CN109778172A - One kind is for non-enzymatic glucose sensor composite nano materials and preparation method thereof - Google Patents
One kind is for non-enzymatic glucose sensor composite nano materials and preparation method thereof Download PDFInfo
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- CN109778172A CN109778172A CN201910128027.1A CN201910128027A CN109778172A CN 109778172 A CN109778172 A CN 109778172A CN 201910128027 A CN201910128027 A CN 201910128027A CN 109778172 A CN109778172 A CN 109778172A
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Abstract
The present invention relates to one kind for non-enzymatic glucose sensor composite nano materials and preparation method thereof, using Cu foil as matrix, connects Co (OH) as conductive bridge by graphene on Cu foil surface2And Cu2O.Preparation method includes: that the RGO/Cu with hierarchical structure is grown on Cu foil by one pot of hydro-thermal method in situ2O/Cu composite material, then by galvanoplastic in RGO/Cu2Co (OH) is generated on O/Cu composite material2To get.Composite nano materials stability of the present invention is good, has the advantages that the high sensitivity to glucose detection, anti-interference selectivity are strong, to improve the detection effect of glucose sensor, has a good application prospect.
Description
Technical field
It is the invention belongs to non-enzymatic glucose sensor field, in particular to a kind of to receive for non-enzymatic glucose sensor to be compound
Rice material and preparation method thereof.
Background technique
Diabetes are recurrent diseases in world wide.If can be with strict control concentration of glucose in normal physiological
In range, then it can control diabetic syndrome.It thereby produces and a series of is suitable for measuring in internal and external physiological solution
The glucometer device of concentration of glucose.Wherein, quickly with the development of sensitive glucose detection to clinical diagnosis, biological skill
Art and food industry are extremely important.Glucose enzyme electrode was proposed by Clark in 1962 earliest, and had been carried out from that time extensively
Research.Although enzymatic glucose sensor shows quick response and highly selective advantage, its preparation procedure it is complicated and
Glucose oxidase easy in inactivation.Compared with traditional enzymatic glucose detection method, the non-enzyme sensor for glucose detection has
Response is fast, advantage at low cost and easily operated.
The sensitivity of non-enzymatic glucose sensor, selectivity and linearly it is heavily dependent on elctro-catalyst chemically
Matter and structure.Noble metal and its alloy can be with direct electrochemistry oxidizing glucoses, but these elctro-catalysts are to glucose detection
High cost and the narrow range of linearity, so that they are difficult to the application of scale.In recent years, base metal transition metal oxide and hydrogen
Oxide has been used for the elctro-catalyst for studying glucose detection.In base metal transition metal hydroxide electrode activity material
In material, cobalt hydroxide (Co (OH)2) it is important one of transistion metal compound.Co(OH)2Non-enzymatic detect glucose in terms of by
To extensive concern, because of Co (OH)2/ CoOOH redox couple makes glucose easily be oxidized to glucolactone.In addition, by
In its good electrochemical stability, high electrocatalytic active and low cost, it is widely used to battery, supercapacitor and sensing
Device.However, the low intrinsic conductivity of the metal hydroxides limits their performances in glucose detection.With Co (OH)2Class
Seemingly, cuprous oxide (Cu2O) also highly useful as non-enzymatic glucose and H2O2The active material of sensor.As a kind of important p-type
Semiconductor, Cu2O have significant catalytic activity, good stability and low cost, be electrochemical sensor ideal material it
One.However, Cu2O has poor electric conductivity.In order to overcome this problem, researcher is absorbed in exploitation high conductivity and branch
Hold the nanocomposite that electroactive material is integrated.
Graphene has biggish specific surface area, unique two-dimensional structure, chemical stability and high conductivity, causes people
Extensive concern.Therefore, if Co (OH)2And (or) Cu2O forms nanocomposite in conjunction with graphene, will overcome single
The disadvantage of component metals oxide conducting difference, improves the electro catalytic activity of electrode.
Summary of the invention
Technical problem to be solved by the invention is to provide one kind for non-enzymatic glucose sensor composite nano materials and
Preparation method, the composite nano materials stability is good, strong with high sensitivity, the anti-interference selectivity to glucose detection
Advantage has a good application prospect to improve the detection effect of glucose sensor.
