CN104089980A - Preparation method of benzene sensor based on anodic alumina nanowire - Google Patents
Preparation method of benzene sensor based on anodic alumina nanowire Download PDFInfo
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Abstract
The invention relates to a preparation method of a benzene sensor based on an anodic alumina nanowire. The benzene sensor electrode is coated with the anodic alumina nanowire. The preparation method includes pretreatment, oxidation, surface modification, and sensor preparation. The sensor provided by the invention has the characteristics of low cost, rapid response, short desorption time, good repeatability and high accuracy. Preparation of the sensor has the advantages of simple process, low material consumption, high process repeatability and controllability, and is convenient for batch production.
Description
Technical field
The present invention relates to sensor technical field, particularly a kind ofly respond fast, accuracy is high, the preparation method of the benzene sensor based on anodised aluminium nano wire of favorable repeatability.
Background technology
Benzene is a kind of colourless, pleasantly sweet transparency liquid at normal temperatures, and has strong aromatic odor.Benzene is flammable, poisonous, is also a kind of carcinogen.Benzene is that a kind of hydrocarbon is also the simplest aromatic hydrocarbons.It is insoluble in water, is soluble in organic solvent, and itself also can be used as organic solvent.Benzene produces paralysis effect to central nervous system, causes acute poisoning.Severe one there will be headache, feels sick, vomiting, in a certain state of delirium, unconsciousness, stupor, tic etc., and severe patient can be dead because of cental system paralysis.A small amount of benzene also can make people produce the phenomenons such as sleepiness, giddy, heart rate are accelerated, have a headache, trembled, Bewu βtseinstrubung, obnubilation.Take in containing the too much food of benzene and can cause the symptoms such as vomiting, stomachache, giddy, insomnia, tic, heart rate quickening, even dead.Because the volatility of benzene is large, be exposed in air and be easy to spread.Therefore how of crucial importance to the detection benzene of benzene rapidly.Mainly rely at present the method for instrumental analysis for Low Concentration of Benzene detection method, as vapor-phase chromatography etc.Although these detections are the concentration of micro-benzene in testing environment accurately, the deficiencies such as but these method ubiquity sense cycle are long, cost is expensive, and, need to, through those of skill in the art's operating instrument equipment of professional training, cannot realize the accurate fast detecting in the scene of micro-benzene in environment.
Chinese patent publication No. CN102021219A, date of publication on April 20th, 2011, name is called the Microbial cell-based biosensors that detects toluene class organic contaminant, this application case discloses a kind of Microbial cell-based biosensors that detects toluene class organic contaminant, utilize regulating and controlling sequence and the regulatory protein gene of pseudomonas putida degrading genes to follow commercialization reporter plasmid sequence, build the Microbial cell-based biosensors and the detection method that detect toluene class organic contaminant, bacterial host is Escherichia coli.Its weak point is, this detection method sense cycle is long, cost is expensive.
Summary of the invention
The object of the invention is to that method sense cycle in order to solve existing detection benzene is long, cost is expensive and need to be through those of skill in the art's operating instrument equipment of professional training, cannot realize micro-benzene in environment the accurate fast detecting in scene defect and provide a kind of and respond fast, accuracy is high, the preparation method of the benzene sensor based on anodised aluminium nano wire of favorable repeatability.
To achieve these goals, the present invention is by the following technical solutions:
A preparation method for benzene sensor based on anodised aluminium nano wire, described preparation method comprises the following steps:
A) pre-treatment: 6-8h that aluminium sheet is annealed at 220-320 DEG C, cooling rear cleaning degrease, then immerses in soak solution, and soak solution temperature is 35-50 DEG C, and soak time is 10-30min; Taking-up is carried out electrochemical polish after cleaning;
B) oxidation: the aluminium sheet that step a) is obtained carries out anodic oxidation, in oxidation solution, be oxidized, oxidation voltage 40V, oxidization time 15-25min, before finishing, oxidation reduces the speed of 3V oxidation voltage in 50s with every 5s, oxidation voltage is down to 10-12V, and after taking-up, putting into massfraction is the phosphoric acid solution reaming of 7-10%, obtains anodic oxidation aluminium sheet;
C) finishing: the anodic oxidation aluminium sheet that step b) is obtained is washed till pH for neutral, then carries out electroplating processes in copper plating bath, time 5-10min; Electroplate rear taking-up, at 600-700 DEG C, dried 25-35min; Anodic oxidation aluminium sheet after copper facing is placed in to alkaline solution 8-10h, obtain anodised aluminium nano-material, then be configured to 5mg/mL anodised aluminium nanowire suspension with deionized water, in anode alumina nanowires suspension, add palladium bichloride, titania or iron oxide, ultrasonic concussion, then drying for standby when adding;
D) prepare sensor: the anodised aluminium nano wire after step c) is modified is coated on sensor electrode, and the number of plies that anodised aluminium nano wire applies is 3-5 layer.
