CN113777856B - Method for regulating nonlinear absorption performance of Prussian blue film and Prussian blue film - Google Patents
Method for regulating nonlinear absorption performance of Prussian blue film and Prussian blue film Download PDFInfo
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- CN113777856B CN113777856B CN202110973013.7A CN202110973013A CN113777856B CN 113777856 B CN113777856 B CN 113777856B CN 202110973013 A CN202110973013 A CN 202110973013A CN 113777856 B CN113777856 B CN 113777856B
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/35—Non-linear optics
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/35—Non-linear optics
- G02F1/355—Non-linear optics characterised by the materials used
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention relates to a method for regulating and controlling nonlinear absorption performance of a Prussian blue film and the Prussian blue film. Compared with the prior art, the invention effectively controls the mixed valence state of the Prussian blue film by adjusting the external voltage, so that the adjustment of the proportion of the high spin state quantity to the low spin quantity has high controllability and reversibility. Different spin state quantity ratios lead to different energy level structures so as to influence the optical performance of the material, and further realize the regulation and control of the nonlinear absorption performance of the Prussian blue film.
Description
Technical Field
The invention belongs to the technical field of nonlinear optics, and relates to a method for regulating and controlling nonlinear absorption performance of a Prussian blue film and the Prussian blue film.
Background
Nonlinear optical materials have received attention for their potential use in optical switching, optical confinement, logic devices, ultra-fast optical communications, data storage, optical computing, image transmission, and mode-locked laser systems. In addition to developing materials that exhibit large nonlinear performance sensitivity, it is also important to develop performance-tunable nonlinear performance materials because dynamic control of optical nonlinearities by external modulation (e.g., electrical modulation) has a range of applications (optical modulation and optical switching).
Meanwhile, the mixed valence transition metal compound has been widely used in the fields of catalysis, superconductivity, photoresponse, electrochromic, battery electrodes and the like. The magnetic properties of these materials are closely related to their electronic state, which is directly linked to the nature of the mixed valence. Prussian blue is a typical mixed valence semiconductor and has been widely used in the fields of pigments and electrochromic smart windows. In addition, prussian blue analogues have broad prospects as active materials for next-generation battery electrodes, showing improved cycle life and rate performance. However, in the prior art, researches on the nonlinear performance of prussian blue are few, and the nonlinear performance of prussian blue at different valence states has not been explored yet.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for regulating and controlling the nonlinear absorption performance of a Prussian blue film and the Prussian blue film. The invention regulates and controls the nonlinear optical performance of the Prussian blue film by regulating the mixing valence proportion through an electrochemical oxidation-reduction method with high controllability and reversibility. The electrochemical regulation nano material is a new regulation method, and provides a new example for constructing a nonlinear material modulated by an electrochemical method. Meanwhile, the method has the advantages of simple process flow, easy operation, high controllability and reversibility, universality and the like, and can be used as an ideal method for regulating and controlling the nonlinear performance of the nano material.
The aim of the invention can be achieved by the following technical scheme:
the first aspect of the invention provides a method for regulating and controlling nonlinear absorption performance of a Prussian blue film, which realizes the regulation and control of nonlinear optical performance of the Prussian blue film by carrying out in-situ electrochemical oxidation reduction on the Prussian blue film.
Preferably, the method is to apply different electrochemical external voltages to the Prussian blue film in an electrolyte containing an electrochemical charge compensation electrolyte by adopting a three-electrode system, so that the Fe element (the chemical valence state is bivalent and trivalent) in the Prussian blue film is subjected to reversible stable oxidation or reduction reaction, and particularly, the oxidation reaction refers to conversion of ferrous iron into ferric iron, and the reduction reaction refers to conversion of ferric iron into ferrous iron. Thereby adjusting the conversion of ferric iron and ferrous iron of the Prussian blue film to realize different mixing valence ratios. The change of the mixing valence proportion causes the energy level structure of the Prussian blue film to change, and the absorption in nonlinear optics is closely related to the energy level structure of the material. Thereby realizing the regulation and control of the nonlinear optical performance of the Prussian blue film.
Preferably, the electrochemical charge compensation electrolyte is a salt of an alkali metal, the alkali metal including Li, na or K, and the salt is a nitrate, sulfate or chloride salt. That is, in the present invention, the electrochemical charge compensation electrolyte may be a salt solution (nitrate, sulfate, chloride) of general alkali metals (Li, na, K).
