CN109283233A - It is a kind of for detecting the self energizing sensor of Microcystin - Google Patents
It is a kind of for detecting the self energizing sensor of Microcystin Download PDFInfo
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Abstract
The invention discloses a kind of for detecting the self energizing sensor of Microcystin, including the molten liquid ﹑ quartz reaction pond ﹑ air vent of light sun pole ﹑ light yin pole ﹑ simulated solar radiant ﹑ electricity solution matter and Microcystin normal concentration solution；The light anode and photocathode insertion are equipped with the quartz reaction pond of electrolyte solution, and are connected to by external circuit, and wherein photocathode is close to air vent；The light source irradiates light anode and photocathode simultaneously；It is characterized in that, the electrolyte solution is under the driving for the automatic bias that the phosphate buffer solution of pH=4~6, the light anode and photocathode generate under the conditions of light irradiates, and the light of constructed double optoelectronic poles driving helps fuel cell system, current path is formed, is produced electricl energy.Sensor of the invention avoids the use of additional power source；It helps fuel cell technology to be used to construct self energizing sensing platform double optoelectronic poles driving light, not only increases energy utilization efficiency, also reduce the cost of manufacture of self energizing sensor.
Description
Technical field
The present invention relates to one kind for detecting cyanophycean toxin Microcystin self energizing sensor, and in particular to a kind of double light
The preparation method of electrode drive photocatalytic fuel cell, belongs to photocatalytic fuel cell and sensory field.
Background technique
Self energizing electrochemical sensor, which refers to, does not need conventional batteries or AC power source, and the one of energy is directly obtained from environment
Class novel sensor voluntarily generates signal realization detection since it can get rid of external energy limitation, enormously simplifies sensor
Preparation process, reduce the expense of detection, be very beneficial for sensor to miniaturization, integrated direction development.
What self energizing electrochemical sensor research at present was mainly realized by the approach of microbial fuel cell.Biomass
Fuel cell only realizes energy conversion single between biomass energy and electric energy, and grinding in the energy and its related fields at present
It in studying carefully, comprehensively utilizes the various energy (such as Guang Neng ﹑ biomass energy and chemical energy), building full Xin ﹑ Gao Xiao ﹑ Wen Dings cheap more of ﹑
Dimension energy conversion fuel cell has become hot research direction.Photoresponse ingredient is introduced into combustion by emerging optical drive fuel cell
Expect to can be realized simultaneously luminous energy/electric energy and chemical energy/electric energy dual conversion in battery, to effectively improve using energy source effect
Rate is the developing direction of future source of energy conversion equipment, is of great significance in terms of practical application and bright prospects.
Existing most of light help fuel cell there is still a need for by biological auxiliary element (such as enzyme ﹑ microorganism), this just gives
Fuel cell brings test in terms of operating Tiao Jian ﹑.Still further aspect, currently, for optoelectronic pole material
Titanium dioxide (TiO is also mainly limited in selection2) the semiconductor nano material of the classics such as ﹑ cadmium telluride (CdTe), but these materials
Expect also not satisfactory in terms of energy utilization efficiency and stability.In addition, helping fuel cell for the light of double optoelectronic poles driving
Building, prerequisite, that is, light anode fermi level should be higher than that photocathode.This just gives the sieve of light anode and photocathode material
Choosing and preparation propose more limitations and require.
Summary of the invention
It is an object of the invention to overcome defect existing in the prior art, provide it is a kind of prepare self energizing detection cyanobacteria poison
The method of the sensor of plain Microcystin, this method is based on photocatalytic fuel cell technology, using TiO2Nano material is light
Anode, azepine graphene (NG-BiOBr) nano material of bismuthyl bromide modification are photocathode, construct the light of double optoelectronic pole drivings
Fuel cell is helped, for constructing novel self-supplying power sensor, solves existing self energizing electrochemical sensor mainly by biology
Matter fuel cell technology, the combustion-supporting material cell power conversion efficiency of light is low compare the problems such as Gao ﹑ operating condition is harsh, and at present for cost
The technical issues of.
