Preparation method of sensor, sensor and application

Abstract

The preparation method of the sensor provided by the invention comprises the following steps: dispersing a sensitive material and a conductive material in a solvent for ultrasonic treatment to obtain a nano composite material solution; the nano composite material solution is dripped to the surface of a conductive substrate and dried to obtain the sensor, the method is simple in process, complex equipment or strict conditions are not needed, and the production cost and energy consumption are remarkably reduced; in the preparation process, the ratio of the sensitive material dispersion liquid to the conductive material dispersion liquid can be flexibly regulated and controlled to optimize the performance so as to meet the sensitivity and stability required in menthone solutions with different concentrations, so that the menthone sensor shows more excellent detection precision and stability in menthone detection; the method is an innovative solution with low cost and high performance. In addition, the invention further provides a sensor and application.

Description

Technical Field

[0001] The present application relates to the field of biological detection technology, and in particular to a method for preparing a sensor, a sensor and applications thereof. Background Art

[0002] Menthone is a common biomarker in antiviral, anti-inflammatory and other drug metabolism and an important basis for food quality or authenticity. In addition, menthone is also one of the biomarkers for brain diseases such as epilepsy.

[0003] In the prior art, the detection methods of menthone mainly focus on two analytical methods: gas chromatography (GC) and liquid chromatography (LC), but they have a series of shortcomings such as high cost, complex operation, high sample pretreatment requirements, limited sensitivity, difficulty in real-time detection, and strict environmental conditions. These shortcomings greatly limit the detection efficiency and scope of menthone in practical applications, and it is urgent to develop new menthone detection methods. Summary of the invention

[0004] In view of this, it is necessary to provide a method for preparing a sensor, a sensor and an application thereof that can effectively improve the detection accuracy and stability of menthone in view of the defects existing in the current menthone detection.

[0005] To solve the above problems, this application adopts the following technical solutions:

[0006] One of the purposes of this application is to provide a method for preparing a sensor, comprising the following steps:

[0007] Dispersing the sensitive material and the conductive material in a solvent and subjecting them to ultrasonic treatment to obtain a nanocomposite material solution;

[0008] The nanocomposite material solution is drop-casted onto the surface of a conductive substrate and dried to obtain a sensor.

[0009] In some embodiments, the step of dispersing the sensitive material and the conductive material in a solvent and subjecting them to ultrasonic treatment to obtain a nanocomposite material solution specifically includes the following steps:

[0010] Dispersing the sensitive material in a solvent to form a sensitive material dispersion, dispersing the conductive material in a solvent to form a conductive material dispersion, wherein the concentration of the sensitive material dispersion is 1 to 50 mg / mL, and the concentration of the conductive material dispersion is 0.5 to 3 mg / mL;

[0011] The sensitive material dispersion and the conductive material dispersion in a volume ratio of 0.2 to 1 are ultrasonically treated for 5 to 30 minutes to obtain a nanocomposite material solution.

[0012] In some embodiments, the sensitive material includes nano-oxides, which are but not limited to oxides of Ni, Cu, Mn, Ti, Au or Pt.

[0013] In some embodiments, the conductive material includes but is not limited to graphene or graphite or carbon nanotubes or MXene.

[0014] In some embodiments, the solvent includes but is not limited to ethanol or deionized water.

[0015] In some embodiments, the step of drop-casting the nanocomposite solution onto the surface of a conductive substrate and drying it to obtain a sensor specifically includes the following steps:

[0016] The nanocomposite solution is drop-casted onto the surface of a conductive substrate and physically dried for 20 to 60 minutes to obtain a sensor, wherein the conductive substrate includes but is not limited to foamed nickel or nano-gold or nano-carbon or platinum black, and the physical drying includes but is not limited to an oven or a heating platform.

[0017] In some of the embodiments, the method further comprises the step of activating the sensor.

[0018] In some embodiments, the step of activating the sensor specifically includes:

[0019] The sensor is placed at the working electrode position of a three-electrode system and immersed in an activator for electrochemical scanning. The scanned sensor is cleaned and physically dried to obtain an activated sensor. The activator includes but is not limited to ferrous and / or ferric ions, potassium chloride and / or potassium ferrocyanide, benzoquinone and / or hydroquinone. The electrochemical method includes but is not limited to CV or It or DPV or LSV.

[0020] The second object of the present application is to provide a sensor prepared by any of the preparation methods described above.

[0021] The third purpose of the present application is to provide an application of the sensor in detecting the concentration of menthone.

[0022] In some embodiments, the concentration range of the detected menthone is 0.2-5 mM.

