CN103265061A - One-dimensional copper oxide nano-array glucose sensor electrode material and preparation method thereof - Google Patents
One-dimensional copper oxide nano-array glucose sensor electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a one-dimensional copper oxide nano-array glucose sensor electrode material and a preparation method thereof. The one-dimensional copper oxide nano-array glucose sensor electrode material is characterized in that a one-dimensional copper oxide nano-array grows on a copper sheet in situ. The preparation method comprises the following steps of based on a three-electrode system, etching the surface of a copper substrate by an anodic oxidation method and carrying out calcination so that a large-area, compact and uniform copper oxide nano-array is formed on the copper substrate. The preparation method has the advantages of mild reaction conditions, simple operation and low cost. The one-dimensional copper oxide nano-array glucose sensor electrode material has structural advantages such as obvious size effect, high specific surface area and high activity site expose. Through vertical growth orientation and independent constitutional units, the one-dimensional copper oxide nano-array glucose sensor electrode material has good conductivity and a good electron transmission capability. Therefore, in electroanalysis detection of a glucose oxidation reaction, the one-dimensional copper oxide nano-array glucose sensor electrode material has excellent sensitivity, a very wide linear range, a very low detection limit, good selectivity, good repeatability and good stability.
Description
Technical field
The invention belongs to the inorganic functional material field, be specifically related to one dimension cupric oxide nano sensor array electrode materials and preparation method thereof, this nano material can be used for the enzyme-free glucose biological sensor electrode.
Background technology
The analysis of various Chemical Composition is to weigh one of major criterion of human health status always in the blood of human body.Wherein the detection of glucose level provides important basis for diabetes clinical diagnosis and measurement metabolism, also provides the most effective solution route [Chem.Rev.2008,108,814] for the getting up early prevention of controlling the complication that is caused by diabetes.The method that detects at present blood sugar is a lot, wherein electrochemical analysis detect blood sugar concentration since its fast, characteristics such as sensitivity, accuracy height receive much concern [Microchim.Acta.2013,180,161].Begin from the eighties of last century the nineties, it is very general that the fixing glucose oxidase Study on Biosensor has become, this glucose oxidase enzyme biologic sensor has highly sensitive, selection type is good, the advantage that response speed is fast, but because the inherent defect that enzyme itself exists, higher relatively as the enzyme price, poor repeatability behind the immobilized enzyme, variety of problems such as different sorts enzyme fixed routine complexity and load enzymatic glucose biosensor operating environment harshness exist, make the fixedly development of glucose carbohydrate oxidase biosensor be subjected to some restrictions, so the research of enzyme-free glucose sensor has caused that people pay close attention to [Biosens.Bioelectron.2010 widely at present, 25,1402].But utilize the electrode materials of the structural advantage research electroanalysis glucose oxidase reaction of material to report but seldom, do not give full play to the structural advantage of material, based on this, we design the cupric oxide nano electrode materials of regulation and control different-shape array structure, to highlight structural advantage in the keying action of cupric oxide nano array electrode material in the reaction of electroanalysis glucose oxidase.
Present stage, copper oxide nano material is applied to the enzyme-free glucose Study on Biosensor to be had a lot, as the carbon nano-tube modified matrix material [Electrochem.Commun.2011 of cupric oxide, 13,363-365], copper oxide nano particle material [CrystEngComm.2010,12,1120-1126] etc.Its preparation method generally adopts hydrothermal method [Electroanalysis, 2010,23,497-502], electrochemical polarization [Electrochim.Acta.2010,55,1612-1618] etc.Though above-mentioned cupric oxide nano array electrode preparation methods is widely adopted, but there is certain limitation in its preparation process, if any the higher relatively synthesis temperature of needs maybe need to be coated in the conductive substrates surface, operate easy inadequately, the needs that have add the surfactivity auxiliary agent, and environment is had certain contaminative; Have synthetic the time need add the copper source or synthetic yield is not high, cost is bigger, the difficult realization that has is to the controllability of material pattern.Therefore develop a kind of simple to operate, environmental friendliness, the preparation method that cost is low, productive rate is high, obtain size homogeneous, compound with regular structure, cupric oxide nano electrode materials that the pattern controllability is good, have very important meaning, can be used as that electroanalysis detects the glucose oxidase reaction a kind of effectively, the electrode materials of excellent performance.
