CN105651836A - Self-driven all-solid-state glucose biosensor and preparation method thereof - Google Patents
Self-driven all-solid-state glucose biosensor and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a self-driven all-solid-state glucose biosensor and a preparation method thereof. According to the self-driven all-solid-state glucose biosensor and the preparation method thereof, self-driven glucose concentration detection is realized, glucose concentration can be detected under the illumination and non-illumination conditions, the linear detection range reaches 2-40 mM, and glucose concentration detection requirements of a normal human body (with the linear detection range of 3.61-6.11 mM) and a diabetic patient; light conversion, light storage and biosensing are integrated to one device, a new field is developed for miniaturization and portability of the biosensor, and the biosensor is assembled by adopting a Sn<2+> doped SnO2 nanosheet array as a photoresponse electrode and adopting a rhombic NiCo2O4 nanorod array as an electrochemical energy storage electrode through a Celgard 2400 diaphragm and a PVA/KOH solid electrolyte.
Description
(1) technical field
The present invention relates to a kind of based on SnO2/NiCo2O4Self-driven all solid state glucose biological sensor and preparation method thereof.
(2) background technology
After human society enters modern civilization, along with the raising day by day of people's living standard, diabetes this kind of " affluenza " begin in worldwide and without restraint spread, and have about 400,000,000 people to suffer the puzzlement of diabetes every year. Therefore, the daily monitoring of diabetes becomes a urgent problem. In order to facilitate routine use, it is necessary to what become by its core component-glucose sensor is small-sized, portable. And existing a lot of glucose sensors typically require an external power supply to provide energy, virtually add the volume of sensor. The miniaturization that self-driven biosensor is then sensor opens new direction.
Solar energy is as the energy inexhaustible on the earth, it is possible to provide good energy source for biosensor. Sn2+The SnO of doping2Nano-chip arrays is a kind of well light sensitive material, it is possible to realize the detection of glucose under sunlight drives. The NiCo of rhombus simultaneously2O4Nanometer stick array is then excellent electrochemical energy storage material, it is possible to by SnO2The solar energy converted stores as electrochemical energy, and under non-illuminated conditions, glucose is detected. This integrated solar converts, energy stores and the biosensor of glucose detection can when without external power supply, realize the blood sugar concentration detection under illumination and non-illuminated conditions, it is also beneficial to carry after biosensor being assembled into full solid-state device, it is possible to really realize the day diabetes management of patient simultaneously.
There is presently no based on SnO2/NiCo2O4The relevant report of self-driven all solid state glucose biological sensor.
(3) summary of the invention
It is an object of the present invention to provide a kind of based on SnO2/NiCo2O4Self-driven all solid state glucose biological sensor and preparation method thereof, it is possible to when without external power supply, it is achieved the blood sugar concentration detection under illumination and non-illuminated conditions.
The technical solution used in the present invention is:
A kind of self-driven all solid state glucose biological sensor, described biosensor is with Sn2+The SnO of doping2Nano-chip arrays is as photoresponse electrode, with rhombus NiCo2O4Nanometer stick array, as electrochemical energy storage electrode, utilizes Celgard2400 diaphragm and PVA/KOH solid electrolyte to assemble.Biosensor, under simulated solar optical mode, measures the photocurrent response of device under different concentration of glucose; Without, under illumination mode, measuring the device fully charged under illumination open circuit voltage variations under different concentration of glucose.
Described photoresponse electrode is prepared as follows: by amount of substance than NaF and the SnCl being 3��4.5:12It is dissolved in deionized water, obtain precursor solution to transfer in water heating kettle inner bag, and put into clean FTO (electro-conductive glass) substrate, after water heating kettle is put into 180��200 DEG C of calorstat insulation 20��24h, taking out FTO substrate cleaning-drying, obtaining growth has Sn2+The SnO of doping2The FTO substrate of nano-chip arrays, i.e. photoresponse electrode.
Described electrochemical energy storage electrode is prepared as follows: by amount of substance than the Ni (NO for 1:2:4��8:4��83)2��6H2O��Co(NO3)2��6H2O��NH4F��C6H12N4It is dissolved in deionized water, obtains precursor solution and transfer in water heating kettle inner bag, and put into clean FTO substrate, after water heating kettle is put into 100��120 DEG C of calorstat insulation 24��28h, taking out FTO substrate cleaning-drying, in atmosphere 200��350 DEG C of annealing 3h, obtaining growth has rhombus NiCo2O4The FTO substrate of nanometer stick array, i.e. electrochemical energy storage electrode.