To achieve the above object, the present invention is by the following technical programs to solve its technical problem:
It is a kind of for detecting the self energizing sensor of Microcystin, including Guang Yang Ji ﹑ Guang Yin Ji ﹑ simulated solar irradiation light
Yuan ﹑ electricity solves matter Rong Ye ﹑ quartz reaction Chi ﹑ air vent and Microcystin normal concentration solution.The light anode and time
Pole insertion is equipped with the quartz reaction pond of electrolyte solution, and is connected to by external circuit, and wherein photocathode is close to air vent；
The light source irradiates light anode and photocathode simultaneously；The electrolyte solution is the phosphate buffer solution of pH=4~6, institute
Under the driving for stating the automatic bias that light anode and photocathode generate under the conditions of light irradiation, the light of constructed double optoelectronic poles driving is helped
Fuel cell system forms current path, produces electricl energy.
The light anode is TiO2Tin indium oxide (being commonly called as ITO) electrode of modification；Photocathode is NG-BiOBr modification
ITO electrode.The light anode TiO2With photocathode nano material (NG-BiOBr) the preparation method is as follows:
Light anode nano material TiO2It is prepared using hydro-thermal method: firstly, by butyl titanate [TiO (C4H9O)4] it is dissolved in nitre
Acid (HNO3) titanyl nitrate [TiO (NO is obtained in solution3)2] solution, then by TiO (NO3)2Solution is transferred to polytetrafluoroethylene (PTFE)
In the reaction kettle of back boxing, 12h is reacted at 160~200 DEG C, through centrifugation, ultrapure water and dehydrated alcohol carrying out washing treatment after natural cooling
Reaction product, it is dry under the conditions of finally placing it in 60 DEG C, obtain light anode nano material TiO2。
Wherein, the HNO3The concentration of solution is 6mol/L；The HNO3With TiO (C4H9O)4Dosage volume ratio be 5
~10:1.
Photocathode nano material NG-BiOBr is prepared using hydro-thermal method: firstly, by five nitric hydrate bismuth (Bi (NO3)3·
5H2O it) is dissolved in ultrapure water, with dilute HNO3Its pH value is adjusted to 3 by solution, spare；In addition, dispersing ten for azepine graphene (NG)
Ultrasonic mixing is uniform in six alkyl trimethyl ammonium bromides (CTAB) solution；Then, by aforementioned Bi (NO3)3·5H2The acid solution of O is slow
It is slow to instill in NG and CTAB mixed solution, above-mentioned mixed liquor is transferred in round-bottomed flask and reacts 3h in 60~120 DEG C of oil baths.Reaction
After the completion, the sediment of preparation ethyl alcohol and ultrapure water are washed 3 times respectively, 80 DEG C of dryings obtain photocathode NG-BiOBr and receive
Rice material.
Wherein, the volumetric usage of solvent for use ultrapure water are as follows: every 0.12g Bi (NO3)3·5H2O solvent for use ultrapure water
Amount is 50mL, and the concentration of the CTAB solution is 8 × 10-3mol/L；The CTAB and Bi (NO3)3·5H2The molar ratio of O is 1:
1, the NG and Bi (NO3)3·5H2O mass ratio are as follows: 0.8~4.5mg:0.12g, the ultrasonic mixing time are 0.5h.
The invention has the following beneficial effects:
(1) the present invention provides a kind of self energizing sensors for detecting Microcystin, which avoids additional
The use of power supply, sensor itself energize platform, are very beneficial for the micromation of sensor and the development of portability；
(2) double optoelectronic poles driving light is helped fuel cell technology to be used to construct self energizing sensing platform by the present invention, is not only mentioned
High energy utilization efficiency, is also greatly reduced the cost of manufacture of self energizing sensor, can look forward to it has extraordinary answer
Use prospect.
