CN110183850A - Copper oxide/poly-dopamine/redox graphene CuO/PDA/rGO preparation method - Google Patents
Copper oxide/poly-dopamine/redox graphene CuO/PDA/rGO preparation method Download PDFInfo
- Publication number
- CN110183850A CN110183850A CN201910467924.5A CN201910467924A CN110183850A CN 110183850 A CN110183850 A CN 110183850A CN 201910467924 A CN201910467924 A CN 201910467924A CN 110183850 A CN110183850 A CN 110183850A
- Authority
- CN
- China
- Prior art keywords
- pda
- rgo
- cuo
- ultrasonic
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/0666—Polycondensates containing five-membered rings, condensed with other rings, with nitrogen atoms as the only ring hetero atoms
- C08G73/0672—Polycondensates containing five-membered rings, condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only one nitrogen atom in the ring
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2248—Oxides; Hydroxides of metals of copper
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Physics & Mathematics (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to the preparation methods of copper oxide/poly-dopamine/redox graphene CuO/PDA/rGO a kind of, firstly, being raw material by reducing agent, graphene oxide of DA, using sonochemical method, regulate and control the process conditions such as ratio and the reaction time of raw material, prepares the good rGO/PDA of electric conductivity;Using the rGO/PDA as conducting base, one-step method is respectively adopted and two-step method has developed two kinds of preparation methods for preparing CuO/rGO/PDA;Wherein, after two-step method refers to rGO/PDA cleaning and freeze-drying by above-mentioned preparation, after mixing with a certain proportion of mantoquita presoma, by regulating and controlling ultrasonic technique condition, CuO/PDA/rGO is prepared;Wherein, one-step method refers to mantoquita precursor solution is directly mixed with the reaction solution of rGO/PDA after, control ultrasonic technique condition, the method for preparing CuO/PDA/rGO.
Description
Technical field
The invention belongs to sonochemistry fields, are related to a kind of copper oxide/poly-dopamine/redox graphene CuO/PDA/
The preparation method of rGO.
Background technique
Dai etc. has developed a kind of pervasive method and has prepared a series of metal hydroxides or oxide and graphene composite wood
Material.Metal ion, which is added in graphene oxide solution, is adsorbed on it in conjunction with the oxygen-containing functional group of surface of graphene oxide
Graphene surface.Metal ion can be nucleated in these adsorption sites, grow, hydrolysis obtains hydroxide or oxide.
Copper oxide is a kind of p-type semiconductor, has relatively broad application in electro-catalysis field.The CuO electricity of nanostructure
Pole material has high specific area and short ion diffusion length, can preferably contact with glucose molecule and charge passes
It passs, and then effectively improves the electro catalytic activity of electrode material.And drawback of the CuO as the conductive difference of metal oxide,
Cause its electric sensing sensitivity insufficient., can be compound by the high nano-carbon material of electric conductivity and CuO for the electric conductivity for improving CuO, system
The nanocomposite of standby CuO and nano-carbon material with very significant high electrochemical performance.Research finds that carbon substrate is made
Be conducive to increase the mechanical stability of the electric conductivity and material between CuO particle for conducting matrix grain, composite material is put in high current
Excellent chemical property is shown in electricity.
Summary of the invention
Technical problems to be solved
In order to avoid the shortcomings of the prior art, the present invention proposes a kind of copper oxide/poly-dopamine/reduction-oxidation graphite
The preparation method of alkene CuO/PDA/rGO.
Technical solution
A kind of sonochemistry two-step method prepares the side copper oxide/poly-dopamine/redox graphene CuO/PDA/rGO
Method, it is characterised in that steps are as follows:
Step 1: it is 8-9's that the HCl solution of the Tris solution of the 0.1M of 50ml, the 0.1M of 14.7ml, which is mixed and made into pH,
Tris-HCl buffer solution 100ml;
Step 2: by the DA of GO solution and 10mg that the concentration of the Tris-HCl buffer solution of 60ml, 2-8ml are 5mg/ml
Powder mixes ice-water bath ultrasound 10min;Supersonic frequency is used to carry out plug-in type reaction, ultrasonic function for the ultrasonic amplitude transformer of 20kHz
Rate is 150W~225W;Using continual ultrasonic and continue aeration by the way of reacted, after 0.5~1h of total sonication time
Centrifugal treating under 8000-12000r/s revolving speed, after cleaning multipass, freeze-drying is no more than for 24 hours, obtains rGO/PDA;
Step 3: the rGO/PDA of 10-40mg is mixed with the copper acetate precursor solution of the 0.01mol/L concentration of 50ml,
The ultrasonic amplitude transformer that supersonic frequency is 20kHz is subjected to plug-in type reaction, ultrasonic power is 150W~225W;Using continual ultrasonic
Mode is reacted, and total sonication time 0.5-1h prepares the composite material of CuO/rGO/PDA, is finally 9000r/s in revolving speed
Under the conditions of centrifugal treating, after cleaning multipass, up to CuO/rGO/PDA nanocomposite after freeze-drying for 24 hours;
Each amount of material is counted by every part in above-mentioned reaction.
