CN113176316B - Sheet Pt/NiCo alloy nano flexible electrode material and application thereof to enzyme-free glucose sensor - Google Patents
Sheet Pt/NiCo alloy nano flexible electrode material and application thereof to enzyme-free glucose sensor Download PDFInfo
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Abstract
The invention discloses a sheet Pt/NiCo alloy nano flexible electrode material and application thereof to an enzyme-free glucose sensor. The structure of the flaky Pt/NiCo alloy nano flexible electrode material is that Pt nano particles are deposited on the surface of a flaky NiCo alloy (the particle size of Pt is below 100 nm), and the flaky Pt/NiCo alloy nano flexible electrode material is prepared by the following method, including pretreatment of carbon cloth, electrochemical deposition of NiCo alloy nano sheets on the carbon cloth, and electrochemical deposition of Pt on the NiCo alloy nano sheets. The invention provides a Pt/NiCo alloy nano flexible electrode material with a sheet structure, which can be used for enzyme-free glucose detection. The Pt/NiCo alloy flexible enzyme-free glucose sensing electrode with the sheet structure, which is constructed by the invention, has the characteristics of high sensitivity, wide linear range, strong anti-interference capability and the like.
Description
Technical Field
The invention belongs to the field of enzyme-free glucose detection, and particularly relates to a flaky Pt/NiCo alloy nano flexible electrode material and application thereof to an enzyme-free glucose sensor.
Background
Diabetes is a serious worldwide health problem. Accurate and real-time monitoring of glucose content in blood of a diabetic patient is an effective means for understanding, diagnosing and treating the condition of the patient. Therefore, developing wearable continuous glucose monitoring devices is especially important for convenient, timely, and effective blood glucose management. At present, the commercial wearable glucose sensing equipment is basically equipment based on a glucolase electrode, and the daily application requirements are difficult to meet due to the defects that the stability and price of the glucolase electrode are poor, and the loaded enzyme is easily interfered by temperature, humidity, pH and other molecules. In addition, most devices based on a glucolase electrode are invasive and require the collection of human blood, which can cause pain. Therefore, the development of the novel flexible enzyme-free glucose sensing electrode has important significance for realizing continuous and real-time glucose detection in a non-invasive or minimally-invasive mode.
At present, the materials for preparing the enzyme-free glucose sensing electrode mainly comprise two materials, namely a noble metal and a transition metal, and the surfaces of the two catalytic materials undergo two different enzyme-free glucose oxidation mechanisms in the process of glucose detection. Due to the good catalytic performance of noble metals, the direct oxidation mechanism of glucose mainly occurs on the surface of noble metals (such as Pt, au and Ag); in the transitionThe indirect oxidation mechanism is generated on the surface of metal (such as Ni, co, etc.), specifically, ni with stronger oxidation capacity is firstly formed 2+ /Ni 3+ (Co 3+ /Co 4+ ) Metallic redox couple, and high-priced Ni 3+ And Co 4+ The glucose is further oxidized. The two metal materials have advantages and disadvantages, and the noble metal glucose has high oxidation activity and high price; transition metals are inexpensive and have poor conductivity, thereby affecting their electrochemical activity. And the performance of the wearable flexible glucose detection equipment is closely related to the structure and catalytic activity of the flexible electrode material. Therefore, the development of a novel Pt/NiCo alloy flexible enzyme-free glucose sensing electrode with a sheet structure is very important for realizing the practical application of wearable continuous enzyme-free glucose monitoring equipment.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a flaky Pt/NiCo alloy nano flexible electrode material.
The technical scheme for realizing the aim of the invention is that the flaky Pt/NiCo alloy nano flexible electrode material is structurally characterized in that Pt nano particles are deposited on the surface of a flaky NiCo alloy (wherein the particle size of Pt is less than 100 nm), and the flaky Pt/NiCo alloy nano flexible electrode material is prepared by adopting the following method. The method comprises the steps of pretreatment of carbon cloth, electrochemical deposition of NiCo alloy nanosheets on the carbon cloth, and electrochemical deposition of Pt on the NiCo alloy nanosheets, and specifically comprises the following steps:
step (1) adopting cyclic voltammetry to perform H-coating on carbon cloth 2 SO 4 Pretreating the solution;
preferably, the cyclic voltammetry uses a voltage range of-1.2 to 1.2V and a sweep rate of 0.1V/S.
