CN108862388B - Method for enhancing heterogeneous molecule doping molybdenum disulfide based on electronic dynamic regulation - Google Patents
Method for enhancing heterogeneous molecule doping molybdenum disulfide based on electronic dynamic regulation Download PDFInfo
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Abstract
The invention discloses a method for reinforcing heterogeneous molecule doping molybdenum disulfide based on electronic dynamic regulation and control, and belongs to the field of micro-nano manufacturing. The invention comprises the following steps: the method comprises the following steps: focusing the single-layer or multi-layer molybdenum disulfide on the surface of the substrate through the femtosecond laser pulse sequence, controlling the processing parameters and the processing position of the femtosecond laser pulse sequence, inducing a defect state with controllable degree and position of the molybdenum disulfide surface meeting the preset use requirement, and effectively adsorbing oxygen in the air by the molybdenum disulfide with defect state/active points in an air environment to obtain the single-layer or multi-layer molybdenum disulfide which is doped with oxygen molecules in a P type manner; step two: and dripping single-layer molybdenum disulfide with defect states/active points with organic/inorganic/biomolecule solution capable of realizing N-type doping, and waiting for natural air drying to obtain the single-layer molybdenum disulfide doped with organic/inorganic/biomolecule N-type. The invention has the advantages of controllable defect state degree and position, simple and flexible operation, and the like.
Description
Technical Field
The invention relates to a method for reinforcing heterogeneous molecule doping molybdenum disulfide based on electronic dynamic regulation and control, and belongs to the field of micro-nano manufacturing.
Background
Molybdenum disulfide is a novel graphene-like two-dimensional material, has wide application in the fields of electronics, optoelectronics, sensing, photocatalysis and the like, and has important significance for regulating and controlling intrinsic characteristics such as an energy band structure.
Currently, one effective method of tuning the band structure of molybdenum disulfide is to dope the molybdenum disulfide by atom exchange or charge transfer with a heterogeneous molecule. The method for doping molybdenum disulfide through single atom exchange is mainly to exchange with the same group of atoms of molybdenum and sulfur atoms, and the doping (chemical doping) of molybdenum disulfide through charge transfer can be realized through various heterogeneous molecules. By enhancing the physicochemical adsorption of molybdenum disulfide on heterogeneous molecules, the charge transfer between molybdenum disulfide and heterogeneous molecules can be enhanced. The enhancement of the physicochemical absorption of heterogeneous molecules by molybdenum disulfide can be achieved by inducing defect active sites.
Methods for inducing single or multiple layers of molybdenum disulfide surface defect active sites include chemical vapor deposition, electron beam, plasma beam, continuous laser processing methods: wherein, the defect state degree and position induced by chemical vapor deposition are uncontrollable, and the process is complex; electron beam and plasma beam irradiation requires vacuum systems, masks and complicated procedures, produces thermal effects, and is flexible and cost effective. Femtosecond laser processing is a novel technology in the field of micro-nano manufacturing. The laser processing method is fast, flexible, non-contact, pollution-free and free of harsh conditions, and the femtosecond laser has the advantages of short pulse duration, high pulse peak power, capability of avoiding thermal effect to prevent thermal oxidation of materials, capability of accurately focusing to position processing and the like.
Disclosure of Invention
In order to solve the problems of uncontrollable defect state degree and position, low thermal effect, low flexibility and the like in the process of doping molybdenum disulfide by induced molybdenum disulfide defect state reinforced heterogeneous molecules by the existing method, the invention discloses a method for reinforcing doping molybdenum disulfide by heterogeneous molecules based on electronic dynamic regulation and control, which aims to solve the technical problems that: the method realizes the enhancement of heterogeneous molecule doping molybdenum disulfide based on electronic dynamic regulation and control, and has the advantages of controllable defect state degree and position, simple and flexible operation and the like.
The object of the present invention is achieved by the following technique.
The invention discloses a method for reinforcing heterogeneous molecule doping molybdenum disulfide based on electronic dynamic regulation, which comprises the following steps:
focusing a femtosecond laser pulse sequence on a single-layer or multi-layer molybdenum disulfide arranged on the surface of a substrate, controlling processing parameters and processing positions of the femtosecond laser pulse sequence according to the degree and position of a defect state required in use requirements, and inducing a defect state with controllable degree and position of the molybdenum disulfide surface meeting the preset use requirements, wherein the defect state of the molybdenum disulfide surface comprises a crack and a nanosheet edge, and the defect state is an active point.
