CN113969171A - Preparation method of doped MXene quantum dots, optical film and QLED - Google Patents
Preparation method of doped MXene quantum dots, optical film and QLED Download PDFInfo
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- C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
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Abstract
The invention discloses a preparation method of doped MXene quantum dots, an optical film and a QLED. The preparation method of the doped MXene quantum dot comprises the following steps: providing MXene; dispersing MXene in a mixed solution of concentrated nitric acid and concentrated sulfuric acid to obtain an MXene quantum dot solution; and adding a sulfur source and/or a nitrogen source into the MXene quantum dot solution for reaction to prepare the doped MXene quantum dot. The MXene quantum dots are subjected to dispersion treatment by adopting the mixed solution of concentrated nitric acid and concentrated sulfuric acid, so that the obtained MXene quantum dots are purer and more beneficial to doping, and the MXene quantum dots are doped by using the inorganic sulfur source and/or the inorganic nitrogen source, so that the defects on the surfaces of the quantum dots can be changed, the size of the quantum dots can be changed by generating hydrogen bonds, and the quantum dots can emit light with different wavelengths.
Description
Technical Field
The invention relates to the technical field of quantum dot material preparation, in particular to a preparation method of doped MXene quantum dots, an optical film and a QLED.
Background
MXene is a kind of metal carbide and metal nitride material with two-dimensional layered structure and similar to sheet-stacked sheet structure, and is two-dimensional crystal of transition metal carbide or carbonitride with chemical formula of Mn+1XnN is 1, 2 or 3, M is a transition metal element in the early stage, and X is carbon or/and nitrogen.
MXene has potential applications in many fields, including as energy storage materials, sensors, catalysts, etc., because of its unique structural, electronic, and chemical properties, and quantum dots derived from two-dimensional inorganic MXene have begun to receive considerable attention.
Disclosure of Invention
At present, the preparation method of MXene quantum dots mainly comprises a chemical solution growth method, an epitaxial growth method, an electric field confinement method and the like.
However, in the actual use process, the inventors found that the above preparation methods have a common disadvantage that the emission wavelength of the MXene quantum dots prepared by the above methods is not controllable, in addition to respective disadvantages such as low conductivity, high cost, low yield and the like.
Based on this, according to the first aspect of the present invention, there is provided a method for preparing doped MXene quantum dots, comprising the steps of:
providing MXene;
dispersing MXene in a mixed solution of concentrated nitric acid and concentrated sulfuric acid to obtain an MXene quantum dot solution;
and adding a sulfur source and/or a nitrogen source into the MXene quantum dot solution for reaction to prepare the doped MXene quantum dot.
According to a second aspect of the present invention, there is provided an optical film comprising a hydrophilic polymer and doped MXene quantum dots dispersed in the hydrophilic polymer, the doped MXene quantum dots being prepared by the preparation method as described above.
According to a third aspect of the present invention, there is provided a QLED comprising a light-emitting layer, wherein the light-emitting layer is made of the optical film as described above.
According to the invention, the preparation method of the doped MXene quantum dots capable of emitting light with different wavelengths is provided.
Drawings
Fig. 1 is a schematic flow chart of a method for preparing doped MXene quantum dots according to an embodiment of the present invention.
Detailed Description
It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
As shown in fig. 1, the preparation method of the doped MXene quantum dot according to the present invention comprises the following steps:
s100, providing MXene;
s200, dispersing MXene in a mixed solution of concentrated nitric acid and concentrated sulfuric acid to obtain an MXene quantum dot solution;
s300, adding a sulfur source and/or a nitrogen source into the MXene quantum dot solution for reaction to prepare the doped MXene quantum dot.
The present invention does not limit the preparation method of MXene to step S100. For example, MXene prepared by any preparation method such as a chemical liquid etching method or the like can be provided.
