CN113376230B - Photoelectrochemical optical fiber microelectrode adopting electrode internal illumination mode and preparation method thereof - Google Patents
Photoelectrochemical optical fiber microelectrode adopting electrode internal illumination mode and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a photoelectrochemical optical fiber microelectrode adopting an internal illumination mode of an electrode. Wherein the optical fiber is made of plastic optical fiber with good toughness and the diameter is less than 1.0 mm. The conductive layer material meets the conditions of colorless transparency and good conductivity, and provides conductivity for the optical fiber. The photoelectric property optical fiber electrode disclosed by the invention has a very small size compared with the traditional photoelectrode, and still has good photoelectric response. And the optical excitation mode of the photoelectrode material realizes creative transformation from external light source excitation to optical fiber internal light source excitation. The new mode of using the internal light source well avoids the limitation of the application scene on the PEC illumination wavelength, and enlarges the selection range of photoelectric materials. The technology is expected to be applied to the fields of in-situ detection of organisms, continuous monitoring of environmental samples and the like.
Description
Technical Field
The invention belongs to the fields of photoelectrochemistry and analytical chemistry, and particularly relates to a photoelectrochemical optical fiber microelectrode adopting an electrode internal illumination mode and a preparation method thereof, which are used for solving the problems that the traditional photoelectrode is large in size and the wavelength of a light source in partial application scenes is limited.
Background
Photoelectrochemistry (PEC) refers to the discipline whereby light, upon irradiation by light, is absorbed by a metal or semiconductor electrode material, causing an electrode reaction to occur. Which is embodied as the conversion of light energy with electrical and chemical energy. PEC sensing technologies built using optoelectronically active materials are increasingly used for substance detection in biological and environmental samples. The technology has high sensitivity, easy miniaturization, lower cost, environmental protection and energy conservation, and is rapidly developed in recent years. PEC sensing technology is limited to off-line detection of samples and is rarely capable of in situ measurement of biological objects. However, the development of in-situ monitoring methods for substances in animals is a key research direction in many fields such as analytical chemistry, life science, and biomedicine, and has great significance for people to understand biological vital functions. The PEC sensing technology is a new star in the sensing field, and the application of the PEC sensing technology in-situ detection of organisms is necessary to be promoted.
The bottleneck in the use of PEC sensing technology for in situ detection of biological objects is mainly three. I.e., larger photoelectrode size, and the animal skin's limitation on the wavelength of the light source. These two limitations cause several specific problems in application. First, the large size of the photoelectrode may cause a relatively large wound on the animal body during the process of being buried in the animal body, increasing the risk of wound infection. This is not conducive to long-term detection. Second, most photovoltaic materials can only be excited in the uv-visible region to generate electrical signals, and uv-visible light hardly penetrates the skin of mammals, making it more difficult to excite the electrodes buried under the skin. The near infrared light can penetrate the skin, but the energy of the near infrared light cannot excite the electrode material. Thirdly, the intensity of the photoelectric signal is in positive correlation with the light receiving area of the photoelectrode, and the reduction in size of the photoelectrode means that the light receiving area of the photoelectrode is reduced and the photoelectric signal is reduced. Obtaining sufficient photoelectric signal intensity in vivo detection, activity of photoelectric materials, and electrode preparation process are very great challenges.
Therefore, the invention develops a photoelectrochemical optical fiber microelectrode adopting an internal illumination mode of the electrode. The photoelectrode is manufactured according to the design method of the photoelectrode, and the cross section size of the photoelectrode does not exceed 1.0 mm. Meanwhile, the light excitation mode of the photoelectrode material realizes creative transformation from external light source excitation to optical fiber internal light source excitation. By means of the excellent light guide performance of the optical fiber, the novel mode of exciting the external photoelectric material by using the electrode internal light source well avoids the limitation of an application scene on the PEC illumination wavelength, enlarges the selection range of the photoelectric material, directly selects the existing photoelectric material, and does not need to explore the preparation of the near-infrared photoelectric material. The most important point is that the conductive film added to the optical fiber provides better conductivity for the optical fiber electrode, promotes the transfer of photoelectrons, and ensures that the photoelectric performance optical fiber electrode can still provide obvious photoelectric signal intensity when the illumination area is smaller. The technology is expected to be applied to the fields of in-situ detection of organisms, continuous monitoring of environmental samples and the like.
