CN111747412A - Two-dimensional BP/Ti3C2Preparation method and application of heterojunction - Google Patents
Two-dimensional BP/Ti3C2Preparation method and application of heterojunction Download PDFInfo
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- CN111747412A CN111747412A CN202010634547.2A CN202010634547A CN111747412A CN 111747412 A CN111747412 A CN 111747412A CN 202010634547 A CN202010634547 A CN 202010634547A CN 111747412 A CN111747412 A CN 111747412A
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- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/921—Titanium carbide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/003—Phosphorus
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- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The invention discloses a two-dimensional BP/Ti3C2A preparation method of a heterojunction relates to the technical field of two-dimensional materials. The method comprises the following steps: s1, preparing black phosphorus dispersion liquid; s2 preparation of Ti3C2Dispersion liquid: dissolving LiF in hydrochloric acid, adding Ti3AlC2Reacting for 24-36 h at 35-40 ℃, centrifuging and washing after the reaction is finished until the pH value of the solution is neutral, thus obtaining Ti3C2A dispersion liquid; s3, dispersing 0.05-0.1 mg/mL black phosphorus and 0.1-0.2 mg/mL Ti3C2Mixing the dispersion liquid, performing ultrasonic treatment for 30-60 min, and freeze-drying to obtain the two-dimensional BP/Ti3C2A heterojunction.The invention adopts the methods of liquid phase stripping and self-assembly, mixes two-dimensional materials with different concentration ratios, utilizes Van der Waals force to lead the stripped atomic layers to generate random stacking, and synthesizes two-dimensional BP/Ti by the freeze drying technology3C2The heterojunction powder of (1). Prepared two-dimensional BP/Ti3C2The heterojunction has excellent stability in air and water and has good saturable absorption effect.
Description
Technical Field
The invention relates to the technical field of two-dimensional materials, in particular to a two-dimensional BP/Ti3C2Heterogeneous natureA method for preparing a junction and its application are provided.
Background
Since the advent of graphene, research on two-dimensional materials is attracting increasing numbers of researchers, black phosphorus and Ti3C2The two-dimensional material has expected application prospect in various fields such as nonlinear optics, two-dimensional electronic devices, energy storage and the like as two emerging two-dimensional materials. However, from black phosphorus and Ti3C2The resulting two-dimensional nanoplate solutions are very unstable in air and water, limiting their development in numerous fields.
Disclosure of Invention
The technical problem to be solved by the invention is how to improve the black phosphorus and the Ti3C2Stability of heterojunction two-dimensional nanomaterials.
In order to solve the above problems, the present invention proposes the following technical solutions:
two-dimensional BP/Ti3C2A method of fabricating a heterojunction, comprising the steps of:
s1, preparing black phosphorus dispersion liquid;
s2 preparation of Ti3C2Dispersion liquid: dissolving LiF in hydrochloric acid, adding Ti3AlC2Reacting for 24-36 h at 35-40 ℃, centrifuging and washing after the reaction is finished until the pH value of the solution is neutral, thus obtaining Ti3C2A dispersion liquid;
s3, dispersing 0.05-0.1 mg/mL black phosphorus and 0.1-0.2 mg/mL Ti3C2Mixing the dispersion liquid, performing ultrasonic treatment for 30-60 min, and freeze-drying to obtain the two-dimensional BP/Ti3C2A heterojunction.
A further technical scheme is that the step S1 specifically includes:
grinding black phosphorus in a solvent, carrying out ice bath probe type ultrasonic stripping for at least 10h, removing impurities, centrifuging at 8000-12000 rpm, and taking the upper layer liquid, namely the black phosphorus dispersion liquid.
The further technical scheme is that the solvent is isopropanol.
The technical scheme is that in the step S2, the concentration of hydrochloric acid is 6-12 mol/L.
The technical scheme is that in the step S3, the temperature of freeze drying is-30 to-35 ℃, and the drying time is 2-3 days.
The further technical proposal is that the Ti3C2The dispersion being a few layers of Ti3C2A nanosheet solution.
The further technical scheme is that in the step S3, the black phosphorus dispersion liquid and Ti3C2The mixing ratio of the dispersion liquid is 1: 0.8-1.2 by volume.
The further technical scheme is that the three-dimensional size of particles in the black scale dispersion liquid is 300-600 nm.
The invention also provides a two-dimensional BP/Ti3C2Heterojunction of the two-dimensional BP/Ti described above3C2The preparation method of the heterojunction is obtained.
