CN103344688A - Working electrode for cylindrical array cross-scale glucose sensor and preparation method of working electrode - Google Patents
Working electrode for cylindrical array cross-scale glucose sensor and preparation method of working electrode Download PDFInfo
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- CN103344688A CN103344688A CN2013102514293A CN201310251429A CN103344688A CN 103344688 A CN103344688 A CN 103344688A CN 2013102514293 A CN2013102514293 A CN 2013102514293A CN 201310251429 A CN201310251429 A CN 201310251429A CN 103344688 A CN103344688 A CN 103344688A
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Abstract
The invention relates to a working electrode for a cylindrical array cross-scale glucose sensor and a preparation method of the working electrode. A covering of a common multi-mode optical fiber is removed, an optical fiber core is pulled out, and an Au (gold) membrane is deposited on the surface of the optical fiber core on the basis of a magnetic control sputtering technique; a plurality of optical fiber cores which are deposited with the Au membrane are closely arranged on a glass substrate and fixed by silver powder conductive glue to form an electrode substrate with the micrometer-scale cylindrical array structure; a ZnO (zinc oxide) nano wire is grown on an optical fiber core array which is deposited with the Au membrane based on a water bath method to form a nano-scale surface in a cylindrical array cross-scale structure and to be used for increasing the adsorption area of GOD, so that the catalytic efficiency of the working electrode for the cross-scale glucose sensor based on a tri-electrode system can be greatly improved.
Description
Technical field
The invention belongs to the micro sensing technical field, be mainly used in fields such as galvanochemistry, biology, medical science, food processing, environmental monitoring, particularly a kind of cylindrical-array shape for blood of human body and the detection of urine concentration of glucose is striden yardstick glucose sensor working electrode and preparation method thereof.
Background technology
In fields such as galvanochemistry, biology, medical science, food processing, environmental monitorings, to concentration of glucose carry out accurately, fast and on-line measurement have a very important role.At present the enzymatic type glucose sensor based on three-electrode system is just receiving increasing concern, and its core mainly is working electrode, comprises GOD, fixing host material and the basal electrode used of GOD; Used measuring method is chronoamperometry or potential method.The ZnO nano wire has that specific surface area is big, isoelectric point is high (IEP～9.5ev), electron mobility height, advantage such as toxicity is low, bio-compatibility good, Heat stability is good, oxidation resistance are strong, with it as host material, not only can adsorb the lower GOD(IEP of isoelectric point～4.2ev) effectively, can promote on a large scale that also the electronics between GOD and the basal electrode shifts.For sensitivity, response speed, the serviceable life of improving enzymatic type glucose sensor, reduce its minimum detectability, prevent coming off and loss of GOD, need to improve the structure of basal electrode and host material, further improve its adsorption area, finally realize the reliable absorption of GOD.
At present mainly contain planar shaped and cylindrical two big classes based on the glucose sensor of striding the yardstick structure with working electrode.The micron order electrode basement that planar shaped is striden yardstick arrangement works electrode comprises that mainly sputter has Si substrate, ITO electro-conductive glass of Au film etc., and there are ZnO nano wire (or nanosphere, nanometer sheet, nano-comb) and Au, Ag nano wire etc. in the nanoscale surface.For example the people such as Liu Xiaowang of Anhui Normal University have deposited the ZnO nano wire film based on thermal decomposition method on ito glass, obtain planar shaped and stride the yardstick structure and be used for the absorption of GOD and fixing, finally prepared the glucose sensor based on chronoamperometry.Cylindrical micron order electrode basement of striding the yardstick structure comprises bonding Au silk, Ag silk, Pt silk, Au-W alloy silk, carbon fiber etc., and there are ZnO nano wire (or nanosphere, nanometer sheet, nano-comb) and Au, Ag nano wire etc. in the nanoscale surface.For example the people such as S.M.U.Ali of Sweden Linkoping university have synthesized the ZnO nano wire film based on immersion method on the Ag silk of φ 250 μ m, obtain the cylindrical yardstick structure of striding, be used for the absorption of GOD and fixing, finally prepared the glucose sensor based on potential method.
The yardstick glucose sensor of striding mentioned in the above-mentioned research does not relate to cylindrical-array shape structure with working electrode.Stride the yardstick structure with planar shaped and compare, the electrode area that cylindrical-array shape is striden the yardstick structure has increased about 3.1 times, has therefore improved the minimum detectability that detects current's intensity, reduced such sensor.