Disclosure of Invention
The invention aims to provide a photoelectrochemical optical fiber microelectrode adopting an electrode internal illumination mode and a preparation method thereof. The technology is used for solving the problems that the traditional photoelectrode in the field of Photoelectrochemistry (PEC) is large in size and the wavelength of a light source in partial application scenes is limited. Is expected to be applied to the fields of in-situ detection of organisms, continuous monitoring of environmental samples and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a photoelectrochemical optical fiber microelectrode adopting an electrode internal illumination mode comprises the following steps:
(1) the structure of the photoelectric performance optical fiber electrode mainly comprises three layers: the optical fiber inner layer, the conductive film layer and the photoelectric material layer.
(2) The type of optical fiber used is a plastic optical fiber.
(3) The optical fiber is processed with a frosted surface.
(4) The selected optical fiber conductive layer material is characterized by being colorless and transparent and good in conductivity.
(5) The optical fiber conducting layer is prepared by a direct current sputtering technology.
(6) Material characteristics of the optical fiber photoelectric material layer: materials having good optoelectronic activity include, but are not limited to, optoelectronic semiconductor materials.
(7) The preparation method of the optical fiber photoelectric material layer comprises two methods: (i) dipping method preparation (ii) electrochemical deposition method preparation.
In some embodiments, step (2) is specifically as follows: the method is characterized in that a commercially available plastic optical fiber is adopted, a fiber core material is modified polymethyl methacrylate (PMMA), a cladding material is epoxy resin, the optical fiber is transparent and colorless, the minimum bending radius is 10 times of the diameter of the optical fiber, the length of transmitted white light is 25-30 meters, and the specification tolerance of the optical fiber is 6% of the diameter. The electrode substrate has the beneficial effect that the plastic optical fiber is not easy to break as the electrode substrate.
In some embodiments, step (3) is specifically as follows: cutting the optical fiber into small sections, and polishing one end of each small optical fiber section by using sand paper to obtain a frosted surface with a certain length. The advantage of this is that the frosted surface provides a crack in the surface of the fiber allowing light to escape from the inside of the light to the side of the fiber. The length of the frosted surface can be adjusted according to the practical application scene, and the longer the frosted surface is, the longer the length of the optical fiber which is penetrated out from the optical fiber is, the larger the area of the semiconductor material which is excited by light is, and the stronger the photocurrent signal is. For ease of illustration, this work is exemplified with a length of 1 cm. Photoelectrochemical experiments generally require that the area of a photoelectrode is controlled, and a rough frosted surface can be loaded with a semiconductor material, so that the area of the frosted surface is the area of the photoelectrode. The boundary between the frosted surface and the smooth surface can be clearly seen by naked eyes, and the photoelectrode material with a fixed area is ensured to be completely immersed in the electrolyte solution, so that the experimental operation is convenient. Full polishing of the fiber electrodes is not recommended.
In some embodiments, step (4) is specifically as follows: the material of the conductive film can be selected from and not limited to materials with colorless transparency and good conductivity such as Indium Tin Oxide (ITO), fluorine-doped tin oxide (FTO) and the like. The light-shielding optical fiber has the beneficial effect that only the colorless and transparent conductive material can not shield the light escaping from the interior of the optical fiber.
In some embodiments, step (5) is specifically as follows: and plating a conductive film on the polished optical fiber by a direct current sputtering method. The conductive film material is Indium Tin Oxide (ITO), the coating film is a film coating machine, the ITO film with a certain thickness is comprehensively sputtered on the optical fiber, and the conductive optical fiber is prepared. The conductive film has the beneficial effect that the insulating plastic optical fiber can conduct electricity through the conductive film.
