CN113861985A - Preparation method of high-yield in-situ passivated mid-infrared HgTe colloidal quantum dots - Google Patents
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Abstract
A method for preparing high-yield in-situ passivated mid-infrared HgTe colloid quantum dots. Belonging to the field of colloidal quantum dot synthesis. Wherein the synthesis process adopts a hot injection method, and HgI containing halogen elements2Reactant as Hg source in reaction I‑The in-situ growth is carried out on the surface of the colloid quantum dot, the purpose of adjusting doping is achieved while the surface is passivated, and the p-type doping effect is achieved. And TMSTe is used as a Te source, and has high reactivity, so that the TMSTe can be fully reacted with Hg precursors, and cannot form a complex with Hg to limit the yield of HgTe.
Description
Technical Field
The invention belongs to the technical field of quantum dots, and particularly relates to a preparation method of high-yield in-situ passivated mid-infrared HgTe Colloidal Quantum Dots (CQDs).
Background art:
quantum Dots (QDs), also known as semiconductor Nanocrystals (NCs), are zero-dimensional nanometric quantum structures consisting of a small number of atoms, with three dimensions between 1-100 nm. In quantum dots, the number of atoms is typically between a few to several hundred. According to the quantum mechanics theory, when the size of the quantum dot is smaller than 2 times of the self exciton Bohr radius, the energy of the carrier in the quantum dot is quantized inevitably in the three-dimensional directions, the state density distribution is a series of discrete functions, and the carrier is restrained by the potential barrier and can not move freely in the three dimensions. Confinement can be attributed to electrostatic potential (generated by external electrodes, doping, strain, impurities, etc.), the interface of two different semiconductor materials and the surface of the semiconductor, or a combination of the three.
Colloidal Quantum Dots (CQDs) show excellent optical characteristics in research of nearly 30 years, and the colloidal quantum dots are widely applied to the fields of solar cells, photoelectric detectors, LEDs and the like due to the characteristics of adjustable optical band gaps, liquid phase synthesis machining, doping and energy level shift adjustment through surface treatment, high stacking density, good flexible substrate compatibility and the like. The HgTe material is a semimetal body, can realize band gap adjustability in the whole infrared range by controlling the size in principle, and has certain research in near infrared, mid infrared and long-wave infrared in recent years.
The synthesis method of HgTe colloidal quantum dots can be divided into two methods, namely aqueous solution synthesis and thermal injection. The aqueous solution synthesis method is to mix H2Te gas is introduced into deionized water solution dissolved in Hg source, HgTe CQDs with different sizes and band gaps are obtained by controlling corresponding reaction temperature and time, but the absorption band edge of the HgTe CQDs prepared by the method can only reach 2.5 mu m, and the medium wave range is basically not realized. In 2011, a Phillippe group adopts a thermal injection method to successfully synthesize HgTe CQDs with a band gap meeting the medium infrared wavelength, but the yield is low and the size distribution is large. In 2017, TMSTe is adopted as a Te source, and n-type HgTe CQDs with high yield and small size distribution are obtained.
The invention content is as follows:
aiming at the defects of the existing mid-infrared HgTe CQDs doping mode, a concentration gradient diffusion doping mode is mostly adopted, and good rectification characteristics are difficult to express in a junction device prepared subsequently. The invention provides a method for using HgI2As a Hg source, TMSTe was used as a Te source and was still synthesized by hot injection. The aim is to control better monodispersity and because of I-The quantum dot surface has strong binding energy, and the doping effect can be realized while the surface is passivated. And the preparation process is simpleIs easy to operate.
