CN111610240B - Photoelectric biosensor constructed based on cathode photoelectrode - Google Patents
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Abstract
The invention discloses a photoelectric biosensor constructed based on a cathode photoelectrode, which comprises Cu x O NPs electrodes, cu x PTZ-CdSe QDs are modified on the surface of an electrode of the O NPs electrode, and under the irradiation of light, the CdSe QDs absorb energy, are subjected to electron-hole separation, and photo-generated electrons are transferred from VB of the CdSe QDs to CB and are finally captured by oxygen dissolved in a solution; holes separated from the CdSe QDs are transferred from VB to the HOMO energy level of PTZ and then transferred from the HOMO energy level of PTZ to VB of CuxO NPs; in addition, the LUMO energy level of PTZ is far higher than the CB energy level of CdSe QD, so that the effect of preventing electron backflow is achieved.
Description
Technical Field
The invention relates to preparation of a cathode photoelectrode and application of photoelectric sensing, in particular to construction of a novel cathode photoelectrode, which has high photocurrent and stability and can be developed as a photoelectric sensor.
Background
In the last decade, the development of the photoelectric chemical sensor is rapid, the stability of the electrode is greatly improved, and the detection sensitivity is also greatly improved. The strength of the response signal of a photoelectric chemical sensor depends to a large extent on the formation of excitons within the electrode, the key process of which is the separation of electron-hole pairs. Methods for improving exciton transport efficiency are mainly used for constructing metal ion doped semiconductor materials or constructing semiconductor heterostructures, and few researchers choose to introduce functional substances, and combine the methods. Therefore, there is still much room for research and development in constructing electrodes combining functional materials with semiconductor heterostructures.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects in the prior art, the invention provides a cathode photoelectrode and a preparation method thereof, wherein the cathode photoelectrode is made of Cu x O NPs and PTZ modified CdSe QDs, composite compositions, wherein PTZ promotes semiconductor materials CdSe QDs and Cu x And the hole transfer between O NPs prevents the recombination of electron-hole pairs, and the strength and the stability of cathode photoelectric signals are improved.
The technical scheme is as follows: in order to achieve the purpose, the invention adopts the technical scheme that:
a cathode photoelectrode comprising Cu x O NPs electrodes, cu x The electrode surface of the O NPs electrode is modified with PTZ-CdSe QDs.
The invention promotes Cu by introducing PTZ into the electrode material x Hole transfer between O NPs and CdSe QDs, and blocking the recombination of electron-hole pairs. The generation method of the photoelectric signal is as follows: under light irradiation, the CdSe QDs absorb energy, undergo electron-hole separation, and photogenerated electrons are transferred from VB of the CdSe QDs to CB and are finally captured by oxygen dissolved in a solution. Holes separated by the CdSe QDs are transferred from VB to the HOMO level of PTZ, and then from the HOMO level of PTZ to VB of CuxO NPs. In addition, the LUMO level of PTZ is much higher than that of CdSe QD (the LUMO level of PTZ is at least 1.5V greater than that of CdSe QD), which acts to prevent electron reflux, and thus, PTZ promotes the semiconductor materials CdSe QDs and Cu x And the hole transfer among the O NPs prevents the recombination of electron-hole pairs, improves the strength and stability of cathode photoelectric signals, and reduces the interference of reducing substances on the cathode photoelectric sensor.
A preparation method of a cathode photoelectrode comprises the following steps:
Preferably: in the step 2, the centrifugal speed is 3000-5000 rpm, and the centrifugal time is 5.0-10.0 min.
Preferably: in the step 3, the concentration of the phenothiazine-ethanol solution is 0.8-1.0 mg/mL, and the volume is 10-15 mL.
Preferably, the following components: in the step 5, the annealing temperature is 450-500 ℃, and the annealing time is 4-5 hours.
Light constructed based on cathode photoelectrodeElectrical biosensors including PTZ-CdSe QDs/Cu x O NPs/FTO electrodes, said PTZ-CdSe QDs/Cu x The surface of the O NPs/FTO electrode is provided with a SOx modification layer.
