CN114136902A - Fe for enhancing and converting3O4Ultrafast optical nonlinearity method of-GO (graphene oxide) composite magneto-optical film - Google Patents
Fe for enhancing and converting3O4Ultrafast optical nonlinearity method of-GO (graphene oxide) composite magneto-optical film Download PDFInfo
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Abstract
Fe for enhancing and converting3O4An ultrafast optical nonlinearity method of a GO (graphene oxide) -composite magneto-optical film belongs to the technical field of photo-electromagnetic materials, can solve the problems that the existing GO-based material has small optical nonlinearity effect and is not easy to tune, and firstly prepares Fe doped with magnetic particles with different concentrations by using a vacuum filtration method3O4-GO composite films; then, sequentially performing SEM, XRD and ultraviolet visible absorption spectrum characterization on the prepared composite film; finally increasing the magnetic field intensity to Fe with different doping concentrations3O4-testing ultrafast optical nonlinearity of GO composite film. The detection result shows that not only can Fe be effectively enhanced by regulating and controlling the magnetic field intensity and the doping concentration3O4Optics of-GO composite magneto-optical filmsNonlinear effects, and it is found that the optical nonlinear absorption thereof has a transition from saturation to anti-saturation absorption and the optical nonlinear refraction thereof has a transition phenomenon from self-focusing to self-defocusing.
Description
Technical Field
The invention belongs to the technical field of photoelectric magnetic materials, and particularly relates to Fe enhancing and converting3O4-ultrafast optical nonlinearity of GO composite magneto-optical film.
Background
Since the birth of lasers, the nonlinear effect generated by the interaction between strong laser and medium is continuously discovered and searched by researchers, and the nonlinear effect is well applied in various fields, in the last decades, researchers have developed components and applications based on the nonlinear absorption effect by using nonlinear materials, such as saturable absorbers in mode-locked lasers, optical limiting devices in laser protection, and the like, but because the existing material devices have the problems of high manufacturing price, low optical damage threshold, poor heat dissipation, poor laser resistance, and the like, in order to search for new materials with more excellent performance, the method has important practical significance in the aspects of realizing high efficiency, high performance, cost reduction, and the like of the devices.
Graphene Oxide (GO) is a new star in graphene family with its unique physical and chemical properties. The graphene oxide still maintains the layered structure of graphite, except that hydroxyl groups (-OH) and epoxy groups are introduced into graphene sheet layers, and the sheet layer edges contain carboxyl groups (-COOH) and carbonyl groups (-C = O). Despite the sp in the raw graphene after introduction of the oxygen-containing functional group2Carbon atom is changed into sp2And sp3The hybridization of carbon atoms and the destruction of large pi bonds lead to the reduction of mechanical properties and photoelectric properties of GO, but it is precisely these oxygen-containing functional groups that bring opportunities for the surface modification of GO.
So far, the main preparation methods for preparing GO thin films based on GO solutions are vacuum filtration, spin coating, dip coating, electrostatic self-assembly, and the like. Among them, though the GO film obtained from the GO film prepared by the vacuum filtration method is thick (generally in the order of micrometers), the hybrid GO film is easy to operate, low in cost, excellent in performance, and easy to prepare by adding suitable nanoparticles or organic matters into the GO solution, and is more and more favored by researchers and industries.
