CN110655065B - System for utilize femto second laser pulse sequence reduction oxidation graphite alkene - Google Patents
System for utilize femto second laser pulse sequence reduction oxidation graphite alkene Download PDFInfo
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- 238000001208 nuclear magnetic resonance pulse sequence Methods 0.000 title claims abstract description 52
- 230000009467 reduction Effects 0.000 title claims abstract description 28
- 229910002804 graphite Inorganic materials 0.000 title description 3
- 239000010439 graphite Substances 0.000 title description 3
- 238000007254 oxidation reaction Methods 0.000 title description 3
- -1 graphite alkene Chemical class 0.000 title description 2
- 230000003647 oxidation Effects 0.000 title description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 81
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 77
- 238000000034 method Methods 0.000 claims abstract description 16
- 230000003247 decreasing effect Effects 0.000 claims abstract description 11
- 230000008878 coupling Effects 0.000 claims description 9
- 238000010168 coupling process Methods 0.000 claims description 9
- 238000005859 coupling reaction Methods 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000011946 reduction process Methods 0.000 claims description 3
- 238000006722 reduction reaction Methods 0.000 abstract description 28
- 230000000694 effects Effects 0.000 abstract description 15
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- 230000003287 optical effect Effects 0.000 abstract 1
- 238000002679 ablation Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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- H01—ELECTRIC ELEMENTS
- H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
- H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
- H01S3/005—Optical devices external to the laser cavity, specially adapted for lasers, e.g. for homogenisation of the beam or for manipulating laser pulses, e.g. pulse shaping
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Abstract
The invention relates to a system for reducing graphene oxide by using a femtosecond laser pulse sequence, and belongs to the technical field of femtosecond laser application. According to the system, the time domain waveform of the femtosecond laser is modulated by using the pulse shaper, the modulated laser is transmitted through the optical system, the modulated laser is focused on the surface of graphene oxide by using the lens, the graphene oxide is processed, and the processed area generates a graphene-like structure due to reduction reaction. And adjusting a phase function corresponding to the femtosecond laser time domain waveform by using a pulse shaper, modulating the femtosecond laser time domain waveform into complex waveforms such as an equal-intensity multi-pulse sequence and a multi-pulse sequence with gradually decreased intensity from a single pulse, optimizing the reduction effect of the graphene oxide, and increasing the reduction degree. The method further exerts the advantages of femtosecond laser reduction of graphene oxide, has the advantages of high processing precision, high energy utilization rate and high reduction degree of graphene oxide, and provides a feasible method for preparing the carbon-based micro-nano device based on graphene oxide.
Description
Technical Field
The invention relates to a system for reducing graphene oxide by using a femtosecond laser pulse sequence, and belongs to the technical field of femtosecond laser application.
Background
Graphene is a widely used two-dimensional material, and has excellent mechanical, electrical, chemical and other properties. Graphene can be synthesized by a number of methods, such as chemical methods, mechanical exfoliation methods, deposition methods, and the like. Graphene oxide is a derivative of graphene, and can be prepared by oxidation reaction of graphite, and compared with graphene, graphene oxide has many more oxygen-containing functional groups in the structure, so that the properties of graphene oxide are completely different, for example, graphene is a good conductor, but graphene oxide does not have conductivity. The method for obtaining graphene by reducing graphene oxide by different methods is a stable and efficient way, and common methods include a thermal method, a chemical reduction method and the like. The laser is focused on the surface of the graphene oxide, so that the graphene oxide can be locally heated and reduced to generate a graphene-like structure, and a composite structure of the graphene oxide and the graphene is prepared, and the composite structure can be used for constructing a carbon-based micro-nano device.
The graphene oxide can be reduced by utilizing laser, different types of laser can be used, continuous laser, picosecond laser, femtosecond laser and the like are reported at present, and the femtosecond laser has the characteristics of small heat affected zone and high processing precision and has irreplaceable effect when a micro-nano device is processed. However, the femtosecond laser has a disadvantage that the thermal effect is not obvious, and the reduction of the graphene oxide just needs to use the thermal effect of the laser, so that the femtosecond laser does not have a high degree of reduction of the graphene oxide.
There is a photo-processing method for preparing a conductive micro-nano structure by using graphene oxide (chinese patent, application No. 200910217941.X), in which a femtosecond laser is focused on the surface of graphene oxide to perform reduction, and the reduction degree of graphene oxide can be controlled by adjusting the power of the laser. However, the effect of adjusting the reduction degree by adjusting the power is limited, and graphene oxide is easily ablated and damaged when the power is high, so that the use of the reduced graphene is affected.
