CN111060575A - Porous Co-P composite electrode for glucose enzyme-free detection and preparation method and application thereof - Google Patents
Porous Co-P composite electrode for glucose enzyme-free detection and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a porous Co-P composite electrode for glucose detection and a preparation method thereof. The Co-P prepared by adopting the electrodeposition and template methods has a three-dimensional ordered porous structure, the structure is beneficial to full contact between an electrode and electrolyte, and rapid electron transfer and ion transmission can be realized. The porous Co-P composite electrode has good electrochemical response performance to glucose, and can be applied to a glucose enzyme-free detection sensor. The detection limit of the electrode on glucose was 9.0. mu.M, and the sensitivity was 368.2. mu.A mM‑1cm‑2。
Description
Technical Field
The invention belongs to the field of biochemical sensors, and relates to a porous Co-P composite electrode for glucose enzyme-free detection and a preparation method and application thereof.
Background
In the 60 s of the 20 th century, transition metal phosphide began to be gradually applied to various fields such as metallurgy, hydrodesulfurization, hydrodenitrogenation, hydrotreating, pesticide synthesis, photocatalytic degradation, lithium ion batteries, and the like. In the early stage, most metal phosphides are synthesized by adopting combustible phosphorus as a phosphorus source and are prepared at high temperature and high pressure, so that the experiment is difficult to carry out, the risk of the experiment is greatly improved, and the research and application of transition metal phosphides are greatly hindered. Later, the method of electrodeposition was successful in preparing a transition metal phosphide film, which was clean,The safe and efficient preparation method is beneficial to the large-scale production of the transition metal phosphide, and the application of the high-performance transition metal phosphide in the aspects of electrocatalysis and energy storage attracts the attention of a large number of scholars. Typical transition metal phosphides include mainly CoP, Co2P、Ni2P、Ni5P4、FeP、Fe2P, etc., most of which can be prepared by a simple electrodeposition method.
At present, the scientific development of materials is rapid, various methods for preparing nano porous materials are reported in large quantity, transition metal phosphide with various nano structures can be designed by applying a nano synthesis technology, and the transition metal phosphide with a large number of defects on the surface has more active sites and shows stronger electronic characteristics.
The transition metal phosphide includes various metal compounds such as nickel phosphide, cobalt phosphide, molybdenum phosphide and copper phosphide. The cobalt phosphide has the advantages of good nonmetal characteristics, good conductivity, rich valence and the like, and is applied to the fields of lithium ion batteries, supercapacitors, catalysts, sensors and the like.
The electro-deposition cobalt-phosphorus alloy is a high-efficiency, energy-saving, clean and safe preparation method, soluble salt is used as a reaction raw material, the safety is high, a cobalt-phosphorus alloy coating can be rapidly produced through the deposition of ions in a solution, the plating solution can be recycled by periodically supplementing the plating solution, and the burden on the environment is reduced. In the past, the cobalt-phosphorus materials are most commonly nanoparticles and powders with lamellar structures, and if the cobalt-phosphorus materials are applied to electrochemical fields such as capacitors, sensors and the like, the nanopowder needs to be adhered to an electrode, and the conductivity of the electrode surface is reduced due to the use of a binder, so that the conduction of electrons is influenced. In addition, after the electrode is recycled for multiple times, atoms are repeatedly embedded and removed, so that nanoparticles or lamella are agglomerated, the specific surface area is greatly reduced, and the electrochemical performance is reduced.
In summary, the cobalt phosphide nanoparticles are easy to agglomerate in the oxidation-reduction process, excellent capacitance performance and good circulation stability cannot be guaranteed, the ordered porous cobalt phosphide has three-dimensional continuous through holes and ligament structures, the stability is greatly improved, and the defects of the materials can be overcome, so that the cobalt phosphide nanoparticles can be applied to an electrochemical detection electrode to obtain a better effect.
Disclosure of Invention
The invention aims to provide a porous Co-P composite electrode for glucose enzyme-free detection.
The porous Co-P composite electrode provided by the invention comprises an electrode, an electrode protection layer and a porous Co-P composite modification layer.
The porous Co-P composite has a three-dimensional ordered porous structure, the structure is favorable for full contact between an electrode and electrolyte, rapid electron transfer and ion transmission can be realized, and the atomic ratio of cobalt to phosphorus is 2: 1; the electrode protection layer is a cobalt layer.
The porous Co-P composite electrode prepared by the invention has a multilayer metal structure, and the cobalt layer is electroplated on the surface of the electrode substrate to be used as a protective layer and a buffer layer, so that the binding force of the electrodeposited Co-P composite and the substrate can be effectively improved, and the stability of the electrode is improved.