A kind of one kettle way sonochemical method prepares the side copper oxide/poly-dopamine/redox graphene CuO/rGO/PDA
Method, it is characterised in that steps are as follows:
Step 1): by the Tris solution of the 0.1M of 50ml, the HCl solution of the 0.1M of 14.7ml and 3.2-8mg hydrochloric acid DOPA
Amine DA is mixed and made into the DA buffer solution for the Tris-HCl that pH is 8-9, and wherein the concentration of DA is 32-80mg/L;
Step 2): the DA buffer solution of Tris-HCl is mixed with GO powder, and supersonic frequency is used to become for the ultrasound of 20kHz
Width bar carries out plug-in type reaction, and ultrasonic power is 150W~225W, using continual ultrasonic and continues to be reacted by the way of aeration,
Accumulative ultrasound 0.5-1h, obtains rGO/PDA solution;The mass ratio of the GO and DA is 1:1~1:4;
Step 3): by the copper acetate precursor solution of the 0.02mol/L concentration of 25ml, the rGO/PDA prepared with 25ml
Solution mixing uses supersonic frequency to carry out plug-in type reaction for the ultrasonic amplitude transformer of 20kHz, and ultrasonic power is 150W~225W,
It is reacted using continual ultrasonic, total sonication time 0.5-1h prepares the composite material of CuO/rGO/PDA, finally exists
Centrifugal treating under 9000r/s is dried overnight in 333K vacuum tank;
Each amount of material is counted by every part in above-mentioned reaction.
Beneficial effect
The preparation method of copper oxide/poly-dopamine/redox graphene CuO/PDA/rGO proposed by the present invention a kind of,
By the high energy of sonochemical method, green, it is mild in the way of, realize the height of two kinds of composite materials of CuO/rGO and CuO/PDA/rGO
Effect preparation.First choice, using its surface GO, a large amount of Cu is adsorbed in oxygen-containing group abundant2+Ion presoma, it is sonicating by controlling
Process conditions are learned, growth in situ goes out the CuO/GO composite material of different-shape: second, select dopamine as adhesive to rGO
Be surface modified, sonochemistry effect under in-situ polymerization and restore GO process formed rGO/PDA, enhance the conduction of GO
Property, while Cu ion is effectively adsorbed on the NH of PDA2Equal groups remove, and it is multiple to realize sonochemistry one kettle way preparation CuO/PDA/rGO
Condensation material.Good interface performance between oxide and nano-sized carbon matrix is glucose sensor, solar battery, biology combustion
Good material foundation is established in the fields such as material battery.Graphene and carbon nanotube.It ensure that its integrity and stability.
The GO that the present invention selects Hummers to prepare is carbon material matrix, and graphene oxide (Graphene) is one kind by carbon
The new material of the individual layer laminated structure of atomic building, it is high-modulus, high intensity possessed by this material, good thermal conductivity, excellent
The performances such as the different specific surface area of carrier mobility and super large make it in electronic device, sensor, energy storage device and answer
The fields such as condensation material illustrate wide application prospect.The amino of poly-dopamine in nano-carbon material by modification simultaneously
Be connected with chemical bonds with CuO, can Reinforced Cu O/rGO Interface adhesive strength.
The present invention program is related to a kind of sonochemistry preparation based on oxide/redox graphene composite material
Two methods;The method for preparing the composite material of CuO/PDA/rGO has the characteristics that cheap, Compound Degree is high.CuO/
There is the composite material of PDA/rGO significant catalytic and electric conductivity can be used for enzyme-free glucose detection.
