CN110133063A - A kind of preparation method and its usage of bismuth molybdate/boron nitrogen-doped graphene photoelectric functional material - Google Patents
A kind of preparation method and its usage of bismuth molybdate/boron nitrogen-doped graphene photoelectric functional material Download PDFInfo
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Abstract
The invention belongs to electrochemical function field of nano material preparation, disclose a kind of preparation method and its usage of bismuth molybdate/boron nitrogen-doped graphene photoelectric functional material.It is specific to use a kind of simple, effective step solvent structure bismuth molybdate nanometer particle load boron nitrogen-doped graphene nanometer sheet, optical electro-chemistry sensor is constructed based on the photoelectric functional material.The bismuth molybdate of preparation/boron nitrogen-doped graphene photoelectric functional material presents excellent photoelectric properties, and the optical electro-chemistry sensor of building can be applied to life analysis field.
Description
Technical field
The invention belongs to electrochemical function field of nano material preparation, it is related to a kind of simply and effectively preparing bismuth molybdate and receiving
The method of rice corpuscles load boron nitrogen-doped graphene nanometer sheet.
Background technique
The advantages of optical electro-chemistry (PEC) sensor combines electrochemical sensor and optical electro-chemistry, basic principle are based on light
Electrochemical process.Optical electro-chemistry sensor is using light as excitaton source, and electric current is detection signal, utilizes light active material and object
Between occur electron transmission and cause the photocurrent variations of photoelectric material to be tested and analyzed.In recent years, optical electro-chemistry sensor
It the advantages such as is simple and convenient to operate by its high sensitivity, device, has in the fields such as chemistry, biology, environment huge using valence
Value.Currently, the further development of PEC biosensor is concentrated mainly on: (1) new strategy for manufacturing PEC sensor-based system is used to mention
High analyte performance and elimination interference；(2) design is able to respond the light active material of visible light or near infrared light, realizes signal amplification
Strategy.The Photoactive metal that design has high photodetachment efficiency and biocompatibility is dedicated in PEC field of biosensors
Semiconductor.Therefore, preparing nontoxic, the efficient visible light-responded light active material of one kind is the necessary condition for preparing PEC sensor.
Bismuth molybdate (Bi2MoO6) it is the visible light-responded photoelectric semiconductor material that a kind of new development is got up, wherein Yin Qite
Different layer structure, band structure (band gap is narrow) and special position has excellent photoelectric properties, is widely used in environment
The fields such as purification, microbial disinfection purification, photodissociation hydrogen manufacturing, solar-energy photo-voltaic cell.But Bi2MoO6Photo-generate electron-hole
Pair recombination rate it is high the defects of limit Bi2MoO6Application and research develop a kind of simple synthesis to overcome this defect
Bi2MoO6The method of base photoelectric functional material is necessary.
Graphene is a kind of novel carbon material, be one kind by single layer of carbon atom with sp2Hydridization connects into hexa-atomic ring skeleton
The two-dimensional atomic crystal of composition has good heating conduction, high light permeable rate, high theoretical specific surface area, good mechanical property
Energy and high electron mobility.Currently, graphene because its excellent performance be just widely used in sensor, electrode material with
And the fields such as functional polymer based composites.Currently, there are many document report Bi2MoO6With answering for graphene-based material
It closes, such as Bi2MoO6/ reduced graphene (Bi2MoO6/ rGO), Ag-rGO/Bi2MoO6Deng, these photoelectric functional materials have it is excellent
Performance, but since carrier mobility rate is slow, the disadvantages such as quantum yield is low limit answering for these photoelectric functional materials
With.To expand its application field, need further to be modified the performance of graphene, wherein more effective method
It is heteroatomic doping such as (N, B).It is reported that boron nitrogen-doped graphene (BNG) has superior physics compared to graphene
Chemical property shows huge development potentiality in multiple fields.Therefore, Bi2MoO6The photoelectric functional material being compounded to form with BNG
Perhaps, material can have excellent photoelectric properties.
Meanwhile lincomycin (LIN) is a kind of narrow-spectrum antibiotic for inhibiting gram-positive bacteria, is widely used to the mankind
And herding.It is some studies have shown that in animal derived food LIN residual may generate some adverse reactions, such as allergic reaction
And bacterial drug resistance.Current common detection method has efficient liquid phase (HPLC), fluorescence and electroluminescent etc..These methods by
It can be used for the detection of LIN in its high-precision, but they have some disadvantages, such as complicated for operation, time-consuming, large-scale instrument,
Sensitivity is low.Therefore, it is necessary to which the sensitive determination for LIN develops a kind of simple, detection method that is quick and having low cost.
Summary of the invention
The present invention is directed to invent a kind of simple, effective Bi2MoO6/ BNG photoelectric functional material preparation method.
The present invention is realized by following specific technical solution:
A kind of Bi2MoO6The preparation method of/BNG photoelectric functional material, includes the following steps:
(1) five nitric hydrate bismuths and two molybdic acid hydrate sodium are dissolved in ethanol solution respectively, at a certain temperature acutely
Two molybdic acid hydrate sodium solutions then, are added drop-wise to five nitric hydrate bismuth solution under magnetic stirring, obtain solution A by stirring；
(2) a certain amount of graphene oxide powder and ammonium pentaborate are dispersed in ethanol solution, ultrasonic disperse is uniform, obtains
Solution B；
(3) under magnetic stirring, after solution B being slowly dropped in solution A, it is kept stirring certain time；Then it will mix
It closes solution and is transferred in stainless steel autoclave and react；It is cooled to room temperature, after centrifugation, with deionized water and ethanol washing；After drying, obtain
To Bi2MoO6/ BNG photoelectric functional material.
In step (1), in the solution A, the amount ratio of five nitric hydrate bismuths, two molybdic acid hydrate bismuths and ethanol solution is
0.2425g:0.065g:10mL, whipping temp are 40~80 DEG C.
In step (2), in the solution B, the amount ratio of ammonium pentaborate, graphene oxide and ethanol solution is 100mg:5-
30mg:10mL.
In step (3), the volume ratio of solution A and solution B is 1:1, and mixing time is 0.5~2h.
In step (3), the reaction temperature is 140-180 DEG C, time 12-24h.
By Bi produced by the present invention2MoO6/ BNG photoelectric functional material is used to prepare optical electro-chemistry sensor to detect antibiosis
The purposes of element.Specific steps are as follows:
(1) in proportion by Bi2MoO6/ BNG photoelectric functional material is scattered in N, is prepared into N-dimethylformamide
Bi2MoO6/ BNG suspension；
(2) Bi of 10 μ L-50 μ L is taken2MoO6/ BNG suspension is modified in ITO electrode respectively, is dried at room temperature for obtaining
Bi2MoO6/ BNG/ITO then drips the adaptation liquid solution of Tu 10-50 μ L LIN, obtains aptamers-Bi2MoO6/ BNG/ITO electricity
Pole；
(3) take the LIN solution drop coating of 10-50 μ L various concentration in aptamers-Bi2MoO6On/BNG/ITO electrode, obtain
LIN/ aptamers-Bi2MoO6/ BNG/ITO electrode, using ITO as working electrode, saturated calomel electrode is as reference electrode, platinum filament
Photoelectrochemical assay is carried out under the irradiation of xenon source by electrochemical workstation three-electrode system as to electrode；It is based on
Bi2MoO6The optical electro-chemistry sensor of/BNG photoelectric functional material building is for detecting LIN.
In step (1), the Bi2MoO6The concentration of/BNG suspension is 5mg/mL.
In step (2), the LIN aptamers sequence: 5 '-CGCG TGAT GTGG TCGA TGCG ATAC GGTG
AGTC GCGC CACG GCTA CACA CGTC TCAG CGA-3′。
In step (3), the concentration of the LIN solution is 1 × 10-12~1 × 10-5mol L–1；The intensity of xenon source is
25%~100%.
Beneficial effects of the present invention
The present invention prepares Bi2MoO6/ BNG photoelectric functional material is successfully established optical electro-chemistry sensing as photoelectric activity material
Platform.
(1) one-step method that the present invention provides one kind under the conditions of mild solvent-thermal method prepares Bi2MoO6The synthesis side of/BNG
Method, synthesis technology is simple, and required raw material is raw material cheap and easily-available in the market, and the period is short, is suitble to industrialized production；
(2) present invention preparation Bi2MoO6/ BNG photoelectric functional material constructs optical electro-chemistry sensing as photoelectric activity material
Device can be used for life analysis field.
(3) proposed by the invention based on Bi2MoO6The photoelectric sensor of/BNG building realizes the detection to LIN.
Detailed description of the invention
Fig. 1 is the Bi of preparation2MoO6The transmission electron microscope picture of/BNG photoelectric functional material；
Fig. 2 is the Bi of preparation2MoO6The X-ray diffraction spectrogram of/BNG photoelectric functional material；
Fig. 3 is the Bi of different content graphene2MoO6The photoelectricity flow graph of/BNG；
Fig. 4 is the photoelectricity flow graph (A) and linear graph (B) for detecting LIN
Specific embodiment
Embodiment 1:
(1)Bi2MoO6The preparation of/BNG photoelectric functional material
Five nitric hydrate bismuth of 0.2425g and bis- molybdic acid hydrate sodium of 0.065g are dissolved in 5mL ethanol solution respectively 60
It is vigorously stirred at DEG C.Then, two molybdic acid hydrate sodium solutions are added drop-wise to five nitric hydrate bismuth solution under magnetic stirring and named
For solution A.
Then, 25mg graphene oxide powder and 100mg ammonium pentaborate are dispersed in 10mL ethanol solution and are ultrasonically treated
It obtains homogeneous solution and is named as solution B.
Later, solution B is slowly dropped to solution A, is kept stirring 1h.Finally, mixed solution is transferred to stainless steel high pressure
It is reacted for 24 hours at 160 DEG C in kettle；It is cooled to room temperature, after centrifugation, respectively three times with deionized water and ethanol washing；After drying, obtain
Bi2MoO6/ BNG photoelectric functional material.
(2) building of optical electro-chemistry sensor
Prepare Bi2MoO6/ BNG (5mg/mL) dispersion liquid takes the dispersion liquid of 40 μ L to modify in processed ITO electrode,
Using ITO electrode as working electrode, saturated calomel electrode is used as reference electrode, platinum filament to electrode, by electrochemical operation
It stands three-electrode system, under the irradiation of xenon source and carries out photoelectrochemical assay in nitrogen atmosphere.
(3) detection of LIN:
Respectively by 10-11, 10-10, 10-9, 10-8, 10-7, 10-6mol L-1LIN be added dropwise to aptamers-Bi2MoO6/BNG/
ITO electrode carries out photoelectric analysis under light source irradiation, and an incremental step by step trend is presented in photoelectric current, with the logarithm of concentration at
Good linear relationship, detection are limited to 3.3 × 10-12mol L-1。
Figure 1A is the Bi that this implementation obtains2MoO6The transmission electron microscope picture of photoelectric functional material, as seen from the figure, bismuth molybdate nanometer
Particle buildup is together and its bismuth molybdate nanometer particle size 10-20nm
B is the Bi that this implementation obtains2MoO6The transmission electron microscope picture of/BNG photoelectric functional material, as seen from the figure, bismuth molybdate nanometer
Uniform particle is dispersed in graphene nanometer sheet surface；
Fig. 2 is the Bi that this implementation obtains2MoO6The X-ray diffraction spectrogram of/BNG photoelectric functional material, as seen from the figure,
Occurs very strong bismuth molybdate crystal diffraction peak at 34.40 °, 36.12 °, 39.58 °, 46.86 °, 47.24 ° of and；
The Bi of Fig. 3 different content graphene2MoO6/ BNG photoelectricity flow graph, respectively 4% (a), 6% (b), 8% (c), 10%
(d), and 12% (e).As can be seen from the figure the photocurrent response of 10% graphene content is most strong.
Fig. 4 is the photoelectricity flow graph (A) and linear graph (B for detecting LIN.It can be seen that the increasing with LIN concentration from figure A,
The intensity of photoelectric current is gradually increased.Figure B can be seen that 10-11-10-6mol L-1Concentration ranges, the logarithm and photoelectricity of LIN concentration
Stream response shows good linear relationship, and detection limit can achieve 3.3 × 10-12mol L-1。
Embodiment 2
(1)Bi2MoO6The preparation of/BNG photoelectric functional material
Five nitric hydrate bismuth of 0.2425g and bis- molybdic acid hydrate sodium of 0.065g are dissolved in 5mL ethanol solution respectively 40
It is vigorously stirred at DEG C.Then, two molybdic acid hydrate sodium solutions are added drop-wise to five nitric hydrate bismuth solution under magnetic stirring and named
For solution A.
Then, 25mg graphene oxide powder and 100mg ammonium pentaborate are dispersed in 10mL ethanol solution and are ultrasonically treated
It obtains homogeneous solution and is named as solution B.
Later, solution B is slowly dropped to solution A, is kept stirring 0.5h.Finally, mixed solution is transferred to stainless steel height
20h is reacted at 140 DEG C in pressure kettle；It is cooled to room temperature, after centrifugation, respectively three times with deionized water and ethanol washing；After drying, obtain
Bi2MoO6/ BNG photoelectric functional material.
(2) building of optical electro-chemistry sensor
Prepare Bi2MoO6/ BNG (5mg/mL) dispersion liquid takes the dispersion liquid of 40 μ L to modify in processed ITO electrode,
Using ITO electrode as working electrode, saturated calomel electrode is used as reference electrode, platinum filament to electrode, by electrochemical operation
It stands three-electrode system, under the irradiation of xenon source and carries out photoelectrochemical assay in nitrogen atmosphere.
(3) detection of LIN:
Respectively by 10-11, 10-10, 10-9, 10-8, 10-7, 10-6mol L-1LIN be added dropwise to aptamers-Bi2MoO6/BNG/
ITO electrode carries out photoelectric analysis under light source irradiation, and an incremental step by step trend is presented in photoelectric current, with the logarithm of concentration at
Good linear relationship, detection are limited to 3.3 × 10-12mol L-1。
Embodiment 3
(1)Bi2MoO6The preparation of/BNG photoelectric functional material
Five nitric hydrate bismuth of 0.2425g and bis- molybdic acid hydrate sodium of 0.065g are dissolved in 5mL ethanol solution respectively 80
It is vigorously stirred at DEG C.Then, two hydration 3 acid sodium solutions of molybdenum are added drop-wise to five nitric hydrate bismuth solution under magnetic stirring and named
For solution A.
Then, 25mg graphene oxide powder and 100mg ammonium pentaborate are dispersed in 10mL ethanol solution and are ultrasonically treated
It obtains homogeneous solution and is named as solution B.
Later, solution B is slowly dropped to solution A, is kept stirring 2h.Finally, mixed solution is transferred to stainless steel high pressure
12h is reacted at 180 DEG C in kettle；It is cooled to room temperature, after centrifugation, respectively three times with deionized water and ethanol washing；After drying, obtain
Bi2MoO6/ BNG photoelectric functional material.
(2) building of optical electro-chemistry sensor
Prepare Bi2MoO6/ BNG (5mg/mL) dispersion liquid takes the dispersion liquid of 40 μ L to modify in processed ITO electrode,
Using ITO electrode as working electrode, saturated calomel electrode is used as reference electrode, platinum filament to electrode, by electrochemical operation
It stands three-electrode system, under the irradiation of xenon source and carries out photoelectrochemical assay in nitrogen atmosphere.
(3) detection of LIN:
Respectively by 10-11, 10-10, 10-9, 10-8, 10-7, 10-6mol L-1LIN be added dropwise to aptamers-Bi2MoO6/BNG/
ITO electrode carries out photoelectric analysis under light source irradiation, and an incremental step by step trend is presented in photoelectric current, with the logarithm of concentration at
Good linear relationship, detection are limited to 3.3 × 10-12mol L-1。
Claims (10)
1. a kind of Bi2MoO6The preparation method of/BNG photoelectric functional material, which comprises the steps of:
(1) five nitric hydrate bismuths and two molybdic acid hydrate sodium are dissolved in ethanol solution respectively, are vigorously stirred at a certain temperature,
Then, two molybdic acid hydrate sodium solutions are added drop-wise to five nitric hydrate bismuth solution under magnetic stirring, obtain solution A；
(2) a certain amount of graphene oxide powder and ammonium pentaborate are dispersed in ethanol solution, ultrasonic disperse is uniform, obtains solution
B；
(3) under magnetic stirring, after solution B being slowly dropped in solution A, it is kept stirring certain time；Then it will mix molten
Liquid, which is transferred in stainless steel autoclave, to react；It is cooled to room temperature, after centrifugation, with deionized water and ethanol washing；After drying, obtain
Bi2MoO6/ BNG photoelectric functional material.
2. Bi as described in claim 12MoO6The preparation method of/BNG photoelectric functional material, which is characterized in that in step (1),
In the solution A, five nitric hydrate bismuths, the amount ratio of two molybdic acid hydrate bismuths and ethanol solution is 0.2425g:0.065g:10mL,
Whipping temp is 40~80 DEG C.
3. Bi as described in claim 12MoO6The preparation method of/BNG photoelectric functional material, which is characterized in that in step (2),
In the solution B, the amount ratio of ammonium pentaborate, graphene oxide and ethanol solution is 100mg:5-30mg:10mL.
4. Bi as described in claim 12MoO6The preparation method of/BNG photoelectric functional material, which is characterized in that in step (3),
The volume ratio of solution A and solution B is 1:1, and mixing time is 0.5~2h.
5. Bi as described in claim 12MoO6The preparation method of/BNG photoelectric functional material, which is characterized in that in step (3),
The reaction temperature is 140-180 DEG C, time 12-24h.
6. by Bi made from any one of Claims 1 to 5 preparation method2MoO6/ BNG photoelectric functional material is used to prepare light
Electrochemical sensor detects the purposes of antibiotic.
7. purposes as claimed in claim 6, which is characterized in that specific steps are as follows:
(1) in proportion by Bi2MoO6/ BNG photoelectric functional material is scattered in N, is prepared into Bi in N-dimethylformamide2MoO6/BNG
Suspension；
(2) Bi of 10 μ L-50 μ L is taken2MoO6/ BNG suspension is modified in ITO electrode respectively, is dried at room temperature for obtaining
Bi2MoO6/ BNG/ITO then drips the adaptation liquid solution of Tu 10-50 μ L LIN, obtains aptamers-Bi2MoO6/ BNG/ITO electricity
Pole；
(3) take the LIN solution drop coating of 10-50 μ L various concentration in aptamers-Bi2MoO6On/BNG/ITO electrode, it is suitable to obtain LIN/
Ligand-Bi2MoO6/ BNG/ITO electrode, using ITO as working electrode, saturated calomel electrode is as reference electrode, platinum filament conduct pair
Electrode carries out photoelectrochemical assay by electrochemical workstation three-electrode system under the irradiation of xenon source；It is based on
Bi2MoO6The optical electro-chemistry sensor of/BNG photoelectric functional material building is for detecting LIN.
8. purposes as claimed in claim 7, which is characterized in that in step (1), the Bi2MoO6The concentration of/BNG suspension
For 5mg/mL.
9. purposes as claimed in claim 7, which is characterized in that in step (2), the LIN aptamers sequence: 5 '-CGCG
TGAT GTGG TCGA TGCG ATAC GGTG AGTC GCGC CACG GCTA CACA CGTC TCAG CGA-3′。
10. purposes as claimed in claim 7, which is characterized in that in step (3), the concentration of the LIN solution is 1 × 10-12~1 × 10-5mol L–1；The intensity of xenon source is 25%~100%.
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| CN111044586A (en) * | 2019-11-06 | 2020-04-21 | 江苏大学 | Preparation method of bismuth-doped polymeric carbon nitride nanocomposite material containing carbon defects |
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| CN113353884A (en) * | 2021-07-19 | 2021-09-07 | 桂林电子科技大学 | Magnesium-based composite hydrogen production material based on in-situ preparation of Bi-Mo-CNTs, and preparation method and application thereof |
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Cited By (10)
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| CN111044586A (en) * | 2019-11-06 | 2020-04-21 | 江苏大学 | Preparation method of bismuth-doped polymeric carbon nitride nanocomposite material containing carbon defects |
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| CN113340954A (en) * | 2021-05-14 | 2021-09-03 | 江苏大学 | Construction method of photo-assisted bipolar self-powered aptamer sensor for detecting lincomycin |
| CN113340954B (en) * | 2021-05-14 | 2023-04-11 | 江苏大学 | Construction method of photo-assisted bipolar self-powered aptamer sensor for detecting lincomycin |
| CN113353884A (en) * | 2021-07-19 | 2021-09-07 | 桂林电子科技大学 | Magnesium-based composite hydrogen production material based on in-situ preparation of Bi-Mo-CNTs, and preparation method and application thereof |
| CN113353884B (en) * | 2021-07-19 | 2022-06-14 | 桂林电子科技大学 | Magnesium-based composite hydrogen production material based on in-situ preparation of Bi-Mo-CNTs, and preparation method and application thereof |
| CN113702461A (en) * | 2021-08-11 | 2021-11-26 | 常州大学 | Preparation method of photoelectrochemistry self-powered sensor and application of photoelectrochemistry self-powered sensor in lincomycin detection |
| CN113702461B (en) * | 2021-08-11 | 2023-11-14 | 常州大学 | Preparation method of photoelectrochemistry self-energized sensor and application of photoelectrochemistry self-energized sensor in detection of lincomycin |
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Application publication date: 20190816 |