Step (2) putting the carbon cloth pretreated in the step (1) into a solution containing Ni 2+ And Co 2+ Carrying out electrochemical deposition in the electrolyte solution to obtain NiCo alloy nanosheets;
preferably, the electrochemical deposition voltage is-1.2 to-0.8V, and the deposition time is 800 to 2000s;
preferably, the Ni is contained 2+ And Co 2+ The electrolyte solution of (A) is Ni-containing 2+ And Co 2+ KCl solution ofLiquid of Ni 2+ Is one of nickel chloride, nickel sulfate and nickel nitrate; co 2+ Is one of cobalt chloride, cobalt sulfate and cobalt nitrate;
step (3) depositing the carbon cloth with NiCo alloy nano sheets in Pt-containing manner 4+ Constant potential deposition is carried out in the electrolyte solution to obtain the Pt/NiCo alloy nanosheet flexible electrode.
Preferably, the Pt is 4+ The electrolyte solution of (a) is a boric acid solution containing chloroplatinic acid.
Preferably, the potentiostatic deposition voltage is from-1.0 to-0.6V and the deposition time is from 20 to 100s.
Preferably, the molar ratio of Pt, ni, and Co in the Pt/NiCo alloy nanosheet flexible electrode is (0.02.
The invention also aims to provide application of the sheet Pt/NiCo alloy nano flexible electrode material in an enzyme-free glucose sensor.
Preferably, in a three-electrode system of the enzyme-free glucose sensor, the counter electrode is a platinum sheet electrode, the reference electrode is a silver chloride electrode, and the working electrode is the sheet Pt/NiCo alloy nano flexible electrode material.
Sensitivity and detection linear range assay conditions: a certain amount of glucose is continuously added into the electrolyte solution to record a current glucose concentration change signal when the I-T is measured by measuring an I-T curve under the condition of voltage of 0.6V, and finally, the sensitivity is calculated by linear fitting according to the glucose concentration and the current signal.
Anti-interference test conditions: the I-T curve was determined by adding 0.5M glucose and 0.1M other interfering substances (Ur, glutamic acid, lysine, cl-, L-leucine, L-valine and proline) continuously to a 0.1M NaOH solution under a voltage of 0.6V.
Serum sample testing: the I-T curve of the working electrode was measured by continuously and alternately adding glucose and serum samples to a 0.1M NaOH solution at a potential of 0.6V, and the concentration of glucose in the serum samples was calculated by the internal standard method.
The invention has the beneficial effects that:
the invention provides a Pt/NiCo alloy nano flexible electrode material with a sheet structure, which can be used for enzyme-free glucose detection. It has the obvious advantages that: the conductivity and the glucose oxidation capability of the transition metal NiCo alloy can be obviously improved by loading a small amount of noble metal Pt; the noble metal Pt and the NiCo alloy are compounded, so that two different glucose oxidation mechanisms can occur on the surface of the electrode at the same time, and the improvement of the glucose sensing performance is facilitated; the sheet-shaped nano structure has higher specific surface area, and is beneficial to the proceeding of electrochemical reaction. The Pt/NiCo alloy flexible enzyme-free glucose sensing electrode with the sheet structure, which is constructed by the invention, has the characteristics of high sensitivity, wide linear range, strong anti-interference capability and the like.
Drawings
FIG. 1 is an SEM image of Pt/NiCo alloy nanoplates prepared according to the invention based on example 1.
FIG. 2 is a TEM and EDS element Mapping image of Pt/NiCo alloy nanosheets based on example 1.
FIG. 3 is an i-t curve of a Pt/NiCo alloy-based flexible enzyme-free glucose sensor electrode of example 1 with the addition of a constant amount of glucose solution to 0.1M NaOH at a voltage of 0.6V.
FIG. 4 is a graph of a linear fit of glucose concentration and amperometric response for a flexible enzyme-free glucose sensing electrode based on the Pt/NiCo alloy of example 1.
FIG. 5 is a graph showing the I-T response of a flexible enzyme-free glucose sensor electrode based on the Pt/NiCo alloy of example 1 measured by the continuous addition of 0.5M glucose, 0.1M other interfering substances (Ur, glutamic acid, lysine, cl-, L-valine and proline, AA) and 0.5M glucose in 0.1M NaOH solution at 0.6V.
FIG. 6 is an I-T curve measured by continuous alternate addition of glucose and serum samples to a 0.1M NaOH solution at a potential of 0.6V for a flexible enzyme-free glucose sensing electrode based on the Pt/NiCo alloy of example 1.
Detailed Description
The invention is described in further detail below with reference to the figures and the detailed description.
Example 1:
(1) Firstly, the carbon cloth is arranged in H 2 SO 4 And (3) treating in the solution, specifically, performing cyclic voltammetry scanning by using carbon cloth as a working electrode, wherein the voltage scanning range is-1.2V-1.2V, and the scanning rate is 0.1V/S.
