CN101629930A - Boron-doped diamond electrode modified with gold-nanofiber composite preparation method - Google Patents
Boron-doped diamond electrode modified with gold-nanofiber composite preparation method Download PDFInfo
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- CN101629930A CN101629930A CN200910032746A CN200910032746A CN101629930A CN 101629930 A CN101629930 A CN 101629930A CN 200910032746 A CN200910032746 A CN 200910032746A CN 200910032746 A CN200910032746 A CN 200910032746A CN 101629930 A CN101629930 A CN 101629930A
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- doped diamond
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Abstract
The invention discloses a boron-doped diamond electrode modified with gold-nanofiber composite preparation method, comprising the following steps: adsorbing negative [AuCl4]<-> on the surface of nanofiber with positive charges according to the electrostatic adsorption principle, then growing gold by chemical reduction method to prepare gold-nanofiber composite which is used to modify a boron-doped diamond electrode and obtaining an electrochemical sensor. The modified electrode overcomes the defect of low electrocatalytic activity for a boron-doped diamond electrode, has electrocatalysis to electrochemical active material, reduces overpotential of the oxidation reaction, increases the detection sensitivity and improves the stability and the selectivity of electrodes.
Description
Technical field
The invention belongs to material preparation and electrochemical sensor technical field, be specifically related to a kind of gold/nanofiber composite modified electrode and preparation method thereof.
Background technology
As the novel electrode material, the boron-doped diamond film since have many conventional electrodes incomparable superiority, be difficult for advantages such as contaminated as wide electrochemical potential window, low background current, fabulous electrochemical stability and surface, the application potential at aspects such as electroanalysis, spectroelectrochemistry, galvanic corrosion electrode and electro-catalysis is huge and development is rapid.Though diamond thin has above-mentioned advantage, also exist simultaneously not enoughly, show as that electro catalytic activity is low, resurfacing is difficult, particularly to the detection of some multiple electroactive substances coexistence systems such as living things system, its selectivity and sensitivity are relatively poor.
Nano material has a good application prospect because it is different from the special nature of macroscopic material and microscopic particle.Material under the nanoscale produces special behavior on chemistry, galvanochemistry.The surface effect of nano material and small-size effect, promptly diameter is little, specific surface area is big, surface energy is high, Atomic coordinate is not enough, makes its surface atom active high, easy and other material generation electron transport effects on every side, useful as catalysts improves catalytic activity.When utilizing nano material that electrode is modified, except the physicochemical characteristic of material itself being introduced the electrode interface, bigger serface, the particle surface that also can have nano material simultaneously have than characteristics such as multi-functional groups, thereby some electrochemical behavior is produced distinctive catalytic effect.The effect of nano material in modified electrode can show as and improve electrocatalysis characteristic, can reduce overpotential, accelerate the speed of electrochemical reaction, the selectivity that improves electrode and sensitivity etc.Nanometer technology combines with electrochemical techniques, makes electrochemical sensor obtain good progress.
The present invention is directed to the shortcoming of boron-doped diamond electrode, utilize gold utensil that excellent electric conductivity, good chemical stability and bio-compatibility are arranged, the combining nano fiber can increase specific surface area, improve characteristics such as catalytic activity, preparation gold/nanofiber composite modified electrode, be used for Electrochemical Detection, be intended to improve electrode performance, improve the sensitivity of electrode.
Summary of the invention
Technical matters: the objective of the invention is for overcoming the low deficiency that waits of electro catalytic activity that novel electrode material boron-doped diamond exists, the preparation method of a kind of gold and nanofiber composite modified electrode is provided, when this modified electrode is used for Electrochemical Detection, can increase specific surface area, promote electron transfer, improve electro catalytic activity, realize highly sensitive detection.
Technical scheme: purpose of the present invention can realize by following scheme:
Utilize Electrostatic Absorption and chemical reduction method at nanofiber superficial growth gold, the preparation gold is boron-doped diamond electrode modified with nanofiber composite, and concrete grammar may further comprise the steps:
1) chooses different nanofibers, it is carried out surface treatment, obtain the nanofiber of positively charged;
2) utilize electrostatic absorption principle, elder generation is at the electronegative gold chloride ion of nanofiber the surface adsorption ([AuCl of positively charged
4]
-), utilize the sodium borohydride reduction method again, at fiber surface growing nano gold as seed;
3) with the parcel nanofiber gold as seed, be reductive agent further with the oxammonium hydrochloride, utilize the chemically grown legal system to be equipped with gold nano grain, obtain gold/nanofiber composite;
4) get a certain amount of gold and nanofiber composite and be added drop-wise to the boron-doped diamond electrode surface, drying obtains gold and nanofiber composite modified electrode under the room temperature.
