CN105353009B - A kind of screen printing electrode and its processing method based on Graphene conductive ink - Google Patents
A kind of screen printing electrode and its processing method based on Graphene conductive ink Download PDFInfo
- Publication number
- CN105353009B CN105353009B CN201510685020.1A CN201510685020A CN105353009B CN 105353009 B CN105353009 B CN 105353009B CN 201510685020 A CN201510685020 A CN 201510685020A CN 105353009 B CN105353009 B CN 105353009B
- Authority
- CN
- China
- Prior art keywords
- electrode
- screen printing
- substrate
- conductive ink
- lead wire
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Inks, Pencil-Leads, Or Crayons (AREA)
- Cold Cathode And The Manufacture (AREA)
Abstract
The invention belongs to heavy metal analysis sensor fields, more particularly to a kind of screen printing electrode and its processing method based on Graphene conductive ink.Including substrate, working electrode is printed on the substrate, to electrode and conductive lead wire, the working electrode and conductive lead wire and to electrical communication between electrode and conductive lead wire, the working electrode and conductive lead wire and to by lead electrical communication, the working electrode is Graphene conductive ink to the material of electrode, conductive lead wire and lead between electrode and conductive lead wire.The present invention has biggish specific surface area, higher electro-catalysis and electro-chemical activity using graphene, make its as working electrode, to the material of electrode, conductive lead wire and lead, and then improve the electron transmission performance of molecules detected or ion on electrode reaction interface, the absorption of heavy metal ion is not only improved using the screen printing electrode of Graphene conductive ink preparation simultaneously, and is conducive to surface-functionalized modification.
Description
Technical field
The invention belongs to heavy metal analysis sensor field, it is related to screen printing electrode, more particularly to a kind of based on graphite
The screen printing electrode and its processing method of alkene electrically conductive ink.
Background technique
In recent years, in the fields such as food, environmental monitoring heavy metals exceeding standard event take place frequently, people are food-safe, ring
Border hygienic issues are increasingly paid attention to, meanwhile, people also need strongly one kind can quickly, conveniently, carry, accurately monitoring a huge sum of money
The analysis means of category.Heavy metal ion sensor becomes the primary choosing quickly detected for people, and screen printing electrode is as one
Kind production is simple, can be mass, is inexpensive, the electrode that can be disposable of detection favorable reproducibility, high sensitivity, solves weight
Metal ion sensor monitors the problems such as response stability as caused by environment, reproducibility and detectable substance pollute on-line, opens up significantly
Research and application extension of the electrochemical methods in the fields such as food, environmental monitoring are opened up.
At this stage, screen printing electrode used in heavy metal ion sensor is mostly silver paste or carbon slurry.Silver paste higher cost,
It is not easily recycled in screen printing electrode use process and easily causes secondary heavy metal pollution.However, preparing silk screen using carbon slurry
When printing electrode, since carbon slurry resistance is larger, and surface of printing electrode is more coarse, and current distribution is uneven is even, is unfavorable for sensitive
The raising of degree.For this purpose, people are by various methods, to solve the problems, such as traditional silk-screened electrode, for example, State Intellectual property right
Office disclose a kind of screen printing electrode, preparation process and its application application number: 200810032125.7 }, the silk screen
It prints electrode, the silk screen used in screen printing process used has the property that the material of silk screen and brush is respectively polyester
And plastics, meshcount are 50 mesh；Silk screen uses 100 mesh titanium valves, the partial size of nano-titanium oxide at a distance from substrate for d=3mm.
20nm (mass ratio of titanium valve and nano-titanium oxide is 90:10).Angle used by brush is 45 ° when printing.The present embodiment
Screen printing electrode substrate material is polyether-ether-ketone (PEEK).Titanium valve/nano oxidized is individually printed on the substrate 6 of printed electrode
Titanium working electrode 2 is also printed with an electrode specification layer 7 on substrate；It is printed with 2 electrodes on substrate 5, is carbon auxiliary electricity respectively
Pole and Ag-AgCl reference electrode, each electrode have been correspondingly connected with a contact conductor, and also there are two electrodes to advise for printing on the substrate
Model layer 3 and 4.Two substrates are bonded together using waterproof silicon rubber.The method accelerate to a certain extent electron transmission and
Catalytic activity, but its electron transmission and catalytic activity effect promoting are limited, and preparation cost is higher, preparation process is relatively complicated,
To increase production cost, production efficiency is reduced.
Summary of the invention
The present invention is for above-mentioned electron transmission and catalytic activity effect promoting are limited, preparation cost is higher, preparation process
The technical problems such as relatively complicated propose a kind of reasonable, of simple structure and low cost, the easy to process and electron transmission of design and urge
Change a kind of good screen printing electrode and its processing method based on Graphene conductive ink of active effect.