For example, in some embodiments, step S100 may include the steps of:
s101, grinding MXene monomers into MXene powder by a ball milling method;
s102, heating MXene powder to 1000-1400 ℃ in an inert atmosphere such as nitrogen or inert gas, calcining, and grinding to obtain powder;
s103, adding the powder into an HF solution, carrying out solid-liquid separation, and washing and drying a solid part to obtain MXene. MXene can be selected from Ti2C、Ti3C2、(Ti0.5,Nb0.5)2C、(V0.5,Cr0.5)3C2、Nb2C、Ti3CN and Ta4C3One or more of (a).
Unless otherwise specified, in the present invention, concentrated nitric acid refers to HNO3The mass content of the nitric acid solution is more than 68 percent, and the concentrated sulfuric acid is H2SO4A sulfuric acid solution having a mass content of 70% or more.
In some embodiments, MXene is dispersed using a mixed solution of concentrated nitric acid and concentrated sulfuric acid in step S200. This is because the inventors found that when etching is performed using, for example, an HF solution in step S100, there may be a case where the powder is not completely broken. Meanwhile, the inventors have also surprisingly found that the above-described mixed solution is capable of oxidizing the portions that are not completely broken, so that the powder is substantially completely broken to form quantum dot particles. In addition, the etching of the above mixed solution is relatively mild as compared with, for example, the strong etching of an HF solution, and quantum dot particles of a predetermined size are easily obtained.
To ensure that the mixed solution has a strong oxidizing property suitable for substantially completely breaking the powder, in some embodiments, the volume of the concentrated nitric acid is less than the volume of the concentrated sulfuric acid in the mixed solution, preferably the volume ratio of the concentrated nitric acid to the concentrated sulfuric acid is 1 (2-5), such that the strong oxidizing property is more suitable, more preferably the volume ratio of the concentrated nitric acid to the concentrated sulfuric acid is 1:3, it is most suitable that the oxidation is strong.
In addition, the inventor also unexpectedly found that, compared with the existing MXene prepared by the chemical liquid phase etching method, which is affected by the concentration and reaction time of the chemical etchant (for example, if the reaction time is too short or the etchant is too corrosive, MXene cannot be prepared, and if the etchant is too corrosive, the MAX phase may be completely dissolved), only MXene with a two-dimensional system and a surface having a functional group such as F, OH can be obtained, and pure MXene quantum dots cannot be obtained, the MXene is dispersed by using a mixed solution of concentrated nitric acid and concentrated sulfuric acid (for example, when MXene is prepared by the chemical liquid phase etching method, MXene is dispersed by using the above mixed solution after being corroded by the HF solution, and MXene can be prevented from being corroded and dissolved by the HF solution), and the obtained MXene quantum dots are purer. Meanwhile, compared with MXene with a two-dimensional system, the obtained MXene quantum dots with a zero-dimensional system have better dispersibility in water and a non-aqueous medium, thereby being more beneficial to functionalization or doping.
In other embodiments, in step S200, the ratio of MXene to mixed solution is (1-5) g:10mL, such as 1g:10mL, 2g:10mL, 3g:10mL, 5g:10mL, and the like. In such a ratio, the strong oxidizing property of the mixed solution can be sufficiently exerted, and MXene can be dispersed into quantum dot particles in a predetermined size. If the ratio is less than 1g to 10mL, excessive etching may be caused, so that the MXene structure is damaged and quantum dots cannot be formed. If the ratio is greater than 5g to 10mL, insufficient etching may result so that MXene is still in the bulk material and no quantum dots are formed.
In still other embodiments, after the step S200, after the step of dispersing MXene in the mixed solution of concentrated nitric acid and concentrated sulfuric acid, the method further includes: heating, cooling to room temperature, and adjusting the pH value to be neutral to obtain the MXene quantum dot solution. Wherein the heating temperature is 90-110 deg.C, such as 90 deg.C, 100 deg.C, 105 deg.C, 110 deg.C, etc. Heating at this temperature can promote the etching of MXene by the mixed solution. The heating time is 10-15 h, such as 10h, 12h, 14h and 15 h. The pH value is adjusted to be neutral, so that the obtained MXene quantum dots are purer and more beneficial to functionalization or doping.