The present invention provides two-dimensional BP/Ti3C2The heterojunction can be applied to the fields of optical communication, lasers, 3D printing, photoelectric sensors and the like.
Compared with the prior art, the invention can achieve the following technical effects:
the invention provides two-dimensional BP/Ti3C2The preparation method of the heterojunction adopts the methods of liquid phase stripping and self-assembly, mixes two-dimensional materials with different concentration ratios, utilizes Van der Waals force to enable the stripped atomic layers to generate random stacking, and synthesizes the two-dimensional BP/Ti by the freeze drying technology3C2The heterojunction powder of (1). Prepared two-dimensional BP/Ti3C2The heterojunction has excellent stability in air and water and has good saturable absorption effect.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 shows two-dimensional BP/Ti obtained in example 1 of the present invention3C2A TEM image of the heterojunction;
FIG. 2 shows two-dimensional BP/Ti obtained in example 1 of the present invention3C2HRTEM images of heterojunctions;
FIG. 3 shows two-dimensional BP/Ti prepared in example 1 of the present invention at different times3C2Ultraviolet-visible absorption spectrum of the heterojunction;
FIG. 4 shows two-dimensional BP/Ti obtained in example 1 of the present invention3C2The saturation absorption characteristics of the heterojunction under different intensities of 1550nm ultrafast pulsed laser;
fig. 5 is a saturated absorption curve of fig. 4.
Detailed Description
The technical solutions in the embodiments will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, wherein like reference numerals represent like elements in the drawings. It is apparent that the embodiments to be described below are only a part of the embodiments of the present invention, and not all of them. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It will be understood that the terms "comprises" and/or "comprising," when used in this specification and the appended claims, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
It is also to be understood that the terminology used in the description of the embodiments of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the embodiments of the invention. As used in the description of embodiments of the present invention and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
The embodiment of the invention provides a two-dimensional BP/Ti3C2A method of fabricating a heterojunction, comprising the steps of:
s1, preparing a black scale dispersion liquid:
weighing 0.1-0.2 g of block black phosphorus (the purity is more than 99.9%), adding a solvent, grinding, preventing black phosphorus from being oxidized in a low-temperature environment, performing ultrasonic treatment for more than 10 hours by using a probe, and obtaining a black phosphorus dispersion liquid at a centrifugal speed of 8000-12000 rpm;
s2 preparation of Ti3C2Dispersion liquid:
dissolving LiF in hydrochloric acid, adding Ti3AlC2Reacting for 24-36 h at 35-40 ℃, centrifuging and washing for 5-7 times after the reaction is finished until the pH value of the solution is neutral, and obtaining Ti3C2A dispersion liquid;
s3, dispersing 0.05-0.1 mg/mL black phosphorus and 0.1-0.2 mg/mL Ti3C2Mixing the dispersion liquid according to a certain proportion, carrying out ultrasonic treatment for 30-60 min, and freeze-drying to obtain the two-dimensional BP/Ti3C2A heterojunction.
Wherein the concentration of the hydrochloric acid is 6-12 mol/L.
In this example, hydrofluoric acid was obtained by reacting hydrochloric acid with lithium fluoride, and then hydrofluoric acid was reacted with Ti3AlC2Mild method of preparing low-layer Ti3C2. By adopting a liquid phase stripping and self-assembly method, two-dimensional materials with different concentration ratios are mixed, van der Waals force is utilized, the stripped atomic layers are randomly stacked, and then two-dimensional BP/Ti is synthesized by a freeze drying technology3C2The heterojunction powder of (1).
Example 1
Example 1 of the present invention provides a two-dimensional BP/Ti3C2A heterojunction and a method for making the same comprising the steps of:
few layer of Ti3C2Preparation of the dispersion: firstly, 10mL of hydrochloric acid with the concentration of 9M is added into a centrifuge tube, then 0.5g of lithium fluoride powder with the purity of 99.9% is slowly added, and the whole process lasts for about 10 minutes, so that lithium fluoride is fully dissolved and hydrofluoric acid is generated; into the centrifugal tube0.5g of Ti with a purity of 99.9% was added3AlC2Powder, slowly added to prevent the reaction from being vigorous. Finally, the centrifuge tube was sealed and left with a vent and stirred in a thermostatic water bath at 40 ℃ for about 24 hours. After the reaction is finished, deionized water is added for centrifugation for 5min at 3500rmp, and washing is repeated for 7 times until neutral Ti is obtained3C2And (3) solution. Putting the solution in a water bath ultrasonic machine with the power of 1000W for ultrasonic treatment for 1h, then centrifuging for 1h at 8000rmp to obtain a black solution, layering the solution by hand shaking, and taking out the upper dark green liquid, namely the few-layer Ti3C2A nanosheet solution.