In order to achieve the above object, the technical solution adopted by the present invention is that the present invention provides a kind of based on graphene conductive
The screen printing electrode of ink, including substrate are printed with working electrode on the substrate, to electrode and conductive lead wire, described
Working electrode and conductive lead wire and to electrical communication between electrode and conductive lead wire, the working electrode and conductive lead wire and
To between electrode and conductive lead wire by lead electrical communication, the working electrode, to the material of electrode, conductive lead wire and lead
Matter is Graphene conductive ink.
Preferably, being also printed with reference electrode on the substrate.
Preferably, the material of the reference electrode is the mixture of silver paste and chlorination silver paste.
Preferably, being also covered with a layer insulating above the lead.
The present invention also provides a kind of above-mentioned methods of the screen printing electrode based on Graphene conductive ink of processing, including
Following steps:
A, Substrate treatment: the substrate reduced first being cleaned by ultrasonic with acetone, is then cleaned by ultrasonic with dehydrated alcohol, natural
It dries；
B, electrode print: using Graphene conductive ink as electrode material, on substrate printing work electrode, to electrode, lead
Electrical lead and lead after finishing printing, are sent into an oven, drying；
C, reference electrode prints: using the mixture of silver paste and chlorination silver paste as reference electrode material, ginseng is printed on substrate
It than electrode, after finishing printing, is sent into an oven, dries；
D, insulating layer prints: using dielectric ink as insulating layer material, insulating layer is printed on substrate, insulating layer is in addition to work
Electrode prints the covering of the place other than electrode, conductive lead wire and reference electrode, after finishing printing, is sent into an oven, dries
Dry, so far screen printing electrode is completed.
E, modified electrode: poly styrene sulfonate and aminosalicylic acid are configured to 0.1~10mg/mL dispersion liquid, wait match
After the completion of setting, configured dispersant liquid drop is coated in the working electrode surface of screen printing electrode, naturally dry.
F, electrode activation: modification working electrode is placed in sulfuric acid or hac buffer or in carbonate buffer solution
It impregnates, using cyclic voltammetry, stablizes to electrochemical signals, rinsed with secondary distilled water, drying.
Preferably, in a step, the substrate reduced first is cleaned by ultrasonic 1~3 time with acetone, clean 5 every time~
Then 15min is cleaned by ultrasonic 1~3 time with dehydrated alcohol to remove the dirt on its surface, cleans 5~15min every time, dry in the air naturally
It is dry.
Preferably, the proportion between the poly styrene sulfonate and aminosalicylic acid is 1:10~10:1.
Preferably, taking the configured dispersant liquid drop of 2~20 μ L to be coated in the work of screen printing electrode in the step e
Make electrode surface, naturally dry.
Compared with prior art, the advantages and positive effects of the present invention are,
1, the present invention has biggish specific surface area, higher electro-catalysis and electro-chemical activity using graphene, makes its work
For working electrode, to the material of electrode, conductive lead wire and lead, and then improve molecules detected or ion in electrode reaction circle
Electron transmission performance on face, while heavy metal ion is not only improved using screen printing electrode prepared by Graphene conductive ink
Absorption, and be conducive to surface-functionalized modification.
2, the present invention simplifies print steps using graphene as while electrode material, by simplifying print steps,
And then it reduces production cost, improve working efficiency.
3, poly styrene sulfonate and aminosalicylic acid are configured to the dispersion liquid of modified electrode by the present invention, and then are improved
The sensitivity of electrode by the activation to working electrode, and then improves the stability and reproducibility of entire screen printing electrode.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment
Attached drawing be briefly described, it should be apparent that, drawings in the following description are some embodiments of the invention, for ability
For the those of ordinary skill of domain, without any creative labor, it can also be obtained according to these attached drawings others
Attached drawing.
Fig. 1 is the structural schematic diagram for the screen printing electrode that embodiment 1 provides；
Fig. 2 is the structural schematic diagram for the screen printing electrode cyclic voltammogram that embodiment 2 provides；
In above each figure, 1, substrate；2, working electrode；3, to electrode；4, conductive lead wire；5, lead；6, reference electrode；7,
Insulating layer.
Specific embodiment
To better understand the objects, features and advantages of the present invention, with reference to the accompanying drawings and examples
The present invention will be further described.It should be noted that in the absence of conflict, in embodiments herein and embodiment
Feature can be combined with each other.
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention, still, the present invention may be used also
To be implemented using other modes described herein are different from, therefore, the present invention is not limited to the specific of specification is described below
The limitation of embodiment.
