CN104713929A - Method for preparing non-enzyme glucose sensor based on silk-screen printing - Google Patents
Method for preparing non-enzyme glucose sensor based on silk-screen printing Download PDFInfo
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- CN104713929A CN104713929A CN201510160186.1A CN201510160186A CN104713929A CN 104713929 A CN104713929 A CN 104713929A CN 201510160186 A CN201510160186 A CN 201510160186A CN 104713929 A CN104713929 A CN 104713929A
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Abstract
The invention discloses a method for preparing a non-enzyme glucose sensor based on silk-screen printing. A nano silver interpolation circuit and a copper oxide/multi-walled carbon nanotube sensing layer are registered in a double-layer manner by virtue of a silk-screen printing machine. The method is low in preparation cost, simple and fast; large-area printing can be carried out; the sensor is used for detecting the content of glucose, and is high in sensitivity, high in response speed and good in stability; the linear range for glucose detection is 1micron to 3mm; and the detection limit is 5nm.
Description
Technical field
The present invention relates to a kind of preparation method of electrochemical sensor, particularly relate to a kind of preparation method of the non-enzymatic electrochemical sensor for glucose detection.
Background technology
Along with the continuous appearance of new material and the play-by-play of more glucosan oxidation mechanism, the use of non-enzyme electrode discloses the latency development of the novel glucose sensor of catalysis glucose oxidase.
In order to develop sensitive height, selectivity is good, detection limit is low non-enzymatic glucose sensor, existing lot of documents reports a series of non-enzymatic eelctro-catalyst, comprises metal (such as: Au, Ag, Pt, Ni and Cu), metal oxide/semiconductor (such as: CuO, Cu
2o, NiO, CoO, Ru
2o, RuO
2with Ni (OH)
2), compound (as Cobalt Phthalocyanine), bimetal nano material or alloy (such as: Pt-Au, Pt-Pb, Ni-Cu and Au-Ag), metal/metal oxide-carbon nano tube compound material (such as: Aunanoparticles-MWNTs, Cu
2o-MWNTs nanocomposites and MnO
2-MWNTs) and based on the material (as CNTs, boric diamond) etc. of carbon.
At present, the electrode of most of non-enzymatic glucose electrochemical sensor is all glass-carbon electrode, metal electrode, or carbon electrode, and its shortcoming is that electrode surface area is little, active area is little, thus affects sensitivity and the degree of accuracy of sensor.
Summary of the invention
The object of the invention is for above-mentioned existing problems, provide a kind of preparation method of the non-enzymatic glucose sensor based on serigraphy, this preparation method's simple and fast, preparation cost are low and can large area printing; The transducer sensitivity of preparation is high, fast response time, good stability
Technical scheme of the present invention:
Based on a preparation method for the non-enzymatic glucose sensor of serigraphy, step is as follows:
1) preparation of copper chloride solution
Be dissolved in by cupric chloride in deionized water, stir 10-20min under normal temperature to dissolving completely, obtain blue copper chloride solution, the amount ratio of cupric chloride and deionized water is 1g:10-20mL;
2) preparation of multi-walled carbon nano-tubes (MWCNT) dispersion liquid
Multi-walled carbon nano-tubes is joined in deionized water, ultrasonic disperse 3 hours, obtain carbon nano tube dispersion liquid, the amount ratio of carbon nano-tube and deionized water is 1mg:5-8mL, then carbon nano tube dispersion liquid mixed with above-mentioned copper chloride solution and stir, obtain multi-walled carbon nano-tubes dispersion liquid, the volume ratio of carbon nano tube dispersion liquid and copper chloride solution is 1:0.5-2;
3) preparation of cupric oxide/multi-walled carbon nano-tubes potpourri
Under magnetic agitation, the NaOH solution that concentration is 8mol/L is dropwise dripped in above-mentioned multi-walled carbon nano-tubes dispersion liquid, the volume ratio of multi-walled carbon nano-tubes dispersion liquid and NaOH solution is 6:7, continue to stir 5-10h, vacuum filtration obtains black solid, vacuum drying chamber 90-120 DEG C of heating 1-2h, obtains cupric oxide/multi-walled carbon nano-tubes potpourri after solid abrasive;
4) preparation of cupric oxide/multi-walled carbon nano-tubes printing slurry
Get terpinol 50-100mL in beaker, the ethyl cellulose of 1.5-3g is added in beaker, after stirring and dissolving, get step 3) cupric oxide/multi-walled carbon nano-tubes solid 2.5 ~ 5g of obtaining, first magnetic agitation 10 ~ 20min, then cell pulverization 10 ~ 20min, obtains cupric oxide/multi-walled carbon nano-tubes printing slurry;
