CN104742549A - Preparation method for decorating silk-screen printing electrode ethanol sensor by nanometer copper oxide - Google Patents
Preparation method for decorating silk-screen printing electrode ethanol sensor by nanometer copper oxide Download PDFInfo
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- CN104742549A CN104742549A CN201510184204.XA CN201510184204A CN104742549A CN 104742549 A CN104742549 A CN 104742549A CN 201510184204 A CN201510184204 A CN 201510184204A CN 104742549 A CN104742549 A CN 104742549A
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- cupric oxide
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Abstract
A preparation method for decorating a silk-screen printing electrode ethanol sensor by nanometer copper oxide includes the steps: 1) preparing mixed solution of copper sulfate and cetyltrimethylammonium bromide ammonium bromide; 2) preparing the copper oxide; 3) preparing copper oxide/graphene printing paste; 4) preparing a nanometer silver circuit interpolation in power exponent form; 5) preparing the ethanol sensor. The preparation method has the advantages that the ethanol sensor is low in preparation cost, simple and rapid, large-area printing can be performed, the prepared sensor is high in sensitivity, rapid in response, fine in stability, the linear range of ethanol detection ranges from 1muM to 3mM, the limit of ethanol detection is 10nM, and sensitivity is 1328.64muA*L*mmol-1cm-2.
Description
Technical field
The present invention relates to a kind of preparation method of serigraphy sensor, particularly relate to the preparation method that a kind of nano cupric oxide modifies screen printing electrode ethanol sensor.
Background technology
Printed electronic is a kind of novel pollution-free industry, and it refers to various function ink, and by suitable printing technology, addition is printed on various base material, the electronic product of preparation large area, flexibility, low cost and device.Recent years, the high speed industrialized development of printed electronic industry has driven the Fashion and Evolution of printed electronic device related industries.Due to the technology relative maturity of current biology sensor, and the problem of most critical is low cost, is easy to produce.And adopt printed electronics, just in time can realize low cost, be easy to produce.
Adopt the method for serigraphy, prepare by organic nanocomposite as electrically conductive ink, the extensive printed sensor of large area, to replace conventional method now used, is the active demand of electronics industry and information industry.
At present, the electrode of most of electrochemical sensor is all glass-carbon electrode, metal electrode or carbon electrode, and its shortcoming is that electrode surface area is little, generation active area is little, thus affects sensitivity and the accuracy of sensor.
In recent years, the concern of ethanol sensor research got more and more.Ethanol sensor is in many fields such as food industry, fermentation industry, alcohol fuel, environment measuring, marine monitoring, traffic safety, drug abuse test, biomedical engineering.Alcohol Biosensor, as the important composition of ethanol sensor and developing direction, has been applied to online or non-online ethanol at present and has detected.Automation process to be realized control to carry out on-line continuous detection by means of sensor in industrial production of ethyl alcohol.
But, the stability of this sensor can be subject to the impact of the factors such as temperature, pH value of solution and dissolved oxygen, and make comparatively loaded down with trivial details, therefore ethanol sensor on-line continuous detects becomes current study hotspot, along with the continuous appearance of new material and the play-by-play of more ethanol sensors, the use of on-line continuous detection technique discloses the latency development of on-line continuous monitoring ethanol sensor.
In order to develop the ethanol sensor of sensitive height, the monitoring of selective good, on-line continuous, existing lot of documents reports a series of decorative material of exploration, comprises metal such as Au, Ag, Pt, Ni and Cu, metal oxide/semiconductor such as CuO, Cu
2o, NiO, CoO, Ru
2o, Ru
2o and Ni (OH)
2, compound is 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 gold-carbon nano tube compound material (Aunanoparticles-MWNTs), cuprous oxide multi-wall carbon nano-tube composite material (Cu
2and manganese oxide carbon nano-composite material (MnO O-MWNTsnanocomposites)
2-MWNTs) and based on the material of carbon as CNTs, boric diamond etc.
Nano material specific area is large, uses it for prepare on-line checkingi ethanol sensor and be expected to obtain good effect. greatly improve the stability of sensor.Wherein, nano cupric oxide has high-specific surface area and better electrical chemism, is the good material of one preparing ethanol sensor.The present invention adopts interpolation circuit, and with the mode printed electrode of printing, this electrode surface area is large, therefore it is large to produce active area, thus improves sensitivity and the accuracy of sensor; The nano cupric oxide sensing material that utilized liquid-phase precipitation method to prepare, has prepared highly sensitive on-line checkingi ethanol sensor.
Summary of the invention
The object of the invention is for above-mentioned existing problems, a kind of nano cupric oxide is provided to modify the preparation method of screen printing electrode ethanol sensor, sensor prepared by the method adopts interpolation circuit, with the mode printed electrode of printing, electrode surface area is large, generation active area is large, greatly can improve sensitivity and the accuracy of sensor.