Summary of the invention
The purpose of this invention is to provide one dimension cupric oxide nano array electrode material and preparation method thereof, and this one dimension cupric oxide nano array is used as the electrode materials that electroanalysis detects the glucose oxidase reaction.
This cupric oxide nano array electrode material is growth in situ one dimension copper oxide nano material and distribute with array format on copper sheet, the shape of this one dimension copper oxide nano material is pipe, rod or banded, the diameter of this copper oxide nano material is 200-300nm, and length is 10-15 μ m; And have characteristics such as the growth of being vertically oriented, size homogeneous, compound with regular structure, pattern be controlled.
This inventive method need not to use any template and tensio-active agent, under the three-electrode system, utilizes anodised method that the copper substrate surface is carried out etching, forms big area, fine and close cupric oxide nano array uniformly through making the copper substrate after the calcining.The advantage of this method is characteristics such as reaction conditions gentleness, simple to operate, environmental friendliness, cost are low, productive rate height.This array cupric oxide nano electrode materials has significant dimensional effect, high-specific surface area, reach structural advantages such as high reactivity site exposure, vertical growth orientation and independent structures unit make its tool good electrical conductivity and electron transport ability, therefore in the time should being used as the reaction of electroanalysis detection glucose oxidase, represented fabulous sensitivity, extremely wide linearity range and extremely low detection line, having good selectivity, repeatability and stable simultaneously, is the electrode materials that a kind of electroanalysis with very big application prospect detects the glucose oxidase reaction.
Cupric oxide nano array electrode preparation methods, concrete steps are as follows:
A. be 99.99% copper sheet concentrated hydrochloric acid ultrasonic cleaning 5-10min with purity, with dehydrated alcohol or acetone ultrasonic cleaning 10min, clean up with deionized water more again that it is standby to obtain the copper substrate; Before using with the insulativity applying material at copper sheet simultaneously (being called the back side), avoid contacting with electrolytic solution.
B. adopting the three-electrode system electrochemical workstation, is working electrode with the copper sheet; Platinum electrode is counter electrode; Saturated calomel electrode is reference electrode, is that the KOH of 0.5-4.5mol/L is electrolyte solution with 40-50ml concentration, copper sheet is immersed area is 0.5-1cm in the electrolyte solution
2, utilize electrochemical workstation to apply constant electric current 0.75-4.0mA cm
-2, carry out the anodic polarization reaction;
C. take out copper sheet behind the polarization reaction 15-25min, use ethanol and deionized water rinsing 2-3 time respectively, be put in the constant temperature air dry oven dry again.
D. with the prepared copper sheet of step c under the atmosphere of nitrogen, 180-200 ℃ of roasting 2-4h obtained in the copper sheet surface growth electrode materials of one dimension cupric oxide nano array.
Fig. 1 is the electron scanning micrograph of cupric oxide nano array, shows on the figure that the densification of cupric oxide nano array covers the copper sheet surface uniformly, and the nanotube diameter is 300nm, and length is 10 μ m.
Fig. 2 is the high power transmission electron microscope photo of cupric oxide nano array, the nanotube pattern of clear demonstration hollow structure among the figure (A).High power photo (B) shows that the atom of two kinds of directions is respectively 0.25nm as its spacing of lattice and 0.27nm belong to respectively (002) crystal face and
Crystal face.Illustration is Fourier transform (FFT) image of CuO nano-array, corresponding high resolution lattice explanation oxide copper nanometer tube array edge
The direction growth.
Fig. 3 is the X-diffraction photo of cupric oxide nano array, shows among the figure that its diffraction peak of cupric oxide nano array and JCPDS compose the normal data (No.48-1548) of monocline phase CuO in the storehouse, fits like a glove, and is pure phase, and is free from foreign meter.
