CN112903792B - Novel multi-functional photoelectrochemistry reaction tank - Google Patents
Novel multi-functional photoelectrochemistry reaction tank Download PDFInfo
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- CN112903792B CN112903792B CN202110111365.1A CN202110111365A CN112903792B CN 112903792 B CN112903792 B CN 112903792B CN 202110111365 A CN202110111365 A CN 202110111365A CN 112903792 B CN112903792 B CN 112903792B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/305—Electrodes, e.g. test electrodes; Half-cells optically transparent or photoresponsive electrodes
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N2021/651—Cuvettes therefore
Abstract
The invention discloses a novel multifunctional photoelectrochemical reaction tank which can realize photoelectrochemical property test of a semiconductor thin film photoelectrode with double-sided and single-sided conduction. And can also be used as a reaction tank for in-situ Raman spectroscopy research. The working area of the working electrode and the distance between the working electrode and the counter electrode are accurately controlled, so that the photoelectrochemical property of the sample is accurately tested, and the carrier transmission distance is tested and analyzed through the front and back incident light test. The invention has the advantages of simple structure and low cost, and can also ensure the accuracy of sample performance test and improve the research quality.
Description
Technical Field
The invention belongs to the field of artificial photosynthesis, and relates to a multifunctional photoelectrochemical reaction tank which can realize photoelectrochemical property analysis and test of a semiconductor thin film photoelectrode, wherein the photoelectrochemical property analysis and test comprises photocurrent, carrier transmission distance and the like, and meanwhile, the reaction tank can also realize in-situ research of Raman spectrum.
Background
The artificial photosynthesis simulates photosynthesis in nature, and solar energy is utilized to convert carbon dioxide and water into hydrogen and organic fuels, such as methane, formic acid, ethanol and the like, so that direct conversion from solar energy to chemical energy is the most promising potential way for fundamentally solving energy and environmental crisis. However, the artificial photosynthesis is not practically popularized at present due to the low energy conversion efficiency of the semiconductor photoelectrode, which is limited by the core energy absorption and conversion center. Therefore, research on artificial photosynthesis has focused on developing and designing efficient semiconductor photoelectrodes.
Photoelectrodes are generally composed of wafers or semiconductor thin films grown on conductive substrates, and their photoelectrochemical property studies mainly include: current-voltage response curves, turn-on potentials, saturated photocurrents, quantum conversion efficiencies, carrier transport distances, and the like. At present, the photoelectrochemical performance of the photoelectrode is mainly tested in a photoelectrochemical reaction tank, and the conventional photoelectrochemical reaction tank mainly comprises the following two types: 1. the square reaction tank consists of quartz glass, and a tank cover made of polytetrafluoroethylene is attached to the square reaction tank to fix three electrodes; 2. a reactor made of polytetrafluoroethylene was equipped with a quartz optical window and a sample holder. Both reaction tanks have respective advantages, however, the defects are also very obvious, and summarizing the photoelectrochemical reaction tanks commonly used at present, the following problems mainly exist:
1. low test precision and poor repeatability
The actual area of the photoelectrodes and the electrode spacing in the reaction tank are difficult to fix, and meanwhile, the position of a sample in a light spot is not fixed, so that the illumination intensity received by the actual operation is uneven, the performance test precision of the sample is low, and the repeatability is poor; in addition, the reaction cell is large in volume, a large amount of electrolyte is needed, and meanwhile, large overpotential is introduced due to mass transfer limitation. Furthermore, the existing reaction cell is difficult to realize front-back incident light test of the sample, so that accurate carrier transmission distance research cannot be performed.
2. Single function, difficult in-situ research
The photoelectrochemical property and the corresponding spectroscopy property of the in-situ research sample are hot spots of the current research, however, the current reaction tank is difficult to match with a testing instrument, and the in-situ research is not strictly in-situ because the in-situ research sample is required to be carried out by depending on a special reaction tank, so that experimental conditions are changed.
3. Is easy to be lost, increases the research cost
The conventional quartz reaction tank is extremely easy to break and has poor reusability; in addition, quartz reaction cells face stability challenges in strongly alkaline electrolytes.