Disclosure of Invention
The invention aims to provide a system for reducing graphene oxide by using a femtosecond laser pulse sequence, wherein a pulse shaper is used for adjusting a phase function corresponding to a femtosecond laser pulse, so that the time domain waveform of the femtosecond laser pulse is changed, the action time of a single pulse is prolonged, the energy utilization rate is improved, and the graphene oxide reduction effect with higher efficiency, higher reduction degree and better processed form is realized.
The invention provides a system for reducing graphene oxide by utilizing a femtosecond laser pulse sequence, which comprises a femtosecond laser, an attenuation sheet, a diaphragm, an electric control shutter, a pulse shaper, a reflecting mirror, a dichroic mirror, a focusing objective lens, a translation stage, a convex lens, a charge coupling element and a computer, wherein the attenuation sheet is arranged on the femtosecond laser; the femtosecond laser generated by the femtosecond laser passes through the attenuation sheet to adjust the laser power, passes through the diaphragm to adjust the diameter of a femtosecond laser spot, and then enters the inlet of the pulse shaper through the electric control shutter; the time domain waveform of the femtosecond laser modulated by the pulse shaper is an equal-intensity multi-pulse sequence or a multi-pulse sequence with gradually decreased intensity, the equal-intensity multi-pulse sequence femtosecond laser is emitted from an outlet of the pulse shaper, reflected by one side of the reflecting mirror and the dichroic mirror and focused by the focusing objective lens to reach the surface of the graphene oxide sample, and the graphene oxide sample is reduced; fixing a graphene oxide sample on a translation table; the other side of the dichroic mirror is provided with an observation system consisting of a convex lens and a charge coupling element, and a graphene oxide sample is observed in real time in the graphene oxide reduction process; the femtosecond laser, the electric control shutter, the pulse shaper, the translation stage and the charge coupling element are respectively connected with a computer through signal lines and are controlled by the computer.
In the pulse sequence femtosecond laser system, the time domain waveform modulated by the pulse shaper comprises an equal-intensity multi-pulse sequence and a multi-pulse sequence with decreasing intensity, and the number of the sub-pulses is 2-5.
The system for reducing graphene oxide by using the femtosecond laser pulse sequence has the advantages that:
according to the system for reducing graphene oxide by using the femtosecond laser pulse sequence, the laser time domain shaping method is used, and the phase function of the laser pulse is adjusted by the pulse shaper, so that the modulation of the laser time domain waveform is realized, a single pulse becomes the pulse sequence, and the energy relation of the pulse sequence can be adjusted. The pulse sequence is equivalent to prolonging the action time of each pulse, so that the heat effect is more obvious, the reduction degree of the graphene oxide is improved, the damage of long-time large energy focusing on the graphene oxide is avoided, the energy utilization rate of the graphene oxide can be improved, the processing effect is simultaneously ensured, and the femtosecond laser reduction method has positive significance for reducing the graphene oxide. In the system for reducing the graphene oxide by using the femtosecond laser pulse sequence, the femtosecond laser single pulse is modulated into the multi-pulse sequence by using the pulse shaper, so that the time of the femtosecond laser pulse acting on the graphene oxide can be prolonged, the thermal effect is more obvious, and the reduction degree of the graphene oxide is higher. In the system, the femtosecond laser single pulse is modulated into a multi-pulse sequence, so that the peak power can be reduced on the basis of keeping the total energy unchanged, the graphene oxide is prevented from being ablated due to overhigh energy, and the integrity of a sample is better kept. Therefore, the efficiency of reducing the graphene oxide by the femtosecond laser is improved, the energy utilization rate is improved, and the processing quality of the graphene oxide is improved.
Drawings
Fig. 1 is a schematic diagram of a system for reducing graphene oxide by using a femtosecond laser pulse sequence according to the present invention.
Fig. 2 is a time domain waveform diagram of an equal intensity three-pulse sequence modulated by a pulse shaper in embodiment 1 of the present invention.
Fig. 3 is a time domain waveform diagram of a multi-pulse sequence with decreasing intensity modulated by a pulse shaper in embodiment 3 of the present invention.
In fig. 1, 1 is a femtosecond laser, 2 is an attenuation sheet, 3 is a diaphragm, 4 is an electrically controlled shutter, 5 is a pulse shaper, 6 is a mirror, 7 is a dichroic mirror, 8 is a focusing objective lens, 9 is a graphene oxide sample, 10 is a translation stage, 11 is a convex lens, 12 is a charge-coupled device, and 13 is a computer.