The present invention provides one kind to be used for non-enzymatic glucose sensor composite nano materials, using Cu foil as matrix, in Cu foil
Surface connects Co (OH) as conductive bridge by graphene2And Cu2O。
The present invention also provides a kind of preparation methods for non-enzymatic glucose sensor composite nano materials, comprising:
(1) ultrasonic disperse in ultrapure water is added in graphite oxide and obtains graphene oxide solution, then by graphene oxide
Solution and Cu foil are transferred in reaction kettle, and 20~25h, cooled to room temperature, washing, vacuum are heated at 160~200 DEG C
It is dry, obtain RGO/Cu2O/Cu composite material；
(2) by above-mentioned RGO/Cu2O/Cu composite material is placed in Co (NO3)2In solution, by being electroplated in RGO/Cu2O/Cu is multiple
Condensation material surface forms Co (OH)2, it is dried in vacuo, obtains for non-enzymatic glucose sensor composite nano materials.
The concentration of graphene oxide solution in the step (1) is 0.01~1mg/mL.
Cu foil (>=99.99%) in the step (1) with a thickness of 0.1~0.5mm.
Washing in the step (1) uses deionized water and ethanol washing 3~4 times.
Co (NO in the step (2)3)2The concentration of solution is 0.05~0.2mol/L.
Electroplating technique parameter in the step (2) are as follows: voltage -1.2~0.2V sweeps 5~50mV/s of speed, scanning circle number
1~3 circle.
Vacuum drying temperature in the step (1) and (2) is 60~80 DEG C, vacuum drying time is 6~for 24 hours.
Beneficial effect
(1) of the invention preparation method is simple, and gained composite nano materials have similar sandwich structure, wherein with
Cu foil is matrix, and graphene connects Co (OH) as conductive bridge2And Cu2O is formed Co (OH)2/RGO/Cu2O/Cu structure；
(2) present invention can not only play the excellent electric property of graphene, and can combine Co (OH)2And Cu2The good electricity of O
Chemical stability and high electrocatalytic active, while synergistic effect can be played on the compound interface of three kinds of nano materials, enhance it
Chemical property；
(3) present invention has the characteristics such as low in cost, stability is good, easy storage, long service life；
(4) present invention has the advantages that the high sensitivity to glucose detection, anti-interference selectivity are strong, to improve grape
The detection effect of sugared sensor, has a good application prospect.
Detailed description of the invention
Fig. 1 is X-ray diffraction (XRD) schematic diagram that non-enzymatic glucose sensor composite nano materials are used in embodiment 1；
Fig. 2 is the FE-SEM photo that non-enzymatic glucose sensor composite nano materials are used in embodiment 2；Left figure is low power
Several Co (OH)2/RGO/Cu2O/Cu structure；Right figure is Co (OH) under high magnification numbe2/RGO/Cu2O/Cu structure；
Fig. 3 is right in 0.1mol/L NaOH solution for non-enzymatic glucose sensor composite nano materials in embodiment 3
1mmol/L glucose carries out the cyclic voltammetry curve that difference sweeps speed；
Fig. 4 is right in 0.1mol/L NaOH solution for non-enzymatic glucose sensor composite nano materials in embodiment 3
The cyclic voltammetry curve of different glucose.
Fig. 5 is according to synthetic material (C in documentu2O- graphene) and embodiment 2 in material carry out catalysis oxidation grape
Sugared current strength comparison.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Graphite oxide used in embodiment is produced by Nanjing Xian Feng Nono-material Science & Technology Ltd.；Drug Co used
(NO3)2·6H2O (>=99%) and Cu foil (>=99.99%) are produced by Sinopharm Chemical Reagent Co., Ltd..
Embodiment 1
(1) graphite oxide for weighing 10mg is scattered in the ultrapure water of 50mL, ultrasonic disperse 1h, obtains graphene oxide point
Dispersion liquid；The Cu foil (>=99.99%) with a thickness of 0.1mm for dispersing liquor and wash clean is transferred in polytetrafluoroethylene (PTFE) simultaneously
It in the stainless steel cauldron of lining, is heated at 160 DEG C for 24 hours, cooled to room temperature, deionized water and ethyl alcohol is successively used after taking-up
Washing 3~4 times；It is then placed into drying, time 6h in 60 DEG C of vacuum drying oven and obtains RGO/Cu2O/Cu composite material.
(2) by above-mentioned RGO/Cu2O/Cu composite material is placed in 0.05mol/L Co (NO3)2In solution, voltage be -1.2~
Between 0.2V, fast 5mV/s is swept, scanning circle number: 1 circle, by being electroplated in RGO/Cu2O/Cu composite material surface forms Co (OH)2,
It is then placed into drying, time 6h in 60 DEG C of vacuum drying oven and obtains Co (OH)2/RGO/Cu2O/Cu composite material.