Therefore, as a researcher, a set of brand-new photoelectrochemical reaction tanks is expected to be designed, so that the problems can be well solved, and the efficiency is improved while the experimental precision and the cost are ensured. The inventor combines the practical experimental experience of the inventor, and finally creates the invention with use value after repeated improvement.
Disclosure of Invention
The invention designs and prepares a novel multifunctional photoelectrochemical reaction tank aiming at a plurality of problems existing in the photoelectrochemical reaction tank in the existing semiconductor photoelectrode performance test.
The invention aims to solve the technical problems:
the problems of inaccurate photoelectric polarity performance test, poor repeatability, single function and high cost limitation caused by design defects of the existing photoelectrochemical reaction tank are solved, the photoelectrochemical reaction tank is double-sided transparent, the sample area and the electrode spacing are fixed, the repeatability is high, the photoelectrochemical reaction tank is suitable for various testing environments and is easy to detach, and the research of artificial photosynthesis is assisted.
The invention adopts the solution scheme that:
the invention discloses a multifunctional photoelectrochemical reaction tank which comprises a main cavity, a quartz window, a front cover plate and a rear cover plate, wherein the front cover plate is arranged on the main cavity; the main cavity has a certain thickness, the center of the main cavity is of a cavity structure, a first window for fixing the illumination area of a sample is formed in one side of the cavity structure, a second window for setting a quartz window is formed in the other opposite side of the cavity structure, and grooves for placing sealing rubber rings are formed in the first window and the second window;
the second window, the quartz window and the front cover plate are sequentially arranged and are mutually clung, and a sealing rubber ring is arranged between the second window and the quartz window; a sample film is placed between the first window and the rear cover plate, the first window and the rear cover plate are tightly attached, and a sealing rubber ring is arranged between the first window and the sample film;
the top of the main cavity is provided with two threaded holes for placing electrodes, and the threaded holes are communicated with the cavity structure;
the front cover plate is provided with a window with a size larger than or equal to that of the second window at a position corresponding to the second window; the size of the quartz window completely covers the window opening and the second window on the front cover plate;
and a window with the same size as the first window is arranged on the rear cover plate corresponding to the first window.
According to the preferred scheme of the invention, the front cover plate, the main cavity body and the rear cover plate are connected and fixed through screws. The front cover plate, the main cavity and the rear cover plate are made of PEEK materials. The sealing rubber ring adopts a polytetrafluoroethylene-protected silica gel sealing ring, so that most electrolyte such as acid, alkali and the like can be prevented from being corroded.
According to a preferred embodiment of the invention, two threaded holes are provided in the top of the main chamber, one for sealing and fixing the reference electrode and the other for sealing and fixing the counter electrode.
According to the preferred scheme of the invention, the optical path from the quartz window to the surface of the sample film is 1cm, and the quartz window can be used for in-situ Raman spectrum testing.
According to the preferred scheme of the invention, the quartz window adopts an ultraviolet fused quartz high-precision window and is used for realizing high permeability of the wave band of 200nm-1000 nm.
The invention also discloses a photoelectrochemical property testing method of the multifunctional photoelectrochemical reaction tank, which comprises the following steps:
1) Before testing, soaking the front cover plate, the main cavity and the rear cover plate in nitric acid for pickling to eliminate the influence of pollutants on experimental results; then assembling a multifunctional photoelectrochemical reaction tank to enable the position of the film to be detected to coincide with the position of the first window of the main cavity;
2) Electrolyte is filled into the cavity structure, the reaction tank is connected with a three-electrode test system, a threaded hole is formed in the top of the main cavity body for sealing and fixing a reference electrode, and a counter electrode is sealed and fixed; the reference electrode is not contacted with the bottom of the hollow structure; taking a conductive adhesive tape connected with a sample film as a working electrode, forming a three-electrode system with the reference electrode and the counter electrode, and performing performance test by adopting a three-electrode analysis system;
3): and replacing the electrolyte, the sample, the reference electrode or the light source according to the test requirement, and performing performance test.
