CN107238650A - A kind of two-dimentional nickel cobalt bimetallic MOFs nanometer sheets and its applied in glucose detection - Google Patents
A kind of two-dimentional nickel cobalt bimetallic MOFs nanometer sheets and its applied in glucose detection Download PDFInfo
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- CN107238650A CN107238650A CN201710432608.5A CN201710432608A CN107238650A CN 107238650 A CN107238650 A CN 107238650A CN 201710432608 A CN201710432608 A CN 201710432608A CN 107238650 A CN107238650 A CN 107238650A
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Abstract
The invention discloses the application in a kind of two-dimentional nickel cobalt bimetallic MOFs nanometer sheets and its glucose detection.The present invention has mainly synthesized two-dimentional nickel cobalt bimetallic MOFs nanometer sheets by one step hydro thermal method from bottom to top in the substrates such as nanoporous acupuncture needle, carbon paper, gold plaque, and it is applied to no enzyme type electrochemical glucose sensor as electrode, the relatively conventional ball polyhedral MOFs materials of the two-dimentional MOFs nanometer sheets material have the more avtive spots of exposure, the advantages of synergy of nickel and cobalt and higher quality charge transport ability, so as to effectively raise its glucose sensing performance.
Description
Technical field
The invention belongs to biosensor technique field, more particularly to a kind of two-dimentional nickel cobalt bimetallic MOFs nanometer sheets and its Portugal
Application in grape sugar detection.
Background technology
The performance without enzyme type glucose biological sensor is improved for the diagnosis of diabetes and is controlled most important.Two-dimentional material
Material is due to having the advantages that larger specific surface area, more avtive spots, faster mass transport can have higher catalysis
Activity.At present, the application study on two-dimensional material on without enzyme type glucose sensor is concentrated mainly on graphene, transition gold
Belong on the materials such as sulfide, metal oxide, layered double hydroxide, and be directly to metal ion or metal cluster
Node and organic ligand bridge to form metal-organic framework (MOFs) material with periodic network structure as electrode material
Almost not having but as glucose sensor, present MOFs synthesis pattern is confined to ball-type mostly, hexahedron, octahedron,
On the polyhedrons such as dodecahedron, wherein two dimension MOFs is seldom synthesized, and it is even more few to do glucose sensing application with two-dimentional MOFs
See.Present two dimension MOFs synthesis is main to be used top-down methods or adds the method for structure directing agent to close with down-top
Into, these synthetic method low yields, cumbersome, and destructible MOFs structure.The purpose of the present invention is to be directed to existing skill
The deficiency of art prepares simple down-top methods there is provided one kind and is prepared for New Two Dimensional nickel cobalt bimetallic MOFs Nano sheet materials
Material, and applied to electrochemical glucose sensor.
The content of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of two-dimentional nickel cobalt bimetallic MOFs nanometer sheets and
Application in its glucose detection.
The purpose of the present invention is achieved through the following technical solutions：A kind of two-dimentional nickel cobalt bimetallic MOFs nanometer sheets, lead to
Following steps are crossed to prepare：
(1) 0.8724g Nickelous nitrate hexahydrates and 0.8731g cabaltous nitrate hexahydrates are dispersed in 100mL deionization
In water, nickel cobalt metal mixed salt solution is obtained；
(2) 0.4348g amino terephthalic acid (TPA)s are dissolved in 20mL DMFs (DMF), obtain organic match somebody with somebody
Liquid solution；
(3) solution that 6mL steps 1 are prepared and the solution that 1mL steps 2 are prepared are taken respectively, are transferred to after mixing and are placed with 5mL
In DMF 25mL reactors, and 6h is reacted at 120 DEG C, obtain purple product；
(4) it will react after obtained purple product cleans with ethanol, and be dried in vacuo at 60 DEG C in step 3, obtain two
Tie up nickel cobalt bimetallic MOFs nanometer sheets.
A kind of application of two-dimentional nickel cobalt bimetallic MOFs nanometer sheets in examination of glucose concentration, the application is：By two dimension
Nickel cobalt bimetallic MOFs nanometer sheets are carried on nano-porous gold wire surface, and concentration of glucose is detected.
Further, the two-dimentional nickel cobalt bimetallic MOFs nanometer sheets are carried on the acupuncture needle surface by the following method：
Organic ligand solution described in nickel cobalt metal mixed salt solution described in 6mL and 1mL is mixed, with 5mL DMF and porous acupuncture needle 120
Hydro-thermal reaction 6h is carried out at DEG C；After cleaning, the acupuncture needle of two-dimentional nickel cobalt bimetallic MOFs nanometer sheets load is obtained.
