CN116709880B - Single photon source based on single phosphorescence molecular field effect transistor and preparation method thereof - Google Patents
Single photon source based on single phosphorescence molecular field effect transistor and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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- H10K50/844—Encapsulations
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
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- H—ELECTRICITY
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
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- H—ELECTRICITY
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/30—Coordination compounds
- H10K85/341—Transition metal complexes, e.g. Ru(II)polypyridine complexes
- H10K85/346—Transition metal complexes, e.g. Ru(II)polypyridine complexes comprising platinum
Abstract
The invention relates to the technical field of molecular photoelectric devices, and provides a single photon source based on a single phosphorescence molecular field effect tube and a preparation method thereof.
Description
Technical Field
The invention relates to the technical field of molecular photoelectric devices, in particular to a preparation method of a single photon source based on a single phosphorescence molecular field effect transistor.
Background
With the development of quantum information technology in recent years, quantum photonics has also received attention. Quantum information technology uses a single quantum object to encode and manipulate information, thereby having a great influence on technology, wherein the most mature quantum key and tamper-proof voting protocol, quantum simulation and calculation and the like are in a commercially viable stage, and guarantee is provided for the data security and reliability of the information age nowadays. One of the biggest achievements in modern science is the proposition of photons, which in order to realize the application potential of quantum photonics, three technologies are required as supports, including photon counters, linear and nonlinear photonic circuits, and single photon sources. In recent years, although great progress has been made in the two aspects, the lack of a single photon source certainly hinders the development of quantum technology, and the generation of single photons is a first condition for single photon communication and is one of the current quantum secret communication research hotspots.
The single photon source, whether continuous laser or pulsed laser or electro-excited, emits only one photon during the spontaneous emission lifetime, also known as the anti-bunching process. The most common single photon sources are spontaneous radiation based on nonlinear frequency conversion or based on single quantum emitters, such as InGaAs near infrared emission, gallium arsenide emission red spectral range, and II-VI telluride or selenide quantum dots, and nitrides are based on III-V quantum dots and the like as single photon sources, and the single photon sources in the prior art can generate single photons, but the preparation condition is harsh due to the fact that the single photons are emitted by utilizing defects of the single photon sources, and the purity of emitted photons is low, and the problems of random generation, uncontrollable emission efficiency and the like of the photons exist.
Disclosure of Invention
The present invention is directed to solving at least one of the technical problems existing in the related art. Therefore, the invention provides a preparation method of a single photon source based on a single phosphorescence molecular field effect transistor, which comprises the following steps:
s1: preparing a dielectric layer;
s2: preparing a graphene array electrode on the dielectric layer;
s3: constructing a graphene nano gap point electrode based on the graphene array electrode;
s4: self-assembling single phosphorescent molecules and the graphene nanometer gap point electrode to obtain a single phosphorescent molecule field effect tube;
s5: plating an h-BN protective layer on the single phosphorescence molecular field effect transistor to obtain a single photon source;
wherein the structural formula of the single phosphorescent molecule comprises:
、、
、
or (b)
One of them.
According to the preparation method of the single photon source based on the single phosphorescence molecular field effect transistor, the step S1 comprises the following steps:
s11: spin-coating photoresist on a pure silicon wafer, carrying out photoetching grid to obtain a first negative film, evaporating metal on the first negative film to obtain a second negative film, immersing the second negative film in acetone solution to remove photoresist and obtain a third negative film;
s12: spin-coating photoresist on the third negative film, and carrying out photoetching grid to obtain a bottom grid;
s13: plating an aluminum film with the thickness of 30-40 mm on the surface of the bottom gate by magnetron sputtering, and then placing the bottom gate in an acetone solution for removing glue to obtain dielectric layer aluminum oxide;
s14: and plating a hafnium oxide film with the thickness of 3-10 mm on the aluminum oxide surface of the dielectric layer by atomic beam deposition to obtain the dielectric layer.
According to the preparation method of the single photon source based on the single phosphorescence molecular field effect transistor, the step S2 comprises the following steps:
s21: performing chemical vapor deposition on the copper sheet to obtain single-layer graphene;
s22: adhering the single-layer graphene to a quartz plate by using a transparent adhesive tape, spin-coating methyl methacrylate on the quartz plate, and etching by using RIE oxygen plasma to obtain a graphene quartz plate;
s23: oxidizing the graphene quartz plate in ferric trichloride solution, soaking in hydrochloric acid aqueous solution, peeling off a graphene layer on the graphene quartz plate, transferring the graphene layer onto the dielectric layer, and removing the colloid to obtain a graphene dielectric layer;
s24: photoetching a strip on the graphene dielectric layer, exposing the strip by ultraviolet, and then performing oxygen plasma etching to obtain a graphene silicon wafer;
s25: exposing the graphene silicon wafer by ultraviolet, and plating a magnetic material on one end of the graphene silicon wafer by using magnetron sputtering to obtain a graphene silicon wafer containing a magnetic electrode;
s26: and exposing the graphene silicon wafer containing the magnetic electrode by ultraviolet, evaporating chromium with the diameter of 8-10 nm and gold with the diameter of 60-80 nm at the other end of the graphene silicon wafer containing the magnetic electrode, and obtaining the graphene silicon wafer containing the magnetic electrode and the gold electrode, namely the graphene array electrode.
According to the preparation method of the single photon source based on the single phosphorescence molecular field effect transistor, the step S3 comprises the following steps:
s31: etching a dotted line with the length of 150 nm and the width of 5 nm on the graphene array electrode by using an electron beam, and developing by using a developing solution to obtain a graphene dot electrode;
s32: and etching the graphene point electrode by using oxygen plasma RIE, and then performing on-off test on the graphene point electrode by using a source meter and a probe station to obtain the graphene nanometer gap point electrode.