5) Nano Silver inserts the preparation referring to circuit
Get the polyurethane web plate that order number is 350, insert the length that refers to lines and be widely respectively 10-20mm, 0.5-3mm, insert and refer to that lines gap is 0.5-3mm, inserting finger number is 12-20 root, after polyurethane web plate is fixed on draw-in groove, open serigraphy electromechanical source, the silver ink of purchase is coated on web plate, be placed on print station by shifting to an earlier date cleaned polyethylene terephthalate (PET) plastic foil, adjustment scraper speed is 150-200mm/s, and the slotting finger circuit printed once, is placed in vacuum drying chamber by semi-automatic printing, 1h is dried at 50 DEG C, obtained for subsequent use;
6) based on the preparation of the non-enzymatic glucose sensor of serigraphy
Above-mentioned Nano Silver is inserted and refers to that circuit is placed on print station as printed substrate, by step 4) cupric oxide/multi-walled carbon nano-tubes printing slurry of obtaining is coated on web plate, adjustment scraper speed is 150-200mm/s, semi-automatic printing once, then be placed in vacuum drying chamber, 1h is dried, the obtained non-enzymatic glucose sensor based on serigraphy at 50 DEG C.
Advantage of the present invention is: low and can large area printing based on preparation method's simple and fast of the non-enzymatic glucose sensor of serigraphy, preparation cost; This transducer sensitivity is high, fast response time, good stability, is 1 μM of-3mM to the range of linearity of glucose detection, detects and is limited to 5nM; .
Accompanying drawing explanation
Fig. 1 is that Nano Silver inserts finger circuit diagram.
Fig. 2 is that obtained sensor is to the chrono-amperometric detection figure of glucose.
Specific embodiments
Below by specific embodiment, further technical scheme of the present invention is specifically described.Should be appreciated that, the following examples just as illustrating, and do not limit the scope of the invention, and the apparent change made according to the present invention of those skilled in the art simultaneously and modification are also contained within the scope of the invention.
Embodiment:
Based on a preparation method for the non-enzymatic glucose sensor of serigraphy, step is as follows:
1) preparation of copper chloride solution
2g cupric chloride is dissolved in 30mL deionized water, stirs 20min under normal temperature to dissolving completely, obtaining blue copper chloride solution;
2) preparation of multi-walled carbon nano-tubes (MWCNT) dispersion liquid
5mg multi-walled carbon nano-tubes is added in 30mL deionized water, ultrasonic disperse 3 hours, obtain carbon nano tube dispersion liquid, then carbon nano tube dispersion liquid mixed with above-mentioned copper chloride solution and stir, obtain multi-walled carbon nano-tubes dispersion liquid, the volume ratio of carbon nano tube dispersion liquid and copper chloride solution is 1:1;
3) preparation of cupric oxide/multi-walled carbon nano-tubes potpourri
Under magnetic agitation, the NaOH solution that concentration is 8mol/L is dropwise dripped in above-mentioned multi-walled carbon nano-tubes dispersion liquid, the volume ratio of multi-walled carbon nano-tubes dispersion liquid and NaOH solution is 6:7, continue to stir 8h, vacuum filtration obtains black solid, vacuum drying chamber 100 DEG C heating 1.52h, obtains cupric oxide/multi-walled carbon nano-tubes potpourri after solid abrasive;
4) preparation of cupric oxide/multi-walled carbon nano-tubes printing slurry
Get terpinol 100mL in beaker, in beaker, add the ethyl cellulose of 3g, after stirring and dissolving, get step 3) cupric oxide/multi-walled carbon nano-tubes solid 5g of obtaining, first magnetic agitation 20min, then cell pulverization 20min, obtain cupric oxide/multi-walled carbon nano-tubes printing slurry;
5) Nano Silver inserts the preparation referring to circuit
Get the polyurethane web plate that order number is 350, insert the length that refers to lines and be widely respectively 15mm, 2mm, insert and refer to that lines gap is 2mm, inserting finger number is 20, after polyurethane web plate is fixed on draw-in groove, open serigraphy electromechanical source, the silver ink of purchase is coated on web plate, be placed on print station by shifting to an earlier date cleaned polyethylene terephthalate (PET) plastic foil, adjustment scraper speed is 200mm/s, and the slotting finger circuit printed once, is placed in vacuum drying chamber by semi-automatic printing, 1h is dried at 50 DEG C, obtained for subsequent use; Fig. 1 is that Nano Silver inserts finger circuit diagram, shows:, lines are even about the slotting finger circuit of printing symmetrically in figure.