The processing parameters comprise laser energy, pulse delay, scanning speed and scanning interval of the femtosecond laser pulse sequence.
The femtosecond laser pulse sequence has the laser energy of 0-0.03 uJ, the pulse delay of 0-10 ps, the scanning speed of 50-1000 um/s and the scanning interval of 0-0.5 um.
Step two, dripping 10-15～10-6M can realize N-type doped organic/inorganic/biomolecule solution, and waits for natural air drying to obtain the organic/inorganic/biomolecule N-type doped single-layer molybdenum disulfide.
Preferably, the concentration of 5ul on the monolayer of molybdenum disulfide droplets having defect states/active sites in step two is 1X 10- 6M/L, i.e. 5X 10-12M in R6G solution, and waiting for natural air drying to obtain a monolayer of molybdenum disulfide doped with R6G molecules in an N type.
The femtosecond laser pulse sequence comprises a femtosecond laser, a femtosecond laser double-pulse generating device, an attenuation sheet group, a continuous gradual change attenuation sheet, a mechanical switch, a dichroic mirror, a focusing objective, a sample to be processed, a precise electric control translation stage, the dichroic mirror, a white light illumination source, a focusing lens, a CCD dynamic imaging unit and a computer. Laser beams emitted by a femtosecond laser enter a femtosecond laser double-pulse generating device, the femtosecond laser pulse sequence is obtained through time domain shaping, the femtosecond laser pulse sequence passes through an attenuation sheet set, the energy is attenuated for the first time, the energy passes through a continuous gradient attenuation sheet, the energy is continuously and gradually attenuated to an energy value meeting the preset use requirement, then the energy is reflected by a dichroic mirror through a mechanical switch, the energy is focused to a sample to be processed on a precise electric control translation table through a focusing objective, illuminating light emitted by a white light source at the top passes through the dichroic mirror, the dichroic mirror and the focusing objective and irradiates the sample to be processed for reflection, the reflected illuminating light returns through the focusing objective and the dichroic mirror, is reflected by the dichroic mirror and reaches a CCD dynamic imaging unit through the focusing lens, a computer is connected with the femtosecond laser, and the femtosecond laser double-pulse generating device is controlled to adjust the length of pulse delay to the duration meeting the preset use requirement, and controlling the mechanical switch to be switched on and off, controlling the precise electric control translation stage to move in the XYZ direction, wherein the movement meets the speed and the position of the preset use requirement, and connecting the precise electric control translation stage with the CCD dynamic imaging unit to monitor the surface of the processed sample.
And controlling the processing parameters and the processing position of the femtosecond laser pulse sequence, namely controlling the energy value, the pulse delay time and the speed and the position of the precise electric control translation stage of the femtosecond laser pulse sequence.
Preferably, the femtosecond laser double-pulse generating device is a femtosecond laser double-pulse generating device based on a michelson interferometer.
Advantageous effects
1. According to the method for enhancing molybdenum disulfide heterogeneous doping based on electronic dynamic regulation, the defect state of a single layer or multiple layers of molybdenum disulfide is controllably induced by using the femtosecond laser pulse sequence, and the physical and chemical adsorption on heterogeneous molecules is enhanced, so that the doping effect of the heterogeneous molecules on a two-dimensional material is enhanced, and the method has the advantages of controllable defect state degree and position, simplicity in operation, flexibility and the like.
2. According to the method for enhancing molybdenum disulfide heterogeneous doping based on electronic dynamic regulation, due to the ultrafast, nonlinear and non-thermal effects of the femtosecond laser pulse sequence, thermal oxidation denaturation of single-layer molybdenum disulfide can not be caused.
3. According to the method for enhancing molybdenum disulfide heterogeneous doping based on electronic dynamic regulation, due to the fact that defect states/active points of molybdenum disulfide are directly induced to enhance physical and chemical adsorption capacity with heterogeneous molecules, external conditions such as pressure injection or heating diffusion are not needed, the method can be suitable for enhancing doping effects of other various organic, inorganic and biological molecules on molybdenum disulfide, and has strong adaptability.