According to the preparation method of the single photon source based on the single phosphorescence molecular field effect transistor, the step S4 comprises the following steps:
s41: placing the graphene nanometer gap point electrode in a two-mouth flask, adding 1- (3-dimethylaminopropyl) -3-2-ethylcarbodiimide hydrochloride and the single phosphorescent molecule into the two-mouth flask, sealing the two-mouth flask, and then performing ventilation operation to ensure that the two-mouth flask is in a nitrogen atmosphere;
s42: 10ml of anhydrous pyridine is extracted by an injector and injected into the two-mouth flask to react for 48 hours, so as to obtain the single phosphorescence molecular field effect tube.
According to the preparation method of the single photon source based on the single phosphorescence molecule field effect transistor, the mol ratio of the single phosphorescence molecule to the 1- (3-dimethylaminopropyl) -3-2 ethyl carbodiimide hydrochloride is 1: 20-1: 40.
the invention also provides a single photon source prepared by the preparation method of the single photon source based on the single phosphorescence molecular field effect tube, which comprises the single phosphorescence molecular field effect tube and an h-BN protective layer; the single phosphorescence molecular field effect transistor is provided with an h-BN protective layer.
The above technical solutions in the embodiments of the present invention have at least one of the following technical effects:
1. the preparation method of the single photon source based on the single phosphorescence molecular field effect transistor, which is provided by the invention, is based on the preparation of the graphene single molecular field effect transistor, has a mature device preparation flow, selects single phosphorescence molecules as functional molecules, can ensure the generation of single photons, and has the characteristics of good stability and long excited state life.
2. According to the preparation method of the single photon source based on the single phosphorescence molecular field effect transistor, provided by the invention, the emission of single photons can be regulated and controlled through the electrical characteristics such as bias voltage, grid voltage and the like based on the construction of a solid grid and an electrical system, so that the generation of the single photons with controllable wavelength can be realized.
3. The preparation method of the single photon source based on the single phosphorescence molecular field effect transistor, provided by the invention, has the advantages that the construction of the magnetic electrode improves the polarization certainty of the single photon source by introducing spin current, and can also realize the high-purity and high-quality single photon source by introducing external factors such as a light source, temperature, a magnetic field and the like for regulation and control, thereby promoting the development of quantum information technology.
4. The invention provides a preparation method of a single photon source based on a single phosphorescence molecular field effect transistor, which uses platinum single phosphorescence molecules as phosphorescence molecules and passes through-NH at the bottom end of the phosphorescence molecules 2 Forming amide covalent bond with-COOH at end of graphene point electrode to bridge, constructing graphene-based structureThe single photon source of the single molecular field effect transistor realizes the emission of single photons with controllable wavelength, provides technical support for the emission of single photons with high purity and high efficiency, and lays a foundation for the further development of quantum information technology.
Additional aspects and advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Drawings
In order to more clearly illustrate the invention or the technical solutions of the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the invention, and other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of the structure of a single photon source made in accordance with the present invention.
Fig. 2 is a light emission diagram of a single photon source provided by the present invention.
Fig. 3 is a morphology diagram of the hand-torn graphene provided by the invention.
Fig. 4 is a characteristic diagram of current variation along with gate voltage when the bias voltage of the graphene single-molecule field effect transistor provided by the invention is 0.1V.
Reference numerals:
1. a graphene dot electrode pair; 2. a gold electrode; 3. a magnetic electrode; 4. a graphene silicon wafer; 5. h-BN protective layer; 6. a single phosphorescent molecule; 7. a hand-torn graphene region; 8. a single photon amplified region.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings, and it is apparent that the described embodiments are some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. The following examples are illustrative of the invention but are not intended to limit the scope of the invention.
Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the embodiments of the present invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
The following describes a method for preparing a single photon source based on a single phosphorescence molecular field effect transistor according to the present invention with reference to fig. 1 to 4.
The invention provides a preparation method of a single photon source based on a single phosphorescence molecular field effect transistor, which comprises the following steps:
s1: preparing a dielectric layer;
s2: preparing a graphene array electrode on the dielectric layer;
s3: constructing a graphene nano gap point electrode based on the graphene array electrode;
s4: self-assembling single phosphorescent molecules and the graphene nanometer gap point electrode to obtain a single phosphorescent molecule field effect tube;
s5: plating an h-BN protective layer on the single phosphorescence molecular field effect transistor to obtain a single photon source;
wherein the structural formula of the single phosphorescent molecule comprises:
、、
、
or (b)
One of them.
Wherein, the liquid crystal display device comprises a liquid crystal display device,the preparation method of the (C) comprises the following steps.