The above-mentioned cupric oxide nano array material that makes is applied to the reaction that electroanalysis detects glucose oxidase, has carried out cyclic voltammetric test, timing testing current, selectivity and stability test respectively, the results are shown in Figure 4-7.
Fig. 4 is the cyclic voltammetric test pattern of cupric oxide nano array, and the oxidation peak of tangible glucose appears in the clear 0.35V of being presented among the figure, and visible cupric oxide nano array electrode material has obvious response when electroanalysis is detected the oxidizing reaction of glucose.
Fig. 5 is the chronoamperogram of cupric oxide nano array, the adding concentration range of glucose is 0.1-1.3mmol/L, utmost point short-time current reaches stable behind each interpolation glucose, illustrate that its time of response is fast, and add electric current rising value basic fixed at every turn, illustrate that its linearity range is wide, it is done linear fit after, sensitivity reaches 1.89mA mM
-1Cm
-2
Fig. 6 is the selectivity test figure of cupric oxide nano array, wherein interfering substance is chosen as xitix (AA) and Dopamine HCL (DA), show among the figure that interfering substance is not obvious to the amplification of electric current, illustrates that cupric oxide nano array electrode material has good selectivity.
Fig. 7 is the stability test figure of cupric oxide nano array, and the time cycle is one month, every interval 5 days, and test cupric oxide nano array electrode is to the current-responsive of 0.02mmol/L glucose, and it is not obvious to find that electric current changes, and electric current descends less than 5% in month cycle.
In sum: the copper oxide nano material of the present invention's preparation detects glucose for electroanalysis and has good response, and it is used for the sensitivity of enzyme-free glucose biosensor can reach 1.89mAmM
-1Cm
-2, linearity range be 0 μ M to 3mM, simultaneously detection line is 0.1 μ M, and is 2.53% to xitix (AA) selectivity, is 3.09% to the selectivity of Dopamine HCL (DA), the range of decrease is 5% in the stability one month.
The invention has the beneficial effects as follows: the original position etching grows the cupric oxide nano array of structurally ordered densification in the copper substrate, this method need not to use any template and tensio-active agent, adopt anodised method preparation under the room temperature, characteristics such as this method reaction conditions gentleness, simple to operate, environmental friendliness, cost are low, productive rate height, product size homogeneous, the compound with regular structure of obtaining has good electroconductibility; By kind and the concentration of control concentration of electrolyte, regulate polarizing current size and time in addition, can synthesize the nano-array with different size size and pattern, realize that the pattern of material is controlled.Because this sintetics has structural advantage as above, makes it represent fabulous chemical property, it will have broad application prospects in fields such as electroanalysis detections.
Description of drawings
Fig. 1 is the SEM figure of the prepared oxide copper nanometer tube array of embodiment 1;
Fig. 2 is the HRTEM figure of the prepared oxide copper nanometer tube array of embodiment 1;
Fig. 3 is the XRD figure of the prepared oxide copper nanometer tube array of embodiment 1;
Fig. 4 is the cyclic voltammogram of the prepared oxide copper nanometer tube array of embodiment 1;
Fig. 5 is the chronoamperogram of the prepared oxide copper nanometer tube array of embodiment 1;
Fig. 6 is the selection performance map of the prepared oxide copper nanometer tube array of embodiment 1;
Fig. 7 is the stability figure of the prepared oxide copper nanometer tube array of embodiment 1;
Fig. 8 is the SEM figure of the prepared cupric oxide nano-rod array of embodiment 2.
Fig. 9 is the SEM figure of the prepared cupric oxide nano band array of embodiment 3.
Figure 10 is the SEM figure of the prepared cupric oxide nano band of embodiment 4 and nano-chip arrays.
Embodiment
Below in conjunction with specific embodiment the present invention is further described.The electrochemical workstation that adopts is the special electrochemical workstation of Cohan.