Detailed description of the invention
Fig. 1: rGO/PDA preparation flow figure
Fig. 2: sonochemical method prepares CuO/PDA/rGO
Fig. 3:CuO/PDA/rGO/GECThe mechanism schematic diagram of electrode direct electrochemistry oxidizing glucose
Specific embodiment
Now in conjunction with embodiment, attached drawing, the invention will be further described:
Embodiment 1:
A) it Tris-HCl buffer: takes 50ml 0.1mol/L Tris solution in 100ml volumetric flask, adds
14.7ml0.1mol/L mixed in hydrochloric acid is uniform, and water is added and is diluted to 100ml, is uniformly mixed;
B) rGO/PDA: taking the Tris-HCl buffer of 60ml in round-bottomed flask, and the GO solution that 8ml 5mg/ml is added [is criticized
10mg Dopamine hydrochloride powder is added in secondary 1] (40mg), ice-water bath ultrasound 10min, then ice-water bath ultrasound 10min passes through choosing
It is that the ultrasonic amplitude transformer that 20kHz rated power is 750W carries out plug-in type reaction, ultrasonic power 225W with supersonic frequency.Using
The mode of continual ultrasonic and intermittent aerating is reacted respectively, adds up ultrasound 0.5h, then in 12000r/s revolving speed centrifuge washing,
With ethanol washing 2 times, it is washed with deionized 1 time.Freeze-drying is no more than for 24 hours, takes out and grinds to obtain rGO/PDA powder;
C) CuO/PDA/rGO: the Cu of 0.01mol/L is configured2+Precursor solution, by the rGO/PDA prepared by the ratio of 1:1
Example is added in precursor solution, is then that the ultrasonic amplitude transformer that 20kHz rated power is 750W carries out by selecting supersonic frequency
Plug-in type reaction, ultrasonic power 225W.It is reacted using continual ultrasonic, adds up ultrasound 0.5h, prepare CuO/PDA/rGO
Composite material
D) it post-processes: product is separated, change liquid separation twice with dehydrated alcohol and ultrapure water centrifugation respectively.Freeze-day with constant temperature
Case, 60 DEG C of vacuum drying 12h.
E) prepared by CuO/PDA/rGO/GCE: dispersing 5mg CuO/PDA/rGO powder ultrasonic in 1ml ethanol solution, surpasses
Sound disperses 10min, obtains black even dispersion liquid, which is applied to the surface pretreated glass-carbon electrode (GCE), electricity
Pole 2.5 μ L Nafion (0.5wt% ethyl alcohol) of drop coating again after natural drying, obtains CuO/PDA/rGO/GCE modified electrode.
F) CuO/PDA/rGO/GCE catalytic performance is studied: electro-chemical test carries out at room temperature in three-electrode system, CuO/
PDA/rGO/GCE is working electrode, and saturated calomel electrode (SCE) is reference electrode, and platinum electrode (Pt) is auxiliary electrode.It prepares
The electrochemical glucose sensor of CuO/PDA/rGO/GCE modified electrode.
Embodiment 2:
A) it Tris-HCl buffer: takes 50ml 0.1mol/L Tris solution in 100ml volumetric flask, adds
14.7ml0.1mol/L mixed in hydrochloric acid is uniform, and water is added and is diluted to 100ml, is uniformly mixed;
B) rGO/PDA: taking the Tris-HCl buffer of 60ml in round-bottomed flask, and the GO solution that 6ml 5mg/ml is added [is criticized
10mg Dopamine hydrochloride powder is added in secondary 1] (30mg), ice-water bath ultrasound 10min, then ice-water bath ultrasound 10min passes through choosing
It is that the ultrasonic amplitude transformer that 20kHz rated power is 750W carries out plug-in type reaction, ultrasonic power 225W with supersonic frequency.Using
The mode of continual ultrasonic and intermittent aerating is reacted respectively, adds up ultrasound 0.5h, then in 12000r/s revolving speed centrifuge washing,
With ethanol washing 2 times, it is washed with deionized 1 time.Freeze-drying is no more than for 24 hours, takes out and grinds to obtain rGO/PDA powder;
C) CuO/PDA/rGO: the Cu of 0.01mol/L is configured2+Precursor solution is added in the ratio of 1:1 in precursor solution
In, it is then that the ultrasonic amplitude transformer that 20kHz rated power is 750W carries out plug-in type reaction, ultrasonic function by selecting supersonic frequency
Rate is 225W.It is reacted using continual ultrasonic, adds up ultrasound 0.5h, prepare the composite material of CuO/PDA/rGO
D) it post-processes: product is separated, change liquid separation twice with dehydrated alcohol and ultrapure water centrifugation respectively.Freeze-day with constant temperature
Case, 60 DEG C of vacuum drying 12h.