Under argon, add into a three-necked flask(30.0 mmol), L-proline (12.0 mmol), cuI (6.0 mmol), K2CO3 (60.0 mmol), and->(60.0 mmol) and DMSO (140.0 ml) were stirred at 120℃for 3 days. After the reaction was completed, the reaction mixture was cooled to room temperature, quantified with water (100 mL), diluted with ethyl acetate (100 mL), the mixture was filtered with silicate, and then washed with ethyl acetate. The organic layer was separated and the aqueous layer was extracted twice with ethyl acetate. Combining the organic layers, drying over anhydrous sodium sulfate, filtering, spin-drying, and purifying with silica gel column chromatography to obtain。
Under argon, add into a three-necked flask(7.70 mmol) hydrogen bromide acid ]20 mL, 48%) and acetic acid (40 mL) solution, reflux at 120 ℃ for 2 days. The mixture was then cooled to room temperature and then neutralized with sodium bicarbonate solution until no gas was generated. The mixture was extracted three times with ethyl acetate. Combining the organic layers, drying, filtering, concentrating the filtrate under reduced pressure to obtain +.>。
Sequentially adding into a double-mouth bottle（30.0 mmol）、/>（33.0 mmol）、CuI（3.0 mmol）、K 2 CO 3 (60.0 mmol) and 100ml DMF are heated to 130-140 ℃ under argon atmosphere, and the temperature is kept for reaction for 30 hours. After the reaction was completed, the mixture was cooled to room temperature, and 1L water was added, followed by extraction with 50 ml ethyl acetate three times, the organic layers were combined, dried, spin-dried, and purified by silica gel chromatography to give。
Will be(3 mmol) dissolved in DMSO solvent of 30 ml, stirred under nitrogen atmosphere, followed by addition of +.>(3 mmol), cuI (0.3 mmol), picolinic acid (0.6 mmol) and K 3 PO 4 (6.3 mmol). After the addition was complete, the reaction mixture was heated to 100 ℃ and reacted under nitrogen atmosphere 6 d. After the completion of the reaction, the reaction mixture was poured into 300 ml water, and extracted three times with methylene chloride (50 ml), and the extracted organic solvent was dried over anhydrous sodium carbonate, followed by removal of the solvent under reduced pressure. The crude product was purified by chromatography on silica gel to give。
Will be(2 mmol) was dissolved in 30 ml redistilled THF under argon and stirred at 0℃for one hour, then 2.5M lithium aluminum hydride (3 mmol) was slowly added dropwise at this temperature. The reaction solution was left to stand at room temperature for further stirring for 6 hours, then the above reaction solution was slowly poured into ice water, extracted three times with methylene chloride (50 ml), and the solvent was removed to obtain an amino-substituted crude product. Then the crude product is dissolved in 20 ml hydrochloric acid (12%) at 0 ℃, 2 ml acetonitrile is added for assisting dissolution, and the mixture is stirred until complete dissolution; then slowly 5 ml at low temperature containing NaNO 2 (3 mmol) and stirring for 30 min; the diazonium salt solution was then poured into a flask containing KBr (4 mmol) and 1.7 ml of 48% aqueous HBr. The solution was heated under reflux for 5 hours, and then extracted three times with dichloromethane. The organic layer was washed with 1 mol/L aqueous NaOH solution and with MgSO 4 Drying, removing solvent, purifying the obtained product by silica gel chromatography to obtain +.>。
Will be（1 mmol）、K 2 PtCl 4 (1.1 mmol) and n-Bu 4 NBr (0.1 mmol) was added sequentially to a dry three-necked flask, and AcOH (52 mL) was then added to the flask under nitrogen atmosphere at room temperature. The reaction mixture was bubbled with nitrogen for 20 minutes, followed by stirring at room temperature for 9 hours. The flask was then placed in an oil bath and the reaction mixture was heated to 110-120 ℃. After 3 days, the resulting mixture was cooled to room temperature and the solvent was dried by spinning. Purifying the residue by silica gel column chromatography to obtain +.>。
Sequentially adding the components into a flask containing 50 ml toluene under nitrogen atmosphere（0.2 mmol）、/>（0.3 mmol）、Pd(PPh 3 ) 4 (0.02 mmol) and 5 ml K 2 CO 3 (2 mmol) of the aqueous solution. After refluxing 1 d under nitrogen and cooling, the reaction mixture was poured into water and extracted three times with dichloromethane (50 ml), the resulting organic layer was dried and the solvent was removed under reduced pressure. Purifying the crude product by silica gel column chromatography to obtain。
Wherein, the liquid crystal display device comprises a liquid crystal display device,the preparation of (2) comprises the following steps.
Sequentially adding into a double-mouth bottle（30.0 mmol）、/>（33.0 mmol）、CuI（3.0 mmol）、K 2 CO 3 (60.0 mmol) and 100ml DMF are heated to 130-140 ℃ under argon atmosphere, and the temperature is kept for reaction for 30 hours. After the reaction was completed, the mixture was cooled to room temperature, and 1L water was added, followed by extraction with 50 ml ethyl acetate three times, the organic layers were combined, dried, spin-dried, and purified by silica gel chromatography to give。
Will be(3 mmol) dissolved in DMSO solvent of 30 ml, stirred under nitrogen atmosphere, followed by addition of +.>（3 mmol), cuI (0.3 mmol), picolinic acid (0.6 mmol) and K 3 PO 4 (6.3 mmol). After the addition was complete, the reaction mixture was heated to 100 ℃ and reacted under nitrogen atmosphere 6 d. After the completion of the reaction, the reaction mixture was poured into 300 ml water, and extracted three times with methylene chloride (50 ml), and the extracted organic solvent was dried over anhydrous sodium carbonate, followed by removal of the solvent under reduced pressure. The crude product was purified by chromatography on silica gel to give。
Will be(2 mmol) was dissolved in 30 ml redistilled THF under argon and stirred at 0℃for one hour, then 2.5M lithium aluminum hydride (3 mmol) was slowly added dropwise at this temperature. The reaction solution was left to stand at room temperature for further stirring for 6 hours, then the above reaction solution was slowly poured into ice water, extracted three times with methylene chloride (50 ml), and the solvent was removed to obtain an amino-substituted crude product. Then the crude product is dissolved in 20 ml hydrochloric acid (12%) at 0 ℃, 2 ml acetonitrile is added for assisting dissolution, and the mixture is stirred until complete dissolution; then slowly 5 ml at low temperature containing NaNO 2 (3 mmol) and stirring for 30 min; the diazonium salt solution was then poured into a flask containing KBr (4 mmol) and 1.7 ml of 48% aqueous HBr. The solution was heated under reflux for 5 hours, and then extracted three times with dichloromethane. The organic layer was washed with 1 mol/LNaOH aqueous solution and with MgSO 4 Drying, removing solvent, purifying the obtained product by silica gel chromatography to obtain +.>。
Will be（1 mmol）、K 2 PtCl 4 (1.1 mmol) and n-Bu 4 NBr (0.1 mmol) was added sequentially to a dry three-necked flask, and AcOH (52 mL) was then added to the flask under nitrogen atmosphere at room temperature. The reaction is carried outThe mixture was bubbled with nitrogen for 20 minutes, followed by stirring at room temperature for 9 hours. The flask was then placed in an oil bath and the reaction mixture was heated to 110-120 ℃. After 3 days, the resulting mixture was cooled to room temperature and the solvent was removed again. Purifying the residue by silica gel column chromatography to obtain +.>。/>
Sequentially adding the components into a flask containing 50 ml toluene under nitrogen atmosphere（0.2 mmol）、/>（0.3 mmol）、Pd(PPh 3 ) 4 (0.02 mmol) and 5 ml K 2 CO 3 (2 mmol) of the aqueous solution. After refluxing 1 d under nitrogen and cooling, the reaction mixture was poured into water and extracted three times with dichloromethane (50 ml), the resulting organic layer was dried and the solvent was removed under reduced pressure. Purifying the crude product by silica gel column chromatography to obtain。
Wherein, the liquid crystal display device comprises a liquid crystal display device,the preparation of (2) comprises the following steps.
