CN112620927B - A method for preparing twinned quantum dots with electric field-assisted femtosecond laser shaping pulses - Google Patents
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- B23K26/062—Shaping the laser beam, e.g. by masks or multi-focusing by direct control of the laser beam
- B23K26/0622—Shaping the laser beam, e.g. by masks or multi-focusing by direct control of the laser beam by shaping pulses
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- B23K26/0643—Shaping the laser beam, e.g. by masks or multi-focusing by means of optical elements, e.g. lenses, mirrors or prisms comprising mirrors
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Abstract
The invention relates to a method for preparing twin crystal quantum dots by electric field assisted femtosecond laser shaping pulses, and belongs to the technical field of femtosecond laser application. The method mainly controls the crystallinity of the quantum dots from two aspects: (1) the intervention of the electric field can quickly guide the directional motion of the cavitation bubbles and the contained nano particles, and can complete the collision of crystal nuclei under higher temperature and pressure, which is the key for forming quantum dots with twin crystal structures. (2) The proportion of coulomb explosion in the ablation process can be controlled by adjusting the femtosecond laser shaping pulse delay, and the concentration of two-dimensional material fragments and atom clusters in the cavitation bubbles is controlled, which is the key for controlling the quantity of twin crystal quantum dots. In addition, the femtosecond laser and the electric field can ionize the solution to generate free oxygen-containing functional groups, so that unsaturated atoms on the edges and the grain boundaries of twin crystal quantum dots can be fully modified, the loading rate of the oxygen-containing functional groups of the quantum dots is improved, and the fluorescence performance of the quantum dots is further improved.
Description
Technical Field
The invention relates to a method for preparing twin crystal quantum dots by field-assisted femtosecond laser shaping pulses, and belongs to the technical field of femtosecond laser application.
Background
Due to the unique quantum effects of quantum dots, great attention has been drawn to biological, optoelectronic and energy-related applications. Two-dimensional material quantum dots have excellent biocompatibility, low cytotoxicity, broad-band light absorption, stable photoluminescence, and photobleaching resistance, and thus have been widely studied in various fields of bio-imaging and light-emitting devices, etc. In order to seek more functional quantum dots and to control the forbidden band width thereof, many attempts have been made in the past in terms of size, hydrophilic oxide group, doping, defects, and the like. The adjustment of the twin crystal structure to the material forbidden band is theoretically calculated by a learner by using simulation means such as DFT and the like: different from defects such as holes and the like, the twin crystal structure can open the band gap without generating local disturbance on the electronic structure, and is an effective means for adjusting the forbidden band of the material. Most of the traditional preparation methods obtain single crystal quantum dots with good crystallinity, the control of the crystal structure state and degree of the quantum dots cannot be realized, and the preparation of twin crystal two-dimensional material quantum dots is not reported at present. According to the classical nucleation theory of the two-dimensional material, the supply of material atoms and the nucleation temperature are adjusted, the regulation and control of the crystallization state of the quantum dots can be realized, the forbidden band structure of the quantum dots is further adjusted, and the improvement and the promotion of the performances in the aspects of electron transmission, photon absorption and emission and the like are realized. Plasma (containing two-dimensional material nano fragments and atom clusters) can be generated on a nanosecond scale in the process of ablating the two-dimensional material nano particle dispersion liquid by femtosecond laser, and micron-sized cavitation bubbles are generated on a microsecond scale, so that a material source and a high-temperature and high-pressure extreme environment are provided for the liquid-phase ablation fragmentation recrystallization process. The regulation and control of laser and environmental parameters in the ablation process is a means for effectively regulating the concentration of atom clusters and the crystallization temperature in the recrystallization process of the two-dimensional material quantum dots, and is an effective way for realizing a new structure of the two-dimensional material quantum dots.
Disclosure of Invention
The invention aims to provide a method for preparing twin crystal quantum dots by electric field assisted femtosecond laser shaping pulses, which introduces a twin crystal structure into quantum dots, further adjusts the forbidden bandwidth of two-dimensional material quantum dots, and realizes the controllable preparation of functional twin crystal quantum dots in a clean, rapid and one-step manner.
