CN105606655A - Palladium-supported acetone gas sensor manufacturing method based on two-dimensional porous nano composite material and application - Google Patents
Palladium-supported acetone gas sensor manufacturing method based on two-dimensional porous nano composite material and application Download PDFInfo
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- CN105606655A CN105606655A CN201610101723.XA CN201610101723A CN105606655A CN 105606655 A CN105606655 A CN 105606655A CN 201610101723 A CN201610101723 A CN 201610101723A CN 105606655 A CN105606655 A CN 105606655A
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- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
Abstract
The invention relates to an acetone gas sensor manufacturing method, in particular to a gas sensor manufactured based on a novel two-dimensional nano composite material and belongs to the technical field of novel nano functional materials and environment monitoring. The acetone gas sensor manufacturing method can be used for detecting the acetone gas content in an environment. The cerium and cobalt double-metal doped titanium dioxide nano sheet in-situ composite carbon nitride two-dimensional nano composite material CeCo-TiO2/g-C3N4 is firstly prepared, the large specific surface area of the material, gas absorption characteristics of mesopores and electron transfer change with material surface gas are utilized to affect lots of sensitive features, and manufacture of the acetone gas sensor having sensitivity and rapid response to acetone gas is achieved.
Description
Technical field
The present invention relates to a kind of preparation method of acetone gas sensor, belong to Nano-function thin films and environmental monitoringTechnical field.
Background technology
Acetone (acetone, CH3COCH3), has another name called dimethyl ketone, is the simplest saturated ketone. A kind of water white transparency liquidBody, has special pungent smell. The organic solvents such as soluble in water and methyl alcohol, ethanol, ether, chloroform, pyridine. It is inflammable, volatile,Chemical property is more active. Acute poisoning main manifestations is the anesthetic effect to central nervous system, occur weak, nauseating, headache,Dizzy, emotional. Severe one is vomitted, out of breath, spasm, even stupor. Irritant to eye, nose, larynx. After oral, first there is mouthLip, throat have burn feeling, rear dry, vomiting, stupor, acid poisoning and the ketosis of occurring.
Mainly contain chemical analysis method and instrument testing method for the detection method of acetone gas. Though chemical analysis method operation letterSingle, but sensitivity is not high and the shortcoming such as cannot reuse; Instrument testing method, is mainly used acetone gas instrumentation to skyAcetone gas concentration in gas quantitatively detects, and has highly sensitive, reusable, automaticity advantages of higher, andBe widely applied in the middle of industrial production.
The acetone gas detector using for instrument testing method, most crucial parts be acetone gas is had qualitativeThe gas sensor of quantitative response, is namely coated with the gas sensor of different nano-functional materials. Gas sensor is a kind ofThe sensor that detects specific gas, principle is that velocity of wave and the frequency based on SAW device can be sent out with the variation of external environmentRaw drift. It mainly comprises semiconductor gas sensor, catalytic combustion type gas sensor and Electro-chemical Gas Sensor etc., itsThe maximum of middle use are semiconductor gas sensors.
Sensitivity is the important sign of gas sensor gas-sensitive property. Sensitivity definition is that sensor is in air atmosphereResistance value RaWith the resistance value R of sensor in certain density tested gas atmospheregRatio,
Therefore, probe into that adsorptivity is strong, stability good, catalytic activity is high, acetone gas is had to specific recognition and can be quantitativeThe gas sensing materials detecting, so preparation have highly sensitive, response fast, the acetone gas of the characteristic such as recovery time is short passesSensor has important using value to industrial production, human health, is also the emphasis of environmental monitoring technology area research simultaneouslyAnd difficult point.
Summary of the invention
The object of the present invention is to provide one prepare simple, highly sensitive, detect and can be used for fast acetone gas inspectionThe preparation method of gas sensor who surveys, prepared sensor, can be used for acetone gas fast, Sensitive Detection. Based on thisObject, first the present invention has prepared a kind of New Two Dimensional nano composite material, i.e. the titanium dioxide of cerium and cobalt dual-metal codopeNanometer sheet original position composite nitride carbon two-dimensional nano composite CeCo-TiO2/g-C3N4, utilize specific area, Jie that this material is largeThe high gas absorption characteristic in hole and electronics transmission are changed by material surface gas and affect responsive many characteristics, have realized acetoneThat gas has is sensitive, the structure of the gas sensor of quick response.