Sequentially adding into a double-mouth bottle（30.0 mmol）、/>（33.0 mmol）、CuI（3.0 mmol）、K 2 CO 3 (60.0 mmol) and 100ml DMF are heated to 130-140 ℃ under argon atmosphere, and the temperature is kept for reaction for 30 hours. After the reaction was completed, the mixture was cooled to room temperature, and 1L water was added, followed by extraction with 50 ml ethyl acetate three times, the organic layers were combined, dried, spin-dried, and purified by silica gel chromatography to give/>。
Sequentially adding into dry double-mouth bottles(15 mmol) and 20 ml tetrahydrofuran, then cooled to 0℃under argon and stirred for 30 minutes. Then using a syringe to contain LiAlH 4 A solution of (30.0 mmol) of tetrahydrofuran was slowly poured into the reaction, the reaction was allowed to proceed at this temperature for 1 hour, and the reaction was slowly allowed to return to room temperature and stirred overnight. After the reaction, the solution is slowly added into a proper amount of ice water, then 50 ml ethyl acetate is extracted for three times, the organic layers are combined, dried and spin-dried, and purified by a silica gel chromatography to obtain +.>。
Sequentially adding into dry double-mouth bottles(10.0 mmol) and 20 ml tetrahydrofuran, then cooled to 0℃under argon and stirred for 30 minutes. Then, a tetrahydrofuran solution containing KOMe (30.0 mmol) was slowly injected into the reaction with a syringe, the temperature was maintained for 1 hour, and CH was then slowly added 3 I (25.0 mmol). The reaction was slowly brought to room temperature and stirred overnight. After the reaction, the solution is slowly added into a proper amount of ice water, then the ethyl acetate of 50 ml is extracted for three times, the organic layers are combined, dried and spin-dried, and purified by a silica gel chromatography to obtain。
Will be(3 mmol) dissolved in DMSO solvent of 30 ml, stirred under nitrogen atmosphere, followed by addition of +.>（3mmol), cuI (0.3 mmol), picolinic acid (0.6 mmol) and K 3 PO 4 (6.3 mmol). After the addition was complete, the reaction mixture was heated to 100 ℃ and reacted under nitrogen atmosphere 6 d. After the completion of the reaction, the reaction mixture was poured into 300 ml water, and extracted three times with methylene chloride (50 ml), and the extracted organic solvent was dried over anhydrous sodium carbonate, followed by removal of the solvent under reduced pressure. The crude product was purified by chromatography on silica gel to give +.>。
Will be(2 mmol) was dissolved in 30 ml redistilled THF under argon and stirred at 0℃for one hour, then 2.5M lithium aluminum hydride (3 mmol) was slowly added dropwise at this temperature. The solvent obtained by the reaction was left to stand at room temperature for further stirring for 6 hours, then the above reaction solution was slowly poured into ice water, and extracted three times with methylene chloride (50 ml), and the solvent was removed to obtain an amino-substituted crude product. Then the crude product is dissolved in 20 ml hydrochloric acid (12%) at 0 ℃, 2 ml acetonitrile is added for assisting dissolution, and the mixture is stirred until complete dissolution; then slowly 5 ml at low temperature containing NaNO 2 (3 mmol) and stirring for 30 min; the diazonium salt solution was then poured into a flask containing KBr (4 mmol) and 1.7 ml of 48% aqueous HBr. The solution was heated under reflux for 5 hours, and then extracted three times with dichloromethane. The organic layer was washed with 1 mol/LNaOH aqueous solution and with MgSO 4 Drying, removing solvent, purifying the obtained product by silica gel chromatography to obtain +.>。
Will be（1 mmol）、K 2 PtCl 4 (1.1 mmol) and n-Bu 4 NBr (0.1 mmol) was sequentially added to a dry three-necked flask, and AcOH (52 mL) was then added to the flask under a nitrogen atmosphere at room temperature. The reaction mixture was bubbled with nitrogen for 20 minutes, followed by stirring at room temperature for 9 hours. The flask was then placed in an oil bath and the reaction mixture was heated to 110-120 ℃. After 3 days, the resulting mixture was cooled to room temperature and the solvent was removed again. Purifying the residue by silica gel column chromatography to obtain +.>。/>
Sequentially adding the components into a flask containing 50 ml toluene under nitrogen atmosphere（0.2 mmol）、/>（0.3 mmol）、Pd(PPh 3 ) 4 (0.02 mmol) and 5 ml K 2 CO 3 (2 mmol) of the aqueous solution. After refluxing 1 d under nitrogen and cooling, the reaction mixture was poured into water and extracted three times with dichloromethane (50 ml), the resulting organic layer was dried and the solvent was removed under reduced pressure. Purifying the crude product by silica gel column chromatography to obtain。
Wherein, the liquid crystal display device comprises a liquid crystal display device,the preparation of (2) comprises the following steps.