A preparation method of photoelectric biosensor based on cathode photoelectrode comprises preparing PTZ-CdSe QDs/Cu x Immersing the O NPs/FTO electrode into 2% PDDA solution and SOx solution in order to modify SOx to PTZ-CdSe QDs/Cu x O NPs/FTO electrode, wherein the PDDA solution contains 0.5M NaCl in a percentage of 2%.
Compared with the prior art, the invention has the following beneficial effects:
the invention promotes semiconductor materials CdSe QDs and Cu by PTZ x And the hole transfer between the O NPs improves the strength and stability of cathode photoelectric signals and improves the photoelectric performance of the cathode photoelectric sensor. Therefore, the cathode photoelectrode can improve the strength and stability of cathode photoelectric signals, reduce the interference of reducing substances on the cathode photoelectric sensor and enable the cathode photoelectrode to have higher stability and sensitivity.
Drawings
FIG. 1 is a TEM image of PTZ-CdSe QDs
FIG. 2 is Cu x SEM image of O NPs
FIG. 3 is Cu x Solid UV absorption Pattern of O NPs
FIG. 4 shows bare FTO (I), cu during assembly x O NPs/FTO(II)，PTZ-CdSe QDs/Cu x O NPs/FTO (III) and SO x /PTZ-CdSe QDs/Cu x Differential photocurrent response of O NP/FTO (IV) electrodes
Fig. 5 is a graph of the photocurrent response to various concentrations of sarcosine from a to i:0.001mM,0.005mM,0.01mM,0.05mM,0.1mM,0.5mM,1mM,2mM,5mM
FIG. 6 is a graph of the photocurrent response of a photoelectric biosensor with increasing sarcosine concentration, the inset being the corresponding calibration curve
FIG. 7 is a schematic diagram of cathode photoelectrode energy levels
Here, cu x O NPs represent copper oxide nanocones, PTZ represents phenothiazine, cdSeQDs represent cadmium selenide quantum dots, TGA represents thioglycolic acid, se tableSelenium, naBH 4 Denotes sodium borohydride, cdCl 2 Represents cadmium chloride, naOH represents sodium hydroxide, naHSe represents sodium hydroselenide, cu represents copper, cuSO 4 Represents copper sulfate, FTO represents fluorine-doped tin oxide glass, VB represents a valence band, CB represents a conduction band, HOMO represents a highest occupied molecular orbital, LUMO represents a lowest unoccupied molecular orbital, TEM represents a transmission electron microscope, SEM represents a scanning electron microscope, SOx represents Sarcosine oxidase, ag/AgCl represents silver/silver chloride, sarcosine represents Sarcosine, PDDA represents poly (diallyldimethylammonium chloride), naCl represents sodium chloride, and S/N represents a signal-to-noise ratio.
Detailed Description
The present invention is further illustrated by the following description in conjunction with the accompanying drawings and the specific embodiments, it is to be understood that these examples are given solely for the purpose of illustration and are not intended as a definition of the limits of the invention, since various equivalent modifications will occur to those skilled in the art upon reading the present invention and fall within the limits of the appended claims.
Example 1:
a cathode photoelectrode comprising Cu x O NPs electrodes, cu x The electrode surface of the O NPs electrode is modified with PTZ-CdSe QDs.
The invention promotes Cu by introducing PTZ into the electrode material x Hole transfer between O NPs and CdSe QDs, and blocking the recombination of electron-hole pairs. The generation method of the photoelectric signal is as follows: under light irradiation, the CdSe QDs absorb energy, undergo electron-hole separation, and photogenerated electrons are transferred from VB of the CdSe QDs to CB and are finally captured by oxygen dissolved in a solution. Holes separated by the CdSe QDs are transferred from VB to the HOMO level of PTZ, and then from the HOMO level of PTZ to VB of CuxO NPs. In addition, the LUMO level of PTZ is much higher than that of CdSe QD (the LUMO level of PTZ is at least 1.5V greater than that of CdSe QD), which acts to prevent electron reflux, and thus, PTZ promotes the semiconductor materials CdSe QDs and Cu x And the hole transfer among the O NPs prevents the recombination of electron-hole pairs, improves the strength and stability of cathode photoelectric signals, and reduces the interference of reducing substances on the cathode photoelectric sensor.