The beneficial effects of the invention are as follows：The present invention has obtained two-dimentional nickel cobalt bimetallic MOFs by simple one step hydro thermal method
Nanometer sheet material, the electrode prepared using the material can apply to electrochemical glucose sensor.In terms of preparation, this method
The preparation of down-top methods is employed, with simple to operate compared with traditional top-down methods, without adding structure directing
The advantages of agent.In terms of catalytic activity, the two-dimentional nickel cobalt bimetallic MOFs nanometer sheet materials synthesized, than existing most of balls
Type and polyhedron MOFs materials have bigger specific surface area, and more avtive spots, the material also has the collaboration of nickel and cobalt
Effect, so as to improve the sensing capabilities to glucose.
Brief description of the drawings
Fig. 1 is the scanning electron microscope diagram piece of two-dimentional nickel cobalt bimetallic MOFs nanometer sheet materials prepared by the present invention
(SEM)。
Fig. 2 is the power spectrum picture (EDS) of two-dimentional nickel cobalt bimetallic MOFs nanometer sheet materials prepared by the present invention.
Fig. 3 is two-dimentional nickel cobalt bimetallic MOFs nanometer sheets material prepared by the present invention in 0.1M NaOH electrolytes
It is not added with 4mM glucose and adds the cyclic voltammogram of 4mM glucose.
Fig. 4 a are the two-dimentional nickel cobalt bimetallic MOFs nanometer sheets materials of the invention prepared in 0.1M NaOH electrolytes
Constantly add the I-T curves of glucose, operating voltage：0.5V.Fig. 4 b correspond to the calibration curve of Fig. 4 a I-T curves.
Embodiment
With reference to embodiment the invention will be further described the present invention technical solution, these embodiments can not
It is not understood as the limitation to technical solution.
Embodiment 1：The present embodiment prepares two-dimentional nickel cobalt bimetallic MOFs nanometer sheet materials, specifically includes following steps：
(1) 0.8724g Nickelous nitrate hexahydrates and 0.8731g cabaltous nitrate hexahydrates are dispersed in 100mL deionization
In water, nickel cobalt metal mixed salt solution is obtained；
(2) 0.4348g amino terephthalic acid (TPA)s are dissolved in 20mL DMFs (DMF), obtain organic match somebody with somebody
Liquid solution；
(3) take the mixed solution obtained in 6mL steps 1 and 1mL steps 2 to be transferred to respectively and be placed with 5mL DMF and one is received
In the 25mL reactors of meter Duo Kong acupuncture needles, and 6h is reacted at 120 DEG C, purple product is obtained on nanoporous acupuncture needle；
(4) it will react after obtained purple product cleans with ethanol, and be dried in vacuo at 60 DEG C in step 3, obtain two
Tie up nickel cobalt bimetallic MOFs nanometer sheets.
The scanning electron microscope diagram (SEM) for the two-dimentional nickel cobalt bimetallic MOFs nanometer sheet materials that Fig. 1 is prepared for the present invention,
As can be seen from the figure it is that two-dimentional nickel cobalt bimetallic MOFs nanometer sheet homogeneous verticals are grown in porous gold substrate, nanometer sheet diameter
About 100nm or so.
The power spectrum picture for the two-dimentional nickel cobalt bimetallic MOFs nanometer sheet materials that Fig. 2 is prepared for the present invention, can from figure
Go out prepared material and contain Ni, Co, C, N, O element, and each element keeps certain pattern, NiCo layered complementary type point
Cloth, illustrates two-dimentional nickel cobalt bimetallic MOFs nanometer sheet materials.In addition, the XRD of nickel cobalt bimetallic MOFs nanometer sheets and theoretical mould
The XRD of plan coincide very much, and further synthesized material is nickel cobalt bimetallic MOFs.
Embodiment 2：The present embodiment is used as glucose biological with prepared two-dimentional nickel cobalt bimetallic MOFs nanometer sheet materials
The application of sensor, key step is as follows：
A, respectively to be modified with the gold electrodes of two-dimentional nickel cobalt bimetallic MOFs nanometer sheets as working electrode, Pt pieces are to electricity
Pole, SCE is reference electrode, is assembled into three-electrode electro Chemical system and is tested；
When b, cyclic voltammetry, electrochemical window elects 0V~0.6V as, and it is 50mV/s to sweep speed；I-T curve voltages are elected as
0.5V, background current constantly adds different glucose solution after 10min reaches stable state, with liquid-transfering gun and serum is carried out
Mixing test, obtains current-responsive value i.e. staircase curve and calibration curve under different concentration of glucose；
Fig. 3 is the two-dimentional nickel cobalt bimetallic MOFs nanometer sheets material prepared by the present invention in 0.1M NaOH electrolytes
It is not added with 4mM glucose and adds the cyclic voltammogram of 4mM glucose, it is seen that adds after glucose, MOFs nanometer sheets
Material oxidation peak current substantially increases, and illustrates that this material has good catalytic effect to glucose, can be used as glucose sensor
Electrode material is used.