Sequentially adding into a double-mouth bottle（33.0 mmol）、/>（30.0 mmol）、CuI（3.0 mmol）、K 2 CO 3 (60.0 mmol) and 100ml DMF are heated to 130-140 ℃ under argon atmosphere, and the temperature is kept for reaction for 30 hours. After the reaction was completed, the mixture was cooled to room temperature, and 1L water was added, followed by extraction three times with 50 ml ethyl acetate, and the organic layers were combined, dried, spin-dried, and extracted with silica gel chromatographyPure, get->。
Will be(3 mmol) dissolved in DMSO solvent of 30 ml, stirred under nitrogen atmosphere, followed by addition of +.>(3 mmol), cuI (0.3 mmol), picolinic acid (0.6 mmol) and K 3 PO 4 (6.3 mmol). After the addition was complete, the reaction mixture was heated to 100 ℃ and reacted under nitrogen atmosphere 6 d. After the completion of the reaction, the reaction mixture was poured into 300 ml water, and extracted three times with methylene chloride (50 ml), and the extracted organic solvent was dried over anhydrous sodium carbonate, followed by removal of the solvent under reduced pressure. The crude product was purified by chromatography on silica gel to give。
Will be(2 mmol) was dissolved in 30 ml redistilled THF under argon and stirred at 0℃for one hour, then 2.5M lithium aluminum hydride (3 mmol) was slowly added dropwise at this temperature. The reaction solution was left to stand at room temperature for further stirring for 6 hours, then the above reaction solution was slowly poured into ice water, extracted three times with methylene chloride (50 ml), and the solvent was removed to obtain an amino-substituted crude product. Then the crude product is dissolved in 20 ml hydrochloric acid (12%) at 0 ℃, 2 ml acetonitrile is added for assisting dissolution, and the mixture is stirred until complete dissolution; then slowly 5 ml at low temperature containing NaNO 2 (3 mmol) and stirring for 30 min; the diazonium salt solution was then poured into a flask containing KBr (4 mmol) and 1.7 ml of 48% aqueous HBr. The solution was heated under reflux for 5 hours, and then extracted three times with dichloromethane. The organic layer was washed with 1 mol/L aqueous NaOH solution and with MgSO 4 Drying, removing solvent, and subjecting the obtained product to silica gel chromatographyPurifying to obtain->。
Will be（1 mmol）、K 2 PtCl 4 (1.1 mmol) and n-Bu 4 NBr (0.1 mmol) was added sequentially to a dry three-necked flask, and AcOH (52 mL) was then added to the flask under nitrogen atmosphere at room temperature. The reaction mixture was bubbled with nitrogen for 20 minutes, followed by stirring at room temperature for 9 hours. The flask was then placed in an oil bath and the reaction mixture was heated to 110-120 ℃. After 3 days, the resulting mixture was cooled to room temperature and the solvent was removed again. Purifying the residue by silica gel column chromatography to obtain +.>。
Sequentially adding the components into a flask containing 50 ml toluene under nitrogen atmosphere（0.2 mmol）、/>（0.3 mmol）、Pd(PPh 3 ) 4 (0.02 mmol) and 5 ml K 2 CO 3 (2 mmol) of the aqueous solution. After refluxing 1 d under nitrogen and cooling, the reaction mixture was poured into water and extracted three times with dichloromethane (50 ml), the resulting organic layer was dried and the solvent was removed under reduced pressure. Purifying the crude product by silica gel column chromatography to obtain +.>。
Wherein, the liquid crystal display device comprises a liquid crystal display device,the preparation of (2) comprises the following steps.
Under argon, add into a three-necked flask(30.0 mmol), L-proline (12.0 mmol), cuI (6.0 mmol), K 2 CO 3 （60.0 mmol）、/>(60.0 mmol) and DMSO (140.0 ml) were stirred at 120℃for 3 days. After the reaction was completed, the reaction mixture was cooled to room temperature, quantified with water (100 mL), diluted with ethyl acetate (100 mL), the mixture was filtered with silicate, and then washed with ethyl acetate. The organic layer was separated and the aqueous layer was extracted twice with ethyl acetate. Combining the organic layers, drying over anhydrous sodium sulfate, filtering, spin-drying, and purifying with silica gel column chromatography to obtain。
Under argon, add into a three-necked flask(7.70 mmol), hydrogen bromide (20 mL, 48%) and acetic acid (40 mL) were refluxed for 2 days at 120 ℃. The mixture was then cooled to room temperature and then neutralized with sodium bicarbonate solution until no gas was generated. The mixture was extracted three times with ethyl acetate. Combining the organic layers, drying, filtering, concentrating the filtrate under reduced pressure to obtain +.>。
Will be(3 mmol) dissolved in DMSO solvent of 30 ml, stirred under nitrogen atmosphere, followed by addition of +.>(3 mmol), cuI (0.3 mmol), picolinic acid (0.6 mmol) and K 3 PO 4 (6.3 mmol). After the addition was complete, the reaction mixture was heated to 100 ℃ and reacted under nitrogen atmosphere 6 d. After the reaction was completed, the reaction mixture was poured into 300 ml water and was treated with methylene chloride(50 ml) extraction was performed three times, and the organic solvent obtained by the extraction was dried over anhydrous sodium carbonate, followed by removal of the solvent under reduced pressure. The crude product was purified by chromatography on silica gel to give。
By mixing the above materials(2 mmol) was dissolved in 30 ml redistilled THF under argon and stirred at 0℃for one hour, then 2.5M lithium aluminum hydride (3 mmol) was slowly added dropwise at this temperature. The solvent obtained by the reaction was left to stand at room temperature for further stirring for 6 hours, then the above reaction solution was slowly poured into ice water, and extracted three times with methylene chloride (50 ml), and the solvent was removed to obtain an amino-substituted crude product. Then the crude product is dissolved in 20 ml hydrochloric acid (12%) at 0 ℃, 2 ml acetonitrile is added for assisting dissolution, and the mixture is stirred until complete dissolution; then slowly 5 ml at low temperature containing NaNO 2 (3 mmol) and stirring for 30 min; the diazonium salt solution was then poured into a flask containing KBr (4 mmol) and 1.7 ml of 48% aqueous HBr. The solution was heated under reflux for 5 hours, and then extracted three times with dichloromethane. The organic layer was washed with 1 mol/L aqueous NaOH solution and with MgSO 4 Drying, removing solvent, purifying the obtained product by silica gel chromatography to obtain +.>。
Will be（1 mmol）、K 2 PtCl 4 (1.1 mmol) and n-Bu 4 NBr (0.1 mmol) was added sequentially to a dry three-necked flask, and AcOH (52 mL) was then added to the flask under nitrogen atmosphere at room temperature. The reaction mixture was bubbled with nitrogen for 20 minutes, followed by stirring at room temperature for 9 hours. The flask was then placed in an oil bath and the reaction mixture was heated to 110-120 ℃. After 3 days, the resulting mixture was cooled to room temperature and the solvent was removed again. The residue was purified by column chromatography on silica gelPurifying by chromatography to obtain ∈10->。
Sequentially adding the components into a flask containing 50 ml toluene under nitrogen atmosphere（0.2 mmol）、/>（0.3 mmol）、Pd(PPh 3 ) 4 (0.02 mmol) and 5 ml K 2 CO 3 (2 mmol) of the aqueous solution. After refluxing 1 d under nitrogen and cooling, the reaction mixture was poured into water and extracted three times with dichloromethane (50 ml), the resulting organic layer was dried and the solvent was removed under reduced pressure. Purifying the crude product by silica gel column chromatography to obtain。
According to the preparation method of the single photon source based on the single phosphorescence molecular field effect transistor, the step S1 comprises the following steps.
