WO2020220106A1 - Modification de la surface d'électrodes sérigraphiées - Google Patents

Modification de la surface d'électrodes sérigraphiées Download PDF

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Publication number
WO2020220106A1
WO2020220106A1 PCT/BR2020/050150 BR2020050150W WO2020220106A1 WO 2020220106 A1 WO2020220106 A1 WO 2020220106A1 BR 2020050150 W BR2020050150 W BR 2020050150W WO 2020220106 A1 WO2020220106 A1 WO 2020220106A1
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WO
WIPO (PCT)
Prior art keywords
modification
screen
printed electrodes
surface according
electrode
Prior art date
Application number
PCT/BR2020/050150
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English (en)
Portuguese (pt)
Inventor
Luiz Ricardo Goulart Filho
Eliton Souto De MEDEIROS
Ana Flávia Oliveira NOTÓRIO
Fabiane Nunes RIELLO
Kaline Do Nascimento FERREIRA
Maria Júlia Rodrigues Da CUNHA
Original Assignee
Cirino Alberto Goulart Eireli - Epp (Biogenetics)
Universidade Federal de Uberlândia
Universidade Federal Da Paraíba - Ufpb
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Cirino Alberto Goulart Eireli - Epp (Biogenetics), Universidade Federal de Uberlândia, Universidade Federal Da Paraíba - Ufpb filed Critical Cirino Alberto Goulart Eireli - Epp (Biogenetics)
Publication of WO2020220106A1 publication Critical patent/WO2020220106A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/28—Electrolytic cell components
    • G01N27/30—Electrodes, e.g. test electrodes; Half-cells
    • G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/48—Biological material, e.g. blood, urine; Haemocytometers
    • G01N33/50—Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/04—Processes of manufacture in general
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the present invention relates to the synthesis, characterization and application of polymeric blends as tools to improve the reading signal, homogenize the surface and facilitate the passage of current in printed electrodes (screen-printed).
  • the invention comprises polymeric structures enriched with different nanomaterials capable of potentiating the electrochemical signal in potentiostat using screen-printed electrodes for diagnosing diseases caused by pathogens and recognized from species-specific ligands.
  • Electrochemistry has as its fundamental objective the study of systems capable of generating useful electrical work from oxirreduction reactions, called galvanic cells, or the reverse process: systems that undergo the oxirreduction process when subjected to electrical work .
  • the electrochemical system is then formed, at least, by two electrodes, or electronic conductors, immersed in an electrolyte that carries the ions.
  • the conduction of electricity being an intrinsic characteristic of the components of this system (TICIANELLI, E. A .; GONZALEZ, E. R. Electrochemistry: Principles and Applications. 2. ed. S ⁇ o Paulo: Edusp, 2005).
  • REPLACEMENT SHEET (RULE 26) previously described. They are: charge transfer (formation of a pair of reactions on the electrodes); ionic conduction (movement of species in the electrolytic solution); displacement of electrode potentials (electrode polarization phenomenon) (TICIANELLi, EA; GONZALEZ, ER Electrochemistry: Principles and Applications. 2. ed. S ⁇ o Paulo: Edusp, 2005).
  • the formation of the double electrical layer is of fundamental importance, since it is formed by the border region between two phases with different compositions leading to the formation of anisotropic forces.
  • the result will be the appearance of a potential difference between the surface and the interior of the solution, which, in this case, can be controlled by an external circuit.
  • This allows to control externally the adsorption of charges and dipoles (TICIANELLI, E. A .; GONZALEZ, E. R. Electrochemistry: Principles and Applications. 2. ed. S ⁇ o Paulo: Edusp, 2005). Together, all of these phenomena will be important for the characterization and functionalization of the electrode surface in a modified electrochemical system.
  • the electrochemistry technique can be considered an object of measurement of species of different natures and associated with a signal transducer system together with processing software allows the creation of (bio) sensors. Able to transform, in this case, currents generated through oxy-reduction reactions into a computational signal that can be interpreted to understand various reactions that take place on the electrode surface (COBBOLD, RSC Transducers for Biomedical Measurements, 1974).
  • IUPAC International Union of Pure and Applied Chemistry
  • biosensors When compared with existing diagnostic techniques for diseases, biosensors have several advantages, including ease of handling, low cost of production, rapid diagnosis, high sensitivity and specificity (SANTANA, LK L, RICARDO, P. C CincinnatiSERUDO, RL, LASMAR, ML, SANTOS, MC; Electrochemical immunosensors and their applications. Scientia Amazónia, Si, v. 6, n. 1, p.31 -41, 2017.
  • the patent BR 102015007505-6 A2 discusses the modification of the electrode surface through the self-assembly technique using magnetic nanoparticles coated with nanoparticles in the construction of diagnostic sensors for schistosomiasis.
  • the patent BR 102012021218-8 A2 uses printed electrodes of modified carbon ink after coming into contact with a solution based on a strong base and crosslinking agent.
  • a polymeric xyloglucan film is used as pre-treatment and stabilization in the construction of a diagnostic sensor for toxic components of Ricina.
  • the patent BR 102016018862-8 A2 brings a different modification, composite electrodes based on graphites and thermoplastic polymers. These electrodes are produced using the dissolution and drying technique and serve to determine organic and inorganic analytes and can be used over a wide pH range and in different electrolytic media.
  • the patent BR 102015028052-1 A2 describes the electrochemical polymerization of poly (3-hydroxyphenolacetic acid) by aqueous dispersion for modification of gold electrodes to form a matrix and hybridization of oligonucleotides in the construction of biosensors.
  • US patent 20130209807 A1 uses modified carbon nanotube sheets for partial or total modification of electrodes that can be applied to sensors, including biosensors.
