CN110514706A - Enzyme-free glucose sensing element and preparation method and application - Google Patents

Enzyme-free glucose sensing element and preparation method and application Download PDF

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Publication number
CN110514706A
CN110514706A CN201910751840.4A CN201910751840A CN110514706A CN 110514706 A CN110514706 A CN 110514706A CN 201910751840 A CN201910751840 A CN 201910751840A CN 110514706 A CN110514706 A CN 110514706A
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mask plate
enzyme
sensing element
glucose sensing
free glucose
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刘晨晨
崔光亮
张品华
王晓丽
李建福
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Linyi University
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Linyi University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
    • 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

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Molecular Biology (AREA)
  • Nanotechnology (AREA)
  • Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Analytical Chemistry (AREA)
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  • General Physics & Mathematics (AREA)
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  • Pathology (AREA)
  • Electrochemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
  • Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
  • Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)

Abstract

The invention discloses a kind of enzyme-free glucose sensing element and preparation method and applications, belong to technical field of biological.Solves the problems such as existing sensor senses ability is low, time-consuming, detection performance is low, the enzyme-free glucose sensing element is the glucose sensing element based on cuprous oxide two-dimensional array.Step: the Cu of deposition on a dielectric base is taken2The orderly nano-micro structure array sample material of O base, one end of the specimen material close to dielectric base center is covered with mask plate I, mask plate I is covered with mask plate II again, makes II center overlapping of axles of mask plate I and mask plate, wherein the width of mask plate II is greater than mask plate I；Golden conductive film is sputtered in dielectric base and II surface of mask plate by sputtering method；Mask plate II is removed, smears drain insulating layer on the specimen material being exposed；Mask plate I is removed, conductive electrode is connected on the gold conductive film of two sides.The present invention can be used for preparing enzyme-free glucose sensing element.