S11: spin-coating photoresist on a pure silicon wafer, performing photoetching grid to obtain a first negative film, evaporating metal on the first negative film to obtain a second negative film, immersing the second negative film in acetone solution to remove photoresist and obtain a third negative film.
Wherein, the surface of the pure silicon wafer is covered with 300-400 nm silicon oxide.
Further, the grid electrode photoetched on the first negative film is mainly used for subsequent needle-down test and can also be used for subsequent photoetching calibration.
Further, metal is evaporated on the first negative film, and 8-10 nm of chromium and 60-80 nm of gold are evaporated by a thermal evaporation method.
S12: and spin-coating photoresist on the third negative film, and carrying out photoetching grid to obtain a bottom grid.
Wherein, the bottom grid needs to be connected with the evaporated metal.
S13: plating an aluminum film with the thickness of 30-40 mm on the surface of the bottom gate by magnetron sputtering, and then placing the bottom gate in acetone solution for photoresist removal to obtain the dielectric layer aluminum oxide.
Wherein, magnetron sputtering is used to plate an aluminum film with the thickness of 30-40 nm on the surface as a grid electrode for applying bias voltage, and after acetone is used for removing glue, the dielectric layer alumina is obtained through natural oxidation.
S14: and plating a hafnium oxide film with the thickness of 3-10 mm on the aluminum oxide surface of the dielectric layer by atomic beam deposition to obtain the dielectric layer.
According to the preparation method of the single photon source based on the single phosphorescence molecular field effect transistor, S2 comprises the following steps.
S21: and performing chemical vapor deposition on the copper sheet to obtain single-layer graphene.
The step S21 is a chemical vapor deposition method, and a manual graphene tearing method may be selected to obtain a graphene layer, and the specific operation steps are as follows.
And sticking a layer of graphene on the graphene blocks through an adhesive tape, tightly attaching the dielectric layer to the adhesive tape, standing for 4-5 h, uncovering the adhesive tape, and screening to obtain the graphene dielectric layer.
Wherein, the time for uncovering the adhesive tape can be shortened by heating for 2min at 110 ℃; further, the color of the graphene is observed under a microscope, screening is performed, and about 2-4 layers of graphene are selected for the next operation.
Further, as shown in fig. 3, the hand-torn graphene region 7 generally has about 2-4 layers of graphene therein.
S22: and adhering the single-layer graphene to a quartz plate by using a transparent adhesive tape, spin-coating methyl methacrylate on the quartz plate, and etching by using RIE oxygen plasma to obtain the graphene quartz plate.
S23: and (3) oxidizing the graphene quartz plate in ferric trichloride solution, then soaking in hydrochloric acid aqueous solution, peeling off a graphene layer on the graphene quartz plate, transferring the graphene layer onto the dielectric layer, and removing the colloid to obtain the graphene dielectric layer.
In one embodiment, a single layer of graphene is obtained by chemical vapor deposition on a copper sheet, the single layer of graphene is glued to a clean quartz sheet by transparent glue, polymethyl methacrylate (950 PMMA) is spin-coated, 600 revolutions per minute of spin coating is s, then 4000 revolutions per minute of spin coating is 40 s, a heating table is used for heating for two minutes, RIE oxygen plasma is used for etching the graphene on the back surface of the copper sheet, after etching is completed, the copper sheet is cut into 1X 1 blocks, the back surface of the obtained copper sheet is placed downwards in a configured ferric trichloride solution, the graphene layer is finally transferred to a dielectric layer by soaking in a hydrochloric acid solution and an aqueous solution, and the glue is removed by heating for 8 minutes at 120 ℃ by using an acetone solution, so that the graphene dielectric layer is obtained.
S24: and photoetching a strip on the graphene dielectric layer, exposing the strip by ultraviolet, and then performing oxygen plasma etching to obtain the graphene silicon wafer.
And exposing the strips with the width of 40 mu m and the length of 200 mu m on the graphene dielectric layer by using ultraviolet photoresist, wherein the portions of the strips which need to be reserved are protected by the photoresist, the rest portions are removed by using a developing solution, the graphene dielectric layer below the photoresist is exposed, and oxygen plasma etching is performed on the exposed graphene dielectric layer, and after etching is completed, the residual photoresist is removed by using acetone, so that the graphene silicon wafer is obtained.