The invention still further relates to a kind of method preparing described self-driven all solid state glucose biological sensor, described method includes:
(1) FTO substrate is cut into 1��3cm �� 2cm size, successively with acetone, ethanol, deionized water ultrasonic cleaning 5��10min, drying for standby;
(2) by amount of substance than NaF and the SnCl being 3��4.5:12Being dissolved in deionized water, obtain precursor solution and transfer in water heating kettle inner bag, and put into clean FTO substrate, after water heating kettle is put into 180��200 DEG C of calorstat insulation 20��24h, take out FTO substrate cleaning-drying, obtaining growth has Sn2+The SnO of doping2The FTO substrate of nano-chip arrays, i.e. photoresponse electrode material;
(3) by amount of substance than the Ni (NO for 1:2:4��8:4��83)2��6H2O��Co(NO3)2��6H2O��NH4F��C6H12N4It is dissolved in deionized water, obtains precursor solution and transfer in water heating kettle inner bag, and put into clean FTO substrate, after water heating kettle is put into 100��120 DEG C of calorstat insulation 24��28h, taking out FTO substrate cleaning-drying, in atmosphere 200��350 DEG C of annealing 3h, obtaining growth has rhombus NiCo2O4The FTO substrate of nanometer stick array, i.e. electrochemical energy storage electrode material;
(4) polyvinyl alcohol and KOH are dissolved in deionized water, 90 DEG C of stirring 6h, be configured to PVA mass fraction be 6��10%, the PVA/KOH solid electrolyte of KOH molar concentration 1mol/L;
(5) step (2) gained photoresponse electrode and step (3) gained electrochemical energy storage electrode and Celgard2400 diaphragm are immersed into 5��10min in step (4) gained PVA/KOH solid electrolyte respectively, then this three part is assembled into device, and draw wire, dry at 60��65 DEG C, remove moisture in PVA/KOH electrolyte, namely obtain all solid state glucose biological sensor of described driving.
The present invention utilizes hydro-thermal method to prepare SnO respectively2/ FTO photoresponse electrode part and NiCo2O4/ FTO electrochemical energy storage electrode part, and utilize Celgard2400 diaphragm and PVA/KOH solid electrolyte to assemble them into full solid-state device, this device is integrated with light conversion, optical storage and three kinds of functions of bio-sensing.
The present invention prepares all solid state biosensor and can work under illumination and non-illuminated conditions: under light illumination, SnO2Can quickly convert solar energy into photo-signal, immerse the device in the glucose solution of variable concentrations, different size of photoelectric current can be produced, such that it is able to realize the detection to concentration of glucose, whole detection process drives without additional power source, simultaneously NiCo under illumination condition2O4Solar energy can be stored with the form of electrochemical energy;Under non-illuminated conditions, glucose is by NiCo2O4The electrochemical energy catalysis of electrode storage, utilizes the equally possible detection realizing concentration of glucose of change of open-circuit voltage.
The beneficial effects are mainly as follows: present invention achieves self-driven concentration of glucose detection, under illumination and non-illuminated conditions, concentration of glucose can be detected, linear probing ranges up to 2��40mM, it is possible to meet the blood sugar concentration detection demand of normal human (3.61��6.11mM) and diabetics. The present invention converts light into, and optical storage and three kinds of functions of bio-sensing are integrated on a device, for the open new world of the miniaturization of biosensing device and portability.