In some embodiments, in step S300, the reaction temperature is 150 to 170 ℃, such as 150 ℃, 160 ℃, 165 ℃ and 170 ℃, and the reaction time is 12 to 15 hours, such as 12 hours, 13 hours, 14 hours and 15 hours, so as to make the reaction more complete. In other embodiments, the reaction is a hydrothermal reaction.
In other embodiments, in step S300, after the reaction, a purification process may be further performed. Wherein the purification treatment can be performed by washing the obtained product with a dialysis membrane. Further, the cut-off molecular weight of the dialysis membrane can be 1000-2000Da, such as 1000Da, 1200Da, 1500Da, 2000Da, etc., and the number of washing times can be 2-4, such as 2, 3, and 4.
In still other embodiments, in step S300, both the sulfur source and the nitrogen source are inorganic. The inorganic substance enables more sufficient doping, i.e., the sulfur source and the nitrogen source as the inorganic substance are more likely to enter MXene, particularly when the reaction is a hydrothermal reaction, than when the organic substance, particularly the nitrogen source, is urea. Preferably, the sulfur source may be selected from sodium thiosulfate (Na)2S2O3) Sulfur powder, sodium sulfide (Na)2S), sodium sulfite (Na)2SO3) And sodium dithionate (Na)2S2O6) Preferably, the nitrogen source may be selected from ammonia (NH)3·H2O), ammonium chloride (NH)4Cl) and ammonium bicarbonate (NH)4HCO3) One or more of (a).
In still other embodiments, in step S300, the ratio of MXene quantum dot solution to sulfur source is 1mL (0.05-0.1) g, such as 1mL:0.05g, 1mL:0.06g, 1mL:0.08g, 1mL:0.1g, etc., and the ratio of MXene quantum dot solution to nitrogen source is 1mL (0.7-1.4) mmol, such as 1: 0.7mmol, 1: 1.05mmol, 1: 1.26mmol and 1: 1.4mmol, etc. It will be appreciated that when both a sulphur source and a nitrogen source are used, the same is true.
By adopting the proportion, particularly after MXene is dispersed by using a mixed solution of concentrated nitric acid and concentrated sulfuric acid (namely the combination of the step S200 and the step S300), the MXene quantum dots can be effectively doped by a sulfur source and/or a nitrogen source, so that the surface electron distribution of the MXene quantum dots is changed, different defects are generated, hydrogen bonds are formed with bound water, a firm and ordered hydrogen bond network is formed through C-O-C bonds, the size of the quantum dots is changed by the generated hydrogen bond network, and the obtained doped quantum dots emit light with different wavelengths.
Specifically, when the sulfur source is used for doping, OS and S are formed in an MXene quantum dot system2Or C-S-C, so that the formation of electronic defects is less, corresponding hydrogen bonds are less, and S-doped MXene quantum dots with smaller sizes can be obtained, so that the light-emitting wavelength of the S-doped MXene quantum dots corresponds to blue light. When the sulfur source is used for doping, N can form pyrrole (with the structure of C-N bond) in the MXene quantum dot system
) C ═ N bond. The electron-shrinkage defect is generated due to the formation of a C ═ N bond, the electron defect site has a strong negative electric type, so that more hydrogen bonds are easily formed with water molecules (the formation barrier of the C-N or C ═ N bond is smaller than that of the C-S bond, so that hydrogen bonds are more easily formed by doping N), and the light-emitting wavelength of the N-doped MXene quantum dot corresponds to green light. When the sulfur source and the nitrogen source are used, the formation of pyrrole-like C-N-C bonds is increased due to the existence of N, the formation of electronic defects is increased due to the C-S-C bonds besides the C-N bonds, a larger hydrogen bond network is finally formed, the size of particles is increased due to the formation of the hydrogen bonds, the corresponding delocalized pi electron energy level is reduced, the wavelength is red-shifted, and the light-emitting wavelength of the S/N doped MXene quantum dots corresponds to red light.
Therefore, the doped MXene quantum dots prepared according to the embodiment of the invention can emit light with different wavelengths, and can be applied to the fields of full-color quantum dot illumination and display.
