CN105784804A - Graphene screen printing electrode and method for heavy metal ion detection - Google Patents
Graphene screen printing electrode and method for heavy metal ion detection Download PDFInfo
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Abstract
The invention discloses a graphene screen printing electrode and method for heavy metal ion detection. The electrode comprises a work electrode, a counter electrode, and a silver chloride reference electrode; graphene powder is taken as the printing slurry to paint the matrix of the work electrode, the work electrode is prepared by a screen printing technology, is individually modified by a chemistry technology, and has an electrode standard layer, which is prepared by printing UV-cured insulating slurry and then curing the slurry by ultraviolet light; the counter electrode is prepared by painting carbon powder printing oil and silver-silver chloride slurry on another matrix; and the electrodes are assembled together through silicone rubber. The invention also discloses a preparation method of the screen printing electrode and a method using the screen printing electrode to detect heavy metal ions. The screen printing electrode and method can be widely used in each field of electrochemical analysis, and the screen printing electrode is especially for the stripping voltammetry for detecting heavy metal ions in surface water, sewage, and beverage.
Description
Technical field
The present invention relates to a kind of Graphene screen printing electrode for detection of heavy metal ion and method, more particularly to a kind of detection of heavy metal ion method based on Graphene screen printing electrode, belong to sensor technical field.
Background technology
The method detecting heavy metal at present mainly has following several: Atomic fluorophotometry (AFS), inductivity coupled plasma mass spectrometry analytical technology (ICP-MS), electrochemical methods, inductively coupled plasma atomic emission spectrum (ICP-AES), high performance liquid chromatography (HPLC), inhibiting AChE, immunoassay, biosensor etc..Wherein the measurement signal of electrochemical analysis method is the signals of telecommunication such as conductance, current potential, electric current, electricity, need not analyze the conversion of signal just can direct record, so the apparatus of electro chemical analysis can accomplish simple miniaturization, it easily is automated and analyzes continuously, being a kind of generally acknowledged quick, sensitive, trace analysis methods accurately, this is also the theoretical foundation that this programme adopts electrochemical methods.
The ultimate principle of electrochemical analysis method is to insert special electrode in solution to be measured, and on electrode, apply specific voltage waveform, promote generation electrochemical reaction in solution, electrode will flow through the faradic currents relevant to material composition in solution, gather and analyze current value and can obtain the configuration information of material composition.Electrochemical reaction electrode, especially working electrode, be the core component of electrochemical analysis method.For stripping voltammetry, being generally adopted three-electrode system to eliminate the IR impact dropped, three electrodes include reference electrode, to electrode (auxiliary electrode), working electrode.Reference electrode generally uses saturated calomel electrode or Ag/AgCl electrode, and electrode generally uses chemically inert platinum electrode, and the kind of working electrode is then a lot, is broadly divided into mercury electrode and the big class of solid electrode two.
Solid electrode is the emphasis of research at present, and its advantage is to use under the electromotive force of calibration, it is possible to by driven by motor high speed rotating, easy to use pollution-free in continuous mobile monitoring system.The preparation of solid electrode is simple, and material shape etc. designs also dependent on needs, and common shape has plate-like, netted, thread, tubulose, spherical etc., and material aspect mostly is noble metal and various carbon electrode, such as Pt, Au, Ag, carbon and graphite etc..
Screen printing electrode sensor technology provide not only the probability of industrialized production, and advantageously account for online, in body is analyzed the problem such as the stability of electrode response, repeatability and cross-contamination, make simple, cheap, be easy to carry, easily microminiaturized and integrated, be the new detecting technique of a kind of great development prospect.The ultimate principle of screen printing technique is: the mesh of screen printing forme image section can pass through ink and bite to stock, and on forme, remainder mesh blocks and can not pass through ink, forms blank on the substrate.The pattern printed mostly adopts photochemistry graphic arts process (i.e. sensitizer stencil making method).With silk screen for supporter, by screen tension on screen frame, on silk screen, then it is coated with photoresists, form light-sensitive surface, then will be combined at the bottom of positive image on light-sensitive surface, through exposure and development, the mesh needing ink image part on forme is not closed, and during printing, ink passes through, then printing forms pattern.Screen printing electrode bar often includes working electrode, reference electrode, auxiliary electrode.The ink of bar of printing electrode generally mainly has silver-colored ink and the big class of carbon printing ink two.Silver ink is used for printing the base rail making electrode strip, to improve electric conductivity；Carbon printing ink is layered on silver rail, as auxiliary electrode, can print Ag-AgCl powder as silver chloride reference electrode.Working electrode can be prepared by bronze, argentum powder, carbon dust ink.