Embodiment 1:
A. be 99.99% copper sheet concentrated hydrochloric acid ultrasonic cleaning 5-10min with purity, again with dehydrated alcohol or acetone ultrasonic cleaning 10min, clean up with deionized water again, and be coated with one deck insulativity material in the one side (back side) of copper sheet, contact with electrolytic solution when avoiding following electrolysis.
B. the copper sheet after handling with step a is working electrode; Platinum electrode is counter electrode; Saturated calomel electrode is reference electrode, is that the KOH of 3.0mol/L is electrolyte solution with 50ml concentration, and copper sheet is immersed in the electrolyte solution, and the immersion area is 1.0cm
2, utilize electrochemical workstation to apply constant electric current 3.0mA cm
-2, carry out the anodic polarization reaction;
C. take out copper sheet behind the polarization reaction 25min, use ethanol and deionized water rinsing 3 sub-electrode surfaces respectively, be put in the constant temperature air dry oven dry again.
D. with the prepared copper sheet of step c under the atmosphere of nitrogen, 200 ℃ of roasting 3h can obtain size homogeneous, structurally ordered oxide copper nanometer tube.Wherein oxide copper nanometer tube size homogeneous is structurally ordered regular, and diameter is 300nm, and length is about 10 μ m.
Prepared oxide copper nanometer tube electrode materials SEM figure sees Fig. 1, and HRTEM figure sees Fig. 2, and XRD figure is seen Fig. 3.
The above-mentioned cupric oxide nano array material that makes is applied to the reaction of electroanalysis glucose oxidase.The reaction of electroanalysis glucose oxidase adopts electrochemical workstation (CHI d660) to detect.Taking place under three-electrode system equally, is working electrode with the oxide copper nanometer tube array, is counter electrode with Pt, and as reference electrode, electrolyte solution is that concentration is the NaOH solution of 1.0mol/L with standard calomel electrode, and wherein the reaction area of working electrode is 1cm
2, the sensing range that the electrochemistry cyclic voltammetric detects is-0.3-0.7V; Obtain Fig. 4.
Detection voltage for the timing current detecting is 0.32V, drips the glucose solution of 0.1mmol/L at every turn, treats that electric current rises when reaching platform, continues 40s and continues to add glucose solution, when the concentration of glucose is 1.3mmol/L, stops to add, and obtains Fig. 5.
For the selectivity analysis, with xitix and Dopamine HCL as interfering substance, add the glucose of 0.2mmol/L first, treat that electric current rises when reaching platform, adds the glucose of 0.2mmol/L and the AA of 0.002mmol/L again, treat that electric current rises when reaching platform again, continue to add the glucose of 0.2mmol/L and the DA of 0.002mmol/L, after reaction finishes, calculate the response value of each electric current, draw a diagram, obtain Fig. 6.
For stability analysis, with one month be the cycle, the response current value of the glucose of 0.2mmol/L is detected at every interval 5 days, the drop-out value of calculated response electric current obtains Fig. 7.
A. be 99.99% copper sheet concentrated hydrochloric acid ultrasonic cleaning 5-10min with purity, again with dehydrated alcohol or acetone ultrasonic cleaning 10min, clean up with deionized water again, and be coated with one deck insulativity material in the one side (back side) of copper sheet, contact with electrolytic solution when avoiding following electrolysis.
B. the copper sheet after handling with step a is working electrode; Platinum electrode is counter electrode; Saturated calomel electrode is reference electrode, is that the KOH of 2.0mol/L is electrolyte solution with 50ml concentration, and copper sheet is immersed in the electrolyte solution, and the immersion area is 1.0cm
2, utilize electrochemical workstation to apply constant electric current 2.5mA cm
-2, carry out the anodic polarization reaction.
C. take out copper sheet behind the polarization reaction 25min, use ethanol and deionized water rinsing 3 sub-electrode surfaces respectively, be put in the constant temperature air dry oven dry again.