Described electrode is a boron-doped diamond electrode.Described nanofiber is polystyrene, polymethylmethacrylate, polyaniline or the shitosan in the organic nanofibers, or is the titania of inorganic nano-fiber.
In the technical program, described nm of gold has excellent electric conductivity, good chemical stability and bio-compatibility.Described nanofiber can be fixed more nm of gold, increases specific surface area, improves catalytic activity.Control ratio golden and nanofiber by the concentration that changes nanofiber, optimize various conditions, obtain best modified electrode material.
Beneficial effect: utilize Electrostatic Absorption and chemical reduction method to prepare gold/nanofiber composite modified electrode according to the present invention, have the following advantages:
1) nm of gold has excellent electric conductivity, good chemical stability and bio-compatibility, be used for the effect that modified electrode can play the nano-scale electrode, effectively accelerate the electron transfer efficiency of electrode surface, promote reaction to carry out, strengthened the chemical property of electrode.
2) nano level fiber has the special nature of nano material, shows unique electricity and chemical property.More gold can be fixed in this nanofiber surface, and its randomness and special construction can increase specific surface area, improves catalytic activity;
3) Zhi Bei gold/nanofiber composite modified electrode has improved electrode performance, overcome the low deficiency of boron-doped diamond electrode electro catalytic activity, electroactive substance had catalytic action, reduce the oxidation reaction overpotential, improve detection sensitivity, reduce detection limit, improve the selectivity and the stability of electrode.
Embodiment
Utilize the nanofiber surface adsorption electronegative [AuCl of electrostatic absorption principle at positively charged
4]
-, utilizing chemical reduction method growth gold again, preparation gold/nanofiber composite is boron-doped diamond electrode modified, is used as electrochemical sensor.
The preparation method may further comprise the steps:
At first, under vigorous stirring with a certain amount of gold chloride (HAuCl
4) in the positively charged nanofiber solution that add to suspend of solution, continue to stir and guarantee electronegative [AuCl
4]
-Ion is adsorbed onto the nanofiber surface of positively charged fully.Dropwise drip a certain amount of sodium borohydride up to observing change in color, so step can obtain nm of gold on the nanofiber surface of positively charged.With the parcel nanofiber gold as seed, further utilize the chemically grown legal system to be equipped with gold nano grain.Concrete grammar is: clean above-mentioned suspending liquid repeatedly with deionized water, water dilutes suspending liquid then, adds certain amount of H AuCl under stirring condition
4And oxammonium hydrochloride, continue to stir the nm of gold that increases with the stabilized nanoscale fiber surface.Control ratio golden and nanofiber by the concentration that changes nanofiber, optimize various conditions, obtain best modified electrode material.Get a certain amount of gold/nanofiber composite for preparing and be added drop-wise to the boron-doped diamond electrode surface, drying obtains gold/nanofiber composite modified electrode under the room temperature.
Embodiment.The preparation of gold/titanium dioxide nanofiber compound
1 TiO
2Nanofiber immerses in the HCl solution of pH1.5, and fully vibration is stirred, and makes its surface lotus that becomes positively charged.
2 under vigorous stirring with the HAuCl of 0.6ml 1wt%
4Solution adds the suspension TiO of 40ml pH1.5
2In the nanofiber solution, keep to stir several hrs and allow electronegative [AuCl
4]
-Be adsorbed onto the TiO of positively charged fully
2The nanofiber surface.
3 dropwise drip 0.5mg ml
-1Sodium borohydride up to observing change in color, so step can be at the TiO of positively charged
2The nanofiber surface obtains nm of gold.
4 with parcel TiO
2The gold of nanofiber further utilizes the chemically grown legal system to be equipped with gold nano grain as seed.Concrete grammar is: clean above-mentioned suspending liquid repeatedly with deionized water, water is diluted to 30ml with suspending liquid then, adds HAuCl under stirring condition
4(1wt%, 0.1ml) and oxammonium hydrochloride (0.04M, 0.5ml), continue to stir increased and stable TiO in 15 minutes
2The nm of gold on nanofiber surface.
5 keep the concentration of gold constant, change TiO
2The concentration of nanofiber, with method for preparing the Au/TiO of four kinds of different proportions
2Nanofiber composite.TiO
2Be respectively 9: 1 with the ratio of gold, 18: 1,27: 1 and 36: 1.