The invention also provides an optical film, which comprises a hydrophilic polymer and doped MXene quantum dots dispersed in the hydrophilic polymer, wherein the doped MXene quantum dots are prepared from any one of the embodiments, and the mass ratio of the doped MXene quantum dots to the doped MXene quantum dots is preferably 1:8, such as 4:7, 1:2, 1:4, 1:5 and the like.
Compared with the case of using a hydrophobic polymer, the inventor finds that the hydrophilic polymer can realize the effect of mixing with the doped MXene quantum dots more uniformly without modifying the surfaces of the MXene quantum dots.
In some embodiments, the hydrophilic polymer may be selected from one or more of polyvinylpyrrolidone, polyacrylic acid, polyvinyl alcohol, and polyethylene oxide.
In addition, the invention also provides a QLED, which comprises a light-emitting layer, wherein the light-emitting layer is made of any one of the optical films.
In the present invention, the type and preparation method of the QLED are not limited, and known QLED types and preparation methods such as those described in CN106252522A, which is incorporated herein by reference in its entirety, may be employed. Further, a QLED may also include, but is not limited to, a cathode, an anode, and optional functional layers such as a hole injection layer and/or a hole transport layer, an electron injection layer and/or an electron transport layer, and the like. A hole injection layer and/or a hole transport layer may be disposed between the anode and the light emitting layer, and an electron injection layer and/or an electron transport layer may be disposed between the cathode and the light emitting layer.
In the present invention, the materials and parameters such as thickness of the cathode, anode and functional layer are not limited as long as the present invention can be implemented, and are not described herein again.
The present invention will be described in detail below with reference to specific examples.
Example 1
(1)MXene：Ti3C2Preparation of
Mixing Ti with a molar ratio of 1:12And ball milling the AlC and the TiC into mixed powder by a ball milling method, wherein the ball milling time is 10 h. Then, the temperature was raised to 1200 ℃ at 5 ℃/min, and after calcination at 1200 ℃ for 3 hours under argon protection, MXene powder was obtained by crushing with a mortar and pestle. Then, 5g of MXene powder was added to 5mL of HF solution (50 mol%), stirred at 25 ℃ for 3 hours to obtain a suspension, which was then washed with deionized water 2 times and centrifuged to obtain Ti3C2Wet deposit. Finally, adding Ti3C2The wet deposit was dried in a vacuum oven at 70 ℃ for 14h to give MXene: ti3C2。
(2)Ti3C2Preparation of Quantum dot solutions
Mixing 1g of Ti3C2Adding into 10mL of mixed solution of concentrated nitric acid and concentrated sulfuric acid (volume ratio of 1:2), and heating at 100 deg.C under reflux for 12 hr to obtain Ti3C2And (4) dispersing. Then, it was diluted with 100mL of deionized water and cooled to 25 ℃ in an ice bath. Subsequently, the resulting product was added to NaOH until the pH reached 7 to obtain Ti3C2A quantum dot solution.
(3) N-doped Ti3C2Preparation of quantum dots
mu.L (0.7mmol) of NH3·H2O to 1mL of Ti3C2The quantum dot solution is transferred to a 50mL reaction kettle and heated to 150 ℃ and kept for 15 h. Then, after the reaction, the product is washed for 2 times by a dialysis membrane (the molecular weight cut-off is 1000Da) and dried to finally obtain the N-doped Ti3C2And (4) quantum dots.
(4) Based on N-doped Ti3C2Preparation of optical thin film of quantum dots
0.1g of N was doped with Ti3C2Adding the quantum dots into 1mL of water to obtain N-doped Ti3C2Quantum dot solution, then uniformly mixing 1mL of the quantum dot solution and 0.5g of polyvinylpyrrolidone (PVP) to obtain N-doped Ti3C2Quantum dot/PVP composite material. Then, N-doped Ti3C2Pouring the quantum dot/PVP composite material into a culture dish, maintaining and aging for 3 days at room temperature to obtain N-doped Ti3C2Quantum dot/PVP thin films.