Technical scheme of the present invention:
Nano cupric oxide modifies a preparation method for screen printing electrode ethanol sensor, and step is as follows:
1) preparation of copper sulphate-hexadecyl trimethylamine ammonium bromide mixed solution
By copper sulphate dissolves in deionized water, under normal temperature, stir 10-30min, then add hexadecyl trimethylamine ammonium bromide (CTAB), after magnetic agitation, obtain copper sulphate-hexadecyl trimethylamine ammonium bromide mixed solution;
2) preparation of cupric oxide
In above-mentioned copper sulphate-hexadecyl trimethylamine ammonium bromide mixed solution, dripping concentration with separatory funnel is the NaOH solution of 8mol/L, and vacuum filtration obtains black precipitate, heats 1-2h, obtain cupric oxide after grinding in vacuum drying chamber at 50-90 DEG C;
3) preparation of cupric oxide/Graphene printing slurry
Terpinol to be mixed with ethyl cellulose and magnetic agitation 10h, then adds step 2) obtained cupric oxide cell pulverization 5-8h, obtain cupric oxide/Graphene printing slurry;
4) 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 8-12 root, after web plate is fixed on draw-in groove, open serigraphy electromechanical source, the silver ink of purchase is coated on web plate, PETG (PET) plastic foil is placed on print station, adjustment scraper speed is 150-200mm/s, the slotting finger circuit printed once, is placed in vacuum drying chamber and dries 1h at 50 DEG C by semi-automatic printing, and obtained Nano Silver is inserted and referred to circuit;
5) preparation of ethanol sensor
Above-mentioned Nano Silver is inserted and refers to that circuit is placed on print station as printed substrate, by step 3) cupric oxide/Graphene printing slurry of obtaining is coated on web plate, adjustment scraper speed is 150-200mm/s, semi-automatic printing once, the sensor printed is placed in vacuum drying chamber and at 55 DEG C, dries 1h, after to be dried, obtained ethanol sensor also puts into sealing bag kept dry.
Described step 1) in the amount ratio of copper sulphate and deionized water be 1g:10-20mL; Copper sulphate and hexadecyl trimethylamine ammonium bromide (CTAB) mass ratio are 40:2-3.
Described step 2) in the volume ratio of copper sulphate-hexadecyl trimethylamine ammonium bromide mixed solution and NaOH solution be 1:0.5-2.
Described step 3) in the amount ratio of ethyl cellulose, terpinol and cupric oxide be 1.5-3g:50-100mL:2.5-5g.
Advantage of the present invention is: this ethanol sensor preparation cost is low, simple and fast, can large area printing; The transducer sensitivity of preparation is high, fast response time, good stability, and the range of linearity detected ethanol is 1 μM of-3mM, and detect and be limited to 10nM, sensitivity is 1328.64 μ ALmmol
-1cm
-2.
Accompanying drawing explanation
Fig. 1 is the X-ray powder diffraction pattern of obtained cupric oxide product.
Fig. 2 is the photo of the ESEM of obtained cupric oxide product.
Fig. 3 is that Nano Silver inserts finger circuit diagram.
Fig. 4 is the chrono-amperometric detection figure of sensor to ethanol.
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:
Nano cupric oxide modifies an ethanol sensor for screen printing electrode, and its preparation methods steps is as follows:
1) preparation of copper sulphate-hexadecyl trimethylamine ammonium bromide mixed solution
By 2g copper sulphate dissolves in 30mL deionized water, under normal temperature, stir 10min, then add 0.1g hexadecyl trimethylamine ammonium bromide (CTAB), after magnetic agitation 30min, obtain copper sulphate-hexadecyl trimethylamine ammonium bromide mixed solution;
2) preparation of cupric oxide
In above-mentioned copper sulphate-hexadecyl trimethylamine ammonium bromide mixed solution, dripping 70mL concentration with separatory funnel is the NaOH solution of 8mol/L, and stir 36h, vacuum filtration obtains black precipitate, in vacuum drying chamber, heat 1.5h at 60 DEG C, after grinding, obtain cupric oxide;
Fig. 1 is the X-ray powder diffraction pattern of obtained cupric oxide, shows in figure: product main component is cupric oxide, and its main crystal orientation is 002 and 111.
Fig. 2 is the photo of the ESEM of obtained cupric oxide, shows in figure: nano cupric oxide is described corolla shape crystal morphology really, and nanometer sheet average-size is 700nm, and thickness is about 60nm.