Graphene has biggish specific surface area, higher electro-catalysis and electro-chemical activity.It is passed in detection of heavy metal ion
In sensor field, the application of graphene can improve the electron transmission performance of molecules detected or ion on electrode reaction interface,
And then greatly improve the performance of sensor.In addition, edge and the rejected region activity with higher of graphene, especially
The graphene oxide as made from chemical oxidization method contains a large amount of oxygen-containing group, and such as-COOH ,-C=O ,-OH isoreactivity are oxygen-containing
Functional group.Therefore graphene or graphene oxide composite material can be used as novel modified electrode material.
Embodiment 1, as shown in Figure 1, the present embodiment provides a kind of screen printing electrode based on Graphene conductive ink, packet
Substrate is included, the shape of substrate is the shape of substrate common in the market, and substrate material selection range is extensive, any to can be used for silk screen
The insulating materials of printing can be used in electrode base sheet, preferably polychlorostyrene second (PVC), polytetrafluoroethylene (PTFE) (PTFE) or PET plastic etc., base
On piece is printed with that working electrode, (specific layout type is as shown in figure 1 shown in a figure, such layout type to electrode and conductive lead wire
Also it is common layout type in the market, naturally it is also possible to using other layout type), screen printing provided by the present embodiment
Brush electrode is three-electrode structure, working electrode and conductive lead wire and to electrical communication between electrode and conductive lead wire, work electricity
Pole and conductive lead wire and between electrode and conductive lead wire pass through lead (lead can also be classified as conductive lead wire, in this implementation
It is for good statement, lead and conductive lead wire is described separately in example) electrical communication, working electrode, to electrode, conductive lead wire with
And the material of lead is Graphene conductive ink, naturally it is also possible to only working electrode and the material selection graphite to electrode
Alkene electrically conductive ink, in the present embodiment, Graphene conductive ink used are that Jining benefit Tener rice company graphene produced is led
Electric ink.
In order to preferably measure the potential of working electrode, in the present embodiment, reference electrode (tool is also printed on substrate
Body position is as shown in figure 1 shown in b figure), in the present embodiment, in order to preferably measure, improve accuracy, the material of reference electrode
Matter is the mixture of silver paste and chlorination silver paste.
Equally, for guard electrode, in the present embodiment, insulating layer has also been printed on substrate, as shown in figure 1 shown in c figure,
Insulating layer mainly cover lead top and substrate on remove working electrode, to electrode, conductive lead wire (conductive lead wire and
Belong at the substrate of same rectangular area with conductive lead wire) and reference electrode other than place, the material of insulating layer is exhausted
Edge ink.
By above-mentioned setting, using the characteristic of graphene, make its as working electrode, to electrode, conductive lead wire and
The material of lead effectively raises the electron transmission performance of molecules detected or ion on electrode reaction interface, while benefit
The absorption of heavy metal ion is not only improved with screen printing electrode prepared by Graphene conductive ink, and is conducive to surface-functionalized
Modification.
Embodiment 2: the production method for present embodiments providing a kind of screen printing electrode based on Graphene conductive ink:
During embodiment provided by the present invention, used screen process press is that Ou Rui that automation equipment in Qingdao has
The production of limit company, the flat screen printer of model ORE-2030, in the present embodiment, some steps also in relation with the screen printer one
A little functions, the structure and structure provided in this embodiment of possible others screen printers are inconsistent, but cannot influence the present invention and be wanted
The range of protection.
1, substrate pre-processes
(1) the PVC substrate cut out is first cleaned by ultrasonic 1 time with acetone, cleans 15min, every time to remove the dirt on its surface
Then dirt is cleaned by ultrasonic 1 time with dehydrated alcohol, cleans 5min, naturally dry every time.
2, electrode print
(2) web plate for being used to print a figure pattern in Fig. 1 is fixed on screen printer horizontal table, web plate and horizontal work
Making the distance between platform is 2cm, and it is 30 degree that adjustment, which scrapes angle,.
(3) by the substrate of naturally dry, it is put in table surface, air pump is opened, using negative-pressure adsorption, it is ensured that substrate is solid
It is fixed, problem of misalignment caused by substrate is mobile when preventing from printing.
(4) Graphene conductive ink is uniformly paved into right amount in web plate close to the place printed electrode and is slightly wider than scraper
The bar paten of width.
(5) booting printing, finishes electrode, working electrode, contact conductor and lead one-step print.
(6) it finishes printing, the substrate printed is placed in baking oven, temperature is adjusted to 90 DEG C, toasts 20min.
3, reference electrode prints
(7) slurry of the Graphene conductive ink on screen printer is recycled, cleans web plate, frictioning and scraper with net washing water,
Prepare the web plate for printing b figure pattern in Fig. 1 (printing is represented region of tiltedly crossing in b figure in Fig. 1).
(8) substrate of drying is placed on workbench, opens air pump, when placement makes print range be located at print station as far as possible
Center.By adjusting the fixation position of web plate, it is directed at baseline, it is fixed.If passing through the micro- of workbench it was found that still there is a little bias
Knob is adjusted to carry out position adjusting.