Example 2
(1)MXene：(Ti0.5,Nb0.5)2Preparation of C
Will (Ti)0.5,Nb0.5)2And ball-milling the AlC into powder by using a ball milling method, wherein the ball milling time is 15 h. Then, the mixture was heated to 1300 ℃ at a rate of 5 ℃/min, calcined at 1300 ℃ for 2.5 hours under argon atmosphere, and crushed with a mortar and pestle to obtain MXene powder. Subsequently, 6g of MXene powder was added to 5mL of HF solution (50 mol%), stirred at 25 ℃ for 4 hours to obtain a suspension, which was then washed with deionized water 2 times and centrifuged to obtain (Ti)0.5,Nb0.5)2C wet deposit. Finally, the process is carried out in a batch,will (Ti)0.5,Nb0.5)2The wet deposit was dried in a vacuum oven at 70 ℃ for 14h to give MXene: (Ti)0.5,Nb0.5)2C。
(2)(Ti0.5,Nb0.5)2Preparation of C quantum dot solution
3g of (Ti)0.5,Nb0.5)2Adding into 10mL of mixed solution of concentrated nitric acid and concentrated sulfuric acid (volume ratio of 1:3), and heating under reflux at 110 deg.C for 10 hr to obtain (Ti)0.5,Nb0.5)2Disperse, dilute with 100mL of deionized water, and cool to 25 ℃ in an ice bath. Subsequently, the obtained product was added to NaOH until the pH reached 7 to obtain (Ti)0.5,Nb0.5)2And C, quantum dot solution.
(3) S-doped (Ti)0.5,Nb0.5)2Preparation of C quantum dots
0.05g of Na2S2O3To 1mL of (Ti)0.5,Nb0.5)2Transferring the C quantum dot solution into a 50mL reaction kettle, heating to 160 ℃, preserving heat for 14h, washing the product for 3 times by using a dialysis membrane (the molecular weight cutoff is 1500Da) after the reaction, and drying to finally obtain S-doped (Ti)0.5,Nb0.5)2And C quantum dots.
(4) Based on S doping (Ti)0.5,Nb0.5)2Preparation of optical film of C quantum dots
0.4g of S was doped (Ti)0.5,Nb0.5)2Adding the C quantum dots into 1mL of water to obtain S-doped (Ti)0.5,Nb0.5)2C quantum dot solution, then uniformly mixing 1mL of the quantum dot solution and 0.8g of polyacrylic acid (PAA) to obtain S-doped (Ti)0.5,Nb0.5)2C quantum dot/PAA composite material. Subsequently, S-doped (Ti)0.5,Nb0.5)2Pouring the C quantum dot/PAA composite material into a culture dish, curing and aging for 3 days at room temperature to obtain S-doped (Ti)0.5,Nb0.5)2C quantum dot/PAA film.
Example 3
(1)MXene：Ta4C3Preparation of
Mixing Ta4AlC3Ball milling into powder by ball milling method for 12 h. Then, the mixture was heated to 1100 ℃ at a rate of 5 ℃/min, calcined at 1100 ℃ for 4 hours under argon atmosphere, and crushed with a mortar and pestle to obtain MXene powder. Then, 8g of MXene powder was added to 5mL of HF solution (50 mol%), stirred at 25 ℃ for 3.5 hours to obtain a suspension, which was then washed 3 times with deionized water and centrifuged to obtain Ta4C3Wet deposit. Finally, Ta4C3Drying the wet sediment in a vacuum oven at 70 ℃ for 14 h; obtaining MXene: ta4C3。
(2)Ta4C3Preparation of Quantum dot solutions
Mixing 5g of Ta4C3The powder was added to a mixed solution of 10mL of concentrated nitric acid and concentrated sulfuric acid (volume ratio: 1:5), and heated under reflux at 90 ℃ for 15 hours to disperse the powder. Then, it was diluted with 100mL of deionized water and cooled to 25 ℃ in an ice bath. Subsequently, the resulting product was added NaOH until the pH reached 7 to obtain Ta4C3A quantum dot solution.