(4) accompanying drawing explanation
Fig. 1 is the Sn that embodiment 1 prepares gained2+The SnO of doping2The electron scanning micrograph of nano-chip arrays;
Fig. 2 is the rhombus NiCo that embodiment 1 prepares gained2O4The electron scanning micrograph of nanometer stick array;
Fig. 3 is that embodiment 1 prepares gained SnO2And NiCo2O4XRD figure spectrum;
Fig. 4 is the photoresponse figure that embodiment 1 prepares the self-driven all solid state biosensor of gained;
Fig. 5 is the transverse electric stream charge and discharge electrograph that embodiment 1 prepares the self-driven all solid state biosensor of gained;
Fig. 6 is the photoresponse result that embodiment 1 prepares the self-driven all solid state biosensor of gained different concentration of glucose under light illumination;
Fig. 7 is that embodiment 1 prepares the self-driven all solid state biosensor of gained under non-illuminated conditions, the open circuit voltage variations result of different concentration of glucose;
Fig. 8 is that embodiment 1 prepares gained self-driven all solid state biosensor anti-interference experimental result under illumination and non-illuminated conditions, and chaff interference is lactose respectively, ascorbic acid, sucrose;
Fig. 9 is the structural representation preparing full solid-state device.
(5) detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described further, but protection scope of the present invention is not limited to that:
Embodiment 1:
1) FTO substrate is cut into 1cm �� 2cm size, respectively successively by acetone, ethanol, deionized water ultrasonic cleaning 10min, then drying for standby;
2) by 8.55mmNaF and 2.85mmSnCl2Being dissolved in 30ml deionized water, obtain precursor liquid and transfer in 50ml water heating kettle inner bag, and put into the FTO substrate of step (1) gained, after water heating kettle is put into 180 DEG C of calorstat insulation 20h, take out cleaning-drying, obtaining growth has Sn2+The SnO of doping2The FTO substrate of nano-chip arrays, referring to Fig. 1;
3) by 2mmNi (NO3)2��6H2O��4mmCo(NO3)2��6H2O��16mmNH4F��8mmC6H12N4It is dissolved in 40ml deionized water, obtain precursor liquid and transfer in 50ml water heating kettle inner bag, and put into the FTO substrate of step (1) gained, after water heating kettle is put into 100 DEG C of calorstat insulation 24h, take out FTO substrate cleaning-drying, 350 DEG C of annealing 3h in atmosphere, obtaining growth has rhombus NiCo2O4The FTO substrate of nanometer stick array, referring to Fig. 2; Gained SnO2And NiCo2O4XRD figure compose referring to Fig. 3;
4) 10gPVA and 5.6gKOH is dissolved in 100ml deionized water, 90 DEG C of stirring 6h, it is configured to required PVA/KOH solid electrolyte;
5) by step (2) gained SnO2/ FTO substrate and step (3) gained NiCo2O4/ FTO substrate and barrier film (Celgard2400) are immersed into 5min in step (4) gained PVA/KOH solid electrolyte respectively, then take out, this three part is assembled into device (structural representation is referring to Fig. 9), and draw wire, dry 12h at 60 DEG C, remove moisture in PVA/KOH electrolyte, namely obtain all solid state glucose biological sensor of described driving;
6) by the SnO of all solid state glucose biological sensor of step (5) gained2/ FTO is as working electrode, NiCo2O4/ FTO is as to electrode and reference electrode, being connected on CHI760 electrochemical workstation, and is immersed in by senser element in 0.1MKOH solution;
7) with 500W arc xenon lamp simulated solar irradiation, the senser element that measuring process (6) connects adds the photocurrent response before and after glucose, and referring to Fig. 4, as seen from the figure, after adding glucose sugar, photoelectric current is obviously reduced;
8) senser element that measuring process (6) connects charge-discharge performance under different constant currents, referring to Fig. 5, figure obtaining changing the device electric capacity when 1A/g according to formula calculating is 180F/g;
9) when there is no applying bias, the senser element that measuring process (6) connects is under light illumination, change to the photoresponse electric current of different concentration of glucose, each concentration of glucose be changed to 2mM, referring to Fig. 6, as seen from the figure, along with concentration of glucose increases, photoelectric current linearly reduces;
10) senser element step (6) connected is fully charged under light illumination, transfer under non-illuminated conditions, measure the response to different concentration of glucose of its open-circuit voltage, each concentration of glucose is changed to 2mM, referring to Fig. 7, as seen from the figure, along with concentration of glucose increases, open-circuit voltage size linearly reduces;
11) under illumination and non-illuminated conditions, the senser element that comparison step (6) connects is to lactose, ascorbic acid, the capacity of resisting disturbance of sucrose, it is all 2mM that three kinds of chaff interferences add concentration, referring to Fig. 8, as seen from the figure, preparing obtained device to lactose, ascorbic acid, three kinds of chaff interferences of sucrose have good capacity of resisting disturbance.