Summary of the invention
The object of the present invention is to provide a kind of cylindrical-array shape to stride yardstick glucose sensor working electrode and preparation method thereof, by the glucose sensor working electrode that preparation method of the present invention makes, its catalytic efficiency height, response speed be fast, low to the detection limit of glucose, signal to noise ratio (S/N ratio) is high, yardstick is little, require lower, with low cost to manufacturing equipment.
For achieving the above object, cylindrical-array shape of the present invention is striden yardstick glucose sensor working electrode, comprise that glass substrate and an end are fixed on the glass substrate with sliver-powder conducting glue, the other end is the unsettled fiber array of being made up of fiber core outside the glass substrate edge, deposit the Au film at fiber core, in the growth of Au film the ZnO nano wire is arranged, be fixed on the GOD on the ZnO nano wire.
The length of described glass substrate is that 30mm, width are that 30mm, thickness are 1.5mm.
The length of described fiber core is 40mm, and diameter is φ 125 μ m, unsettled 20mm outside the glass substrate edge.
The thickness of described Au film is 300nm.
Described ZnO nano wire is the regular hexagon structure, adopts immersion method to be grown on the Au film, and its length is 1～2 μ m, and the regular hexagon diameter is φ 0.1～0.3 μ m.
Described GOD vigor is 40U/mg.
A kind of cylindrical-array shape is striden the preparation method that the yardstick glucose sensor is used working electrode, may further comprise the steps:
1) getting some fiber cores, is the Au film of 300nm on the fiber core surface based on the magnetron sputtering technique deposit thickness;
2) based on standard cleaning technology glass substrate is cleaned, wherein the long 30mm of glass substrate, wide 30mm, thickness are 1.5mm;
3) fiber core that will deposit the Au film closely is arranged on the cleaned glass substrate with array way, form cylindrical-array shape assembly, wherein cylindrical-array shape assembly one end is bonded on the glass substrate with sliver-powder conducting glue, the other end is unsettled 20mm outside the glass substrate edge, at room temperature dry fixing laggard column criterion clean cylindrical-array shape fiber core assembly;
4) compound concentration is the ZnO nano wire Seed Layer solution of 1mmol/L;
5) the cylindrical-array shape fiber core assembly overhanging portion that will deposit the Au film immerses ZnO nano wire Seed Layer solution, obtains ZnO nano wire Seed Layer on Au film surface;
6) the cylindrical-array shape assembly that will deposit ZnO nano wire Seed Layer places 150 ℃ vacuum drier to finish annealing in process;
7) compound concentration is the ZnO nano wire growth-promoting media of 0.025mol/L;
8) the cylindrical-array shape structure overhanging portion that will deposit Seed Layer immerses in the ZnO nano wire growth-promoting media, based on hydro-thermal method under 90 ℃ on cylindrical-array shape assembly growing ZnO nano-wire, obtain cylindrical-array shape and stride the yardstick structure;
9) the ultrasonic cleaning growth has the cylindrical-array shape of ZnO nano wire to stride the yardstick structure, and at room temperature dry;
10) compound concentration is that 0.01mol/L, pH are 7.4 PBS solution;
11) be that the GOD of 40U/mg joins in the above-mentioned PBS solution with vigor, preparation GOD concentration is the GOD solution of 40mg/mL;
12) growth there is the cylindrical-array shape of ZnO nano wire stride yardstick structure overhanging portion and immerses in the GOD solution, keep taking out behind the 15min, and at room temperature dry, obtain one deck and be fixed on the GOD that is used for catalytic action on the ZnO nano wire.
Described fiber core adopts multimode optical fiber, peels off its covering after soaking with acetone, and extracting diameter out is the multimode optical fiber fibre core of φ 125 μ m, and clip length is the fiber core of 40mm, carries out standard cleaning then.
The present invention utilizes mechanical assembly technology that the cylindrical fiber fibre core that deposits the Au film is assembled, and obtains micron-sized cylindrical-array shape structure, and method is simple, strong operability, cost are low, and can not obtain such array structure with conventional Micrometer-Nanometer Processing Technology.At last, with planar shaped, the cylindrical yardstick structure of striding, and rectangle and triangular array are striden the yardstick structure and are compared, cylindrical-array shape is striden the yardstick structure and is had unique wettability, can improve GOD adsorption effect thereon effectively, and then make cylindrical-array shape stride the sensitivity of yardstick glucose sensor, the linearity, Michaelis constant to be significantly improved.
The present invention strides the yardstick structure with cylindrical-array shape and introduces glucose sensor with in the design of working electrode, and its distinguishing feature comprises following three aspects:
1) the some multimode optical fiber fibre cores that deposit the Au film is closely arranged, formed micron-sized cylindrical-array shape electrode basement, thereby the planar substrates basal electrode is converted to cylindrical-array shape, enlarged markedly the area of basal electrode.
