CN114334223A - Conductive slurry and application thereof - Google Patents
Conductive slurry and application thereof Download PDFInfo
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- CN114334223A CN114334223A CN202111388623.7A CN202111388623A CN114334223A CN 114334223 A CN114334223 A CN 114334223A CN 202111388623 A CN202111388623 A CN 202111388623A CN 114334223 A CN114334223 A CN 114334223A
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Abstract
The invention provides a conductive paste and application, wherein the conductive paste is obtained by mixing Prussian blue, a carbon source, a binder and a solvent, and the conductive paste can be prepared into a working electrode of an electrochemical sensor in a screen printing mode, so that the preparation method is simple and convenient and is easy to popularize; the electrochemical sensor composed of the working electrode is used for detecting hydrogen peroxide, and the electrochemical sensor electrode pair H directly prepared from the conductive paste2O2The detection has higher selectivity and sensitivity.
Description
Technical Field
The invention belongs to the technical field of conductive materials, and particularly relates to conductive paste and application thereof.
Background
With the development of interdisciplines in a new era, knowledge and technical methods among the disciplines are continuously fused, and scientific research and production application, as well as human life, are gradually and closely related. The crossing of subject fields such as materials, physics, chemistry, biomedicine and the like shows good development activity and research potential in the fields of environmental protection, biomedicine, national defense and military industry and the like. Especially, the sensor with good biocompatibility and sensitivity is widely applied to clinical medicine and disease detection. Aiming at different detection substances, a series of material researches and application conversions with novel functions and excellent performance are also driven. For example, multifunctional carbon materials such as graphene and carbon nanotubes have excellent conductivity and stability, are easy to be miniaturized and manufactured in batches, further exhibit good compatibility from a plurality of angles such as size and electrical properties, and are very suitable for research and development and electrochemical detection of biosensors.
Therefore, in the prior art, research and development of composite materials are carried out by utilizing the excellent conductivity of carbon materials, and the composite materials are popularized and applied to a series of biosensors. For example, the Prussian blue/PDDA-graphene composite membrane modified electrode is applied to a hydrogen peroxide enzyme-free sensor. However, in the prior art, a glassy carbon electrode is commonly used as an electrode substrate to adsorb graphene, and prussian blue is modified on the surface of the electrode substrate adsorbed with the graphene in an electrodeposition manner, so that the electrode preparation process is long, the process is very complicated, and the popularization is not facilitated.
Therefore, it is necessary to provide a simple preparation method for H2O2The conductive paste with high selectivity and sensitivity, and the sensor electrode and the sensor prepared by using the conductive paste.
Disclosure of Invention
Based on the existing problems, the invention provides the conductive paste and the application thereof, and the electrode directly prepared from the conductive paste can solve the problems of long preparation process and complicated process in the existing preparation of the sensor electrode for detecting hydrogen peroxide by using a carbon source and prussian blue as raw materials.
In a first aspect, the present invention provides an electroconductive paste obtained by mixing a carbon source, prussian blue, a binder and a solvent.
Preferably, the carbon source comprises: any one of graphene, graphite, carbon nanotubes and ink;
the adhesive comprises: any one of polyvinylidene fluoride, sodium hydroxymethyl cellulose, styrene-butadiene rubber, polyacrylic acid and salt binder thereof, polytetrafluoroethylene, polyvinyl alcohol, LA132/LA133 aqueous binder, polybutylacrylate and polyacrylonitrile;
the solvent comprises: any one of 1-methyl-2-pyrrolidone, N-dimethylformamide, dimethyl sulfoxide and deionized water.
Preferably, the carbon source accounts for 45-55% of the total mass of the carbon source, the Prussian blue and the binder in the conductive paste by taking the total mass as 100%; the binder accounts for 10-20% of the total mass.
Preferably, the mass ratio of the carbon source to the prussian blue is 10: 1-5: 3.
preferably, the mass ratio of the carbon source to the prussian blue is 2: 1; the weight volume ratio of the carbon source to the solvent is 1 mg: 15 μ l.
Preferably, the mixing can be achieved by stirring with a stirrer or by manual stirring.