In the technical program, anodised aluminium nano-material own wt is light, and therefore the sensor of preparation has superiority in weight, is conducive to be fixed on different positions compared with the sensor of lightweight, is easy to use; Anodised aluminium nano-material is not yielding and broken, can keep the shape maintains of sensor constant; Anodised aluminium nano-material has the feature of porous, is therefore conducive to tested gas permeation and enters, and increases the suction-operated of anodised aluminium nano-material for tested gas molecule, increases and detects effect; Anodised aluminium nano-material has good compatibility, can and be plated between its surperficial metal and produces affinity, is therefore plated in its surperficial metal difficult drop-off, has increased the stability of sensor construction; Anodised aluminium nano-material also has fabulous electrical insulating property, it is hereby ensured that electrode normally works in a good dielectric base; Anodised aluminium nano-material is easy to preparation, and favorable repeatability, is convenient to large quantities of preparations;
Step b) adopts step-down processing before the end of oxidation, can reduce the thickness of anodised aluminium surface barrier, if do not take step-down processing, barrier layer thickness is 50 microns of left and right, and takes step-down processing of the present invention, and the thickness on restraining barrier is 18 microns of left and right;
Reaming is the diameter in order to increase the hole on alumina formwork, also makes the diameter homogenization more of hole simultaneously, is conducive to improve the dielectricity of anodic oxidation aluminium formwork, thereby improves the sensitivity and the accuracy that detect, increases the stability of sensor construction; If not reaming, the hole diameter on alumina formwork is not of uniform size, and this must reduce stability and the dielectricity of sensor construction, reduces detection sensitivity and accuracy; Pore-enlargement is too short, falls flat, and via hole overlong time, can reduce the degree of adhering to of noble metal on porous anodic alumina template.
As preferably, in step a), cleaning degrease solution used is the mixed liquor of ethanol and cyclohexanol, and the volume ratio of ethanol and cyclohexanol is 1:2-4, uses vibration of ultrasonic wave cleansing solution when cleaning; Soak solution is the sodium bicarbonate of massfraction 10-15% and the potassium hydroxide mixed solution that massfraction is 2-4%, and the volume ratio of sodium bicarbonate and potassium hydroxide is 1:2-5.
As preferably, in step b), oxidation solution is that mass concentration is the mixed solution of the citric acid of 8-10%, succinic acid that mass concentration is 0.3-0.5% and the mass concentration potassium permanganate that is 0.9-1.5%.
As preferably, in step b), pore-enlargement is 30-45min, and the temperature of phosphoric acid solution is 50-55 DEG C.
As preferably, step c) neutral and alkali solution is the mixed solution of NaOH and cupric chloride; In every 1mL anodised aluminium nanowire suspension, add 1mg palladium bichloride, titania or iron oxide; The composition of copper plating bath is: the rare earth oxide of 1-butyl-3-methylimidazole paratoluenesulfonic acid sodium salt, 33-38g/L potassium tartrate and the 4.8-7.3g/L of 20-24g/L cupric chloride, 0.1-0.8g/L nickel chloride, 45-65mg/L polyglycol, 1.2-3.6g/L.
As preferably, in alkaline solution, the mass concentration of NaOH and cupric chloride is respectively: NaOH 5-7% and cupric chloride 10-12%.
As preferably, ultrasonic processing 55-65W.
As preferably, aluminium sheet adopts high-purity aluminium sheet of purity >=99.999%.