(9) by silver paste and silver chlorate slurry agitation uniformly (silver paste and the harmonic proportion of chlorination silver paste in 1:10~10:1,
1:10 in the present embodiment), appropriate slurry is uniformly paved into one for being slightly wider than blade width in scraper lower position, printing,
Reference electrode is formed on substrate.
(10) after finishing printing, the substrate printed is placed in baking oven, temperature is adjusted to 90 DEG C, toasts 20min.
4, insulating layer prints
(11) by the silver paste and the recycling of chlorination silver paste mixed slurry on screen printer, web plate and frictioning are cleaned with net washing water,
Scraper prepares for printing c figure pattern web plate in Fig. 1 (for the overlay area on substrate).
(12) substrate of drying is placed on workbench, it is used in the same step of method (7).It is mixed well with appropriate 789 solvent
Dielectric ink, appropriate slurry are uniformly paved into one for being slightly wider than blade width in scraper lower position, printing, on substrate
Form insulating layer.
(13) after finishing printing, the substrate printed is placed in baking oven, temperature is adjusted to 80 DEG C, toasts 20min, drying knot
After beam to get arrive screen printing electrode.
5, modified electrode
(14) PSS (poly styrene sulfonate) and aminosalicylic acid are configured to 0.1mg/mL dispersion liquid, PSS and amino water
The ratio of poplar acid is 1:10.
(15) the configured good dispersant liquid drop of 2 μ L is taken to be coated in the working electrode of SPE electrode (i.e. to electrode and working electrode)
Surface, naturally dry, modified electrode work are completed.
6, electrode activation
(16) modification SPE electrode is placed in sulfuric acid or hac buffer or is impregnated in carbonate buffer solution, Ag/
AgCl (3.0MKCl) is reference electrode, and platinum electrode is used as to electrode and SPE electrode as working electrode.First in 0.5-1.2V
Between enclosed with cyclic voltammetry (Cyclic Voltammetric, CV) with the velocity scanning 20 of 1.0V/s, then in 1.5-2.0V
Between, it is enclosed with the velocity scanning 30 of 70mV/s, until electrochemical signals are stablized.
(17) SPE electrode is rinsed with secondary distilled water, dries (or naturally dry in air) under infrared light irradiation, electricity
Pole activation is completed.
Detection:
Detect the Trace Cadmium in food.Solution to be measured is immersed into the screen printing electrode lower end, is dissolved out with differetial-potential
Trace Cadmium in voltammetric determination food samples, initial potential -0.05V, electrodeposition current potential -1.30V, current potential increment 0.001V/S, electricity
Product time 100s, equilibration time 10s.In the HAc-NaAc buffer solution system that pH is 4.6 or so, Cd2+In -0.75V (vs
SCE) there is sensitive dissolution peak, peak current is in Cd2+Concentration is 2.0 × 10-7~8.0 × 10-5The good linear relationship of Shi Chengxian,
Its regression equation is y=2.102 × 106X+5.001, related coefficient 0.9996, detection are limited to 1.1 × 10-7moL/L。
Embodiment 3: the production method for present embodiments providing a kind of screen printing electrode based on Graphene conductive ink:
1, substrate pre-processes
(1) the PTFE substrate cut out is first cleaned by ultrasonic 2 times with acetone, cleans 10min, every time to remove the dirt on its surface
Then dirt is cleaned by ultrasonic 2 times with dehydrated alcohol, cleans 10min, naturally dry every time.
2, electrode print
(2) web plate for being used to print a figure pattern in Fig. 1 is fixed on screen printer horizontal table, web plate and horizontal work
Making the distance between platform is 3cm, and it is 50 degree that adjustment, which scrapes angle,.
(3) by the substrate of naturally dry, it is put in table surface, air pump is opened, using negative-pressure adsorption, it is ensured that substrate is solid
It is fixed, problem of misalignment caused by substrate is mobile when preventing from printing.
(4) Graphene conductive ink is uniformly paved into right amount in web plate close to the place printed electrode and is slightly wider than scraper
The bar paten of width.
(5) booting printing, finishes electrode, working electrode, contact conductor and lead one-step print.
(6) it finishes printing, the substrate printed is placed in baking oven, temperature is adjusted to 120 DEG C, toasts 30min.
3, reference electrode prints
(7) slurry of the Graphene conductive ink on screen printer is recycled, cleans web plate, frictioning and scraper with net washing water,
Prepare the web plate for printing b figure pattern in Fig. 1.
(8) substrate of drying is placed on workbench, opens air pump, when placement makes print range be located at print station as far as possible
Center.By adjusting the fixation position of web plate, it is directed at baseline, it is fixed.If passing through the micro- of workbench it was found that still there is a little bias
Knob is adjusted to carry out position adjusting.