E) prepared by CuO/PDA/rGO/GCE: dispersing 5mg CuO/PDA/rGO powder ultrasonic in 1ml ethanol solution, surpasses
Sound disperses 10min, obtains black even dispersion liquid, which is applied to the surface pretreated glass-carbon electrode (GCE), electricity
Pole 2.5 μ L Nafion (0.5wt% ethyl alcohol) of drop coating again after natural drying, obtains CuO/PDA/rGO/GCE modified electrode.
F) CuO/PDA/rGO/GCE catalytic performance is studied: electro-chemical test carries out at room temperature in three-electrode system, CuO/
PDA/rGO/GCE is working electrode, and saturated calomel electrode (SCE) is reference electrode, and platinum electrode (Pt) is auxiliary electrode.It prepares
The electrochemical glucose sensor of CuO/PDA/rGO/GCE modified electrode.
Embodiment 3:
A) it Tris-HCl buffer: takes 50ml 0.1mol/L Tris solution in 100ml volumetric flask, adds
14.7ml0.1mol/L mixed in hydrochloric acid is uniform, and water is added and is diluted to 100ml, is uniformly mixed;
B) rGO/PDA: taking the Tris-HCl buffer of 60ml in round-bottomed flask, and the GO solution that 4ml 5mg/ml is added [is criticized
10mg Dopamine hydrochloride powder is added in secondary 1] (20mg), ice-water bath ultrasound 10min, then ice-water bath ultrasound 10min passes through choosing
It is that the ultrasonic amplitude transformer that 20kHz rated power is 750W carries out plug-in type reaction, ultrasonic power 225W with supersonic frequency.Using
The mode of continual ultrasonic and intermittent aerating is reacted respectively, adds up ultrasound 0.5h, then in 12000r/s revolving speed centrifuge washing,
With ethanol washing 2 times, it is washed with deionized 1 time.Freeze-drying is no more than for 24 hours, takes out and grinds to obtain rGO/PDA powder;
C) CuO/PDA/rGO: the Cu of 0.01mol/L is configured2+Precursor solution is added in the ratio of 1:1 in precursor solution
In, it is then that the ultrasonic amplitude transformer that 20kHz rated power is 750W carries out plug-in type reaction, ultrasonic function by selecting supersonic frequency
Rate is 225W.It is reacted using continual ultrasonic, adds up ultrasound 0.5h, prepare the composite material of CuO/PDA/rGO
D) it post-processes: product is separated, change liquid separation twice with dehydrated alcohol and ultrapure water centrifugation respectively.Freeze-day with constant temperature
Case, 60 DEG C of vacuum drying 12h.
E) prepared by CuO/PDA/rGO/GCE: dispersing 5mg CuO/PDA/rGO powder ultrasonic in 1ml ethanol solution, surpasses
Sound disperses 10min, obtains black even dispersion liquid, which is applied to the surface pretreated glass-carbon electrode (GCE), electricity
Pole 2.5 μ L Nafion (0.5wt% ethyl alcohol) of drop coating again after natural drying, obtains CuO/PDA/rGO/GCE modified electrode.
F) CuO/PDA/rGO/GCE catalytic performance is studied: electro-chemical test carries out at room temperature in three-electrode system, CuO/
PDA/rGO/GCE is working electrode, and saturated calomel electrode (SCE) is reference electrode, and platinum electrode (Pt) is auxiliary electrode.It prepares
The electrochemical glucose sensor of CuO/PDA/rGO/GCE modified electrode.