As preferably, when electroplating processes, adopt two electrolytic tanks, utilize three-electrode system, auxiliary electrode is iridium tantalum titanium electrode, and contrast electrode is saturated calomel electrode SCE, and working electrode is the anodic oxidation aluminium sheet of bottom spray platinum.
The invention has the beneficial effects as follows:
1) sensor cost of the present invention is low, and fast, desorption time is short in response, favorable repeatability, and accuracy is high;
2) preparation process of sensor of the present invention is simple, and material consumption is few, and the repeatability of technique and controllability are very high, is convenient to batch production.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the anodic oxidation aluminium sheet prepared of embodiment 1.
Fig. 2 is the scanning electron microscope (SEM) photograph of the anodised aluminium nano wire prepared of embodiment 1.
Fig. 3 is benzene concentration detection model.
Embodiment
Below in conjunction with specific embodiment and accompanying drawing, the present invention will be further explained:
Embodiment 1
A preparation method for benzene sensor based on anodised aluminium nano wire, described preparation method comprises the following steps:
A) pre-treatment: just high-purity aluminium sheet of purity >=99.999% 8h that anneals at 220 DEG C, cooling rear cleaning degrease, then immerses in soak solution, and soak solution temperature is 35 DEG C, and soak time is 30min; After taking out and cleaning, after taking out and cleaning, in the ethanol that is 2:1 in volume ratio and perchloric acid mixed solution, (Ra≤0.01 μ m) carries out electrochemical polish 5min; Cleaning degrease solution used is the mixed liquor of ethanol and cyclohexanol, and the volume ratio of ethanol and cyclohexanol is 1:2, uses vibration of ultrasonic wave cleansing solution when cleaning; Soak solution is the sodium bicarbonate of massfraction 10% and the potassium hydroxide mixed solution that massfraction is 2%, and the volume ratio of sodium bicarbonate and potassium hydroxide is 1:2; Ultrasonic processing 55W;
B) oxidation: the aluminium sheet that step a) is obtained carries out anodic oxidation, in oxidation solution, be oxidized, oxidation voltage 40V, oxidization time 15min, before finishing, oxidation reduces the speed of 3V oxidation voltage in 50s with every 5s, oxidation voltage is down to 10V, after taking-up, puts into massfraction and be 7% phosphoric acid solution reaming, obtain anodic oxidation aluminium sheet; Pore-enlargement is 30min, and the temperature of phosphoric acid solution is 55 DEG C; Oxidation solution is the mixed solution of mass concentration is 8% citric acid, mass concentration is 0.3% succinic acid and the mass concentration potassium permanganate that is 0.9%;
C) finishing: the anodic oxidation aluminium sheet that step b) is obtained is washed till pH for neutral, then carries out electroplating processes in copper plating bath, time 5min; Electroplate rear taking-up, at 600 DEG C, dried 35min; Anodic oxidation aluminium sheet after copper facing is placed in to alkaline solution 8h, obtain anodised aluminium nano-material, then be configured to 5mg/mL anodised aluminium nanowire suspension with deionized water, in anode alumina nanowires suspension, add palladium bichloride, ultrasonic concussion, then drying for standby when adding; Wherein, alkaline solution is the mixed solution of mass concentration 5% NaOH and mass concentration 10% cupric chloride; In every 1mL anodised aluminium nanowire suspension, add 1mg palladium bichloride; The composition of copper plating bath is: the cerium oxide of 1-butyl-3-methylimidazole paratoluenesulfonic acid sodium salt, 33g/L potassium tartrate and the 4.8g/L of 20g/L cupric chloride, 0.1g/L nickel chloride, 45mg/L polyglycol, 1.2g/L; When electroplating processes, adopt two electrolytic tanks, utilize three-electrode system, auxiliary electrode is iridium tantalum titanium electrode, and contrast electrode is saturated calomel electrode SCE, and working electrode is the anodic oxidation aluminium sheet of bottom spray platinum; Ultrasonic processing 55W;
D) prepare sensor: the anodised aluminium nano wire after step c) is modified is coated on sensor electrode, and the number of plies that anodised aluminium nano wire applies is 3 layers.