[0023] This application adopts the above technical solution, and its beneficial effects are as follows:

[0024] The preparation method, sensor and application of the sensor provided in the present application are as follows: a sensitive material and a conductive material are dispersed in a solvent and ultrasonically treated to obtain a nanocomposite solution; the nanocomposite solution is drop-cast onto the surface of a conductive substrate and dried to obtain a sensor. The method has a simple process and does not require complex equipment or strict conditions, which significantly reduces production costs and energy consumption; and during the preparation process, the ratio of the sensitive material dispersion and the conductive material dispersion can be flexibly adjusted to optimize performance to meet the sensitivity and stability required in menthone solutions of different concentrations, so that better detection accuracy and stability are exhibited in menthone detection, and the method is an innovative solution with both low cost and high performance. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings required for use in the embodiments of the present application or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0026] Figure 1 CV curve of the SPCE / CuO@MWCNTs sensor provided in the embodiment of the present application in a mixed solution of KCl and K3[Fe(CN)6].

[0027] Figure 2 The sensor prepared in Example 1 of the present application shows the detection curve of different concentrations of menthone (a) and the fitting curve of the characteristic peak-to-peak current of menthone at 0.82V (b).

[0028] Figure 3 The sensor prepared in Example 2 of the present application shows the detection curve of different concentrations of menthone (a) and the fitting curve of the characteristic peak-to-peak current of menthone at 0.82V (b).

[0029] Figure 4 The sensor prepared in Example 3 of the present application shows the detection curve of different concentrations of menthone (a) and the fitting curve of the peak current of the characteristic peak of menthone at 0.82V (b).

[0030] Figure 5 The sensor prepared in Example 4 of the present application shows the detection curve of different concentrations of menthone (a) and the fitting curve of the peak current of the characteristic peak of menthone at 0.82V (b). DETAILED DESCRIPTION

[0031] Embodiments of the present application are described in detail below, and examples of the embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals throughout represent the same or similar elements or elements having the same or similar functions. The embodiments described below with reference to the accompanying drawings are exemplary and are intended to be used to explain the present application, and should not be construed as limiting the present application.

[0032] In the description of the present application, it should be understood that the terms "upper", "lower", "horizontal", "inside", "outside", etc., indicating orientations or positional relationships, are based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present application and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation on the present application.

[0033] In addition, the terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of the features. In the description of this application, the meaning of "plurality" is two or more, unless otherwise clearly and specifically defined.

[0034] In order to make the objectives, technical solutions and advantages of the present application more clearly understood, the present application is further described in detail below in conjunction with the accompanying drawings and embodiments.

[0035] The method for preparing the sensor provided in the embodiment of the present application specifically comprises the following steps:

[0036] Step S110: dispersing the sensitive material and the conductive material in a solvent and subjecting them to ultrasonic treatment to obtain a nanocomposite material solution.

[0037] In some embodiments, the step of dispersing the sensitive material and the conductive material in a solvent and subjecting them to ultrasonic treatment to obtain a nanocomposite material solution specifically includes the following steps:

[0038] Dispersing the sensitive material in a solvent to form a sensitive material dispersion, dispersing the conductive material in a solvent to form a conductive material dispersion, wherein the concentration of the sensitive material dispersion is 1 to 50 mg / mL, and the concentration of the conductive material dispersion is 0.5 to 3 mg / mL;

[0039] The sensitive material dispersion and the conductive material dispersion in a volume ratio of 0.2 to 1 are ultrasonically treated for 5 to 30 minutes to obtain a nanocomposite material solution.

[0040] In some embodiments, the sensitive material includes nano-oxides, which are but not limited to oxides of Ni, Cu, Mn, Ti, Au or Pt.

[0041] In some embodiments, the conductive material includes but is not limited to graphene or graphite or carbon nanotubes or MXene.

[0042] In some embodiments, the solvent includes but is not limited to ethanol or deionized water.

[0043] It can be understood that this embodiment uses ethanol or deionized water as a solvent and uses sensitive materials and conductive materials as solutes to form a nanocomposite solution. The ratio of sensitive materials to conductive materials is adjusted to optimize performance and better meet actual application requirements.

[0044] Step S120: drop-casting the nanocomposite material solution onto the surface of a conductive substrate and drying it to obtain a sensor.

[0045] In some embodiments, the step of drop-casting the nanocomposite solution onto the surface of a conductive substrate and drying it to obtain a sensor specifically includes the following steps:

[0046] The nanocomposite solution is drop-casted onto the surface of a conductive substrate and physically dried for 20 to 60 minutes to obtain a sensor, wherein the conductive substrate includes but is not limited to foamed nickel or nano-gold or nano-carbon or platinum black, and the physical drying includes but is not limited to an oven or a heating platform.