In order to achieve the purpose, the invention adopts the following scheme:
according to the theory of soft and hard acids and bases, I-Is soft alkali, Hg2+Is a soft acid, so HgI2Middle Hg+And I-The binding energy is strong and the preparation of the precursor solution requires elevated temperatures to break this strong bond. In the course of the reaction I-Will adsorb on the surface of HgTe colloid quantum dot, passivate the surface and adjust the doping. TMSTe is used as a reactant, a complex is not formed with Hg, the reaction activity is higher, the mass of the synthesized HgTe colloidal quantum dot meets the stoichiometric ratio calculation result, the full reaction is shown, and the yield of the colloidal quantum dot is high.
A method for preparing high-yield in-situ passivated mid-infrared HgTe Colloidal Quantum Dots (CQDs) specifically comprises the following steps:
(1) preparing Hg precursor solution;
(2) preparing a Te precursor solution;
(3) after the temperature is stable, injecting a Te precursor, and simultaneously controlling the temperature and the reaction time;
(4) stopping heating after the reaction is finished, injecting a solvent for quenching, and cooling in a water bath;
(5) purifying, dissolving and storing.
The preparation method of the Hg precursor solution in the step (1) comprises the following specific steps: a. purification of oleylamine (OAm) ligand: taking a certain amount of oleylamine, injecting into a three-neck flask, degassing at 147 deg.C for 3 hr, and then degassing in N2Cooling to room temperature under the atmosphere, and storing in a glove box for later use; b. preparing an Hg precursor solution: weighing a certain amount of HgI2Placing the powder into a three-neck flask, mixing oleylamine with the powder, degassing at room temperature for 20min, and degassing at 140 deg.C for 1 hr to destroy strong binding energy of Hg-I; then the temperature is reduced to 120 ℃ and N is introduced into the mixture2Keeping the temperature for 20min until the temperature is stable; preferably per 0.1mmol of HgI2Powder corresponds to 4mL oleylamine.
The step (2) of preparing the Te precursor solution comprises the following steps: mix TMSTe and hexane in a glass bottle in a glovebox for use; preferably 0.5mL hexane per 0.05mmol TMSTe (ditrimethylsilyl tellurium).
The step (3) is as follows: taking out the Te precursor solution by using an injection needle tube, injecting the Te precursor solution into the Hg precursor solution at 120 ℃, starting timing and simultaneously controlling the temperature to be 113-120 ℃ until the reaction is finished; wherein the molar ratio of Hg to Te is 2: 1.
The step (4) of quenching the reaction comprises the following steps: and (3) taking a Tetrachloroethylene (TCE) solvent, quickly injecting the solvent into the system in the step (3) when the reaction is finished, and quickly cooling the solvent to room temperature in an ice water bath.
The purification step in the step (5) is as follows: pouring the quenched solution into a centrifuge tube, adding anhydrous methanol into the centrifuge tube, centrifuging for 5min at a methanol to sample volume ratio of 2:1 and 4500r.p.m, pouring out the supernatant, leaving a black precipitate, rinsing the precipitate with anhydrous ethanol for 1 time, and washing with N2And (5) drying. The mass of the purified powder is 16mg, and the calculation result of the stoichiometric ratio is satisfied. The precipitate was then dispersed in TCE and stored in a glove box.
The HgTe CQDs synthesized by the method are controlled within 20 percent in size distribution, and the temperature control temperature and time are respectively changed to find that the size distribution tends to decrease first and then increase along with the extension of the temperature control time at different growth temperatures. The TEM image shows that different temperature control temperatures need to match the optimal temperature control growth time. And spin-coating CQDs solution on the photoetched silicon wafer to prepare the field effect transistor, and obtaining an obvious p-type doping effect through a tested transfer curve.
The invention has the beneficial effects that:
(1) the HgTe CQDs prepared by the method have good monodispersity and uniform size distribution.
(2) The HgTe CQDs prepared by the invention have obvious p-type doping characteristics.
(3) The HgTe CQDs prepared by the invention has weaker C-H peak strength (about 2900 cm) in Fourier infrared spectrum-1Peak position of (a), indicating the surface passivation effect of I-.
