CN105651813B - A kind of novel aniline gas sensor and preparation method thereof - Google Patents
A kind of novel aniline gas sensor and preparation method thereof Download PDFInfo
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- CN105651813B CN105651813B CN201410633403.XA CN201410633403A CN105651813B CN 105651813 B CN105651813 B CN 105651813B CN 201410633403 A CN201410633403 A CN 201410633403A CN 105651813 B CN105651813 B CN 105651813B
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- gas sensor
- metal
- aniline
- nickel dimethylglyoximate
- aniline gas
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Abstract
The invention discloses a kind of novel aniline gas sensors and preparation method thereof.Sensor composition includes: insulating ceramics substrate, a pair of metal electrodes and metal extraction wire on insulating ceramics substrate and the nickel dimethylglyoximate layer of nanomaterial being sprayed on metal electrode.Nickel dimethylglyoximate nano material is with NiCl2In the presence of ultrasonic wave, prepared by room temperature to 50 DEG C of reactions for aqueous solution and dimethylglyoxime ethanol solution.The sensor has fine response to aniline, and response and recovery are fast, and non-sintered, performance is stablized, and can work at room temperature.The aniline steam of 260-1300ppm concentration range can be used to measure.
Description
Technical field
The present invention relates to sensor fields, and in particular, to a kind of aniline gas sensor based on nickel chelate and its
Preparation method.
Background technique
The core of gas detecting system is gas sensor, it is typically mounted in detecting head.The essence of gas sensor
It is a kind of converter that certain gas concentration signal can be converted into exporting with it at the electricity of certain relationship.Its working principle one
As be that gas molecule and gas sensitive surface occur adsorption and desorption, catalysis burning, redox etc. and interact so that material
Electrochemical properties change, under additional circuit, pass through the measurement to electric current, voltage change in circuit, realize gas inspection
It surveys.Gas sensor is mainly used in toxic, flammable, the leak detection and alarm of explosion hazard gases, prevents from leaking because of these gases
Cause fire, explosion and intoxication accident.Currently, most commonly used is metal-oxide semiconductor (MOS) gas sensor, its advantage is that
Detection limit is low, and the Monitoring lower-cut concentration of some this kind of gas sensors reaches ppb level.The shortcomings that this kind of gas sensor is
Operating temperature is high, and energy consumption is high and poor selectivity.Gas sensor based on metallo-chelate is few, mainly big with the metal phthalein mountain valley with clumps of trees and bamboo
Ring complex is as sensitive material.
Aniline is important industrial chemicals, is mainly used for medicine and thiofide, and manufacture resin and coating
Raw material.Aniline to blood and nerve toxicity strongly, The book of Changes skin absorb.Mainly cause methemoglobinemia,
Hemolytic anemia and liver, renal damage.Acute poisoning: patient's lip, finger tip, auricle cyanosis, have headache, dizziness, Nausea and vomiting,
Finger is numb, absent-minded etc.；When severe intoxication, skin, mucous membrane are seriously livid purple, have difficulty in breathing, twitch, or even stupor, shock.
In addition, the mixture of aniline and air is also inflammable, explosive, explosion limit is 1.3% ~ 11.0%.Develop can in the environment quickly,
The gas sensor of aniline is accurately detected, provides necessary data with very important reality meaning to administer air environment
Justice.Currently, the gas sensor for being able to detect aniline is seldom.
Ultrasonic wave has unique effect in terms of preparing inorganic nano material, and phonochemistry method, which has become preparation, has spy
The useful technology of one kind of different performance new material, the specific physical that acoustic cavitation is caused, chemical environment have been preparation nano material
Important approach is provided, is mainly had in preparation method, ultrasonic atomizatio decomposition method, metallorganic ultrasonic decomposition method, chemistry
Precipitation method harmony electrochemical process etc., has gradually formed goalkeeper's ultrasonic technology and the chemical new science-combined closely is sonicating
It learns.