6) based on the preparation of the non-enzymatic glucose sensor of serigraphy
Above-mentioned Nano Silver is inserted and refers to that circuit is placed on print station as printed substrate, by step 4) cupric oxide/multi-walled carbon nano-tubes printing slurry of obtaining is coated on web plate, adjustment scraper speed is 200mm/s, semi-automatic printing once, then be placed in vacuum drying chamber, 1h is dried, the obtained non-enzymatic glucose sensor based on serigraphy at 50 DEG C.
Fig. 2 be obtained sensor to the chrono-amperometric detection figure of glucose, show in figure: this glucose sensor detection limit is low, linear zone field width, fast response time.
Claims (1)
1., based on a preparation method for the non-enzymatic glucose sensor of serigraphy, it is characterized in that step is as follows:
1) preparation of copper chloride solution
Be dissolved in by cupric chloride in deionized water, stir 10-20min under normal temperature to dissolving completely, obtain blue copper chloride solution, the amount ratio of cupric chloride and deionized water is 1g:10-20mL;
2) preparation of multi-walled carbon nano-tubes (MWCNT) dispersion liquid
Multi-walled carbon nano-tubes is joined in deionized water, ultrasonic disperse 3 hours, obtain carbon nano tube dispersion liquid, the amount ratio of carbon nano-tube and deionized water is 1mg:5-8mL, then carbon nano tube dispersion liquid mixed with above-mentioned copper chloride solution and stir, obtain multi-walled carbon nano-tubes dispersion liquid, the volume ratio of carbon nano tube dispersion liquid and copper chloride solution is 1:0.5-2;
3) preparation of cupric oxide/multi-walled carbon nano-tubes potpourri
Under magnetic agitation, the NaOH solution that concentration is 8mol/L is dropwise dripped in above-mentioned multi-walled carbon nano-tubes dispersion liquid, the volume ratio of multi-walled carbon nano-tubes dispersion liquid and NaOH solution is 6:7, continue to stir 5-10h, vacuum filtration obtains black solid, vacuum drying chamber 90-120 DEG C of heating 1-2h, obtains cupric oxide/multi-walled carbon nano-tubes potpourri after solid abrasive;
4) preparation of cupric oxide/multi-walled carbon nano-tubes printing slurry
Get terpinol 50-100mL in beaker, the ethyl cellulose of 1.5-3g is added in beaker, after stirring and dissolving, get step 3) cupric oxide/multi-walled carbon nano-tubes solid 2.5 ~ 5g of obtaining, first magnetic agitation 10 ~ 20min, then cell pulverization 10 ~ 20min, obtains cupric oxide/multi-walled carbon nano-tubes printing slurry;
5) Nano Silver inserts the preparation referring to circuit
Get the polyurethane web plate that order number is 350, insert the length that refers to lines and be widely respectively 10-20mm, 0.5-3mm, insert and refer to that lines gap is 0.5-3mm, inserting finger number is 12-20 root, after polyurethane web plate is fixed on draw-in groove, open serigraphy electromechanical source, the silver ink of purchase is coated on web plate, be placed on print station by shifting to an earlier date cleaned polyethylene terephthalate (PET) plastic foil, adjustment scraper speed is 150-200mm/s, and the slotting finger circuit printed once, is placed in vacuum drying chamber by semi-automatic printing, 1h is dried at 50 DEG C, obtained for subsequent use;
6) based on the preparation of the non-enzymatic glucose sensor of serigraphy
Above-mentioned Nano Silver is inserted and refers to that circuit is placed on print station as printed substrate, by step 4) cupric oxide/multi-walled carbon nano-tubes printing slurry of obtaining is coated on web plate, adjustment scraper speed is 150-200mm/s, semi-automatic printing once, then be placed in vacuum drying chamber, 1h is dried, the obtained non-enzymatic glucose sensor based on serigraphy at 50 DEG C.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106841353A (en) * | 2017-02-27 | 2017-06-13 | 天津理工大学 | A kind of preparation method and applications without enzyme electrochemica biological sensor electrode |