Drawings
FIG. 1 is an XRD diffraction pattern of HgTe CQDs synthesized in example 1 of the present invention;
FIG. 2 is a photograph under a transmission electron microscope of example 1-3HgTe CQDs of the present invention; the temperature used for differentiation is exemplified by the corresponding reaction time (i.e., the nucleus growth time). FIG. 3 is a graph showing the particle size of quantum dots with the prolonged reaction time at different temperature control temperatures of HgTe CQDs in the experimental examples 2-3;
FIG. 4 is a histogram of the particle size distribution of 100 particles of HgTe CQDs in example 1 of the present invention;
FIG. 5 is a graph showing an absorption spectrum of HgTe CQDs reacted at 120 ℃ for 3min in example 3 of the present invention;
FIG. 6 is a transfer curve of a field effect transistor fabricated with HgTe CQDs of the present invention example 1, showing a significant p-type doping behavior.
Detailed Description
To further illustrate the present invention, the preparation method of high yield in-situ passivated mid-infrared HgTe Colloidal Quantum Dots (CQDs) is described in detail below with reference to the examples.
Example 1
A preparation method of high-yield in-situ passivated mid-infrared HgTe Colloid Quantum Dots (CQDs) comprises the following specific steps:
(1) preparation of Hg precursor: for the preparation of the oleylamine ligand solution, a quantity of OAm was taken in a three-necked flask, degassed at 147 ℃ for 3h and subsequently placed under N2Cooling to room temperature under the atmosphere, and storing in a glove box for later use. 45.4mg (0.1mmol) of HgI were taken2The powder was placed in a three-necked flask, 4ml of OAm was taken in a glove box, and charged into the three-necked flask together with HgI2The powders were mixed and degassed at room temperature for 20min and then the temperature was raised to 140 ℃ and degassed for 1 h. The temperature was then lowered to 120 ℃ and held for 20min to stabilize the temperature.
(2) Preparation of Te precursor: mu.L (0.05mmol) of TMSTe was taken and mixed into 0.5ml of hexane;
(3) and (3) quickly injecting the Te precursor into the Hg precursor solution at 120 ℃, starting timing, setting the temperature to 113 ℃, and reacting for 10 min. At the end of the reaction, 15ml of TCE was injected into the flask to quench the reaction and cooled to room temperature in a water bath.
(4) The quenched solution was poured into a centrifuge tube toAdding anhydrous methanol and methanol into a centrifugal tube: quench solution 2:1 (v/v%), 4000 r.p.m. centrifuge for 5 min. Pouring out supernatant, rinsing with anhydrous ethanol for 1 time, and precipitating with N2After blow drying, the black precipitate was dispersed in 2ml of TCE and stored in a glove box.
Preparing a field effect transistor: heavily p-doped Si/SiO2The pieces were cut to a size of 1cm × 1cm, and successively cleaned with acetone, absolute ethanol, and deionized water by ultrasonic cleaning. Spin-coating photoresist AZ5214 on the silicon wafer at the rotation speed of 500 r.p.m.10 s and 4000 r.p.m.50 s, and baking the silicon wafer on a baking tray at 110 ℃ for 3min to fully dry the photoresist. The silicon wafer was exposed to uv light for 1.2s using an MJB4 reticle. And then the silicon chip is placed in a drying oven at 125 ℃ for 2min for 8s, and after being taken out, the silicon chip is subjected to flood exposure for another time for 22s under ultraviolet light. The exposed silicon wafer was developed in a developer for 39s and rinsed with deionized water for 10 s. The substrate was cleaned under oxygen plasma and dried for 5min to remove excess developer. The electrode evaporation adopts an electron beam evaporation method. Firstly, Ti with the thickness of 10nm is evaporated to be used as an adhesion layer, Au with the thickness of 70nm is deposited, the adhesion layer is ultrasonically stripped after being soaked in acetone for 1 hour, and the adhesion layer is washed and dried by ethanol and deionized water. HgTe QDs were dispersed in octane and prepared to 25mg/ml, spin-coated at 2000 r.p.m.30 s and subjected to solid phase ligand exchange with a volume ratio of 1:1:50(EDT: HCl: absolute ethanol), followed by washing with absolute ethanol, and the above steps were repeated 10 times to obtain quantum dot thin films about 200nm thick.