2) adopt immersion method depositing growing ZnO nano-wire on the cylindrical-array shape basal electrode of Au film, form micro-nano cylindrical-array shape and stride the yardstick structure, not only further increased the adsorption area of GOD, utilized ZnO nano wire excellent physical chemistry, also improve the wettability of striding the yardstick working electrode, made the catalytic efficiency of glucose sensor, detection sensitivity all significantly improve.
3) utilize mechanical assembly technology that the cylindrical fiber fibre core that deposits the Au film is assembled, obtain micron-sized cylindrical-array shape structure, method is simple, strong operability, cost are low; Because the fiber core yardstick is little, also be convenient to the microminiaturization of such glucose sensor in addition.
The invention has the beneficial effects as follows, the fiber core that deposits the Au film closely is arranged in formation cylindrical array basal electrode on the glass substrate, not only obtain the base electrode structure that Micrometer-Nanometer Processing Technology is difficult for processing, and enlarged markedly the area of basal electrode; Secondly be suspended on the cylindrical-array shape assembly Au film superficial growth ZnO nano wire of glass substrate outer rim based on immersion method, form cylindrical-array shape and stride the yardstick structure, further increase the adsorption area of GOD, the wettability that the yardstick structure is striden in improvement, the catalytic efficiency that improves GOD; At last, the multimode optical fiber fibre core that utilizes mechanical assembly method will deposit the Au film closely is arranged on the glass substrate, and method is simple, operation shape is strong, cost is low, but also is convenient to the microminiaturization of this glucose sensor.
The prepared cylindrical-array shape of this invention is striden yardstick glucose sensor working electrode, not only can be applicable to the detection of concentration of glucose in the blood of human body and urine in the medical science, and in fields such as biology, food processing, galvanochemistry, environmental monitoring, significant application prospect is also arranged.
Description of drawings
Fig. 1 is front view of the present invention;
Fig. 2 is the cut-open view of Fig. 1.
Embodiment
The present invention is described in further detail below in conjunction with accompanying drawing and case study on implementation:
Referring to Fig. 1,2, the present invention includes length is 30mm, width is 30mm, thickness is that 1.5mm glass substrate 1 and an end are fixed on the glass substrate 1 with sliver-powder conducting glue 2, the fiber array of being formed by fiber core 3 of the other end unsettled 20mm outside glass substrate 1 edge, the length of described fiber core 3 is 40mm, diameter is φ 125 μ m, deposit the Au film 4 that thickness is 300nm at fiber core 3, in the growth of Au film ZnO nano wire 5 is arranged, described ZnO nano wire 5 is the regular hexagon structure, adopt immersion method to be grown on the Au film 4, its length is 1～2 μ m, the regular hexagon diameter is φ 0.1～0.3 μ m, and vigor is also fixedly arranged on ZnO nano wire 5 is the GOD6 of 40U/mg.
Referring to Fig. 1,2, preparation method of the present invention may further comprise the steps:
1) gets one of multimode optical fiber, with peelling off its covering after the acetone immersion, extracting diameter out is the multimode optical fiber fibre core 3 of φ 125 μ m, clip length is some sections of the fiber cores of 40mm, carry out standard cleaning then: use acetone, deionized water, absolute ethyl alcohol, deionized water ultrasonic cleaning 5min, 2min, 2min, 2min successively, then 100 ℃ of down oven dry, be the Au film 4 of 300nm on fiber core 3 surfaces based on the magnetron sputtering technique deposit thickness;
2) based on standard cleaning technology glass substrate 1 is cleaned: use acetone, deionized water, absolute ethyl alcohol, deionized water ultrasonic cleaning 5min, 2min, 2min, 2min successively, 100 ℃ of oven dry down, wherein the long 30mm of glass substrate, wide 30mm, thickness are 1.5mm then;
3) fiber core 3 that will deposit Au film 4 closely is arranged on the cleaned glass substrate 1 with array way, form cylindrical-array shape assembly, wherein cylindrical-array shape assembly one end is bonded on the glass substrate 1 with sliver-powder conducting glue 2, the other end is unsettled 20mm outside the glass substrate edge, at room temperature dry fixing laggard column criterion is cleaned: use acetone, deionized water, absolute ethyl alcohol, deionized water ultrasonic cleaning 5min, 2min, 2min, 2min successively, under 100 ℃, dry then cylindrical-array shape fiber core assembly;