Preferably, the concentration of the electrochemical charge compensation electrolyte in the electrolyte is 0.01-1mol/L. It is further preferable that the concentration of the electrochemical charge compensation electrolyte in the electrolyte solution is 0.1mol/L.
Preferably, the pH of the electrolyte is 2-3. Further preferably, the pH of the electrolyte is 2.5.
Preferably, the electrolyte containing the electrochemical charge compensation electrolyte is an aqueous solution of the electrochemical charge compensation electrolyte.
Preferably, in the three-electrode system, the counter electrode is a platinum sheet, and the reference electrode is an Ag/AgCl electrode.
Preferably, the electrochemical external voltage is not less than-0.2V and not more than 1.4V relative to the Ag/AgCl electrode.
Preferably, the Prussian blue film is synthesized by an electrochemical deposition method.
The invention also provides a Prussian blue film with adjustable nonlinear absorption performance, which is obtained by adopting the method.
The invention effectively controls the mixed valence state of the Prussian blue film by adjusting the external voltage, so that the adjustment of the proportion of the high spin state quantity to the low spin quantity has high controllability and reversibility. Different spin state quantity ratios lead to different energy level structures so as to influence the optical performance of the material, and further realize the regulation and control of the nonlinear absorption performance of the Prussian blue film.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the invention, the mutual conversion of ferric iron and ferrous iron is controlled through electrochemical oxidation reduction, so that the change of the mixing valence proportion of materials is realized, the regulation and control of Prussian blue energy level is realized, and the nonlinear optical performance of the Prussian blue film is regulated and controlled.
(2) The material adopted by the invention has excellent stability in weak acid solution and atmospheric environment, and the cyclic voltammogram shows that after 1000 circles of circulation, no obvious weakening or distortion of peak shape occurs.
(3) The invention has simple process flow, simple operation and low cost, and is expected to be produced in large quantities.
In a word, the change of the mixing valence proportion is controllably and reversibly realized by controlling the interconversion of ferric iron and ferrous iron through electrochemical oxidation-reduction, and the regulation and control of the Prussian blue energy level are realized, so that the nonlinear optical performance of the Prussian blue film is regulated and controlled.
Drawings
Fig. 1 is an X-ray spectroscopy (EDS) image of a prussian blue film without any voltage applied.
Fig. 2 is a raman spectrum image of a prussian blue film to which no voltage is applied.
Fig. 3 is an ultraviolet-visible photoelectron spectroscopy (UV-Vis) image, wherein fig. 3 (b 1) is an absorption change curve during film reduction, fig. 3 (b 2) is an absorption change curve during film oxidation, and fig. 3 (b 3) is an absorption peak position change magnification curve at some voltages.
FIG. 4 is a summary of Z-scan and fitted curves of Prussian blue under different external voltage conditions, in order of-0.2V, 0.3V, 0.4V, 0.5V, 0.6V, 0.8V, 1.1V, 1.4V.
FIG. 5 shows cyclic voltammograms of Prussian blue films, with voltages ranging from-0.2V to 1.4V, reference electrode being an Ag/AgCl electrode and counter electrode being a platinum sheet.
Detailed Description
A method for regulating and controlling nonlinear absorption performance of Prussian blue film realizes the regulation and control of nonlinear optical performance of Prussian blue film by carrying out in-situ electrochemical oxidation reduction on Prussian blue film.
According to the method, a three-electrode system is adopted, and different electrochemical external voltages are applied to the Prussian blue film in electrolyte containing electrochemical charge compensation electrolyte, so that reversible and stable oxidation or reduction reaction occurs to Fe element (the chemical valence state is bivalent and trivalent) in the Prussian blue film, and particularly, the oxidation reaction refers to conversion of ferrous iron into ferric iron, and the reduction reaction refers to conversion of ferric iron into ferrous iron. Thereby adjusting the conversion of ferric iron and ferrous iron of the Prussian blue film to realize different mixing valence ratios. The change of the mixing valence proportion causes the energy level structure of the Prussian blue film to change, and the absorption in nonlinear optics is closely related to the energy level structure of the material. Thereby realizing the regulation and control of the nonlinear optical performance of the Prussian blue film.