Cathode lightPreparation method of electrode, synthesizing CdSe QDs: 55.3mg Se powder and NaBH 4 The solution (5.32 mg/mL,10 mL) was added to a three-necked flask in sequence, and stirred until the solution became clear, transparent and colorless, to synthesize a precursor NaHSe. Adding CdCl 2 The solution (0.458 mg/mL,50 mL) and TGA (20. Mu.L) were added to another three-necked flask, and after adjusting the solution to pH =10.0 with NaOH (1M), 70. Mu.L of NaHSe precursor was added to the solution and refluxed at 100 ℃ for 4h to synthesize TGA-CdSe QDs. The TGA-CdSe QDs obtained were purified by aggregation with HCl (1M, 10mL) overnight, centrifuged at 5000rpm for 5.0min, and the supernatant was aspirated, while the lower layer was left as a precipitate. The precipitate was dissolved in a prepared PTZ-ethanol solution (0.8 mg/mL,10 mL) to synthesize PTZ-CdSe QDs (see FIG. 1). In saturated CuSO 4 Two cleaned FTO electrodes were placed in solution in opposition and then at 100mVs -1 Scanning at a scanning speed of 0.0-4.0V for 20 sections, electrochemically depositing to obtain Cu film, and rapidly rinsing the electrode in ultrapure water to remove residual CuSO 4 . The obtained Cu film was annealed at 450 ℃ for 4 hours in a tube furnace to form Cu x O NPs electrodes (see fig. 2). As shown in FIG. 3, cu x The O NPs electrode has a wider light absorption area and has excellent light absorption capacity. Cu to be prepared x After the O NPs electrode was immersed in PTZ-CdSe QDs at 4 ℃ for 3 hours, it was washed clean with ultrapure water for further photocurrent detection.
As shown in FIG. 7, the electrodes are made of CdSe QDs, PTZ and Cu x The three materials of O NPs are compounded, CB and VB of CdSe QDs are-1.6V and 1.3V respectively, HOMO of PTZ is 0.92V, and Cu x CB and VB of O NPs are-0.8V and 0.65V, respectively. Under light irradiation, cdSe QDs absorb energy, undergo electron-hole separation, and photogenerated electrons are transferred from VB of the CdSe QDs to CB and are finally captured by oxygen dissolved in the solution. Meanwhile, due to the existence of PTZ, holes separated from CdSe QD are transferred from VB to HOMO energy level of PTZ and then transferred from the HOMO energy level of PTZ to Cu x VB of O NPs. In addition, the LUMO energy level of PTZ is much higher than the CB of CdSe QDs, acting to prevent electron reflux.
The cathode photoelectrode obtained in example 1 was used to construct a photoelectric biosensor, and the photoelectric biosensor was used for detecting sarcosine.
A cathode photoelectrode was prepared as in example 1. PTZ-CdSe QDs/Cu x The O NPs/FTO electrode was immersed in 2% PDDA (containing 0.5M NaCl) and SOx solution in this order for 15 minutes to decorate SOx on the electrode, and this process was repeated 3 times to complete the sensor preparation for further photocurrent detection. The electrode photocurrent variation during assembly is shown in fig. 4. The sensor is used for detecting the concentration of sarcosine by adopting a three-electrode system, a platinum wire electrode is used as an auxiliary electrode, and an Ag/AgCl electrode is used as a reference electrode. The assembled electrodes were immersed in sarcosine solutions at concentrations of 0.001mM,0.005mM,0.01mM,0.05mM,0.1mM,0.5mM,1mM,2mM, and 5mM, respectively, and the electrochemical station scanned the time-current curve to detect the change in cathode photocurrent (see FIG. 5). As shown in fig. 6, the sensor linear range is 0.001mM to 1mM, calibration curve: i (μ a) =0.74552lg (Csar/mM) -4.46391 (correlation coefficient R = 0.9989), and the detection limit was 0.2 μ M according to S/N = 3.
