CN110231385A - A method of preparing coalescence crystalviolet-gold composite nano particle modified electrode - Google Patents
A method of preparing coalescence crystalviolet-gold composite nano particle modified electrode Download PDFInfo
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- CN110231385A CN110231385A CN201910431939.6A CN201910431939A CN110231385A CN 110231385 A CN110231385 A CN 110231385A CN 201910431939 A CN201910431939 A CN 201910431939A CN 110231385 A CN110231385 A CN 110231385A
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- 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
- G01N27/3278—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction involving nanosized elements, e.g. nanogaps or nanoparticles
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Abstract
Coalescence crystalviolet-gold composite nano particle modified electrode method is prepared the invention discloses a kind of.Its method and step: it is deposited on electrode first with cyclic voltammetry by crystalviolet is coalesced, electrode is then placed in HAuCl4Solution in, reacted in 60 DEG C of thermostat water baths for 24 hours and coalescence crystalviolet-gold composite nano particle modified electrode can be obtained afterwards.The method of the present invention preparation process only needs two steps, high-efficient, at low cost, and the fitting in coalescence crystalviolet-gold composite modified electrode prepared by the present invention has Nano grade size, has broad application prospects in field of bioanalysis.
Description
Technical field
The invention belongs to inorganic-organic hybridization nano particle synthetic technology and electrochemical fields, in particular to a kind of to prepare
Coalesce crystalviolet-gold composite nano particle modified electrode method.
Background technique
" composite nano particle " refers to that two or more substance is combined together in some way on nanoscale
And the compound particle constituted.Composite nano particle not only remains the characteristic of single nano material, moreover it is possible to promote single nanometer material
The performances such as optical electro-chemistry, the thermodynamics of material, thus composite nano particle is shown well in fields such as bio-sensing, environmental protections
Application prospect.
Coalescence crystalviolet common are engine dyeing material as one kind, and larger heterocycle conjugated system is contained in molecule, and electrochemistry is living
Property it is strong, electronics conduction velocity is fast, and stronger suction-operated can be generated with electrode, be commonly used for electrode modified material.In addition, Jenner
A kind of rice corpuscles nano material high as bioaffinity and compatibility, is commonly used for field of bioanalysis, however, individually
Gold nano-material usually has the characteristics that synthesis condition harshness, light-exposed mutability, thus, find a kind of simple and efficient preparation gold
The method of nano material is the key that improve chemical analysis efficiency.
In the recombination process of coalescence crystalviolet and gold nano particulate, the form of coalescence crystalviolet itself can change, and coalesce
Crystalviolet-gold composite nano particle can not only promote the stability and adsorptivity of single organic dyestuff, moreover it is possible to it is raw to make up organic dyestuff
The feature of object compatibility difference, thus, coalescence crystalviolet-gold composite nano particle can be realized the major progress of Electroanalytical Chemistry.
Summary of the invention
Coalescence crystalviolet-gold composite nano particle modified electrode method is prepared the object of the present invention is to provide a kind of.
Specific steps are as follows:
(1) by the ITO conductive glass electrode cut out in advance respectively with analysis pure acetone, dehydrated alcohol and each ultrasound of secondary water
5min is cleaned, it is stand-by after measuring conducting surface with multimeter after drying.
(2) successively measuring 1mL concentration is 2 × 10-3The crystal violet solution of mol/L, 4mL concentration are the KNO of 0.5mol/L3It is molten
Liquid, 5mL concentration are that the PBS buffer solution that 0.1mol/L, pH are 6.8 is placed in 20mL beaker and uniformly mixes, and it is poly- that electro-deposition is made
The bottom liquid of crystal violet.
(3) three-electrode system is established in the bottom liquid of electro-deposition obtained coalescence crystalviolet in step (2), wherein working electrode
It is Pt electrode to electrode for conductive glass electrode made from step (1), reference electrode is Ag/AgCl electrode, uses cyclic voltammetry
Electro-deposition is carried out, electric potential scanning range is -1.0V~1.8V, scanning speed 0.1V/s, and scanning number of segment is 40.Electro-deposition terminates
Afterwards, electrode is taken out and is rinsed well with secondary water, coalescence crystalviolet electrode can be obtained after air drying.