Detailed Description
The structure of the system for reducing graphene oxide by using a femtosecond laser pulse sequence is shown in fig. 1, and the system comprises a femtosecond laser 1, an attenuation sheet 2, a diaphragm 3, an electric control shutter 4, a pulse shaper 5, a reflecting mirror 6, a dichroic mirror 7, a focusing objective 8, a translation stage 10, a convex lens 11, a charge coupling element 12 and a computer 13. The femtosecond laser generated by the femtosecond laser 1 is subjected to laser power adjustment by the attenuation sheet 2 and then to femtosecond laser spot diameter adjustment by the diaphragm 3, and then enters the inlet of the pulse shaper 5 by the electric control shutter 4; the time domain waveform of the femtosecond laser modulated by the pulse shaper 5 is an equal-intensity multi-pulse sequence or a multi-pulse sequence with gradually decreased intensity, the equal-intensity multi-pulse sequence femtosecond laser is emitted from an outlet of the pulse shaper 5, and reaches the surface of the graphene oxide sample 9 through reflection of the reflecting mirror 6 and one side of the dichroic mirror 7 and focusing of the focusing objective 8, so that the graphene oxide sample is reduced. A graphene sample 9 is fixed on a translation stage 10; the other side of the dichroic mirror 7 is provided with an observation system consisting of a convex lens 11 and a charge coupling element 12, and a graphene oxide sample is observed in real time in the graphene oxide reduction process; the femtosecond laser 1, the electric control shutter 4, the pulse shaper 5, the translation stage 10 and the charge coupling element 12 are respectively connected with a computer 13 through signal wires and controlled by the computer.
In the pulse sequence femtosecond laser system, the time domain waveform modulated by the pulse shaper comprises an equal-intensity multi-pulse sequence and a multi-pulse sequence with decreasing intensity, and the number of the sub-pulses is 2-5.
In the embodiment of the invention, the pulse shaper 5 can change the frequency domain phase function of the femtosecond laser pulse, modulate the femtosecond laser pulse into pulse sequences of different forms by reasonably setting the form and parameters of the phase function, and can optimize the effect of reducing the graphene oxide.
In the embodiment of the present invention, the femtosecond laser 1 used is an Astrella type femtosecond laser manufactured by cohenent corporation, and the main parameters thereof are as follows: a center wavelength of 800nm, a repetition frequency of 1000Hz, and an outlet pulse width of 35 fs. The pulse shaper 5 used was manufactured by Biophotonic corporation under the product model MIIPS-HD.
The invention is further described with reference to the following figures and examples.
Example 1
The femtosecond laser 1 is turned on to generate femtosecond laser, the diameter of a light spot is modulated to be 8mm through the diaphragm 2, and the laser power is adjusted to be 200 muW through the attenuation sheet 3. The computer 13 controls the pulse shaper 5 to compress the femtosecond laser pulses to obtain conversion limit pulses, modifies parameters of the pulse sequence by using a multi-pulse generation function of the pulse shaper 5, sets the number of the pulses of the pulse sequence to be 3, the pulse time domain interval to be 500fs, the intensity to be equal, and observes time domain waveforms of the pulses in real time until required pulse waveforms are obtained, wherein the time domain waveforms are shown in fig. 2. Setting the scanning speed of the translation stage 10 to be 2 mu m/s and the interval to be 1 mu m, and opening the electric control shutter 4 to carry out laser scanning reduction on the GO 9. And after scanning, reducing the GO 9 by using single pulse laser to compare the reduction effect of the method. The oxygen content (mass percentage) of the graphene oxide is reduced by about 10% after the single pulse laser reduction, and the sample has a phenomenon of local excessive ablation, while the oxygen content of the graphene oxide is reduced by about 15% after the modulated triple pulse sequence reduction, and the phenomenon of local excessive ablation does not occur, and example 1 proves the feasibility of the method and the effect of improving the reduction degree and the quality of the reduced sample.
Example 2
The computer 13 controls the pulse shaper 5 to compress the pulses to obtain conversion limit pulses, modifies parameters of the pulse sequences by using the multi-pulse generation function of the pulse shaper 5, sets the number of the pulses of the pulse sequences to be 5, the pulse time domain interval to be 500fs and the intensity to be equal intensity, and observes the time domain waveforms of the pulses in real time until the required pulse waveforms are obtained. Setting the scanning speed of the translation stage 10 to be 2 mu m/s and the interval to be 1 mu m, and opening the electric control shutter 4 to carry out laser scanning reduction on the GO 9. After the modulated five-pulse sequence is reduced, the oxygen content of the graphene oxide is only reduced by about 8%, and the phenomenon of local excessive ablation is avoided. Example 2 illustrates that too many pulses of the pulse sequence with equal intensity result in excessively dispersed energy, and the electron excitation effect on the graphene oxide is reduced, which is not beneficial to increasing the reduction degree of the graphene oxide, and the total energy of the pulses needs to be correspondingly increased to further improve the reduction effect.