In the present invention, the electrochemical charge compensation electrolyte is preferably a salt of an alkali metal, more preferably the alkali metal includes Li, na or K, and still more preferably the salt is a nitrate, sulfate or chloride salt. That is, in the present invention, the electrochemical charge compensation electrolyte is preferably a salt solution (nitrate, sulfate, chloride) of general alkali metals (Li, na, K). In the present invention, the concentration of the electrochemical charge compensation electrolyte in the electrolyte is preferably 0.01 to 1mol/L. It is further preferable that the concentration of the electrochemical charge compensation electrolyte in the electrolyte solution is 0.1mol/L. In the present invention, the electrolyte preferably has a pH of 2 to 3. Further preferably, the pH of the electrolyte is 2.5. It is further preferred that the electrolyte containing the electrochemical charge compensation electrolyte is an aqueous solution of the electrochemical charge compensation electrolyte.
In the invention, in a three-electrode system, the counter electrode is a platinum sheet, and the reference electrode is an Ag/AgCl electrode. Preferably, the electrochemical external voltage is not less than-0.2V and not more than 1.4V relative to the Ag/AgCl electrode.
In the invention, the Prussian blue film is preferably synthesized by an electrochemical deposition method.
Prussian blue film with adjustable nonlinear absorption performance obtained by the method.
The invention will now be described in detail with reference to the drawings and specific examples. The present embodiment is implemented on the premise of the technical scheme of the present invention, and a detailed implementation manner and a specific operation process are given, but the protection scope of the present invention is not limited to the following examples.
In the following examples, prussian blue films were synthesized by electrochemical deposition. In general, K is 3 [Fe(CN) 6 ](10mM)、FeCl 3 6H2O (10 mM) and KCl (50 mM) were dissolved in deionized water at room temperature. The Pt sheet and the saturated Ag/AgCl electrode are used as an auxiliary electrode and a reference electrode respectively, and the pretreated FTO is used as a working electrode. Deposition occurs at about 3cm of the working electrode surface 2 Is within the rectangular area of (c). Electrochemical workstations (CHI 760, CH Instruments) are used for performing constant current deposition. Prussian blue filmThe deposition was carried out at a current density of-25. Mu.A/cm 2 for a deposition time of 240s. After that, the film was subjected to ultrasonic treatment in water for 10 minutes, and then dried at 60 ℃. The electrochemical redox process was performed using the CHI760E electrochemical workstation, shanghai Chen Hua instruments Co., ltd.) using the i-t Amperemetric i-t Curve program.
Example 1
Prussian blue film was synthesized by electrochemical deposition. The FTO substrate loaded with the prussian blue film is used as a working electrode, and 0.1M KCl electrolyte (diluted hydrochloric acid is added dropwise to adjust the pH to 2.5) is injected into the quartz electrolytic cell. One platinum wire and an Ag/AgCl electrode are inserted into the electrolyte and respectively used as a counter electrode and a reference electrode, and the redox process is realized by charging for 1min under the voltage of 0.6V. A nonlinear response test was performed on it at a single beam nonlinear transmittance setting.
Results of single beam nonlinear transmittance evaluation of Prussian blue nonlinear response in an open aperture Z scanning system (Z-scan) show that the nonlinear absorption coefficient beta of Prussian blue 0 ＝-95.38cm GW -1 。
Example 2
Prussian blue film was synthesized by electrochemical deposition. The FTO substrate loaded with the prussian blue film is used as a working electrode, and 0.1M KCl electrolyte (diluted hydrochloric acid is added dropwise to adjust the pH to 2.5) is injected into the quartz electrolytic cell. A platinum wire and an Ag/AgCl electrode are inserted into the electrolyte and respectively used as a counter electrode and a reference electrode, and the redox process is realized by charging for 1min under the voltage of 0.3V. A nonlinear response test was performed on it at a single beam nonlinear transmittance setting.
Results of single beam nonlinear transmittance evaluation of Prussian blue nonlinear response in an open aperture Z scanning system (Z-scan) show that the nonlinear absorption coefficient beta of Prussian blue 0 ＝-112.93cm GW -1 。
Example 3
Prussian blue film was synthesized by electrochemical deposition. The FTO substrate loaded with the prussian blue film is used as a working electrode, and 0.1M KCl electrolyte (diluted hydrochloric acid is added dropwise to adjust the pH to 2.5) is injected into the quartz electrolytic cell. One platinum wire and an Ag/AgCl electrode are inserted into the electrolyte and respectively used as a counter electrode and a reference electrode, and the redox process is realized by charging for 1min under the voltage of 0.8V. A nonlinear response test was performed on it at a single beam nonlinear transmittance setting.