Preferably, the binder is added in multiple portions during mixing with the manual stirring.
In a second aspect, the present invention provides a use of the conductive paste according to any one of the first aspect, for preparing an electrode of an electrochemical sensor.
Preferably, the conductive paste for preparing an electrode of an electrochemical sensor includes: and preparing the conductive paste into a working electrode in a screen printing mode.
Preferably, the electrodes of the electrochemical sensor are used to detect hydrogen peroxide.
Compared with the prior art, the conductive paste and the application thereof provided by the invention have the following advantages:
the conductive paste provided by the invention is prepared by mixing Prussian blue, a carbon source, a binder and a solvent, and can be prepared into a working electrode of an electrochemical sensor in a screen printing mode, so that the preparation method is simple and convenient and is easy to popularize; the electrochemical sensor composed of the working electrode is used for detecting hydrogen peroxide, and the electrochemical sensor electrode pair H directly prepared from the conductive paste2O2The detection has higher selectivity and sensitivity.
Drawings
FIG. 1 shows a graph of the test of electrodes for different concentrations of hydrogen peroxide in an embodiment of the present invention.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The specific experimental procedures or conditions are not indicated in the examples and can be performed according to the procedures or conditions of the conventional experimental procedures described in the prior art in this field. The reagents and other instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
In order to solve the problems of long preparation process and complicated process in the prior art when a sensor electrode for detecting hydrogen peroxide is prepared by taking a carbon source and prussian blue as raw materials, the technical concept provided by the invention is as follows: prussian blue and a carbon source are used as basic raw materials, a binder and a solvent are added and uniformly mixed to obtain conductive paste, the conductive paste can be prepared into an electrochemical sensor electrode in a screen printing mode and used for detecting hydrogen peroxide, and the electrochemical sensor electrode directly prepared from the conductive paste is used for H2O2The detection has higher selectivity and sensitivity. Based on the technical concept, the inventor provides the conductive paste and the application thereof, and the specific implementation contents are as follows:
in a first aspect, the present invention provides an electroconductive paste obtained by mixing prussian blue, a carbon source, a binder and a solvent.
In specific implementation, in order to provide a proper liquid phase environment for mixing and dispersing the slurry and ensure the viscosity of the slurry, besides the basic raw materials, a proper solvent, a proper dispersing agent, a proper adhesive and the like are added, and the proper solvent, the proper dispersing agent, the proper adhesive and the like jointly form an organic carrier in slurry preparation. Wherein, the solvent is the main component of the organic carrier, and the organic solvent with approximate boiling point can be selected according to the actual sintering or fixed temperature required after printing and coating, so as to ensure the full mixing and pre-dispersion of the basic raw materials.
In the examples of the present invention, 1-methyl-2-pyrrolidone (NMP) is preferably used as the solvent.
The other main component of the organic vehicle is an adhesive, also called an adhesive or a binder. Since the powder has insufficient adhesion to a substrate such as glass after being dispersed in an organic solvent and is liable to fall off in a powder state during sintering, which leads to failure in electrode printing, it is necessary to add a suitable binder to increase the viscosity of the paste and the adhesion to the substrate, and the binder should be selected so as not to deteriorate the original excellent properties of the material.
On the basis, polyvinylidene fluoride (PVDF) is preferably used as the adhesive in the embodiment of the invention.
In addition, in order to avoid agglomeration of the powder raw material in the organic carrier and maintain the storage stability of the slurry, a certain amount of dispersant needs to be added in the preparation and production processes of the slurry. The dispersant can adjust the electrostatic repulsion to the powder raw material, but if it is added excessively, it causes a decrease in the dispersion stability of the slurry due to excessive agglomeration of the dispersant itself. Finally, in the invention, due to the consideration of solvent volatilization, toxicity and the like, and the addition of the dispersing agent, although the printing and film forming effects are greatly improved, the conductivity of the electrode is weakened like the adhesive, and the conversion of practical application is not facilitated, so that the dispersing liquid is not adopted for mixing raw materials and distilling out the solvent.