The invention also aims to provide a preparation method of the porous Co-P composite electrode.
The method specifically comprises the following steps:
s1, preparation of a polystyrene template: the method comprises the following steps of (1) carrying out electrophoretic deposition in polystyrene microsphere emulsion with positive charges by using a polyimide copper-clad plate as a substrate to obtain a polystyrene template electrode;
s2, preparing a porous Co-P composite electrode: directly electrodepositing Co-P on a polystyrene template by adopting an electrodeposition method, and removing the template by chloroform to obtain the three-dimensional ordered porous Co-P composite electrode.
Further, in step S1, the polyimide copper-clad plate is pre-cleaned and dried before use, and the cleaning includes cleaning with acetone, deionized water, an acidic mixed solution and deionized water in sequence, wherein the acidic mixed solution consists of: 0.4M Na2S2O8、0.1M CuSO4And 0.4M H2SO4。
Further, in the step S1, the concentration of the polystyrene microsphere emulsion is 1 wt%.
Further, in the step S1, the voltage of the electrophoretic deposition is 4V, and the time is 2 min.
In order to obtain three-dimensional porous Co-P with proper performance, a great deal of experimental screening needs to be carried out on the electroplating solution for electrodeposition, and the concentration of main salt in the electroplating solution, the technological condition of electrodeposition, and complexing agents and additives can influence the property of the coating. If the proportion of the main salt in the plating solution is too low, it is difficult to form a continuous ordered porous morphology with a high porosity, and if the proportion is too high, the components forming the porous framework are difficult to support a three-dimensional porous structure due to too low content, resulting in too poor material bonding force.
Further, in the step S2, the electrodeposition solution is composed of: 180g/L of cobalt sulfate, 50g/L of phosphoric acid and 15g/L of phosphorous acid;
when Co-P is electrodeposited, the surface of the plating layer is rough and uneven due to too high or too low current density, the pores of the porous structure are small and few due to the reduction of the current density, and the stable ordered structure is not maintained due to too high current density.
Further, in the step S2, the current density is 4 to 10ASD, preferably 6 ASD; the electrodeposition time is 1-5 min, preferably 2 min.
Scanning and observing the porous Co-P electrode prepared by the invention by adopting an SEM electron microscope.
As shown in attached figure 1, the three-dimensional ordered porous structure Co-P composite electrode prepared by the invention is a scanning electron microscope image with different multiples. From the figure, a uniform ordered porous structure can be observed, with pores of about 150nm diameter. The multilevel pore structure is beneficial to full contact between the electrode and electrolyte and quickens ion transfer, and the ligament connecting the pores is beneficial to electron transmission and ensures the rapid transfer of electrons in the charging and discharging process.
Another object of the present invention is to provide an application of the porous Co-P composite electrode.
The porous Co-P composite electrode prepared by the invention has good electrochemical response performance to glucose, and can be applied to a glucose detection sensor.
The porous Co-P electrode prepared by the method is subjected to glucose response performance test by methods such as cyclic voltammetry scanning and chronoamperometric detection.
As shown in attached figure 2, the porous Co-P composite electrode prepared by the invention is put into 0.1M KOH solution and cyclic voltammetry scanning is carried out. As can be seen from the graph, when 10mM glucose was added, the current of the porous Co-P electrode increased from 0.2V and an oxidation peak appeared at 0.57V, and the current increase Δ I reached 1.0mA cm-2Therefore, the electrochemical response of the porous Co-P is most obvious, and the porous structure prepared by the method can greatly improve the catalytic performance of the electrode on glucose.
As shown in attached figure 3, the porous Co-P composite electrode prepared by the invention is placed into 0.1M KOH buffer solution, glucose solution is gradually dropped, test potential is selected to be 0.6V, and timing current detection is carried out. As can be seen from the graph, the current rapidly increased and remained stable with the increase of the glucose concentration, the submission trend was stepped, and the detection limit of the electrode for glucose was calculated to be 9.0. mu.M.
As shown in figure 4, the response current density data of the porous Co-P composite electrode prepared by the invention to glucose solutions with different concentrations are linearly fitted with the glucose concentration. As can be seen from the figure, when the concentration range of the glucose is 3.40-10.20 mM, the porous Co-P electrode has good linear response to the glucose, the correlation coefficient of a linear fitting equation is 0.998, and the sensitivity of detecting the glucose by the electrode can be calculated to be 368.2 muA mM-1cm-2。
The porous Co-P electrode prepared by the invention has lower detection limit and high sensitivity for detecting glucose.
