CN108414589A - Foam-like porous carbon net/nickel nano particle three-dimensional composite and its synthetic method and application - Google Patents
Foam-like porous carbon net/nickel nano particle three-dimensional composite and its synthetic method and application Download PDFInfo
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- CN108414589A CN108414589A CN201810082353.9A CN201810082353A CN108414589A CN 108414589 A CN108414589 A CN 108414589A CN 201810082353 A CN201810082353 A CN 201810082353A CN 108414589 A CN108414589 A CN 108414589A
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- 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
- G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- 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
Abstract
The present invention relates to a kind of synthetic methods of foam-like porous carbon net/nickel nano particle three-dimensional composite comprising following steps：1）By the fresh dry bagasse soaking at room temperature Jing Guo pulverization process in NiSO415 ~ 20 days in solution, take out, it is dry, obtain the bagasse of load nickel ion；2）By step 1）The bagasse for loading nickel ion calcines 1.5 ~ 2.5 h to get to foam-like porous carbon net/nickel nano particle three-dimensional composite under atmosphere of inert gases in 850 ~ 950 DEG C.Preparation method of the present invention green, simple, low consumption and raw material are cheap and easy to get；The foam-like porous carbon net/nickel nano particle three-dimensional composite being prepared can be used for making the high-performance analysis device of glucose electrochemical sensing assays, realize quick, sensitive, the highly selective detection to glucose, have potential application prospect.
Description
Technical field
The invention belongs to new material technology fields, and in particular to a kind of foam-like porous carbon net/nickel nano particle three-dimensional is multiple
Close object, its green synthesis method and the application in electrochemical glucose sensor structure.
Background technology
Biological material is cheap and easy to get, the functional group there are many environmentally protective and surfaces and micro constitutent, by simple
High-temperature calcination can be prepared carbon material.Currently, pomelo peel, bluish dogbane stem, cushaw stem, silk and discarded coffee grounds etc., this
A little biological materials are all used for the preparation of various pattern carbon materials.In recent years, by three-dimensional porous prepared by biological material
Self-supporting carbon material due to its enhancing mass transfer characteristic, big surface area, excellent mechanical stability and electric conductivity and
Hypotoxicity, and attract wide public concern.These excellent characteristics make three-dimensional porous carbon material become supported active catalyst particles
The good carrier of grain, thus shown in electro-catalysis, energy storage, fuel cell and electrochemical sensor field and potentially answered
Use foreground.And seek surface area greatly and the biological material of excellent adsorption becomes the three-dimensional porous carbon-active material compound of synthesis
Critical issue.In the present invention, propose, using discarded bagasse as carbon source, to utilize the official of its unique porous structure and surface
Adsorbing metal nickel ion can be rolled into a ball, then passes through the simple high-temperature calcination technology of a step, prepares foam-like porous carbon net/nickel and receive
Rice corpuscles three-dimensional composite.This preparation method green, simple, low consumption and turn waste into wealth, the glucose electricity constructed by the material
Chemical sensor has excellent performance, thus has potential application prospect in the measurement of glucose.
Invention content
Present invention aims to overcome that prior art defect, provides a kind of green, simple, low consumption foam-like porous carbon
Net/nickel nano particle three-dimensional composite and its synthetic method.
The present invention also provides above-mentioned foam-like porous carbon net/nickel nano particle three-dimensional composite and its in glucose electrification
The application in sensor structure is learned, quick, sensitive, the highly selective detection to glucose is realized, there is potential application
Foreground.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of synthetic method of foam-like porous carbon net/nickel nano particle three-dimensional composite comprising following steps：
1）By the fresh dry bagasse room temperature Jing Guo pulverization process（20~25℃）It is immersed in NiSO415 ~ 20 days in solution, take out,
It is dry, obtain the bagasse of load nickel ion；
2）By step 1）Load nickel ion bagasse under atmosphere of inert gases in 850 ~ 950 DEG C calcine 1.5 ~ 2.5 h to get
To foam-like porous carbon net/nickel nano particle three-dimensional composite.