Description

Enzyme-free glucose sensing element and preparation method and application
Technical field
The present invention relates to a kind of enzyme-free glucose sensing element and preparation method and applications, belong to Measurement for Biotechnique neck Domain.
Background technique
Currently, glucose sensor mainly includes enzyme (based on glucose oxidase) and without enzyme (based on electrochemical oxidation) Two kinds, wherein oxidizing ferment base glucose sensor higher cost, and the structure based on enzyme itself and there are many problems, it is such as steady It is qualitative it is poor, reproducibility is lower, is easy to be affected by the ambient, enzyme-free glucose sensor overcomes these well It is insufficient.But the selectivity of no enzyme sensor is bad, poor anti jamming capability etc. is also a problem to be solved.Noble metal and its mixing Object such as gold, platinum, nickel, Jin-silver, gold-platinum enzyme-free glucose sensor is widely studied, but these materials that there are sensibility is low, The disadvantages of poor selectivity, lead to that sensor senses ability is low, time-consuming, detection performance is low.And since cost of manufacture is high, It cannot be widely applied to commodity production.
Summary of the invention
The technical problem to be solved by the present invention is overcoming the deficiencies of the prior art and provide, a kind of transmission speed is fast, electric conductivity Good, high sensitivity enzyme-free glucose sensing element；The present invention additionally provides the system of this enzyme-free glucose sensing element simultaneously Preparation Method and application.
The enzyme-free glucose sensing element is the glucose sensing element based on cuprous oxide two-dimensional array.
Utilize electric signal before and after enzyme-free glucose sensing element and glucose exposure based on cuprous oxide two-dimensional array Change to react concentration of glucose, the present invention utilizes four Probe-detection methods, passes through systematic characterization test, and detection oxidation is sub- Curent change of the copper two-dimensional material before and after contacting glucose, obtains the linear relationship of current-responsive and concentration of glucose, that is, builds The corresponding relationship of vertical current detection value and concentration of glucose, the detection of concentration of glucose, such as Fig. 3 are realized with this.
Preferred enzyme-free glucose sensing element, the cuprous oxide two-dimensional array is Cu2The orderly nano-micro structure battle array of O base Column material.
The preparation method of the enzyme-free glucose sensing element, comprising the following steps:
(1) Cu of deposition on a dielectric base is taken2The orderly nano-micro structure array sample material of O base, is covered with mask plate I and is leaned on One end of the specimen material at nearly dielectric base center, then mask plate I is covered with mask plate II, make in mask plate I and mask plate II Mandrel is overlapped, and wherein the width of mask plate II is greater than mask plate I；
(2) golden conductive film is sputtered in dielectric base and II surface of mask plate by sputtering method；
(3) mask plate II is removed, smears drain insulating layer on the specimen material being exposed；
(4) mask plate I is removed, conductive electrode is connected on the gold conductive film of two sides and is passed to get to the enzyme-free glucose Sensing unit.
The present invention utilizes the two-dimensional structure array material of electrochemical deposition experimental method building, has low manufacture cost, inspection Survey the advantages such as performance is good, using its two-dimensional nanostructure, cyclic array, large specific surface area, electron-transport speed fastly, electric conductivity The features such as good, high sensitivity, good selectivity, realize the detection to concentration of glucose.And what the present invention constructed receive microsensor Part has the characteristics that manufacturing technology requirement is low, at low cost, is easy to scale commodity production.The present invention provides a kind of new spirits Quick, fast and accurately enzyme-free glucose detecting element and application method.
The Cu2The preparation method of the orderly nano-micro structure array sample material of O base the following steps are included:
A, electric depositing solution is configured using copper nitrate, nitric acid, ultrapure water as raw material, the concentration of copper nitrate is 50mM/L, nitric acid 20μL；
B, the anode and cathode of electro-deposition, electrode long 2-2.5cm, wide 1-2mm are with the ultrapure copper foil of 30 μ m-thicks；
C, two copper electrodes are connected with power positive cathode respectively, then the parallel width in electrochemical growth room that is put into is 10-20mm, length are in the dielectric base of 15-25mm；
D, electrolyte is added dropwise between spacing is two electrodes of 6-10mm, covered simultaneously guarantees not produce between coverslip Anger bubble；
