CN104089994A - Preparation method of ammonia sensor based on anodic alumina nanowire - Google Patents
Preparation method of ammonia sensor based on anodic alumina nanowire Download PDFInfo
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Abstract
The invention relates to a preparation method of an ammonia sensor based on an anodic alumina nanowire. The ammonia 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 ammonia gas sensor based on anodised aluminium nano wire of favorable repeatability.
Background technology
Ammonia is mineral compound, is gas under normal temperature, and the smell of colourless irritant stench is soluble in water.Ammonia is the major product of ammonia synthesizing industry and the secondary product of coking industry, the mucous membrane of energy skin ambustion, eyes, respiratory apparatus, and people sucks too much, can cause lung swelling, so that dead.Ammonia has corrosion and spread effect to the skin histology of contact, can absorb the moisture in skin histology, makes histone sex change, and makes tissue fat saponification, destroys membrane structure.The solubleness of ammonia is high, so mainly the upper respiratory tract of animal or human's body is had and stimulated and corrosive attack, is often attracted on mucocutaneous and eye conjunctiva, thereby produce, stimulates and inflammation.Can benumb respiratory tract cilium and infringement mucous epithelium tissue, make pathogenic microorganism be easy to immerse, weaken human body the resistibility ammonia of disease is sucked to human body with gas form conventionally, ammonia easily enters blood by alveolar after being inhaled into lung, be combined with haemoglobin, destroy fortune oxygen function.Enter IA ammonia, small part is neutralized by carbon dioxide, and remainder is absorbed into blood, and a small amount of ammonia can excrete with sweat, urine or breathing.
Suck in a short time after a large amount of ammonias can occur shedding tears, pharyngalgia, hoarseness, cough, sputum streaked with blood silk, uncomfortable in chest, expiratory dyspnea, can be with dizzy, headache, feel sick, vomiting, the phenomenon such as weak, can there is pulmonary edema, adult respiratory distress syndrome (ARDS) in severe patient, respiratory tract symptom may occur simultaneously.If the ammonia sucking is too much, cause ammonia excessive concentration in blood, will cause by the reflex of trigeminal neuralgia tip heart stop fight and breath stopped, threat to life.
Long Term Contact ammonia, may there is the symptoms such as Skin pigmentation or finger ulcer in groups of people.In room air, ammonia is mainly from the mixed earth adjuvant using in building operation.In adjuvant, contain material in a large amount of ammonia, in body of wall, along with the variation of the environmental factors such as temperature, humidity, be reduced into ammonia and discharge.
For low concentration ammonia detection method, mainly rely at present the method for instrumental analysis, as vapor-phase chromatography etc.Although these detections are the concentration of micro-ammonia 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-ammonia 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 in order to solve that the method sense cycle of existing detection ammonia 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-ammonia 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 ammonia gas 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 ammonia gas 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 ℃, cooling rear cleaning degrease, then immerses in soak solution, and soak solution temperature is 35-50 ℃, 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 for the first time, in oxidation solution, be oxidized, oxidation voltage 45V, oxidization time 15-25min, immerses in the nitric acid of mass concentration 2.5% and the oxalic acid equal-volume mixed solution of mass concentration 3.8% and soaks 4-6h after taking out; Then in the oxidation solution identical with being oxidized for the first time oxidation solution used, carry out anodic oxidation for the second time, oxidation voltage 40V, oxidization time 50-70min, before finishing, oxidation with every 10s, reduces the speed of 8V oxidation voltage in 30s, oxidation voltage is down to 10-12V, 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 ℃, dried 25-35min; Anodic oxidation aluminium sheet after copper facing is placed in to alkaline solution 8-10h, obtain anodised aluminium nano-material, then with deionized water, be configured to 5mg/mL anodised aluminium nanowire suspension, 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 8-10 layer.
In the technical program, anodised aluminium nano-material own wt is light, and therefore the sensor of preparation has superiority in weight, compared with the sensor of lightweight, is conducive to be fixed on different positions, 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 anodised aluminium nano-material for the suction-operated of 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 to process before the end of oxidation, can reduce the thickness of anodised aluminium surface barrier, if do not take step-down to process, barrier layer thickness is 50 microns of left and right, and takes step-down of the present invention to process, and the thickness on restraining barrier is 18 microns of left and right;
Reaming is in order to increase the diameter of 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 sensitivity and the accuracy detecting, and 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 in the time of 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 that the citric acid of 8-10% is, the mixed solution of the potassium permanganate that the rare-earth element gadolinium of 0.13-0.45mg/L and mass concentration are 0.9-1.5%.