S25: and exposing the graphene silicon wafer by ultraviolet, and plating a magnetic material of 70nm on one end of the graphene silicon wafer by using magnetron sputtering to obtain the graphene silicon wafer containing the magnetic electrode 3.
Spin-coating ultraviolet photoresist on a graphene silicon wafer, carrying out photoetching electrodes, carrying out development after ultraviolet exposure, and plating a 70nm magnetic electrode 3 on the graphene silicon wafer after development by using magnetron sputtering, wherein the magnetic electrode 3 comprises any one of iron, cobalt or nickel metal; finally, removing redundant metal and photoresist by using acetone to obtain the graphene silicon wafer containing the magnetic electrode 3, as shown in figure 1. The magnetic electrode 3 results in efficient spin filtering such that only one spin type passes, thereby introducing a spin current in the test, affecting the polarization properties of the emitted photons.
S26: and exposing the graphene silicon wafer containing the magnetic electrode 3 by ultraviolet, evaporating 8-10 nm chromium and 60-80 nm gold at the other end of the graphene silicon wafer containing the magnetic electrode 3, and obtaining the graphene silicon wafer containing the magnetic electrode and the gold electrode, namely a graphene array electrode.
The method comprises the steps of spin coating ultraviolet photoresist on a graphene silicon wafer containing a magnetic electrode 3, carrying out photoetching electrode, carrying out development after ultraviolet exposure, carrying out evaporation plating on the graphene silicon wafer containing the magnetic electrode 3 by using a thermal evaporation plating method after development, wherein 8 nm chromium and 80 nm gold are used as electrodes at the other end, namely a gold electrode 2, finally removing redundant metal and photoresist by using acetone to obtain a graphene array electrode, and as shown in fig. 1, the graphene array electrode comprises a graphene silicon wafer 4, a gold electrode 2 and a magnetic electrode 3, wherein the graphene silicon wafer 4 is positioned at the bottommost layer, and the gold electrode 2 and the magnetic electrode are respectively arranged at two ends of the graphene silicon wafer 4.
As shown in fig. 1, the portion between the magnetic electrode 3 and the gold electrode 2 is referred to as a graphene channel.
Further, the conductivity of the graphene array electrode obtained above was tested at a voltage of 50 mV using an SM-6-probe stage, and a graphene array electrode having a conductivity of the order of 10 μa was selected.
According to the preparation method of the single photon source based on the single phosphorescence molecular field effect transistor, S3 comprises the following steps.
S31: and etching the graphene array electrode with the length of 150 nm and the width of 5 nm by using an electron beam, and developing by using a developing solution to obtain the graphene dot electrode.
Wherein PMMA was spin-coated on the graphene array electrode, and the graphene dot electrode was obtained by etching 150 a nm a length and 5 a nm a width of a dotted line in each graphene channel with an electron beam, and developing with an isopropyl alcohol diluted methyl isobutyl ketone (MIBK, volume ratio: MIBK/isopropyl alcohol=1/3) solution.
S32: and etching the graphene point electrode by using oxygen plasma RIE, and then performing on-off test on the graphene point electrode by using a source meter and a probe station to obtain the graphene nanometer gap point electrode.
As shown in fig. 1, the graphene nano gap point electrode is based on a graphene array electrode, a graphene point electrode pair 1 is etched by a dotted line, and a nano gap of 1-10 nm is formed between the graphene point electrode pair 1.
According to the preparation method of the single photon source based on the single phosphorescence molecular field effect transistor, the step S4 comprises the following steps.
S41: placing the graphene nanometer gap point electrode in a two-mouth flask, adding 1- (3-dimethylaminopropyl) -3-2-ethylcarbodiimide hydrochloride and the single phosphorescent molecule into the two-mouth flask, sealing the two-mouth flask, and then performing ventilation operation to ensure that the two-mouth flask is in a nitrogen atmosphere.
S42: 10ml of anhydrous pyridine is extracted by an injector and injected into the two-mouth flask to react for 48 hours, so as to obtain the single phosphorescence molecular field effect tube.
And taking out the prepared single phosphorescence molecular field effect tube from the two-mouth flask, respectively cleaning the single phosphorescence molecular field effect tube with acetone and ultrapure water for three times, and finally drying the surface for standby by nitrogen.
Wherein platinum single phosphorescence molecules are taken as phosphorescence molecules, and pass through-NH at the bottom end of the platinum single phosphorescence molecules 2 The graphene single-molecule field effect tube is obtained by bridging amide covalent bonds formed in the nanogap by-COOH at the end of the graphene nanogap electrode, and according to fig. 4, it can be seen that the graphene single-molecule field effect tube shows conductivity characteristics varying with the grid voltage under the condition of constant bias voltage, which indicates that phosphorescent molecules are successfully connected into the graphene nanogap electrode, and can be regulated and controlled by adjusting the grid voltage.
Further, preparing a layer of hexagonal boron nitride with the thickness of 1-20 nm, namely an h-BN protective layer 5 on the surface of a graphene single-molecule field effect tube to obtain a single photon source, wherein as shown in figure 1, on a graphene silicon wafer 4, one end is a gold electrode 2, one end is a magnetic electrode 3, a graphene point electrode pair 1 is prepared between the gold electrode 2 and the magnetic electrode 3, amide covalent bonds are formed between nano gaps of the graphene point electrode pair 1 by introducing single phosphorescent molecules 6 to carry out bridging, the single phosphorescent molecular field effect tube is obtained, and the single-photon source is obtained by plating an h-BN protective layer 5 on the single phosphorescent molecular field effect tube.
Further, as can be seen from fig. 2, the single photon source emits a single photon with high purity and good stability, wherein the single photon amplification region 8 can further prove that the single photon source prepared by the invention emits a single photon with high purity and good stability. Because the functional molecule of the single photon source is a single phosphorescence molecule, only one photon can be emitted at the next time under the given excitation, and the relative position between the front line molecular orbit and the fermi level of the electrode is determined under the given grid, the position of electrons reaching the excited state is basically controllable, so that the purity of the emitted single photon is higher, and under the regulation of different grid voltages, the relative position between the front line molecular orbit and the fermi level of the electrode can be regulated, so that charges reach different excited states, and photons with different wavelengths can be emitted.