Drawings
FIG. 1 is a flow chart of a method for enhancing molybdenum disulfide heterodoping based on electronic dynamic regulation and control according to the present invention;
FIG. 2 is a schematic diagram of an embodiment of enhancing molybdenum disulfide heterodoping based on electronic dynamic regulation;
FIG. 3 is a schematic diagram of a femtosecond laser pulse sequence processing optical path;
FIG. 4 is a femtosecond laser pulse sequence induced defect state morphology diagram of a molybdenum disulfide surface;
FIG. 5 is a fluorescence spectrum of P-type molybdenum disulfide doped with oxygen molecules in air obtained in example 1;
FIG. 6 is a fluorescence spectrum of P-type molybdenum disulfide doped with oxygen molecules in air obtained in example 2;
FIG. 7 is a fluorescence spectrum of N-type doped molybdenum disulfide with R6G molecules obtained in example 3;
the device comprises a 1-femtosecond laser, a 2-femtosecond laser double-pulse generating device based on a Michelson interferometer, a 3-attenuation sheet group, a 4-continuous gradual attenuation sheet, a 5-mechanical switch, a 6-dichroic mirror, a 7-focusing objective lens, an 8-to-be-processed sample, a 9-six-dimensional precise electric control translation stage, a 10-dichroic mirror, an 11-white light illuminating source, a 12-focusing lens, a 13-CCD dynamic imaging unit and a 14-computer.
Detailed Description
The present invention will be further explained with reference to the drawings and examples (the method flow chart of the embodiment of the present invention is shown in fig. 1, the implementation principle chart is shown in fig. 2, and the processing optical path diagram of the femtosecond laser pulse sequence is shown in fig. 3).
Example 1
The embodiment discloses a method for enhancing molybdenum disulfide heterogeneous doping based on electronic dynamic regulation, which comprises the following specific steps:
(1.1) the femtosecond laser generates femtosecond laser light in a pulse form of a single pulse.
(1.2) the laser beam enters a femtosecond laser double-pulse generating device based on a Michelson interferometer, and a femtosecond laser pulse sequence is obtained through time domain shaping, wherein the energy ratio of two sub-pulses is 1: 1.
And (1.3) focusing the femtosecond laser pulse sequence in the step (1.2) on the upper surface of the sample to be processed through a focusing objective lens to modify the material. The numerical aperture of the focusing objective used here is 0.5.
(1.4) adjusting the energy of the femtosecond laser to 0.01uJ through a neutral density attenuation sheet; controlling a double-pulse generating device by using a computer to adjust the pulse delay to 0.1 ps; the six-dimensional precise electric control translation stage is controlled by a computer to move relative to the focusing position of the laser beam, and the processing speed of the femtosecond laser pulse sequence is adjusted to be 100 um/s.
And (1.5) the defect state of the single-layer molybdenum disulfide surface induced by the femtosecond laser pulse sequence in (1.4), wherein the defect state is an active point, and the appearance of the defect state is shown in FIG. 4.
(1.6) placing the sample in (1.5) in an air environment, wherein the monolayer molybdenum disulfide with the defect state/active point effectively adsorbs oxygen in the air, so that the monolayer molybdenum disulfide doped with oxygen molecules (P type doping) is obtained, the fluorescence spectrogram is shown in fig. 5, and the fluorescence photon energy is increased.
Example 2
The embodiment discloses a method for enhancing molybdenum disulfide heterogeneous doping based on electronic dynamic regulation, which comprises the following specific steps:
(2.1) the femtosecond laser generates femtosecond laser light in a pulse form of a single pulse.
(2.2) the laser beam enters a femtosecond laser double-pulse generating device based on a Michelson interferometer, and a femtosecond laser pulse sequence is obtained through time domain shaping, wherein the energy ratio of two sub-pulses is 1: 1.
And (2.3) focusing the femtosecond laser pulse sequence in the step (2.2) on the upper surface of the sample to be processed through a focusing objective lens to modify the material. The numerical aperture of the focusing objective used here is 0.5.
(2.4) adjusting the energy of the femtosecond laser to 0.01uJ through a neutral density attenuation sheet; controlling a double-pulse generating device by using a computer to adjust the pulse delay to 5 ps; the six-dimensional precise electric control translation stage is controlled by a computer to move relative to the focusing position of the laser beam, and the processing speed of the femtosecond laser pulse sequence is adjusted to be 100 um/s.