Example 2
A preparation method of high-yield in-situ passivated mid-infrared HgTe Colloid Quantum Dots (CQDs) comprises the following specific steps:
(1) preparation of Hg precursor: for the preparation of the oleylamine ligand solution, a quantity of OAm was taken in a three-necked flask, degassed at 147 ℃ for 3h and subsequently placed under N2Cooling to room temperature under the atmosphere, and storing in a glove box for later use. 45.4mg (0.1mmol) of HgI were taken2The powder was placed in a three-necked flask, 4ml of OAm was taken in a glove box, and charged into the three-necked flask together with HgI2The powders were mixed and degassed at room temperature for 20min and then the temperature was raised to 140 ℃ and degassed for 1 h. The temperature was then lowered to 120 ℃ and held for 20min to stabilize the temperature.
(2) Preparation of Te precursor: mixing 14 μ L of TMSTe in 0.5ml of hexane
(3) And (3) quickly injecting the Te precursor into the Hg precursor solution at 120 ℃, starting timing, setting the temperature to 115 ℃, and respectively taking samples for reaction for 1,3,5,7 and 10min to quench in the TCE solution. At the end of the reaction, 15ml of TCE was injected into the flask to quench the reaction and cooled to room temperature in a water bath.
(4) The quenched solution was poured into a centrifuge tube, and anhydrous methanol, methanol: quench solution 2:1 (v/v%), 4000 r.p.m. centrifuge for 5 min. Pouring out supernatant, rinsing with anhydrous ethanol for 1 time, and precipitating with N2After blow drying, the black precipitate was dispersed in 2ml of TCE and stored in a glove box.
Example 3
A preparation method of high-yield in-situ passivated mid-infrared HgTe Colloid Quantum Dots (CQDs) comprises the following specific steps:
(1) preparation of Hg precursor: for the preparation of the oleylamine ligand solution, a quantity of OAm was taken in a three-necked flask, degassed at 147 ℃ for 3h and subsequently placed under N2Cooling to room temperature under the atmosphere, and storing in a glove box for later use. 45.4mg (0.1mmol) of HgI were taken2The powder was placed in a three-necked flask, 4ml of OAm was taken in a glove box, and charged into the three-necked flask together with HgI2The powders were mixed and degassed at room temperature for 20min and then the temperature was raised to 140 ℃ and degassed for 1 h. The temperature was then lowered to 120 ℃ and held for 20min to stabilize the temperature.
(2) Preparation of Te precursor: mixing 14 μ L of TMSTe in 0.5ml of hexane
(3) And (3) quickly injecting the Te precursor into the Hg precursor solution at 120 ℃, starting timing, setting the temperature to 120 ℃, and respectively taking samples for reaction for 1,3,5,7 and 10min, and quenching in the TCE solution. At the end of the reaction, 15ml of TCE was injected into the flask to quench the reaction and cooled to room temperature in a water bath.
(4) The quenched solution was poured into a centrifuge tube, and anhydrous methanol, methanol: quench solution 2:1 (v/v%), 4000 r.p.m. centrifuge for 5 min. Pouring out supernatant, rinsing with anhydrous ethanol for 1 time, and precipitating with N2After blow drying, the black precipitate was dispersed in 2ml of TCE and stored in a glove boxIn (1).