E, indoor temperature control will be grown at -1.7 to -2.0 DEG C, placed 10-20 minutes；Electrolyte keeps permanent after freezing Temperature state is placed 20 minutes；First applying DC voltage on the electrode, object to be deposited changes semisinusoidal deposition potential into after starting growth, Sample gradually deposits on a dielectric base, and dielectric base is taken out after deposition, cleans 3--5 times with ultrapure water to get deposition is arrived Cu on a dielectric base2The orderly nano-micro structure array sample material of O base.
Preferably, the Cu2The orderly nano-micro structure array sample material width of O base is greater than 5mm.
Preferably, I width of mask plate is 0.5-1mm, and II width of mask plate is 2-3mm.
Preferably, the resistance of the golden conductive film is less than 20 Ω/cm.
Preferably, DC voltage described in step e is 0.5-0.6V.
Preferably, semisinusoidal deposition potential voltage described in step e be 0.2-0.7V, frequency 0.5-1Hz.
Preferably, the enzyme-free glucose sensing element is connected on matched four probe conductions tester can be into The detection of horizontal electrical signal acquires.
Compared with prior art the beneficial effects of the present invention are:
(1) Cu prepared by the present invention2The orderly nano-micro structure array material of O base is two-dimensional structure material and long-range order, steady Qualitative height.State modulator when for building enzyme-free glucose sensing element is highly beneficial.Based on conductance preferential growth principle, material The electric conductivity of material has very strong advantage.
(2) enzyme-free glucose sensing element preparation method of the invention is simple, easy to store, and testing cost is low, as a result can be straight Reading is connect, is a kind of sensitive, fast and accurately clinical and family disease detection method.
(3) enzyme-free glucose sensing element high sensitivity (detection accuracy can achieve 0.1mM) of the invention, detection range (0.1-15mM) greatly.Detection electric current and the linear relationship that concentration of glucose is met are as shown in Figure 3.The nano effect of material, week Phase property structure provides big specific surface area, improves the contact area of device and glucose, to promote the electric oxygen of glucose Change catalysis, while to ascorbic acid present in blood of human body, urea, the different kinds of ions such as cysteine have very strong anti-interference Property.
Detailed description of the invention
Fig. 1 is the preparation flow figure of enzyme-free glucose sensing element of the present invention；
Fig. 2 is the Cu2The orderly nano-micro structure array material scanning electron microscope diagram of O base；
Fig. 3 is based on Cu2The linear relationship chart of O base orderly nano-micro structure array material concentration of glucose and electric current.
Specific embodiment
The present invention will be further described combined with specific embodiments below.
Embodiment 1
The enzyme-free glucose sensing element is the glucose sensing element based on cuprous oxide two-dimensional array.
The preparation method of the enzyme-free glucose sensing element, comprising the following steps:
Cu2The preparation of the orderly nano-micro structure array sample material of O base:
Electric depositing solution is configured using copper nitrate, nitric acid, ultrapure water as raw material, the concentration of copper nitrate is 50mM/L, 20 μ of nitric acid L；The anode and cathode of electro-deposition, electrode long 2cm, wide 1mm are with the ultrapure copper foil of 30 μ m-thicks；By two copper electrodes respectively with Power positive cathode is connected, and then the parallel width in electrochemical growth room that is put into is 10mm, and length is in the dielectric base of 15mm； Electrolyte is added dropwise between spacing is two electrodes of 6mm, covered simultaneously guarantees between coverslip without generating bubble；
Indoor temperature control will be grown at -1.7 DEG C, placed 10 minutes；Electrolyte keeps temperature constant state to place after freezing 20 minutes；First apply the DC voltage of 0.5V on the electrode, object to be deposited changes that voltage is 0.2V, frequency is into after starting growth The semisinusoidal deposition potential of 0.5Hz, sample gradually deposit on a dielectric base, and dielectric base is taken out after deposition, and use is ultrapure Water cleans 3--5 times to get the Cu to deposition on a dielectric base2The orderly nano-micro structure array sample material of O base.
The preparation of enzyme-free glucose sensing element:
(1) Cu of the deposition of width 5.5mm on a dielectric base is taken2The orderly nano-micro structure array sample material of O base, with covering Diaphragm plate I covers one end of the specimen material close to dielectric base center, then covers mask plate I with mask plate II, makes I He of mask plate II center overlapping of axles of mask plate, wherein I width of mask plate is 0.5mm, and II width of mask plate is 2mm；
(2) golden conductive film, the resistance of golden conductive film are sputtered in dielectric base and II surface of mask plate by sputtering method 19.8Ω/cm；
(3) mask plate II is removed, smears drain insulating layer on the specimen material being exposed；
(4) mask plate I is removed, conductive electrode is connected on the gold conductive film of two sides and is passed to get to the enzyme-free glucose Sensing unit.
Embodiment 2
The enzyme-free glucose sensing element, it is characterised in that: the cuprous oxide two-dimensional array is Cu2O base has Sequence nano-micro structure array material.