Further, step 1）Specially：Fresh 0.4 ~ 1.0 g of dry bagasse for pulverization process of learning from else's experience, soaking at room temperature exist
The NiSO of a concentration of 0.05 ~ 0.2 mol/L of 25 mL415 ~ 20 days in solution, take out, in 60 ~ 80 DEG C of dry 12 ~ 15 h.
The present invention provides the foam-like porous carbon net/nickel nano particle three-dimensional being prepared using the above method is compound
Object.
The present invention also provides utilize above-mentioned foam-like porous carbon net/prepared Portugal of nickel nano particle three-dimensional composite
The application of grape sugar electrochemical sensor and the electrochemical glucose sensor in glucose assays.
The present invention utilizes functional group's adsorbing metal nickel of its unique porous structure and surface using discarded bagasse as raw material
Then ion passes through the simple high-temperature calcination technical finesse of a step, has prepared foam-like porous carbon net/nickel nano particle three
Tie up compound.Compared to the prior art, beneficial effects of the present invention：
1）The synthesis preparation method green of foam-like porous carbon net/nickel nano particle three-dimensional composite of the present invention, simple, low consumption and
Raw material are cheap and easy to get；
2）The unique foam-like porous carbon net of material/nickel nano particle three-dimensional composite structure of the present invention enhances electrolyte and electricity
The efficiency of transmission of son, convenient for its application in electrochemistry and electroanalysis field；
3）Foam-like porous carbon net/nickel nano particle three-dimensional composite of the present invention can be used for making glucose electrochemical sensing assays
High-performance analysis device, realize quick, sensitive, the highly selective detection to glucose, have potential application prospect.
Description of the drawings
Fig. 1 is 1 foam-like porous carbon net of comparative example（a）It is multiple with 1 foam-like porous carbon net of embodiment/nickel nano particle three-dimensional
Close object（b）SEM figure；
Fig. 2 is the XRD characterization figure of foam-like porous carbon net/nickel nano particle three-dimensional composite；
Fig. 3 is the sensor of foam-like porous carbon net/nickel nano particle three-dimensional composite preparation in 0 and 5 mmol/L（a）And not
With 1,2,3,4,5 mmol/L of concentration（b）Cyclic voltammogram in glucose solution；Wherein, 0.1 mol/L NaOH are to support electricity
Electrolyte solution；
In Fig. 4（a）For under the detection current potential of 0.45 V, different glucose is added into 0.1 mol/L NaOH solutions
When, the current-responsive of sensor prepared by foam-like porous carbon net of the present invention/nickel nano particle three-dimensional composite；（b）For oxidation
The linear relationship chart of electric current and concentration of glucose；
Fig. 5 is that 0.5 mM glucose is added into 0.1 mol/L NaOH solutions under the detection current potential of 0.45 V
（Glucose）With the object that may interfere with of same concentration, such as hydrogen peroxide（H2O2）, sodium chloride（NaCl）, dopamine（DA）, Vitamin C
Acid（AA）, uric acid（UA）When with 0.5 mM glucose, the electric current of sensor prepared by three-dimensional structure nano-complex of the present invention is rung
It answers.
Specific implementation mode
Technical scheme of the present invention is further discussed in detail with reference to embodiments, but protection scope of the present invention
It is not limited thereto.
Embodiment 1
A kind of synthetic method of foam-like porous carbon net/nickel nano particle three-dimensional composite comprising following steps：
1）Fresh 0.7 g of dry bagasse for pulverization process of learning from else's experience is put into beaker, and 25 mL concentration are added into beaker at room temperature
For the NiSO of 0.1 mol/L4Solution impregnates 18 days, takes out, and in 80 DEG C of dry 14 h, obtains the bagasse of load nickel ion；
2）By step 1）The bagasse of nickel ion is loaded full of Ar2High temperature process furnances in 900 DEG C calcine 2 h to get to
Foam-like porous carbon net/nickel nano particle three-dimensional composite.