Detailed description of the invention
Fig. 1 is the structure chart of self energizing Microcystin sensor；
Fig. 2 is the detection schematic diagram of self energizing Microcystin sensor；
Fig. 3 is the dependency graph that the light of building helps Microcystin (MC-LR) concentration and V-I of self energizing sensing platform；
Fig. 4 is the correlation that the light of building helps Microcystin (MC-LR) concentration and P-I curve of self energizing sensing platform
Figure；
Fig. 5 is peak power output PmaxWith the linear correlation curve figure of corresponding Microcystins Concentration.
Specific embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings.
It is a kind of for detecting the self energizing sensor of Microcystin, structural schematic diagram as shown in Figure 1, include light sun
The molten liquid ﹑ quartz reaction pond ﹑ air vent of pole ﹑ light yin pole ﹑ simulated solar radiant ﹑ electricity solution matter and Microcystin normal concentration
Solution.The light anode and photocathode insertion are equipped with the quartz reaction pond of electrolyte solution, and are connected to by external circuit, wherein
Photocathode is close to air vent；The light source irradiates light anode and photocathode simultaneously；It is characterized in that the electrolyte is molten
Liquid is the drive for the automatic bias that the phosphate buffer solution of pH=4~6, the light anode and photocathode generate under the conditions of light irradiates
Under dynamic, the light of constructed double optoelectronic poles driving helps fuel cell system, forms current path, produces electricl energy.When drawing in system
When entering Microcystin, Microcystin consumes the hole of photoanode surface, it is suppressed that the recombination of light induced electron and hole, from
And enhance the output of entire self energizing system electric energy.When the concentration of Microcystin gradually increases, the output of electric energy also by
Cumulative plus (Fig. 2) thus establishes the corresponding relationship between Microcystins Concentration and electric power signal intensity, draws self energizing method
The standard curve of Sensitive Detection Microcystin.
Embodiment 1
1. the preparation of optoelectronic pole
(1) preparation of light anode: firstly, by 4mL [TiO (C4H9O)4] it is dissolved in the HNO of 20mL 6mol/L3It is obtained in solution
TiO(NO3)2Solution, then by the TiO (NO3)2Solution is transferred in the reaction kettle that polytetrafluoroethylene (PTFE) is back boxing, anti-at 160 DEG C
It answers 12h, through centrifugation, ultrapure water and dehydrated alcohol carrying out washing treatment reaction product after natural cooling, finally places it in 60 DEG C of conditions
Lower drying obtains light anode nano material TiO2.N,N-dimethylformamide (DMF) is dispersed by powder ultrasonic obtained above
In, it is configured to 6mg/mL ultrasonic disperse liquid.Pipetting the 20 above-mentioned dispersant liquid drops of μ L and being applied to effective area is 0.5cm2ITO electrode table
One layer of uniform membrane structure of ITO electrode surface self-assembling formation, light anode can be observed in face, the heating, drying under infrared lamp at this time
Preparation is completed.
(2) preparation of photocathode: firstly, by 0.12g Bi (NO3)3·5H2O is dissolved in 50mL ultrapure water, with dilute HNO3It is molten
Its pH value is adjusted to 3 by liquid, spare；In addition, dispersing 8 × 10 for 0.8mg NG-3Ultrasonic mixing is uniform in mol/L CTAB solution；
Then, the Bi (NO that will be got ready3)3·5H2O acid solution is slowly dropped into NG and CTAB mixed solution, and above-mentioned mixed liquor is transferred to circle
3h is reacted in 60 DEG C of oil baths in the flask of bottom.After the reaction was completed, the sediment of preparation ethyl alcohol and ultrapure water are washed 3 times respectively,
80 DEG C of dryings obtain photocathode NG-BiOBr nano material.It disperses powder ultrasonic obtained above in DMF, is configured to
6mg/mL ultrasonic disperse liquid.Pipetting the 20 above-mentioned dispersant liquid drops of μ L and being applied to effective area is 0.5cm2ITO electrode surface, in infrared
Heating, drying under lamp, can be observed one layer of uniform membrane structure of ITO electrode surface self-assembling formation at this time, and photocathode preparation is completed.
