CN110297021A - Bismuth dopen Nano SiC/carbon nanotube paste electrode sensor preparation method - Google Patents
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Abstract
The invention discloses a kind of preparation methods of bismuth dopen Nano SiC/ carbon nanotube paste electrode sensor, which is characterized in that uses 1- butyl -3- methylimidazole villaumite dissolution bismuth citrate and cellulose that light yellow viscous liquid is made and adulterates the glutinous agent of carbon containing quantum dispensing for bismuth;Then, in the agate mortar, nano SiC: 45 ~ 48%, oxide/carbon nanometer tube: 25 ~ 28%, bismuth doping carbon quantum dot adhesive: 10 ~ 14%, polyethylene glycol: 4 ~ 6%, ethyl alcohol: 8 ~ 12%, grinding uniformly adulterates carbon quantum dot mixture carbon paste to get nano SiC/carbon nanotube/bismuth;The loading of mixture carbon paste is connected with the interior of conducting wire to pass through in the glass tube for Φ 5mm to get bismuth dopen Nano SiC/ carbon nanotube paste electrode sensor.The advantages that electrode prepared by the application improves 4 ~ 6 times than common carbon paste electrode electric conductivity, and electrochemical window mouth width, preparation method are simple, surface easily updates, aftercurrent is small.Detection sensitivity is high, and selectivity is good.
Description
Technical field
The present invention relates to a kind of preparation method of electrochemical sensor, in particular to a kind of bismuth dopen Nano SiC/carbon is received
The preparation method and application of mitron paste electrode sensor.Belong to electrochemical analysis field.
Background technique
By sp3 hydridization covalent bond between Si-C in silicon carbide, Si-C bond energy is very strong, and SiC is made to have many advantageous properties,
Such as wear-resisting, high mechanical strength, hardness is big, chemical property is stable, corrosion-resistant, thermal stability, high temperature resistant, background current is small, interferes
Small, excellent semiconductor material, therefore silicon carbide has very big application value, it is wide in many fields such as optics, electricity, machinery
General application, it is ideal carrier material.Since carbon atom takes SP in carbon nanotube (CNTs)2Hydridization compares SP3Hydridization,
SP2S orbital composition is bigger in hydridization, and carbon nanotube is made to have high-modulus and high intensity.The P electronics of carbon atom in carbon nanotube
Large-scale delocalized pi-bond is formed, since conjugation is significant, carbon nanotube has some special electrical properties.When CNTs's
When caliber is greater than 6nm, electric conductivity decline;When caliber is less than 6nm, CNTs can be seen as having the one of excellent conductive performance
Tie up quantum wire.In addition, carbon nanotube is overlapping with the compound also inhibition carbon nanotubes lamella of other nanostructures.By high capacity
Silicon carbide or conducting polymer and carbon nanotube carry out that lamination is compound, and one side carbon nanotube is kept apart by other substances, energy
Enough reduce is reunited, and the mobility of electrolyte is increased, on the other hand, carbon nanotube be it is compound after fake capacitance substance provide electronics
The three-dimensional network of conduction.Composite material exhibits based on carbon nanotube go out synergistic effect, maintain while obtaining high capacity
Good high rate performance.
Carbon paste electrode is the Carbon Materials using electric conductivity, if the adhesive of graphite powder and hydrophobicity is mixed and made into paste,
Then it is coated in the surface of electrode bar or is packed into electrode tube and manufactured a kind of electrode.Since carbon paste electrode is nontoxic, electric
The advantages that chemical window is wide, preparation method is simple, at low cost, surface easily updates, aftercurrent is small, is widely used to electrochemistry
In analysis, biosensor preparation and environment measuring, food and medicine analysis.But there is also some disadvantages for carbon paste electrode, such as conductive
Performance is poor, and sensitivity is low, stability difference etc..In order to improve the performance of carbon paste electrode, using nanometer TiB2/ carbon nanotube is compound
Conductive material of the material as carbon paste electrode dissolves cellulose and bismuth citrate conduct using 1- butyl -3- methylimidazole villaumite
Adhesive substantially improves the performance of electrode.1- butyl -3- methylimidazole villaumite is that have completely from molecular at room temperature in liquid
The salt of state has many advantages, such as that property is stable, electric conductivity is excellent and electrochemical window mouth width, is widely used in material, synthesis, life
The fields such as object catalysis and separating and extracting.Ionic liquid accelerates electron transfer rate, improves electrode sensitivity and selectivity.
For quantitative detection cephalosporins, reach to high sensitivity, selectivity required by drug test
The good, demands such as detection time is short.