The preparation method of the enzyme-free glucose sensing element, comprising the following steps:
Cu2The preparation of the orderly nano-micro structure array sample material of O base:
Electric depositing solution is configured using copper nitrate, nitric acid, ultrapure water as raw material, the concentration of copper nitrate is 50mM/L, 20 μ of nitric acid L；The anode and cathode of electro-deposition, electrode long 2.5cm, wide 2mm are with the ultrapure copper foil of 30 μ m-thicks；Two copper electrodes are distinguished It is connected with power positive cathode, then the parallel width in electrochemical growth room that is put into is 20mm, and length is the dielectric base of 25mm On；Electrolyte is added dropwise between spacing is two electrodes of 10mm, covered simultaneously guarantees between coverslip without generating bubble；
Indoor temperature control will be grown at -2.0 DEG C, placed 20 minutes；Electrolyte keeps temperature constant state to place after freezing 20 minutes；First apply the DC voltage of 0.6V on the electrode, object to be deposited changes that voltage is 0.7V, frequency is into after starting growth The semisinusoidal deposition potential of 1Hz, sample gradually deposit on a dielectric base, and dielectric base is taken out after deposition, uses ultrapure water Cleaning 3--5 times to get the Cu to deposition on a dielectric base2The orderly nano-micro structure array sample material of O base.
The preparation of enzyme-free glucose sensing element:
(1) Cu of the deposition of width 6mm on a dielectric base is taken2The orderly nano-micro structure array sample material of O base, uses exposure mask Plate I covers one end of the specimen material close to dielectric base center, then covers mask plate I with mask plate II, make mask plate I and cover II center overlapping of axles of diaphragm plate, wherein I width of mask plate is 1mm, and II width of mask plate is 3mm；
(2) golden conductive film, the resistance 18 of golden conductive film are sputtered in dielectric base and II surface of mask plate by sputtering method Ω/cm；
(3) mask plate II is removed, smears drain insulating layer on the specimen material being exposed；
(4) mask plate I is removed, conductive electrode is connected on the gold conductive film of two sides and is passed to get to the enzyme-free glucose Sensing unit.
Embodiment 3
The enzyme-free glucose sensing element, it is characterised in that: the cuprous oxide two-dimensional array is Cu2O base has Sequence nano-micro structure array material.
The preparation method of the enzyme-free glucose sensing element, comprising the following steps:
Cu2The preparation of the orderly nano-micro structure array sample material of O base:
Electric depositing solution is configured using copper nitrate, nitric acid, ultrapure water as raw material, the concentration of copper nitrate is 50mM/L, 20 μ of nitric acid L；The anode and cathode of electro-deposition, electrode long 2.2cm, wide 1.5mm are with the ultrapure copper foil of 30 μ m-thicks；By two copper electrodes point It is not connected with power positive cathode, then the parallel width in electrochemical growth room that is put into is 15mm, and length is the insulation base of 20mm On bottom；Electrolyte is added dropwise between spacing is two electrodes of 8mm, covered simultaneously guarantees between coverslip without generating bubble；
Indoor temperature control will be grown at -1.9 DEG C, placed 15 minutes；Electrolyte keeps temperature constant state to place after freezing 20 minutes；First apply the DC voltage of 0.55V on the electrode, object to be deposited changes that voltage is 0.5V, frequency is into after starting growth The semisinusoidal deposition potential of 0.7Hz, sample gradually deposit on a dielectric base, and dielectric base is taken out after deposition, and use is ultrapure Water cleans 3--5 times to get the Cu to deposition on a dielectric base2The orderly nano-micro structure array sample material of O base.
The preparation of enzyme-free glucose sensing element:
(1) Cu of the deposition of width 6.2mm on a dielectric base is taken2The orderly nano-micro structure array sample material of O base, with covering Diaphragm plate I covers one end of the specimen material close to dielectric base center, then covers mask plate I with mask plate II, makes I He of mask plate II center overlapping of axles of mask plate, wherein I width of mask plate is 0.8mm, and II width of mask plate is 2.5mm；
(2) golden conductive film, the resistance 19 of golden conductive film are sputtered in dielectric base and II surface of mask plate by sputtering method Ω/cm；
(3) mask plate II is removed, smears drain insulating layer on the specimen material being exposed；
(4) mask plate I is removed, conductive electrode is connected on the gold conductive film of two sides and is passed to get to the enzyme-free glucose Sensing unit.
The enzyme-free glucose sensing element of the present invention metal oxide materials stable based on property, property are stablized, Ke Yichang Time storage, element validity period greatly prolongs, and construction procedures are simple, and technical requirements are low, is easy to commercially produce, knot of the present invention Structure is simple, and detection reproducibility is strong, and technical indicator is reliable and stable.