The invention realizes the controllable preparation of the single-crystal and twin-crystal two-dimensional material quantum dots by using the method of pulse ablation of the two-dimensional material nanoparticle dispersion liquid by electric field assisted femtosecond laser shaping. The method mainly controls the crystallinity of the quantum dots from two aspects: (1) the intervention of the electric field can quickly guide the directional motion of the cavitation bubbles and the contained nano particles, and can complete the collision of crystal nuclei under higher temperature and pressure, which is the key for forming quantum dots with twin crystal structures. (2) The proportion of coulomb explosion in the ablation process can be controlled by adjusting the femtosecond laser shaping pulse delay, and the concentration of two-dimensional material fragments and atom clusters in the cavitation bubbles is controlled, which is the key for controlling the quantity of twin crystal quantum dots. In addition, the femtosecond laser and the electric field can ionize the solution to generate free oxygen-containing functional groups, so that unsaturated atoms on the edges and the grain boundaries of twin crystal quantum dots can be fully modified, the loading rate of the oxygen-containing functional groups of the quantum dots is improved, and the fluorescence performance of the quantum dots is further improved.
The purpose of the invention is realized by the following technical scheme:
a method for preparing twin crystal quantum dots by electric field assisted femtosecond laser shaping pulse composition comprises ablating dispersion liquid by femtosecond laser with the assistance of an external electric field to obtain twin crystal quantum dots;
the dispersion comprises: two-dimensional material dispersions such as a graphene dispersion and a molybdenum disulfide dispersion;
the femtosecond laser comprises a single pulse and a shaped double pulse; when the femtosecond laser is a shaped double pulse, the first sub-pulse is focused on the nano-sheet in the two-dimensional material dispersion liquid, and hot electrons are accumulated. And when the second sub-pulse arrives (pulse delay is 0-10ps), the recombination of electrons and phonons on the two-dimensional material nano-sheet is not completed, the ionization induction is enhanced, and the coulomb explosion of the nano-sheet is enhanced. The laser shaping pulse can induce and control the coulomb explosion degree, and as coulomb explosion is the main reason of the reduction of the size of the nanometer particles, the adjustment of different time delays of the femtosecond laser shaping pulse can realize the control of the density of the charged atomic cluster particles in the plasma, which is the material basis of the nucleation of the twin crystal quantum dots. This stage occurs within the nanosecond timescale after the femtosecond laser interacts with the slave material.
The electric field is provided by a power supply connected with a platinum electrode (with the voltage of 0-5V). Plasma generated by femtosecond laser liquid phase ablation evolves in two-dimensional material dispersion liquid to form charged cavitation bubbles, a large number of charged atomic cluster particles are gathered in the cavitation bubbles, an external electric field pulls the charged particles to move and accelerate in the cavitation bubbles, so that the charged particles collide into bonds under the environment with higher temperature and high pressure, the cavitation bubbles generated in the laser ablation process and two-dimensional material fragments and atomic clusters contained in the cavitation bubbles and generated by the plasma move directionally, the collision probability of the atomic clusters in the bubbles is increased, and the recrystallization of the two-dimensional material is realized, which is a key condition for forming twin crystal quantum dots. This stage occurs within the microsecond time scale after the femtosecond laser interacts with the slave material.
The specific implementation method comprises the following steps:
placing an electrode in a two-dimensional material dispersion liquid, introducing current, and setting output current (0-5V) to realize stable supply of a direct current electric field;
irradiating the femtosecond laser into the two-dimensional material dispersion liquid; the relative motion of the two-dimensional material nanoparticles and the laser spots in the dispersion can be realized by moving the translation stage on which the dispersion is placed or stirring the dispersion until all the materials are processed by laser;
focusing the femtosecond laser in the two-dimensional material dispersion liquid, adjusting related optical devices, selecting different femtosecond laser shaping pulse delays (0-10ps), and selecting proper energy for processing;
and step four, filtering the processed sample through a cellulose membrane to obtain the two-dimensional material quantum dots in different crystallization states.