In specific embodiments, the carbon source comprises: any one of graphene, graphite, carbon nanotubes, and ink.
In specific implementation, the total mass of the carbon source, the Prussian blue and the binder in the conductive slurry is 100%, wherein the carbon source accounts for 45-55% of the total mass; the binder accounts for 10 to 20 percent of the total mass.
In specific implementation, the mass ratio of the carbon source to the prussian blue is 10: 1-5: 3.
in specific implementation, the mass ratio of the carbon source to the prussian blue is 2: 1; the weight volume ratio of the graphene to the solvent is 1 mg: 15 μ l.
In specific implementation, the following three performances are comprehensively considered when the electrode slurry is prepared by the method disclosed by the invention:
i. adhesiveness: whether used for screen printing or manual coating, the manufactured electrode paste has good adhesion to a used substrate, and is required to be uniformly mixed and easily shaped, so that the use of an adhesive in the manufacturing process of the paste is particularly important, and the proper proportion of a solvent and the adhesive is favorable for the adhesion and the shaping in the manufacturing process of the electrode.
Conductivity: in order to ensure the normal operation in the electrochemical test environment, the electrode made of the slurry should have good conductivity, so the ratio of the adhesive to the conductive raw material is very critical, and the addition of excessive substances with poor conductivity can cause the resistance of the electrode to increase, thereby affecting the electrical signal strength during the test.
Sensitivity: the most important performance of the biosensor is the detection sensitivity for a specific analyte, and therefore, the ratio of electrochemically active materials for the analyte has the greatest influence on the application value of the sensor. Both the amount of the sensitivity-affecting material and the structural contact with the analyte are ensured, and the functionalization and the application of the biosensor can be realized to the maximum extent.
Therefore, in order to prepare electrode slurry with excellent performance, the carbon source, the prussian blue composition and the binder and solvent use amount need to be adjusted according to different mass ratios. The mixing of the binder and the solvent ensures that the slurry has good adhesiveness on the glass substrate, and the usage amount of the binder is above 5% of the total amount of the basic raw materials through a soaking test of a hydrogen peroxide solution and a PBS buffer solution, otherwise, the sintered electrode is easy to fall off. However, the amount of binder used must not be too large for conductivity reasons, which would result in too high a resistance of the slurry after mixing. When a multimeter is used for testing electrodes with different adhesive addition amounts, the mass proportion of the adhesive is not suitable to exceed 20% of the basic raw material, once the mass proportion exceeds the proportion, the resistance of the actual electrode reaches more than 1k omega, and the magnitude order of current in the actual testing process is influenced.
In addition, the key for ensuring the testing sensitivity of the electrode is the addition of prussian blue, and the prussian blue has good activity on the electrocatalytic reduction of hydrogen peroxide, so that the sufficient prussian blue in the slurry can ensure the testing sensitivity of the electrode and the sensor. However, in practical tests, the conductivity of prussian blue is still far from that of graphene, and excessive addition not only fails to structurally achieve large surface area contact with the analyte, but also has a small effect on the conductivity. Therefore, the ratio of prussian blue in the base stock should not exceed half of that of graphene when tested, otherwise sensitivity and conductivity are reduced.
In specific implementation, the optimal ratio of the carbon source-Prussian blue group is 2:1,
in specific implementation, the mixing mode can be realized by stirring and mixing with a stirrer or manually stirring and mixing.
In specific implementation, when manual stirring and mixing are adopted, the binder needs to be added for multiple times.
In a second aspect, the present invention provides a use of the conductive paste of any one of the first aspect above for preparing an electrode of an electrochemical sensor.
In specific implementation, the conductive paste for preparing the electrode of the electrochemical sensor comprises: the conductive paste is prepared into a working electrode in a screen printing mode.
In particular implementations, the electrodes of the electrochemical sensor are used to detect hydrogen peroxide.
In specific implementation, the conductive paste provided by the invention is obtained by mixing Prussian blue, a carbon source, a binder and a solvent, and can be prepared into a working electrode of an electrochemical sensor in a screen printing mode, so that the preparation method is simple and convenient and is easy to popularize; the electrochemical sensor composed of the working electrode is used for detecting hydrogen peroxide, and the electrochemical sensor electrode pair H directly prepared from the conductive paste2O2The detection has higher selectivity and sensitivity.