According to a preferred embodiment of the invention, an Ag/AgCl reference electrode and a Pt wire counter electrode are used.
The center of the sample back cover plate is provided with a window with the same size as the center of the back of the main cavity, so that a front and back illumination contrast test with the same area can be realized, and the carrier transmission distance and service life can be calculated.
Compared with the prior art, the invention has the advantages that:
1. the invention has simple and flexible structure, is convenient to detach and clean, is acid and alkali resistant, is suitable for various complex electrolyte systems, can ensure the purity of the electrolyte and avoid the pollution from a reaction tank.
2. The invention realizes the complete fixation of the position and the area of the sample in the incident light spot, greatly reduces the test error caused by human factors, and effectively improves the accuracy and the repeatability of the performance test of the sample.
3. The invention fixes the position and the area of the test sample through the sealing ring and the sample cover plate, avoids the traditional complex working electrode preparation process adopting conductive silver paste, epoxy resin, glass tube and the like, greatly simplifies the test flow and improves the test efficiency.
4. The invention has the multifunctional characteristic, can be used as a conventional photoelectrochemical reaction tank and also can be used as an in-situ Raman spectrum test tank, greatly reduces the experiment cost, and realizes in-situ research in the true sense.
5. The invention adopts integrated design, has compact structure, elegant appearance, convenient operation and low manufacturing cost, and is easy to popularize and use on a large scale.
Drawings
FIG. 1 is a schematic view of a partial structure of the present invention;
FIG. 2 is a schematic diagram of the working and assembly of the present invention;
fig. 3 shows the semiconductor photovoltaic voltage-current response and internal quantum conversion efficiency measured using the present invention.
Detailed Description
The invention is further illustrated and described below in connection with specific embodiments. The technical features of the embodiments of the invention can be combined correspondingly on the premise of no mutual conflict.
Step one: and assembling the quartz window side of the reaction tank. As shown in FIG. 1, the novel multifunctional photoelectrochemical reaction tank mainly comprises a reaction tank main body (shown in FIGS. 1a,1b and 1 c) and a front cover plate and a rear cover plate (shown in FIGS. 1d and 1 e), is processed by adopting PEEK materials through CNC technology, and has the advantages of acid and alkali resistance and high strength. Immersing the reaction tank part in nitric acid with the concentration of 1M for pickling for 1h before testing so as to eliminate the influence of pollutants on experimental results; then placing the cleaned reaction tank on dust-free cloth, and placing a sealing rubber ring in a corresponding notch to ensure that the sealing ring is attached to the notch and protrudes by about 0.2mm; then willClean quartz window (FIG. 1f, 3X 3cm 2 ) Placed on the sealing ring (2X 2 cm) 2 ) Ensuring that the quartz window is at the right center of the rubber ring; and finally, covering the front cover plate on the quartz window, and fixing the quartz window through 8 screws. When the screws are screwed, 8 screws are screwed in sequence for multiple times according to the diagonal direction. Tightening part of the screw at a time causes the quartz plate to be broken by a large shearing force.
Step two: preparation of the samples and sample side assembly. The sample is mainly a film on a conductive substrate, taking a film sample on FTO as an example, firstly cutting the sample into a size of about 1 x 1.5cm 2 Is etched with dilute hydrochloric acid at the corners of the 1.5cm long side to expose a portion of the FTO conductive substrate where a good ohmic contact is made with the conductive tape and silver paste. Placing the prepared electrode material sample at a sample window on the reaction tank towards the quartz window to ensure that the film sample in the sealing ring area is complete and no substrate or conductive area is exposed; and finally, covering the rear cover plate on the sample, and fixing the sample by adopting 8 screws. Here, the position coincidence of the sample window on the cover plate and the sample window reserved by the main body is ensured, and attention is paid to the attention of screwing.
