CN106435680A - Preparation method based on cuprous oxide non-enzyme glucose sensor - Google Patents

Preparation method based on cuprous oxide non-enzyme glucose sensor Download PDF

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CN106435680A
CN106435680A CN201610864118.8A CN201610864118A CN106435680A CN 106435680 A CN106435680 A CN 106435680A CN 201610864118 A CN201610864118 A CN 201610864118A CN 106435680 A CN106435680 A CN 106435680A
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electrolyte
preparation
electrode
glucose sensor
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余晓皎
张�杰
唐喜颜
胡德秀
杨谦
钮金芬
寇松
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Xian University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D9/00—Electrolytic coating other than with metals
    • C25D9/04—Electrolytic coating other than with metals with inorganic materials
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/28—Electrolytic cell components
    • G01N27/30—Electrodes, e.g. test electrodes; Half-cells
    • G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/416—Systems
    • G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage

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Abstract

The invention discloses a preparation method based on a cuprous oxide non-enzyme glucose sensor. The preparation method comprises the following specific steps: (1) ITO electric conducting glass is ultrasonically cleaned by solvent in an ultrasonic instrument for future use; (2) preparation of electrolyte: mixed liquid of copper acetate and lactic acid or copper acerate and glacial acetic acid is used as the electrolyte; (3) the pH of the electrolyte prepared in the step (2) is adjusted; (4) the electrolyte treated in the step (3) serves as electrolyte; the ITO electric conducting glass cleaned in the step (1) serves as a working electrode; a calomel electrode and a platinum electrode respectively serve as a reference electrode and a counter electrode; and an electrochemical deposition method is adopted to deposit and stir to obtain a Cu2O film electrode; and (5) the Cu2O film electrode obtained in the step (4) is cleaned and dried to obtain a Cu2O non-enzyme glucose sensor. The prepared sensor electrodes can quickly respond to glucose, and is wide in linear range, high in sensitivity, excellent in stability and low in detecting lower limit.