In some embodiments, step (6) is specifically as follows: as an example of the photoelectric semiconductor, zinc oxide (ZnO) is used. The beneficial effect is that ZnO is easy to obtain.
In some embodiments, step (7) is specifically as follows: (i) the preparation method comprises the following steps: and dispersing the prepared photoelectric semiconductor nano-particles by using a solvent. Dipping the dispersion liquid by using a frosted end of the optical fiber, and drying. This process was repeated 3 times. Namely, the ZnO nano-layer is loaded on the conductive optical fiber. (ii) Preparing by an electrochemical deposition method: a three-electrode system is adopted, an ITO conductive optical fiber is used as a working electrode, a potentiostatic method is adopted in an electrochemical workstation, a required potential is set, and a semiconductor nano-layer can grow on the frosted end of the ITO conductive optical fiber after electrodeposition for a period of time. The photoelectric semiconductor layer is prepared, so that the optical fiber electrode has photoelectric response performance.
The current optical fiber electrode reports few and is almost used for a spectrum-electrochemical system, but not a photoelectrochemical system. In the spectrum-electrochemical system, the optical fiber electrode is used as an electro-catalytic electrode to directly catalyze the oxidation-reduction reaction in the electrolyte to degrade target substances. Without collecting the electrical signal generated at the fiber electrode. And our fiber electrode is designed for acquiring photocurrent signals.
The function and principle of each structure of the photoelectrochemical optical fiber microelectrode are as follows:
inner layer of optical fiber: optical fibers are capable of transmitting light over long distances because they utilize the principle of the difference in refractive index between the core material and the cladding material of the optical fiber. The light can be transmitted forward in the optical fiber by means of total reflection without overflowing from the side wall of the optical fiber, so that the energy loss is small, and the light can be transmitted for a long distance. The photoelectrochemical optical fiber electrode is designed to enable light in an optical fiber to excite a semiconductor material on the surface of the optical fiber, and light needs to overflow from the side wall of the optical fiber, so that cracks are artificially formed on the surface of the optical fiber by frosting the side wall of the optical fiber, and the total reflection mode of the light is damaged due to the fact that a medium is not uniform. Therefore, light can only overflow from the frosted surface of the optical fiber to irradiate the semiconductor material coated on the surface of the optical fiber, and the purpose of exciting the semiconductor is achieved.
A conductive film layer: since the optical fiber itself is not conductive, a conductive layer needs to be added as an electrode. The conductive film layer is located between the optical fiber and the semiconductor material, and in order to enable the semiconductor material to be irradiated with light overflowing from the optical fiber without being blocked, the conductive film layer must be colorless and transparent. Therefore, indium tin oxide which is colorless and transparent and has better conductivity is selected as a conductive film material of the optical fiber electrode.
Photoelectric material layer: a semiconductor material having photoelectric activity can be changed from an insulator to a conductor under excitation of light to generate an electrochemical signal such as a photocurrent or a photovoltage, and is an essential part of photoelectrochemistry. When the semiconductor is illuminated, electrons on the valence band are excited and jump to the conduction band, and holes corresponding to positive charges are left on the original valence band, so that electron-hole pairs are formed in the semiconductor. Due to the connection of the external circuit, the photo-excited electrons flow to the external circuit, so that a photocurrent signal can be obtained in the external circuit. The redox material in the environment of the photoelectrode reacts with the photo-generated electrons or holes in the semiconductor, so that the charge transmission of the semiconductor is influenced, and the photoelectric signal collected in an external circuit is changed.
The invention has the remarkable characteristics that:
(1) the invention constructs a photoelectrochemical optical fiber microelectrode adopting an internal illumination mode of an electrode, and realizes a mode that a photoelectrode material is excited by a light source from the inside of the electrode to generate a photoelectric signal for the first time.
(2) The photoelectrochemical optical fiber microelectrode adopting the internal illumination mode of the electrode, which is constructed by the invention, has smaller size than most of the existing photoelectrochemical electrodes and is very portable.
(3) Simple operation and can be prepared rapidly in batches.
(4) The photoelectrochemical optical fiber microelectrode adopting the electrode internal illumination mode, which is constructed by the invention, has an obvious photoelectric signal.