(9) by silver paste and silver chlorate slurry agitation uniformly (silver paste and the harmonic proportion of chlorination silver paste in 1:10~10:1,
In the present embodiment it is 5:5), appropriate slurry is uniformly paved into one for being slightly wider than blade width in scraper lower position, print
Brush, forms reference electrode on substrate.
(10) after finishing printing, the substrate printed is placed in baking oven, temperature is adjusted to 120 DEG C, toasts 30min.
4, insulating layer prints
(11) by the silver paste and the recycling of chlorination silver paste mixed slurry on screen printer, web plate and frictioning are cleaned with net washing water,
Scraper prepares for printing c figure pattern web plate in Fig. 1.
(12) substrate of drying is placed on workbench, it is used in the same step of method (7).It is mixed well with appropriate 789 solvent
Dielectric ink, appropriate slurry are uniformly paved into one for being slightly wider than blade width in scraper lower position, printing, on substrate
Form insulating layer.
(13) after finishing printing, the substrate printed is placed in baking oven, temperature is adjusted to 120 DEG C, toasts 30min, drying
After to get arrive screen printing electrode.
5, modified electrode
(14) PSS (poly styrene sulfonate) and aminosalicylic acid are configured to 5mg/mL dispersion liquid, PSS and aminosalicyclic
The ratio of acid is 5:5.
(15) the configured good dispersant liquid drop of 10 μ L is taken to be coated in the working electrode of SPE electrode (i.e. to electrode and working electrode)
Surface, naturally dry, modified electrode work are completed.
6, electrode activation
(16) modification SPE electrode is placed in sulfuric acid or hac buffer or is impregnated in carbonate buffer solution, Ag/
AgCl (3.0M KCl) is reference electrode, and platinum electrode is used as to electrode and SPE electrode as working electrode.First in 0.5-1.2V
Between enclosed with cyclic voltammetry (Cyclic Voltammetric, CV) with the velocity scanning 20 of 1.0V/s, then in 1.5-2.0V
Between, it is enclosed with the velocity scanning 30 of 70mV/s, until electrochemical signals are stablized.
(17) SPE electrode is rinsed with secondary distilled water, dries (or naturally dry in air) under infrared light irradiation, electricity
Pole activation is completed.
Detection:
Detect the trace copper in food.Solution to be measured is immersed into the screen printing electrode lower end, with square wave Stripping Voltammetry
Method measures trace copper in food samples, initial potential -0.05V, electrodeposition current potential -1.30V, current potential increment 0.001V/S, square wave frequency
Rate 20Hz, square wave amplitude 0.02V, electrodeposition time 100s, equilibration time 10s.In the NH4Cl solution system that pH is 4.0 or so,
Cu2+There is sensitive dissolution peak at -0.22V (vs SCE), peak current is in Cu2+Concentration is 2.0 × 10-7~8.0 × 10-5Shi Chengxian
Good linear relationship, regression equation are y=1.035 × 106x+3.426, and related coefficient 0.9997 detects and is limited to 3.1
×10-7moL/L。
Embodiment 4, the production method for present embodiments providing a kind of screen printing electrode based on Graphene conductive ink:
1, substrate pre-processes
(1) PET base cut out is first cleaned by ultrasonic 3 times with acetone, cleans 15min, every time to remove the dirt on its surface
Then dirt is cleaned by ultrasonic 3 times with dehydrated alcohol, cleans 15min, naturally dry every time.
2, electrode print
(2) web plate for being used to print a figure pattern in Fig. 1 is fixed on screen printer horizontal table, web plate and horizontal work
Making the distance between platform is 5cm, and it is 70 degree that adjustment, which scrapes angle,.
(3) by the substrate of naturally dry, it is put in table surface, air pump is opened, using negative-pressure adsorption, it is ensured that substrate is solid
It is fixed, problem of misalignment caused by substrate is mobile when preventing from printing.
(4) Graphene conductive ink is uniformly paved into right amount in web plate close to the place printed electrode and is slightly wider than scraper
The bar paten of width.
(5) booting printing, finishes electrode, working electrode, contact conductor and lead one-step print.
(6) it finishes printing, the substrate printed is placed in baking oven, temperature is adjusted to 150 DEG C, toasts 20min.
3, reference electrode prints
(7) slurry of the Graphene conductive ink on screen printer is recycled, cleans web plate, frictioning and scraper with net washing water,
Prepare the web plate for printing b figure pattern in Fig. 1.
(8) substrate of drying is placed on workbench, opens air pump, when placement makes print range be located at print station as far as possible
Center.By adjusting the fixation position of web plate, it is directed at baseline, it is fixed.If passing through the micro- of workbench it was found that still there is a little bias
Knob is adjusted to carry out position adjusting.