As shown in FIG. 5, the porous Co-P composite electrode prepared according to the present invention was placed in a 0.1M KOH buffer solution, and 0.10mM glucose, 0.01mM Ascorbic Acid (AA), 0.01mM Uric Acid (UA), and 0.01mM dopamine (UA) were sequentially added, and a chronoamperometric test was performed. As can be seen from the figure, obvious current response is generated after glucose is added, and the current change of the added interfering substances is far smaller than the current response of the glucose, which shows that the porous Co-P electrode prepared by the invention has good anti-interference performance on the glucose and can be used for detecting the glucose in a complex test environment.
The invention has the beneficial effects that:
(1) the invention adopts a simple and feasible method to prepare the porous three-dimensional Co-P structure, greatly improves the electrode performance, has lower preparation cost and does not need special environment and large-scale instruments.
(2) When the electrode is used for detecting glucose, the electrode has lower detection limit, higher sensitivity and good anti-interference performance.
(3) The electrode is used for the enzyme-free glucose sensor, can realize continuous glucose detection, and avoids enzyme inactivation easily caused by external environment influence, thereby ensuring the reliability of the detection result
Drawings
The invention is further illustrated by means of the attached drawings, but the embodiments in the drawings do not constitute any limitation to the invention, and for a person skilled in the art, other drawings can be obtained on the basis of the following drawings without inventive effort.
FIG. 1 is an SEM scanning electron microscope image of a three-dimensional ordered porous structure Co-P composite electrode prepared by the invention;
FIG. 2 is a plot of cyclic voltammetry scans of a porous Co-P composite electrode prepared according to the present invention before and after addition of glucose in 0.1M KOH solution;
FIG. 3 is a chronoamperometric view of a porous Co-P composite electrode prepared according to the present invention on glucose solutions of different concentrations;
FIG. 4 is a linear fit graph of response current density and glucose concentration of porous Co-P composite electrode prepared by the invention to glucose solutions of different concentrations;
FIG. 5 is a graph showing the selectivity of the porous Co-P composite electrode prepared by the present invention to glucose.
Detailed Description
In order that the objects, aspects and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the following detailed description and the accompanying drawings.
Example 1
Preparing a porous Co-P composite electrode:
s1, preparation of a polystyrene template: ultrasonically oscillating a polyimide copper-clad plate in acetone for 30min to remove oil, cleaning the deoiled substrate with deionized water, and soaking in 0.4M Na2S2O8、0.1M CuSO4And 0.4M H2SO4Removing the surface oxide film from the mixed solution, and then washing and drying the mixed solution by using deionized water.
Taking a polyimide copper-clad plate as a working electrode and a platinum sheet as a counter electrode, carrying out electrophoretic deposition in 1 wt% of polystyrene microsphere emulsion, wherein the voltage of the electrodeposition is 4V, the time is 2min, and drying the electrode in a drying oven at 100 ℃ to obtain the polystyrene microsphere template.
S2, preparing a porous Co-P composite electrode: carrying out electrodeposition on the polystyrene template prepared in the previous step, wherein the polystyrene template is taken as a working electrode by adopting a programmable direct-current power supply, a platinum sheet is taken as a counter electrode, the current density is 6ASD, the electrodeposition time is 2min, and the composition of an electrodeposition solution is as follows: 180g/L of cobalt sulfate, 50g/L of phosphoric acid and 15g/L of phosphorous acid; and after the electrodeposition is finished, taking out the electrode, washing the electrode by using deionized water, drying the electrode in an oven, and soaking the dried electrode in a chloroform solution for 30 min. And washing and drying the electrode by using deionized water to obtain the porous Co-P composite electrode.
Example 2
Preparing a porous Co-P composite electrode:
s1, preparation of a polystyrene template: ultrasonically oscillating a polyimide copper-clad plate in acetone for 30min to remove oil, cleaning the deoiled substrate with deionized water, and soaking in 0.4M Na2S2O8、0.1M CuSO4And 0.4M H2SO4Removing the surface oxide film from the mixed solution, and then washing and drying the mixed solution by using deionized water.
Taking a polyimide copper-clad plate as a working electrode and a platinum sheet as a counter electrode, carrying out electrophoretic deposition in 1 wt% of polystyrene microsphere emulsion, wherein the voltage of the electrodeposition is 4V, the time is 5min, and drying the electrode in a drying oven at 100 ℃ to obtain the polystyrene microsphere template.
S2, preparing a porous Co-P composite electrode: carrying out electrodeposition on the polystyrene template prepared in the previous step, wherein the polystyrene template is taken as a working electrode by adopting a programmable direct-current power supply, a platinum sheet is taken as a counter electrode, the current density is 2ASD, the electrodeposition time is 5min, and the composition of an electrodeposition solution is as follows: 180g/L cobalt sulfate, 50g/L phosphoric acid and 15g/L phosphorous acid.