Cognitive based on above each point, present inventors have recognized that grapheme material is a kind of Two-dimensional Carbon material, there is excellent electricity and electrochemical properties, plan to select graphene powder material to replace carbon printing ink material, and adopt screen printing technique preparation to prepare graphene powder screen printing electrode as working electrode based on screen printing technique, so that the significantly improving of electrode performance, and it is expected to the detection for trace heavy metal ion.Thus forming the design of the present invention.
Summary of the invention
It is an object of the invention to provide the screen printing electrode of a kind of graphene powder material, preparation method and the detection of heavy metal ion method based on this electrode, measure, to overcome existing silver or the easy amalgamate of gold electrode to cause, the shortcoming that repeatability is poor.
A kind of screen printing electrode of graphene powder, it is characterized in that, including adopting graphene powder as working electrode printing slurry, the working electrode being prepared and being individually chemically modified process by screen printing technique on a matrix, this working electrode has one adopt light admittedly to insulate slurry prints with the electrode specification layer of ultraviolet light polymerization；Another matrix adopts carbon dust ink and silver-silver chloride slurry print to electrode and silver chloride reference electrode；Electrode and silver chloride reference electrode surface are had the electrode dielectric layer that an insulation slurry is printed by described auxiliary；Described working electrode, silicone rubber is adopted to be assemblied together at electrode and silver chloride reference electrode.Described graphene powder, adopts chemical gaseous phase depositing process to prepare.
A kind of screen printing electrode preparation technology, it is characterised in that comprise the following steps: on an electrode matrix, adopts graphene powder as printing slurry, prepares Graphene working electrode by screen printing technique and dry；Electrode surface insulation slurry printed electrode insulating barrier；On another electrode matrix, carbon dust ink and silver-silver chloride slurry is adopted to print electrode and reference electrode and dry；To electrode and reference electrode surface insulation slurry printed electrode insulating barrier；Graphene working electrode is individually chemically modified process；Adopt silicone rubber by described working electrode, carbon to electrode and silver chloride reference electrode assembling to together with.
A kind of screen printing electrode preparation technology, it is characterised in that in Graphene working electrode printing process, drying temperature is 80～100 DEG C；In the described printing process to electrode and reference electrode, drying temperature is 100～150 DEG C.
Described chemical modification processes: is soaked in by Graphene working electrode in the mercuric chloride dressing agent solution of 0.1～0.2mol/mL and reduces at constant potential-0.3～-0.1V (relative to saturated calomel electrode), the preferred value of constant potential is-0.2V, cleans 2-4 clean dry for standby with distilled water.
A kind of method applying described screen printing electrode mensuration heavy metal ion, it is characterized in that: in acetate buffer solution, add sample to be tested, solution is immersed in described screen printing electrode lower end, adopts stripping volt ampere analysis method, measure concentration of heavy metal ion according to the peak current obtained.Described heavy metal is copper, lead or cadmium.
The present invention is had the advantage that: instant invention overcomes the deficiency that exists of mercury film electrode being matrix with silver or gold electrode, it is provided that a kind of make simply, cost is low and highly sensitive, the screen printing electrode preparation technology of favorable reproducibility and surface modification method.Compared with prior art, it is many that Graphene electrodes has detection heavy metal kind to the present invention, and chemical stability height, specific surface area is big, and sensitivity is advantages of higher more.Working electrode individually prints and is convenient for chemical modification, it is to avoid modify contaminated aqueous solution Ag/AgCl reference electrode.Graphene electrodes working electrode is particularly suitable for the Voltammetry heavy metal ion in food analysis and environmental monitoring (such as Pb2+、Cu2+Deng).