Example 4:
A) it Tris-HCl buffer: takes 50ml 0.1mol/L Tris solution in 100ml volumetric flask, adds
14.7ml0.1mol/L mixed in hydrochloric acid is uniform, and water is added and is diluted to 100ml, is uniformly mixed;
B) rGO/PDA: weighing the Dopamine hydrochloride of 3.2mg, is put into the Tris-HCl buffer of 100ml, stirs evenly,
The mixed solution for taking out 25ml, is added the GO powder of 12.8mg, is uniformly mixing to obtain dispersion liquid.Then by selecting supersonic frequency
The ultrasonic amplitude transformer for being 750W for 20kHz rated power carries out plug-in type reaction, ultrasonic power 225W.Using continual ultrasonic into
Row reaction, adds up ultrasound 0.5h, obtains the solution of rGO/PDA;
C) CuO/PDA/rGO: the Cu of 0.02mol/L is configured2+Precursor solution 25ml, by it with 25ml's prepared above
The mixing of rGO/PDA dispersion liquid, and pH=8.5 is adjusted with ammonium hydroxide, it stirs evenly, is then 20kHz volume by selecting supersonic frequency
Determine the ultrasonic amplitude transformer that power is 750W and carries out plug-in type reaction, ultrasonic power 225W.It is reacted, is tired out using continual ultrasonic
Ultrasound 0.5h is counted, the composite material of CuO/PDA/rGO is prepared
D) it post-processes: product is separated, change liquid separation twice with dehydrated alcohol and ultrapure water centrifugation respectively.Freeze-day with constant temperature
Case, 60 DEG C of vacuum drying 12h.
E) prepared by CuO/PDA/rGO/GCE: dispersing 5mg CuO/PDA/rGO powder ultrasonic in 1ml ethanol solution, surpasses
Sound disperses 10min, obtains black even dispersion liquid, which is applied to the surface pretreated glass-carbon electrode (GCE), electricity
Pole 2.5 μ L Nafion (0.5wt% ethyl alcohol) of drop coating again after natural drying, obtains CuO/PDA/rGO/GCE modified electrode.
F) CuO/PDA/rGO/GCE catalytic performance is studied: electro-chemical test carries out at room temperature in three-electrode system, CuO/
PDA/rGO/GCE is working electrode, and saturated calomel electrode (SCE) is reference electrode, and platinum electrode (Pt) is auxiliary electrode.It prepares
The electrochemical glucose sensor of CuO/PDA/rGO/GCE modified electrode.
Example 5:
A) it Tris-HCl buffer: takes 50ml 0.1mol/L Tris solution in 100ml volumetric flask, adds
14.7ml0.1mol/L mixed in hydrochloric acid is uniform, and water is added and is diluted to 100ml, is uniformly mixed;
B) rGO/PDA: weighing the Dopamine hydrochloride of 3.2mg, is put into the Tris-HCl buffer of 100ml, stirs evenly,
The mixed solution for taking out 25ml, is added the GO powder of 12.8mg, is uniformly mixing to obtain dispersion liquid.Then by selecting supersonic frequency
The ultrasonic amplitude transformer for being 750W for 20kHz rated power carries out plug-in type reaction, ultrasonic power 225W.Using continual ultrasonic into
Row reaction, adds up ultrasound 0.5h, obtains the solution of rGO/PDA;
C) CuO/PDA/rGO: the Cu of 0.02mol/L is configured2+Precursor solution 25ml, by it with 25ml's prepared above
The mixing of rGO/PDA dispersion liquid, and pH=7.0 is adjusted with ammonium hydroxide, it stirs evenly, is then 20kHz volume by selecting supersonic frequency
Determine the ultrasonic amplitude transformer that power is 750W and carries out plug-in type reaction, ultrasonic power 225W.It is reacted, is tired out using continual ultrasonic
Ultrasound 0.5h is counted, the composite material of CuO/PDA/rGO is prepared
D) it post-processes: product is separated, change liquid separation twice with dehydrated alcohol and ultrapure water centrifugation respectively.Freeze-day with constant temperature
Case, 60 DEG C of vacuum drying 12h.
E) prepared by CuO/PDA/rGO/GCE: dispersing 5mg CuO/PDA/rGO powder ultrasonic in 1ml ethanol solution, surpasses
Sound disperses 10min, obtains black even dispersion liquid, which is applied to the surface pretreated glass-carbon electrode (GCE), electricity
Pole 2.5 μ L Nafion (0.5wt% ethyl alcohol) of drop coating again after natural drying, obtains CuO/PDA/rGO/GCE modified electrode.
F) CuO/PDA/rGO/GCE catalytic performance is studied: electro-chemical test carries out at room temperature in three-electrode system, CuO/
PDA/rGO/GCE is working electrode, and saturated calomel electrode (SCE) is reference electrode, and platinum electrode (Pt) is auxiliary electrode.It prepares
The electrochemical glucose sensor of CuO/PDA/rGO/GCE modified electrode.