And after the electrodeposition is finished, taking out the electrode, washing the electrode by deionized water, drying the electrode in an oven, and soaking the dried electrode in a chloroform solution for 30 min. And washing and drying the electrode by using deionized water to obtain the porous Co-P composite electrode.
Example 3
Preparing a porous Co-P composite electrode:
s1, preparation of a polystyrene template: ultrasonically oscillating a polyimide copper-clad plate in acetone for 30min to remove oil, cleaning the deoiled substrate with deionized water, and soaking in 0.4M Na2S2O8、0.1M CuSO4And 0.4M H2SO4Removing the surface oxide film from the mixed solution, and then washing and drying the mixed solution by using deionized water.
Taking a polyimide copper-clad plate as a working electrode and a platinum sheet as a counter electrode, carrying out electrophoretic deposition in 1 wt% of polystyrene microsphere emulsion, wherein the voltage of the electrodeposition is 4V, the time is 5min, and drying the electrode in a drying oven at 100 ℃ to obtain the polystyrene microsphere template.
S2, preparing a porous Co-P composite electrode: performing electrodeposition on the polystyrene template prepared in the previous step, wherein a programmable direct-current power supply is adopted, the polystyrene template is used as a working electrode, a platinum sheet is used as a counter electrode, the current density is 1.2ASD, the electrodeposition time is 6 min, and the electrodeposition solution comprises the following components: 180g/L cobalt sulfate, 50g/L phosphoric acid and 15g/L phosphorous acid.
And after the electrodeposition is finished, taking out the electrode, washing the electrode by deionized water, drying the electrode in an oven, and soaking the dried electrode in a chloroform solution for 30 min. And washing and drying the electrode by using deionized water to obtain the porous Co-P composite electrode.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single technical solution, and such description is for clarity only, and those skilled in the art should take the description as a whole, and the technical solutions in the embodiments may be combined appropriately to form other embodiments that those skilled in the art can understand. The technical details not described in detail in the present invention can be implemented by any of the prior arts in the field. In particular, all technical features of the invention which are not described in detail can be achieved by any prior art.
Claims (10)
1. The porous Co-P composite electrode is characterized by comprising an electrode, an electrode protection layer and a porous Co-P composite modification layer.
2. The porous Co-P composite electrode of claim 1, wherein the porous Co-P composite has a three-dimensional ordered porous structure comprising cobalt and phosphorus in an atomic ratio of 2: 1; the electrode protection layer is a cobalt layer.
3. The method for preparing a porous Co-P composite electrode according to claim 1, comprising the steps of:
s1, preparation of a polystyrene template: the method comprises the following steps of (1) carrying out electrophoretic deposition in polystyrene microsphere emulsion with positive charges by using a polyimide copper-clad plate as a substrate, and drying to obtain a polystyrene template electrode;
s2, preparing a porous Co-P composite electrode: directly electrodepositing Co-P on a polystyrene template by adopting an electrodeposition method, and removing the polystyrene template by chloroform to obtain the three-dimensional ordered porous Co-P composite electrode.
4. The method for preparing the porous Co-P composite electrode according to the method of claim 3, wherein in the step S1, the polyimide copper-clad plate is pre-cleaned and dried before use, and the cleaning comprises sequentially cleaning with acetone, deionized water, an acidic mixed solution and deionized water.
5. The method for preparing a porous Co-P composite electrode according to claim 3, wherein the polystyrene microsphere emulsion is 1 wt% in the step S1.
6. The method for preparing a porous Co-P composite electrode according to claim 3, wherein in step S1, the voltage of the electrophoretic deposition is 4V and the time is 2 min.
7. The method for preparing a porous Co-P composite electrode according to claim 3, wherein in step S2, the electrodeposition solution comprises: 180g/L cobalt sulfate, 50g/L phosphoric acid and 15g/L phosphorous acid.
8. The method for preparing a porous Co-P composite electrode according to claim 3, wherein in step S2, the electrodeposition reaction conditions are as follows: the current density is 4.0-10.0 ASD, preferably 6.0 ASD; the electrodeposition time is 1-5 min, preferably 2 min.
9. The method for preparing the porous Co-P composite electrode according to the method of claim 4, wherein the acidic mixed solution comprises the following components: 0.4M Na2S2O8、0.1M CuSO4And 0.4M H2SO4。
10. The use of a porous Co-P composite electrode as claimed in any one of claims 1 to 3, wherein the porous Co-P composite electrode has good electrochemical response to glucose and can be used in a glucose sensor.
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| CN115512977A (en) * | 2022-10-14 | 2022-12-23 | 重庆文理学院 | FeP hollow nanorod for supercapacitor and preparation method thereof |
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