Summary of the invention
The purpose of the present invention is to provide it is a kind of using ultrasonic technology prepare nickel dimethylglyoximate nano material method and
A kind of novel aniline gas sensor based on nickel dimethylglyoximate nano material.
Aniline gas sensor provided by the present invention is successively by insulating substrate, a pair of metal electrodes, metal extraction wire
And nickel dimethylglyoximate layer of nanomaterial composition, it wherein include polyvinyl alcohol adhesive in nickel dimethylglyoximate layer of nanomaterial.
The insulating substrate is aluminum oxide ceramic square substrate.
The metal electrode is the interdigital electrode as made by metal Au, and the distance between two electrodes are 1mm.
The metal lead-outs are made of Pt metal silk.
The diameter of nano particles of the nickel dimethylglyoximate layer of nanomaterial is 80-200 nm；The nickel dimethylglyoximate nanometer
Material layer with a thickness of 50-120 μm.
The detailed preparation method of aniline gas sensor, including below step.
1) dimethylglyoxime nickel nano particle is prepared, under the ultrasonic wave of 30 KHz, dimethylglyoxime ethanol solution is added dropwise
Enter NiCl2In aqueous solution, reaction temperature is room temperature to 50 DEG C of ranges, NiCl2Molar ratio with dimethylglyoxime is 2:1, anti-to it
It should filter completely, obtain cerise precipitating, be washed with distilled water precipitating 3 times, obtained nickel dimethylglyoximate solid is put into baking
Case is dried 4 hours at 115 DEG C.
2) the dimethylglyoxime nickel nano particle and polyvinyl alcohol for preparing step 1) grinds 1-2 hours, makes after dilution
At slurry.
3) Au slurry is coated on the insulating substrate after cleaning and interdigital electrode is made, welding metal lead-out wire after drying.
4) slurry prepared by step 2 is prepared into diacetyl on electronic spray gun spraying to metal electrode and insulating substrate
Oxime nickel layer of nanomaterial, then drying obtains sensor element.
The utility model has the advantages that aniline gas sensor provided by the invention has response and restores fast, performance is stablized, production letter
It is single, do not need the advantages of being sintered, working at room temperature.
Detailed description of the invention
Fig. 1 is a series of responsiveness that the aniline gas sensor is exposed to inorganic gas and volatile organic compounds.
Fig. 2 is the responsiveness of aniline gas sensor prepared by embodiment 1 with concentration of aniline change curve.
Specific embodiment
The present invention is described in further detail below by specific embodiment, but the present invention is not limited thereto.
Embodiment 1.
1) 2.32 grams of (0.02 mole) dimethylglyoximes are weighed, are put into 250 milliliters of beakers, 100 milliliters of ethyl alcohol dissolution systems are added
At dimethylglyoxime ethanol solution.Separately take 2.37 grams of (0.01 mole) NiCl2·6H2O is put into 250 milliliters of beakers, adds 100 milliliters
NiCl is made in distilled water dissolution solution2Aqueous solution will fill NiCl2The beaker of aqueous solution is put into ultrasonic thermostatic water bath pot, heating
To 50 DEG C, adjusts ultrasonic frequency to 30 KHz, NiCl is added dropwise in dimethylglyoxime ethanol solution2In aqueous solution, dimethylglyoxime
With NiCl2Molar ratio be 2:1.It to its fully reacting, is cooled to room temperature, filters, obtain cerise precipitating.It is washed with distilled water
Precipitating 3 times, is put into baking oven for obtained nickel dimethylglyoximate solid, dries 4 hours at 115 DEG C.
2) it by the drying nickel dimethylglyoximate of step 1) preparation and 0.05% polyvinyl alcohol, grinds 2 hours, after dilution
Slurry is made.
3) aluminum oxide ceramic square substrate is taken, the sodium hydroxide solution that concentration is 6 mol/Ls is put into and boils 15 points
Clock takes out after cooling, with distilled water flushing three times, is placed in baking oven and dries.Au slurry is coated on to the Al 2 O pottery cleaned
Interdigital electrode is made on ceramic chip, dries, then the Pt wire bond of diameter 0.1mm is connected on electrode as lead-out wire.