(2) The treated carbon cloth was coated with a solution containing 0.1M KCl, 0.05M NiCl 2 And 0.05M CoCl 2 applying-1V voltage in the solution to carry out electrochemical deposition for 1200s, and obtaining NiCo alloy nano sheets.
(3) Depositing NiCo alloy nanosheets on a carbon cloth containing 5mM H 2 PtCl 6 0.1M KCl and 0.5M H 3 BO 3 And (3) carrying out constant potential deposition for 60s under the voltage of-0.9V applied in the solution to obtain the Pt/NiCo alloy nanosheet flexible electrode. As shown in fig. 1, which is an SEM image of Pt/NiCo nanosheets prepared according to this example, it is evident that particulate Pt was successfully loaded onto NiCo nanosheets. Fig. 2 is a TEM image and an EDS element Mapping image of the Pt/NiCo nanosheet prepared according to the present example, from which it can also be seen that the prepared material is a lamellar structure, and the Mapping image shows that the Ni, co and Pt elements are uniformly distributed throughout the lamellar structure, proving that the prepared lamellar structure is indeed Pt/NiCo nanosheet.
(4) The prepared Pt/NiCo alloy nanosheet flexible electrode is used for testing glucose sensing performance in 0.1M NaOH solution electrolyte, and specifically is a three-electrode system, wherein the counter electrode is a platinum sheet electrode, the reference electrode is a silver-silver chloride electrode, and the working electrode is the prepared Pt/NiCo alloy nanosheet flexible electrode.
Example 2:
(1) Firstly, the carbon cloth is arranged in H 2 SO 4 And (3) treating in the solution, specifically, performing cyclic voltammetry scanning by using carbon cloth as a working electrode, wherein the voltage scanning range is-1.2V-1.2V, and the scanning rate is 0.1V/S.
(2) The treated carbon cloth was coated with a solution containing 0.1M KCl and 0.05M NiSO 4 And 0.05M CoSO 4 Applying a voltage of-1.2V to carry out electrochemical deposition for 800s in the solution to obtain NiCo alloy nano sheets.
(3) Depositing NiCo alloy nanosheets on a carbon cloth containing 5mM H 2 PtCl 6 0.1M KCl and 0.5M H 3 BO 3 Constant potential deposition in solution under-1.0VAnd 20s, obtaining the Pt/NiCo alloy nanosheet flexible electrode. It is obvious from SEM images and TEM images that granular Pt is successfully loaded on NiCo nano-sheets.
(4) The prepared Pt/NiCo alloy nanosheet flexible electrode is used for testing glucose sensing performance in 0.1M NaOH solution electrolyte, and specifically is a three-electrode system, wherein the counter electrode is a platinum sheet electrode, the reference electrode is a silver chloride electrode, and the working electrode is the prepared Pt/NiCo alloy nanosheet flexible electrode.
Example 3:
(1) Firstly, carbon cloth is coated on H 2 SO 4 And (3) treating in the solution, specifically, performing cyclic voltammetry scanning by using carbon cloth as a working electrode, wherein the voltage scanning range is-1.2V-1.2V, and the scanning rate is 0.1V/S.
(2) Coating the treated carbon cloth with a solution containing 0.1M KCl and 0.05M Ni (NO) 3 ) 2 And 0.05M Co (NO) 3 ) 2 applying-0.8V voltage in the solution to carry out electrochemical deposition for 2000s, and obtaining NiCo alloy nano sheets.
(3) Depositing NiCo alloy nanosheets on a carbon cloth containing 4mM H 2 PtCl 6 0.1M KCl and 0.5M H 3 BO 3 And (3) carrying out constant potential deposition for 100s under the voltage of-0.6V applied in the solution to obtain the Pt/NiCo alloy nanosheet flexible electrode. It is obvious from SEM images and TEM images that granular Pt is successfully loaded on NiCo nano-sheets.
(4) The prepared Pt/NiCo alloy nanosheet flexible electrode is used for testing glucose sensing performance in 0.1M NaOH solution electrolyte, and specifically is a three-electrode system, wherein the counter electrode is a platinum sheet electrode, the reference electrode is a silver-silver chloride electrode, and the working electrode is the prepared Pt/NiCo alloy nanosheet flexible electrode. .
Example 4:
(1) Firstly, the carbon cloth is arranged in H 2 SO 4 And (3) treating in the solution, specifically, performing cyclic voltammetry scanning by using carbon cloth as a working electrode, wherein the voltage scanning range is-1.2V-1.2V, and the scanning rate is 0.1V/S.