And (2.5) the defect state of the single-layer molybdenum disulfide surface induced by the femtosecond laser pulse sequence in (2.4), wherein the defect state is an active point, and the appearance of the defect state is shown in FIG. 4.
(2.6) placing the sample in (2.5) in an air environment, wherein the monolayer molybdenum disulfide with the defect state/active points effectively adsorbs oxygen in the air, so that the monolayer molybdenum disulfide doped with oxygen molecules (P-type doping) is obtained, the fluorescence spectrum of the monolayer molybdenum disulfide is shown in fig. 6, and the fluorescence photon energy of the monolayer molybdenum disulfide is increased.
Example 3
The embodiment discloses a method for enhancing molybdenum disulfide heterogeneous doping based on electronic dynamic regulation, which comprises the following specific steps:
(3.1) the femtosecond laser generates femtosecond laser in a pulse form of a single pulse.
And (3.2) enabling the laser beam to enter a femtosecond laser double-pulse generating device based on a Michelson interferometer, and obtaining a femtosecond laser pulse sequence through time domain shaping, wherein the energy ratio of two sub-pulses is 1: 1.
And (3.3) focusing the femtosecond laser pulse sequence in the step (3.2) on the upper surface of the sample to be processed through a focusing objective lens to modify the material. The numerical aperture of the focusing objective used here was 0.5.
(3.4) adjusting the energy of the femtosecond laser to 0.01uJ through a neutral density attenuation sheet; controlling a double-pulse generating device by using a computer to adjust the pulse delay to 5 ps; the six-dimensional precise electric control translation stage is controlled by a computer to move relative to the focusing position of the laser beam, and the processing speed of the femtosecond laser pulse sequence is adjusted to 200 um/s.
And (3.5) the defect state of the single-layer molybdenum disulfide surface induced by the femtosecond laser pulse sequence in (3.4), wherein the defect state is an active point, and the appearance of the defect state is shown in FIG. 4.
(3.6) 5ul of coating solution was dropped on the surface of the sample in (3.5) to a concentration of 1X 10-6The M/L solution of R6G, the monolayer of molybdenum disulfide with defect state/active point effectively adsorbs R6G molecules, and the monolayer of molybdenum disulfide doped with R6G molecules (N type doping) is obtained, the fluorescence spectrum of which is shown in FIG. 7, and the fluorescence photon energy is reduced.
The doping effect of the substance molecules on the molybdenum disulfide is mainly achieved through charge transfer, and the method can be applied to Surface Enhanced Raman Scattering (SERS) detection of the substance molecules. Surface Enhanced Raman Scattering (SERS) is a useful tool for micro-analysis of organic and biological molecules, and is mainly used for concentration detection of organic and biological molecules. Mechanisms of SERS substrate raman enhancement include electromagnetic field enhancement (mainly metal SERS substrates) and chemical enhancement (mainly occurring in new two-dimensional materials). By applying the femtosecond laser pulse sequence modified molybdenum disulfide with defect states/active points to Raman detection, compared with original molybdenum disulfide grown by chemical vapor deposition, the enhancement factor is improved by 2.5 times.
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 (5)
1. A method for reinforcing heterogeneous molecule doping molybdenum disulfide based on electronic dynamic regulation and control is characterized in that: comprises the following steps of (a) carrying out,
focusing a single-layer or multi-layer molybdenum disulfide arranged on the surface of a substrate through a femtosecond laser pulse sequence, controlling processing parameters and processing positions of the femtosecond laser pulse sequence according to the degree and position of a defect state required in use requirements, and inducing a defect state with controllable degree and position of the molybdenum disulfide surface meeting the preset use requirements, wherein the defect state of the molybdenum disulfide surface comprises a crack and a nanosheet edge, the defect state is an active point, and in an air environment, the molybdenum disulfide with the defect state/active point effectively adsorbs oxygen in the air to obtain the single-layer or multi-layer molybdenum disulfide which is doped with oxygen molecule P type; a concentration of 5ul on a monolayer of molybdenum disulfide droplets having defect states/active sites was 1X 10-6M/L, i.e. 5X 10-12The solution R6G of M is naturally dried to obtain monolayer molybdenum disulfide doped with R6G molecular N type;
step two, dripping 10-15～10-6M organic/inorganic substance/biomolecule solution capable of realizing N-type doping, and waiting for natural air drying to obtain organic/inorganic substance/biomolecule N-type doped single-layer disulfideAnd (4) molybdenum melting.