Example 6:
A) it Tris-HCl buffer: takes 50ml 0.1mol/L Tris solution in 100ml volumetric flask, adds
14.7ml0.1mol/L mixed in hydrochloric acid is uniform, and water is added and is diluted to 100ml, is uniformly mixed;
B) rGO/PDA: weighing the Dopamine hydrochloride of 3.2mg, is put into the Tris-HCl buffer of 100ml, stirs evenly,
The mixed solution for taking out 25ml, is added the GO powder of 6.4mg, is uniformly mixing to obtain dispersion liquid.Then by selecting supersonic frequency
The ultrasonic amplitude transformer for being 750W for 20kHz rated power carries out plug-in type reaction, ultrasonic power 225W.Using continual ultrasonic into
Row reaction, adds up ultrasound 0.5h, obtains the solution of rGO/PDA;
C) CuO/PDA/rGO: the Cu of 0.02mol/L is configured2+Precursor solution 25ml, by it with 25ml's prepared above
The mixing of rGO/PDA dispersion liquid, and pH=8.5 is adjusted with ammonium hydroxide, it stirs evenly, is then 20kHz volume by selecting supersonic frequency
Determine the ultrasonic amplitude transformer that power is 750W and carries out plug-in type reaction, ultrasonic power 225W.It is reacted, is tired out using continual ultrasonic
Ultrasound 0.5h is counted, the composite material of CuO/PDA/rGO is prepared
D) it post-processes: product is separated, change liquid separation twice with dehydrated alcohol and ultrapure water centrifugation respectively.Freeze-day with constant temperature
Case, 60 DEG C of vacuum drying 12h.
E) prepared by CuO/PDA/rGO/GCE: dispersing 5mg CuO/PDA/rGO powder ultrasonic in 1ml ethanol solution, surpasses
Sound disperses 10min, obtains black even dispersion liquid, which is applied to the surface pretreated glass-carbon electrode (GCE), electricity
Pole 2.5 μ L Nafion (0.5wt% ethyl alcohol) of drop coating again after natural drying, obtains CuO/PDA/rGO/GCE modified electrode.
The research of CuO/PDA/rGO/GCE catalytic performance: electro-chemical test carries out at room temperature in three-electrode system, CuO/
PDA/rGO/GCE is working electrode, and saturated calomel electrode (SCE) is reference electrode, and platinum electrode (Pt) is auxiliary electrode.It prepares
The electrochemical glucose sensor of CuO/PDA/rGO/GCE modified electrode.
Claims (2)
1. a kind of sonochemistry two-step method prepares copper oxide/poly-dopamine/redox graphene CuO/PDA/rGO method,
It is characterized by the following steps:
Step 1: the HCl solution of the Tris solution of the 0.1M of 50ml, the 0.1M of 14.7ml is mixed and made into the Tris- that pH is 8-9
HCl buffer solution 100ml;
Step 2: by the concentration of the Tris-HCl buffer solution of 60ml, 2-8ml be 5mg/ml GO solution and 10mg DA powder,
Mix ice-water bath ultrasound 10min;Supersonic frequency is used to carry out plug-in type reaction for the ultrasonic amplitude transformer of 20kHz, ultrasonic power is
150W~225W;Using continual ultrasonic and continue to be reacted by the way of aeration, in 8000- after 0.5~1h of total sonication time
Centrifugal treating under 12000r/s revolving speed, after cleaning multipass, freeze-drying is no more than for 24 hours, obtains rGO/PDA;
Step 3: the rGO/PDA of 10-40mg being mixed with the copper acetate precursor solution of the 0.01mol/L concentration of 50ml, will be surpassed
The ultrasonic amplitude transformer that acoustic frequency is 20kHz carries out plug-in type reaction, and ultrasonic power is 150W~225W;Using continual ultrasonic mode
It is reacted, total sonication time 0.5-1h prepares the composite material of CuO/rGO/PDA, is finally 9000r/s condition in revolving speed
Lower centrifugal treating, after cleaning multipass, up to CuO/rGO/PDA nanocomposite after freeze-drying for 24 hours;
Each amount of material is counted by every part in above-mentioned reaction.