(9) by silver paste and silver chlorate slurry agitation uniformly (silver paste and the harmonic proportion of chlorination silver paste in 1:10~10:1,
In the present embodiment it is 10:1), appropriate slurry is uniformly paved into one for being slightly wider than blade width in scraper lower position, print
Brush, forms reference electrode on substrate.
(10) after finishing printing, the substrate printed is placed in baking oven, temperature is adjusted to 150 DEG C, toasts 20min.
4, insulating layer prints
(11) by the silver paste and the recycling of chlorination silver paste mixed slurry on screen printer, web plate and frictioning are cleaned with net washing water,
Scraper prepares for printing c figure pattern web plate in Fig. 1.
(12) substrate of drying is placed on workbench, it is used in the same step of method (7).It is mixed well with appropriate 789 solvent
Dielectric ink, appropriate slurry are uniformly paved into one for being slightly wider than blade width in scraper lower position, printing, on substrate
Form insulating layer.
(13) after finishing printing, the substrate printed is placed in baking oven, temperature is adjusted to 150 DEG C, toasts 20min, drying
After to get arrive screen printing electrode.
5, modified electrode
(14) PSS (poly styrene sulfonate) and aminosalicylic acid are configured to 10mg/mL dispersion liquid, PSS and amino water
The ratio of poplar acid is 10:1.
(15) the configured good dispersant liquid drop of 10 μ L is taken to be coated in the working electrode of SPE electrode (i.e. to electrode and working electrode)
Surface, naturally dry, modified electrode work are completed.
6, electrode activation
(16) modification SPE electrode is placed in sulfuric acid or hac buffer or is impregnated in carbonate buffer solution, Ag/
AgCl (3.0M KCl) is reference electrode, and platinum electrode is used as to electrode and SPE electrode as working electrode.First in 0.5-1.2V
Between enclosed with cyclic voltammetry (Cyclic Voltammetric, CV) with the velocity scanning 20 of 1.0V/s, then in 1.5-2.0V
Between, it is enclosed with the velocity scanning 30 of 70mV/s, until electrochemical signals are stablized.
(17) SPE electrode is rinsed with secondary distilled water, dries (or naturally dry in air) under infrared light irradiation, electricity
Pole activation is completed.
Detection:
Detect the micro amount of arsenic in food.Solution to be measured is immersed into the screen printing electrode lower end, with square wave Stripping Voltammetry
Method measures micro amount of arsenic in food samples, initial potential -0.05V, electrodeposition current potential -1.30V, current potential increment 0.001V/S, square wave frequency
Rate 20Hz, square wave amplitude 0.02V, electrodeposition time 100s, equilibration time 10s.In the NH4Cl solution system that pH is 4.0 or so,
There is sensitive dissolution peak at 0.36V (vs SCE) in arsenic, and peak current is 2.0 × 10 in arsenic concentration-7~8.0 × 10-5Shi Chengxian is good
Linear relationship, regression equation is y=5.220 × 106x+1.131, related coefficient 0.9995, detection is limited to 0.91 ×
10-7moL/L。
The above described is only a preferred embodiment of the present invention, being not that the invention has other forms of limitations, appoint
What those skilled in the art changed or be modified as possibly also with the technology contents of the disclosure above equivalent variations etc.
It imitates embodiment and is applied to other fields, but without departing from the technical solutions of the present invention, according to the technical essence of the invention
Any simple modification, equivalent variations and remodeling to the above embodiments, still fall within the protection scope of technical solution of the present invention.
Claims (10)
1. a kind of screen printing electrode based on Graphene conductive ink, including substrate, be printed on the substrate working electrode,
To electrode and conductive lead wire, the working electrode and conductive lead wire and to electrical communication between electrode and conductive lead wire, institute
State working electrode and conductive lead wire and between electrode and conductive lead wire pass through lead electrical communication, which is characterized in that it is described
Working electrode is Graphene conductive ink to the material of electrode, conductive lead wire and lead.
2. a kind of screen printing electrode based on Graphene conductive ink according to claim 1, which is characterized in that described
Reference electrode is also printed on substrate.
3. a kind of screen printing electrode based on Graphene conductive ink according to claim 2, which is characterized in that described
The material of reference electrode is the mixture of silver paste and chlorination silver paste.
4. a kind of screen printing electrode based on Graphene conductive ink according to claim 3, which is characterized in that described
A layer insulating is also covered with above lead.
5. a kind of processing method of the screen printing electrode based on Graphene conductive ink described in the claims 4 is processed,
It is characterized in that the following steps are included:
A, Substrate treatment: the substrate reduced first is cleaned by ultrasonic with acetone, is then cleaned by ultrasonic with dehydrated alcohol, is dried in the air naturally
It is dry；
B, electrode print: using Graphene conductive ink as electrode material, on substrate printing work electrode, electrode, conduction are drawn
Line and lead after finishing printing, are sent into an oven, drying；
C, reference electrode prints: using the mixture of silver paste and chlorination silver paste as reference electrode material, reference electricity is printed on substrate
Pole after finishing printing, is sent into an oven, drying；
D, insulating layer prints: using dielectric ink as insulating layer material, insulating layer is printed on substrate, after finishing printing, is sent into and dries
In case, drying, so far screen printing electrode is completed.