Embodiment 2:
1) FTO substrate is cut into 1cm �� 2cm size, respectively successively by acetone, ethanol, deionized water ultrasonic cleaning 10min, then drying for standby;
2) by 8.55mmNaF and 2.85mmSnCl2Being dissolved in 30ml deionized water, obtain precursor liquid and transfer in 50ml water heating kettle inner bag, and put into the FTO substrate of step (1) gained, after water heating kettle is put into 180 DEG C of calorstat insulation 20h, take out cleaning-drying, obtaining growth has Sn2+The SnO of doping2The FTO substrate of nano-chip arrays;
3) by 2mmNi (NO3)2��6H2O��4mmCo(NO3)2��6H2O��8mmNH4F��8mmC6H12N4It is dissolved in 40ml deionized water, obtains precursor liquid and transfer in 50ml water heating kettle inner bag, and put into the FTO substrate of step (1) gained, after water heating kettle is put into 100 DEG C of calorstat insulation 24h, taking out FTO substrate cleaning-drying, 250 DEG C of annealing 3h, are given birth in atmosphere
Long have rhombus NiCo2O4The FTO substrate of nanometer stick array;
4) 8gPVA and 5.6gKOH is dissolved in 100ml deionized water, 90 DEG C of stirring 6h, it is configured to required PVA/KOH solid electrolyte;
5) by step (2) gained SnO2/ FTO substrate and step (3) gained NiCo2O4/ FTO substrate and barrier film (Celgard2400) are immersed into 5min in step (4) gained PVA/KOH solid electrolyte respectively, then take out, this three part is assembled into device, and draw wire, dry 12h at 60 DEG C, remove moisture in PVA/KOH electrolyte, namely obtain all solid state glucose biological sensor of described driving;
6) by the SnO of all solid state biosensor of step (5) gained2/ FTO is as working electrode, NiCo2O4/ FTO, as to electrode and reference electrode, being connected on CHI760 electrochemical workstation, immerses the device in 0.1MKOH solution;
7) with 500W arc xenon lamp simulated solar irradiation, the senser element that measuring process (6) connects adds the photocurrent response before and after glucose, and result shows, after adding glucose sugar, photoelectric current is obviously reduced;
8) senser element that measuring process (6) connects charge-discharge performance under different constant currents;
9) when there is no applying bias, the senser element that measuring process (6) connects under light illumination, the change to the photoresponse electric current of different concentration of glucose, each concentration of glucose be changed to 2mM, result shows, along with concentration of glucose increases, photoelectric current linearly reduces;
10) senser element step (6) connected is fully charged under light illumination, transfer under non-illuminated conditions, measure the response to different concentration of glucose of its open-circuit voltage, each concentration of glucose is changed to 2mM, result shows, along with concentration of glucose increases, open-circuit voltage size linearly reduces;
11) under illumination and dark condition, the senser element that comparison step (6) connects is to lactose, ascorbic acid, the capacity of resisting disturbance of sucrose, it is all 2mM that three kinds of chaff interferences add concentration, and result shows, prepares obtained device to lactose, ascorbic acid, three kinds of chaff interferences of sucrose have good capacity of resisting disturbance.
To sum up, biosensor of the present invention achieves self-driven concentration of glucose detection, under illumination and non-illuminated conditions, can concentration of glucose be detected, linear probing ranges up to 2��40mM, it is possible to meet the blood sugar concentration detection demand of normal human and diabetics.
Claims (4)
1. one kind based on SnO2/NiCo2O4Self-driven all solid state glucose biological sensor, described biosensor is with Sn2+The SnO of doping2Nano-chip arrays is as photoresponse electrode, with rhombus NiCo2O4Nanometer stick array, as electrochemical energy storage electrode, utilizes Celgard2400 diaphragm and PVA/KOH solid electrolyte to assemble.
2. biosensor as claimed in claim 1, it is characterised in that described photoresponse electrode is prepared as follows: by amount of substance than NaF and the SnCl being 3��4.5:12Being dissolved in deionized water, obtain precursor solution and transfer in water heating kettle inner bag, and put into clean FTO substrate, after water heating kettle is put into 180��200 DEG C of calorstat insulation 20��24h, take out FTO substrate cleaning-drying, obtaining growth has Sn2+The SnO of doping2The FTO substrate of nano-chip arrays, i.e. photoresponse electrode.