4) compound concentration is the ZnO nano wire Seed Layer solution of 1mmol/L;
Get 0.06585g zinc acetate (C
4H
6O
4Zn2H
2O), put into the 50mL beaker, and add the 24mL absolute ethyl alcohol; Beaker is placed on the magnetic stirring apparatus, heats while stirring with the rotating speed of 200r/min, dissolve fully until zinc acetate, after naturally cool to room temperature; Take out the 4mL acetic acid zinc solution, add the 32mL absolute ethyl alcohol, seal the beaker mouth with preservative film, put into water-bath and get solution A in 65 ℃ of heating 5min;
Get 0.024g solid sodium hydroxide (NaOH), put into the 50mL beaker, add the 30mL absolute ethyl alcohol; Beaker is placed on the magnetic stirring apparatus, heats while stirring with the rotating speed of 200r/min, dissolve fully until NaOH, after naturally cool to room temperature; Get the 4mL sodium hydroxide solution, add the 10mL absolute ethyl alcohol, seal the beaker mouth with preservative film, put into water-bath and get solution B in 65 ℃ of heating 5min;
Solution A and solution B are mixed in another beaker, seal the beaker mouth with preservative film, put into water-bath in 65 ℃ of heating 30min; Naturally cool to room temperature after the taking-up, obtaining concentration is the ZnO nano wire Seed Layer solution of 1mmol/L;
5) the cylindrical-array shape fiber core assembly overhanging portion that will deposit Au film 4 immerses ZnO nano wire Seed Layer solution, keeps taking out behind the 2min, obtains Au film 4 lip-deep ZnO nano wire Seed Layer;
6) the cylindrical-array shape assembly that will deposit ZnO nano wire Seed Layer places 150 ℃ vacuum drier to finish annealing in process;
7) compound concentration is the ZnO nano wire growth-promoting media of 0.025mol/L;
Get 3.71g zinc nitrate (Zn (NO
3)
26H
2O), 1.75g hexamethylenetetramine (C
6H
12N
4) and put into same beaker, adding the 500mL deionized water, the rotating speed with 300r/min on magnetic stirring apparatus heats while stirring, and is heated to 90 ℃, and obtaining concentration is the ZnO nano wire growth-promoting media of 0.025mol/L;
8) the cylindrical-array shape structure overhanging portion that will deposit Seed Layer immerses in the ZnO nano wire growth-promoting media, based on hydro-thermal method under 90 ℃ on cylindrical-array shape assembly growing ZnO nano-wire 5, obtain cylindrical-array shape and stride the yardstick structure;
9) the ultrasonic cleaning growth has the cylindrical-array shape of ZnO nano wire 5 to stride the yardstick structure, and at room temperature dry;
10) compound concentration is that 0.01mol/L, pH are 7.4 PBS solution;
11) be that the GOD of 40U/mg joins in the above-mentioned PBS solution with vigor, preparation GOD concentration is the GOD solution of 40mg/mL;
13) growth there is the cylindrical-array shape of ZnO nano wire 5 stride yardstick structure overhanging portion and immerses in the GOD solution, keep taking out behind the 15min, and at room temperature dry, obtain one deck and be fixed on the GOD6 that is used for catalytic action on the ZnO nano wire 5.
Claims (8)
1. a cylindrical-array shape is striden yardstick glucose sensor working electrode, it is characterized in that: comprise that glass substrate (1) and an end are fixed on the glass substrate (1) with sliver-powder conducting glue (2), the other end is the unsettled fiber array of being made up of fiber core (3) outside glass substrate (1) edge, deposit Au film (4) at fiber core (3), in the growth of Au film ZnO nano wire (5) is arranged, be fixed on the GOD(6 on the ZnO nano wire (5)).
2. cylindrical-array shape according to claim 1 is striden yardstick glucose sensor working electrode, it is characterized in that: the length of described glass substrate (1) is that 30mm, width are that 30mm, thickness are 1.5mm.
3. cylindrical-array shape according to claim 1 is striden yardstick glucose sensor working electrode, it is characterized in that: the length of described fiber core (3) is 40mm, and diameter is φ 125 μ m, unsettled 20mm outside glass substrate (1) edge.
4. cylindrical-array shape according to claim 1 is striden yardstick glucose sensor working electrode, it is characterized in that: the thickness of described Au film (4) is 300nm.
5. cylindrical-array shape according to claim 1 is striden yardstick glucose sensor working electrode, it is characterized in that: described ZnO nano wire (5) is the regular hexagon structure, adopt immersion method to be grown on the Au film (4), its length is 1～2 μ m, and the regular hexagon diameter is φ 0.1～0.3 μ m.