2. a kind of one kettle way sonochemical method prepares the side copper oxide/poly-dopamine/redox graphene CuO/rGO/PDA
Method, it is characterised in that steps are as follows:
Step 1): by the Tris solution of the 0.1M of 50ml, the HCl solution of the 0.1M of 14.7ml and 3.2-8mg Dopamine hydrochloride DA
It is mixed and made into the DA buffer solution for the Tris-HCl that pH is 8-9, wherein the concentration of DA is 32-80mg/L;
Step 2): the DA buffer solution of Tris-HCl is mixed with GO powder, uses supersonic frequency for the ultrasonic amplitude transformer of 20kHz
Plug-in type reaction is carried out, ultrasonic power is 150W~225W, using continual ultrasonic and continues to be reacted by the way of aeration, add up
Ultrasonic 0.5-1h obtains rGO/PDA solution;The mass ratio of the GO and DA is 1:1~1:4;
Step 3): by the copper acetate precursor solution of the 0.02mol/L concentration of 25ml, the rGO/PDA solution that is prepared with 25ml
Mixing uses supersonic frequency to carry out plug-in type reaction for the ultrasonic amplitude transformer of 20kHz, and ultrasonic power is 150W~225W, uses
Continual ultrasonic is reacted, and total sonication time 0.5-1h prepares the composite material of CuO/rGO/PDA, finally at 9000r/s
Centrifugal treating is dried overnight in 333K vacuum tank;
Each amount of material is counted by every part in above-mentioned reaction.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201910467924.5A CN110183850A (en) | 2019-05-31 | 2019-05-31 | Copper oxide/poly-dopamine/redox graphene CuO/PDA/rGO preparation method |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201910467924.5A CN110183850A (en) | 2019-05-31 | 2019-05-31 | Copper oxide/poly-dopamine/redox graphene CuO/PDA/rGO preparation method |
Publications (1)
Publication Number | Publication Date |
---|---|
CN110183850A true CN110183850A (en) | 2019-08-30 |
Family
ID=67719336
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201910467924.5A Pending CN110183850A (en) | 2019-05-31 | 2019-05-31 | Copper oxide/poly-dopamine/redox graphene CuO/PDA/rGO preparation method |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN110183850A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR20210110953A (en) * | 2020-03-02 | 2021-09-10 | 가천대학교 산학협력단 | Activated carbon fibers coated with polydopamine and cupric oxide, antimicrobial filter comprising the same, and the manufacturing method of the same |
CN114965627A (en) * | 2022-05-26 | 2022-08-30 | 新余学院 | Reduced graphene oxide/ammonium nickel phosphate/GCE composite electrode and preparation method and application thereof |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107164020A (en) * | 2017-04-06 | 2017-09-15 | 江苏大学 | A kind of graphene poly-dopamine copper nano composite material and preparation method thereof |
CN108054021A (en) * | 2017-12-07 | 2018-05-18 | 南阳理工学院 | Bicarbonate nickel-poly-dopamine-graphene composite material and preparation method and application |
CN108414598A (en) * | 2018-02-12 | 2018-08-17 | 西北工业大学 | It prepares CuO/rGO@PNIPAm electrodes and constructs enzyme-free glucose sensor and method |
CN108940269A (en) * | 2017-11-03 | 2018-12-07 | 深圳大学 | A kind of Nanoalloy and preparation method thereof |
CN109440153A (en) * | 2018-11-27 | 2019-03-08 | 河北北方学院 | Microwave-electrochemical preparation method of CuHA/GO/ dopamine composite coating |
-
2019
- 2019-05-31 CN CN201910467924.5A patent/CN110183850A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107164020A (en) * | 2017-04-06 | 2017-09-15 | 江苏大学 | A kind of graphene poly-dopamine copper nano composite material and preparation method thereof |
CN108940269A (en) * | 2017-11-03 | 2018-12-07 | 深圳大学 | A kind of Nanoalloy and preparation method thereof |
CN108054021A (en) * | 2017-12-07 | 2018-05-18 | 南阳理工学院 | Bicarbonate nickel-poly-dopamine-graphene composite material and preparation method and application |
CN108414598A (en) * | 2018-02-12 | 2018-08-17 | 西北工业大学 | It prepares CuO/rGO@PNIPAm electrodes and constructs enzyme-free glucose sensor and method |
CN109440153A (en) * | 2018-11-27 | 2019-03-08 | 河北北方学院 | Microwave-electrochemical preparation method of CuHA/GO/ dopamine composite coating |
Non-Patent Citations (2)
Title |
---|
DIPANWITA MAJUMDAR等: ""Ultrasound assisted formation of reduced graphene oxide-copper (II) oxide nanocomposite for energy storage applications"", 《COLLOID AND SURFACES A: PHYSICOCHEMICAL AND ENGINEERING ASPECTS》 * |