4) slurry prepared by step 2 is prepared on electronic spray gun spraying to Au electrode and aluminum oxide ceramic substrate
At the nickel dimethylglyoximate layer of nanomaterial with a thickness of 50 μm, sensor element is obtained in 115 DEG C of drying.
Embodiment 2.
1) 2.32 grams of (0.02 mole) dimethylglyoximes are weighed, are put into 250 milliliters of beakers, 100 milliliters of ethyl alcohol dissolution systems are added
At dimethylglyoxime ethanol solution.Separately take 2.37 grams of (0.01 mole) NiCl2·6H2O is put into 250 milliliters of beakers, adds 100 milliliters
NiCl is made in distilled water dissolution solution2Aqueous solution will fill NiCl2The beaker of aqueous solution is put into ultrasonic thermostatic water bath pot, is adjusted super
To 30 KHz NiCl is added dropwise at room temperature in dimethylglyoxime ethanol solution by frequency of sound wave2In aqueous solution, dimethylglyoxime with
NiCl2Molar ratio be 2:1.It to its fully reacting, filters, obtains cerise precipitating.It is washed with distilled water precipitating 3 times, will
To nickel dimethylglyoximate solid be put into baking oven, 115 DEG C dry 4 hours.
2) it by the dimethylglyoxime nickel nano particle of step 1) preparation and 0.1% polyvinyl alcohol, grinds 1 hour, dilution
After slurry is made.
3) aluminum oxide ceramic square substrate is taken, the sodium hydroxide solution that concentration is 6 mol/Ls is put into and boils 10 points
Clock takes out after cooling, with distilled water flushing three times, is placed in baking oven and dries.Au slurry is coated on the aluminum oxide cleaned
Interdigital electrode is made on ceramic substrate, dries, then the Pt wire bond of diameter 0.1mm is connected on electrode as lead-out wire.
4) slurry prepared by step 2 is prepared on electronic spray gun spraying to Pt electrode and aluminum oxide ceramic substrate
At the nickel dimethylglyoximate layer of nanomaterial with a thickness of 120 μm, sensor element is obtained in 105 DEG C of drying.
Claims (7)
1. a kind of aniline gas sensor, it is characterised in that: successively drawn by insulating ceramics substrate, a pair of metal electrodes, metal
Conducting wire and chelate nickel dimethylglyoximate (II) layer of nanomaterial form, wherein chelate nickel dimethylglyoximate (II) layer of nanomaterial
In include a kind of polyvinyl alcohol adhesive.
2. by aniline gas sensor described in claim 1, it is characterised in that: the concentration of the polyvinyl alcohol adhesive is
0.05% or 0.1%.
3. by aniline gas sensor described in claim 1, it is characterised in that: the insulating ceramics substrate is aluminum oxide
Square insulating ceramic substrate.
4. by aniline gas sensor described in claim 1, it is characterised in that: the metal electrode is made of metal Au
Interdigital electrode, the distance between two electrodes are 1mm.
5. by aniline gas sensor described in claim 1, it is characterised in that: the metal extraction wire is Pt metal
Silk, Pt are connected between metal electrode by welding method.