Preparation of black phosphorus dispersion: putting 0.1g of block black phosphorus in an agate mortar, adding isopropanol, grinding for 1h, putting in a probe ultrasonic machine, and ultrasonically treating for about 10h, wherein an ice bag is used for keeping a low-temperature environment in the process to prevent the black phosphorus from being oxidized; and centrifuging at 3000rmp for 30min to remove impurities, centrifuging at 8000rmp, and collecting the upper layer of yellowish liquid as the black phosphorus dispersion.
BP/Ti3C2And (3) synthesis of heterojunction: mixing Ti3C2Mixing the dispersion (0.2mg/mL) and BP dispersion (0.1mg/mL) at a ratio of 1:1, performing ultrasonic treatment for 30min, drying in a freeze dryer for 72h (-35 deg.C) to obtain powder sample which is two-dimensional BP/Ti3C2A heterojunction.
And (3) performance testing:
(1) two-dimensional BP/Ti obtained in example 13C2The microstructure of the heterojunction is observed by a transmission electron microscope, wherein pictures of a common Transmission Electron Microscope (TEM) and a high-resolution transmission electron microscope (HRTEM) are shown in fig. 1 and fig. 2.
As shown in FIGS. 1 and 2, TEM and HRTEM tests prove that the BP nano material and Ti are combined3C2The nanosheets being stacked together by van der Waals forces to form a two-dimensional BP/Ti3C2Heterojunction, two-dimensional BP/Ti obtained3C2The heterojunction size is about 2um, and the lattice spacings 0.27nm and 0.14nm are respectively assigned to BP (040) and Ti3C2(110) Of (c) is performed.
(2) To, forTwo-dimensional BP/Ti obtained in example 13C2Performing ultraviolet-visible light absorption spectrum test on the heterojunction to obtain two-dimensional BP/Ti3C2The stability of the heterojunction in air and water environments was investigated, as shown in FIG. 3, two-dimensional BP/Ti3C2The heterojunction is exposed in air and water for 0-60h, and all absorption spectra have no obvious change, which indicates that the two-dimensional BP/Ti3C2The heterojunction has excellent environmental stability.
(3) Two-dimensional BP/Ti prepared in example 1 by Z-scan technique3C2The nonlinear optical properties of the heterojunction were studied, and absorption tests were performed at different intensities of 1550nm ultrafast pulsed laser, and the results are shown in FIG. 4, where two-dimensional BP/Ti was observed with the intensity of the mid-infrared incident light from 142nJ to 360nJ3C2The normalized transmission of the heterojunction gradually increased, indicating that two-dimensional BP/Ti3C2The heterojunction has strong nonlinear saturation absorption effect, and the characteristic is very important for Q-switching and mode-locked pulse lasers. The Z-scan curve is fitted by equations (1) and (2) as shown in fig. 5.
Two-dimensional BP/Ti3C2The absorption coefficient of the heterojunction is as in formula (1):
α=α0+αNL(1);
wherein, α0=ln(TLN) L and αNLβ I is an absorbing and non-absorbing fraction, TLNIs the linear transmittance, L is the measured thickness of the sample, β is the nonlinear absorption coefficient, and I is the incident light intensity.
The Z-scan curve can be fitted by the following equation (2):
wherein β is the nonlinear absorption coefficient, I0Is the intensity at which z is 0,is an effective measurement of the thickness of the sample, Z isLength of interaction of incident light intensity with sample medium, Z0Is the rayleigh length.
Further, the transmittance T has the following relationship with the incident light intensity I:
where I is the incident light intensity, Δ R is the modulation depth, IsatIs the saturation intensity, AnsIs an unsaturated loss.
Thus, the two-dimensional BP/Ti of example 1 can be calculated3C2β, Δ R, and I of the heterojunction in the mid-infrared bandsatRespectively are-0.269 cm/GW, 58.2% and 1.13GW/cm2Other two-dimensional materials such as BP have a Δ R of 12.4%, SnS has a Δ R of 12.5%, GeP has a Δ R of 21.94%. As can be seen, the two-dimensional BP/Ti prepared in example 1 of the present invention3C2Heterojunctions have a higher modulation depth at the same thickness than other two-dimensional materials. For a saturable absorber, a higher modulation depth value has a stronger modulation capability on the optical pulse.