D. with the prepared copper sheet of step c under the atmosphere of nitrogen, 200 ℃ of roasting 3h can obtain size homogeneous, structurally ordered cupric oxide nano-rod.Wherein cupric oxide nano-rod size homogeneous is structurally ordered regular, and diameter is 350nm, and length is about 15 μ m.
The SEM figure of prepared cupric oxide nano array sees Fig. 9.XRD is consistent with HRTEM and embodiment 1.
The above-mentioned cupric oxide nano array material that makes is applied to the reaction of electroanalysis glucose oxidase.Its reaction conditions is identical with embodiment 1.Cyclic voltammetric and timing electric current characterize, and select performance and stability figure and embodiment 1 basically identical.
Embodiment 3:
A. be 99.99% copper sheet concentrated hydrochloric acid ultrasonic cleaning 5-10min with purity, again with dehydrated alcohol or acetone ultrasonic cleaning 10min, clean up with deionized water again, and be coated with one deck insulativity material in the one side (back side) of copper sheet, contact with electrolytic solution when avoiding following electrolysis.
B. the copper sheet after handling with step a is working electrode; Platinum electrode is counter electrode; Saturated calomel electrode is reference electrode, is that the KOH of 1.5mol/L is electrolyte solution with 50ml concentration, and copper sheet is immersed in the electrolyte solution, and the immersion area is 1.0cm
2, utilize electrochemical workstation to apply constant electric current 2.0mA cm
-2, carry out the anodic polarization reaction.
C. take out copper sheet behind the polarization reaction 20min, use ethanol and deionized water rinsing 3 sub-electrode surfaces respectively, be put in the constant temperature air dry oven dry again.
D. with the prepared copper sheet of step c under the atmosphere of nitrogen, 200 ℃ of roasting 3h can obtain size homogeneous, structurally ordered cupric oxide nano array.Wherein cupric oxide nano band array sizes homogeneous is structurally ordered regular, and its thickness is 30 nanometers, and length is 3 μ m.
The SEM figure of prepared cupric oxide nano array sees Fig. 9.XRD is consistent with HRTEM and embodiment 1.
The above-mentioned cupric oxide nano array material that makes is applied to the reaction of electroanalysis glucose oxidase.Its reaction conditions is identical with embodiment 1.Cyclic voltammetric and timing electric current characterize, and select performance and stability figure and embodiment 1 basically identical.
Embodiment 4:
A. be 99.99% copper sheet concentrated hydrochloric acid ultrasonic cleaning 5-10min with purity, again with dehydrated alcohol or acetone ultrasonic cleaning 10min, clean up with deionized water again, and be coated with one deck insulativity material in the one side (back side) of copper sheet, contact with electrolytic solution when avoiding following electrolysis.
B. the copper sheet after handling with step a is for making electrode; Platinum electrode is counter electrode; Saturated calomel electrode is reference electrode, is that the KOH of 3.0mol/L is electrolyte solution with 40ml concentration, and copper sheet is immersed in the electrolyte solution, and the immersion area is 0.5cm
2, utilize electrochemical workstation to apply constant electric current 2.0mA cm
-2, carry out the anodic polarization reaction.
C. take out copper sheet behind the polarization reaction 25min, use ethanol and deionized water rinsing 3 sub-electrode surfaces respectively, be put in the constant temperature air dry oven dry again.
D. with the prepared copper sheet of step c under the atmosphere of nitrogen, 200 ℃ of roasting 3h can obtain size homogeneous, structurally ordered cupric oxide nano array.Wherein oxide copper nanometer tube array size homogeneous is structurally ordered regular, and diameter is 250nm, and length is about 10 μ m.
The SEM figure of prepared cupric oxide nano array sees Figure 10.XRD is consistent with HRTEM and embodiment 1.
The above-mentioned cupric oxide nano array material that makes is applied to the reaction of electroanalysis glucose oxidase.Its reaction conditions is identical with embodiment 1.Cyclic voltammetric and timing electric current characterize, and select performance and stability figure and embodiment 1 basically identical.