(4) it is the HAc-NaAc buffer solution that 0.2mol/L, pH are 6,50 μ L that 300 μ L concentration are added in 20mL vial
Concentration is 0.2mol/L hexadecyltrimethylammonium chloride solution, the HAuCl that 50 μ L mass fractions are 1%4Solution, 5mL bis- times
Coalescence crystalviolet-gold composite nano particle growth-promoting media is made in water.Coalescence crystalviolet electrode obtained in step (3) is put into growth
In liquid, is reacted in 60 DEG C of waters bath with thermostatic control of Yu Yu and take out coalescence crystalviolet film afterwards for 24 hours, rinsed well with secondary water, drying can obtain
To coalescence crystalviolet-gold composite nano particle film.
ITO conductive glass electrode in the step (1) is the glass electrode of doped indium tin oxide.
PBS buffer solution in the step (2) is Na2HPO4-NaH2PO4Buffer solution.The advantages of the method for the present invention, is such as
Under:
(1) the method for the present invention preparation process is simple, only relates to simply cleaning and deposition process, and preparation condition is mild, at
This is low, may be implemented to be mass produced.
(2) there is the method for the present invention coalescence crystalviolet-gold composite particles modified electrode obtained good film forming and electricity to urge
Change activity, is applicable in the detection such as glucose, it is as a result satisfactory.
Detailed description of the invention
It is that coalescence crystalviolet-gold composite nano particle modified electrode scanning electron prepared by the embodiment of the present invention 1 is aobvious in Fig. 1
Micro mirror photo (SEM).
It is the X ray diffracting spectrum of coalescence crystalviolet electrode prepared by the embodiment of the present invention 1 in Fig. 2.
It is coalescence crystalviolet-gold composite nano particle modified electrode X-ray diffraction prepared by the embodiment of the present invention 1 in Fig. 3
Map.
Fig. 4 is the coalescence crystalviolet electrode (b) and coalesce that the glass-carbon electrode (a) in comparative example 1 is prepared with the embodiment of the present invention 1
Crystalviolet-gold composite nano particle modified electrode (c) follows linear sweep voltammetry figure to glucose responding.
Specific embodiment
Embodiment
The present embodiment is for illustrating the present invention coalescence crystalviolet-gold composite nano particle modified electrode synthetic method and its shape
Looks, composition analysis.
(1) by the 1cm × 3cm ITO conductive glass electrode cut out in advance respectively with analysis pure acetone, dehydrated alcohol and two
Secondary water is respectively cleaned by ultrasonic 5min, stand-by after measuring conducting surface with multimeter after drying.
(2) successively measuring 1mL concentration is 2 × 10-3The crystal violet solution of mol/L, 4mL concentration are the KNO of 0.5mol/L3It is molten
Liquid, 5mL concentration are that the PBS buffer solution that 0.1mol/L, pH are 6.8 is placed in 20mL beaker and uniformly mixes, and it is poly- that electro-deposition is made
The bottom liquid of crystal violet.
(3) three-electrode system is established in the bottom liquid of electro-deposition obtained coalescence crystalviolet in step (2), wherein working electrode
It is Pt electrode to electrode for conductive glass electrode made from step (1), reference electrode is Ag/AgCl electrode, uses cyclic voltammetry
Electro-deposition is carried out, electric potential scanning range is -1.0V~1.8V, scanning speed 0.1V/s, and scanning number of segment is 40.Electro-deposition terminates
Afterwards, electrode is taken out and is rinsed well with secondary water, coalescence crystalviolet electrode can be obtained after air drying.
(4) it is the HAc-NaAc buffer solution that 0.2mol/L, pH are 6,50 μ L that 300 μ L concentration are added in 20mL vial
Concentration is 0.2mol/L hexadecyltrimethylammonium chloride solution, the HAuCl that 50 μ L mass fractions are 1%4Solution, 5mL bis- times
Coalescence crystalviolet-gold composite nano particle growth-promoting media is made in water.Coalescence crystalviolet film obtained in step (3) is put into growth
In liquid, is reacted in 60 DEG C of waters bath with thermostatic control of Yu Yu and take out coalescence crystalviolet electrode afterwards for 24 hours, rinsed well with secondary water, drying can obtain
To coalescence crystalviolet-gold composite nano particle film.
ITO conductive glass electrode in the step (1) is the glass electrode of doped indium tin oxide.
PBS buffer solution in the step (2) is Na2HPO4-NaH2PO4Buffer solution.