Example 3
The computer 13 controls the pulse shaper 5 to compress the pulse to obtain the conversion limit pulse, and then selects a phase function in a polynomial form by using the phase function modulation function of the pulse shaper 5, wherein the mathematical form of the phase function is as follows:
wherein,
the phase bias does not affect the waveform of the pulse;
for group delay, this parameter only affects the position of the laser pulse in the time domain and not the waveform;
for group delay dispersion, this parameter controls the linear chirp of the pulse, affecting the pulse width;
this parameter controls the second-order chirp of the pulse, affecting the pulse shape, for third-order dispersion. In setting the phase function of the pulse shaper 5,
the time domain waveform of the pulse is observed in real time, a pulse sequence with decreasing intensity is obtained under the parameter, the number of measurable sub-pulses is 4, and the time domain waveform is shown in figure 3. Setting the scanning speed of the translation stage 10 to be 2 mu m/s and the interval to be 1 mu m, and opening the electric control shutter 4 to carry out laser scanning reduction on the GO 9. After the modulated intensity decreasing pulse sequence is reduced, the oxygen content of the graphene oxide is reduced by about 18%, and the phenomenon of local excessive ablation is avoided. Embodiment 3 illustrates the reduction effect of the intensity decreasing pulse sequence, because the energy of the first sub-pulse is higher, more electrons can be excited in the graphene oxide, and when the electrons are not relaxed, the subsequent sub-pulses can excite the graphene oxide again with lower energy, so that the interaction between the pulse sequence and the graphene oxide is more sufficient, the utilization rate of the energy is further increased, and thus a higher reduction degree is obtained, and meanwhile, because the energy of a single pulse is prevented from being too high, the reduced sample is not subjected to local excessive ablation.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (1)
1. A method for reducing graphene oxide by using a time-domain shaped femtosecond laser pulse sequence is characterized by comprising the following steps:
(1) the method comprises the following steps of establishing a processing system for reducing graphene oxide by using a femtosecond laser pulse sequence, wherein the processing system comprises a femtosecond laser, an attenuation sheet, a diaphragm, an electric control shutter, a pulse shaper, a reflecting mirror, a dichroic mirror, a focusing objective lens, a translation stage, a convex lens, a charge coupling element and a computer; the femtosecond laser generated by the femtosecond laser passes through the attenuation sheet to adjust the laser power, passes through the diaphragm to adjust the diameter of a femtosecond laser spot, and then enters the inlet of the pulse shaper through the electric control shutter; the time domain waveform of the femtosecond laser modulated by the pulse shaper is an equal-intensity multi-pulse sequence or a multi-pulse sequence with gradually decreased intensity, the multi-pulse sequence femtosecond laser is emitted from an outlet of the pulse shaper, reflected by one side of the reflecting mirror and the dichroic mirror and focused by the focusing objective lens to reach the surface of the graphene oxide sample, and the graphene oxide sample is reduced; fixing a graphene oxide sample on a translation table; the other side of the dichroic mirror is provided with an observation system consisting of a convex lens and a charge coupling element, and a graphene oxide sample is observed in real time in the graphene oxide reduction process; the femtosecond laser, the electric control shutter, the pulse shaper, the translation stage and the charge coupling element are respectively connected with a computer through signal lines and controlled by the computer;
(2) opening a femtosecond laser, adjusting the diameter of a laser spot to be 8mm before focusing through the size of a diaphragm, adjusting the laser power to be 200 mu W through an attenuation sheet, and enabling the femtosecond laser to reach the surface of the graphene oxide sample through the focusing of a focusing objective lens;
(3) controlling a pulse shaper to compress femtosecond laser pulses to obtain conversion limit pulses, then setting the number of pulse sequences to generate pulse sequences with equal intensity, or selecting a phase function by utilizing a phase function modulation function to obtain a pulse sequence with gradually decreased intensity;
(4) and (3) placing a translation table at the scanning speed of 2 mu m/s and the interval of 1 mu m, and opening an electric control shutter to perform scanning reduction on the graphene oxide.
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