6. by aniline gas sensor described in claim 1, it is characterised in that: chelate nickel dimethylglyoximate (II) nanometer
The diameter of nano particles of material layer is 80-200nm；Chelate nickel dimethylglyoximate (II) layer of nanomaterial with a thickness of 50-
120μm。
7. preparing the preparation method of aniline gas sensor described in any one of claim 1-5, including below step:
1) chelate nickel dimethylglyoximate (II) nanoparticle is prepared, under the ultrasonic wave of 30KHz, dropwise by diacetylmonoxime ethanol solution
NiCl is added2In aqueous solution, reaction temperature is room temperature to 50 DEG C of ranges, dimethylglyoxime and NiCl2Molar ratio be 2:1, it is anti-to it
It should filter completely, obtain cerise precipitating, be washed with distilled water precipitating 3 times, obtained chelate nickel dimethylglyoximate (II) is solid
Body is put into baking oven, dries 4 hours at 115 DEG C；
2) chelate nickel dimethylglyoximate (II) nanoparticle prepared by step 1) is mixed with binder, is ground 1-2 hours, dilution
After slurry is made；
3) Au slurry is coated on the insulating ceramics substrate after cleaning, welding metal extraction wire after drying；
4) by the slurry of step 2) preparation with electronic spray gun spraying in being prepared into chelate on metal electrode and insulating ceramics substrate
Nickel dimethylglyoximate (II) layer of nanomaterial, then 105-115 DEG C of drying obtains sensor element.
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| CN201410633403.XA CN105651813B (en) | 2014-11-12 | 2014-11-12 | A kind of novel aniline gas sensor and preparation method thereof |
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| CN201410633403.XA CN105651813B (en) | 2014-11-12 | 2014-11-12 | A kind of novel aniline gas sensor and preparation method thereof |
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| CN105651813A CN105651813A (en) | 2016-06-08 |
| CN105651813B true CN105651813B (en) | 2019-01-11 |
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| CN110907502A (en) * | 2018-09-17 | 2020-03-24 | 中国科学院大连化学物理研究所 | Aniline sensor taking three-dimensional foamy graphene material as sensing film |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1885025A (en) * | 2006-07-11 | 2006-12-27 | 电子科技大学 | Organic nitrogen oxide sensitive composite material and nitrogen oxide gas sensor |
| WO2012154314A1 (en) * | 2011-03-31 | 2012-11-15 | 3M Innovative Properties Company | Method and device for indicating moisture based on bis (glyoxime) -transition metal complexes |
| CN102788822A (en) * | 2012-07-19 | 2012-11-21 | 西南交通大学 | Preparation method of nanometer composite film ammonia gas sensor |
| CN103336034A (en) * | 2013-05-09 | 2013-10-02 | 中国科学院化学研究所 | Aniline gas sensor and preparation method thereof |
-
2014
- 2014-11-12 CN CN201410633403.XA patent/CN105651813B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1885025A (en) * | 2006-07-11 | 2006-12-27 | 电子科技大学 | Organic nitrogen oxide sensitive composite material and nitrogen oxide gas sensor |
| WO2012154314A1 (en) * | 2011-03-31 | 2012-11-15 | 3M Innovative Properties Company | Method and device for indicating moisture based on bis (glyoxime) -transition metal complexes |
| CN102788822A (en) * | 2012-07-19 | 2012-11-21 | 西南交通大学 | Preparation method of nanometer composite film ammonia gas sensor |
| CN103336034A (en) * | 2013-05-09 | 2013-10-02 | 中国科学院化学研究所 | Aniline gas sensor and preparation method thereof |
Non-Patent Citations (5)
| Title |
|---|
| Ahmad Nozad Golikand等.Methanol electrooxidation on a nickel electrode modified by nickel–dimethylglyoxime complex formed by electrochemical synthesis.《Journal of Electroanalytical Chemistry 》.2005,第588卷第155-160页. |
| Applications of Ultrasound to the Synthesis of Nanostructured Materials;Jin Ho Bang等;《Adv. Mater. 》;20101231;第22卷;第1039-1059页 |
| Determination of ammonia in air using a novel ammonia sensor based on a nickel(II) macrocyclic complex;Tiexiang Fu;《Journal of Electroanalytical Chemistry》;20080315;第618卷;第2.1节，图1 |
| The Structure of Nickel dimethylglyoxime;L. EDWARD GODYCKI等;《Acta Cryst.》;19531231;第6卷;第487页 |
| 氨敏线性传感器研究;傅铁祥 等;《传感技术学报》;20110930(第3期);第225-229页 |
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