In order to make the present invention more understandable to those skilled in the art, a conductive paste and an application thereof according to the present invention are described below by way of specific examples.
Example 1:
1. slurry mixing and electrode fabrication
The electrode slurry prepared in this embodiment uses graphene and prussian blue as basic raw materials, 1-methyl-2-pyrrolidone (NMP) as a solvent, and polyvinylidene fluoride (PVDF) as an adhesive, and is uniformly dispersed and mixed to prepare a test electrode of a hydrogen peroxide sensor in a screen printing manner.
i, slurry preparation:
weighing 4mg of graphite and 2.4mg of Prussian blue in a weighing boat, adding 60 mu L of NMP solvent by using a liquid transfer gun, fully and uniformly mixing graphene and Prussian blue, and sequentially adding 10% of PVDF powder by mass to adjust the viscosity degree of the slurry. Note that PVDF powder cannot be added to the initial relatively dilute slurry at once, otherwise agglomeration tends to occur and there is insufficient mixing with the base stock in the slurry.
ii, electrode manufacturing process: the conductive paste is fixed on an insulating substrate (glass slide) by utilizing a screen printing technology to prepare a three-electrode system, wherein the working electrode and the counter motor are both prepared from the conductive paste prepared in the embodiment through screen printing. And finally, putting the prepared three-electrode system into a well-set 60 ℃ oven for drying for 30min, so that the slurry is firmly bonded and formed, and the falling off in the subsequent soaking and testing processes is prevented. And finally, using a hot melt adhesive gun for shaping, dividing the adding area of the test solution, and marking the name of the slurry on the glass slide to finish the electrode manufacturing.
Example 2:
1. slurry mixing and electrode fabrication
i, slurry preparation: weighing 5mg of graphene and 2mg of Prussian blue in a weighing boat, adding 75 mu L of NMP solvent by using a liquid transfer gun, fully and uniformly mixing the graphene and the Prussian blue, and sequentially adding 15% of PVDF powder by mass to adjust the viscosity degree of the slurry. Note that PVDF powder cannot be added to the initial relatively dilute slurry at once, otherwise agglomeration tends to occur and there is insufficient mixing with the base stock in the slurry.
ii, electrode manufacturing process: the conductive paste is fixed on an insulating substrate (glass slide) by utilizing a screen printing technology to prepare a three-electrode system, wherein the working electrode and the counter motor are both prepared from the conductive paste prepared in the embodiment through screen printing. And finally, putting the prepared three-electrode system into a well-set 60 ℃ oven for drying for 30min, so that the slurry is firmly bonded and formed, and the falling off in the subsequent soaking and testing processes is prevented. And finally, using a hot melt adhesive gun for shaping, dividing the adding area of the test solution, and marking the name of the slurry on the glass slide to finish the electrode manufacturing.
Example 3:
1. preparation of solutions
Preparation of PBS buffer solution: 0.2925g of sodium dihydrogen phosphate powder was weighed on a balance using a weigh boat, and 35mL of deionized water was added to prepare a 50mmol/L sodium dihydrogen phosphate solution. Then 4.0g of sodium hydroxide is weighed, and 40mL of deionized water is added to prepare 0.5mol/L sodium hydroxide solution. Titrating the sodium dihydrogen phosphate solution with sodium hydroxide solution under a pH meter until the pH value is 7.5 to obtain the required PBS buffer solution.
Preparation of hydrogen peroxide solution: a hydrogen peroxide solution of 30% mass fraction was used to prepare 3mL of a 100mmol/L hydrogen peroxide solution.