[0047] In some of the embodiments, the method further comprises the step of activating the sensor.

[0048] In some embodiments, the step of activating the sensor specifically includes:

[0049] The sensor is placed at the working electrode position of a three-electrode system and immersed in an activator for electrochemical scanning. The scanned sensor is cleaned and physically dried to obtain an activated sensor. The activator includes but is not limited to ferrous and / or ferric ions, potassium chloride and / or potassium ferrocyanide, benzoquinone and / or hydroquinone. The electrochemical method includes but is not limited to CV or It or DPV or LSV.

[0050] The sensor preparation method provided in the above-mentioned embodiment of the present application has a simple process and does not require complex equipment or strict conditions, which significantly reduces production costs and energy consumption; and in the preparation process, the ratio of the sensitive material dispersion and the conductive material dispersion can be flexibly adjusted to optimize the performance to meet the sensitivity and stability required in menthone solutions of different concentrations, so that better detection accuracy and stability are exhibited in menthone detection, which is an innovative solution with both low cost and high performance.

[0051] The sensor prepared in the above embodiment of the present application can be used for the concentration detection of menthone

[0052] Furthermore, the sensor provided in this embodiment has a detection sensitivity of 41.04 μA·mM in detecting the concentration of menthone. -1 cm -2 ; The detection concentration range is 0.2-5mM.

[0053] See also Figure 1 CV curves of SPCE / CuO@MWCNTs sensor in KCl and K3[Fe(CN)6] mixed solution. Figure 1 It can be seen that the above sensor can show good sensitivity and stability in menthone solutions of different concentrations.

[0054] The above technical solution of the present application is described in detail below in conjunction with specific embodiments.

[0055] In the following examples, the concentration of the sensitive material dispersion is 10 mg / mL, 5 mg / mL, and 1 mg / mL, and the concentration of the conductive material dispersion is 2 mg / mL or 0 mg / mL. For specific examples, see the following description.

[0056] Example 1

[0057] The sensor preparation method provided in this embodiment is as follows:

[0058] CuO is dispersed in deionized water to form a sensitive material dispersion, and carbon nanotubes are dispersed in a solvent to form a conductive material dispersion. The concentration of the sensitive material dispersion is 10 mg / mL, and the concentration of the conductive material dispersion is 2 mg / mL.

[0059] The sensitive material dispersion and the conductive material dispersion in a volume ratio of 1 were ultrasonically treated for 30 minutes to obtain a nanocomposite material solution.

[0060] The nanocomposite solution was drop-cast onto the surface of nickel foam and physically dried for 20 minutes to obtain a sensor.

[0061] See also Figure 2 , which are the detection curves (a) of the sensor prepared in Example 1 for different concentrations of menthone and the fitting curve (b) for the peak current of the characteristic peak of menthone at 0.82V, from Figure 2 It can be seen that the menthone detection effect of the electrode prepared with 10 mg / mL CuO and 2 mg / mL carbon nanotubes as the formula.

[0062] Example 2

[0063] The sensor preparation method provided in this embodiment is as follows:

[0064] NiO is dispersed in deionized water to form a sensitive material dispersion, and carbon nanotubes are dispersed in a solvent to form a conductive material dispersion. The concentration of the sensitive material dispersion is 5 mg / mL, and the concentration of the conductive material dispersion is 2 mg / mL.

[0065] The sensitive material dispersion and the conductive material dispersion in a volume ratio of 0.2 were ultrasonically treated for 50 minutes to obtain a nanocomposite material solution.

[0066] The nanocomposite solution was drop-cast onto a platinum black surface and physically dried for 60 minutes to obtain a sensor.

[0067] See also Figure 3 , which are the detection curves (a) of the sensor prepared in Example 2 for different concentrations of menthone and the fitting curve (b) for the peak current of the characteristic peak of menthone at 0.82V, from Figure 3 It can be seen that the menthone detection effect of the electrode prepared with 5 mg / mL NiO and 2 mg / mL carbon nanotubes as the formula.

[0068] Example 3

[0069] The sensor preparation method provided in this embodiment is as follows:

[0070] Cu2O is dispersed in deionized water to form a sensitive material dispersion, and carbon nanotubes are dispersed in a solvent to form a conductive material dispersion. The concentration of the sensitive material dispersion is 1 mg / mL, and the concentration of the conductive material dispersion is 2 mg / mL.

[0071] The sensitive material dispersion and the conductive material dispersion in a volume ratio of 0.5 were ultrasonically treated for 10 minutes to obtain a nanocomposite material solution.

