CN105675681A - Preparation method and application of nano-wire modified electrode - Google Patents
Preparation method and application of nano-wire modified electrode Download PDFInfo
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- CN105675681A CN105675681A CN201510739449.4A CN201510739449A CN105675681A CN 105675681 A CN105675681 A CN 105675681A CN 201510739449 A CN201510739449 A CN 201510739449A CN 105675681 A CN105675681 A CN 105675681A
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Abstract
The invention relates to a preparation method and application of a nano-wire modified electrode and especially relates to the preparation method and the application of a gold (Au) super-long nano-wire modified electrode. The preparation method includes the steps of: synthesizing Te super-long nano-wires through a hydro-thermal method; and synthesizing Au super-long nano-wires with the Te super-long nano-wires as a template; and fixing the Au super-long nano-wire onto the surface of a work electrode to prepare the Au super-long nano-wire modified electrode. A nitrite sensor has a linear relationship when the nitrite concentration is 1.0-970 [mu]mol/L and can reach 0.2 [mu]mol/L in detection limit.
Description
Technical field
The present invention relates to the preparation method of a kind of nano wire modified electrode, refer in particular to preparation method and the application thereof of a kind of gold Au overlong nanowire modified electrode.
Background technology
Pickling food are because of the local flavor of its uniqueness and like by consumers in general containing a large amount of VITAMIN, calcium, phosphorus and other inorganics, but it contains nitrite, also make a lot of prestige and far it. Nitrite has potential toxicity, and it generates carcinogens nitrosamine with secondary amine reaction in stomach. The World Health Organization specifies: in pickling food, nitrite content must not more than 0.2mg/kg, and nitrite in drinking water must not more than 3mg L-1. Therefore, accurately detect the nitrite in food and tap water most important. The method of detection nitrite has spectrophotometry, chromatography, electrochemistry etc. at present. Electrochemical sensor is a kind of easy, inexpensive, test mode fast. At present, the gordian technique that suitable electrode materials is development electrochemical sensor is developed.
The special character of nano material makes it have widespread use in the research of sensor, nano material has big specific surface area, causes Active sites to increase, can significantly increase test substance electronics transfer rate on modified electrode, thus improves the susceptibility of sensor. Gold Au nano material becomes the metallic element most in nano material with research vigor and development potentiality, because it has unusual optics, electrical properties, has a wide range of applications at nanoelectronics, nano optoelectronics, Catalysis work and biomedical sector. In the Au nano material of different shape, nano particle synthesis aspect research is maximum. Compared with Au nano particle, Au overlong nanowire has more excellent bioaffinity and linear optical property. Prior art has had reporting for work about Template synthesis Au overlong nanowire.
Summary of the invention
It is an object of the invention to provide a kind of by templated synthesis of tellurium Te overlong nanowire gold Au overlong nanowire, and prepare nitrite (with Sodium Nitrite) sensor electrode in this electrode, it is achieved to the detection of nitrite.
The object of the invention can be achieved through the following technical solutions:
The present invention discloses the preparation method of a kind of nano wire modified electrode, and the method is gold Au overlong nanowire by templated synthesis of tellurium Te overlong nanowire, and its step is as follows:
Step 1, synthesis Te overlong nanowire
1.0g polyvinylpyrrolidone and 0.01g sodium tellurite are dissolved in 35mL redistilled water, ultrasonic disperse 1 hour, form stable solution, 1.65mL (40wt%) hydrazine hydrate and 3.35mL (28wt%) ammonia soln is added in solution, move in the reactor of teflon lined of 50mL after short mix, the retort furnace putting into 180 ° of C after being closed by reactor reacts 4 hours, after reaction terminates, room temperature cools 12 hours, the acetone of 80-200mL is added in cooling fluid, static 12-24 hour, centrifugal, Te overlong nanowire is obtained with after second distillation water washing five times,
Step 2, taking Te overlong nanowire as templated synthesis Au overlong nanowire
Take 10mgHAuCl4·4H2O is dissolved in 10mL distilled water, fully stirs and obtains 2.5mmol/LHAuCl4Solution; Taking 1.0mgTe overlong nanowire is scattered in the distilled water of 25mL, stirs after evenly and adds 1-5mL2.5mmol/LHAuCl4Solution and maintenance ultrasonic power 50-200w, ultrasonic reaction 20-60 minute, makes Te overlong nanowire HAuCl4Automatic by electric current displacement response generation Au overlong nanowire, product redistilled water is cleaned 5-10 time to remove remaining chlorauric acid solution after terminating by reaction, and in 50 DEG C of vacuum drying ovens, drying 6 hours, obtain Au overlong nanowire;
Taking Te overlong nanowire as the experimental principle of templated synthesis Au overlong nanowire is:
HAuCl4·3H2O+Te=Au+TeO3 2-+4Cl-+7H+
Step 3, the preparation of Au overlong nanowire modified electrode
Gained Au overlong nanowire is dissolved in the redistilled water of 20mL and obtains the Au overlong nanowire aqueous solution, 1mL5wt% naphthols is added in obtained aqueous solution, stir after evenly and obtain mixing solutions, get 1-5 μ L mixing solutions and drip the glassy carbon electrode surface being coated onto and handling well, dry with infrared lamp, obtain Au overlong nanowire modified electrode.