As preferably, in step b), pore-enlargement is 30-45min, and the temperature of phosphoric acid solution is 50-55 ℃.
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 chlorination 1-benzyl-3 methylimidazole, 33-38g/L potassium tartrate and the 1.3-4.2g/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, during 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.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the anodic oxidation aluminium sheet of embodiment 1 preparation.
Fig. 2 is the scanning electron microscope (SEM) photograph of the anodised aluminium nano wire of embodiment 1 preparation.
Fig. 3 is ammonia 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 ammonia gas sensor based on anodised aluminium nano wire, described preparation method comprises the following steps:
A) pre-treatment: high-purity aluminium sheet of purity >=99.999% 8h that anneals at 220 ℃ just, cooling rear cleaning degrease, then immerses in soak solution, and soak solution temperature is 35 ℃, and soak time is 30min; After taking-up is cleaned, after taking-up is cleaned, 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 in the time of 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 for the first time, in oxidation solution, be oxidized, oxidation voltage 45V, oxidization time 25min, immerses in the nitric acid of mass concentration 2.5% and the oxalic acid equal-volume mixed solution of mass concentration 3.8% and soaks 4h after taking out; Then in the oxidation solution identical with being oxidized for the first time oxidation solution used, carry out anodic oxidation for the second time, oxidation voltage 40V, oxidization time 50min, before finishing, oxidation with every 10s, reduces the speed of 8V oxidation voltage in 30s, oxidation voltage is down to 10V, after taking-up, put into massfraction and be 7% phosphoric acid solution reaming, obtain anodic oxidation aluminium sheet; Oxidation solution is that mass concentration is 8% citric acid, the rare-earth element gadolinium of 0.13mg/L and the mixed solution of the potassium permanganate that mass concentration is 0.9%; Pore-enlargement is 30min, and the temperature of phosphoric acid solution is 55 ℃;
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 ℃, dried 35min; Anodic oxidation aluminium sheet after copper facing is placed in to alkaline solution 8h, obtain anodised aluminium nano-material, then with deionized water, be configured to 5mg/mL anodised aluminium nanowire suspension, 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 chlorination 1-benzyl-3 methylimidazole, 33g/L potassium tartrate and the 1.3g/L of 20g/L cupric chloride, 0.1g/L nickel chloride, 45mg/L polyglycol, 1.2g/L; During 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, dry after applying, then continue to apply, the number of plies that anodised aluminium nano wire applies is 8 layers.
Embodiment 2
A preparation method for ammonia gas sensor based on anodised aluminium nano wire, described preparation method comprises the following steps:
A) pre-treatment: high-purity aluminium sheet of purity >=99.999% 7h that anneals at 280 ℃ just, cooling rear cleaning degrease, then immerses in soak solution, and soak solution temperature is 45 ℃, and soak time is 20min; After taking-up is cleaned, after taking-up is cleaned, 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 in the time of 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 for the first time, in oxidation solution, be oxidized, oxidation voltage 45V, oxidization time 20min, immerses in the nitric acid of mass concentration 2.5% and the oxalic acid equal-volume mixed solution of mass concentration 3.8% and soaks 5h after taking out; Then in the oxidation solution identical with being oxidized for the first time oxidation solution used, carry out anodic oxidation for the second time, oxidation voltage 40V, oxidization time 60min, before finishing, oxidation with every 10s, reduces the speed of 8V oxidation voltage in 30s, oxidation voltage is down to 12V, after taking-up, put into massfraction and be 8% phosphoric acid solution reaming, obtain anodic oxidation aluminium sheet; Oxidation solution is that mass concentration is 9% citric acid, the rare-earth element gadolinium of 0.31mg/L and the mixed solution of the potassium permanganate that mass concentration is 1.2%; Pore-enlargement is 40min, and the temperature of phosphoric acid solution is 52 ℃;
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 ℃, dried 30min; Anodic oxidation aluminium sheet after copper facing is placed in to alkaline solution 9h, obtain anodised aluminium nano-material, then with deionized water, be configured to 5mg/mL anodised aluminium nanowire suspension, 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 chlorination 1-benzyl-3 methylimidazole, 35g/L potassium tartrate and the 2.8g/L of 22g/L cupric chloride, 0.5g/L nickel chloride, 50mg/L polyglycol, 2.4g/L; During 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, dry after applying, then continue to apply, the number of plies that anodised aluminium nano wire applies is 9 layers.