In order to further expand the wide application of GO-based thin films in optics, electricity, magnetism and mechanics, a single GO thin film is difficult to meet the requirements of high performance and multiple functions, and a functionalized GO hybrid thin film is urgently needed to solve the problem. The chemical functionalization of GO thin films is caused by oxygen-containing groups in GO, which takes full advantage of the superior properties of GO and functionalized materials. A wide variety of multifunctional materials can be attached to the GO thin film, including organic materials, dye ion molecules, dielectrics, metal nanoparticles, and magnetic nanoparticles. Based on the strong coupling effect between GO and the functionalized material, the photoelectric property of the GO-based hybrid film is greatly improved. For example, researchers have prepared gold nanoparticle-doped GO thin films using vacuum filtration, and gold nanoparticle-hybridized GO thin films exhibit several times enhanced optical nonlinear refraction and nonlinear absorption due to the combined action of various nonlinear mechanisms and photoinduced electron transfer mechanisms. In addition, researchers prepare the composite metamaterial with the dielectric thin film and the GO alternating by using an electrostatic self-assembly method, and the GO-based hybrid thin film is controllably reduced by femtosecond micro-nano processing, so that accurate regulation and control of conductivity, energy band gap and dielectric constant are realized. These studies lay the foundation for the development of high-performance optoelectronic integrated devices. Although the GO-based hybrid film functionalized by metal nanoparticles and a dielectric material can effectively improve the photoelectric characteristics of the GO-based hybrid film, the research on the GO-based hybrid film functionalized by magnetic nanoparticles is rarely reported at present, and by combining the magneto-optical performance and the photoelectric performance of the composite materials, the optical nonlinearity is hopefully tuned/improved, the enhanced magneto-optical effect and the enhanced magneto-optical storage density are hopefully realized, and thus, a photo-electromagnetic integrated multifunctional integrated device is developed.
Disclosure of Invention
Aiming at the problems that the optical nonlinear effect of the existing GO-based material is small and difficult to tune, the invention provides Fe enhancement and conversion3O4-ultrafast optical nonlinearity of GO composite magneto-optical film. The preparation method has the advantages of simple process, low cost and mild conditions, and the obtained Fe3O4the-GO composite film has uniform dispersion and smooth surface, and can effectively improve the performanceAnd flexible conversion of Fe3O4The optical nonlinear effect of the GO composite film can be realized, a novel magneto-optical medium which can be used for a saturable absorber and an optical limiting device can be developed, the experimental test light path is simple, the numerical values of the optical nonlinear absorption coefficient and the optical nonlinear refractive index of a sample can be measured, and the sign values of the optical nonlinear absorption coefficient and the optical nonlinear refractive index can be judged.
The invention adopts the following technical scheme:
fe for enhancing and converting3O4-a method for ultrafast optical nonlinearity of GO composite magneto-optical film, comprising the steps of:
(1) fe doped with magnetic particles with different concentrations is prepared by vacuum filtration3O4-GO composite films;
(2) sequentially carrying out SEM, XRD and ultraviolet visible absorption spectrum on the prepared composite film to represent the morphology and structural characteristics of the composite film;
(3) increasing the magnetic field for different doping concentrations of Fe3O4-GO composite films were tested for optical non-linearity.
In the above technical solution, further technical features are as follows:
the method is used for preparing Fe3O4The sheet diameter of Graphene Oxide (GO) dispersion liquid of the-GO composite film is 150nm, the concentration of the Graphene Oxide (GO) dispersion liquid is 2mg/ml, and Fe3O4The magnetic nanoparticle dispersion had a particle size of 150nm and a concentration of 10 mg/ml.
The diameter of the inorganic alumina filter membrane used in the vacuum filtration method is 47mm, and the thickness is 60
The aperture of the filter membrane is 100 nm.
The Fe for preparing the composite film3O4The doping amounts of (A) were 0.01mL, 0.025mL, 0.03mL, and 0.05mL, respectively.
The optimized Z-scanning optical path consists of a femtosecond laser, a half-wave plate, a beam splitter, a focusing lens, an electric displacement platform, a magnetic field device with adjustable size and an optical power meter (an optical power probe I and an optical power probe II), and is arranged along the flyThe second laser is sequentially provided with a half-wave plate, a beam splitter, a focusing lens and an optical power probe II in the pulse light wave direction, and one side of the beam splitter is provided with the optical power probe I and the optical power probe Fe3O4-GO composite film between focusing lens and optical power probe II, Fe3O4-GO composite membranes fixed on motorized displacement stages, Fe3O4The surface of the-GO composite film is perpendicular to the direction of the pulsed light wave, Fe3O4The two sides of the GO composite film are provided with adjustable magnetic field devices. Magnetic field devices are added on two sides of the material, so that the influence of the change of the magnetic field on the optical nonlinearity of the material containing the magnetic material can be tested.