Wherein, the Au overlong nanowire of described modified electrode surface coverage, length is 1-100 μm, and diameter is 20-50nm.
The invention also discloses the application of the Au overlong nanowire modified electrode described in utilization in nitrite detects.
Compared with prior art, its advantage is in the present invention:
(1) described Au overlong nanowire modified electrode preparation method is simple, environmental protection, without additional go back original reagent under, Te overlong nanowire and HAuCl4Solution occurs electric current displacement response to generate Au overlong nanowire automatically;
(2), there is good catalytic effect, and present wide linearity range in described Au overlong nanowire modified electrode to nitrite. Its detectability can reach 0.2 μm of ol/L.
Accompanying drawing explanation
Fig. 1 is in embodiment 1, the SEM figure of Au overlong nanowire; Fig. 2 is in embodiment 1, the X-ray powder diffraction figure of Au overlong nanowire; Fig. 3 is in embodiment 1, and bare electrode and Au overlong nanowire are to the cyclic voltammetry curve of 1mmol/L Sodium Nitrite; Fig. 4 is in embodiment 1, and Au overlong nanowire sensor is to the chronoa mperometric plot of nitrite; Fig. 5 is in embodiment 1, the linear relationship chart of chronoa mperometric plot electric current and nitrite anions concentration; Fig. 6 is in embodiment 2, and bare electrode and Au overlong nanowire modified electrode are to the cyclic voltammetry curve of 1mmol/L nitrite; Fig. 7 is in embodiment 3, and bare electrode and Au overlong nanowire modified electrode are to the cyclic voltammetry curve of 1mmol/L nitrite.
Embodiment
The present invention discloses the basic preparation method of a kind of nano wire modified electrode, and the method is gold Au overlong nanowire by templated synthesis of tellurium Te overlong nanowire, and its step is as follows:
Step 1, synthesis Te overlong nanowire
1.0g polyvinylpyrrolidone and 0.01g sodium tellurite are dissolved in 35mL redistilled water, ultrasonic disperse 1 hour, form stable solution, 1.65mL (40wt%) hydrazine hydrate and 3.35mL (28wt%) ammonia soln is added in solution, move in the reactor of teflon lined of 50mL after short mix, the retort furnace putting into 180 ° of C after being closed by reactor reacts 4 hours, after reaction terminates, room temperature cools 12 hours, the acetone of 80-200mL is added in cooling fluid, static 12-24 hour, centrifugal, Te overlong nanowire is obtained with after second distillation water washing five times,
Step 2, taking Te overlong nanowire as templated synthesis Au overlong nanowire
Take 10mgHAuCl4·4H2O is dissolved in 10mL distilled water, fully stirs and obtains 2.5mmol/LHAuCl4Solution; Taking 1.0mgTe overlong nanowire is scattered in the distilled water of 25mL, stirs after evenly and adds 1-5mL2.5mmol/LHAuCl4Solution and maintenance ultrasonic power 50-200w, ultrasonic reaction 20-60 minute, makes Te overlong nanowire HAuCl4Automatic by electric current displacement response generation Au overlong nanowire, product redistilled water is cleaned 5-10 time to remove remaining chlorauric acid solution after terminating by reaction, and in 50 DEG C of vacuum drying ovens, drying 6 hours, obtain Au overlong nanowire;
Taking Te overlong nanowire as the experimental principle of templated synthesis Au overlong nanowire is:
HAuCl4·3H2O+Te=Au+TeO3 2-+4Cl-+7H+
Step 3, the preparation of Au overlong nanowire modified electrode
Gained Au overlong nanowire is dissolved in the redistilled water of 20mL and obtains the Au overlong nanowire aqueous solution, 1mL5wt% naphthols is added in obtained aqueous solution, stir after evenly and obtain mixing solutions, get 1-5 μ L mixing solutions and drip the glassy carbon electrode surface being coated onto and handling well, dry with infrared lamp, obtain Au overlong nanowire modified electrode.