Embodiment 2
A preparation method for benzene sensor based on anodised aluminium nano wire, described preparation method comprises the following steps:
A) pre-treatment: just high-purity aluminium sheet of purity >=99.999% 7h that anneals at 280 DEG C, cooling rear cleaning degrease, then immerses in soak solution, and soak solution temperature is 45 DEG C, and soak time is 20min; After taking out and cleaning, after taking out and cleaning, in the ethanol that is 2:1 in volume ratio and perchloric acid mixed solution, (Ra≤0.01 μ m) carries out electrochemical polish 5min; Cleaning degrease solution used is the mixed liquor of ethanol and cyclohexanol, and the volume ratio of ethanol and cyclohexanol is 1:3, uses vibration of ultrasonic wave cleansing solution when cleaning; Soak solution is the sodium bicarbonate of massfraction 12% and the potassium hydroxide mixed solution that massfraction is 3%, and the volume ratio of sodium bicarbonate and potassium hydroxide is 1:3; Ultrasonic processing 60W;
B) oxidation: the aluminium sheet that step a) is obtained carries out anodic oxidation, in oxidation solution, be oxidized, oxidation voltage 40V, oxidization time 20min, before finishing, oxidation reduces the speed of 3V oxidation voltage in 50s with every 5s, oxidation voltage is down to 12V, after taking-up, puts into massfraction and be 8.5% phosphoric acid solution reaming, obtain anodic oxidation aluminium sheet; Pore-enlargement is 40min, and the temperature of phosphoric acid solution is 52 DEG C; Oxidation solution is the mixed solution of mass concentration is 9% citric acid, mass concentration is 0.4% succinic acid and the mass concentration potassium permanganate that is 1.2%;
C) finishing: the anodic oxidation aluminium sheet that step b) is obtained is washed till pH for neutral, then carries out electroplating processes in copper plating bath, time 8min; Electroplate rear taking-up, at 650 DEG C, dried 30min; Anodic oxidation aluminium sheet after copper facing is placed in to alkaline solution 9h, obtain anodised aluminium nano-material, then be configured to 5mg/mL anodised aluminium nanowire suspension with deionized water, in anode alumina nanowires suspension, add titania, ultrasonic concussion, then drying for standby when adding; Wherein, alkaline solution is the mixed solution of mass concentration 6% NaOH and mass concentration 11% cupric chloride; In every 1mL anodised aluminium nanowire suspension, add 1mg titania; The composition of copper plating bath is: the praseodymium oxide of 1-butyl-3-methylimidazole paratoluenesulfonic acid sodium salt, 35g/L potassium tartrate and the 5.3g/L of 22g/L cupric chloride, 0.5g/L nickel chloride, 50mg/L polyglycol, 2.4g/L; When electroplating processes, adopt two electrolytic tanks, utilize three-electrode system, auxiliary electrode is iridium tantalum titanium electrode, and contrast electrode is saturated calomel electrode SCE, and working electrode is the anodic oxidation aluminium sheet of bottom spray platinum; Ultrasonic processing 60W;
D) prepare sensor: the anodised aluminium nano wire after step c) is modified is coated on sensor electrode, and the number of plies that anodised aluminium nano wire applies is 4 layers.