As shown in Figure 1, it will thus be seen that the composite nano materials that the present embodiment obtains are Co (OH)2/RGO/Cu2O/Cu is compound
Material.
Embodiment 2
(1) graphite oxide for weighing 15mg is scattered in the ultrapure water of 50mL, ultrasonic disperse 1h, obtains graphene oxide point
Dispersion liquid；The Cu foil (>=99.99%) with a thickness of 0.25mm for dispersing liquor and wash clean is transferred to polytetrafluoroethylene (PTFE) simultaneously
It in the stainless steel cauldron of liner, is heated at 180 DEG C for 24 hours, cooled to room temperature, deionized water and second is successively used after taking-up
Alcohol washs 3~4 times；It is then placed into drying, time 12h in 70 DEG C of vacuum drying oven and obtains RGO/Cu2O/Cu composite wood
Material.
(2) by above-mentioned RGO/Cu2O/Cu composite material is placed in 0.1mol/L Co (NO3)2In solution, voltage be -1.2V~
Between 0.2, fast 25mV/s is swept, scanning circle number: 2 circles, by being electroplated in RGO/Cu2O/Cu composite material surface forms Co (OH)2,
It is then placed into drying, time 12h in 70 DEG C of vacuum drying oven and obtains Co (OH)2/RGO/Cu2O/Cu composite material.
As shown in Figure 2, it will thus be seen that the composite nano materials that the present embodiment obtains have sandwich structure, and graphene is made
Co (OH) is connected for conductive bridge2And Cu2O。
Embodiment 3
(1) graphite oxide for weighing 20mg is scattered in the ultrapure water of 50mL, ultrasonic disperse 1h, obtains graphene oxide point
Dispersion liquid；The Cu foil (>=99.99%) with a thickness of 0.5mm for dispersing liquor and wash clean is transferred in polytetrafluoroethylene (PTFE) simultaneously
It in the stainless steel cauldron of lining, is heated at 200 DEG C for 24 hours, cooled to room temperature, deionized water and ethyl alcohol is successively used after taking-up
Washing 3~4 times；It is then placed into drying in 80 DEG C of vacuum drying oven, the time is for 24 hours, to obtain RGO/Cu2O/Cu composite material.
(2) by above-mentioned RGO/Cu2O/Cu composite material is placed in 0.2mol/L Co (NO3)2In solution, voltage be -1.2~
Between 0.2V, fast 50mV/s is swept, scanning circle number: 3 circles, by being electroplated in RGO/Cu2O/Cu composite material surface forms Co (OH)2,
It is then placed into drying in 80 DEG C of vacuum drying oven, the time is for 24 hours, to obtain Co (OH)2/RGO/Cu2O/Cu composite material.
As shown in Figure 3, it can be seen that with the increase for sweeping speed, the redox current potential of composite nano materials can become
Change.As shown in Figure 4, it can be seen that be added after different glucose, the redox current of composite nano materials significantly increases
By force.
According in embodiment 2 Parameter Conditions preparation non-enzymatic glucose sensor composite nano materials, specifically: weigh
The graphite oxide of 15mg is scattered in the ultrapure water of 50mL, and ultrasonic disperse 1h obtains graphene oxide dispersion；By graphite oxide
The Cu foil (>=99.99%) with a thickness of 0.25mm of dispersion liquid and wash clean is transferred to the stainless steel of polytetrafluoroethyllining lining simultaneously
It in reaction kettle, is heated at 180 DEG C for 24 hours, cooled to room temperature, deionized water and ethanol washing 3~4 times is used after taking-up.So
It is placed in drying, time 12h in 70 DEG C of vacuum drying oven afterwards and obtains RGO/Cu2O/Cu composite material.By RGO/Cu2O/Cu is multiple
Condensation material is placed in 0.1mol/L Co (NO3)2Electrochemistry plating is carried out in solution, voltage sweeps fast 25mV/ between -1.2~0.2V
S, scanning circle number: 2 circles, by being electroplated in RGO/Cu2O/Cu composite material surface forms Co (OH)2, it is then placed into 70 DEG C true
Dry in empty baking oven, time 12h obtains Co (OH)2/RGO/Cu2O/Cu composite material.
And the metal hydroxides prepared with Parameter Conditions in embodiment 3-graphene composite nano material compares, can be with
Find out and be added after glucose, the oxidation peak current of composite nano materials significantly increases.