Accompanying drawing explanation
Fig. 1 is silk screen printing Graphene electrodes structural representation of the present invention.
In figure: 1.Ag/AgCl reference electrode；2. carbon is to electrode；3. Graphene working electrode；4. insulating barrier.
Detailed description of the invention
Below in conjunction with accompanying drawing, the invention will be further described.
Embodiment 1: a kind of graphene powder screen printing work technology for preparing electrode prepared based on silk screening techniques through chemical modification
Described in summary of the invention, Graphene screen printing electrode of the present invention is to adopt silicone rubber to assemble the Ag/AgCl reference electrode of electrode with carbon the working electrode of the Graphene screen printing electrode through chemical modification.The spacing of electrode is 1cm by Ag/AgCl reference electrode and carbon, between Graphene screen printing work electrode is located therein.
So, the preparation work of graphene powder screen printing electrode is the importance implementing the present invention, so the processing technology of graphene powder silk screen Yin Sa technology for preparing electrode first gives details are as follows:
(1) PVC matrix of the size (250 × 200mm) that cuts with a paper cutter out etc., first cleans the substrate cut out with detergent, to remove the dirt on its surface, then clean with dehydrated alcohol, then rinse for several times with secondary water, be put in baking oven, 90 DEG C, 15min, dry for standby.
(2) before printed electrode, half tone, the workbench of instrument, frictioning and scraper are cleaned after cotton dips a small amount of net washing water and cleans, to remove the superincumbent dust of attachment, it is ensured that the quality of printing.
(3) first piece of half tone is then fixed, the distance of about 3mm between half tone and horizontal table；Adjust the position of scraper and frictioning, so as to become 70 degree of angles with horizontal plane.Tentatively regulated its dynamics by knob bolts, dynamics is too big, it is possible to can scratch half tone, and dynamics is too little, and slurry may not print.After adjusting, by half tone pinch grip lock jail.Adding the viscosity of appropriate solvent adjustment Graphene slurry, and stir, appropriate slurry is in half tone near the place printed electrode, and is uniformly paved into the bar paten being slightly wider than blade width.
(4) substrate step (1) dried, is put in table surface, opens air pump, adopts negative-pressure adsorption, it is ensured that substrate is fixed, it is prevented that during printing, the problem of misalignment caused is moved in substrate.
(5) start, examination print, again adjust the dynamics of scraper and frictioning, it is ensured that reached good printing effect.Semiautomatic-mode is selected during printing.
(6) ground floor Graphene slurry finishes printing, and places in baking oven, 90 DEG C, 30min.
(7) reclaim additional size, clean half tone, frictioning and scraper with net washing water, prepare second block of web plate.
(8) substrate of drying is taken a piece of it is positioned on workbench, open air pump, during placement, make print range be positioned at print station central authorities as far as possible.
(9) by adjusting the fixed position of half tone, baseline is made to be directed at, fixing.If finding to still have a little bias, carry out position adjustments by the vernier knob of workbench.
(10) being stirred by Graphene slurry, appropriate slurry is in scraper lower position, is uniformly paved into one that is slightly wider than blade width, printing.
(11), after finishing printing, baking oven is placed, 90 DEG C, 15min.
Embodiment 2: the concentration of lead ion in screen printing electrode detection sample in Application Example 1
The inventive sensor (i.e. Graphene screen printing electrode described in the embodiment 1) method for detecting content of heavy metal lead, adopts stripping volt ampere analysis method, first, is connected with electrochemical analytical instrument by described sensor；Secondly, sample to be tested is mixed with 5mL0.1M acetic acid/sodium acetate solution；Finally, sensor electrode lower end being immersed solution, start stripping volt ampere analysis method, voltammetry analytical parameters is: burning voltage+0.55V50s, accumulating potential-0.6V120s, equilibration time 40s, square wave amplitude 36mV, current potential step value 3mV, frequency 15Hz, operating potential window :-0.6V-+0.2V.Presenting good linear relationship within the scope of dissolution peak current and≤1000 μ g/L lead concentrations, phase relation is 0.997, and detection is limited to 1.06 μ g/L.