The light source is an ultrafast fiber laser (Fianium, W2031) with a wavelength of 532nm, a repetition frequency of 1MHz, a pulse width of 330fs, and a single pulse energy of 1μJ, average power is about 1W, and emergent light spot is 2 mm.
The focal length of the focusing lens is 150 mm.
The measuring range of the electric displacement platform is 100mm, and the minimum displacement distance is 2.5μm, realizing accurate control by computer software, placing the sample on a motor-driven displacement platform, and moving the sample along the direction from-Z to + Z, wherein the position of Z =0 is coincident with the focal point of the focusing lens. The magnetic field device can be adjusted within the range of 0-4000 Oe, and the influence of the change of a magnetic field on a nonlinear material containing a magnetic material can be tested.
The optical power meter (Newport 2936-R) records optical power values, wherein the reference light enters the optical power probe I to realize real-time monitoring of the output power change of the laser, and the other part of the light finally enters the optical power probe II to realize third-order nonlinear measurement. The power meter has the characteristics of high sampling rate (250kHz), high resolution (0.0004%), high precision (+/-0.2%), wide frequency measurement range (1Hz-250kHz) and the like, and can measure the wavelength of 200nm-1800 nm. The measuring power range of the probe of the optical power meter is 20pW-2W, the photosensitive diameter is 3mm, and the measured maximum energy is 5μJ. Therefore, the power meter can well meet the characteristics of the light source used in the experiment.
The movement of the displacement platform and the recording of the experimental data by the optical power probe can both utilize computer programming to realize automatic operation.
The invention has the following beneficial effects:
aiming at the problems that the existing GO-based material has small optical nonlinear effect and is difficult to tune, the invention provides a method for enhancing and converting Fe3O4-ultrafast optical nonlinearity of GO composite magneto-optical film. The preparation method has the advantages of simple process, low cost and mild conditions, and the obtained Fe3O4the-GO composite film has uniform dispersion and smooth surface, and can effectively improve and flexibly convert Fe3O4The optical nonlinear effect of the GO composite film can be realized, a novel magneto-optical medium which can be used for a saturable absorber and an optical limiting device can be developed, the experimental test light path is simple, the numerical values of the optical nonlinear absorption coefficient and the optical nonlinear refractive index of a sample can be measured, and the sign values of the optical nonlinear absorption coefficient and the optical nonlinear refractive index can be judged.
Drawings
FIG. 1 is GO film and Fe made by the present invention3O4Comparison of SEM images of GO composite films, where (a) is GO film and (b) is Fe3O4-GO composite films.
FIG. 2 is GO film and Fe made by the present invention3O4-comparison of XRD patterns of GO composite films.
FIG. 3 is GO film and Fe made by the present invention3O4-contrast of uv-vis absorption spectrum images of GO composite films.
FIG. 4 is GO film and Fe made by the present invention3O4Comparison of hysteresis loop images of GO composite films.
FIG. 5 is a graph of Fe enhancement and conversion according to the present invention3O4Experimental optical path schematic of the method for optical nonlinear effects of GO composite magneto-optical films, in which: 1-a femtosecond laser; 2-a half-wave plate; 3-a beam splitter; 4-optical power probe I; 5-a focusing lens; 6-Fe3O4-GO composite films; 7-a magnetic field device; 8-optical power probe II.
FIG. 6 is Fe measured using the optical path diagram of the present invention3O4-GO composite films inOpen and closed cell Z-scan curves at different laser energies.
FIG. 7 is Fe measured using the optical path diagram of the present invention3O4Open and closed cell Z-scan curves of GO composite films at different magnetic field strengths.
Detailed Description
In order to clearly explain the technical features of the present invention, the following detailed description of the present invention is provided with reference to the accompanying drawings.
Example 1
Fe for enhancing and converting3O4-a method for ultrafast optical nonlinearity of a GO composite magneto-optical film, said method comprising the steps of:
(1) fe doped with magnetic particles with different concentrations is prepared by vacuum filtration3O4-GO composite magneto-optical films;
（2）Fe3O4the doping amounts of (A) were 0.01mL, 0.025mL, 0.03mL, and 0.05mL, respectively.