2. Slurry mixing and electrode fabrication
i, slurry preparation: weighing 4mg of graphene and 2mg of Prussian blue in a weighing boat, adding 45 mu L of NMP solvent by using a liquid transfer gun, fully and uniformly mixing the graphene and the Prussian blue, and sequentially adding 10% of PVDF powder by mass to adjust the viscosity degree of the slurry. Note that PVDF powder cannot be added to the initial relatively dilute slurry at once, otherwise agglomeration tends to occur and there is insufficient mixing with the base stock in the slurry.
ii, electrode manufacturing process: the conductive paste is fixed on an insulating substrate (glass slide) by utilizing a screen printing technology to prepare a three-electrode system, wherein the working electrode and the counter motor are both prepared from the conductive paste prepared in the embodiment through screen printing. And finally, putting the prepared three-electrode system into a well-set 60 ℃ oven for drying for 30min, so that the slurry is firmly bonded and formed, and the falling off in the subsequent soaking and testing processes is prevented. And finally, using a hot melt adhesive gun for shaping, dividing the adding area of the test solution, and marking the name of the slurry on the glass slide to finish the electrode manufacturing.
iii detection of graphene-Prussian blue electrode
Connecting the manufactured detection electrode with an electrochemical workstation according to a corresponding three-electrode system, selecting an i-t test mode and setting parameters, wherein the voltage is-0.1V, the maximum detection time is 3000s, and the actual detection intensity range of the electric signal is adjusted according to different electrode materials.
The pipette tip was set at 100. mu.L, and after adding 100. mu.L of PBS buffer to the well of the detection electrode and covering it uniformly in the well, the test was started in CHI 660E.
After the detection curve of the PBS solution is leveled, a pause key is pressed, 10 mu L of hydrogen peroxide solution with the concentration of 10mmol/L is added by a pipette, and after the hydrogen peroxide solution is uniformly mixed by the pipette, the test is continued until the detection curve is leveled.
The hydrogen peroxide solutions of 10mmol/L, 20mmol/L, 40mmol/L, 60mmol/L, 80mmol/L, 100mmol/L were added and tested in the order described above, and the test was terminated and the connection was broken after the last set of curves leveled off.
FIG. 1 shows a graph of the test of electrodes for different concentrations of hydrogen peroxide in an embodiment of the present invention.
The conductive paste and the application thereof provided by the invention are described in detail, and the principle and the implementation mode of the invention are explained by applying specific examples, and the description of the examples is only used for helping to understand the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.
Claims (10)
1. The conductive paste is characterized by being prepared by mixing a carbon source, Prussian blue, a binder and a solvent.
2. The electroconductive paste according to claim 1, wherein the carbon source comprises: any one of graphene, graphite, carbon nanotubes and ink;
the adhesive comprises: any one of polyvinylidene fluoride, sodium hydroxymethyl cellulose, styrene-butadiene rubber, polyacrylic acid and salt binder thereof, polytetrafluoroethylene, polyvinyl alcohol, LA132/LA133 aqueous binder, polybutylacrylate and polyacrylonitrile;
the solvent comprises: any one of 1-methyl-2-pyrrolidone, N-dimethylformamide, dimethyl sulfoxide and deionized water.
3. The conductive paste according to claim 1, wherein the carbon source accounts for 45-55% of the total mass of the carbon source, the Prussian blue and the binder, based on 100% of the total mass of the conductive paste; the binder accounts for 10-20% of the total mass.
4. The electroconductive paste according to claim 1, wherein the mass ratio of the carbon source to the Prussian blue is 10: 1-5: 3.
5. the electroconductive paste according to claim 1, wherein the mass ratio of the carbon source to the Prussian blue is 2: 1; the weight volume ratio of the carbon source to the solvent is 1 mg: 15 μ l.
6. The conductive paste according to claim 1, wherein the mixing is performed by stirring with a stirrer or by manual stirring.
7. The conductive paste as claimed in claim 1, wherein said binder is added in a plurality of portions when said mixing is carried out by said manual stirring.
8. Use of the electroconductive paste according to any one of claims 1 to 7 for the preparation of an electrode for an electrochemical sensor.
9. The use according to claim 8, wherein the conductive paste is used for preparing an electrode of an electrochemical sensor comprising: and preparing the conductive paste into a working electrode in a screen printing mode.
10. Use according to claim 8, wherein the electrodes of the electrochemical sensor are used for detecting hydrogen peroxide.
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