2. the building that pair optoelectronic pole driving light helps fuel cell
The quartz reaction of the phosphate buffer solution equipped with pH=4 by light anode prepared by step 1 and photocathode insertion
Pond, and be connected to by external circuit, wherein photocathode is close to air vent.Described in simulated solar radiant is irradiated simultaneously
Under the driving for the automatic bias that light anode and photocathode, light anode and photocathode generate under the conditions of light irradiates, double optoelectronic poles are constituted
The light of driving helps fuel cell system, forms current path, produces electricl energy.
3. self energizing sensor is for detecting Microcystin
Fuel cell is helped to be used for the detection of Microcystin light constructed by step 2, when introducing microcystin in system
When plain, Microcystin consumes the hole of photoanode surface, it is suppressed that the recombination of light induced electron and hole, to enhance whole
The output of a self energizing system electric energy.When the concentration of Microcystin gradually increases, the output of electric energy is also gradually increased, thus
The corresponding relationship between Microcystins Concentration and electric power signal intensity is established, self energizing method Sensitive Detection microcystin is drawn
The standard curve of element.
Fig. 3 and Fig. 4 is respectively Microcystin (MC-LR) concentration and electricity that constructed light helps self energizing sensing platform
The relational graph of piezo-electric flow curve (V-I) and power output curve (P-I).As seen from the figure, light helps the maximum of self energizing sensing platform
Output power (Pmax) increase with the increase of MC-LR concentration, thus MC-LR can be quantified by V-I and P-I curve.Into one
Step carries out concrete analysis to data and knows, PmaxGood linear relationship is presented with the logarithm of MC-LR concentration, as a result such as Fig. 5 institute
Show.
Embodiment 2
1. the preparation of optoelectronic pole
(1) preparation of light anode: firstly, by 5mL [TiO (C4H9O)4] it is dissolved in the HNO of 40mL 6mol/L3It is obtained in solution
TiO(NO3)2Solution, then by the TiO (NO3)2Solution is transferred in the reaction kettle that polytetrafluoroethylene (PTFE) is back boxing, anti-at 180 DEG C
It answers 12h, through centrifugation, ultrapure water and dehydrated alcohol carrying out washing treatment reaction product after natural cooling, finally places it in 60 DEG C of conditions
Lower drying obtains light anode nano material TiO2.It disperses powder ultrasonic obtained above in DMF, it is super to be configured to 6mg/mL
Sound dispersion liquid.Pipetting the 20 above-mentioned dispersant liquid drops of μ L and being applied to effective area is 0.5cm2ITO electrode surface, heated under infrared lamp
Drying, can be observed one layer of uniform membrane structure of ITO electrode surface self-assembling formation at this time, and light anode preparation is completed.
(2) preparation of photocathode: firstly, by 0.12g Bi (NO3)3·5H2O is dissolved in 50mL ultrapure water, with dilute HNO3It is molten
Its pH value is adjusted to 3 by liquid, spare；In addition, dispersing 8 × 10 for 2.0mg NG-3Ultrasonic mixing is uniform in mol/L CTAB solution；
Then, the Bi (NO that will be got ready3)3·5H2O acid solution is slowly dropped into NG and CTAB mixed solution, and above-mentioned mixed liquor is transferred to circle
3h is reacted in 80 DEG C of oil baths in the flask of bottom.After the reaction was completed, the sediment of preparation ethyl alcohol and ultrapure water are washed 3 times respectively,
80 DEG C of dryings obtain photocathode NG-BiOBr nano material.It disperses powder ultrasonic obtained above in DMF, is configured to
6mg/L ultrasonic disperse liquid.Pipetting the 20 above-mentioned dispersant liquid drops of μ L and being applied to effective area is 0.5cm2ITO electrode surface, in infrared
Heating, drying under lamp, can be observed one layer of uniform membrane structure of ITO electrode surface self-assembling formation at this time, and photocathode preparation is completed.
2. the building that pair optoelectronic pole driving light helps fuel cell
The quartz reaction pond of the phosphate buffer solution equipped with pH=5 by light anode described in step 1 and photocathode insertion, and
It is connected to by external circuit, wherein photocathode is close to air vent.Simulated solar radiant is irradiated to the light sun simultaneously
Under the driving for the automatic bias that pole and photocathode, light anode and photocathode generate under the conditions of light irradiates, double optoelectronic pole drivings are constituted
Light help fuel cell system, form current path, produce electricl energy.