Comparative example 1
A kind of preparation method of foam-like porous carbon net, specially：Fresh 0.7 g of dry bagasse for pulverization process of learning from else's experience,
Full of Ar2High temperature process furnances in 2 h are calcined in 900 DEG C to get to foam-like porous carbon net.
Material characterization.
The present invention uses scanning electron microscope（SEM）Measure the morphology and size of product；With X-ray powder diffraction instrument
（XRD）Detect the phase structure of product.
Fig. 1 is 1 foam-like porous carbon net of comparative example（a）It is multiple with 1 foam-like porous carbon net of embodiment/nickel nano particle three-dimensional
Close object（b）SEM figure.It can be seen that from Fig. 1 a：It is foam-like porous carbon net knot by the carbon material that bagasse dinectly bruning obtains
The aperture of structure, hole is micron order.It is calcined after it adsorbs nickel ion and obtains porous carbon net/nickel nano particle three-dimensional composite, shape
Looks are as shown in Figure 1 b.It can be seen that in Fig. 1 b：Porous carbon net surface has a large amount of nano particle, nano particle diameter to differ, small
About 100 nm of particle diameter, about 500 nm of bulky grain diameter.
Fig. 2 is the XRD characterization figure of 1 foam-like porous carbon net of embodiment/nickel nano particle three-dimensional composite.It can be with from Fig. 2
Find out：The characteristic diffraction peak of carbon and nickel is it is obvious that illustrate the bagasse for having adsorbed nickel ion during high-temperature calcination, nickel
Ion is reduced to metal nickel nano particle, to form foam-like porous carbon net/nickel nano particle three-dimensional composite.
Application of the material in glucose is built without enzyme electrochemical sensor.
Electrochemical glucose sensor is prepared using above-mentioned foam-like porous carbon net/nickel nano particle three-dimensional composite, is had
Body is：By 10 microlitres, foam-like porous carbon net/nickel nano particle three-dimensional composite aqueous dispersions drop coating of 2 mg/mL in cleaning
Dry glassy carbon electrode surface, dry to get.Utilize three-electrode system（There is foam-like porous carbon net/nickel nano particle with drop coating
The glass-carbon electrode of three-dimensional composite aqueous dispersions is working electrode, and Pt are auxiliary electrode, and saturated calomel electrode is reference electrode）
Carry out the Electrochemical Detection of glucose.
The present invention is based on glucose electrochemistry biographies prepared by above-mentioned foam-like porous carbon net/nickel nano particle three-dimensional composite
Sensor has the characteristics that.
（1）Electrocatalysis characteristic is strong
Fig. 3 is the sensor of foam-like porous carbon net/nickel nano particle three-dimensional composite preparation in 0 and 5 mmol/L（a）And not
With 1,2,3,4,5 mmol/L of concentration（b）Cyclic voltammogram in glucose solution；Wherein, 0.1 mol/L NaOH are to support electricity
Electrolyte solution.As can be seen from Figure 3：Sensor prepared by foam-like porous carbon net/nickel nano particle three-dimensional composite is to glucose
Sugar has apparent electric catalyticing effect, the addition of glucose that its oxidation current is caused to increase sharply, and this oxidation current is with glucose
The increase of concentration and increase.
（2）High sensitivity, detection limit low and response quickly
In Fig. 4（a）For under the detection current potential of 0.45 V, different glucose is added into 0.1 mol/L NaOH solutions
When, the current-responsive of sensor prepared by foam-like porous carbon net of the present invention/nickel nano particle three-dimensional composite；（b）For oxidation
The linear relationship chart of electric current and concentration of glucose.As can be seen from Figure 4：Sensor prepared by the three-dimensional manometer compound is to grape
Sugar has rapid and sensitively responds, and response time when reaching current maxima 90% is less than 3 s, detects limit down to 2.5 μ
Mol/L, linear response range are 5 ~ 1250 μM, and detection sensitivity is 221 μ A mM-1 cm-2, with document report by shaddock
Skin is three-dimensional porous carbon/nickel nano particle compound enzyme-free glucose sensor that raw material is prepared（4.8 μm of ol/ of detection limit
L, 207.3 μ A mM of detection sensitivity-1 cm-2, L. Wang, Y. Zhang, J. Yu, J. He, H. Yang, Y.