Embodiment 3
A preparation method for benzene sensor based on anodised aluminium nano wire, described preparation method comprises the following steps:
A) pre-treatment: just high-purity aluminium sheet of purity >=99.999% 6h that anneals at 320 DEG C, cooling rear cleaning degrease, then immerses in soak solution, and soak solution temperature is 50 DEG C, and soak time is 10min; After taking out and cleaning, after taking out and cleaning, in the ethanol that is 2:1 in volume ratio and perchloric acid mixed solution, (Ra≤0.01 μ m) carries out electrochemical polish 5min; Cleaning degrease solution used is the mixed liquor of ethanol and cyclohexanol, and the volume ratio of ethanol and cyclohexanol is 1:4, uses vibration of ultrasonic wave cleansing solution when cleaning; Soak solution is the sodium bicarbonate of massfraction 15% and the potassium hydroxide mixed solution that massfraction is 4%, and the volume ratio of sodium bicarbonate and potassium hydroxide is 1:5; Ultrasonic processing 65W;
B) oxidation: the aluminium sheet that step a) is obtained carries out anodic oxidation, in oxidation solution, be oxidized, oxidation voltage 40V, oxidization time 25min, before finishing, oxidation reduces the speed of 3V oxidation voltage in 50s with every 5s, oxidation voltage is down to 10V, after taking-up, puts into massfraction and be 7% phosphoric acid solution reaming, obtain anodic oxidation aluminium sheet; Pore-enlargement is 45min, and the temperature of phosphoric acid solution is 50 DEG C; Oxidation solution is the mixed solution of mass concentration is 10% citric acid, mass concentration is 0.5% succinic acid and the mass concentration potassium permanganate that is 1.5%;
C) finishing: the anodic oxidation aluminium sheet that step b) is obtained is washed till pH for neutral, then carries out electroplating processes in copper plating bath, time 10min; Electroplate rear taking-up, at 700 DEG C, dried 25min; Anodic oxidation aluminium sheet after copper facing is placed in to alkaline solution 10h, obtain anodised aluminium nano-material, then be configured to 5mg/mL anodised aluminium nanowire suspension with deionized water, in anode alumina nanowires suspension, add iron oxide, ultrasonic concussion, then drying for standby when adding; Wherein, alkaline solution is the mixed solution of mass concentration 7% NaOH and mass concentration 12% cupric chloride; In every 1mL anodised aluminium nanowire suspension, add 1mg iron oxide; The composition of copper plating bath is: the lanthana of 1-butyl-3-methylimidazole paratoluenesulfonic acid sodium salt, 38g/L potassium tartrate and the 7.3g/L of 24g/L cupric chloride, 0.8g/L nickel chloride, 65mg/L polyglycol, 3.6g/L; When electroplating processes, adopt two electrolytic tanks, utilize three-electrode system, auxiliary electrode is iridium tantalum titanium electrode, and contrast electrode is saturated calomel electrode SCE, and working electrode is the anodic oxidation aluminium sheet of bottom spray platinum; Ultrasonic processing 65W;
D) prepare sensor: the anodised aluminium nano wire after step c) is modified is coated on sensor electrode, and the number of plies that anodised aluminium nano wire applies is 5 layers.
Anodic oxidation aluminium sheet prepared by embodiment 1 does electron-microscope scanning, the results are shown in Figure 1; Anodised aluminium nano wire prepared by embodiment 1 does electron-microscope scanning, the results are shown in Figure 2;
Select electric current-time (i-t) analytic function under the constant voltage of CHI660 electrochemical analyser, by the reference electrode of CHI electrochemical analyser with electrode is connect to one end of sensor electrode, working electrode connects the other end of sensor electrode, and test voltage is constant is 0.1V.It is stable to sensor response that the response time of sensor is set as being exposed to benzene gas from sensor, and secondary response is stable to be again set as being blown into sensor from drying nitrogen release time.All experiments are all at room temperature carried out.Adopt successively sensor prepared by embodiment 1-3 to concentration be respectively 180,150,120,90,60, the benzene gas of 30ppm detects, between every two concentration in testing process, all pass into high pure nitrogen sensor air chamber is cleaned, make sensor response return to baseline value.Then adopt the response of electric current-time curve method survey sensor to benzene gas, prepared sensor all has sensitive response to the benzene gas of variable concentrations, pass into benzene gas in air chamber after, its electric conductivity has been produced to impact, the electric current that benzene gas concentration is passed through is more greatly less.Relation between detection electric current and benzene gas concentration as shown in Figure 3, obtains sensor according to Fig. 3 through linear fit and detects the relation between electric current and benzene gas concentration, and physical relationship formula is:
, R=0.9812, utilizes this formula, and we just can detect electric current according to sensor and realize the detection to tested benzene sample.