Results of single beam nonlinear transmittance evaluation of Prussian blue nonlinear response in an open aperture Z scanning system (Z-scan) show that the nonlinear absorption coefficient beta of Prussian blue 0 ＝-94.35cm GW -1 。
Comparative example 1
Prussian blue film was synthesized by electrochemical deposition. The non-linear response test was performed without redox treatment at a single beam non-linear transmittance setting.
The results of the nonlinear transmittance evaluation of the single beam in an open aperture Z scanning system (Z-scan) for the nonlinear response of tin disulfide show that the nonlinear absorption coefficient beta 0 ＝-81.62cm GW -1 。
Fig. 1 is an X-ray spectroscopy (EDS) image of a prussian blue film obtained by an electrochemical deposition method without any voltage applied thereto, which reveals the chemical composition of the prussian blue film.
The raman spectrum image of fig. 2 reveals the microscopic chemical composition of the prussian blue film, corresponding to the results of fig. 1. For PB 2151cm -1 The peak at this point is related to the stretching vibration of the c≡n bond. 286cm -1 And 220cm -1 The peaks at these can be attributed to the distorted vibrations of the Fe-CN-Fe bond and C-Fe-C, respectively. 1097cm -1 And 563cm -1 The two peaks at which are assigned to FTO.
The ultraviolet-visible photoelectron spectroscopy (UV-Vis) image of fig. 3 reveals the linear absorption characteristics of the prussian blue film and the linear absorption changes at different applied voltages. Wherein b1 is the absorption change curve in the film reduction process, b2 is the absorption change curve in the film oxidation process, and b3 is the absorption peak position change amplification curve under some voltages.
FIG. 4 is a summary of Z-scan and fitting curves of Prussian blue films under different applied voltages, and FIGS. 4 (a) to 4 (i) are sequentially-0.2V, 0.3V, 0.4V, 0.5V, 0.6V, 0.8V, 1.1V, and 1.4V.
The cyclic voltammogram of fig. 5 shows that the materials all exhibit excellent stability and reversibility during the test of the above examples.
Example 4
Most of them are the same as in example 1 except that the voltage is adjusted to-0.2V.
Example 5
Most of them are the same as in example 1 except that the voltage is adjusted to 1.1V.
Example 6
Most of them are the same as in example 1 except that the voltage is adjusted to 1.4V.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.
Claims (3)
1. A method for regulating and controlling nonlinear absorption performance of Prussian blue film is characterized in that the in-situ electrochemical oxidation reduction is carried out on the Prussian blue film to realize the regulation and control of nonlinear optical performance of the Prussian blue film;
according to the method, a three-electrode system is adopted, different electrochemical external voltages are applied to the Prussian blue film in electrolyte containing electrochemical charge compensation electrolyte, and the conversion of ferric iron and ferrous iron of the Prussian blue film is regulated to realize different mixed valence ratios, so that the nonlinear optical performance of the Prussian blue film is regulated;
the electrochemical charge compensation electrolyte is alkali metal salt, wherein the alkali metal comprises Li, na or K, and the salt is nitrate, sulfate or chloride;
the concentration of the electrochemical charge compensation electrolyte in the electrolyte is 0.01-1 mol/L;
the pH value of the electrolyte is 2-3;
the electrolyte containing the electrochemical charge compensation electrolyte is an aqueous solution of the electrochemical charge compensation electrolyte;
in the three-electrode system, the counter electrode is a platinum sheet, and the reference electrode is an Ag/AgCl electrode;
the electrochemical external voltage is not less than-0.2. 0.2V and not more than 1.4. 1.4V relative to the Ag/AgCl electrode.
2. The method for regulating and controlling the nonlinear absorption performance of the Prussian blue film according to claim 1, wherein the Prussian blue film is synthesized by an electrochemical deposition method.
3. A prussian blue film having tunable nonlinear absorption properties obtained by the method of claim 1 or 2.
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| JPH0482889A (en) * | 1990-07-20 | 1992-03-16 | Hitachi Chem Co Ltd | Tetraphenylporphyrin derivative, its production, production of lb film and benzaldehyde derivative |
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| JPH0482889A (en) * | 1990-07-20 | 1992-03-16 | Hitachi Chem Co Ltd | Tetraphenylporphyrin derivative, its production, production of lb film and benzaldehyde derivative |
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| CN107991819A (en) * | 2017-11-23 | 2018-05-04 | 北京工业大学 | One kind improves Prussian blue electrochomeric films in LiClO4The method of cyclical stability in/PC electrolyte |
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