It is grown what is mentioned in document (New J.Chem, 2017,41,9223-9229) on the graphene oxide of reduction
The Cu of hollow cube2O is detected for non-enzymatic glucose and is compared with synthesis composite nano materials in embodiment 2, can be seen
The oxidation peak current of composite nano materials of the invention is stronger out, and picture is as shown in Figure 5.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, although referring to aforementioned reality
Applying example, invention is explained in detail, for those skilled in the art, still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features.It is all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. one kind is used for non-enzymatic glucose sensor composite nano materials, it is characterised in that: using Cu foil as matrix, on Cu foil surface
Co (OH) is connected as conductive bridge by graphene2And Cu2O。
2. a kind of preparation method for non-enzymatic glucose sensor composite nano materials, comprising:
(1) ultrasonic disperse in ultrapure water is added in graphite oxide and obtains graphene oxide solution, then by graphene oxide solution
And Cu foil is transferred in reaction kettle, 20~25h is heated at 160~200 DEG C, cooled to room temperature, washing, vacuum are dry
It is dry, obtain RGO/Cu2O/Cu composite material；
(2) by above-mentioned RGO/Cu2O/Cu composite material is placed in Co (NO3)2In solution, by being electroplated in RGO/Cu2O/Cu composite wood
Expect that surface forms Co (OH)2, it is dried in vacuo, obtains for non-enzymatic glucose sensor composite nano materials.
3. a kind of preparation method for non-enzymatic glucose sensor composite nano materials according to claim 2, special
Sign is: the concentration of the graphene oxide solution in the step (1) is 0.01~1mg/mL.
4. a kind of preparation method for non-enzymatic glucose sensor composite nano materials according to claim 2, special
Sign is: Cu foil in the step (1) with a thickness of 0.1~0.5mm.
5. a kind of preparation method for non-enzymatic glucose sensor composite nano materials according to claim 2, special
Sign is: the washing in the step (1) uses deionized water and ethanol washing 3~4 times.
6. a kind of preparation method for non-enzymatic glucose sensor composite nano materials according to claim 2, special
Sign is: the Co (NO in the step (2)3)2The concentration of solution is 0.05~0.2mol/L.
7. a kind of preparation method for non-enzymatic glucose sensor composite nano materials according to claim 2, special
Sign is: the electroplating technique parameter in the step (2) are as follows: voltage -1.2~0.2V sweeps 5~50mV/s of speed, scanning circle number 1
~3 circles.
8. a kind of preparation method for non-enzymatic glucose sensor composite nano materials according to claim 2, special
Sign is: vacuum drying temperature in the step (1) and (2) is 60~80 DEG C, vacuum drying time is 6~for 24 hours.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111359624A (en) * | 2020-04-21 | 2020-07-03 | 中国科学院大学温州研究院(温州生物材料与工程研究所) | Core-shell hollow Cu (OH)2@Au@Co(OH)2Composite material, preparation method and application |
| CN112858405A (en) * | 2021-01-14 | 2021-05-28 | 东北大学 | Cu for non-enzymatic blood sugar detection2Preparation method of O yolk shell nanospheres |
| CN112881484A (en) * | 2021-01-14 | 2021-06-01 | 东北大学 | Preparation method of 3D electrode for non-enzymatic blood glucose detection |
| CN113219018A (en) * | 2020-01-21 | 2021-08-06 | 王翔郁 | Non-enzymatic sensor, non-enzymatic sensing device and method for manufacturing the same |
| TWI738190B (en) * | 2020-01-21 | 2021-09-01 | 國立清華大學 | None-enzyme sensor, non-enzyme sensor element and fabricating method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113219018A (en) * | 2020-01-21 | 2021-08-06 | 王翔郁 | Non-enzymatic sensor, non-enzymatic sensing device and method for manufacturing the same |
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| CN111359624B (en) * | 2020-04-21 | 2022-12-02 | 中国科学院大学温州研究院(温州生物材料与工程研究所) | Core-shell hollow Cu (OH) 2 @Au@Co(OH) 2 Composite material, preparation method and application |
| CN112858405A (en) * | 2021-01-14 | 2021-05-28 | 东北大学 | Cu for non-enzymatic blood sugar detection2Preparation method of O yolk shell nanospheres |
| CN112881484A (en) * | 2021-01-14 | 2021-06-01 | 东北大学 | Preparation method of 3D electrode for non-enzymatic blood glucose detection |
| CN112881484B (en) * | 2021-01-14 | 2021-11-16 | 东北大学 | Preparation method of 3D electrode for non-enzymatic blood glucose detection |
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Application publication date: 20190521 |