3) preparation of cupric oxide/Graphene printing slurry
After 100mL terpinol and 3g ethyl cellulose mix and blend being dissolved, add 5g step 2) obtained cupric oxide/Graphene mixture, first magnetic agitation 10h, then cell pulverization 5h, obtain cupric oxide/Graphene printing slurry;
4) 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 10, after web plate is fixed on draw-in groove, open serigraphy electromechanical source, the silver ink of purchase is coated on web plate, PETG (PET) plastic foil is placed on print station, adjustment scraper speed is 200mm/s, the slotting finger circuit printed once, is placed in vacuum drying chamber and dries 1h at 50 DEG C by semi-automatic printing, and obtained Nano Silver is inserted and referred to circuit; Fig. 3 is that Nano Silver inserts finger circuit diagram, shows: show in figure:, lines are even about the slotting finger circuit of printing symmetrically in figure;
5) preparation of ethanol sensor
Above-mentioned Nano Silver is inserted and refers to that circuit is placed on print station as printed substrate, by step 3) the cupric oxide printing slurry that obtains is coated on web plate, adjustment scraper speed is 200mm/s, semi-automatic printing once, the sensor printed is placed in vacuum drying chamber and at 50 DEG C, dries 1h, after to be dried, obtained ethanol sensor also puts into sealing bag kept dry.
Fig. 4 be obtained sensor to the chrono-amperometric detection figure of ethanol, show in figure: this ethanol sensor detection limit is low, linear zone field width, fast response time.
Claims (4)
1. nano cupric oxide modifies a preparation method for screen printing electrode ethanol sensor, it is characterized in that step is as follows:
1) preparation of copper sulphate-hexadecyl trimethylamine ammonium bromide mixed solution
By copper sulphate dissolves in deionized water, under normal temperature, stir 10-30min, then add hexadecyl trimethylamine ammonium bromide (CTAB), after magnetic agitation, obtain copper sulphate-hexadecyl trimethylamine ammonium bromide mixed solution;
2) preparation of cupric oxide
In above-mentioned copper sulphate-hexadecyl trimethylamine ammonium bromide mixed solution, dripping concentration with separatory funnel is the NaOH solution of 8mol/L, and vacuum filtration obtains black precipitate, heats 1-2h, obtain cupric oxide after grinding in vacuum drying chamber at 50-90 DEG C;
3) preparation of cupric oxide/Graphene printing slurry
Terpinol to be mixed with ethyl cellulose and magnetic agitation 10h, then adds step 2) obtained cupric oxide cell pulverization 5-8h, obtain cupric oxide/Graphene printing slurry;
4) 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 8-12 root, after web plate is fixed on draw-in groove, open serigraphy electromechanical source, the silver ink of purchase is coated on web plate, PETG (PET) plastic foil is placed on print station, adjustment scraper speed is 150-200mm/s, the slotting finger circuit printed once, is placed in vacuum drying chamber and dries 1h at 50 DEG C by semi-automatic printing, and obtained Nano Silver is inserted and referred to circuit;
5) preparation of ethanol sensor
Above-mentioned Nano Silver is inserted and refers to that circuit is placed on print station as printed substrate, by step 3) cupric oxide/Graphene printing slurry of obtaining is coated on web plate, adjustment scraper speed is 150-200mm/s, semi-automatic printing once, the sensor printed is placed in vacuum drying chamber and at 55 DEG C, dries 1h, after to be dried, obtained ethanol sensor also puts into sealing bag kept dry.
2. nano cupric oxide modifies the preparation method of screen printing electrode ethanol sensor according to claim 1, it is characterized in that: described step 1) in the amount ratio of copper sulphate and deionized water be 1g:10-20mL; Copper sulphate and hexadecyl trimethylamine ammonium bromide (CTAB) mass ratio are 40:2-3.
3. nano cupric oxide modifies the preparation method of screen printing electrode ethanol sensor according to claim 1, it is characterized in that: described step 2) in the volume ratio of copper sulphate-hexadecyl trimethylamine ammonium bromide mixed solution and NaOH solution be 1:0.5-2.
4. nano cupric oxide modifies the preparation method of screen printing electrode ethanol sensor according to claim 1, it is characterized in that: described step 3) in the amount ratio of ethyl cellulose, terpinol and cupric oxide be 1.5-3g:50-100mL:2.5-5g.
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Cited By (3)
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 |
CN107576700A (en) * | 2017-09-01 | 2018-01-12 | 湖南工程学院 | Nano cupric oxide modified electrode and the method that Nilvadipine is analyzed with modified electrode |
MD4495C1 (en) * | 2016-09-09 | 2018-01-31 | Николай АБАБИЙ | Ethanol sensor based on copper oxide |
-
2015
- 2015-04-17 CN CN201510184204.XA patent/CN104742549A/en active Pending
Cited By (4)
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 |
MD4495C1 (en) * | 2016-09-09 | 2018-01-31 | Николай АБАБИЙ | Ethanol sensor based on copper oxide |
CN107576700A (en) * | 2017-09-01 | 2018-01-12 | 湖南工程学院 | Nano cupric oxide modified electrode and the method that Nilvadipine is analyzed with modified electrode |
CN107576700B (en) * | 2017-09-01 | 2019-07-16 | 湖南工程学院 | Nano cupric oxide modified electrode and the method for analyzing Nilvadipine with modified electrode |
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