Example 2
In this example, Fe was measured by using the optical path diagram of the present invention3O4Z-scan of open and closed cells of GO composite films at different doping concentrations, with the following steps:
(1) firstly, fixing an experimental sample on an electric displacement platform, then turning on a laser, and converting pulse light waves emitted by the femtosecond laser into parallel light after passing through a beam expanding collimation system;
(2) then, the light is divided into two parts by a beam splitter, wherein one part of the light is reflected to enter the optical power probe I as reference light, and the other part of the transmitted light beam enters a focusing lens to be focused and then enters the surface of a sample;
(3) the light beam after penetrating through the sample continuously transmits along the original direction to enter a light power probe II, and the computer is used for programming control of the electric displacement platform and the power meter, so that automatic data recording can be realized, and Z scanning data of the open hole can be obtained;
(4) adding a small aperture diaphragm in front of the optical power probe II to measure Z scanning data of closed pores;
(5) selecting different doping concentrations of Fe3O4And repeating the operation for multiple times to measure the GO composite film, obtaining a curve chart of experimental data through data recorded by two optical power meter probes and the position of the sample in the moving process, and further calculating the third-order optical nonlinear coefficient of the sample according to the Z scanning curves of the open pores and the closed pores.
Example 3
This example is the measurement of Fe using the optical path diagram of the present invention3O4Z-scan of GO composite films at open and closed pores of different magnetic field strength, with the following steps:
(1) fe doped with magnetic particles with different concentrations is prepared by vacuum filtration3O4-GO composite magneto-optical films;
（2）Fe3O4the doping amounts of (A) were 0.01mL, 0.025mL, 0.03mL, and 0.05mL, respectively.
Example 4
In this example, Fe was measured by using the optical path diagram of the present invention3O4Z-scan of open and closed cells of GO composite films at different doping concentrations, with the following steps:
(1) firstly, fixing an experimental sample on an electric displacement platform, then turning on a laser, and converting pulse light waves emitted by the femtosecond laser into parallel light after passing through a beam expanding collimation system;
(2) then, the light is divided into two parts by a beam splitter, wherein one part of the light is reflected to enter the optical power probe I as reference light, the other part of the transmitted light beam enters a focusing lens to be focused and then enters the surface of a sample, and the sample is placed in a magnetic field device with tunable intensity;
(3) the light beam after penetrating through the sample continuously transmits along the original direction to enter a light power probe II, and the computer is used for programming control of the electric displacement platform and the power meter, so that automatic data recording can be realized, and Z scanning data of the open hole can be obtained;
(4) adding a small aperture diaphragm in front of the optical power probe II to measure Z scanning data of closed pores;
(5) selection of Fe of different magnetic field strengths3O4-GO complexAnd repeating the operation for multiple times of measurement on the film, obtaining a curve chart of experimental data through the data recorded by the two optical power meter probes and the position of the sample in the moving process, and further calculating the three-order optical nonlinear coefficient of the sample according to the Z scanning curves of the open pore and the closed pore.
(1) Fe was prepared as in example 13O4-GO composite film was examined by Scanning Electron Microscope (SEM) and the results are shown in figure 1.
As can be seen from FIG. 1, the GO film has a flat surface and no wrinkles, indicating that a uniform film is prepared by using a vacuum filtration method. And in the composite magnetic GO film, Fe3O4The magnetic nanoparticles are clearly present at the surface of the GO thin film, and they are uniformly distributed throughout the Fe3O4No aggregation was observed on the-GO composite films, indicating Fe prepared by vacuum filtration3O4The quality of the-GO composite film is good.
(2) Fe prepared in example 13O4XRD detection is carried out on the-GO composite film, and the result is shown in the attached figure 2.