(5) The invention can be extended to the fields of construction of a portable photoelectrochemistry testing system, rapid and continuous monitoring of environmental samples, minimally invasive detection of biological samples and the like.
Drawings
FIG. 1 is a view showing the construction of a photoelectrochemical (ZnO) optical fiber microelectrode employing an internal illumination pattern of an electrode according to the present invention;
FIG. 2 is a photocurrent-time curve of a nano ZnO fiber electrode in the present invention;
FIG. 3 shows the photoelectrochemistry (TiO) using the internal illumination mode of the electrode according to the present invention 2 ) A structural diagram of the optical fiber microelectrode;
FIG. 4 shows a nano TiO compound in the present invention 2 Photocurrent-time curves of the fiber electrodes;
FIG. 5 is a comparison of the device of the photoelectrochemical optical fiber microelectrode of the internal illumination mode of the electrode of the present invention and a conventional common optical electrode of the external illumination mode in the embedded application scenario;
FIG. 6 is TiO with conventional external illumination mode in the industry 2 Photocurrent curves of the loaded conductive glass electrode in buried application scenarios.
Detailed Description
In order to make the content of the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto.
Example 1
Polishing the optical fiber:
the diameter of a plastic optical fiber sold in the market is 1.0 mm, the plastic optical fiber is transparent and colorless, a fiber core material is modified polymethyl methacrylate (PMMA), a cladding material is oxygen resin, the minimum bending radius is 10 times of the diameter of the optical fiber, the length of transmitted white light is 25-30 m, and the specification tolerance of the optical fiber is 6% of the diameter. Cutting optical fiber into 9~10 cm's segment, use abrasive paper to carry out 360 degrees with the one end of optical fiber segment and polish, obtain the frosting of length about 1.0 cm. And finally, ultrasonically cleaning the polished optical fiber by using ethanol and ultrapure water in sequence.
Preparing an optical fiber conductive film:
and plating a conductive film on the polished optical fiber by a direct current sputtering (DC sputtering) method. The conductive film material is Indium Tin Oxide (ITO), the coating film is a JCP-350M3 coating machine of Beijing Taikono science and technology limited, the ITO film with the thickness of 300 nm is comprehensively sputtered on the optical fiber under the conditions that the sputtering current is 60 mA and the sputtering voltage is 325V, and the conductive optical fiber is prepared.
Preparing an optical fiber photoelectric material layer:
two preparation methods are provided, in this case, zinc oxide (ZnO) is used as an example of the photoelectric material. (i) The preparation method comprises the following steps: and dispersing the prepared semiconductor nano particles by using a solvent. Zinc oxide (ZnO) nanoparticles having a particle size of about 30 nm were selected as a commercially available ZnO as an electro-optical material, a dispersion having a concentration of 1.0 mg/mL was prepared using ultrapure water, and the dispersion was dipped in a ground end of an optical fiber and dried at 37 ℃. This process was repeated 3 times. Namely, the ZnO nano-layer is loaded on the conductive optical fiber. (ii) Preparing by an electrochemical deposition method: a three-electrode system is adopted, ITO conductive optical fibers are used as working electrodes, a platinum wire electrode is used as a counter electrode, and an Ag/AgCl electrode is used as a reference electrode. Zinc nitrate solution with pH value of 7.5 is used as electrolyte, and the temperature of the electrolyte is kept constant in 85 ℃ water bath during the whole process of electrodeposition. The electrochemical workstation adopts a potentiostatic method, the potential is set to be-0.76V, the electro-deposition time is about 2700 s, and then a white ZnO nano-layer can grow on the ITO conductive optical fiber. The ZnO covered length is the length of the optical fiber frosted surface, and only the rough frosted surface can firmly load ZnO nanoparticles.
In the case, ZnO can be replaced by other semiconductor materials, and corresponding experimental parameters are changed accordingly. A photoelectric property fiber electrode is prepared, and the structure diagram of the photoelectric property fiber electrode is shown in figure 1.