Step three: the reaction tank is connected with a three-electrode test system. Electrodes are respectively inserted into interfaces of a reference electrode (Ag/AgCl) and a counter electrode (Pt wire) reserved on the main body of the reaction tank, and screws are screwed down, so that the reference electrode can not be directly contacted with the bottom. Finally, the adhesive tape connected with the sample is used as a working electrode, and the three-electrode system is formed by the adhesive tape, the reference electrode instrument and the counter electrode instrument, and a three-electrode analysis system, such as an electrochemical workstation, is adopted for performance test. The assembled reaction cell is shown in fig. 2.
Step four: according to the test requirement, the electrolyte, the sample, the reference electrode or the light source can be replaced to perform photoelectrochemical property test. For testing of the same electrolyte, the quartz window part is not required to be disassembled for each test, and the sample cover plate is only required to be opened to replace the sample.
Examples:
in order to further illustrate the technical means of the invention, the specific implementation steps and details of the novel multifunctional photoelectrochemical reaction tank provided by the invention are described in detail below by taking a p-type semiconductor-copper bismuth oxygen film photocathode prepared by adopting a reactive sputtering method on FTO conductive glass as an example with reference to fig. 3.
Photoelectrode preparation: the photoelectrode adopted in this time is a copper bismuth oxide film prepared on the FTO conductive glass by a reactive sputtering process. Two independent radio frequency power supplies are adopted to control two metal targets: bismuth and copper, and the sputtering power was adjusted to 20W and 25W. The reactive sputtering atmosphere was 86% Ar and 14% oxygen at a pressure of 10mT. And sputtering for 1h, and calcining the obtained film in air at 500 ℃ for 1h to obtain a sample. The resulting sample was cut into 1X 1.5cm pieces 2 And one corner was erased with dilute hydrochloric acid, the portion FTO was exposed, and an electrode was made of a conductive tape for testing.
Preparing an electrolyte: the electrolyte was 1M phosphate buffer, including 0.1M sodium persulfate as a sacrificial agent, and the pH of the electrolyte was 8.2.
And (3) assembling a reaction tank: firstly, fixing two sealing rings in corresponding grooves of a main cavity, then sequentially stacking and placing a quartz window cover plate, a quartz window, a main cavity (with the front face facing downwards), a sample (with the conductive face facing downwards), a sample cover plate, and then screwing up a fixing screw; and then swinging a positive reaction tank, injecting electrolyte from the top, finally inserting a reference electrode and a counter electrode, screwing up a sealing interface, and finishing assembly.
And (3) testing:
1. the data shown in FIG. 3a were obtained from the I-V curves of the front and back test specimens under AM1.5 illumination.
2. The incident photon quantum conversion efficiency (IPCE) under front and back illumination of the sample tested in this reaction cell is shown in fig. 3 b.
The above is merely the most common test function of the present invention, but the function of the present invention is not limited thereto. The invention can also be used for researching in-situ Raman spectrum, in-situ ultrafast spectrum and the like. Any researcher familiar with the field of photoelectrochemistry research can perform a characteristic research according to the invention according to his own research direction.
Claims (6)
1. A photoelectrochemical property test method based on a multifunctional photoelectrochemical reaction tank comprises a main cavity, a quartz window, a front cover plate and a rear cover plate; the main cavity has a certain thickness, the center of the main cavity is of a cavity structure, a first window for fixing the illumination area of a sample is formed in one side of the cavity structure, a second window for setting a quartz window is formed in the other opposite side of the cavity structure, and grooves for placing sealing rubber rings are formed in the first window and the second window;
the second window, the quartz window and the front cover plate are sequentially arranged and are mutually clung, and a sealing rubber ring is arranged between the second window and the quartz window; a sample film is placed between the first window and the rear cover plate, the first window and the rear cover plate are tightly attached, and a sealing rubber ring is arranged between the first window and the sample film;
the top of the main cavity is provided with two threaded holes for placing electrodes, and the threaded holes are communicated with the cavity structure;
the front cover plate is provided with a window with a size larger than or equal to that of the second window at a position corresponding to the second window; the size of the quartz window completely covers the window opening and the second window on the front cover plate;
the rear cover plate is provided with a window with the same size as the first window at a position corresponding to the first window, and is used for realizing front and rear illumination contrast tests with the same area, and the carrier transmission distance and service life are obtained through calculation;
the optical path from the quartz window to the surface of the sample film is 1cm, and the quartz window is used for in-situ Raman spectrum testing;
the photoelectrochemical property testing method is characterized by comprising the following steps of:
1) Before testing, soaking the front cover plate, the main cavity and the rear cover plate in nitric acid for pickling to eliminate the influence of pollutants on experimental results; then assembling a multifunctional photoelectrochemical reaction tank to enable the position of the film to be detected to coincide with the position of the first window of the main cavity;
2) Electrolyte is filled into the cavity structure, the reaction tank is connected with a three-electrode test system, a threaded hole is formed in the top of the main cavity body for sealing and fixing a reference electrode, and a counter electrode is sealed and fixed; the reference electrode is not contacted with the bottom of the hollow structure; taking a conductive adhesive tape connected with a sample film as a working electrode, forming a three-electrode system with the reference electrode and the counter electrode, and performing performance test by adopting a three-electrode analysis system;
3) The electrolyte, sample, reference electrode or light source may be replaced as required for the test.