6. cylindrical-array shape according to claim 1 is striden yardstick glucose sensor working electrode, it is characterized in that: described GOD vigor is 40U/mg.
7. a cylindrical-array shape is striden the preparation method that the yardstick glucose sensor is used working electrode, it is characterized in that may further comprise the steps:
1) getting some fiber cores (3), is the Au film (4) of 300nm on fiber core (3) surface based on the magnetron sputtering technique deposit thickness;
2) based on standard cleaning technology glass substrate (1) is cleaned, wherein the long 30mm of glass substrate, wide 30mm, thickness are 1.5mm;
3) fiber core (3) that will deposit Au film (4) closely is arranged on the cleaned glass substrate (1) with array way, form cylindrical-array shape assembly, wherein cylindrical-array shape assembly one end is bonded on the glass substrate (1) with sliver-powder conducting glue (2), the other end is unsettled 20mm outside the glass substrate edge, at room temperature dry fixing laggard column criterion clean cylindrical-array shape fiber core assembly;
4) compound concentration is the ZnO nano wire Seed Layer solution of 1mmol/L;
5) the cylindrical-array shape fiber core assembly overhanging portion that will deposit Au film (4) immerses ZnO nano wire Seed Layer solution, obtains ZnO nano wire Seed Layer on Au film (4) surface;
6) the cylindrical-array shape assembly that will deposit ZnO nano wire Seed Layer places 150 ℃ vacuum drier to finish annealing in process;
7) compound concentration is the ZnO nano wire growth-promoting media of 0.025mol/L;
8) the cylindrical-array shape structure overhanging portion that will deposit Seed Layer immerses in the ZnO nano wire growth-promoting media, based on hydro-thermal method under 90 ℃ on cylindrical-array shape assembly growing ZnO nano-wire (5), obtain cylindrical-array shape and stride the yardstick structure;
9) the ultrasonic cleaning growth has the cylindrical-array shape of ZnO nano wire to stride the yardstick structure, and at room temperature dry;
10) compound concentration is that 0.01mol/L, pH are 7.4 PBS solution;
11) be that the GOD of 40U/mg joins in the above-mentioned PBS solution with vigor, preparation GOD concentration is the GOD solution of 40mg/mL;
12) growth there is the cylindrical-array shape of ZnO nano wire stride yardstick structure overhanging portion and immerses in the GOD solution, keep taking out behind the 15min, and at room temperature dry, obtain one deck and be fixed on the GOD(6 that is used for catalytic action on the ZnO nano wire).
8. cylindrical-array shape according to claim 7 is striden the preparation method that the yardstick glucose sensor is used working electrode, it is characterized in that: described fiber core (3) adopts multimode optical fiber, with peelling off its covering after the acetone immersion, extracting diameter out is the multimode optical fiber fibre core (3) of φ 125 μ m, clip length is the fiber core of 40mm, carries out standard cleaning then.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103657565A (en) * | 2013-11-28 | 2014-03-26 | 西安交通大学 | Photo-catalytic reactor and preparation method thereof, based on three-dimensional cylindrical hierarchical structure array |
| CN104267464A (en) * | 2014-10-17 | 2015-01-07 | 浙江南方通信集团股份有限公司 | Optical fiber array and manufacturing method thereof |
| CN106128769A (en) * | 2016-07-04 | 2016-11-16 | 西安交通大学 | A kind of three-dimensional dye-sensitized solar cell working electrode and preparation method thereof |
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| CN103063720A (en) * | 2013-01-05 | 2013-04-24 | 西安交通大学 | Electrode for trans-scale glucose biosensor based on ZnO nanowire and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103063720A (en) * | 2013-01-05 | 2013-04-24 | 西安交通大学 | Electrode for trans-scale glucose biosensor based on ZnO nanowire and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103657565A (en) * | 2013-11-28 | 2014-03-26 | 西安交通大学 | Photo-catalytic reactor and preparation method thereof, based on three-dimensional cylindrical hierarchical structure array |
| CN103657565B (en) * | 2013-11-28 | 2015-07-01 | 西安交通大学 | Photo-catalytic reactor and preparation method thereof, based on three-dimensional cylindrical hierarchical structure array |
| CN104267464A (en) * | 2014-10-17 | 2015-01-07 | 浙江南方通信集团股份有限公司 | Optical fiber array and manufacturing method thereof |
| CN106128769A (en) * | 2016-07-04 | 2016-11-16 | 西安交通大学 | A kind of three-dimensional dye-sensitized solar cell working electrode and preparation method thereof |
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Application publication date: 20131009 |