6. a kind of processing method of screen printing electrode based on Graphene conductive ink according to claim 5, special
Sign is, further comprising the steps of:
E, modified electrode: being configured to 0.1~10mg/mL dispersion liquid for poly styrene sulfonate and aminosalicylic acid, to be configured complete
Configured dispersant liquid drop is coated in the working electrode surface of screen printing electrode, naturally dry by Cheng Hou.
7. a kind of processing method of screen printing electrode based on Graphene conductive ink according to claim 6, special
Sign is, further comprising the steps of:
F, electrode activation: modification working electrode is placed in sulfuric acid or hac buffer or is soaked in carbonate buffer solution
Bubble is stablized to electrochemical signals, is rinsed with secondary distilled water using cyclic voltammetry,
Drying.
8. according to a kind of described in any item processing of the screen printing electrode based on Graphene conductive ink of claim 5~7
Method, which is characterized in that in a step, by the substrate reduced first with acetone be cleaned by ultrasonic 1~3 time, every time clean 5~
Then 15min is cleaned by ultrasonic 1~3 time with dehydrated alcohol to remove the dirt on its surface, cleans 5~15min every time, dry in the air naturally
It is dry.
9. a kind of processing method of screen printing electrode based on Graphene conductive ink according to claim 6, special
Sign is that the proportion between the poly styrene sulfonate and aminosalicylic acid is 1:10~10:1.
10. a kind of processing method of screen printing electrode based on Graphene conductive ink according to claim 9, special
Sign is, in the step e, the configured dispersant liquid drop of 2~20 μ L is taken to be coated in the working electrode surface of screen printing electrode,
Naturally dry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510685020.1A CN105353009B (en) | 2015-10-20 | 2015-10-20 | A kind of screen printing electrode and its processing method based on Graphene conductive ink |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510685020.1A CN105353009B (en) | 2015-10-20 | 2015-10-20 | A kind of screen printing electrode and its processing method based on Graphene conductive ink |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105353009A CN105353009A (en) | 2016-02-24 |
| CN105353009B true CN105353009B (en) | 2019-02-22 |
Family
ID=55329015
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510685020.1A Active CN105353009B (en) | 2015-10-20 | 2015-10-20 | A kind of screen printing electrode and its processing method based on Graphene conductive ink |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105353009B (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108490040A (en) * | 2018-02-23 | 2018-09-04 | 天智羲王管道科技有限公司 | Graphene gas is printed on one side capacitive sensing structure |
| CN110902645A (en) * | 2018-09-18 | 2020-03-24 | 深圳正峰印刷有限公司 | Printing process of bioelectrical signal sensor |
| CN112057084A (en) * | 2020-09-07 | 2020-12-11 | 浙江大学 | Double-sided screen printing electrode based on flexible plastic substrate and method thereof |
| US20220099673A1 (en) * | 2020-09-28 | 2022-03-31 | Academia Sinica | Biosensor, bio-sensing system comprising the same and method for preparing the same |
| CN112473757B (en) * | 2020-11-19 | 2021-12-17 | 江南大学 | Micro-fluidic chip detection system for food safety rapid detection |
| CN112697866A (en) * | 2020-11-23 | 2021-04-23 | 河北大学 | Printed electrode material, preparation method of printed electrode and application of printed electrode material in quinolone pesticide detection |
| CN112730552B (en) * | 2020-11-26 | 2023-02-10 | 武汉市农业科学院 | Modified screen printing electrode and application thereof |
| CN112697864B (en) * | 2020-12-16 | 2022-04-01 | 浙江大学 | Integrated four-electrode gas sensor and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102507696A (en) * | 2011-10-19 | 2012-06-20 | 浙江大学 | Ion-selective electrode based on graphene electrode and preparation method thereof |
| CN102998348A (en) * | 2012-11-27 | 2013-03-27 | 重庆医科大学 | Preparation method of dehydrogenase-electrochemical biosensor |
| CN202854091U (en) * | 2012-08-19 | 2013-04-03 | 济南大学 | Screen-printed electrode immunosensor synchronously detecting diethylstilbestrol and estradiol |
| CN203083964U (en) * | 2012-09-07 | 2013-07-24 | 济南大学 | Screen-printed electrode sensor prepared by nitrogen doped graphene and used for detecting bisphenol A |
| CN104634848A (en) * | 2015-01-25 | 2015-05-20 | 浙江大学 | Nitrite electrochemical sensor and manufacturing method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8702931B2 (en) * | 2011-04-18 | 2014-04-22 | Indian Institute Of Science | Low cost electrochemical disposable sensor for measuring glycated hemoglobin |