(2) Coating the treated carbon cloth with a solution containing 0.1M KCl and 0.05M Ni (NO) 3 ) 2 And 0.05M CoCl 2 Solution of (2)And applying a voltage of-0.9V for electrochemical deposition for 1500s to obtain the NiCo alloy nanosheet.
(3) Depositing NiCo alloy nanosheets on carbon cloth containing 3mM H 2 PtCl 6 0.1M KCl and 0.5M H 3 BO 3 And (3) carrying out constant potential deposition for 150s under the voltage of-0.8V applied in the solution to obtain the Pt/NiCo alloy nanosheet flexible electrode.
(4) The prepared Pt/NiCo alloy nanosheet flexible electrode is used for testing glucose sensing performance in 0.1M NaOH solution electrolyte, and specifically is a three-electrode system, wherein the counter electrode is a platinum sheet electrode, the reference electrode is a silver-silver chloride electrode, and the working electrode is the prepared Pt/NiCo alloy nanosheet flexible electrode. It is obvious from SEM images and TEM images that granular Pt is successfully loaded on NiCo nano-sheets.
(4) The prepared Pt/NiCo alloy nanosheet flexible electrode is used for testing glucose sensing performance in 0.1M NaOH solution electrolyte, and specifically is a three-electrode system, wherein the counter electrode is a platinum sheet electrode, the reference electrode is a silver chloride electrode, and the working electrode is the prepared Pt/NiCo alloy nanosheet flexible electrode.
Example 5:
(1) Firstly, carbon cloth is coated on H 2 SO 4 And (3) treating in the solution, specifically, performing cyclic voltammetry scanning by using carbon cloth as a working electrode, wherein the voltage scanning range is-1.2V-1.2V, and the scanning rate is 0.1V/S.
(2) The treated carbon cloth was coated with a solution containing 0.1M KCl, 0.05M NiCl 2 And 0.05M CoSO 4 Applying a voltage of-1.0V to carry out electrochemical deposition for 1100s in the solution to obtain NiCo alloy nano sheets.
(3) Depositing NiCo alloy nanosheets on carbon cloth containing 3mM H 2 PtCl 6 0.1M KCl and 0.5M H 3 BO 3 And (3) carrying out constant potential deposition for 40s under the voltage of-0.9V applied in the solution to obtain the Pt/NiCo alloy nanosheet flexible electrode. It is obvious from the SEM image that granular Pt is successfully loaded on NiCo nano-sheets.
(4) The prepared Pt/NiCo alloy nanosheet flexible electrode is used for testing glucose sensing performance in 0.1M NaOH solution electrolyte, and specifically is a three-electrode system, wherein the counter electrode is a platinum sheet electrode, the reference electrode is a silver-silver chloride electrode, and the working electrode is the prepared Pt/NiCo alloy nanosheet flexible electrode.
Sensitivity and detection linear range test:
the Pt/NiCo alloy nanosheet flexible electrode prepared in example 1 is tested for glucose sensing performance in 0.1M NaOH solution electrolyte, specifically, a three-electrode system is adopted, wherein the counter electrode is a platinum sheet electrode, the reference electrode is a silver-silver chloride electrode, and the working electrode is the prepared Pt/NiCo alloy nanosheet flexible electrode. FIG. 3 shows the i-t curve of a Pt/NiCo alloy-based flexible enzyme-free glucose sensor electrode with a constant addition of glucose solution to 0.1M NaOH at a voltage of 0.6V. For comparison, the I-T curve of NiCo nanosheets was also determined. It can be seen from fig. 3 that the corresponding current on the Pt/NiCo electrode increases significantly with the addition of glucose, and that the current response on the Pt/NiCo electrode is significantly higher than that of the NiCo electrode. FIG. 4 is a graph of a linear fit of the glucose concentration and the amperometric response based on the above I-T curve, and the analysis showed that the Pt/NiCo electrode has a good linear relationship between the current and the glucose concentration in the ranges of glucose concentrations of 1. Mu.M-8 mM and 8mM-20mM, respectively, and the sensitivity was 4903.43. Mu.A. MM. MM, respectively -1 ·cm -2 And 2258.21 μ A. MM -1 ·cm -2 . The sensitivity of Pt/NiCo electrode is much higher than that of NiCo electrode at 2095.48 muA-mM between 1 muM and 12mM -1 ·cm -2 . The detection limit of the Pt/NiCo electrode was calculated to be about 0.2 μ M based on a signal-to-noise ratio of 3. Therefore, the Pt/NiCo electrode has the advantages of low detection limit, high sensitivity, wide detection range and the like, and is an ideal electrode material for constructing a non-enzymatic glucose sensor.