Wherein, the Au overlong nanowire of described modified electrode surface coverage, length is 1-100 μm, and diameter is 20-50nm.
Below in conjunction with drawings and Examples, the invention will be further described.
Embodiment 1
(1) Te overlong nanowire is synthesized
1.0g polyvinylpyrrolidone and 0.01g sodium tellurite are dissolved in 35mL redistilled water, ultrasonic disperse 1 hour, form stable solution, 1.65mL (40wt%) hydrazine hydrate and 3.35mL (28wt%) ammonia soln is added in solution, move in the reactor of teflon lined of 50mL after short mix, the retort furnace putting into 180 ° of C after being closed by reactor reacts 4 hours, after reaction terminates, room temperature cools 12 hours, the acetone of 120mL is added in cooling fluid, static 12 hours, centrifugal, Te overlong nanowire is obtained with after second distillation water washing 5 times,
(2) taking Te overlong nanowire as templated synthesis Au overlong nanowire
Accurately take 10mgHAuCl4·4H2O is dissolved in 10mL distilled water, fully stirs and obtains 2.5mmol/LHAuCl4Solution; Accurately taking 1.0mgTe overlong nanowire is scattered in the distilled water of 25mL, stirs after evenly and adds 2mL2.5mmol/LHAuCl4Solution, keeps ultrasonic power 50w, ultrasonic reaction 30 minutes, under existing without any other reagent, and Te overlong nanowire and HAuCl4Automatically generating Au overlong nanowire (accompanying drawing 1) by electric current displacement response, product redistilled water is cleaned 5 times, in 50 ° of C vacuum drying ovens, drying 6 hours, obtain Au overlong nanowire;
(3) preparation of Au overlong nanowire modified electrode
Gained Au overlong nanowire is dissolved in the redistilled water of 20mL and obtains the Au overlong nanowire aqueous solution, 1mL5wt% naphthols is added in obtained aqueous solution, stir after evenly and obtain mixing solutions, get 1 μ L mixing solutions and drip the glassy carbon electrode surface being coated onto and handling well, dry with infrared lamp, obtain Au overlong nanowire modified electrode.
Fig. 2 is the X-ray powder diffraction figure of Au overlong nanowire obtained in the present embodiment.
Fig. 3 is that the Au overlong nanowire sensor obtained in the present embodiment is to the cyclic voltammetry curve of 1mmol/L nitrite. Wherein, a curve is bare electrode, and b curve is Au overlong nanowire modified electrode. As can be seen from Figure 3, for the nitrite of same concentrations, Au overlong nanowire modified electrode has higher oxidation current, illustrates that nitrite is had good electric catalyticing characteristic by Au overlong nanowire.
Fig. 4 is that the Au overlong nanowire sensor obtained in the present embodiment is to the chronoa mperometric plot of nitrite. As can be seen from Figure 4, along with nitrite concentration increases, step-flow increases sharply, and the time of response is less than 5s. Fig. 5 is the linear relationship chart of chronoa mperometric plot phase induced current from different nitrite concentration, as shown in interior illustration, there is linear relationship within 1.0 μm of ol/L～0.97mmol/L scopes, and detection is limited to 0.2 μm of ol/L.