As can be seen from figure 2, the pure GO film has a GO peak at 10.52 ° and 21.72 ° corresponding to graphite. And Fe3O4Besides the GO peaks corresponding to graphite at 10.45 degrees and 24.63 degrees, the GO composite film has an obvious peak position at about 35.15 degrees, and the peak is a diffraction peak corresponding to iron ions through comparison of XRD standard JCPD cards, thereby further indicating that Fe is successfully prepared3O4-GO composite films.
(3) Fe prepared in example 13O4The detection result of the-GO composite film by ultraviolet visible absorption spectrum is shown in the attached figure 3.
As shown in FIG. 3, GO film is combined with Fe3O4the-GO composite film has better linear absorption characteristics in a visible light wave band, and shows absorption resonance peaks and absorption shoulders around 233nm and 305nm respectively, while Fe in a given wave band3O4The absorption of the-GO composite film is stronger than that of the GO film, and the magnetic nano particles and the GO film are mainly thinCaused by coupling of the film, thus Fe3O4the-GO composite film is expected to realize stronger optical nonlinearity and larger magneto-optical effect.
(4) Fe prepared in example 13O4The hysteresis loop test of the-GO composite film is shown in the attached FIG. 4.
As can be seen from the attached figure 4, the GO film has no hysteresis loop from-4000 Oe to 4000Oe and is almost a straight line passing through the origin and positioned in two quadrants and four quadrants, which shows that the pure GO film has diamagnetism and is insensitive to an applied magnetic field, mainly due to sp2And sp3Hybridization of carbon atoms. And Fe3O4the-GO composite film shows a good hysteresis loop with a saturation magnetization of about 0.00085emu/g and a small coercive force (several tens of Oe), and thus Fe can be demonstrated3O4-GO composite films are characterized by (sub) ferromagnetism.
(5) Fe prepared in example 13O4The data of open-cell and closed-cell Z-scans of the GO composite film at different doping concentrations are fitted and plotted, and the result is shown in FIG. 6.
As can be seen from FIG. 6, pure GO films and Fe with a dopant level of 0.01mL3O4The open-pore Z-scan curve of the GO composite film shows a peak at the position of a focal point, which indicates that the composite film has a saturated absorption effect and is converted into an anti-saturated absorption effect from the saturated absorption effect with the increase of the doping concentration. While pure GO films and Fe with a dopant level of 0.01mL3O4The appearance of a distinct valley-first peak-second curve of the closed cell Z-scan of the GO composite film indicates the presence of a positive nonlinear refraction (self-focusing) effect and the transition from a valley-first peak-second peak self-focusing effect to a peak-first valley self-defocusing effect with increasing doping concentration. And pure Fe3O4The nanoparticles themselves do not exhibit optical nonlinearity and therefore follow Fe3O4The mechanism for increasing the optical nonlinear enhancement of the composite film by the concentration of the nano particles comes from the GO film and the Fe3O4The nanoparticles act together. Fe3O4The nanoparticles can be used asIs a transfer center of energy and electrons and forms an electron donor-acceptor composite structure with the GO thin film, thereby enhancing the transfer of the energy and the electrons and improving the optical nonlinearity of the GO thin film.
(6) Fe prepared in example 13O4The data of open-cell and closed-cell Z-scans of GO composite films at different magnetic field strengths are fitted and plotted, and the results are shown in FIG. 7.
As can be seen from FIG. 7, Fe3O4The open-cell and closed-cell Z-scans of GO composite films exhibit reverse saturation absorption and peak-to-valley self-defocusing effects, respectively, and they exhibit a substantially increasing trend with increasing magnetic field, since the increase in magnetic field allows Fe3O4The disordered and endless magnetic domains of the GO composite film are gradually arranged in an oriented mode, the magnetic moment of the GO composite film is enhanced, and Fe is caused3O4The electron and energy transfer between the magnetic nanoparticles and the GO thin film is enhanced, so that the ultrafast optical nonlinear effect of the GO thin film is enhanced. In addition, Fe3O4Incorporation of magnetic nanoparticles leads to increased reduction of GO films, resulting in sp2/sp3The energy band width of the composite film is increased and reduced, so that the ultrafast optical nonlinearity is improved.