Application example 1
The application of the photoelectric performance optical fiber electrode comprises the following steps:
the ZnO fiber electrode of example 1 was subjected to Photoelectrochemical (PEC) testing. The experimental setup was as shown in fig. 5 (a), with a three-electrode system, ITO conductive fiber as the working electrode, an electrode clamp to clamp the ITO conductive film part without ZnO load, a platinum wire electrode as the counter electrode, and an Ag/AgCl electrode as the reference electrode. Sodium sulfate aqueous solution with a concentration of 0.1M was used as the electrolyte. The time-current curve was measured using an electrochemical workstation under the irradiation of a fiber-dedicated internal light source with a wavelength of 280 nm, as shown in FIG. 2. Experimental results show that the nano ZnO optical fiber electrode with the load length of 1.0 cm can generate photocurrent with the strength of about 30 nA, and the nano ZnO optical fiber electrode has stable strength and obvious effect.
Example 2
The steps of polishing the optical fiber, preparing the conductive film of the optical fiber, and the like are the same as those of example 1.
Preparing the optical fiber photoelectric material layer: in the present case, titanium dioxide (TiO) is selected 2 ) As an example of an optoelectronic material. Prepared using a dipping method: and dispersing the prepared semiconductor nano particles by using a solvent. Selecting commercially available TiO with particle size of about 20 nm 2 The nanoparticles were used as photoelectric materials, and a dispersion solution with a concentration of 1.0 mg/mL was prepared with ultrapure water, and the dispersion solution was dipped in a polished end of an optical fiber, and dried at 37 ℃. This process was repeated 3 times. I.e. TiO is loaded on the conductive optical fiber 2 A nanolayer.
TiO in case of 2 The method can be replaced by other semiconductor materials, and corresponding experimental parameters are changed accordingly. A photoelectric property fiber electrode is prepared, and the structure diagram of the photoelectric property fiber electrode is shown in figure 3.
Application example 2
The application of the photoelectric performance optical fiber electrode comprises the following steps:
for TiO in example 2 2 The plastic fiber electrode was subjected to PEC testing. The experimental setup is shown in FIG. 5 (A), using a three-electrode system, TiO 2 The coated ITO conductive optical fiber is used as a working electrode, and an electrode clamp clamps the unloaded TiO 2 The ITO conductive film of (1), the platinum wire electrode as a counter electrode, and the Ag/AgCl electrode as a reference electrode. Sodium sulfate aqueous solution with a concentration of 0.1M was used as the electrolyte. The time-current curve was measured using an electrochemical workstation under the irradiation of a fiber-dedicated internal light source with a wavelength of 280 nm, as shown in FIG. 4. The experimental result shows that the nano TiO with the load length of 1.0 cm 2 The optical fiber electrode can generate photocurrent with the strength of about 35 nA, and has stable strength and obvious effect. The size of the optical fiber electrode is extremely small compared with the size of the conventional photoelectrochemical electrode, so that the optical fiber electrode is suitable for the application that the large-size electrode cannot be involved in.
To highlight the application advantages of the present invention, the application effect of the PEC fiber electrode in the internal illumination mode of the present invention and the PEC sheet electrode in the external illumination mode conventional in the art in embedded sample detection is compared. FIG. 5 is a comparative view of the device, since the electrodes are embedded in the sample, corresponding to the electrodes being inserted in a light-tight black cuvette. FIG. 5 (A), TiO on PEC fiber electrode of the invention 2 Excited by light introduced from the inside of the fiber, a very strong photocurrent signal can still be generated (see fig. 4). Looking back at fig. 5 (B), a conventional PEC sheet electrode, commonly used in the industry, must be excited with an external light source to excite the photovoltaic material. In the test scene of the embedded sample, the external light source cannot penetrate through the sample to reach the surface of the electrode, so that the photoelectric material on the electrode cannot be excited, and therefore, a photoelectric signal cannot be obtained, and the test is invalid. Therefore, conventional PEC electrodes cannot be applied in embedded sample testing. For comparison, the present example shows conventional TiO 2 Loaded conductive glass electrodes photocurrent curves were irradiated in a black sample cell using an external xenon lamp. As can be clearly seen from fig. 6, no photocurrent signal was generated, and the irregular fluctuation curve was derived from the error of the electrochemical device itself.