(3) S/N doped Ta4C3Preparation of quantum dots
0.1g of Na2S2O6And 1.4mmol of NH4Cl to 1mL of Ta4C3Transferring the quantum dot solution into a 50mL reaction kettle, heating to 170 ℃, preserving heat for 13h, cleaning the product for 4 times by using a dialysis membrane (the molecular weight cut-off is 2000Da) after the reaction, and drying to finally obtain the N/S doped Ta4C3And (4) quantum dots.
(4) Ta based on S/N doping4C3Preparation of optical thin film of quantum dots
0.4g of S/N was doped with Ta4C3Adding the quantum dots into 1mL of water to obtain N/S doped Ta4C3Quantum dot solution, then 1mL of the quantum dot solution and 0.7g of polyethylene oxide (PEO) were mixed homogeneously to give N/S doped Ta4C3A quantum dot/PEO composite. Then, N/S doped Ta4C3QuantumPouring the point/PEO composite material into a culture dish, curing and aging for 3 days at room temperature to obtain the N/S doped Ta4C3Quantum dot/PEO films.
While the present invention has been described with reference to exemplary embodiments, it is to be understood that the invention is not limited to the disclosed exemplary embodiments. The scope of the claims is to be accorded the broadest interpretation so as to encompass all such modifications and equivalent structures and functions.
Claims (10)
1. A preparation method of doped MXene quantum dots is characterized by comprising the following steps:
providing MXene;
dispersing MXene in a mixed solution of concentrated nitric acid and concentrated sulfuric acid to obtain an MXene quantum dot solution;
and adding a sulfur source and/or a nitrogen source into the MXene quantum dot solution for reaction to prepare the doped MXene quantum dot.
2. The preparation method according to claim 1, wherein the ratio of MXene to the mixed solution is (1-5) g:10mL,
in the mixed solution, the volume of the concentrated nitric acid is less than that of the concentrated sulfuric acid, preferably, the volume ratio of the concentrated nitric acid to the concentrated sulfuric acid is 1 (2-5), and more preferably, the volume ratio of the concentrated nitric acid to the concentrated sulfuric acid is 1: 3.
3. The method according to claim 1, wherein the sulfur source and the nitrogen source are both inorganic substances,
preferably, the sulphur source is selected from one or more of sodium thiosulphate, sulphur powder, sodium sulphide, sodium sulphite and sodium dithionate,
preferably, the nitrogen source is selected from one or more of ammonia, ammonium chloride and ammonium bicarbonate.
4. The preparation method of claim 1, wherein the ratio of MXene quantum dot solution to sulfur source is 1mL (0.05-0.1) g,
the ratio of the MXene quantum dot solution to the nitrogen source is 1mL (0.7-1.4) mmol.
5. The production method according to claim 1, characterized in that, after MXene is dispersed in a mixed solution of concentrated nitric acid and concentrated sulfuric acid, the production method further comprises:
heating, cooling to room temperature, and adjusting the pH value to be neutral to obtain the MXene quantum dot solution, wherein the heating temperature is 90-110 ℃, and the time is 10-15 h.
6. The method according to claim 1, wherein the reaction is carried out at a temperature of 150 to 170 ℃ for 12 to 15 hours.
7. The method according to claim 1, wherein MXene is selected from Ti2C、Ti3C2、(Ti0.5,Nb0.5)2C、(V0.5,Cr0.5)3C2、Nb2C、Ti3CN and Ta4C3One or more of (a).
8. An optical film, comprising a hydrophilic polymer and doped MXene quantum dots dispersed in the hydrophilic polymer,
the doped MXene quantum dot is prepared by the preparation method of any one of claims 1 to 7.
9. An optical film as recited in claim 8, wherein the hydrophilic polymer is selected from one or more of polyvinylpyrrolidone, polyacrylic acid, polyvinyl alcohol, and polyethylene oxide.
10. A QLED comprising a light-emitting layer, characterized in that the light-emitting layer is made of the optical film according to claim 8 or 9.
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