Embodiment 3: in Application Example 1, screen printing electrode is to the assay method of trace copper in sample
Solution to be measured is immersed in described screen printing electrode lower end, measures trace copper in beverage sample, initial potential-0.05V with square wave stripping voltammetry, electrodeposition current potential-1.30V, current potential increment 0.001V/S, square wave frequency 20Hz, square wave amplitude 0.02V, electrodeposition time 100s, equilibration time 10s.In the NH4Cl solution system that pH is about 4.0, Cu2+Sensitive dissolution peak occur at-0.22V, dissolution peak current is at Cu2+Concentration presents good linear relationship when being 1-500ug/L, detection is limited to 1ug/L.
It must be noted that the graphene powder CVD method that the present invention relates to prepares (such as CN2014102565656, CN201410364096X etc.), the insulating layer material etc. of Graphene slurry and use it is made up of graphene powder, it is all that described in prior art or " a kind of carbon nanocoils tiny array electrode preparation method for detection of heavy metal ion " filed an application with the application, no further details to be given herein simultaneously.
Claims (7)
1. a Graphene screen printing electrode, it is characterised in that including:
1. adopt graphene powder as working electrode printing slurry on an electrode matrix, by screen printing technique preparation and be individually chemically modified the working electrode of process, this working electrode has adopt light admittedly to insulate an electrode specification layer using ultraviolet light polymerization that slurry prints；
2. on another electrode matrix, adopt that carbon dust ink and silver-silver chloride slurry print to electrode and silver-silver chloride reference electrode；Electrode and silver-silver chloride reference electrode surface are had the electrode dielectric layer that an insulation slurry is printed by described carbon；
3. described working electrode, silicone rubber is adopted to assemble at electrode and silver-silver chloride reference electrode；
Described electrode matrix is PVC material；
Described chemical modification processes: is soaked in by Graphene working electrode in the mercuric chloride dressing agent solution of 0.1～0.2mol/mL and is reducing relative to saturated calomel electrode constant potential-0.3～-0.1V.
2. by the electrode described in claim 1, it is characterised in that:
1. the constant potential that chemical modification processes is-0.2V；
2. the spacing of electrode is 1cm and between Graphene working electrode is located therein by Ag/AgCl reference electrode and carbon.
3. the method making electrode as claimed in claim 1 or 2, it is characterized in that graphene powder screen printing work electrode step is: on an electrode matrix, adopt graphene powder as printing slurry, prepare Graphene working electrode by screen printing technique and dry；Electrode surface insulation slurry printed electrode insulating barrier；On another electrode matrix, carbon dust ink and silver-silver chloride slurry is adopted to print electrode and reference electrode and dry；To electrode and reference electrode surface insulation slurry printed electrode insulating barrier；Graphene working electrode is individually chemically modified process；Adopt silicone rubber by described working electrode, to electrode and silver chloride reference electrode assembling to together with.
4. method as claimed in claim 3, it is characterised in that:
(1) manufacturing process steps of Graphene working electrode is:
1. before printed electrode, clean after half tone, the workbench of instrument, frictioning and scraper are first dipped a small amount of net washing water with cleaning cotton, to remove the superincumbent dust of attachment；
2. first piece of half tone is then fixed, the distance of 3～5mm between half tone and horizontal table；Adjusting the position of scraper and frictioning again, so as to become 70 degree of angles with horizontal plane, tentatively regulated its dynamics by knob bolts, dynamics is too big, it is possible to can scratch half tone, and dynamics is too little, and slurry may not print；After adjusting, by half tone pinch grip lock jail.Add the viscosity of appropriate solvent adjustment Graphene slurry, and stir, fall slurry in the close place printed electrode of half tone, be uniformly paved into the bar paten being slightly wider than blade width；
3. the matrix will dried, is put in table surface, opens air pump, adopts negative-pressure adsorption, it is ensured that substrate is fixed, it is prevented that during printing, matrix moves the problem of misalignment caused；
4. start shooting, examination print, again adjust the dynamics of scraper and frictioning, it is ensured that the printing effect reached；Semiautomatic-mode is selected during printing；
5. ground floor Graphene slurry finishes printing, and places in baking oven, 80～100 DEG C, 30min；
6. reclaim additional size, clean half tone, frictioning and scraper with net washing water, prepare second block of web plate；
7. the substrate of drying is taken and a piece of be positioned on workbench, open air pump, during placement, make print range be positioned at print station central authorities as far as possible；
8. by adjusting the fixed position of half tone, baseline is made to be directed at, fixing.If finding to still have a little bias, carry out position adjustments by the vernier knob of workbench；
9. being stirred by Graphene slurry, appropriate slurry is in scraper lower position, is uniformly paved into one that is slightly wider than blade width, printing；
10., after finishing printing, baking oven is placed, 80～100 DEG C, 15min；
(2) on the electrode matrix of another drying, make carbon to electrode and Ag/AgCl reference electrode, dry temperature 100～150 DEG C；
(3) silicone rubber is adopted to be assembled into electrode at electrode and Ag/AgCl reference electrode in the Graphene working electrode on (1) and (2) two electrode matrixs dried, carbon；
Described drying electrode matrix is the equal-sized PVC matrix that cuts with a paper cutter out, is first cleaned with detergent by the matrix cut out, to remove the dirt on its surface, then clean with dehydrated alcohol again, then rinse for several times with secondary water, be put in baking oven, 90 DEG C, 15min, dry.