Description

A kind of preparation method based on Red copper oxide no enzyme type glucose sensor
Technical field
The invention belongs to technical field of nanometer material preparation is and in particular to a kind of passed based on Red copper oxide no enzyme type glucose The preparation method of sensor.
Background technology
Glucose is widespread in nature, and belongs to a kind of monosaccharide, and changes of contents in human body for the glucose is to people Class healthy closely bound up.On the one hand the metabolism of human body is exactly wherein content in human body for the glucose, and For diabeticss, its changes of contents is also critically important.Check that in human body, the most commonly used method of blood sugar content height is at present Extract blood measuring, for this method probably when dealing with improperly, patient can be caused infect, present one A little sensors obtain for the very difficult detection of glucose of low concentration, and susceptiveness is also very poor.Pass for containing enzymatic glucose at present The restrictive condition of sensor is more, and the activity of glucoseoxidase is subject to many impacts, temperature, the humidity of air, Acidity of Aikalinity All there is impact on it, or even the inactivation of enzyme can be caused, so that the precision of enzyme sensor is reduced even ineffective.Therefore, Research one kind no enzyme type glucose sensor has very big significance.
Content of the invention
It is an object of the invention to provide a kind of preparation method based on Red copper oxide no enzyme type glucose sensor is so that make Standby sensor electrode can respond rapidly to glucose, and range of linearity width, and sensitivity is high, under good stability, detection Limit is low.
The technical solution adopted in the present invention is, a kind of preparation side based on Red copper oxide no enzyme type glucose sensor Method, specifically implements according to following steps：
Step 1, ITO electro-conductive glass is cleaned with solvent supersonic in Ultrasound Instrument, standby；
Step 2, preparation electrolyte：Using the mixed liquor of Schweinfurt green and lactic acid or Schweinfurt green and glacial acetic acid as electrolyte；
The pH of the electrolyte that step 3, regulating step 2 are prepared；
, as electrolyte, the ITO electro-conductive glass that step 1 is cleaned is as work for step 4, the electrolyte after through step 3 Make electrode, calomel electrode and platinum electrode, respectively as reference electrode with to electrode, using electrochemical deposition method deposition and stirring, obtain To Cu2O membrane electrode；
Step 5, the Cu that step 4 is obtained2Cu is obtained after the cleaning of O membrane electrode, drying2O enzyme-free glucose sensor.
The feature of the present invention also resides in,
With acetone and dehydrated alcohol, ITO electro-conductive glass is cleaned by ultrasonic successively in step 1.
In step 2, acetic acid copper concentration is 14～30mmol/L, and lactic acid concn is 0.1～3.0mol/L, the concentration of glacial acetic acid For 0.05mol/L～1.0mol/L.
Step 3 is specially：Add the NaOH solution of 5mol/L in the electrolyte prepared toward described step 2, until electrolyte PH value is 4.9～11.0.
In step 4, deposition voltage is -0.47～-0.12V, and mixing speed is 100rpm～200rpm, and sedimentation time is 60min.
The invention has the beneficial effects as follows, a kind of preparation method based on Red copper oxide no enzyme type glucose sensor, preparation Cu2O sensor purity is higher, and structure and morphology is regular, and grainiess is homogeneous, wherein by the Cu of sword-shaped skeleton2O system The electrode reaction made is rapid, range of linearity width (5.55-111.01uM), sensitivity height (35.39mA cm-2·mM-1), detection Low (the 1mg L of lower limit-1), good stability, there is huge application prospect.
Brief description
Fig. 1 is a kind of Cu of the preparation method preparation based on Red copper oxide no enzyme type glucose sensor of the present invention2O thin film XRD figure；
Fig. 2 is that the present invention is a kind of continuously to be added in 0.78V based on the preparation method of Red copper oxide no enzyme type glucose sensor Plus Cu in various concentration of glucose2The ampere response curve of O；
Fig. 3 is a kind of preparation method based on Red copper oxide no enzyme type glucose sensor of the present invention to Cu2O is to glucose The glucose responding current data being repeated 6 times.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
A kind of preparation method based on Red copper oxide no enzyme type glucose sensor of the present invention, specifically real according to following steps Apply：