Embodiment 2
(1) Te overlong nanowire is synthesized: with embodiment 1
(2) taking Te overlong nanowire as templated synthesis Au overlong nanowire: with embodiment 1
(3) preparation of Au overlong nanowire modified electrode
Gained Au overlong nanowire is dissolved in the redistilled water of 20mL and obtains the Au overlong nanowire aqueous solution, 1mL5wt% naphthols is added in obtained aqueous solution, stir after evenly and obtain mixing solutions, get 2 μ L mixing solutionss and drip the glassy carbon electrode surface being coated onto and handling well, dry with infrared lamp, obtain Au overlong nanowire modified electrode;
Fig. 5 is that the Au overlong nanowire sensor obtained in the present embodiment is to the cyclic voltammetry curve of 1mmol/L nitrite. Wherein, a curve is bare electrode, and b curve is Au overlong nanowire modified electrode in embodiment 1, and c curve is the Au overlong nanowire modified electrode in the present embodiment. As Fig. 5 display: in the present embodiment Au overlong nanowire modified electrode to the catalysis peak current of nitrite lower than Au overlong nanowire modified electrode in embodiment 1, this is owing to increasing along with nano wire film thickness, hindering the electron transmission of nitrite anions at electrode surface.
Embodiment 3
(1) Te overlong nanowire is synthesized: with embodiment 1
(2) taking Te overlong nanowire as templated synthesis Au overlong nanowire: with embodiment 1
(3) preparation of Au overlong nanowire modified electrode
Gained Au overlong nanowire is dissolved in the redistilled water of 20mL and obtains the Au overlong nanowire aqueous solution, 1mL5wt% naphthols is added in obtained aqueous solution, stir after evenly and obtain mixing solutions, get 3 μ L mixing solutionss and drip the glassy carbon electrode surface being coated onto and handling well, dry with infrared lamp, obtain Au overlong nanowire modified electrode;
Fig. 6 obtains Au overlong nanowire sensor to the cyclic voltammetry curve of 1mmol/L nitrite in the present embodiment. Wherein, a curve is bare electrode, and b curve is Au overlong nanowire modified electrode in embodiment 1, and c curve is the Au overlong nanowire modified electrode in embodiment 2, and d curve is the Au overlong nanowire modified electrode in the present embodiment. Same proof is along with the increase of nano wire film thickness, and peak current reduces.
Claims (3)
1. a preparation method for nano wire modified electrode, the method is gold Au overlong nanowire by templated synthesis of tellurium Te overlong nanowire, and its step is as follows:
Step 1, synthesis Te overlong nanowire
1.0g polyvinylpyrrolidone and 0.01g sodium tellurite are dissolved in 35mL redistilled water, ultrasonic disperse 1 hour, form stable solution, 1.65mL (40wt%) hydrazine hydrate and 3.35mL (28wt%) ammonia soln is added in solution, move in the reactor of teflon lined of 50mL after short mix, the retort furnace putting into 180 ° of C after being closed by reactor reacts 4 hours, after reaction terminates, room temperature cools 12 hours, the acetone of 80-200mL is added in cooling fluid, static 12-24 hour, centrifugal, Te overlong nanowire is obtained with after second distillation water washing five times,
Step 2, taking Te overlong nanowire as templated synthesis Au overlong nanowire
Take 10mgHAuCl4·4H2O is dissolved in 10mL distilled water, fully stirs and obtains 2.5mmol/LHAuCl4Solution;Taking 1.0mgTe overlong nanowire is scattered in the distilled water of 25mL, stirs after evenly and adds 1-5mL2.5mmol/LHAuCl4Solution and maintenance ultrasonic power 50-200w, ultrasonic reaction 20-60 minute, makes Te overlong nanowire HAuCl4Automatic by electric current displacement response generation Au overlong nanowire, product redistilled water is cleaned 5-10 time to remove remaining chlorauric acid solution after terminating by reaction, and in 50 DEG C of vacuum drying ovens, drying 6 hours, obtain Au overlong nanowire;
Step 3, the preparation of Au overlong nanowire modified electrode
Gained Au overlong nanowire is dissolved in the redistilled water of 20mL and obtains the Au overlong nanowire aqueous solution, 1mL5wt% naphthols is added in obtained aqueous solution, stir after evenly and obtain mixing solutions, get 1-5 μ L mixing solutions and drip the glassy carbon electrode surface being coated onto and handling well, dry with infrared lamp, obtain Au overlong nanowire modified electrode.
2. the preparation method of nano wire modified electrode according to claim 1, is characterized in that, the Au overlong nanowire of described modified electrode surface coverage, and length is 1-100 μm, and diameter is 20-50nm.
3. one kind utilizes the application of the Au overlong nanowire modified electrode described in claim 1 or 2 in nitrite detects.
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| CN107322007A (en) * | 2017-08-21 | 2017-11-07 | 南京师范大学 | A kind of preparation method of ultra-fine overlength Au nano wires |
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