Fig. 4 a are the two-dimentional nickel cobalt bimetallic MOFs nanometer sheets materials of the invention prepared in 0.1M NaOH electrolytes
Constantly add the I-T curves of glucose, operating voltage：0.5V.Fig. 4 b correspond to the calibration curve of Fig. 4 a I-T curves.From
It can be seen that in figure, the sensitivity of the electrode is 370 μ AmM-1, the response time, to be less than 1s, the range of linearity be 6 μM of -8.9mM, detection pole
It is limited to 1 μM.
In addition, according to art-disclosed techniques, being respectively synthesized hexahedron (A), octahedra (B), dodecahedron (C) structure
Nickel cobalt bimetallic MOFs materials；Then by hexahedron (A), octahedra (B), dodecahedron (C) structure nickel cobalt bimetallic
MOFs materials are modified gold electrode respectively, degree of modification step (a) unanimously, and as working electrode according to described in step b
Method carry out cyclic voltammetry.Test result indicates that, compared to materials A B C, two-dimentional nickel cobalt bimetallic of the invention
MOFs nanometer sheets have higher sensitivity, the bigger range of linearity and smaller response time.
Claims (3)
1. a kind of two-dimentional nickel cobalt bimetallic MOFs nanometer sheets, it is characterised in that prepared by following steps：
(1) 0.8724g Nickelous nitrate hexahydrates and 0.8731g cabaltous nitrate hexahydrates are dispersed in 100mL deionized water,
Obtain nickel cobalt metal mixed salt solution；
(2) 0.4348g amino terephthalic acid (TPA)s are dissolved in 20mL DMFs (DMF), obtain organic ligand molten
Liquid；
(3) solution that 6mL steps 1 are prepared and the solution that 1mL steps 2 are prepared are taken respectively, are transferred to after mixing and are placed with 5mL DMF's
In 25mL reactors, and 6h is reacted at 120 DEG C, obtain purple product；
(4) it will react after obtained purple product cleans with ethanol, and be dried in vacuo at 60 DEG C in step 3, obtain two-dimentional nickel
Cobalt dual-metal MOFs nanometer sheets.
2. a kind of a kind of the answering in examination of glucose concentration of two-dimentional nickel cobalt bimetallic MOFs nanometer sheets described in claim 1
It is with, it is characterised in that the application：Two-dimentional nickel cobalt bimetallic MOFs nanometer sheets are carried on nano-porous gold wire surface, to Portugal
Grape sugar concentration is detected.
3. application according to claim 2, it is characterised in that the two-dimentional nickel cobalt bimetallic MOFs nanometer sheets pass through following
Method is carried on the acupuncture needle surface：Organic ligand solution described in nickel cobalt metal mixed salt solution described in 6mL and 1mL is mixed,
Hydro-thermal reaction 6h is carried out at 120 DEG C with 5mL DMF and porous acupuncture needle；After cleaning, two-dimentional MOFs nanometers of nickel cobalt bimetallic is obtained
The acupuncture needle of piece load.