Claims (10)

1. a kind of enzyme-free glucose sensing element, it is characterised in that: be the glucose sensing member based on cuprous oxide two-dimensional array Part.
2. enzyme-free glucose sensing element according to claim 1, it is characterised in that: the cuprous oxide two-dimensional array It is Cu2The orderly nano-micro structure array material of O base.
3. a kind of preparation method of enzyme-free glucose sensing element of any of claims 1 or 2, it is characterised in that including following step It is rapid:
(1) Cu of deposition on a dielectric base is taken2The orderly nano-micro structure array sample material of O base is covered with mask plate I close to absolutely One end of the specimen material of edge base center, then mask plate I is covered with mask plate II, make II central axis of mask plate I and mask plate It is overlapped, wherein the width of mask plate II is greater than mask plate I；
(2) golden conductive film is sputtered in dielectric base and II surface of mask plate by sputtering method；
(3) mask plate II is removed, smears drain insulating layer on the specimen material being exposed；
(4) mask plate I is removed, connects conductive electrode on the gold conductive film of two sides to get the enzyme-free glucose sensing element is arrived Part.
4. the preparation method of enzyme-free glucose sensing element according to claim 3, it is characterised in that: the Cu2O base The preparation method of orderly nano-micro structure array sample material the following steps are included:
A, electric depositing solution is configured using copper nitrate, nitric acid, ultrapure water as raw material, the concentration of copper nitrate is 50mM/L, 20 μ L of nitric acid；
B, the anode and cathode of electro-deposition, electrode long 2-2.5cm, wide 1-2mm are with the ultrapure copper foil of 30 μ m-thicks；
C, two copper electrodes are connected with power positive cathode respectively, then the parallel width in electrochemical growth room that is put into is 10- 20mm, length are in the dielectric base of 15-25mm；
D, electrolyte is added dropwise between spacing is two electrodes of 6-10mm, covered simultaneously guarantees between coverslip without generating gas Bubble；
E, indoor temperature control will be grown at -1.7 to -2.0 DEG C, placed 10-20 minutes；Electrolyte keeps constant temperature shape after freezing State is placed 20 minutes；First apply DC voltage on the electrode, object to be deposited changes semisinusoidal deposition potential, sample into after starting growth It gradually deposits on a dielectric base, dielectric base is taken out after deposition, clean 3--5 times with ultrapure water to get exhausted to being deposited on Cu in edge substrate2The orderly nano-micro structure array sample material of O base.
5. the preparation method of enzyme-free glucose sensing element according to claim 4, it is characterised in that: the Cu2O base Orderly nano-micro structure array sample material width is greater than 5mm.
6. the preparation method of enzyme-free glucose sensing element according to claim 5, it is characterised in that: the mask plate I width is 0.5-1mm, and II width of mask plate is 2-3mm.
7. the preparation method of enzyme-free glucose sensing element according to claim 6, it is characterised in that: the gold is conductive The resistance of film is less than 20 Ω/cm.
8. the preparation method of enzyme-free glucose sensing element according to claim 7, it is characterised in that: described in step e DC voltage is 0.5-0.6V.
9. the preparation method of enzyme-free glucose sensing element according to claim 8, it is characterised in that: described in step e Semisinusoidal deposition potential voltage is 0.2-0.7V, frequency 0.5-1Hz.
10. a kind of application of enzyme-free glucose sensing element described in claim 1-2 or 4-9, it is characterised in that: described Enzyme-free glucose sensing element is connected on matched four probe conductions tester the detection acquisition that can carry out electric signal.
CN201910751840.4A 2019-08-15 2019-08-15 Enzyme-free glucose sensing element and preparation method and application Pending CN110514706A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105671604A (en) * 2016-01-26 2016-06-15 临沂大学 Improved method for two-dimensional electrochemical construction of nano-micro electrical component
CN106435680A (en) * 2016-09-29 2017-02-22 西安理工大学 Preparation method based on cuprous oxide non-enzyme glucose sensor
CN109507267A (en) * 2018-11-27 2019-03-22 临沂大学 The sensing material and preparation method thereof fast detected for biological hydrogen sulfide

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105671604A (en) * 2016-01-26 2016-06-15 临沂大学 Improved method for two-dimensional electrochemical construction of nano-micro electrical component
CN106435680A (en) * 2016-09-29 2017-02-22 西安理工大学 Preparation method based on cuprous oxide non-enzyme glucose sensor
CN109507267A (en) * 2018-11-27 2019-03-22 临沂大学 The sensing material and preparation method thereof fast detected for biological hydrogen sulfide

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