Claims (9)
1. a preparation method for the benzene sensor based on anodised aluminium nano wire, is characterized in that, described preparation method comprises the following steps:
A) pre-treatment: 6-8h that aluminium sheet is annealed at 220-320 DEG C, cooling rear cleaning degrease, then immerses in soak solution, and soak solution temperature is 35-50 DEG C, and soak time is 10-30min; Taking-up is carried out electrochemical polish after cleaning;
B) oxidation: the aluminium sheet that step a) is obtained carries out anodic oxidation, in oxidation solution, be oxidized, oxidation voltage 40V, oxidization time 15-25min, before finishing, oxidation reduces the speed of 3V oxidation voltage in 50s with every 5s, oxidation voltage is down to 10-12V, and after taking-up, putting into massfraction is the phosphoric acid solution reaming of 7-10%, obtains anodic oxidation aluminium sheet;
C) finishing: the anodic oxidation aluminium sheet that step b) is obtained is washed till pH for neutral, then carries out electroplating processes in copper plating bath, time 5-10min; Electroplate rear taking-up, at 600-700 DEG C, dried 25-35min; Anodic oxidation aluminium sheet after copper facing is placed in to alkaline solution 8-10h, obtain anodised aluminium nano-material, then be configured to 5mg/mL anodised aluminium nanowire suspension with deionized water, in anode alumina nanowires suspension, add palladium bichloride, titania or iron oxide, ultrasonic concussion, then drying for standby when adding;
D) prepare sensor: the anodised aluminium nano wire after step c) is modified is coated on sensor electrode, and the number of plies that anodised aluminium nano wire applies is 3-5 layer.
2. the preparation method of a kind of benzene sensor based on anodised aluminium nano wire according to claim 1, it is characterized in that, in step a), cleaning degrease solution used is the mixed liquor of ethanol and cyclohexanol, the volume ratio of ethanol and cyclohexanol is 1:2-4, uses vibration of ultrasonic wave cleansing solution when cleaning; Soak solution is the sodium bicarbonate of massfraction 10-15% and the potassium hydroxide mixed solution that massfraction is 2-4%, and the volume ratio of sodium bicarbonate and potassium hydroxide is 1:2-5.
3. the preparation method of a kind of benzene sensor based on anodised aluminium nano wire according to claim 1, it is characterized in that, in step b), oxidation solution is that mass concentration is the mixed solution of the citric acid of 8-10%, succinic acid that mass concentration is 0.3-0.5% and the mass concentration potassium permanganate that is 0.9-1.5%.
4. the preparation method of a kind of benzene sensor based on anodised aluminium nano wire according to claim 1, is characterized in that, in step b), pore-enlargement is 30-45min, and the temperature of phosphoric acid solution is 50-55 DEG C.
5. the preparation method of a kind of benzene sensor based on anodised aluminium nano wire according to claim 1, is characterized in that, step c) neutral and alkali solution is the mixed solution of NaOH and cupric chloride; In every 1mL anodised aluminium nanowire suspension, add 1mg palladium bichloride, titania or iron oxide; The composition of copper plating bath is: the rare earth oxide of 1-butyl-3-methylimidazole paratoluenesulfonic acid sodium salt, 33-38g/L potassium tartrate and the 4.8-7.3g/L of 20-24g/L cupric chloride, 0.1-0.8g/L nickel chloride, 45-65mg/L polyglycol, 1.2-3.6g/L.
6. according to the preparation method of a kind of benzene sensor based on anodised aluminium nano wire described in claim 5, it is characterized in that, in alkaline solution, the mass concentration of NaOH and cupric chloride is respectively: NaOH 5-7% and cupric chloride 10-12%.
7. according to the preparation method of a kind of benzene sensor based on anodised aluminium nano wire described in claim 1 or 2 or 3 or 4 or 5, it is characterized in that ultrasonic processing 55-65W.
8. according to the preparation method of a kind of benzene sensor based on anodised aluminium nano wire described in claim 1 or 2 or 3 or 4 or 5, it is characterized in that, aluminium sheet adopts high-purity aluminium sheet of purity >=99.999%.
9. according to the preparation method of a kind of benzene sensor based on anodised aluminium nano wire described in claim 1 or 2 or 3 or 4 or 5, it is characterized in that, when electroplating processes, adopt two electrolytic tanks, utilize three-electrode system, auxiliary electrode is iridium tantalum titanium electrode, and contrast electrode is saturated calomel electrode SCE, and working electrode is the anodic oxidation aluminium sheet of bottom spray platinum.
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| CN114622192A (en) * | 2022-03-16 | 2022-06-14 | 莫纶(珠海)新材料科技有限公司 | Preparation method of copper/aluminum oxide composite fiber |
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| CN114622192A (en) * | 2022-03-16 | 2022-06-14 | 莫纶(珠海)新材料科技有限公司 | Preparation method of copper/aluminum oxide composite fiber |
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