The above-described embodiments should not be construed as limiting the scope of the invention, and any alternative modifications or alterations to the embodiments of the present invention will be apparent to those skilled in the art.
The present invention is not described in detail, but is known to those skilled in the art.
Claims (10)
1. Fe for enhancing and converting3O4-a method for ultrafast optical nonlinearity of a GO composite magneto-optical film, characterized by: the method comprises the following steps:
firstly, preparing Fe doped with magnetic particles with different concentrations by using a vacuum filtration method3O4-GO composite films;
secondly, sequentially carrying out SEM, XRD and ultraviolet visible absorption spectrum on the prepared composite film to represent the morphology and structural characteristics of the composite film;
thirdly, increasing the magnetic field to Fe with different doping concentrations through the optical path device3O4-testing ultrafast optical nonlinearity of GO composite film.
2. An enhancement and conversion of Fe according to claim 13O4-a method for ultrafast optical nonlinearity of a GO composite magneto-optical film, characterized by: for Fe in the first step3O4The sheet diameter of the graphene oxide dispersion liquid of the-GO composite film is 150nm, the concentration of the graphene oxide dispersion liquid is 2mg/ml, and Fe3O4The magnetic nanoparticle dispersion had a particle size of 150nm and a concentration of 10 mg/ml.
3. An enhancement and conversion of Fe according to claim 13O4-a method for ultrafast optical nonlinearity of a GO composite magneto-optical film, characterized by: in the first step, the vacuum filtration method uses an inorganic alumina filter membrane with the diameter of 47mm and the thickness of 60 mm
The aperture of the filter membrane is 100 nm.
4. An enhancement and conversion of Fe according to claim 13O4-a method for ultrafast optical nonlinearity of a GO composite magneto-optical film, characterized by: fe of the prepared composite film3O4The doping amounts of (A) were 0.01mL, 0.025mL, 0.03mL, and 0.05mL, respectively.
5. An enhancement and conversion of Fe according to claim 13O4-a method for ultrafast optical nonlinearity of a GO composite magneto-optical film, characterized by: in the third step, the optical path device comprises a femtosecond laser, a half-wave plate, a beam splitter, a focusing lens and an optical power probe II are sequentially arranged along the pulse optical wave direction of the femtosecond laser, and an optical power probe I and an optical power probe Fe are arranged on one side of the beam splitter3O4-GO composite film located in focusing lens and optical power probe IIM. Fe3O4-GO composite membranes fixed on motorized displacement stages, Fe3O4The surface of the-GO composite film is perpendicular to the direction of the pulsed light wave, Fe3O4The two sides of the GO composite film are provided with adjustable magnetic field devices.
6. An enhancement and conversion of Fe according to claim 53O4-a method for ultrafast optical nonlinearity of a GO composite magneto-optical film, characterized by: the light source of the femtosecond laser is an ultrafast fiber laser, the wavelength is 532nm, the repetition frequency is 1MHz, the pulse width is 330fs, the single-pulse energy is 1 muJ, the average power is 1W, and the size of an emergent light spot is 2 mm.
7. An enhancement and conversion of Fe according to claim 53O4-a method for ultrafast optical nonlinearity of a GO composite magneto-optical film, characterized by: the focal length of the focusing lens is 150 nm.
8. An enhancement and conversion of Fe according to claim 53O4-a method for ultrafast optical nonlinearity of a GO composite magneto-optical film, characterized by: the measuring range of the electric displacement platform is 100mm, the minimum displacement distance is 2.5 mu m, and the electric displacement platform moves along the pulse light wave direction.
9. An enhancement and conversion of Fe according to claim 53O4-a method for ultrafast optical nonlinearity of a GO composite magneto-optical film, characterized by: the measuring power range of the optical power probe I and the optical power probe II is 20pW-2W, the photosensitive diameter is 3mm, and the measured maximum energy is 5 muJ.
10. An enhancement and conversion of Fe according to claim 53O4-a method for ultrafast optical nonlinearity of a GO composite magneto-optical film, characterized by: the adjustable range of the magnetic field device is 0-4000 Oe.
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