Example 2
This example differs from example 1 in that 55mg of Se powder and NaBH are mixed 4 The solution (5 mg/mL,11 mL) was added to a three-necked flask in sequence, and stirred until the solution became clear, transparent and colorless, to synthesize a precursor NaHSe. Adding CdCl 2 The solution (0.4 mg/mL,60 mL) and TGA (19. Mu.L) were added to another three-necked flask, and after adjusting the solution to pH =10.0 with NaOH (0.9M), 68. Mu.L of NaHSe precursor was added to the solution and refluxed at 95 ℃ for 5h to synthesize TGA-CdSe QDs. The TGA-CdSe QDs thus obtained were purified by accumulating with HCl (0.9M, 11mL) overnight, centrifuged at 3000rpm for 10.0min, and then the supernatant was aspirated, and the lower layer was precipitated. The precipitate was dissolved in a prepared PTZ-ethanol solution (0.7 mg/mL,11 mL) to synthesize PTZ-CdSe QDs (see FIG. 1). In saturated CuSO 4 Two cleaned FTO electrodes were placed in solution in opposition and then at 99mVs -1 Scanning at a scanning speed of 0.0-4.0V for 40 sections, electrochemically depositing to obtain Cu film, and rapidly rinsing the electrode in ultrapure water to remove residual CuSO 4 . The obtained Cu film was placed in a tube furnace and annealed at 480 ℃ for 4.5 hours to form Cu x O NPs electrodes (see fig. 2). As shown in FIG. 3, cu x The O NPs electrode has a wide light absorption area and excellent light absorption capacity. Will prepareCu of (2) x After the O NPs electrode was immersed in PTZ-CdSe QDs at 3 ℃ for 4 hours, it was washed clean with ultrapure water for further photocurrent detection.
Example 3
This example differs from examples 1 and 2 in that 56mg of Se powder and NaBH are mixed 4 The solution (6 mg/mL,9 mL) was added to a three-necked flask in sequence, and stirred until the solution became clear, transparent and colorless, to synthesize a precursor NaHSe. Adding CdCl 2 The solution (0.5 mg/mL,45 mL) and TGA (21. Mu.L) were added to another three-necked flask, and after adjusting the solution to pH =10.0 with NaOH (1.1M), 71. Mu.L of NaHSe precursor was added to the solution and refluxed at 110 ℃ for 3.9h to synthesize TGA-CdSe QDs. The TGA-CdSe QDs thus obtained were purified by accumulating in HCl (1.1M, 9mL) overnight, and after centrifugation at 4500rpm for 8min, the supernatant was aspirated, while the lower precipitate was retained. The precipitate was dissolved in a prepared PTZ-ethanol solution (0.9 mg/mL,9 mL) to synthesize PTZ-CdSe QDs (see FIG. 1). In saturated CuSO 4 Two cleaned FTO electrodes were placed in solution in opposition and then at 100mVs -1 Scanning 30 sections at a scanning speed in the range of 0.0-4.0V, obtaining a Cu film by electrochemical deposition, and rapidly rinsing the electrode in ultrapure water to remove residual CuSO 4 . The obtained Cu film was annealed at 500 ℃ for 5 hours in a tube furnace to form Cu x O NPs electrodes (see fig. 2). As shown in FIG. 3, cu x The O NPs electrode has a wider light absorption area and has excellent light absorption capacity. Cu to be prepared x After the O NPs electrodes were immersed in PTZ-CdSe QDs at 5 ℃ for 2.5 hours, they were washed clean with ultrapure water for further photocurrent detection.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.