  • the present invention aims to develop a matrix of polymeric blends enriched with nanomaterials and / or chemical compounds as a tool for modifying the surface of graphite “screen-printed” electrodes.
  • the acquisition of micro and nanofibers that constitute the polymeric matrix was based on the production of solutions of polymeric blends of hydrophobic polymers such as, for example, poly (lactic acid), PLA, and hydrophilic polymers, such as, poly (ethylene glycol), PEG, but not exclusive to these polymers.
  • the solutions can be enriched with other nanomaterials (such as nanotubes and nanoparticles) and these materials may or may not be associated with chemical compounds, both in concentrations varying from 0.5 to 50% of the total polymer mass used (m / m).
  • These solutions will be injected through a system of concentric nozzles, preferably, but not exclusive, at a fixed rate of 10 to 750 uL / min, ideally between 70 and 130 uL / min.
  • the external nozzle will release through a compressed gas system (stored in a cylinder or produced in a compressor) the gas with a pressure of 5 to 100 psi, which is responsible for dragging the enriched polymer solutions (100/0 - 0 / 100% m / v or v / v) transforming them into fibers, ejected towards the collector.
  • a compressed gas system stored in a cylinder or produced in a compressor
  • FTIR analysis allows the determination of the presence of materials and / or chemical compounds, incorporated in the fibers, through their bands or absorbance peaks in the infrared region.
  • Cyclic voltammetry analysis technique in which a potential is applied to the working electrode and the originating electric current is measured. Through this technique it is possible to evaluate the formed oxy-reduction profile. The modification leads to an increase in the measured current reading.
  • Figure 1 shows the micrograph of the micro and nanofibrillar structure of the polymeric matrix in question.
  • Figure 2 shows the graphs of mass loss and derived from the mass losses of the constituent materials and of the polymeric matrix acquired by thermogravimetry, showing the thermal behavior until its degradation.
  • Figure 3 shows the thermal curves obtained by differential scanning calorimetry (DSC), in order to evaluate the processing of the materials produced for the claim in question.
  • DSC differential scanning calorimetry
  • Figure 4 presents the graphs of Fourier Transform Infrared Spectroscopy (FTIR), to which it was possible to identify the absorption frequencies of the functional groups characteristic of the constituent materials and of the polymeric matrices.
  • FTIR Fourier Transform Infrared Spectroscopy
  • Figure 5 shows a schematic of the electrode model used.
  • the diagram illustrates the divisions of the printed electrodes: where 1 is the work area; 2 the counter electrode (both of the same material); 3 represents the silver-coated reference electrode.
  • the diagram illustrates how the polymeric matrix is placed on the electrode, in the work area, for functionalization.
  • Figure 6 illustrates three graphs of the reading in cyclic voltammetry.
  • the readings were made on ten different virgin electrodes, without modification on the surface, and there is no pattern in the curves read.
  • the cyclic voltammetry reading was performed on the same electrodes after the modification and in this case the curves have already demonstrated a standard behavior in all electrodes.
  • the voltammetry technique was used on stabilized electrodes after successive washes.
  • Figure 7 is a Scanning Electron Microscopy image of the work surface of the virgin electrode and the modified electrode.
  • the images (A), (C) and (E) refer to the surface of a virgin electrode in different magnifications.
  • the images are of the surface of an electrode modified in different magnifications.
  • Figure 8 is an image and the respective EDS analysis graph - capable of analyzing the electrode surface components.
  • the image shows the field in which the EDS analysis was performed and in (B) which chemical components were found during the analysis and the respective quantity in proportions for the virgin electrode.
  • (C) and (D) respectively represent the field in which the analysis was performed and the quantification of chemical elements for the modified electrode.
  • Figure 9 represents the graphs of reading by cyclic voltammetry with different scanning speeds to determine the active area of the electrode using the Randles-Sevicik formula.
  • (A) represents the reading graph of different cyclic voltammetry curves with increasing scan speed for the virgin electrode, compared with the readings made on two electrodes with different modifications (in C and E).
  • the lines represented in the graphs (B), (D) and (F) refer to the peak currents, obtained from the cyclic voltammetry curves, for each scan speed.
  • FIG 10 are the graphs representing the active areas of the electrodes, before and after modification with the different types of polymeric matrix.
  • the data are in unit of measure with absolute values and in (B) a normalization of the same data was made to percentage taking as reference the virgin electrode.
  • the nomenclatures from El to E-VII, visible in both (A) and (B) refer to different types of material combinations for modifying the electrode surface.
  • Figure 11 represents cyclic voltammetry readings for different phases of changes in the electrode surface, throughout the process.
  • the continuous line represents the virgin electrode, without modification
  • the dotted line represents in (A) the modification with the polymeric matrix and in (B) the sample adsorption after the modification.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Molecular Biology (AREA)
  • Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Analytical Chemistry (AREA)
  • Pathology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Nanotechnology (AREA)
  • Urology & Nephrology (AREA)
  • Hematology (AREA)
  • Biomedical Technology (AREA)
  • Inorganic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Biotechnology (AREA)
  • Cell Biology (AREA)
  • Composite Materials (AREA)
  • Microbiology (AREA)
  • Manufacturing & Machinery (AREA)
  • Food Science & Technology (AREA)
  • Medicinal Chemistry (AREA)
  • Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)