Summary of the invention
The purpose of the application is using 1- butyl -3- methylimidazole villaumite dissolution cellulose and bismuth citrate as gluing
Agent, silicon carbide and carbon nanotube prepare a kind of bismuth dopen Nano SiC/carbon nanotube paste electrode sensor as conductive material, mention
Bismuth dopen Nano SiC/carbon nanotube paste electrode sensor preparation method is supplied, and in application detection drug.
Instrument and reagent
CHI660B electrochemical workstation (Shanghai Chen Hua instrument company), experiment use three-electrode system: platinum electrode is auxiliary electricity
Pole, Ag/AgCl are reference electrode (SCE), and bismuth dopen Nano SiC/carbon nanotube paste electrode sensor is working electrode;KQ-
250E type ultrasonic cleaner (Kun Feng ultrasonic instrument Co., Ltd).
Nano SiC, oxide/carbon nanometer tube, 1- butyl -3- methylimidazole villaumite, dehydrated alcohol, sulfuric acid, hydrochloric acid, citric acid
Bismuth, cellulose, Macrogol 600, agents useful for same are that analysis is pure, and water is deionized water.
The purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method of bismuth dopen Nano SiC/carbon nanotube paste electrode sensor, which is characterized in that this method tool
There is following processing step:
(1) bismuth adulterates carbon containing quantum dispensing and sticks agent: in a kettle, being added by following mass percent, 1- butyl -3- methyl miaow
Azoles villaumite: 81 ~ 85%, bismuth citrate: 4 ~ 6%, cellulose: 10 ~ 14%, it stirs evenly, the sum of each component mass percent is percentage
Hundred, sealing, be placed in 120 ± 2 DEG C of baking ovens, 8 ~ 10h of isothermal reaction is cooled to room temperature and mixes to get light yellow viscous liquid for bismuth
Miscellaneous carbon containing quantum dispensing sticks agent;
(2) nano SiC/carbon nanotube/bismuth doping carbon quantum dot mixture carbon paste preparation: in the agate mortar, by following matter
It measures percentage to be added, nano SiC: 45 ~ 48%, oxide/carbon nanometer tube: 25 ~ 28%, bismuth doping carbon quantum dot adhesive: 10 ~ 14%,
Polyethylene glycol: 4 ~ 6%, ethyl alcohol: 8 ~ 12%, the sum of each component mass percent is absolutely, to grind uniformly to get nano SiC
/ carbon nanotube/bismuth adulterates carbon quantum dot mixture carbon paste;
(3) bismuth dopen Nano SiC/carbon nanotube paste electrode sensor preparation: the loading of step (2) mixture carbon paste is connected with
In the interior glass tube through being Φ 5mm of conducting wire, gas is excluded, is compacted, it is dry, it is polished, is polished with abrasive paper for metallograph, deionized water,
Ethanol washing is to get bismuth dopen Nano SiC/carbon nanotube paste electrode sensor.
Oxide/carbon nanometer tube described in step (2) is that multi-walled carbon nanotube caliber is less than 6nm.
Polyethylene glycol described in step (2) is Macrogol 600.
Bismuth dopen Nano SiC/steps are as follows for carbon nanotube paste electrode sensor measurement cefalexin:
(1) standard solution is prepared: preparing the cefalexin standard solution of one group of various concentration including blank standard specimen, bottom liquid
For 2.2mol/L HCl solution;
It (2) is reference electrode by Ag/AgCl, platinum electrode is auxiliary electrode, nanometer TiB prepared by the present invention2/ carbon nanotube
Composite paste electrode forms three-electrode system, connects CHI660B electrochemical workstation, and bottom liquid is 2.2mol/L HCl solution ,-
The potential range of 1.2 ~ 1.6V,.Then the solution is scanned using chronoamperometry, operating voltage is -0.52V, takes various concentration
The peak point current of lower cefalexin and cefalexin concentration are worked curve;This method shows very highly selective and sensitivity,
The concentration of response current and cefalexin is 4.0 × 10-8~8.0×10-4It is in good linear relationship within the scope of mol/L, it is related
Coefficients R=0.9989, detection are limited to 1.68 × 10-8mol/L;
(3) detection of cefalexin: the cefalexin standard solution in step (1) is replaced with sample to be tested, according to step (2)
Method is detected, according to response the difference of current reduction△IAnd working curve, obtain containing for cefalexin in sample to be tested
Amount, the rate of recovery is between 95.12 ~ 103.26%.