Ye, Y. Song, A green and simple strategy to prepare graphene foam-like three-
dimensional porous carbon/Ni nanoparticles for glucose sensing, Sens.
Actuators B, 2017, 239, 172–179）There is enzyme with Nano carbon balls are mixed by mulberry silk for the nitrogen that raw material is prepared
Sensor（Detection limit 39.1 μm of ol/L, 82.4 μ A mM of detection sensitivity-1 cm-2, T. Li, Y. Li, C. Wang,
Z.-D. Gao, Y.-Y. Song, Nitrogen-doped carbon nanospheres derived from cocoon
silk as metal-free electrocatalyst for glucose sensing, Talanta, 2015, 144,
1245–1251）It compares, detection limit is relatively low, and detection sensitivity greatly improves.
（3）Selectivity is good, is suitable for the analysis of biological sample
Fig. 5 is that 0.5 mM glucose is added into 0.1 mol/L NaOH solutions under the detection current potential of 0.45 V
（Glucose）With the object that may interfere with of same concentration, such as hydrogen peroxide（H2O2）, sodium chloride（NaCl）, dopamine（DA）, Vitamin C
Acid（AA）, uric acid（UA）When with 0.5 mM glucose, the electric current of sensor prepared by three-dimensional structure nano-complex of the present invention is rung
It answers.As can be seen from Figure 5：The current-responsive of interfering substance is very faint compared with the current-responsive of glucose, shows this foam
Shape porous carbon net/nickel nano particle three-dimensional composite sensor can be used for the selective determination of glucose, common in organism
Interfering substance to the electrocatalytic oxidation galvanic current of glucose without significantly interfering with.
Embodiment 2
A kind of synthetic method of foam-like porous carbon net/nickel nano particle three-dimensional composite comprising following steps：
1）Fresh 0.4 g of dry bagasse for pulverization process of learning from else's experience is put into beaker, and 25 mL concentration are added into beaker at room temperature
For the NiSO of 0.05 mol/L4Solution impregnates 15 days, takes out, and in 60 DEG C of dry 12 h, obtains the bagasse of load nickel ion；
2）By step 1）The bagasse of nickel ion is loaded full of Ar2High temperature process furnances in 850 DEG C calcine 1.5 h to get
To foam-like porous carbon net/nickel nano particle three-dimensional composite.
Embodiment 3
A kind of synthetic method of foam-like porous carbon net/nickel nano particle three-dimensional composite comprising following steps：
1）Fresh 1.0 g of dry bagasse for pulverization process of learning from else's experience is put into beaker, and 25 mL concentration are added into beaker at room temperature
For the NiSO of 0.2 mol/L4Solution impregnates 20 days, takes out, and in 70 DEG C of dry 15 h, obtains the bagasse of load nickel ion；
2）By step 1）The bagasse of nickel ion is loaded full of Ar2High temperature process furnances in 950 DEG C calcine 2.5 h to get
To foam-like porous carbon net/nickel nano particle three-dimensional composite.
To the electrochemical sensor using embodiment 2 and 3 foam-like porous carbon nets/nickel nano particle three-dimensional composite synthesis
Carry out electro-catalysis and the sensing analysis performance test of glucose, the results showed that the performance of electrochemical sensors prepared with embodiment 1
Quite.Illustrate that the present invention is based on glucose electrochemical sensings prepared by foam-like porous carbon net/nickel nano particle three-dimensional composite
Device realizes quick, sensitive, the highly selective detection to glucose, and superiority is notable compared with existing report document, has latent
Application prospect.
Claims (5)
1. a kind of synthetic method of foam-like porous carbon net/nickel nano particle three-dimensional composite, which is characterized in that including walking as follows
Suddenly：
1）By the fresh dry bagasse soaking at room temperature Jing Guo pulverization process in NiSO415 ~ 20 days in solution, take out, it is dry, it obtains
Load the bagasse of nickel ion；
2）By step 1）Load nickel ion bagasse under atmosphere of inert gases in 850 ~ 950 DEG C calcine 1.5 ~ 2.5 h to get
To foam-like porous carbon net/nickel nano particle three-dimensional composite.