2. The method for enhancing the doping of the heterogeneous molecule with the molybdenum disulfide as claimed in claim 1 based on electronic dynamic regulation, wherein: the processing parameters comprise laser energy, pulse delay, scanning speed and scanning interval of the femtosecond laser pulse sequence.
3. The method for enhancing the doping of the heterogeneous molecules with the molybdenum disulfide based on the electronic dynamic regulation and control as claimed in claim 2, wherein: the femtosecond laser pulse sequence has the laser energy of 0-0.03 uJ, the pulse delay of 0-10 ps, the scanning speed of 50-1000 um/s and the scanning interval of 0-0.5 um.
4. The method for enhancing heterogeneous molecular doping of molybdenum disulfide based on electronic dynamic regulation as claimed in claim 1, 2 or 3, wherein: the femtosecond laser pulse sequence in the first step comprises a femtosecond laser (1), a femtosecond laser double-pulse generating device (2), an attenuation sheet group (3), a continuous gradual attenuation sheet (4), a mechanical switch (5), a dichroic mirror (6), a focusing objective lens (7), a sample to be processed (8), a precise electric control translation stage 9, a dichroic mirror 10, a white light illumination light source 11, a focusing lens 12, a CCD dynamic imaging unit (13) and a computer (14); laser beams emitted by a femtosecond laser (1) enter a femtosecond laser double-pulse generating device (2), a femtosecond laser pulse sequence is obtained through time domain shaping, the energy of the femtosecond laser pulse sequence is attenuated once through an attenuation sheet set (3) and then passes through a continuous gradient attenuation sheet (4), the energy is continuously and gradually attenuated to an energy value meeting the preset use requirement, then the energy is reflected by a dichroic mirror (6) through a mechanical switch (5), and is focused to a sample (8) to be processed on a precise electric control translation platform (9) through a focusing objective lens (7), illumination light emitted by a white light illumination light source (11) at the top irradiates the sample (8) to be processed through the dichroic mirror (10), the dichroic mirror (6) and the focusing objective lens (7) for reflection, and the reflected illumination light returns through the focusing objective lens (7) and the dichroic mirror (6), the device is reflected by a dichroic mirror (10), reaches a CCD dynamic imaging unit (13) through a focusing lens (12), is connected with a femtosecond laser (1), controls a femtosecond laser double-pulse generating device (2) to adjust the length of pulse delay to the duration meeting the preset use requirement, controls the opening and closing of a mechanical switch (5), controls a precise electric control translation table (9) to move in the XYZ direction, meets the speed and position of the preset use requirement, and is connected with the CCD dynamic imaging unit (13) to monitor the surface of a processed sample.
5. The method for enhancing the doping of the heterogeneous molecule with the molybdenum disulfide as claimed in claim 4, which is based on electronic dynamic regulation and control, and is characterized in that: the femtosecond laser double-pulse generating device (2) is a femtosecond laser double-pulse generating device (2) based on a Michelson interferometer.
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| CN109911848B (en) * | 2019-04-12 | 2019-12-20 | 湖南城市学院 | Device and method for precisely controlling and transmitting nanowires |
| CN110104687B (en) * | 2019-05-30 | 2021-11-16 | 国家纳米科学中心 | Oxygen doping modification method of two-dimensional material |
| CN110787816B (en) * | 2019-11-23 | 2022-06-21 | 台州学院 | Quadruple-modified molybdenum disulfide electrocatalyst and preparation method thereof |
| CN111003724B (en) * | 2019-12-09 | 2022-02-01 | 中科院合肥技术创新工程院 | Method for regulating oxygen defect of cerium dioxide nano material by pulse laser irradiation in liquid phase |
| CN112240942B (en) * | 2020-10-15 | 2024-05-03 | 陕西师范大学 | Method for regulating and controlling charge density and defect number of defect sites on surface of high-orientation pyrolytic graphite |
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