6 repeated washing Au/TiO
2Nanofiber composite is removed unnecessary ion in the solution.Respectively with the Au/TiO of 20 μ l different proportions
2Nanofiber composite is added drop-wise to the BDD electrode surface, and drying obtains Au/TiO under the room temperature
2Nanofiber is modified diamond electrode.
Claims (3)
1. gold and the boron-doped diamond electrode modified preparation method of nanofiber composite, it is characterized in that utilizing Electrostatic Absorption and chemical reduction method at nanofiber superficial growth gold, the preparation gold is boron-doped diamond electrode modified with nanofiber composite, and concrete grammar may further comprise the steps:
1) chooses different nanofibers, it is carried out surface treatment, obtain the nanofiber of positively charged;
2) utilize electrostatic absorption principle, elder generation is at the electronegative gold chloride ion of nanofiber the surface adsorption ([AuCl of positively charged
4]
-), utilize the sodium borohydride reduction method again, at fiber surface growing nano gold as seed;
3) with the parcel nanofiber gold as seed, be reductive agent further with the oxammonium hydrochloride, utilize the chemically grown legal system to be equipped with gold nano grain, obtain gold/nanofiber composite;
4) get a certain amount of gold and nanofiber composite and be added drop-wise to the boron-doped diamond electrode surface, drying obtains gold and nanofiber composite modified electrode under the room temperature.
2. gold according to claim 1 and the boron-doped diamond electrode modified preparation method of nanofiber composite is characterized in that described electrode is a boron-doped diamond electrode.
3. gold according to claim 1 and the boron-doped diamond electrode modified preparation method of nanofiber composite, it is characterized in that described nanofiber is polystyrene, polymethylmethacrylate, polyaniline or the shitosan in the organic nanofibers, or be the titania of inorganic nano-fiber.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910032746A CN101629930A (en) | 2009-06-19 | 2009-06-19 | Boron-doped diamond electrode modified with gold-nanofiber composite preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910032746A CN101629930A (en) | 2009-06-19 | 2009-06-19 | Boron-doped diamond electrode modified with gold-nanofiber composite preparation method |
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|---|---|
| CN101629930A true CN101629930A (en) | 2010-01-20 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103487483A (en) * | 2013-09-12 | 2014-01-01 | 同济大学 | Electrochemical analyzing method for constructing 17beta-estradiol aptamer sensor based on dendritic gold modification BDD electrode |
| CN104007157A (en) * | 2014-05-29 | 2014-08-27 | 河南工业大学 | Preparation and application for electrochemical sensor based on nano-structure boron-doped diamond electrode |
| CN104090011A (en) * | 2014-07-09 | 2014-10-08 | 东南大学 | Preparation method for nanogold-nanofiber functional composite modified electrode |
| CN105036069A (en) * | 2015-06-19 | 2015-11-11 | 首都师范大学 | Gold/poly(o-aminophenol), gold/poly(p-phenylenediamine) and gold/poly(o-phenylenediamine) nanoparticles as well as preparation method and application thereof |
| CN109306551A (en) * | 2018-07-18 | 2019-02-05 | 湘潭大学 | A kind of boron doped titanic oxide nanofiber and preparation method thereof and application as lithium ion battery negative material |
-
2009
- 2009-06-19 CN CN200910032746A patent/CN101629930A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103487483A (en) * | 2013-09-12 | 2014-01-01 | 同济大学 | Electrochemical analyzing method for constructing 17beta-estradiol aptamer sensor based on dendritic gold modification BDD electrode |
| CN103487483B (en) * | 2013-09-12 | 2015-07-29 | 同济大学 | Electrochemical analysis method BDD electrode being constructed 17 beta estradiol aptamer sensor is modified based on dendritic gold |
| CN104007157A (en) * | 2014-05-29 | 2014-08-27 | 河南工业大学 | Preparation and application for electrochemical sensor based on nano-structure boron-doped diamond electrode |
| CN104090011A (en) * | 2014-07-09 | 2014-10-08 | 东南大学 | Preparation method for nanogold-nanofiber functional composite modified electrode |
| CN105036069A (en) * | 2015-06-19 | 2015-11-11 | 首都师范大学 | Gold/poly(o-aminophenol), gold/poly(p-phenylenediamine) and gold/poly(o-phenylenediamine) nanoparticles as well as preparation method and application thereof |
| CN109306551A (en) * | 2018-07-18 | 2019-02-05 | 湘潭大学 | A kind of boron doped titanic oxide nanofiber and preparation method thereof and application as lithium ion battery negative material |
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Application publication date: 20100120 |