2. the synthetic method of foam-like porous carbon net/nickel nano particle three-dimensional composite as described in claim 1, feature exist
In step 1）Specially：Fresh 0.4 ~ 1.0 g of dry bagasse for pulverization process of learning from else's experience, soaking at room temperature are a concentration of in 25 mL
The NiSO of 0.05 ~ 0.2 mol/L415 ~ 20 days in solution, take out, in 60 ~ 80 DEG C of dry 12 ~ 15 h.
3. the foam-like porous carbon net/nickel nano particle three-dimensional composite being prepared using claims 1 or 2 the method.
4. utilizing the prepared glucose electricity of foam-like porous carbon net/nickel nano particle three-dimensional composite described in claim 3
Chemical sensor.
5. foam-like porous carbon net/nickel nano particle three-dimensional composite is in electrochemical glucose sensor structure described in claim 3
Application in building.
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Cited By (7)
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| CN109387552A (en) * | 2018-10-12 | 2019-02-26 | 温州大学 | A kind of copper-based porous carbon microsphere composite material and preparation method and purposes |
| CN109437322A (en) * | 2018-11-05 | 2019-03-08 | 浙江工业大学 | A kind of compound carbon ball of metal oxide and preparation method thereof |
| CN109678133A (en) * | 2019-01-14 | 2019-04-26 | 桂林电子科技大学 | A kind of C-base composte material and its preparation method and application of nickel oxide doping |
| CN111847421A (en) * | 2020-07-29 | 2020-10-30 | 中国科学院宁波材料技术与工程研究所 | Ordered mesoporous carbon material, mesoporous carbon dopamine sensor, and preparation method and application thereof |
| CN112779550A (en) * | 2021-01-11 | 2021-05-11 | 中山大学 | Three-dimensional micron tubular hydrogen evolution reaction electrocatalyst and preparation method thereof |
| WO2022062409A1 (en) * | 2020-09-24 | 2022-03-31 | 江苏大学 | Enzyme-free glucose sensor, manufacturing method for same, and uses thereof |
| US11733199B2 (en) | 2020-09-24 | 2023-08-22 | Jiangsu University | Fabrication method of enzyme-free glucose sensor and use of enzyme-free glucose sensor fabricated by the same |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109387552A (en) * | 2018-10-12 | 2019-02-26 | 温州大学 | A kind of copper-based porous carbon microsphere composite material and preparation method and purposes |
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| CN109437322A (en) * | 2018-11-05 | 2019-03-08 | 浙江工业大学 | A kind of compound carbon ball of metal oxide and preparation method thereof |
| CN109678133A (en) * | 2019-01-14 | 2019-04-26 | 桂林电子科技大学 | A kind of C-base composte material and its preparation method and application of nickel oxide doping |
| CN111847421A (en) * | 2020-07-29 | 2020-10-30 | 中国科学院宁波材料技术与工程研究所 | Ordered mesoporous carbon material, mesoporous carbon dopamine sensor, and preparation method and application thereof |
| CN111847421B (en) * | 2020-07-29 | 2022-03-04 | 中国科学院宁波材料技术与工程研究所 | Application of ordered mesoporous carbon dopamine sensor |
| WO2022062409A1 (en) * | 2020-09-24 | 2022-03-31 | 江苏大学 | Enzyme-free glucose sensor, manufacturing method for same, and uses thereof |
| US11733199B2 (en) | 2020-09-24 | 2023-08-22 | Jiangsu University | Fabrication method of enzyme-free glucose sensor and use of enzyme-free glucose sensor fabricated by the same |
| CN112779550A (en) * | 2021-01-11 | 2021-05-11 | 中山大学 | Three-dimensional micron tubular hydrogen evolution reaction electrocatalyst and preparation method thereof |
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