In addition, the two-dimensional BP/Ti prepared in example 1 of the present invention3C2The lower saturation intensity of the heterojunction is more favorable for establishing a pulse laser, and the requirement on the light intensity in the cavity is relatively lower. The pronounced Saturable Absorption (SA) characteristics of these mid-infrared bands imply that the two-dimensional BP/Ti prepared according to example 1 of the present invention3C2Heterojunctions can potentially be applied to SA-based generated pulsed lasers.
In conclusion, the two-dimensional BP/Ti prepared by the method provided by the invention3C2The heterojunction has better stability in air and water, has good saturable absorption effect, and greatly expands two-dimensional BP/Ti3C2The use of (1).
In the above embodiments, the descriptions of the respective embodiments have respective emphasis, and for parts that are not described in detail in a certain embodiment, reference may be made to related descriptions of other embodiments.
While the invention has been described with reference to specific embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. Two-dimensional BP/Ti3C2The preparation method of the heterojunction is characterized by comprising the following steps:
s1, preparing black phosphorus dispersion liquid;
s2 preparation of Ti3C2Dispersion liquid: dissolving LiF in hydrochloric acid, adding Ti3AlC2Reacting for 24-36 h at 35-40 ℃, centrifuging and washing after the reaction is finished until the pH value of the solution is neutral, thus obtaining Ti3C2A dispersion liquid;
s3, dispersing 0.05-0.1 mg/mL black phosphorus and 0.1-0.2 mg/mL Ti3C2Mixing the dispersion liquid, performing ultrasonic treatment for 30-60 min, and freeze-drying to obtain the two-dimensional BP/Ti3C2A heterojunction.
2. The two-dimensional BP/Ti of claim 13C2The method for preparing a heterojunction is characterized in that the step S1 specifically includes:
grinding black phosphorus in a solvent, carrying out ice bath probe type ultrasonic stripping for at least 10h, removing impurities, centrifuging at 8000-12000 rpm, and taking the upper layer liquid, namely the black phosphorus dispersion liquid.
3. The two-dimensional BP/Ti of claim 23C2The preparation method of the heterojunction is characterized in that the solvent is isopropanol.
4. The two-dimensional BP/Ti of claim 13C2The preparation method of the heterojunction is characterized in that in the step S2, the concentration of hydrochloric acid is 6-12 mol/L.
5. The two-dimensional BP/Ti of claim 13C2The preparation method of the heterojunction is characterized in that in the step S3, the freeze drying temperature is-30 to-35 ℃, and the drying time is 2 to 3 days.
6. The two-dimensional BP/Ti of claim 13C2A method for preparing a heterojunction, characterized in that said Ti is3C2The dispersion being a few layers of Ti3C2A nanosheet solution.
7. The two-dimensional BP/Ti of claim 13C2The method for preparing a heterojunction is characterized in that in the step S3, the black phosphorus dispersion liquid and Ti3C2The mixing ratio of the dispersion liquid is 1: 0.8-1.2 by volume.
8. The two-dimensional BP/Ti of claim 13C2The preparation method of the heterojunction is characterized in that the three-dimensional size of particles in the black phosphorus dispersion liquid is 300-600 nm.
9. Two-dimensional BP/Ti3C2Heterojunction characterized by the two-dimensional BP/Ti according to any of claims 1 to 83C2The preparation method of the heterojunction is obtained.
10. The two-dimensional BP/Ti of claim 93C2The heterojunction is applied to the preparation of lasers, photoelectric sensors and 3D ink-jet printing equipment.
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CN115084470A (en) * | 2022-07-01 | 2022-09-20 | 湘潭大学 | C 3 N/MoS 2 Van der Waals heterojunction composite material and preparation method and application thereof |
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Cited By (3)
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CN115084470A (en) * | 2022-07-01 | 2022-09-20 | 湘潭大学 | C 3 N/MoS 2 Van der Waals heterojunction composite material and preparation method and application thereof |
CN117594364A (en) * | 2024-01-18 | 2024-02-23 | 河南师范大学 | Preparation method and application of mechanical property enhanced black phosphazene/MXene piezoelectricity composite membrane electrode |
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