3. self energizing sensor is for detecting Microcystin
Fuel cell is helped to be used for the detection of Microcystin light constructed by step 2, when introducing microcystin in system
When plain, Microcystin consumes the hole of photoanode surface, it is suppressed that the recombination of light induced electron and hole, to enhance whole
The output of a self energizing system electric energy.When the concentration of Microcystin gradually increases, the output of electric energy is also gradually increased, thus
The corresponding relationship between Microcystins Concentration and electric power signal intensity is established, self energizing method Sensitive Detection microcystin is drawn
The standard curve of element.
Embodiment 3
1. the preparation of optoelectronic pole
(1) preparation of light anode: firstly, by 5mL TiO (C4H9O)4It is dissolved in the HNO of 50mL 6mol/L3It is obtained in solution
TiO(NO3)2Solution, then by the TiO (NO3)2Solution is transferred in the reaction kettle that polytetrafluoroethylene (PTFE) is back boxing, anti-at 200 DEG C
It answers 12h, through centrifugation, ultrapure water and dehydrated alcohol carrying out washing treatment reaction product after natural cooling, finally places it in 60 DEG C of conditions
Lower drying obtains light anode nano material TiO2.It disperses powder ultrasonic obtained above in DMF, is configured to 6mg/L ultrasound
Dispersion liquid.Pipetting the 20 above-mentioned dispersant liquid drops of μ L and being applied to effective area is 0.5cm2ITO electrode surface, under infrared lamp heat dry
It is dry, one layer of uniform membrane structure of ITO electrode surface self-assembling formation can be observed at this time, light anode preparation is completed.
(2) preparation of photocathode: firstly, by 0.12g Bi (NO3)3·5H2O is dissolved in 50mL ultrapure water, with dilute HNO3It is molten
Its pH value is adjusted to 3 by liquid, spare；In addition, dispersing 8 × 10 for 4.5mg NG-3Ultrasonic mixing is uniform in mol/L CTAB solution；
Then, the Bi (NO that will be got ready3)3·5H2O acid solution is slowly dropped into NG and CTAB mixed solution, and above-mentioned mixed liquor is transferred to circle
3h is reacted in 120 DEG C of oil baths in the flask of bottom.After the reaction was completed, the sediment of preparation ethyl alcohol and ultrapure water are washed 3 times respectively,
80 DEG C of dryings obtain photocathode NG-BiOBr nano material.It disperses powder ultrasonic obtained above in DMF, is configured to
6mg/mL ultrasonic disperse liquid.Pipetting the 20 above-mentioned dispersant liquid drops of μ L and being applied to effective area is 0.5cm2ITO electrode surface, in infrared
Heating, drying under lamp, can be observed one layer of uniform membrane structure of ITO electrode surface self-assembling formation at this time, and photocathode preparation is completed.
2. the building that pair optoelectronic pole driving light helps fuel cell
The quartz reaction pond of the phosphate buffer solution equipped with pH=6 by light anode described in step 1 and photocathode insertion, and
It is connected to by external circuit, wherein photocathode is close to air vent.Simulated solar radiant is irradiated to the light sun simultaneously
Under the driving for the automatic bias that pole and photocathode, light anode and photocathode generate under the conditions of light irradiates, double optoelectronic pole drivings are constituted
Light help fuel cell system, form current path, produce electricl energy.