-
2015
- 2015-10-20 CN CN201510685020.1A patent/CN105353009B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102507696A (en) * | 2011-10-19 | 2012-06-20 | 浙江大学 | Ion-selective electrode based on graphene electrode and preparation method thereof |
| CN202854091U (en) * | 2012-08-19 | 2013-04-03 | 济南大学 | Screen-printed electrode immunosensor synchronously detecting diethylstilbestrol and estradiol |
| CN203083964U (en) * | 2012-09-07 | 2013-07-24 | 济南大学 | Screen-printed electrode sensor prepared by nitrogen doped graphene and used for detecting bisphenol A |
| CN102998348A (en) * | 2012-11-27 | 2013-03-27 | 重庆医科大学 | Preparation method of dehydrogenase-electrochemical biosensor |
| CN104634848A (en) * | 2015-01-25 | 2015-05-20 | 浙江大学 | Nitrite electrochemical sensor and manufacturing method thereof |
Non-Patent Citations (1)
| Title |
|---|
| A graphene screen-printed carbon electrode for real-time measurements of unoccupied active sites in a cellulase;Nicolaj Cruys-Bagger et al.;《Analytical Biochemistry》;20131201;第447卷;全文 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105353009A (en) | 2016-02-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105353009B (en) | A kind of screen printing electrode and its processing method based on Graphene conductive ink | |
| Li et al. | Novel hierarchical sea urchin-like Prussian blue@ palladium core–shell heterostructures supported on nitrogen-doped reduced graphene oxide: Facile synthesis and excellent guanine sensing performance | |
| Tan et al. | Electrochemical sensor based on molecularly imprinted polymer reduced graphene oxide and gold nanoparticles modified electrode for detection of carbofuran | |
| Niu et al. | Electrochemical stripping analysis of trace heavy metals using screen-printed electrodes | |
| CN103308675B (en) | The preparation of the screen printing electrode immunosensor of quick detection Microcystin and detection method | |
| CN103675066B (en) | A kind of preparation of sulfhydrylation graphene modified electrode and trace heavy metal detection method thereof | |
| Zhang et al. | High sensitive on-site cadmium sensor based on AuNPs amalgam modified screen-printed carbon electrodes | |
| Bernalte et al. | Characterisation of screen-printed gold and gold nanoparticle-modified carbon sensors by electrochemical impedance spectroscopy | |
| CN202854091U (en) | Screen-printed electrode immunosensor synchronously detecting diethylstilbestrol and estradiol | |
| CN107345931B (en) | It is a kind of based on carbonitride-binary metal boron oxide compound composite material bisphenol-A optical electro-chemistry sensor and its preparation and application | |
| Tran et al. | Micro-patterning of single-walled carbon nanotubes and its surface modification with gold nanoparticles for electrochemical paper-based non-enzymatic glucose sensor | |
| CN106053564B (en) | A kind of method that graphite-phase nitrogen carbide-chitosan-modified electrode detects protocatechuic acid as working electrode | |
| CN105466991B (en) | Bisphenol-A disposable paper base sensor and its preparation method and application | |
| CN107389763A (en) | A kind of carbon paste electrode and its preparation, detection method for being used to detect hydroquinones | |
| CN105784804A (en) | Graphene screen printing electrode and method for heavy metal ion detection | |
| CN107202828A (en) | A kind of estradiol optical electro-chemistry sensor and its preparation and application based on boron doping iron cobalt/cobalt oxide two-dimensional nano composite | |
| Zhao et al. | All-printed flexible electrochemical sensor based on polyaniline electronic ink for copper (II), lead (II) and mercury (II) ion determination | |
| CN105928996A (en) | Preparation of graphene oxide and polyaniline-modified electrode and assembled electrochemical detection device | |
| CN203083964U (en) | Screen-printed electrode sensor prepared by nitrogen doped graphene and used for detecting bisphenol A | |
| Petroni et al. | Simple and inexpensive electrochemical platform based on novel homemade carbon ink and its analytical application for determination of nitrite | |
| Aguila et al. | A biosensor based on Coriolopsis gallica laccase immobilized on nitrogen-doped multiwalled carbon nanotubes and graphene oxide for polyphenol detection | |
| CN102692435A (en) | Method for detecting 1,8-diaminonaphthalene based on electrochemical DNA biosensor | |
| CN103402327B (en) | A kind of manufacture method printed electrode for Portable heavy metal detection | |
| CN109399556A (en) | A kind of preparation method of the flexible micro-nano pressure sensor based on mode of printing | |
| CN104614428A (en) | Nano-silver ink-based inkjet printing silver/silver chloride reference electrode and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |