CN106124588A - A kind of preparation method of electrochemistry nonyl phenol sensor based on titania-doped/molybdenum bisuphide composite - Google Patents
A kind of preparation method of electrochemistry nonyl phenol sensor based on titania-doped/molybdenum bisuphide composite Download PDFInfo
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- 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
- G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
- G01N27/3275—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/76—Chemiluminescence; Bioluminescence
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- 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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- 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
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- G01N27/416—Systems
- G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
Abstract
The invention discloses the preparation method of a kind of electrochemica biological sensor.The method comprises the steps of firstly, preparing a kind of New Two Dimensional nano-electrode material titania-doped/molybdenum bisuphide composite Cu TiO2/MoS2The i.e. two-dimensional nano composite of copper-doped titanium dioxide nano square In-situ reaction molybdenum bisuphide, utilizes the good biocompatibility of this material and big specific surface area, nonyl phenol antibody in load, when detecting, owing to copper-doped titanium dioxide can be with catalyzing hydrogen peroxide in-situ preparation O2, producing electrochemical signals, recycling antibody is combined the impact on electron transport ability with the specific quantification of antigen so that current intensity reduces accordingly, finally achieves the structure of the biosensor using unmarked electrochemical method detection nonyl phenol.
Description
Technical field
The present invention relates to the preparation method of a kind of electrochemica biological sensor.Belong to Nano-function thin films to pass with biological
Sensor technical field.
Background technology
Environmental estrogens refers to that a class enters after body, has the synthesis of normal endocrine material in interfering bodies, discharges, transports
The processes such as defeated, combination, metabolism, activate or suppress the function of hormonal system, thus destroy maintenance organism stability and regulation and control are made
Compound, environmental estrogens is of a great variety, including artificial-synthetic compound and natural plant estrogen, be distributed widely in from
So in boundary.Nonyl phenol is a kind bisphenols synthetic estrogen.At present, the method for detection nonyl phenol mainly has chromatography, matter
Spectrometry etc..This type of method instrument is valuable, operation complexity, and laboratory personnel just can detect after needing professional training.Therefore, research and development
Low cost, to detect nonyl phenol sensor fast, highly sensitive, high specificity significant.
Electrochemica biological sensor is widely used in facing due to advantages such as it are highly sensitive, specificity is good, easy and simple to handle
The fields such as bed diagnosis, pharmaceutical analysis, environmental monitoring.The most especially more with the research of unmarked electrochemical immunosensor, it is crucial
Technology be to improve the fixed amount of modified electrode antagonist and to the test signal response speed of end liquid and size.Titanium dioxide is
A kind of photocatalyst material being most widely used, simultaneously because good biocompatibility, is also commonly used as electrode matrix material.By
Can expose more high miller index surface in sheet-like titanium dioxide nanomaterial, have higher catalysis activity, titanium dioxide is received
Rice sheet has ratio nanoparticle preferably application prospect, and the research for titanium dioxide nanoplate also receives much concern.But, dioxy
The sensitivity that change titanium poorly conductive also limit the electrochemical sensor built by single titanium dioxide nano material is the highest,
It is unfavorable for actual application.Semiconductor nano material is modified or is combined special nano material, on the one hand adds electrode ratio
Surface area, strengthens electrodes conduct ability, and on the other hand the two can produce concerted catalysis effect, and bigger enhancing is to hydrogen peroxide
Solution H2O2Catalytic response speed and current responsing signal size, be greatly improved detection sensitivity.Therefore, design, prepare height
Effect, stable titanium dioxide nanoplate and trim thereof are the key technologies preparing electrochemical sensor.
(chemical formula is MoS to molybdenum bisuphide2) nano material, there is two-dimensional layered structure, be most widely used solid profit
One of lubrication prescription.Lamellar two-dimension nano materials after its stripping, is the semiconductor nano material of excellent performance, except having big ratio
Surface area, can improve load capacity as catalyst and the carrier of biological antibody, also has simultaneously as promoter excellent
Electron transmission performance.
At present, most synthesizing mean be all be separately synthesized after, then catalyst is combined with carrier, process is numerous
Trivial, productivity is the highest.Therefore, for In-situ reaction preparation, there is the two dimensional nano electrodes material of good electric chemical property to have extensively
Application prospect and important scientific meaning.
Summary of the invention
It is an object of the invention to provide a kind of prepare simple, highly sensitive, detection quickly, the electrochemical student of high specificity
The preparation method of thing sensor, prepared sensor, can be used for quick, the Sensitive Detection of nonyl phenol.Based on this purpose, this
Bright be first prepared for a kind of New Two Dimensional nano-electrode material titania-doped/molybdenum bisuphide composite Cu-TiO2/
MoS2, i.e. the two-dimensional nano composite of copper-doped titanium dioxide nano square In-situ reaction molybdenum bisuphide, utilizes this material
Good biocompatibility and big specific surface area, nonyl phenol antibody in load, when detecting, due to Copper-cladding Aluminum Bar titanium dioxide
Titanium can be with catalyzing hydrogen peroxide in-situ preparation O2, producing electrochemical signals, recycling antibody is combined with the specific quantification of antigen
Impact on electron transport ability so that current intensity reduces accordingly, finally achieves employing unmarked electrochemical method inspection
Survey the structure of the biosensor of nonyl phenol.
The technical solution used in the present invention is as follows:
1. a preparation method for electrochemistry nonyl phenol sensor based on titania-doped/molybdenum bisuphide composite, its
It is characterised by that described electrochemistry nonyl phenol sensor is by working electrode, titania-doped/molybdenum bisuphide composite, nonyl
Phenol antibody, bovine serum albumin form;Described titania-doped/molybdenum bisuphide composite is that copper-doped titanium dioxide is received
The two-dimensional nano composite Cu-TiO of rice square In-situ reaction molybdenum bisuphide2/MoS2;
It is characterized in that, described preparation method includes following preparation process:
A. Cu-TiO is prepared2/MoS2;
B. electrochemistry nonyl phenol sensor is prepared;
Wherein, step a prepares Cu-TiO2/MoS2Concretely comprise the following steps:
(1) take 0.6 g molybdenum disulfide powder and 0.2 ~ 2.0 mmol mantoquita joins 3 ~ 10 mL n-butyllithium solutions jointly
In, at nitrogen protection and 30 ~ 60 DEG C, stir 12 ~ 48 hours, obtain reacted solution;
(2) utilize reacted solution in non-polar solven washing step (1), at 30 ~ 60 DEG C, then carry out water bath sonicator
Process, after having processed, the solution after recycling non-polar solven carrying out washing treatment, vacuum drying, obtain the molybdenum bisuphide of copper intercalation
Nano material;
(3) the molybdenum disulfide nano material taking the copper intercalation that 10 ~ 500 mg steps (2) prepare joins 5 mL butyl titanates
In, after stirring 1 hour, it is slowly added to 0.5 ~ 0.8 mL Fluohydric acid. while stirring, then at 160 ~ 200 DEG C in a kettle.
React 18 ~ 24 hours;
(4) by the product of step (3) gained, after ultra-pure water and dehydrated alcohol centrifuge washing three times, at 50 DEG C, vacuum is done
Dry, i.e. prepare Cu-TiO2/MoS2;
Described n-butyllithium solution is the hexane solution of n-BuLi, and concentration is 1.6 mol/L;
Described mantoquita is selected from one of following: copper sulfate, copper chloride, copper nitrate, copper acetate, organocopper compound;
Described non-polar solven is selected from one of following: hexane, hexamethylene, carbon tetrachloride, benzene, toluene;
Described water bath sonicator processes, and the process time is 1 hour;
Step b prepares concretely comprising the following steps of electrochemistry nonyl phenol sensor:
(1) with ITO electro-conductive glass as working electrode, at the Cu-TiO of electrode surface drop coating 8 ~ 12 L2/MoS2Colloidal sol, under room temperature
Dry;
(2) the electrode buffer solution PBS that will obtain in step (1), continues at electrode surface drop coating 8 ~ 12 L 10
The nonyl phenol antibody-solutions of g/mL, preserves in 4 DEG C of refrigerators and dries;
(3) the electrode PBS that will obtain in step (2), continuing in electrode surface drop coating 8 ~ 12 L concentration is 100 g/
The bovine serum albumin solution of mL, preserves in 4 DEG C of refrigerators and dries;
(4) the electrode PBS that will obtain in step (3), preserves in 4 DEG C of refrigerators after drying, i.e. prepares electrochemistry nonyl
Base phenol sensor;
Described Cu-TiO2/MoS2Colloidal sol is by the Cu-TiO of 50 mg2/MoS2Powder is dissolved in 10 mL ultra-pure waters, and ultrasonic
The hydrosol prepared after 30 min;
Described PBS is the phosphate buffered solution of 10 mmol/L, and the pH value of described phosphate buffered solution is 7.4.
The application of the electrochemica biological sensor prepared by preparation method the most of the present invention, it is characterised in that include
Following applying step:
A. standard solution preparation: prepare the nonyl phenol standard solution of one group of variable concentrations including blank standard specimen;
B. working electrode is modified: be work by the electrochemica biological sensor prepared by preparation method as claimed in claim 1
Electrode, by the drop coating respectively of the nonyl phenol standard solution of the variable concentrations of preparation in step a to working electrode surface, 4 DEG C of refrigerators
Middle preservation;
C. working curve is drawn: using saturated calomel electrode electrode as reference electrode, platinum electrode is as to electrode, with step b
The working electrode composition three-electrode system modified, connects electrochemical workstation, successively adds 15 mL PBS in a cell
H with 20 L 5 mol/L2O2;By the working electrode of chronoamperometry detection assembling to H2O2Response;Blank standard specimen
Response current is designated asI 0, the response current of the nonyl phenol standard solution containing variable concentrations is denoted asI i, response current reduces
Difference is ΔI = I 0-I i, ΔIMass concentration with nonyl phenol standard solutionCBetween linear, draw ΔI-C
Working curve;
D. the detection of nonyl phenol: replace the nonyl phenol standard solution in step a with testing sample, according to the side in step b and c
Method detects, the difference DELTA reduced according to response electrical signal intensityIAnd working curve, obtain nonyl phenol in testing sample
Content.
The useful achievement of the present invention
(1) electrochemistry nonyl phenol sensor of the present invention preparation is simple, easy to operate, it is achieved that quick, clever to sample
Selective enumeration method quick, high, and low cost, can be applicable to portable inspectiont, has market development prospect;
(2) present invention uses the method for In-situ reaction to be prepared for New Two Dimensional nano-electrode material Cu-TiO first2/MoS2, should
Method mainly has three advantages: one is, due to copper growth in situ on nano titania square fully and titanium dioxide
Nano square contact, utilize the metal surface plasma body effect of copper, be effectively increased semiconductor substrate electron transmission ability and
Catalysis activity, although solving, titanium dioxide nanoplate specific surface area is bigger and mesoporous characteristic is applicable to electrochemistry substrate material
Material, but the technical problem that electro-chemical activity is the highest and current signal is unstable;Two are, due to molybdenum bisuphide lamellar two-dimensional nano
The load characteristic of material and nano titania square thereon fully dispersed, greatly increases electron transmission ability, solves
Determined titanium dioxide nanoplate poorly conductive and current responsing signal weak and be unfavorable for preparing the technical problem of electrochemical sensor;
Three are, due to copper ion the most not only as intercalation material but also as reaction dopant material, finally use In-situ reaction
Method achieves one pot of preparation of this composite, not only saves time, spillage of material, and make the Copper-cladding Aluminum Bar of preparation
Nano titania square can preferably evenly spread to above molybdenum bisuphide lamellar two-dimension nano materials.Therefore, this material
Effective preparation, there is important scientific meaning and using value;
(3) present invention is first by Cu-TiO2/MoS2It is applied in the preparation of electrochemica biological sensor, significantly improves electric current
The strength and stability of signal, substantially increases the detection sensitivity of electrochemical sensor so that electrochemica biological sensor is real
Show the application in real work;The application of this material, is also associated biomolecule sensor, such as Optical Electro-Chemistry sensor, electroluminescent
Chemiluminescence sensors etc. provide Technical Reference, have the most potential use value.
Detailed description of the invention
Embodiment 1 Cu-TiO2/MoS2Preparation
(1) take 0.6 g molybdenum disulfide powder and 0.2 mmol mantoquita joins in 3mL n-butyllithium solution jointly, protect at nitrogen
Protect with at 60 DEG C, stir 12 hours, obtain reacted solution;
(2) utilize reacted solution in non-polar solven washing step (1), at 60 DEG C, then carry out water bath sonicator process,
After having processed, the solution after recycling non-polar solven carrying out washing treatment, vacuum drying, obtain the molybdenum disulfide nano material of copper intercalation
Material;
(3) the molybdenum disulfide nano material taking the copper intercalation that 500 mg steps (2) prepare joins in 5 mL butyl titanates, stirs
After mixing 1 hour, it is slowly added to 0.5 mL Fluohydric acid. while stirring, then reacts 18 hours in a kettle. at 160 DEG C;
(4) by the product of step (3) gained, after ultra-pure water and dehydrated alcohol centrifuge washing three times, at 50 DEG C, vacuum is done
Dry, i.e. prepare Cu-TiO2/MoS2;
Described n-butyllithium solution is the hexane solution of n-BuLi, and concentration is 1.6 mol/L;
Described mantoquita is copper sulfate;
Described non-polar solven is hexane;
Described water bath sonicator processes, and the process time is 1 hour.
Embodiment 2 Cu-TiO2/MoS2Preparation
(1) take 0.6 g molybdenum disulfide powder and 1.0 mmol mantoquitas join in 5 mL n-butyllithium solutions jointly, protect at nitrogen
Protect with at 30 DEG C, stir 24 hours, obtain reacted solution;
(2) utilize reacted solution in non-polar solven washing step (1), at 30 DEG C, then carry out water bath sonicator process,
After having processed, the solution after recycling non-polar solven carrying out washing treatment, vacuum drying, obtain the molybdenum disulfide nano material of copper intercalation
Material;
(3) the molybdenum disulfide nano material taking the copper intercalation that 200 mg steps (2) prepare joins in 5 mL butyl titanates, stirs
After mixing 1 hour, it is slowly added to 0.6 mL Fluohydric acid. while stirring, then reacts 20 hours in a kettle. at 180 DEG C;
(4) by the product of step (3) gained, after ultra-pure water and dehydrated alcohol centrifuge washing three times, at 50 DEG C, vacuum is done
Dry, i.e. prepare Cu-TiO2/MoS2;
Described n-butyllithium solution is the hexane solution of n-BuLi, and concentration is 1.6 mol/L;
Described mantoquita is copper chloride;
Described non-polar solven is carbon tetrachloride;
Described water bath sonicator processes, and the process time is 1 hour.
Embodiment 3 Cu-TiO2/MoS2Preparation
(1) take 0.6 g molybdenum disulfide powder and 2.0 mmol mantoquitas join in 10 mL n-butyllithium solutions, at nitrogen jointly
Protection, with at 50 DEG C, is stirred 48 hours, is obtained reacted solution;
(2) utilize reacted solution in non-polar solven washing step (1), at 50 DEG C, then carry out water bath sonicator process,
After having processed, the solution after recycling non-polar solven carrying out washing treatment, vacuum drying, obtain the molybdenum disulfide nano material of copper intercalation
Material;
(3) the molybdenum disulfide nano material taking the copper intercalation that 10 mg steps (2) prepare joins in 5 mL butyl titanates, stirs
After mixing 1 hour, it is slowly added to 0.8 mL Fluohydric acid. while stirring, then reacts 24 hours in a kettle. at 200 DEG C;
(4) by the product of step (3) gained, after ultra-pure water and dehydrated alcohol centrifuge washing three times, at 50 DEG C, vacuum is done
Dry, i.e. prepare Cu-TiO2/MoS2;
Described n-butyllithium solution is the hexane solution of n-BuLi, and concentration is 1.6 mol/L;
Described mantoquita is copper acetate;
Described non-polar solven is benzene;
Described water bath sonicator processes, and the process time is 1 hour.
The preparation method of embodiment 4 electrochemistry nonyl phenol sensor
(1) with ITO electro-conductive glass as working electrode, at the Cu-TiO of electrode surface drop coating 8 L2/MoS2Colloidal sol, dries in the air under room temperature
Dry;
(2) the electrode buffer solution PBS that will obtain in step (1), continues at electrode surface drop coating 8 L 10 g/mL
Nonyl phenol antibody-solutions, 4 DEG C of refrigerators preserve and dry;
(3) the electrode PBS that will obtain in step (2), continuing in electrode surface drop coating 8 L concentration is 100 g/mL
Bovine serum albumin solution, 4 DEG C of refrigerators preserve and dry;
(4) the electrode PBS that will obtain in step (3), preserves in 4 DEG C of refrigerators after drying, i.e. prepares electrochemistry nonyl
Base phenol sensor;
Described Cu-TiO2/MoS2Colloidal sol is by the Cu-TiO of 50 mg2/MoS2Powder is dissolved in 10 mL ultra-pure waters, and ultrasonic
The hydrosol prepared after 30 min;
Described PBS is the phosphate buffered solution of 10mmol/L, and the pH value of described phosphate buffered solution is 7.4.
The preparation method of embodiment 5 electrochemistry nonyl phenol sensor
(1) with ITO electro-conductive glass as working electrode, at the Cu-TiO of electrode surface drop coating 10 L2/MoS2Colloidal sol, dries in the air under room temperature
Dry;
(2) the electrode buffer solution PBS that will obtain in step (1), continues at electrode surface drop coating 10 L 10 g/
The nonyl phenol antibody-solutions of mL, preserves in 4 DEG C of refrigerators and dries;
(3) the electrode PBS that will obtain in step (2), continuing in electrode surface drop coating 10 L concentration is 100 g/mL
Bovine serum albumin solution, 4 DEG C of refrigerators preserve and dry;
(4) the electrode PBS that will obtain in step (3), preserves in 4 DEG C of refrigerators after drying, i.e. prepares electrochemistry nonyl
Base phenol sensor;
Described Cu-TiO2/MoS2Colloidal sol is by the Cu-TiO of 50 mg2/MoS2Powder is dissolved in 10 mL ultra-pure waters, and ultrasonic
The hydrosol prepared after 30 min;
Described PBS is the phosphate buffered solution of 10 mmol/L, and the pH value of described phosphate buffered solution is 7.4.
The preparation method of embodiment 6 electrochemistry nonyl phenol sensor
(1) with ITO electro-conductive glass as working electrode, at the Cu-TiO of electrode surface drop coating 12 L2/MoS2Colloidal sol, dries in the air under room temperature
Dry;
(2) the electrode buffer solution PBS that will obtain in step (1), continues at electrode surface drop coating 12 L 10 g/
The nonyl phenol antibody-solutions of mL, preserves in 4 DEG C of refrigerators and dries;
(3) the electrode PBS that will obtain in step (2), continuing in electrode surface drop coating 12 L concentration is 100 g/mL
Bovine serum albumin solution, 4 DEG C of refrigerators preserve and dry;
(4) the electrode PBS that will obtain in step (3), preserves in 4 DEG C of refrigerators after drying, i.e. prepares electrochemistry nonyl
Base phenol sensor;
Described Cu-TiO2/g-C3N4Colloidal sol is by the Cu-TiO of 50 mg2/g-C3N4Powder is dissolved in 10 mL ultra-pure waters, and
The hydrosol prepared after ultrasonic 30 min;
Described PBS is the phosphate buffered solution of 10 mmol/L, and the pH value of described phosphate buffered solution is 7.4.
The electrochemistry nonyl phenol sensor of embodiment 7 embodiment 1 ~ 6 preparation, is applied to the detection of nonyl phenol, and step is such as
Under:
(1) standard solution preparation: prepare the nonyl phenol standard solution of one group of variable concentrations including blank standard specimen;
(2) working electrode is modified: be work by the electrochemistry nonyl phenol sensor prepared by preparation method as claimed in claim 1
Make electrode, by the drop coating respectively of the nonyl phenol standard solution of the variable concentrations of preparation in step (1) to working electrode surface, 4 DEG C
Refrigerator preserves;
(3) working curve is drawn: using saturated calomel electrode electrode as reference electrode, platinum electrode is as to electrode, with step b
The working electrode composition three-electrode system modified, connects electrochemical workstation, successively adds 15 mL PBS in a cell
H with 20 L 5 mol/L2O2;By the working electrode of chronoamperometry detection assembling to H2O2Response;Blank standard specimen
Response current is designated asI 0, the response current of the nonyl phenol standard solution containing variable concentrations is denoted asI i, the difference of response current reduction
Value is ΔI = I 0-I i, ΔIMass concentration with nonyl phenol standard solutionCBetween linear, draw ΔI-C
Working curve;The linear detection range of nonyl phenol is: 0.009 ~ 200 ng/mL, and detection is limited to: 3.0 pg/mL;
(4) detection of nonyl phenol: replace the nonyl phenol standard solution in step (1) with testing sample, according to step (2) and (3)
In method detect, according to response electrical signal intensity reduce difference DELTAIAnd working curve, obtain nonyl in testing sample
The content of base phenol.
Claims (4)
1. a preparation method for electrochemistry nonyl phenol sensor based on titania-doped/molybdenum bisuphide composite, its
It is characterised by that described electrochemistry nonyl phenol sensor is by working electrode, titania-doped/molybdenum bisuphide composite, nonyl
Phenol antibody, bovine serum albumin form;Described titania-doped/molybdenum bisuphide composite is that copper-doped titanium dioxide is received
The two-dimensional nano composite Cu-TiO of rice square In-situ reaction molybdenum bisuphide2/MoS2。
2. electrochemistry nonyl phenol sensor based on titania-doped/molybdenum bisuphide composite as claimed in claim 1
Preparation method, it is characterised in that described preparation method includes following two preparation process:
A. Cu-TiO is prepared2/MoS2;
B. electrochemistry nonyl phenol sensor is prepared.
3. electrochemistry nonyl phenol based on the titania-doped/molybdenum bisuphide composite sensing as described in claim 1 and 2
The preparation method of device, it is characterised in that described Cu-TiO2/MoS2Concrete preparation process be:
(1) take 0.6 g molybdenum disulfide powder and 0.2 ~ 2.0 mmol mantoquita joins 3 ~ 10 mL n-butyllithium solutions jointly
In, at nitrogen protection and 30 ~ 60 DEG C, stir 12 ~ 48 hours, obtain reacted solution;
(2) utilize reacted solution in non-polar solven washing step (1), at 30 ~ 60 DEG C, then carry out water bath sonicator
Process, after having processed, the solution after recycling non-polar solven carrying out washing treatment, vacuum drying, obtain the molybdenum bisuphide of copper intercalation
Nano material;
(3) the molybdenum disulfide nano material taking the copper intercalation that 10 ~ 500 mg steps (2) prepare joins 5 mL butyl titanates
In, after stirring 1 hour, it is slowly added to 0.5 ~ 0.8 mL Fluohydric acid. while stirring, then at 160 ~ 200 DEG C in a kettle.
React 18 ~ 24 hours;
(4) by the product of step (3) gained, after ultra-pure water and dehydrated alcohol centrifuge washing three times, at 50 DEG C, vacuum is done
Dry, i.e. prepare Cu-TiO2/MoS2;
Described n-butyllithium solution is the hexane solution of n-BuLi, and concentration is 1.6 mol/L;
Described mantoquita is selected from one of following: copper sulfate, copper chloride, copper nitrate, copper acetate, organocopper compound;
Described non-polar solven is selected from one of following: hexane, hexamethylene, carbon tetrachloride, benzene, toluene;
Described water bath sonicator processes, and the process time is 1 hour.
4. electrochemistry nonyl phenol based on the titania-doped/molybdenum bisuphide composite sensing as described in claim 1 and 2
The preparation method of device, it is characterised in that the concrete preparation process of described electrochemistry nonyl phenol sensor is:
(1) with glass-carbon electrode as working electrode, at the Cu-TiO of electrode surface drop coating 8 ~ 12 L2/MoS2Colloidal sol, dries in the air under room temperature
Dry;
(2) the electrode buffer solution PBS that will obtain in step (1), continues at electrode surface drop coating 8 ~ 12 L 10
The nonyl phenol antibody-solutions of g/mL, preserves in 4 DEG C of refrigerators and dries;
(3) the electrode PBS that will obtain in step (2), continuing in electrode surface drop coating 8 ~ 12 L concentration is 100 g/
The bovine serum albumin solution of mL, preserves in 4 DEG C of refrigerators and dries;
(4) the electrode PBS that will obtain in step (3), preserves in 4 DEG C of refrigerators after drying, i.e. prepares electrochemistry nonyl
Base phenol sensor;
Described Cu-TiO2/MoS2Colloidal sol is by the Cu-TiO of 50 mg2/MoS2Powder is dissolved in 10 mL ultra-pure waters, and ultrasonic
The hydrosol prepared after 30 min;
Described PBS is the phosphate buffered solution of 10 mmol/L, and the pH value of described phosphate buffered solution is 7.4.
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CN106892458A (en) * | 2017-02-05 | 2017-06-27 | 桂林理工大学 | A kind of two-dimentional MoS2The preparation method of PbS nano particle composite materials |
CN110323424A (en) * | 2019-05-29 | 2019-10-11 | 景德镇陶瓷大学 | The preparation method of titania modified molybdenum disulfide lithium ion battery negative material |
CN111697083A (en) * | 2020-06-04 | 2020-09-22 | 青海盐湖工业股份有限公司 | Device for realizing PN junction effect based on brine environment |
TWI715019B (en) * | 2019-04-11 | 2021-01-01 | 大陸商業成科技(成都)有限公司 | Nano composite material, method for making same, and package structure |
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