YINGLIN XIAO等: ""Polydopamine functionalized grapheme/NiFe2O4 nanocomposite with improving Li stotage performances"", 《NANO ENERGY》 * |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR20210110953A (en) * | 2020-03-02 | 2021-09-10 | 가천대학교 산학협력단 | Activated carbon fibers coated with polydopamine and cupric oxide, antimicrobial filter comprising the same, and the manufacturing method of the same |
KR102326339B1 (en) * | 2020-03-02 | 2021-11-15 | 가천대학교 산학협력단 | Activated carbon fibers coated with polydopamine and cupric oxide, antimicrobial filter comprising the same, and the manufacturing method of the same |
CN114965627A (en) * | 2022-05-26 | 2022-08-30 | 新余学院 | Reduced graphene oxide/ammonium nickel phosphate/GCE composite electrode and preparation method and application thereof |
CN114965627B (en) * | 2022-05-26 | 2024-02-02 | 新余学院 | Reduced graphene oxide/nickel ammonium phosphate/GCE composite electrode and preparation method and application thereof |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN110038634B (en) | Oxygen evolution reaction catalyst based on MXene and metal organic framework compound composite structure and synthesis method thereof | |
CN102078826B (en) | Preparation method and application of ionic liquid modified carbon sphere loaded platinum nanoparticle catalyst | |
CN104289248B (en) | A kind of carbon nano tube compound material and its preparation method and application | |
CN102723504B (en) | Multi-wall carbon nano-tube carried core-shell silver-platinum cathode catalyst and preparation method | |
CN107331872B (en) | A kind of preparation method and applications of the MnO 2/silver composite nano materials based on graphene/carbon nano-tube | |
CN106960965B (en) | A kind of preparation method of the different structural material supported precious metal nano-particle processed of black phosphorus titanium dioxide | |
CN101740785B (en) | Palladium/graphene nano electro-catalyst and preparation method thereof | |
CN112495408B (en) | Preparation method of electrocatalytic hydrogen evolution nano material | |
CN107170998A (en) | A kind of preparation method of black phosphorus graphene composite material supported precious metal nano-particle | |
CN105576216A (en) | Preparation method and application of alpha-nickel sulfide/graphene composite material | |
CN107746051A (en) | A kind of nitrogen-doped graphene nanobelt nano-cobaltic-cobaltous oxide hybrid material and preparation method thereof | |
CN104977342A (en) | Graphene-exfoliation hydrotalcite-like compound composite material immobilized protein modified electrode, production method and application thereof | |
CN103480406A (en) | Nitrogen-doped graphene/nitrogen-doped carbon nanotube/tricobalt tetraoxide composite paper and preparation method thereof | |
CN105070924B (en) | A kind of DMFC molybdenum sulfide functionalized carbon nano-tube carries Pt catalyst and preparation method thereof | |
CN110961162B (en) | Catalyst carrier, precious metal catalyst, and preparation method and application thereof | |
CN109935840A (en) | A kind of preparation method of fuel cell Pt base catalyst | |
CN110183850A (en) | Copper oxide/poly-dopamine/redox graphene CuO/PDA/rGO preparation method | |
CN108878911A (en) | A kind of nitrogen-doped carbon nanometer pipe load Pt catalyst and the preparation method and application thereof based on eutectic solvent | |
CN110197905A (en) | A kind of modifying carbon material and the electrode of liquid flow cell of class graphene nanometer sheet prepared therefrom modification | |
CN108539219A (en) | A kind of sulfur and nitrogen co-doped carbon nanotube carries PtCu alloy catalysts and the preparation method and application thereof | |
CN104993160A (en) | Preparing method for non-precious metal ion complexation Schiff base graphene catalyst | |
CN108172849A (en) | Based on the monoatomic manganese dioxide-carbon nano tube composite catalyst of palladium and its preparation | |
CN109351364A (en) | A kind of preparation method and applications of graphene/class graphite phase carbon nitride/Pd nano particle multi-level nano-structure composite material | |
Yang et al. | Facile synthesis of Fe-MOF/rGO nanocomposite as an efficient electrocatalyst for nonenzymatic H2O2 sensing | |
CN113851664B (en) | Method for preparing hollow sphere electrocatalyst containing sp-nitrogen doped graphite alkyne, prepared material and application |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190830 |