The device for realizing the method is a femtosecond laser; a mechanical switch; a half-wave plate; a polarizing plate; an energy attenuation sheet; a first reflector; a second reflector; a beam splitter; a horizontally movable mirror; a third reflector; a fourth mirror; a cylindrical lens; a platinum electrode; a container; a two-dimensional material dispersion; a six degree of freedom translation stage; a computer controller; a digital source table.
Connection relation: the femtosecond laser generates femtosecond laser pulses, the pulses pass through a mechanical switch, a half-wave plate and a polaroid, the energy is adjusted through an energy attenuation plate, the direction of a light path is adjusted through a first reflecting mirror and a second reflecting mirror, the beam splitter is divided into two beams of laser with equal energy and vertical direction, and the beam splitter transmits the laser to the horizontally movable reflecting mirror and returns to the original path; the beam splitter reflected laser and the transmission return laser are combined again through the beam splitter and then reach a third reflector, then a fourth reflector adjusts the direction of a light path, a cylindrical mirror vertically enters two-dimensional material dispersion liquid to be processed, the two-dimensional material dispersion liquid is provided with a stable direct current electric field through platinum electrodes arranged at two ends of a container, direct current is provided by a digital original meter, the two-dimensional material dispersion liquid is arranged on a six-axis moving translation table, a computer controls a mechanical switch, and the six-axis moving platform and the horizontally-movable reflector move linearly; the shaping pulse delay can be adjusted by horizontally moving the mirror position.
Advantageous effects
1. The invention relates to a method for preparing twin crystal quantum dots by electric field assisted femtosecond laser shaping pulses, which utilizes an external electric field to draw charged particles in cavitation bubbles to move and collide into bonds at high temperature and high pressure to obtain the twin crystal quantum dots;
2. the invention relates to a method for preparing twin crystal quantum dots by electric field assisted femtosecond laser shaping pulses, which has the advantages of ultrafast speed, nonlinearity and the like, so that the coulomb explosion degree of a material in a laser liquid phase ablation process can be regulated and controlled, the charged particle concentration in cavitation bubbles is controlled, and the controllable preparation of the twin crystal quantum dots is realized.
Drawings
FIG. 1 is a diagram of a method of practicing the present invention;
FIG. 2 shows the structural morphology of the graphene quantum dots obtained in the comparative example;
fig. 3 is a structural morphology of the graphene quantum dots obtained in example 1;
fig. 4 is a structural morphology of the graphene quantum dots obtained in example 2;
fig. 5 shows the fluorescence lifetime performance test results of the graphene quantum dots obtained in the comparative example, the example 1, and the example 2.
The device comprises a 1-femtosecond laser, a 2-mechanical switch, a 3-half-wave plate, a 4-polarizing plate, a 5-energy attenuation plate, a 6-first reflector, a 7-second reflector, an 8-beam splitter, a 9-horizontally movable reflector, a 10-third reflector, a 11-fourth reflector, a 12-cylindrical lens, a 13-platinum electrode, a 14-container, a 15-two-dimensional material dispersion liquid, a 16-six-degree-of-freedom translation table, a 17-computer controller and an 18-digital source meter.
Detailed Description
The present invention will be further described with reference to the drawings, comparative examples and examples.