Embodiment 3
A preparation method for ammonia gas sensor based on anodised aluminium nano wire, described preparation method comprises the following steps:
A) pre-treatment: high-purity aluminium sheet of purity >=99.999% 6h that anneals at 320 ℃ just, cooling rear cleaning degrease, then immerses in soak solution, and soak solution temperature is 50 ℃, and soak time is 10min; After taking-up is cleaned, after taking-up is cleaned, 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 in the time of 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 for the first time, in oxidation solution, be oxidized, oxidation voltage 45V, oxidization time 15min, immerses in the nitric acid of mass concentration 2.5% and the oxalic acid equal-volume mixed solution of mass concentration 3.8% and soaks 6h after taking out; Then in the oxidation solution identical with being oxidized for the first time oxidation solution used, carry out anodic oxidation for the second time, oxidation voltage 40V, oxidization time 70min, before finishing, oxidation with every 10s, reduces the speed of 8V oxidation voltage in 30s, oxidation voltage is down to 10V, after taking-up, put into massfraction and be 10% phosphoric acid solution reaming, obtain anodic oxidation aluminium sheet; Oxidation solution is that mass concentration is 10% citric acid, the rare-earth element gadolinium of 0.45mg/L and the mixed solution of the potassium permanganate that mass concentration is 1.5%; Pore-enlargement is 45min, and the temperature of phosphoric acid solution is 50 ℃;
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 ℃, dried 25min; Anodic oxidation aluminium sheet after copper facing is placed in to alkaline solution 10h, obtain anodised aluminium nano-material, then with deionized water, be configured to 5mg/mL anodised aluminium nanowire suspension, 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 chlorination 1-benzyl-3 methylimidazole, 38g/L potassium tartrate and the 4.2g/L of 24g/L cupric chloride, 0.8g/L nickel chloride, 65mg/L polyglycol, 3.6g/L; During 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 to embodiment 1 preparation is done electron-microscope scanning, the results are shown in Figure 1; Anodised aluminium nano wire to embodiment 1 preparation is done 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 ammonia 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 ammonia 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 ammonia gas, prepared sensor all has sensitive response to the ammonia gas of variable concentrations, pass into ammonia gas in air chamber after, its electric conductivity has been produced to impact, the electric current that ammonia gas concentration is passed through is more greatly less.Relation between detection electric current and ammonia gas concentration as shown in Figure 3, obtains sensor according to Fig. 3 through linear fit and detects the relation between electric current and ammonia gas concentration, and physical relationship formula is:
, R=0.97225, utilizes this formula, and we just can detect electric current according to sensor and realize the detection to tested ammonia sample.
Claims (9)
1. a preparation method for the ammonia gas 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 ℃, cooling rear cleaning degrease, then immerses in soak solution, and soak solution temperature is 35-50 ℃, 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 for the first time, in oxidation solution, be oxidized, oxidation voltage 45V, oxidization time 15-25min, immerses in the nitric acid of mass concentration 2.5% and the oxalic acid equal-volume mixed solution of mass concentration 3.8% and soaks 4-6h after taking out; Then in the oxidation solution identical with being oxidized for the first time oxidation solution used, carry out anodic oxidation for the second time, oxidation voltage 40V, oxidization time 50-70min, before finishing, oxidation with every 10s, reduces the speed of 8V oxidation voltage in 30s, oxidation voltage is down to 10-12V, 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 ℃, dried 25-35min; Anodic oxidation aluminium sheet after copper facing is placed in to alkaline solution 8-10h, obtain anodised aluminium nano-material, then with deionized water, be configured to 5mg/mL anodised aluminium nanowire suspension, 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 8-10 layer.
2. the preparation method of a kind of ammonia gas 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 in the time of 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 ammonia gas 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 that the citric acid of 8-10% is, the mixed solution of the potassium permanganate that the rare-earth element gadolinium of 0.13-0.45mg/L and mass concentration are 0.9-1.5%.
4. the preparation method of a kind of ammonia gas 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 ℃.
5. the preparation method of a kind of ammonia gas 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 chlorination 1-benzyl-3 methylimidazole, 33-38g/L potassium tartrate and the 1.3-4.2g/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 ammonia gas 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 ammonia gas 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 ammonia gas 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 ammonia gas sensor based on anodised aluminium nano wire described in claim 1 or 2 or 3 or 4 or 5, it is characterized in that, during 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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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105129723A (en) * | 2015-07-30 | 2015-12-09 | 西北大学 | Controllable preparation method for large area porous micronano composite structure |
| CN110514729A (en) * | 2019-09-05 | 2019-11-29 | 吉林大学 | A kind of sensitive electrode and preparation method thereof detected for ammonia nitrogen Direct Electrochemistry in water |
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