Step 1, ITO electro-conductive glass is cleaned with solvent supersonic in Ultrasound Instrument, standby, during cleaning, use successively acetone and Dehydrated alcohol is cleaned by ultrasonic to ITO electro-conductive glass；
Step 2, preparation electrolyte：Using the mixed liquor of Schweinfurt green and lactic acid or Schweinfurt green and glacial acetic acid as electrolyte, its In, acetic acid copper concentration is 14～30mmol/L, and lactic acid concn is 0.1～3.0mol/L, the concentration of glacial acetic acid be 0.05mol/L～ 1.0mol/L；
The pH of the electrolyte that step 3, regulating step 2 are prepared, adds 5mol/L toward step 2 in the electrolyte specially prepared NaOH solution, until electrolyte ph be 4.9～11.0；
, as electrolyte, the ITO electro-conductive glass that step 1 is cleaned is as work for step 4, the electrolyte after through step 3 Make electrode, calomel electrode and platinum electrode, respectively as reference electrode with to electrode, using electrochemical deposition method deposition and stirring, sink Long-pending voltage is -0.47～-0.12V, and mixing speed is 100rpm～200rpm, and sedimentation time is 60min, obtains Cu2O thin-film electro Pole；
Step 5, the Cu that step 4 is obtained2Cu is obtained after the cleaning of O membrane electrode, drying2O enzyme-free glucose sensor.
Sensor electrode pair using the preparation method preparation based on Red copper oxide no enzyme type glucose sensor for the present invention The electrochemical determination method of glucose is as follows：By Cu2O glucose sensor electrode without enzyme is placed in the NaOH of 0.1mol/L Row measures；Under the current potential between -0.8～1.2V, sweep speed is controlled to 10mV/s, and cyclic voltammetry scans steady to figure Fixed；After current stabilization, add glucose solution, and record current response, in 0.78V about the oxidation peak of glucose occurs； It is being continuously added to different glucose solution, is obtaining an ampere response curve, response concentration range is being 1～20mg/L, matching is bent Line, obtaining linear equation is J (mA cm-2)=- 0.129C (mg L-1) -0.301, using this linear equation and respective concentration Ratio, you can obtain Cu2The sensitivity of O electrode pair glucose solution.Measure in anti-interference corresponding to 2mg/L glucose In, add glucose, vitamin C, NaCl and histidine, and study response ampere curvilinear motion；To Cu2O is to glucose The response current being repeated 6 times, you can draw Cu2The stability to glucose responding for the O.
Fig. 1 is the Cu under different preparation conditions2O thin film XRD figure, it will be seen from figure 1 that all strong and sharp diffraction maximums Occur in 2 θ and be 29.55 °, 36.42 °, 42.30 °, 61.34 °, 74.40 ° and 77.75 ° of position, that is, correspond to Cu2O's (110), (111), (200), (220), (311) and (222) crystal face, match with normal data JCPDS No.05-0667, table It is now Cu2O cuprite structure, but the Cu under different system2Diffraction peak intensity difference corresponding to each crystal orientation of O thin film.From figure In as can be seen that from S1To S3-Cu2The diffraction peak intensity of O thin film (220) crystal face gradually becomes strong, the diffraction peak intensity of (110) crystal face Degree gradually weakens, and the diffraction peak intensity of (110) and (200) crystal face gradually weakens, and has arrived S3-Cu2O thin film its (110) and (200) Crystallographic plane diffraction peak is wholly absent.
Fig. 2 is Cu2The ampere response curve of O membrane electrode, wherein horizontal linear are the response curve to glucose for the substrate, It can be seen that when just adding glucose, after swift and violent response in electric current, current signal becomes zero, afterwards with glucose The electric current that changes of concentration does not have any response.Wherein black broken line is Cu2The ampere response curve to glucose for the O, can see Go out the increasing current with glucose in solutions concentration and stepped shape change occurs, and in each concentration change, electric current is sent out Raw response, instantaneous increase, slowly decrease up to afterwards balance, reach stable.Illustrate that it is rapid to glucose responding.
Fig. 3 is Cu2The response current datagram that O is repeated 6 times, wherein horizontal dotted line are the peak current value of response current, Solid horizontal line is response current balanced balanced current value.It can be seen that the peak current value of each response current has this certain Difference (this be probably every time add glucose after be not uniformly dispersed in the solution lead to), but the balance of response current Current value does not have particularly apparent difference.It will thus be seen that Cu2O has stronger stability to glucose responding, repeats After repeatedly, still there is preferable response performance.