Advantages of the present invention and effect are:
(1) present invention prepares bismuth dopen Nano SiC/carbon nanotube paste electrode sensor, and silicon carbide is added in carbon paste electrode,
Bismuth citrate and cellulose are dissolved using 1- butyl -3- methylimidazole villaumite bismuth doping are made contain carbon quantum dot as adhesive,
The carbon paste electrode that silicon carbide and oxide/carbon nanometer tube are mixed with improves 4 ~ 6 times than common carbon paste electrode electric conductivity, electricity
The advantages that chemical window is wide, preparation method is simple, at low cost, surface easily updates, aftercurrent is small;
(2) present invention prepares bismuth dopen Nano SiC/carbon nanotube paste electrode sensor during preparation without using toxic
Reagent, environment-friendly and green prepared simple and easy;
(3) present invention is prepared into bismuth dopen Nano SiC/carbon nanotube paste electrode sensor and is used successfully to drug, biological sample head
It in the detection of cefalexin, solves cefalexin detection difficult, improves the sensitivity of detection.
Specific embodiment
Embodiment 1
(1) bismuth adulterates carbon containing quantum dispensing and sticks agent: it in a kettle, is separately added into, 1- butyl -3- methylimidazole villaumite: 83g,
Bismuth citrate: 5g, cellulose: 12g is stirred evenly, and sealing is placed in 120 ± 2 DEG C of baking ovens, and isothermal reaction 9h is cooled to room temperature,
It is that bismuth adulterates the glutinous agent of carbon containing quantum dispensing up to light yellow viscous liquid;
(2) preparation of nano SiC/carbon nanotube/bismuth doping carbon quantum dot mixture carbon paste: in the agate mortar, respectively plus
Enter, nano SiC: 46g, oxide/carbon nanometer tube: 27g, bismuth adulterate carbon quantum dot adhesive: 12g, polyethylene glycol: 5g, ethyl alcohol: 13
ML, grinding uniformly adulterate carbon quantum dot mixture carbon paste to get nano SiC/carbon nanotube/bismuth;
(3) bismuth dopen Nano SiC/carbon nanotube paste electrode sensor preparation: the loading of step (2) mixture carbon paste is connected with
In the interior glass tube through being Φ 5mm of conducting wire, gas is excluded, is compacted, it is dry, it is polished, is polished with abrasive paper for metallograph, deionized water,
Ethanol washing is to get bismuth dopen Nano SiC/carbon nanotube paste electrode sensor.
Embodiment 1
(1) bismuth adulterates carbon containing quantum dispensing and sticks agent: it in a kettle, is separately added into, 1- butyl -3- methylimidazole villaumite: 84g,
Bismuth citrate: 6g, cellulose: 10g is stirred evenly, and sealing is placed in 120 ± 2 DEG C of baking ovens, and isothermal reaction 8h is cooled to room temperature,
It is that bismuth adulterates the glutinous agent of carbon containing quantum dispensing up to light yellow viscous liquid;
(2) preparation of nano SiC/carbon nanotube/bismuth doping carbon quantum dot mixture carbon paste: in the agate mortar, respectively plus
Enter, nano SiC: 48g, oxide/carbon nanometer tube: 25g, bismuth adulterate carbon quantum dot adhesive: 10g, polyethylene glycol: 6g, ethyl alcohol:
14mL, grinding uniformly adulterate carbon quantum dot mixture carbon paste to get nano SiC/carbon nanotube/bismuth;
(3) bismuth dopen Nano SiC/carbon nanotube paste electrode sensor preparation: the loading of step (2) mixture carbon paste is connected with
In the interior glass tube through being Φ 5mm of conducting wire, gas is excluded, is compacted, it is dry, it is polished, is polished with abrasive paper for metallograph, deionized water,
Ethanol washing is to get bismuth dopen Nano SiC/carbon nanotube paste electrode sensor.
Embodiment 3
(1) bismuth adulterates carbon containing quantum dispensing and sticks agent: it in a kettle, is separately added into, 1- butyl -3- methylimidazole villaumite: 82g,
Bismuth citrate: 4g, cellulose: 14g is stirred evenly, and sealing is placed in 120 ± 2 DEG C of baking ovens, and isothermal reaction 10h is cooled to room temperature,
It is that bismuth adulterates the glutinous agent of carbon containing quantum dispensing up to light yellow viscous liquid;
(2) preparation of nano SiC/carbon nanotube/bismuth doping carbon quantum dot mixture carbon paste: in the agate mortar, respectively plus
Enter, nano SiC: 45g, oxide/carbon nanometer tube: 28g, bismuth adulterate carbon quantum dot adhesive: 14g, polyethylene glycol: 4g, ethyl alcohol:
11mL, grinding uniformly adulterate carbon quantum dot mixture carbon paste to get nano SiC/carbon nanotube/bismuth;
(3) bismuth dopen Nano SiC/carbon nanotube paste electrode sensor preparation: the loading of step (2) mixture carbon paste is connected with
In the interior glass tube through being Φ 5mm of conducting wire, gas is excluded, is compacted, it is dry, it is polished, is polished with abrasive paper for metallograph, deionized water,
Ethanol washing is to get bismuth dopen Nano SiC/carbon nanotube paste electrode sensor.