Comparative example
The method for controllably preparing twin-crystal graphene quantum dots in the graphene dispersion liquid by one step through femtosecond laser shaping pulse composite external electric field comprises the following specific steps:
(1) the femtosecond laser generates femtosecond laser, and the pulse form is single pulse;
(2) laser instrument light beam gets into the beam splitter, divides into two bundles with a laser, but the position of adjustment horizontal migration's speculum to realize the optical path difference of two bundles of light, two bundles of light return back and close a bundle in beam splitter department, form the dipulse laser of different pulse delays so far, obtain femto second laser plastic pulse through the time domain plastic, the sub-pulse energy ratio is 1: 1;
(3) focusing the femtosecond laser shaping pulse in the step (2) into graphene dispersion liquid to be processed through a cylindrical mirror, and performing laser liquid phase ablation;
(4) controlling the position of the horizontally movable reflector by using a computer, and adjusting the pulse delay to be 0 ps; controlling the voltage of an external electric field by using a digital source meter, and setting the input voltage to be 0V; the relative motion of the graphene dispersion liquid and the laser is realized by utilizing the movement of a six-axis translation table, so that the large-area ablation processing of the graphene dispersion liquid is completed;
(5) and (3) filtering the graphene dispersion liquid ablated in the step (4) through a cellulose membrane, wherein the obtained filtrate is the processed graphene quantum dot, the appearance is shown in figure 2, and the crystallization state is good.
Example 1
The method for controllably preparing twin-crystal graphene quantum dots in the graphene dispersion liquid by one step through femtosecond laser shaping pulse composite external electric field comprises the following specific steps as shown in figure 1:
(1) the step of- (3) is consistent with the comparative example;
(4) controlling the position of the horizontally movable reflector by using a computer, and adjusting the pulse delay to be 0 ps; controlling the voltage of an external electric field by using a digital source meter, and setting the input voltage to be 5V; the relative motion of the graphene dispersion liquid and the laser is realized by utilizing the movement of a six-axis translation table to realize large-area ablation processing;
(5) and (3) filtering the ablated graphene dispersion liquid in the step (4) through a cellulose membrane, wherein the obtained filtrate is the processed graphene quantum dot, the morphology is shown in figure 3, twin crystal structures appear in the quantum dot, and line defects appear.
Example 2
The method for controllably preparing twin-crystal graphene quantum dots in the graphene dispersion liquid by one step through femtosecond laser shaping pulse composite external electric field comprises the following specific steps:
(1) the step of- (3) is consistent with the comparative example;
(4) controlling the position of the horizontally movable reflector by using a computer, and adjusting the pulse delay to be 10 ps; controlling the voltage of an external electric field by using a digital source meter, and setting the input voltage to be 5V; the relative motion of the graphene dispersion liquid and the laser is realized by utilizing the movement of a six-axis translation table to realize large-area ablation processing;
(5) and (3) filtering the ablated graphene dispersion liquid in the step (4) through a cellulose membrane, wherein the obtained filtrate is the processed graphene quantum dots, the appearance is shown in figure 4, the polycrystalline state is more, and the twin crystal quantity is further improved.
By utilizing the experimental method, the characterization of the morphology structure and the fluorescence property of a series of graphene quantum dots prepared by ablating the graphene nanoparticle dispersion liquid is carried out, and the obtained graphene quantum dots with the average particle size of 2-3nm and similar single-layer or double-layer sizes are proved, and twin-crystal graphene quantum dots begin to appear after an electric field is introduced; after the femtosecond laser shaping pulse delay is adjusted and an electric field is added, the number of twin graphene quantum dots and the polyploid number (the polyploid graphene quantum dots can appear at most) of a single quantum dot are obviously increased. The fluorescence performance is also improved along with the increase of the proportion of twin graphene quantum dots, and the fluorescence lifetime is prolonged (as shown in fig. 5).
Compared with the comparative example, in the case of the example 1, the other processing environments are not changed, only the electric field is introduced into the femtosecond laser liquid phase ablation (the voltage intensity is adjusted from 0V to 5V), the directional motion of the cavitation bubbles and the contained nano particles can be rapidly guided, and the collision of crystal nuclei can be completed under higher temperature and pressure, which is the key point for forming the twin-crystal graphene quantum dots.
Compared with the example 1, other processing environments are unchanged, only the shaping femtosecond laser pulse delay interval is adjusted (from 0ps delay to 10ps delay), the proportion of coulomb explosion in the ablation process can be controlled by adjusting the femtosecond laser shaping pulse delay by using the method, and the concentration of small graphene fragments and carbon clusters in the cavitation bubbles is controlled, which is the key for controlling the number of twin-crystal graphene quantum dots.