Embodiment 1
A kind of preparation method based on Red copper oxide no enzyme type glucose sensor of the present invention, specifically real according to following steps Apply：
Step 1, ITO electro-conductive glass is cleaned with solvent supersonic in Ultrasound Instrument, standby, during cleaning, use successively acetone and Dehydrated alcohol is cleaned by ultrasonic to ITO electro-conductive glass；
Step 2, preparation electrolyte：Using the mixed liquor of Schweinfurt green and glacial acetic acid as electrolyte, wherein, acetic acid copper concentration is 14mmol/L, the concentration of glacial acetic acid is 0.1mol/L；
The pH of the electrolyte that step 3, regulating step 2 are prepared, adds 5mol/L toward step 2 in the electrolyte specially prepared NaOH solution, until electrolyte ph be 4.9；
, as electrolyte, the ITO electro-conductive glass that step 1 is cleaned is as work for step 4, the electrolyte after through step 3 Make electrode, calomel electrode and platinum electrode, respectively as reference electrode with to electrode, using electrochemical deposition method deposition and stirring, sink Long-pending voltage is -0.12V, and mixing speed is 100rpm, and sedimentation time is 60min, obtains Cu2O membrane electrode；
Step 5, the Cu that step 4 is obtained2Cu is obtained after the cleaning of O membrane electrode, drying2O enzyme-free glucose sensor.
Prepared Cu under the conditions of being somebody's turn to do2O pattern is polyhedral structure.
Embodiment 2
A kind of preparation method based on Red copper oxide no enzyme type glucose sensor of the present invention, specifically real according to following steps Apply：
Step 1, ITO electro-conductive glass is cleaned with solvent supersonic in Ultrasound Instrument, standby, during cleaning, use successively acetone and Dehydrated alcohol is cleaned by ultrasonic to ITO electro-conductive glass；
Step 2, preparation electrolyte：Using the mixed liquor of Schweinfurt green and lactic acid as electrolyte, wherein, acetic acid copper concentration is 14mmol/L, lactic acid concn is 0.1mol/L；
The pH of the electrolyte that step 3, regulating step 2 are prepared, adds 5mol/L toward step 2 in the electrolyte specially prepared NaOH solution, until electrolyte ph be 4.9；
, as electrolyte, the ITO electro-conductive glass that step 1 is cleaned is as work for step 4, the electrolyte after through step 3 Make electrode, calomel electrode and platinum electrode, respectively as reference electrode with to electrode, using electrochemical deposition method deposition and stirring, sink Long-pending voltage is -0.12V, and mixing speed is 100rpm, and sedimentation time is 60min, obtains Cu2O membrane electrode；
Step 5, the Cu that step 4 is obtained2Cu is obtained after the cleaning of O membrane electrode, drying2O enzyme-free glucose sensor.
Prepared Cu under this condition2O pattern is sword-shaped dendroid, and has obvious electro-catalysis response to glucose Performance.
Embodiment 3
A kind of preparation method based on Red copper oxide no enzyme type glucose sensor of the present invention, specifically real according to following steps Apply：
Step 1, ITO electro-conductive glass is cleaned with solvent supersonic in Ultrasound Instrument, standby, during cleaning, use successively acetone and Dehydrated alcohol is cleaned by ultrasonic to ITO electro-conductive glass；
Step 2, preparation electrolyte：Using the mixed liquor of Schweinfurt green and lactic acid as electrolyte, wherein, acetic acid copper concentration is 20mmol/L, lactic acid concn is 3.0mol/L；
The pH of the electrolyte that step 3, regulating step 2 are prepared, adds 5mol/L toward step 2 in the electrolyte specially prepared NaOH solution, until electrolyte ph be 11.0；
, as electrolyte, the ITO electro-conductive glass that step 1 is cleaned is as work for step 4, the electrolyte after through step 3 Make electrode, calomel electrode and platinum electrode, respectively as reference electrode with to electrode, using electrochemical deposition method deposition and stirring, sink Long-pending voltage is -0.47V, and mixing speed is 200rpm, and sedimentation time is 60min, obtains Cu2O membrane electrode；
Step 5, the Cu that step 4 is obtained2Cu is obtained after the cleaning of O membrane electrode, drying2O enzyme-free glucose sensor.
Prepared Cu under this condition2O pattern is triangular pyramidal.