Embodiment 4
(1) bismuth adulterates carbon containing quantum dispensing and sticks agent: it in a kettle, is separately added into, 1- butyl -3- methylimidazole villaumite: 85g,
Bismuth citrate: 4g, cellulose: 11g is stirred evenly, and sealing is placed in 120 ± 2 DEG C of baking ovens, isothermal reaction 8.5h is cooled to room
Temperature is that bismuth adulterates the glutinous agent of carbon containing quantum dispensing to get light yellow viscous liquid;
(2) preparation of nano SiC/carbon nanotube/bismuth doping carbon quantum dot mixture carbon paste: in the agate mortar, respectively plus
Enter, nano SiC: 47g, oxide/carbon nanometer tube: 26g, bismuth adulterate carbon quantum dot adhesive: 11g, polyethylene glycol: 4g, ethyl alcohol: 15
ML, grinding uniformly adulterate carbon quantum dot mixture carbon paste to get nano SiC/carbon nanotube/bismuth;
(3) bismuth dopen Nano SiC/carbon nanotube paste electrode sensor preparation: the loading of step (2) mixture carbon paste is connected with
In the interior glass tube through being Φ 5mm of conducting wire, gas is excluded, is compacted, it is dry, it is polished, is polished with abrasive paper for metallograph, deionized water,
Ethanol washing is to get bismuth dopen Nano SiC/carbon nanotube paste electrode sensor.
Bismuth dopen Nano SiC/carbon nanotube paste electrode sensor prepared by the present invention is used successfully to drug, biological sample
In the detection of middle cefalexin, therefore sensor prepared by the present invention can be widely applied to biological medicine, biology sample detection etc.
Related fields solves the difficulty of cefalexin detection.
Claims (4)
1. a kind of preparation method of bismuth dopen Nano SiC/carbon nanotube paste electrode sensor, which is characterized in that this method tool
There is following processing step:
(1) bismuth adulterates carbon containing quantum dispensing and sticks agent: in a kettle, being added by following mass percent, 1- butyl -3- methyl miaow
Azoles villaumite: 81 ~ 85%, bismuth citrate: 4 ~ 6%, cellulose: 10 ~ 14%, it stirs evenly, the sum of each component mass percent is percentage
Hundred, sealing, be placed in 120 ± 2 DEG C of baking ovens, 8 ~ 10h of isothermal reaction is cooled to room temperature and mixes to get light yellow viscous liquid for bismuth
Miscellaneous carbon containing quantum dispensing sticks agent;
(2) nano SiC/carbon nanotube/bismuth doping carbon quantum dot mixture carbon paste preparation: in the agate mortar, by following matter
It measures percentage to be added, nano SiC: 45 ~ 48%, oxide/carbon nanometer tube: 25 ~ 28%, bismuth doping carbon quantum dot adhesive: 10 ~ 14%,
Polyethylene glycol: 4 ~ 6%, ethyl alcohol: 8 ~ 12%, the sum of each component mass percent is absolutely, to grind uniformly to get nano SiC
/ carbon nanotube/bismuth adulterates carbon quantum dot mixture carbon paste;
(3) bismuth dopen Nano SiC/carbon nanotube paste electrode sensor preparation: the loading of step (2) mixture carbon paste is connected with
In the interior glass tube through being Φ 5mm of conducting wire, gas is excluded, is compacted, it is dry, it is polished, is polished with abrasive paper for metallograph, deionized water,
Ethanol washing is to get bismuth dopen Nano SiC/carbon nanotube paste electrode sensor.
2. a kind of preparation method of bismuth dopen Nano SiC/carbon nanotube paste electrode sensor according to claim 1,
It is characterized in that, oxide/carbon nanometer tube described in step (2) is that multi-walled carbon nanotube caliber is less than 6nm.
3. a kind of preparation method of bismuth dopen Nano SiC/carbon nanotube paste electrode sensor according to claim 1,
It is characterized in that, polyethylene glycol described in step (2) is Macrogol 600.
4. a kind of preparation method institute of bismuth dopen Nano SiC/carbon nanotube paste electrode sensor according to claim 1
Bismuth dopen Nano SiC/carbon nanotube paste electrode sensor of preparation.
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