Based on the above experiments, it is proved that the PEC fiber electrode in the internal illumination mode of the invention breaks through the limitation that the conventional PEC fiber electrode cannot be tested in an embedded sample. Therefore, the embedded detection of living organisms, the continuous online detection of environmental samples and the like are very promising potential application scenes of the invention.
The above description is only a preferred embodiment of the present invention, and all the equivalent changes and modifications made according to the claims of the present invention should be covered by the present invention.
Claims (6)
1. A photoelectrochemical optical fiber microelectrode adopting an electrode internal illumination mode is characterized in that: the optical fiber comprises an optical fiber inner layer, a conductive film layer and a photoelectric material layer, wherein the optical fiber inner layer is a plastic optical fiber, the conductive film layer is made of indium tin oxide and fluorine-doped tin oxide, and the photoelectric material layer is made of zinc oxide, titanium dioxide, tungsten trioxide and molybdenum disulfide;
the preparation method of the photoelectrochemical optical fiber microelectrode adopting the electrode internal illumination mode comprises the following steps:
(1) preparing an inner layer of the optical fiber: cutting the plastic optical fiber into small sections by using the plastic optical fiber as a material of an optical fiber inner layer, and processing one end of the small sections of the plastic optical fiber into a frosted surface by using abrasive paper;
(2) preparing a conductive film layer: plating a conductive film on the small plastic optical fiber polished in the step (1) by adopting a direct current sputtering method to obtain a conductive optical fiber;
(3) preparing the photoelectric material layer: and preparing the photoelectric material layer on the conductive film layer of the frosted end of the conductive optical fiber by adopting a dipping method or an electrochemical deposition method.
2. The photoelectrochemical optical fiber microelectrode adopting an internal illumination mode of an electrode according to claim 1, wherein: the diameter of the plastic optical fiber in the step (1) is not more than 1.0 mm, the fiber core material is modified polymethyl methacrylate PMMA, the cladding material is epoxy resin, the plastic optical fiber is transparent and colorless, the minimum bending radius is 10 times of the diameter of the optical fiber, the length of transmitted white light is 25-30 m, and the specification tolerance of the optical fiber is 6% of the diameter.
3. The photoelectrochemical optical fiber microelectrode adopting an internal illumination mode of an electrode according to claim 1, wherein: the step (2) is specifically as follows: and (2) plating a conductive film on the small plastic optical fiber section polished in the step (1) by adopting a direct current sputtering method, wherein the conductive film is made of indium tin oxide or fluorine-doped tin oxide, and the film is plated by adopting a film plating machine.
4. The photoelectrochemical optical fiber microelectrode adopting an internal illumination mode of an electrode according to claim 1, wherein: the step (3) is specifically as follows: the preparation method comprises the following steps: dispersing prepared photoelectric semiconductor nano particles by using a solvent, dipping a fiber frosted end into the dispersion liquid, drying, and repeating the process for 3 times, namely loading a photoelectric material layer on the conductive film layer.
5. The photoelectrochemical optical fiber microelectrode adopting an internal illumination mode of an electrode according to claim 1, wherein: the step (3) is specifically as follows: preparing by an electrochemical deposition method: and (3) adopting a three-electrode system, taking the conductive optical fiber obtained in the step (2) as a working electrode, taking a photoelectric semiconductor salt solution as an electrolyte, taking a platinum wire electrode as a counter electrode and taking an Ag/AgCl electrode as a reference electrode, and carrying out electrochemical deposition to grow a photoelectric material layer on the frosted end of the conductive optical fiber.
6. The photoelectrochemical optical fiber microelectrode adopting an internal illumination mode of an electrode according to claim 4 or 5, wherein: the photoelectric semiconductor comprises zinc oxide, titanium dioxide, tungsten trioxide and molybdenum disulfide.
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