And (3) anti-interference testing:
the anti-interference performance of the electrode in the glucose detection process is tested in 0.1M NaOH solution electrolyte by using the Pt/NiCo alloy nanosheet flexible electrode prepared in the embodiment 1, and specifically the Pt/NiCo alloy nanosheet flexible electrode is a three-electrode system, wherein the counter electrode is a platinum sheet electrode, the reference electrode is a silver-silver chloride electrode, and the working electrode is the prepared Pt/NiCo alloy nanosheet flexible electrode. FIG. 5 shows that the Pt/NiCo alloy flexible enzyme-free glucose sensing electrode is at 0.6VThe anti-interference test under the pressure shows that the Pt/NiCo electrode pair Ur, glutamic acid, lysine and Cl - L-valine, proline, AA and the like have obvious anti-interference performance.
Serum sample testing:
the detection effect of the Pt/NiCo alloy nanosheet flexible electrode prepared in the embodiment 1 on a real serum sample is tested in 0.1M NaOH solution electrolyte, and specifically a three-electrode system is adopted, wherein the counter electrode is a platinum sheet electrode, the reference electrode is a silver-silver chloride electrode, and the working electrode is the prepared Pt/NiCo alloy nanosheet flexible electrode. FIG. 6 is an I-T curve measured by continuous alternate addition of glucose and serum samples to a 0.1M NaOH solution at a potential of 0.6V for a Pt/NiCo alloy nanosheet flexible electrode. As can be seen from the figure, the Pt/NiCo alloy nanosheet flexible electrode also has good current response to glucose in an actual serum sample. In addition, the glucose concentration of the serum sample is obtained according to an I-T curve measured by the Pt/NiCo alloy nanosheet flexible electrode, and the recovery rate is calculated. The recovery of the electrode test serum samples was within an acceptable range of 94.2% -103.7%. Therefore, the Pt/NiCo alloy nanosheet flexible electrode has high feasibility in the aspect of actual detection of glucose.
The above embodiments are not intended to limit the present invention, and the present invention is not limited to the above embodiments, and all embodiments are within the scope of the present invention as long as the requirements of the present invention are met.
Claims (4)
1. A flaky Pt/NiCo alloy nano flexible electrode material is characterized in that Pt nanoparticles are deposited on the surface of a flaky NiCo alloy, and the flaky Pt/NiCo alloy nano flexible electrode material is prepared by the following method:
step (1) adopting cyclic voltammetry to perform H-coating on carbon cloth 2 SO 4 Pretreating the solution;
step (2) putting the carbon cloth pretreated in the step (1) into a solution containing Ni 2+ And Co 2+ Carrying out electrochemical deposition in the electrolyte solution to obtain NiCo alloy nanosheets; wherein the electrochemical deposition voltage is-1.2 to-0.8V, and the deposition time is 800 to 2000s;
step (3) depositingCarbon cloth of NiCo alloy nano-sheet containing Pt 4+ Performing constant potential deposition in the electrolyte solution to obtain the Pt/NiCo alloy nanosheet flexible electrode, wherein the constant potential deposition voltage is-1.0 to-0.6V, and the deposition time is 20 to 100s; the molar ratio of Pt, ni, and Co in the Pt/NiCo alloy nanosheet flexible electrode is (0.02.
2. The Pt/NiCo alloy nano flexible electrode material in a sheet form as claimed in claim 1, wherein the cyclic voltammetry in step (1) adopts a voltage range of-1.2V and a scanning rate of 0.1V/S.
3. The Pt/NiCo alloy nano flexible electrode material in the form of sheet as claimed in claim 1, wherein the Ni content in step (2) 2+ And Co 2+ The electrolyte solution of (A) is Ni-containing 2+ And Co 2+ KCl solution of (2), wherein Ni 2+ Is one of nickel chloride, nickel sulfate and nickel nitrate; co 2+ Is one of cobalt chloride, cobalt sulfate and cobalt nitrate.
4. The Pt/NiCo alloy nano flexible electrode material in sheet form of claim 1, wherein the Pt in step (3) is 4+ The electrolyte solution of (a) is a boric acid solution containing chloroplatinic acid.
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| CN104777203A (en) * | 2015-04-02 | 2015-07-15 | 天津大学 | Preparation method of Pt-Ni alloy nano tube array electrode and application for enzyme-free glucose sensor |
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