The above detailed description is intended to illustrate the objects, aspects and advantages of the present invention, and it should be understood that the above detailed description is only exemplary of the present invention and is not intended to limit the scope of the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (6)
1. A method for preparing twin crystal quantum dots by electric field assisted femtosecond laser shaping pulses is characterized in that: the femtosecond laser ablates the dispersion liquid under the assistance of an external electric field to obtain twin crystal quantum dots; the dispersion is a two-dimensional material dispersion; the electric field is a direct current electric field, and the voltage range is more than 0V and less than or equal to 5V.
2. The method of claim 1, wherein: the two-dimensional material dispersion liquid is graphene dispersion liquid or molybdenum disulfide dispersion liquid.
3. The method of claim 1, wherein: the femtosecond laser includes a single pulse or a shaped double pulse.
4. The method of claim 3, wherein: when the femtosecond laser is the shaped double pulse, the time interval between the femtosecond laser shaping pulses is adjusted, the coulomb explosion degree can be induced and controlled, and coulomb explosion is the main reason of reducing the size of the nano particles, so that the control of the charged atom cluster particle density in the plasma can be realized, and the quantity and the structure of twin crystal quantum dots can be further controlled from the substance foundation layer of quantum dot nucleation.
5. The method for preparing twin crystal quantum dots by electric field assisted femtosecond laser shaping pulse as claimed in any one of claims 1 to 4, wherein: the method comprises the following concrete steps:
placing an electrode in a two-dimensional material graphene dispersion liquid, introducing current, setting the output voltage to be more than 0V and less than or equal to 5V, and realizing stable supply of a direct current electric field;
irradiating the femtosecond laser into the two-dimensional material dispersion liquid; the relative motion of two-dimensional material nanoparticles and laser spots in the dispersion liquid is realized by moving a translation platform on which the dispersion liquid is placed or stirring the dispersion liquid until all materials are processed by laser; focusing femtosecond laser in two-dimensional material dispersion liquid, adjusting related optical devices, selecting different femtosecond laser shaping pulse delays for 0-10ps, and selecting proper energy for processing;
and thirdly, filtering the processed sample through a cellulose membrane to obtain the two-dimensional material quantum dots in different crystalline states.
6. Apparatus for implementing the method according to any of claims 1 to 4, characterized in that: the device comprises a femtosecond laser, a mechanical switch, a half-wave plate, a polarizing plate, an energy attenuation plate, a first reflector, a second reflector, a beam splitter, a horizontally movable reflector, a third reflector, a fourth reflector, a cylindrical lens, a platinum electrode, a container, two-dimensional material dispersion liquid, a six-degree-of-freedom translation table, a computer controller and a digital source meter;
the femtosecond laser generates femtosecond laser pulse, and the pulse passes through the mechanical switch, the half-wave plate and the polaroid and then is communicated with the laser
After the energy attenuation sheet adjusts energy, the direction of a light path is adjusted through the first reflector and the second reflector, the light path reaches the beam splitter and is divided into two beams of laser with equal energy and vertical direction, and the beam splitter transmits the laser to the horizontally movable reflector and returns in the original path; the beam splitter reflected laser and the transmission return laser are combined again through the beam splitter and then reach a third reflector, then a fourth reflector adjusts the direction of a light path, the light path is vertically incident into two-dimensional material dispersion liquid to be processed through a cylindrical lens, the two-dimensional material dispersion liquid is provided with a stable direct current electric field through platinum electrodes arranged at two ends of a container, direct current is provided by a digital source meter, the two-dimensional material dispersion liquid is arranged on a six-freedom-degree translation table, and a computer controller controls a mechanical switch, the six-freedom-degree translation table and a horizontally movable reflector to move linearly; the shaping pulse delay can be adjusted by horizontally moving the mirror position.
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