Claims (3)
1. one dimension cupric oxide nano array glucose sensor electrode material, this electrode materials is growth in situ one dimension copper oxide nano material and distribute with array format on the copper sheet surface, the shape of epontic one dimension copper oxide nano material is pipe, rod or banded, its diameter is 200-300nm, and length is 10-15 μ m; And have the growth of being vertically oriented, size homogeneous, compound with regular structure.
2. one dimension cupric oxide nano array glucose sensor electrode material according to claim 1, it is characterized in that this copper oxide nano material detects glucose for electroanalysis and has good response, it is used for the sensitivity of enzyme-free glucose biosensor can reach 1.89 mAmM
-1Cm
-2, linearity range be 0 μ M to 3 mM, simultaneously detection line is 0.1 μ M, and is 2.53% to xitix (AA) selectivity, is 3.09% to the selectivity of Dopamine HCL (DA), the range of decrease is 5% in the stability one month.
3. the described one dimension cupric oxide nano of claim 1 array glucose sensor electrode preparation methods, concrete steps are as follows:
A. be 99.99% copper sheet concentrated hydrochloric acid ultrasonic cleaning 5-10min with purity, with dehydrated alcohol or acetone ultrasonic cleaning 10min, clean up with deionized water more again that it is standby to obtain the copper substrate; Before using with the insulativity applying material in the copper sheet one side, contact with electrolytic solution avoiding;
B. adopting the three-electrode system electrochemical workstation, is working electrode with the copper sheet; Platinum electrode is counter electrode; Saturated calomel electrode is reference electrode, is that the KOH of 0.5-4.5 mol/L is electrolyte solution with 40-50ml concentration, copper sheet is immersed area is 0.5-1 cm in the electrolyte solution
2, utilize electrochemical workstation to apply constant electric current 0.75-4.0 mA cm
-2, carry out the anodic polarization reaction;
C. take out copper sheet behind the polarization reaction 15-25min, use ethanol and deionized water rinsing 2-3 time respectively, be put in the constant temperature air dry oven dry again;
D. with the prepared copper sheet of step c under the atmosphere of nitrogen, 180-200 ℃ of roasting 2-4 h obtained in the copper sheet surface growth electrode materials of one dimension cupric oxide nano array.
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| CN103454328A (en) * | 2013-09-15 | 2013-12-18 | 西北有色金属研究院 | Glucose detection Cu-based CuO membrane electrode and reparation method thereof |
| CN103531817A (en) * | 2013-10-17 | 2014-01-22 | 山东玉皇化工有限公司 | Three-dimensional copper nanowire array current collector for lithium ion battery and production method of three-dimensional copper nanowire array current collector |
| CN104713927A (en) * | 2015-03-16 | 2015-06-17 | 常州大学 | Electrochemical method for detecting sucralose in food |
| CN105040060A (en) * | 2015-05-25 | 2015-11-11 | 牡丹江师范学院 | Preparation method of non-enzyme glucose sensor electrode material based on CuO film |
| CN108982627A (en) * | 2018-06-13 | 2018-12-11 | 湖北工程学院 | A kind of detection method of enzyme-free glucose optical electro-chemistry sensor and concentration of glucose |
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| CN104713927A (en) * | 2015-03-16 | 2015-06-17 | 常州大学 | Electrochemical method for detecting sucralose in food |
| CN105040060A (en) * | 2015-05-25 | 2015-11-11 | 牡丹江师范学院 | Preparation method of non-enzyme glucose sensor electrode material based on CuO film |
| CN108982627A (en) * | 2018-06-13 | 2018-12-11 | 湖北工程学院 | A kind of detection method of enzyme-free glucose optical electro-chemistry sensor and concentration of glucose |
| CN109161958A (en) * | 2018-10-26 | 2019-01-08 | 长春理工大学 | A kind of method and device preparing copper surface super hydrophobic structure |
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| CN110550649A (en) * | 2019-08-23 | 2019-12-10 | 安徽大学 | Porous copper oxide nanobelt assembled film, electrode plate, preparation method and application thereof |
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