Claims (6)
1. The photoelectric biosensor constructed based on the cathode photoelectrode is characterized in that the cathode photoelectrode comprises Cu x O NPs electrodes, cu x The electrode surface of the O NPs electrode is modified withPTZ-CdSe QDs；
The preparation method of the cathode photoelectrode comprises the following steps:
step 1, synthesizing TGA-CdSe QDs: mixing Se powder with NaBH 4 Adding the solution into a container, stirring until the solution is in a clear, transparent and colorless state, and synthesizing a precursor NaHSe; adding CdCl 2 Adding the solution and TGA into another container to obtain a second solution, adjusting the pH value of the second solution to 10, adding a precursor NaHSe into the second solution, refluxing at 100 ℃, and synthesizing TGA-CdSe QDs;
step 2, TGA-CdSe QDs aggregation purification: aggregating and purifying the TGA-CdSe QDs obtained in the step 1 by using hydrochloric acid overnight, centrifuging, sucking out supernatant, and keeping a lower-layer precipitate;
step 3, synthesis of PTZ-CdSe QDs: dissolving the precipitate obtained in the step 2 in a phenothiazine-ethanol solution, continuously stirring until the precipitate is completely dissolved, and synthesizing PTZ-CdSe QDs;
step 4, preparing a Cu film: two cleaned FTO electrodes were placed in opposition in a saturated copper sulfate solution and then at 100mVs -1 The scanning speed of the electrode is in the range of 0.0-4.0V, 20-40 sections are scanned, the copper film is obtained by electrochemical deposition, the electrode is quickly washed in ultrapure water, and the residual CuSO is removed 4 Obtaining an electrode with a copper film;
step 5, cu x Preparing an O NPs photocathode electrode: annealing the electrode with the copper film obtained in step 4 to form Cu x An O NPs electrode;
step 6, PTZ-CdSe QDs/Cu x Preparing an O NPs/FTO electrode: the Cu obtained in the step 5 x Soaking the O NPs electrode into the PTZ-CdSe QDs obtained in the step 3 at the temperature of 4 ℃ for 1-3 hours, and then washing the PTZ-CdSe QDs/Cu by using ultrapure water to obtain the PTZ-CdSe QDs/Cu x O NPs/FTO electrodes;
the PTZ-CdSe QDs/Cu x The surface of the O NPs/FTO electrode is provided with a SOx modification layer.
2. The photoelectric biosensor constructed on the basis of the cathode photoelectrode according to claim 1, wherein the photoelectric signal is generated by the following method: under the irradiation of light, the CdSe QDs absorb energy, and electrons and holes are separated, so that photo-generated electrons are transferred from VB of the CdSe QDs to CB and are finally captured by oxygen dissolved in a solution; holes separated from CdSe QDs are transferred from VB to the HOMO energy level of PTZ, and then transferred from the HOMO energy level of PTZ to VB of CuxO NPs; in addition, the LUMO energy level of PTZ is far higher than the CB energy level of CdSe QDs, and the function of preventing the backflow of electrons is realized.
3. The photoelectric biosensor constructed based on the cathode photoelectrode according to claim 2, wherein: in the step 2, the centrifugal speed is 3000-5000 rpm, and the centrifugal time is 5.0-10.0 min.
4. The photoelectric biosensor constructed based on the cathode photoelectrode according to claim 3, wherein: in the step 3, the concentration of the phenothiazine-ethanol solution is 0.8-1.0 mg/mL, and the volume is 10-15 mL.
5. The photoelectric biosensor constructed based on the cathode photoelectrode according to claim 4, wherein: in the step 5, the annealing temperature is 450-500 ℃, and the annealing time is 4-5 hours.
6. The method for preparing the photoelectric biosensor constructed on the basis of the cathode photoelectrode as claimed in claim 1 is characterized in that: the prepared PTZ-CdSe QDs/Cu x Immersing the O NPs/FTO electrode into 2% PDDA solution and SOx solution in order to modify SOx to PTZ-CdSe QDs/Cu x O NPs/FTO electrode, wherein 2% of the PDDA solution contains 0.5M NaCl.
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