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Cited By (13)
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|---|---|---|---|---|
| CN107837820A (en) * | 2017-11-21 | 2018-03-27 | 南京工业大学 | A kind of preparation method of two-dimentional MOFs material loads nano-particle |
| CN109400906A (en) * | 2018-12-12 | 2019-03-01 | 太原理工大学 | The method of more metal MOFs materials is directly prepared using bimetal complex |
| CN109776812A (en) * | 2019-02-21 | 2019-05-21 | 河北工业大学 | The preparation method of Cu base two-dimensional sheet MOFs material |
| CN111044590A (en) * | 2019-11-26 | 2020-04-21 | 云南大学 | CuNi-MOF nano-material modified electrode and application thereof |
| CN111154110A (en) * | 2019-12-30 | 2020-05-15 | 北京交通大学 | Two-dimensional frame structure electrode material and preparation method thereof, electrochemical enzyme-free glucose sensor and preparation method and application thereof |
| CN111537589A (en) * | 2020-05-13 | 2020-08-14 | 山东大学 | Method for detecting glucose based on cobalt-based metal organic framework enzyme-free glucose sensor |
| CN112403440A (en) * | 2020-11-18 | 2021-02-26 | 山西大学 | Magnetic recyclable CoNi-MOFs @ GR adsorbent, preparation method and application to adsorption of organic dye |
| CN112759514A (en) * | 2021-02-04 | 2021-05-07 | 福州大学 | Synthetic method of columnar copper fumarate with double-enzyme activity |
| CN113176315A (en) * | 2021-03-15 | 2021-07-27 | 杭州电子科技大学 | NiO/Au nanotube array flexible electrode with core-shell structure and application thereof |
| CN113933371A (en) * | 2021-10-25 | 2022-01-14 | 扬州大学 | Preparation method of flexible biosensor electrode |
| CN114235920A (en) * | 2021-12-20 | 2022-03-25 | 天津工业大学 | NiCo LDH/NiCoS @ C composite material and preparation method and application thereof |
| CN114539545A (en) * | 2022-01-13 | 2022-05-27 | 中国科学院宁波材料技术与工程研究所 | Bimetal-organic framework material and preparation method and application thereof |
| CN115109262A (en) * | 2022-06-10 | 2022-09-27 | 湖北工业大学 | Metal organic framework nanosheet, preparation method, working electrode and sensor |
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Cited By (18)
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| CN107837820A (en) * | 2017-11-21 | 2018-03-27 | 南京工业大学 | A kind of preparation method of two-dimentional MOFs material loads nano-particle |
| CN109400906A (en) * | 2018-12-12 | 2019-03-01 | 太原理工大学 | The method of more metal MOFs materials is directly prepared using bimetal complex |
| CN109400906B (en) * | 2018-12-12 | 2021-04-30 | 太原理工大学 | Method for directly preparing multi-metal MOFs material by utilizing bimetallic complex |
| CN109776812B (en) * | 2019-02-21 | 2021-11-23 | 河北工业大学 | Preparation method of Cu-based two-dimensional flaky MOFs material |
| CN109776812A (en) * | 2019-02-21 | 2019-05-21 | 河北工业大学 | The preparation method of Cu base two-dimensional sheet MOFs material |
| CN111044590A (en) * | 2019-11-26 | 2020-04-21 | 云南大学 | CuNi-MOF nano-material modified electrode and application thereof |
| CN111154110A (en) * | 2019-12-30 | 2020-05-15 | 北京交通大学 | Two-dimensional frame structure electrode material and preparation method thereof, electrochemical enzyme-free glucose sensor and preparation method and application thereof |
| CN111537589A (en) * | 2020-05-13 | 2020-08-14 | 山东大学 | Method for detecting glucose based on cobalt-based metal organic framework enzyme-free glucose sensor |
| CN111537589B (en) * | 2020-05-13 | 2021-09-21 | 山东大学 | Method for detecting glucose based on cobalt-based metal organic framework enzyme-free glucose sensor |
| CN112403440A (en) * | 2020-11-18 | 2021-02-26 | 山西大学 | Magnetic recyclable CoNi-MOFs @ GR adsorbent, preparation method and application to adsorption of organic dye |
| CN112403440B (en) * | 2020-11-18 | 2022-03-18 | 山西大学 | Magnetic recyclable CoNi-MOFs @ GR adsorbent, preparation method and application to adsorption of organic dye |
| CN112759514A (en) * | 2021-02-04 | 2021-05-07 | 福州大学 | Synthetic method of columnar copper fumarate with double-enzyme activity |
| CN113176315A (en) * | 2021-03-15 | 2021-07-27 | 杭州电子科技大学 | NiO/Au nanotube array flexible electrode with core-shell structure and application thereof |
| CN113933371A (en) * | 2021-10-25 | 2022-01-14 | 扬州大学 | Preparation method of flexible biosensor electrode |
| CN113933371B (en) * | 2021-10-25 | 2023-12-22 | 扬州大学 | Preparation method of flexible biosensor electrode |
| CN114235920A (en) * | 2021-12-20 | 2022-03-25 | 天津工业大学 | NiCo LDH/NiCoS @ C composite material and preparation method and application thereof |
| CN114539545A (en) * | 2022-01-13 | 2022-05-27 | 中国科学院宁波材料技术与工程研究所 | Bimetal-organic framework material and preparation method and application thereof |
| CN115109262A (en) * | 2022-06-10 | 2022-09-27 | 湖北工业大学 | Metal organic framework nanosheet, preparation method, working electrode and sensor |
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