3. self energizing sensor is for detecting Microcystin
Fuel cell is helped to be used for the detection of Microcystin light constructed by step 2, when introducing microcystin in system
When plain, Microcystin consumes the hole of photoanode surface, it is suppressed that the recombination of light induced electron and hole, to enhance whole
The output of a self energizing system electric energy.When the concentration of Microcystin gradually increases, the output of electric energy is also gradually increased, thus
The corresponding relationship between Microcystins Concentration and electric power signal intensity is established, self energizing method Sensitive Detection microcystin is drawn
The standard curve of element.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention.It is all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (6)
1. a kind of for detecting the self energizing sensor of Microcystin, including light sun pole ﹑ light yin pole ﹑ simulated solar radiant ﹑
Electricity solves matter Rong Ye ﹑ quartz reaction Chi ﹑ air vent and Microcystin normal concentration solution；The light anode and photocathode are inserted
Enter the quartz reaction pond of electrolyte solution is housed, and be connected to by external circuit, wherein photocathode is close to air vent；It is described
Light source irradiates light anode and photocathode simultaneously；It is characterized in that, the electrolyte solution is the phosphate-buffered of pH=4~6
Under the driving for the automatic bias that solution, the light anode and photocathode generate under the conditions of light irradiates, constructed double optoelectronic poles are driven
Dynamic light helps fuel cell system, forms current path, produces electricl energy.
2. according to claim 1 for detecting the self energizing sensor of Microcystin, which is characterized in that the light
Anode is TiO2The indium-tin oxide electrode of modification；The photocathode is the ITO electrode of NG-BiOBr modification.
3. according to claim 2 for detecting the self energizing sensor of Microcystin, which is characterized in that the light sun
Pole nano material TiO2It is prepared using hydro-thermal method, comprising:
By butyl titanate [TiO (C4H9O)4] it is dissolved in HNO3Titanyl nitrate [TiO (NO is obtained in solution3)2] solution；
By TiO (NO3)2Solution is transferred in the reaction kettle that polytetrafluoroethylene (PTFE) is back boxing, is reacted at 160~200 DEG C, natural cooling
By centrifugation, ultrapure water and dehydrated alcohol carrying out washing treatment reaction product；
It is dry under the conditions of placing it in 60 DEG C, obtain light anode nano material TiO2。
4. according to claim 3 for detecting the self energizing sensor of Microcystin, which is characterized in that the HNO3
The concentration of solution is 6mol/L；The HNO3With TiO (C4H9O)4Dosage volume ratio be 5~10:1.
5. according to claim 2 for detecting the self energizing sensor of Microcystin, which is characterized in that photocathode is received
Rice material NG-BiOBr is prepared using hydro-thermal method, comprising:
By five nitric hydrate bismuth (Bi (NO3)3·5H2O it) is dissolved in ultrapure water, with dilute HNO3Its pH value is adjusted to 3 by solution, spare；
It is uniform that ultrasonic mixing in cetyl trimethylammonium bromide (CTAB) solution is dispersed by azepine graphene (NG)；
By aforementioned Bi (NO3)3·5H2The acid solution of O is slowly dropped into NG and CTAB mixed solution, and above-mentioned mixed liquor is transferred to circle
It is reacted in the flask of bottom in 60~120 DEG C of oil baths；
After the reaction was completed, dry by the sediment ethyl alcohol and milli-Q water of preparation, obtain NG-BiOBr nanometers of materials of photocathode
Material.
6. according to claim 5 for detecting the self energizing sensor of Microcystin, which is characterized in that wherein, institute
With the volumetric usage of solvent ultrapure water are as follows: every 0.12g Bi (NO3)3·5H2The amount of O solvent for use ultrapure water is 50mL, described
The concentration of CTAB solution is 8 × 10-3mol/L；The CTAB and Bi (NO3)3·5H2The molar ratio of O is 1:1, the NG and Bi
(NO3)3·5H2O mass ratio are as follows: 0.8~4.5mg:0.12g, the ultrasonic mixing time are 0.5h.
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| CN112382510A (en) * | 2020-10-23 | 2021-02-19 | 华中科技大学 | Near-infrared light catalytic electrode, preparation method and application |
| CN112461905A (en) * | 2020-10-19 | 2021-03-09 | 江苏大学 | Construction method of novel photo-assisted bipolar self-powered adapter sensor |
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| CN114527176A (en) * | 2022-02-18 | 2022-05-24 | 常州大学 | Construction method of photoelectrochemical self-powered sensor for sensitive detection of microcystin |
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