2. The photoelectrochemical property testing method according to claim 1, wherein the front cover plate, the main cavity and the rear cover plate are connected and fixed by screws.
3. The method for testing photoelectrochemical properties according to claim 1, wherein the front cover plate, the main cavity and the rear cover plate are made of PEEK material.
4. The method for testing photoelectrochemical properties according to claim 1, wherein the sealing rubber ring is a polytetrafluoroethylene-protected silica gel sealing ring.
5. The method of claim 1, wherein two threaded holes in the top of the main cavity are used to seal and fix the reference electrode and the counter electrode.
6. The photoelectrochemical property testing method of claim 1, wherein the quartz window is an ultraviolet fused quartz high-precision window for realizing high permeability of 200nm-1000nm bands.
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| CN103852501A (en) * | 2014-03-21 | 2014-06-11 | 华中科技大学 | Multifunctional photoelectrochemical testing device |
| CN104165916A (en) * | 2014-08-18 | 2014-11-26 | 天津大学 | Simulation battery device for field optics and photodynamics measurement |
| CN104897639A (en) * | 2015-05-06 | 2015-09-09 | 同济大学 | In-situ Raman light electrochemical cell by employing TiO2NTs/Ti sheet shape electrode and application thereof |
| WO2016133528A1 (en) * | 2015-02-20 | 2016-08-25 | Halliburton Energy Services, Inc. | Thin-layer spectroelectrochemical cell for use in subterranean formation operations |
| CN110018208A (en) * | 2019-05-13 | 2019-07-16 | 中国科学院化学研究所 | A kind of thin layer electrochemistry reaction tank for non-linear spectral in situ detection |
| CN210953905U (en) * | 2019-10-12 | 2020-07-07 | 福州大学 | Flow type spectrum electrochemical electrolytic cell |
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| US9022652B2 (en) * | 2012-09-28 | 2015-05-05 | Uchicago Argonne, Llc | Transmission-geometry electrochemical cell for in-situ scattering and spectroscopy investigations |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103852501A (en) * | 2014-03-21 | 2014-06-11 | 华中科技大学 | Multifunctional photoelectrochemical testing device |
| CN104165916A (en) * | 2014-08-18 | 2014-11-26 | 天津大学 | Simulation battery device for field optics and photodynamics measurement |
| WO2016133528A1 (en) * | 2015-02-20 | 2016-08-25 | Halliburton Energy Services, Inc. | Thin-layer spectroelectrochemical cell for use in subterranean formation operations |
| CN104897639A (en) * | 2015-05-06 | 2015-09-09 | 同济大学 | In-situ Raman light electrochemical cell by employing TiO2NTs/Ti sheet shape electrode and application thereof |
| CN110018208A (en) * | 2019-05-13 | 2019-07-16 | 中国科学院化学研究所 | A kind of thin layer electrochemistry reaction tank for non-linear spectral in situ detection |
| CN210953905U (en) * | 2019-10-12 | 2020-07-07 | 福州大学 | Flow type spectrum electrochemical electrolytic cell |
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