Claims (5)

1. a kind of preparation method based on Red copper oxide no enzyme type glucose sensor is it is characterised in that specifically according to following step Rapid enforcement：
Step 1, ITO electro-conductive glass is cleaned with solvent supersonic in Ultrasound Instrument, standby；
Step 2, preparation electrolyte：Using the mixed liquor of Schweinfurt green and lactic acid or Schweinfurt green and glacial acetic acid as electrolyte；
The pH of the electrolyte that step 3, the described step 2 of regulation are prepared；
Step 4, using the electrolyte after described step 3 as electrolyte, the ITO electro-conductive glass that described step 1 is cleaned is made For working electrode, calomel electrode and platinum electrode respectively as reference electrode with to electrode, using electrochemical deposition method deposition with stir Mix, obtain Cu2O membrane electrode；
Step 5, the Cu that described step 4 is obtained2Cu is obtained after the cleaning of O membrane electrode, drying2O enzyme-free glucose sensor.
2. a kind of preparation method based on Red copper oxide no enzyme type glucose sensor according to claim 1, its feature It is, with acetone and dehydrated alcohol, ITO electro-conductive glass is cleaned by ultrasonic successively in described step 1.
3. a kind of preparation method based on Red copper oxide no enzyme type glucose sensor according to claim 1, its feature It is, in described step 2, acetic acid copper concentration is 14～30mmol/L, lactic acid concn is 0.1～3.0mol/L, the concentration of glacial acetic acid For 0.05mol/L～1.0mol/L.
4. a kind of preparation method based on Red copper oxide no enzyme type glucose sensor according to claim 1, its feature It is, described step 3 is specially：Add the NaOH solution of 5mol/L in the electrolyte prepared toward described step 2, until electrolyte PH value is 4.9～11.0.
5. a kind of preparation method based on Red copper oxide no enzyme type glucose sensor according to claim 1, its feature It is, in described step 4, deposition voltage is -0.47～-0.12V, mixing speed is 100rpm～200rpm, sedimentation time is 60min.
CN201610864118.8A 2016-09-29 2016-09-29 Preparation method based on cuprous oxide non-enzyme glucose sensor Pending CN106435680A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107192753A (en) * 2017-05-24 2017-09-22 中国科学技术大学 A kind of glucose sensing electrodes and its preparation method and application
CN108978189A (en) * 2018-07-13 2018-12-11 武汉纺织大学 Carbon nano-tube/poly pyrroles composite fibre and preparation method and its application in transistor sensor
CN110514706A (en) * 2019-08-15 2019-11-29 临沂大学 Enzyme-free glucose sensing element and preparation method and application
CN111321443A (en) * 2020-03-02 2020-06-23 辽宁工程技术大学 Preparation method of cuprous oxide film with reducible forbidden band width

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102735732A (en) * 2012-07-19 2012-10-17 西南大学 Preparation and application of nano-cuprous oxide based enzyme-free hydrogen peroxide sensor electrode
CN104569096A (en) * 2015-02-05 2015-04-29 盐城工学院 Construction method and detection method of cuprous oxide membrane-based enzyme free-oxygen sensitive glucose photo electrochemical sensor
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
CN105116030A (en) * 2015-07-27 2015-12-02 中国海洋大学 Cu2O@CuO semi-core-shell structure nano composite material and preparation method therefor

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102735732A (en) * 2012-07-19 2012-10-17 西南大学 Preparation and application of nano-cuprous oxide based enzyme-free hydrogen peroxide sensor electrode
CN104569096A (en) * 2015-02-05 2015-04-29 盐城工学院 Construction method and detection method of cuprous oxide membrane-based enzyme free-oxygen sensitive glucose photo electrochemical sensor
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
CN105116030A (en) * 2015-07-27 2015-12-02 中国海洋大学 Cu2O@CuO semi-core-shell structure nano composite material and preparation method therefor

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107192753A (en) * 2017-05-24 2017-09-22 中国科学技术大学 A kind of glucose sensing electrodes and its preparation method and application
CN107192753B (en) * 2017-05-24 2019-08-27 中国科学技术大学 A kind of glucose sensing electrodes and its preparation method and application
CN108978189A (en) * 2018-07-13 2018-12-11 武汉纺织大学 Carbon nano-tube/poly pyrroles composite fibre and preparation method and its application in transistor sensor
CN110514706A (en) * 2019-08-15 2019-11-29 临沂大学 Enzyme-free glucose sensing element and preparation method and application
CN111321443A (en) * 2020-03-02 2020-06-23 辽宁工程技术大学 Preparation method of cuprous oxide film with reducible forbidden band width

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Application publication date: 20170222