It is analyzed by scanning electron microscope (SEM), has studied coalescence crystalviolet electrode and coalescence crystalviolet-gold composite Nano is micro-
The pattern of grain modified electrode, as can be seen from Figure 1 coalescing crystalviolet-gold composite nano particle modified electrode surface has dispersibility to receive
Rice gold particle.
By X-ray diffraction analysis, coalescence crystalviolet electrode and coalescence crystalviolet-gold composite nano particle modified electrode are had studied
Material composition, Fig. 2 and Fig. 3 the result shows that, data result made from the present embodiment shows to coalesce crystalviolet film and coalesces crystalviolet-
Golden composite nano particle modified electrode material composition is clear.
In summary, it was demonstrated that purple-golden composite nano particle modified electrode pattern of crystalline polyimide and material composition are clear, clear.
Comparative example 1:
Coalescence crystalviolet-gold composite nano particle modified electrode property prepared by the present invention is measured in terms of electrochemical field
Energy.
1) respectively with bare glassy carbon electrode (a), coalescence crystalviolet electrode (b) and coalescence crystalviolet-gold composite nano particle modification electricity
Pole (b) is used as working electrode, and Ag/AgCl electrode is reference electrode, and Pt electrode is to form three-electrode system to electrode.With
0.1mol/L NaOH is bottom liquid, and glucose concentration is 1.0 × 10-3Mol/L, scanning speed 100mV/s, linear scan volt
Antu, as a result such as Fig. 3.
As seen from Figure 4 to coalesce crystalviolet-gold composite nano particle modified electrode as the electrification of the glucose of working electrode
Learning signal has apparent enhancing, shows that the oxidation of glucose can be catalyzed also by coalescing crystalviolet-gold composite nano particle modified electrode
It is former.
In conclusion coalescence crystalviolet prepared by the present invention-gold composite nano particle modified electrode has good electro-catalysis
Performance combines the good characteristic of organic dyestuff (coalescence crystalviolet), gold nano-material, has in electrochemical field and widely answer
With.
Claims (3)
1. a kind of prepare coalescence crystalviolet-gold composite nano particle modified electrode method, it is characterised in that specific steps:
(1) the ITO conductive glass electrode cut out in advance is respectively cleaned by ultrasonic with analysis pure acetone, dehydrated alcohol and secondary water respectively
5min, it is stand-by after measuring conducting surface with multimeter after drying；
(2) successively measuring 1mL concentration is 2 × 10-3The crystal violet solution of mol/L, 4mL concentration are the KNO of 0.5mol/L3Solution,
5mL concentration is that the PBS buffer solution that 0.1mol/L, pH are 6.8 is placed in 20mL beaker and uniformly mixes, and electro-deposition crystalline polyimide is made
Purple bottom liquid；
(3) three-electrode system is established in the bottom liquid of electro-deposition obtained coalescence crystalviolet in step (2), wherein working electrode is step
Suddenly conductive glass electrode made from (1) is Pt electrode to electrode, and reference electrode is Ag/AgCl electrode, is carried out with cyclic voltammetry
Electro-deposition, electric potential scanning range are -1.0V~1.8V, scanning speed 0.1V/s, and scanning number of segment is 40, after electro-deposition,
Electrode is taken out and is rinsed well with secondary water, coalescence crystalviolet electrode can be obtained after air drying；
(4) it is the HAc-NaAc buffer solution that 0.2mol/L, pH are 6,50 μ L concentration that 300 μ L concentration are added in 20mL vial
For 0.2mol/L hexadecyltrimethylammonium chloride solution, the HAuCl that 50 μ L mass fractions are 1%4Solution, 5mL secondary water, system
Crystalviolet-gold composite nano particle growth-promoting media must be coalesced, coalescence crystalviolet electrode obtained in step (3) is put into growth-promoting media,
Coalescence crystalviolet electrode is taken out afterwards for 24 hours in reacting in 60 DEG C of waters bath with thermostatic control, is rinsed well with secondary water, coalescence can be obtained in drying
Crystalviolet-gold composite nano particle film.
2. preparation method according to claim 1, it is characterised in that the ITO conductive glass electrode in the step (1) is
The glass electrode of doped indium tin oxide.
3. preparation method according to claim 1, it is characterised in that the PBS buffer solution in the step (2) is
Na2HPO4-NaH2PO4Buffer solution.
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Application publication date: 20190913 |