Claims (9)
1. A method for preparing high-yield in-situ passivated mid-infrared HgTe Colloidal Quantum Dots (CQDs) is characterized by comprising the following steps:
(1) preparing Hg precursor solution;
(2) preparing a Te precursor solution;
(3) after the temperature is stable, injecting a Te precursor, and simultaneously controlling the temperature and the reaction time;
(4) stopping heating after the reaction is finished, injecting a solvent for quenching, and then cooling in a water bath;
(5) purifying, dissolving and storing;
the preparation method of the Hg precursor solution in the step (1) comprises the following specific steps: a. purification of oleylamine (OAm) ligand: taking a certain amount of oleylamine, injecting into a three-neck flask, degassing at 147 deg.C for 3 hr, and then degassing in N2Cooling to room temperature under the atmosphere, and storing in a glove box for later use; b. preparing an Hg precursor solution: weighing a certain amount of HgI2Placing the powder into a three-neck flask, mixing oleylamine with the powder, degassing at room temperature for 20min, and degassing at 140 deg.C for 1 hr to destroy strong binding energy of Hg-I; then the temperature is reduced to 120 ℃ and N is introduced into the mixture2Keeping the temperature for 20min until the temperature is stable; preferably per 0.1mmol of HgI2Powder corresponds to 4mL oleylamine.
The step (2) of preparing the Te precursor solution comprises the following steps: mix TMSTe and hexane in a glass bottle in a glovebox for use; preferably 0.5mL hexane per 0.05mmol of TMSTe (bistrimethylsilyl tellurium).
The step (3) is as follows: taking out the Te precursor solution by using an injection needle tube, injecting the Te precursor solution into the Hg precursor solution at 120 ℃, starting timing and simultaneously controlling the temperature to be 113-120 ℃ until the reaction is finished; wherein the molar ratio of Hg to Te is 2: 1. The mass of the prepared HgTe CQDs is about 16mg (about 0.05mmol), and the quantitative calculation result of the stoichiometric ratio is satisfied.
2. A method of producing high yield in situ passivated mid-red according to claim 1The external HgTe Colloid Quantum Dot (CQDs) method is characterized in that the HgI of every 0.1mmol in the step (1)2Powder corresponds to 4mL oleylamine.
3. A method for preparing high yield in situ passivated mid-infrared HgTe Colloidal Quantum Dots (CQDs) according to claim 1 wherein step (2) is performed with 0.5mL hexane per 0.05 mmole of tmste (bistrimethylsilyl tellurium).
4. A method for preparing high yield in situ passivated mid-infrared HgTe Colloidal Quantum Dots (CQDs) according to claim 1 wherein the molar ratio of Hg to Te in step (3) is 2: 1.
5. The method for preparing high yield in-situ passivated mid-infrared HgTe Colloidal Quantum Dots (CQDs) according to claim 1 wherein said step (4) of quenching the reaction comprises the steps of: and (3) taking a Tetrachloroethylene (TCE) solvent, quickly injecting the solvent into the system in the step (3) when the reaction is finished, and quickly cooling the solvent to room temperature in an ice water bath.
6. The method for preparing high yield in-situ passivated mid-infrared HgTe Colloidal Quantum Dots (CQDs) according to claim 1 wherein said step (5) of purifying comprises the steps of: pouring the quenched solution into a centrifuge tube, adding anhydrous methanol into the centrifuge tube at a volume ratio of methanol to sample of 2:1, centrifuging, pouring out the supernatant, leaving a black precipitate, rinsing the precipitate with anhydrous ethanol for 1 time, and adding N2Blow-drying, dispersing in TCE, and storing in glove box.
7. A method of preparing high yield in situ passivated mid-infrared HgTe Colloidal Quantum Dots (CQDs) prepared according to the method of any one of claims 1-6.
8. A method of producing high yield in situ passivated mid-infrared HgTe Colloidal Quantum Dots (CQDs) prepared according to the method of any of claims 1-6, the HgTe CQDs size distribution being controlled to within 20%.
9. A method of preparing high yield in-situ passivated mid-infrared HgTe Colloidal Quantum Dots (CQDs) prepared according to the method of any of claims 1-6, being p-type doped.
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