3. biosensor as claimed in claim 1, it is characterised in that described electrochemical energy storage electrode is prepared as follows: by amount of substance than the Ni (NO for 1:2:4��8:4��83)2��6H2O��Co(NO3)2��6H2O��NH4F��C6H12N4It is dissolved in deionized water, obtains precursor solution and transfer in water heating kettle inner bag, and put into clean FTO substrate, after water heating kettle is put into 100��120 DEG C of calorstat insulation 24��28h, taking out FTO substrate cleaning-drying, in atmosphere 200��350 DEG C of annealing 3h, obtaining growth has rhombus NiCo2O4The FTO substrate of nanometer stick array, i.e. electrochemical energy storage electrode.
4. preparing a method for self-driven all solid state glucose biological sensor described in claim 1, described method includes:
(1) FTO substrate is cut into 1��3cm �� 2cm size, successively with acetone, ethanol, deionized water ultrasonic cleaning 5��10min, drying for standby;
(2) by amount of substance than NaF and the SnCl being 3��4.5:12Being dissolved in deionized water, obtain precursor solution and transfer in water heating kettle inner bag, and put into clean FTO substrate, after water heating kettle is put into 180��200 DEG C of calorstat insulation 20��24h, take out FTO substrate cleaning-drying, obtaining growth has Sn2+The SnO of doping2The FTO substrate of nano-chip arrays, i.e. photoresponse electrode material;
(3) by amount of substance than the Ni (NO for 1:2:4��8:4��83)2��6H2O��Co(NO3)2��6H2O��NH4F��C6H12N4It is dissolved in deionized water, obtains precursor solution and transfer in water heating kettle inner bag, and put into clean FTO substrate, after water heating kettle is put into 100��120 DEG C of calorstat insulation 24��28h, taking out FTO substrate cleaning-drying, in atmosphere 200��350 DEG C of annealing 3h, obtaining growth has rhombus NiCo2O4The FTO substrate of nanometer stick array, i.e. electrochemical energy storage electrode material;
(4) polyvinyl alcohol and KOH are dissolved in deionized water, 90 DEG C of stirring 6h, be configured to PVA mass fraction be 6��10%, the PVA/KOH solid electrolyte of KOH molar concentration 1mol/L;
(5) step (2) gained photoresponse electrode and step (3) gained electrochemical energy storage electrode and Celgard2400 diaphragm are immersed into 5��10min in step (4) gained PVA/KOH solid electrolyte respectively, then this three part is assembled into device, dry at 60��65 DEG C, remove moisture in PVA/KOH electrolyte, namely obtain all solid state glucose biological sensor of described driving.
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| CN106525933A (en) * | 2016-11-03 | 2017-03-22 | 天津大学 | Method for producing polypyrrole-coated nickel cobaltate nano wire array graphene electrode and application of graphene electrode for detecting heavy metallic lead ion |
| CN106770547A (en) * | 2016-12-07 | 2017-05-31 | 海南大学 | A kind of synthetic method of cobalt acid nickel hollow ball non-enzymatic biological sensor sensing material |
| CN109580738A (en) * | 2018-11-13 | 2019-04-05 | 云南大学 | A kind of preparation method of non-enzymatic glucose electrolytic catalysis material |
| CN109772334A (en) * | 2018-12-28 | 2019-05-21 | 宁夏大学 | A kind of big mesoporous nickel cobalt glucose-sensitive material of high-specific surface area and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106770547A (en) * | 2016-12-07 | 2017-05-31 | 海南大学 | A kind of synthetic method of cobalt acid nickel hollow ball non-enzymatic biological sensor sensing material |
| CN109580738A (en) * | 2018-11-13 | 2019-04-05 | 云南大学 | A kind of preparation method of non-enzymatic glucose electrolytic catalysis material |
| CN109772334A (en) * | 2018-12-28 | 2019-05-21 | 宁夏大学 | A kind of big mesoporous nickel cobalt glucose-sensitive material of high-specific surface area and preparation method thereof |
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| CN105651836B (en) | 2018-06-19 |
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