[0072] The nanocomposite solution was drop-cast onto the nanocarbon surface and physically dried for 40 minutes to obtain a sensor.

[0073] See also Figure 4 , which are the detection curves (a) of the sensor prepared in Example 3 for different concentrations of menthone and the fitting curve (b) for the peak current of the characteristic peak of menthone at 0.82V, from Figure 4 It can be seen that the menthone detection effect of the electrode prepared with 1 mg / mL Cu2O and 2 mg / mL carbon nanotubes as the formula.

[0074] Example 4

[0075] The sensor preparation method provided in this embodiment is as follows:

[0076] CuO was dispersed in deionized water and ultrasonically treated for 10 minutes to form a sensitive material dispersion, and the sensitive material dispersion was drop-cast onto the surface of the nanocarbon and physically dried for 40 minutes to obtain a sensor. The concentration of the sensitive material dispersion was 5 mg / mL.

[0077] See also Figure 5 , which are the detection curves (a) of the sensor prepared in Example 4 for different concentrations of menthone and the fitting curve (b) for the peak current of the characteristic peak of menthone at 0.82V. Figure 5 As can be seen from the graph, the electrode prepared with 5 mg / mL CuO alone failed to detect menthone (ie, no oxidation peak appeared near the potential of 0.82 V).

[0078] The above are only preferred embodiments of the present application, and only specifically describe the technical principles of the present application. These descriptions are only for explaining the principles of the present application and cannot be interpreted as limiting the scope of protection of the present application in any way. Based on the explanation here, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present application, and other specific implementation methods of the present application that can be associated with the technicians in this field without creative work, should be included in the scope of protection of the present application.

Claims

1. A method for preparing a sensor, characterized in that: The steps include: Dispersing the sensitive material and the conductive material in a solvent and subjecting them to ultrasonic treatment to obtain a nanocomposite material solution; The nanocomposite material solution is drop-casted onto the surface of a conductive substrate and dried to obtain a sensor.

2. The method for preparing a sensor according to claim 1, characterized in that: The step of dispersing the sensitive material and the conductive material in a solvent and subjecting them to ultrasonic treatment to obtain a nanocomposite material solution specifically includes the following steps: Dispersing the sensitive material in a solvent to form a sensitive material dispersion, dispersing the conductive material in a solvent to form a conductive material dispersion, wherein the concentration of the sensitive material dispersion is 1 to 50 mg / mL, and the concentration of the conductive material dispersion is 0.5 to 3 mg / mL; The sensitive material dispersion and the conductive material dispersion in a volume ratio of 0.2 to 1 are ultrasonically treated for 5 to 30 minutes to obtain a nanocomposite material solution.

3. The method for preparing the sensor according to claim 2, characterized in that: The sensitive material includes nano-oxides, which are but not limited to oxides of Ni, Cu, Mn, Ti, Au or Pt.

4. The method for preparing the sensor according to claim 2, characterized in that: The conductive material includes but is not limited to graphene or graphite or carbon nanotubes or MXene.

5. The method for preparing the sensor according to claim 2, characterized in that: The solvent includes, but is not limited to, ethanol or deionized water.

6. The method for preparing a sensor according to claim 1, characterized in that: The step of drop-casting the nanocomposite solution onto the surface of a conductive substrate and drying it to obtain a sensor specifically includes the following steps: The nanocomposite solution is drop-casted onto the surface of a conductive substrate and physically dried for 20 to 60 minutes to obtain a sensor, wherein the conductive substrate includes but is not limited to foamed nickel or nano-gold or nano-carbon or platinum black, and the physical drying includes but is not limited to an oven or a heating platform.

7. The method for preparing a sensor according to claim 1, characterized in that: The method also includes the step of activating the sensor.

8. The method for preparing a sensor according to claim 7, characterized in that: The step of activating the sensor specifically includes: The sensor is placed at the working electrode position of a three-electrode system and immersed in an activator for electrochemical scanning. The scanned sensor is cleaned and physically dried to obtain an activated sensor. The activator includes but is not limited to ferrous and / or ferric ions, potassium chloride and / or potassium ferrocyanide, benzoquinone and / or hydroquinone. The electrochemical method includes but is not limited to CV or It or DPV or LSV.

9. A sensor, characterized in that: The compound is prepared by the preparation method according to any one of claims 1 to 7.

10. Use of the sensor according to claim 8 in detecting the concentration of menthone.

11. Use of the sensor according to claim 9 in detecting menthone concentration, characterized in that: The concentration range of the detected menthone is 0.2-5 mM.

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