Meanwhile, in the testing process, the testing temperature can be changed by using a TTPX low-temperature probe station, a specific light source is applied to the device by using a laser, the spectrum characteristics of the emitted single photons are regulated and controlled by using a PPMS comprehensive physical property measuring system to apply magnetic fields with different intensities, and the like, so that the purity and the emission efficiency of the single photon source are further improved.
According to the preparation method of the single photon source based on the single phosphorescence molecule field effect transistor, the mol ratio of the single phosphorescence molecule to the 1- (3-dimethylaminopropyl) -3-2 ethyl carbodiimide hydrochloride is 1: 20-1: 40.
the invention also provides a single photon source prepared by the preparation method of the single photon source based on the single phosphorescence molecular field effect tube, which comprises the single phosphorescence molecular field effect tube and an h-BN protective layer; the single phosphorescence molecular field effect transistor is provided with an h-BN protective layer.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (7)
1. The preparation method of the single photon source based on the single phosphorescence molecular field effect transistor is characterized by comprising the following steps:
s1: preparing a dielectric layer;
s2: preparing a graphene array electrode on the dielectric layer;
s3: constructing a graphene nano gap point electrode based on the graphene array electrode;
s4: self-assembling single phosphorescent molecules and the graphene nanometer gap point electrode to obtain a single phosphorescent molecule field effect tube;
s5: plating an h-BN protective layer on the single phosphorescence molecular field effect transistor to obtain a single photon source;
wherein the structural formula of the single phosphorescent molecule comprises:
、、
、
or (b)
One of them.
2. The method for preparing a single photon source based on a single phosphorescence molecular field effect transistor according to claim 1, wherein the step S1 comprises the following steps:
s11: spin-coating photoresist on a pure silicon wafer, carrying out photoetching grid to obtain a first negative film, evaporating metal on the first negative film to obtain a second negative film, immersing the second negative film in acetone solution to remove photoresist and obtain a third negative film;
s12: spin-coating photoresist on the third negative film, and carrying out photoetching grid to obtain a bottom grid;
s13: plating an aluminum film with the thickness of 30-40 mm on the surface of the bottom gate by magnetron sputtering, and then placing the bottom gate in an acetone solution for removing glue to obtain dielectric layer aluminum oxide;
s14: and plating a hafnium oxide film with the thickness of 3-10 mm on the aluminum oxide surface of the dielectric layer by atomic beam deposition to obtain the dielectric layer.
3. The method for preparing a single photon source based on a single phosphorescence molecular field effect transistor according to claim 1, wherein the step S2 comprises the following steps:
s21: performing chemical vapor deposition on the copper sheet to obtain single-layer graphene;
s22: adhering the single-layer graphene to a quartz plate by using a transparent adhesive tape, spin-coating methyl methacrylate on the quartz plate, and etching by using RIE oxygen plasma to obtain a graphene quartz plate;
s23: oxidizing the graphene quartz plate in ferric trichloride solution, soaking in hydrochloric acid aqueous solution, peeling off a graphene layer on the graphene quartz plate, transferring the graphene layer onto the dielectric layer, and removing the colloid to obtain a graphene dielectric layer;
s24: photoetching a strip on the graphene dielectric layer, exposing the strip by ultraviolet, and then performing oxygen plasma etching to obtain a graphene silicon wafer;
s25: exposing the graphene silicon wafer by ultraviolet, and plating a magnetic material on one end of the graphene silicon wafer by using magnetron sputtering to obtain a graphene silicon wafer containing a magnetic electrode;
s26: and exposing the graphene silicon wafer containing the magnetic electrode by ultraviolet, evaporating chromium with the diameter of 8-10 nm and gold with the diameter of 60-80 nm at the other end of the graphene silicon wafer containing the magnetic electrode, and obtaining the graphene silicon wafer containing the magnetic electrode and the gold electrode, namely the graphene array electrode.
4. The method for preparing a single photon source based on a single phosphorescence molecular field effect transistor according to claim 1, wherein the step S3 comprises the following steps:
s31: etching a dotted line with the length of 150 nm and the width of 5 nm on the graphene array electrode by using an electron beam, and developing by using a developing solution to obtain a graphene dot electrode;
s32: and etching the graphene point electrode by using oxygen plasma RIE, and then performing on-off test on the graphene point electrode by using a source meter and a probe station to obtain the graphene nanometer gap point electrode.
5. The method for preparing a single photon source based on a single phosphorescence molecular field effect transistor according to claim 1, wherein the step S4 comprises the following steps:
s41: placing the graphene nanometer gap point electrode in a two-mouth flask, adding 1- (3-dimethylaminopropyl) -3-2-ethylcarbodiimide hydrochloride and the single phosphorescent molecule into the two-mouth flask, sealing the two-mouth flask, and then performing ventilation operation to ensure that the two-mouth flask is in a nitrogen atmosphere;
s42: 10ml of anhydrous pyridine is extracted by an injector and injected into the two-mouth flask to react for 48 hours, so as to obtain the single phosphorescence molecular field effect tube.
6. The method for preparing a single photon source based on single phosphorescence molecular field effect transistor according to claim 5, wherein the molar ratio of single phosphorescence molecule to 1- (3-dimethylaminopropyl) -3-2 ethylcarbodiimide hydrochloride is 1: 20-1: 40.
7. a single photon source prepared by the method for preparing single photon source based on single phosphorescence molecular field effect transistor according to any one of claims 1-6, comprising single phosphorescence molecular field effect transistor and h-BN protective layer; the single phosphorescence molecular field effect transistor is provided with an h-BN protective layer.
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