5. by the method described in claim 4, it is characterised in that:
1. described electrode matrix is of a size of 250 × 200mm；
2. the operating temperature of Graphene 90 DEG C.
6. the electrode described in claim 1 or 2 is for the method for detection of heavy metal ion, it is characterized in that addition sample to be tested in acetate buffer solution, solution is immersed in described screen printing electrode lower end, adopt stripping volt ampere analysis method, measuring concentration of heavy metal ion according to the peak current obtained, described heavy metal is copper, lead or cadmium.
7. by the method described in claim 6, it is characterised in that:
1. the step of employing stripping volt ampere analysis method detection heavy metal Pb is: first, be connected with electrochemical analytical instrument by described sensor；Secondly, sample to be tested is mixed with 5mL0.1M acetic acid/sodium acetate solution；Finally, sensor electrode lower end being immersed solution, start stripping volt ampere analysis method, voltammetry analytical parameters is: burning voltage+0.55V50s, accumulating potential-0.6V120s, equilibration time 40s, square wave amplitude 36mV, current potential step value 3mV, frequency 15Hz, operating potential window :-0.6V-+0.2V；Presenting linear relationship within the scope of dissolution peak current and lead concentration 0≤1000 μ g/L, phase relation is 0.997, and detection is limited to 1.06 μ g/L；
2. solution to be measured is immersed in described screen printing electrode lower end, measure trace copper in beverage sample, initial potential-0.05V with square wave stripping voltammetry, electrodeposition current potential-1.30V, current potential increment 0.001V/S, square wave frequency 20Hz, square wave amplitude 0.02V, electrodeposition time 100s, equilibration time 10s；It is the NH of 4.0 at pH4In Cl solution system, Cu2+Sensitive dissolution peak occur at-0.22V, dissolution peak current is at Cu2+Concentration presents good linear relationship when being 1-500ug/L, detection is limited to 1ug/L.
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| CN108318543A (en) * | 2018-01-30 | 2018-07-24 | 河海大学常州校区 | A kind of heavy metal ion sensor and its operating method based on grapheme material |
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| CN114216948A (en) * | 2021-11-01 | 2022-03-22 | 佛山科学技术学院 | Electrochemical method for detecting arsenic ions in solution |
| CN114216948B (en) * | 2021-11-01 | 2023-09-26 | 佛山科学技术学院 | Electrochemical method for detecting arsenic ions in solution |
| CN114487030A (en) * | 2022-03-30 | 2022-05-13 | 山东省科学院海洋仪器仪表研究所 | High-precision ocean conductivity measuring electrode manufacturing method based on silk-screen printing |
| CN115372429A (en) * | 2022-07-21 | 2022-11-22 | 桂林电子科技大学 | Construction method of screen printing electrode of single-channel double-working electrode |
| CN115372429B (en) * | 2022-07-21 | 2024-08-13 | 桂林电子科技大学 | Construction method of screen printing electrode of single-channel double-working electrode |
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