect is characterized by comprising the following steps:
selecting a certain substrate material, and cleaning the surface of the substrate material;
preparing a metal film by using a physical vapor deposition method, wherein the thickness of the metal film is 0.5-200 nm;
annealing the metal film under a vacuum condition or a protective atmosphere to prepare a metal nanoparticle array;
depositing or oxidizing the metal nanoparticle array to grow a protective layer, wherein the protective layer is an oxide or a nitride;
placing the substrate loaded with the metal nanoparticle array in a quantum dot precursor solution, and fixing or scanning and irradiating the metal nanoparticle array by using a light source, wherein the power density of the light source is 0.1-5W/cm2The light source is pulse type or continuous type laser;
and step six, after the step five is finished, carrying out ultrasonic cleaning on the substrate by using trichloromethane, and then carrying out ultrasonic cleaning on the substrate by using ethanol to prepare the controllable quantum dot array.
2. The method for preparing a controlled quantum dot array based on photothermal effect according to claim 1, wherein the metal thin film component In step two is composed of any one or more of Au, Ag, Cu, Al, In, Pt and Pd.
3. The method for preparing a controlled quantum dot array based on photothermal effect as claimed in claim 1, wherein the deposition in the physical vapor deposition method in the second step is any one of sputtering deposition, pulsed laser deposition and evaporation deposition.
4. The method for preparing a controlled quantum dot array based on photothermal effect according to claim 1, wherein the metal nanoparticle array in step three can be prepared by photolithography instead of the annealing treatment.
5. The method for preparing the controllable quantum dot array based on the photothermal effect according to claim 1, wherein the thickness of the protective layer in the fourth step is 0.1-100 nm.
6. The method for preparing the controllable quantum dot array based on the photothermal effect according to claim 1, wherein the quantum dot precursor solution in step five is in a flowing state.
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| CN109004508B (en) * | 2018-07-03 | 2020-01-17 | 北京邮电大学 | Single photon source based on quantum dots |
| CN111979526B (en) * | 2020-08-21 | 2022-10-28 | 南京工程学院 | Method and equipment for manufacturing zinc sulfide, lead sulfide and cadmium sulfide quantum dots |
| CN111826636B (en) * | 2020-08-21 | 2022-12-13 | 南京工程学院 | Method and equipment for manufacturing zinc oxide, titanium oxide or nickel oxide quantum dots in same cavity |
| CN113566979B (en) * | 2021-06-11 | 2023-06-13 | 北京理工大学 | Piezoelectric resonant infrared sensor, array thereof and manufacturing method thereof |
| CN113725341A (en) * | 2021-08-23 | 2021-11-30 | 广东工业大学 | Method for improving quantum dot light intensity |
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