Abstract

La présente invention concerne la synthèse, la caractérisation et l'utilisation de mélanges polymères comme moyens pour améliorer le signal de lecture, homogénéiser la surface et faciliter le passage de courant dans des électrodes sérigraphiées. Ainsi, l'invention concerne des matrices polymères enrichies en différents nanomatériaux. Ces matériaux sont capables de potentialiser le signal électrochimique en potentiostat utilisant des électrodes sérigraphiées pour le diagnostic de maladies causées par des agents pathogènes et reconnues à partir de ligands espèce-spécifiques.
PCT/BR2020/050150 2019-05-02 2020-05-04 Modification de la surface d'électrodes sérigraphiées WO2020220106A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
BRBR1020190089628 2019-05-02
BR102019008962-8A BR102019008962A2 (pt) 2019-05-02 2019-05-02 modificação da superfície de eletrodos screen-printed

Publications (1)

Publication Number Publication Date
WO2020220106A1 true WO2020220106A1 (fr) 2020-11-05

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BR (1) BR102019008962A2 (fr)
WO (1) WO2020220106A1 (fr)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007120442A2 (fr) * 2003-07-25 2007-10-25 Dexcom, Inc. Système d'électrode double pour capteur d'analyte continu
BR102016018862A2 (pt) * 2016-08-16 2018-03-06 Universidade Federal Do Rio De Janeiro - Ufrj Eletrodos compósitos a base de grafite e polímeros termoplásticos

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007120442A2 (fr) * 2003-07-25 2007-10-25 Dexcom, Inc. Système d'électrode double pour capteur d'analyte continu
BR102016018862A2 (pt) * 2016-08-16 2018-03-06 Universidade Federal Do Rio De Janeiro - Ufrj Eletrodos compósitos a base de grafite e polímeros termoplásticos

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
ZARE, Y ET AL.: "Polymer/metal nanocomposites for biomedical applications", MATERIALS SCI. AND ENGINEERING, 2016, pages 195 - 203, XP029365410, DOI: 10.1016/j.msec.2015.11.023 *

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