CN106983517A (en) * | 2017-03-31 | 2017-07-28 | 北京工业大学 | One kind is without flexible blood glucose microsensor of enzyme nanometer and preparation method thereof |
CN107525825A (en) * | 2016-06-21 | 2017-12-29 | 天津理工大学 | It is prepared by a kind of gas sensor based on screen printing technique |
CN108896640A (en) * | 2018-08-17 | 2018-11-27 | 成都师范学院 | A kind of preparation method and application of the nano silver without enzymatic electrochemical glucose sensor |
CN109304952A (en) * | 2018-09-01 | 2019-02-05 | 哈尔滨工程大学 | A kind of preparation method of the printable formula temperature sensor of the ionic liquid containing pyrenyl |
CN109342518A (en) * | 2018-09-10 | 2019-02-15 | 天津科技大学 | A kind of preparation method and application of the non-enzyme sensor of the glucose based on screen printing electrode |
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JPH09159644A (en) * | 1995-12-11 | 1997-06-20 | Dainippon Printing Co Ltd | Biosensor and manufacture thereof |
CN101603941A (en) * | 2009-07-16 | 2009-12-16 | 中国科学院长春应用化学研究所 | Nano nickel particles/carbon nano-fiber composite material prepares the method for non-enzymatic glucose sensor |
CN101661858A (en) * | 2009-08-31 | 2010-03-03 | 福州大学 | Surface chemical metal plating carbon nanotube field-emission cathode preparation method |
US20130075276A1 (en) * | 2011-09-26 | 2013-03-28 | Arkray, Inc. | Glucose Sensor |
US20140061044A1 (en) * | 2012-09-06 | 2014-03-06 | Amrita Vishwa Vidyapeetham | Non-enzymatic glucose sensor |
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2015
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Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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JPH09159644A (en) * | 1995-12-11 | 1997-06-20 | Dainippon Printing Co Ltd | Biosensor and manufacture thereof |
CN101603941A (en) * | 2009-07-16 | 2009-12-16 | 中国科学院长春应用化学研究所 | Nano nickel particles/carbon nano-fiber composite material prepares the method for non-enzymatic glucose sensor |
CN101661858A (en) * | 2009-08-31 | 2010-03-03 | 福州大学 | Surface chemical metal plating carbon nanotube field-emission cathode preparation method |
US20130075276A1 (en) * | 2011-09-26 | 2013-03-28 | Arkray, Inc. | Glucose Sensor |
US20140061044A1 (en) * | 2012-09-06 | 2014-03-06 | Amrita Vishwa Vidyapeetham | Non-enzymatic glucose sensor |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107525825A (en) * | 2016-06-21 | 2017-12-29 | 天津理工大学 | It is prepared by a kind of gas sensor based on screen printing technique |
CN106841353A (en) * | 2017-02-27 | 2017-06-13 | 天津理工大学 | A kind of preparation method and applications without enzyme electrochemica biological sensor electrode |
CN106983517A (en) * | 2017-03-31 | 2017-07-28 | 北京工业大学 | One kind is without flexible blood glucose microsensor of enzyme nanometer and preparation method thereof |
CN108896640A (en) * | 2018-08-17 | 2018-11-27 | 成都师范学院 | A kind of preparation method and application of the nano silver without enzymatic electrochemical glucose sensor |
CN109304952A (en) * | 2018-09-01 | 2019-02-05 | 哈尔滨工程大学 | A kind of preparation method of the printable formula temperature sensor of the ionic liquid containing pyrenyl |
CN109342518A (en) * | 2018-09-10 | 2019-02-15 | 天津科技大学 | A kind of preparation method and application of the non-enzyme sensor of the glucose based on screen printing electrode |
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