The technical solution used in the present invention is as follows:
1. a preparation method for the acetone gas sensor based on two-dimentional porous nano composite supported palladium, described twoDimension porous nano composite is the titanium dioxide nanoplate original position composite nitride carbon two-dimensional nano of cerium and cobalt dual-metal codopeComposite CeCo-TiO2/g-C3N4, described palladium is Pd nano particle;
It is characterized in that, described preparation method comprises following preparation process:
（1）CeCo-TiO2/g-C3N4Preparation;
(2) preparation of acetone gas sensor;
Wherein, step (1) is prepared CeCo-TiO2/g-C3N4Concrete steps be:
First, get 0.8mmol cerium salt and 0.8 ~ 1.2mmol cobalt salt and join in 5mL butyl titanate, in whipping process, slowSlowly add 0.5 ~ 0.8mL hydrofluoric acid, reaction kettle for reaction 18 ~ 24 hours, be cooled to after room temperature, with super at 160 ~ 200 DEG CAfter pure water and absolute ethyl alcohol centrifuge washing three times, vacuum drying at 50 DEG C; Secondly, get the dried solid of 150 ~ 250mg with400mg melamine mixes, and grind into powder; Then, the powder of grinding is put into Muffle furnace, programming rate is 1 ~ 3DEG C/min, at 480 ~ 560 DEG C, calcine 0.5 ~ 5 hour; Finally, the powder after calcining is cooled to room temperature, makes CeCo-TiO2/g-C3N4；
It is one of following that described cerium salt is selected from: cerous sulfate, cerium chloride, cerous nitrate;
It is one of following that described cobalt salt is selected from: cobaltous sulfate, cobalt chloride, cobalt nitrate;
The concrete steps that step (2) is prepared acetone gas sensor are:
First, get the CeCo-TiO of preparation in step (1)2/g-C3N4100mg and 0.5 ~ 2.0mmol palladium bichloride are placed in mortarIn, add absolute ethyl alcohol, be ground to and be evenly coated in insulating ceramics tube-surface after pasty state and form film, at room temperature dry; SoAfter, the platinum filament of earthenware both sides and heater strip and base are welded; Finally, the element having welded is placed on to detectorIn device, by regulating heating voltage to carry out burin-in process to 4.22V, make acetone gas sensor.
2. the application of the prepared acetone gas sensor of preparation method of the present invention, is characterized in that Ke YiyingFor the detection of acetone gas, detect and be limited to 0.001mg/m3。
Useful achievement of the present invention
(1) acetone gas sensor of the present invention preparation is simple, easy to operate, has realized quick, clever to acetone gasQuick, high selectivity detects, and has future develop;
(2) the present invention has prepared New-type matrix material CeCo-TiO first2/g-C3N4, because cerium, cobalt are at titanium dioxide nanoplateOn growth in situ and fully contact with titanium dioxide nanoplate, utilize the metal surface plasma body effect and two of cerium, cobaltPerson's mutual promoting action, has effectively improved semiconductor substrate electronics transmission capacity and catalytic activity, has solved titanium dioxide and has receivedAlthough rice sheet specific area is larger and mesoporous high gas absorption characteristic is applicable to air-sensitive host material, gas-sensitive activity is not highAnd the unsettled technical problem of impedance variations; Simultaneously due to carbonitride g-C3N4Good electric conductivity, add titanium dioxide and receiveThe abundant dispersion thereon of rice sheet, has greatly increased electronics transmission capacity, has solved the impedance of air-sensitive host material and has become with gasThe technical problem of changing and respond fast; And by the doping of Metal Palladium, the technology that has solved specific detection acetone gas is askedTopic. Therefore, effective preparation of this material, has important scientific meaning and using value.
Detailed description of the invention
Embodiment 1CeCo-TiO2/g-C3N4Preparation
First, get 0.8mmol cerium salt and 0.8mmol cobalt salt and join in 5mL butyl titanate, in whipping process, slowly addEnter 0.5mL hydrofluoric acid, reaction kettle for reaction 24 hours, be cooled to after room temperature at 160 DEG C, with ultra-pure water and absolute ethyl alcohol fromAfter heart washing three times, vacuum drying at 50 DEG C; Secondly, get the dried solid of 150mg and mix with 400mg melamine, andGrind into powder; Then, the powder of grinding is put into Muffle furnace, programming rate is 1 DEG C/min, at 480 DEG C, calcines 5Hour; Finally, the powder after calcining is cooled to room temperature, makes CeCo-TiO2/g-C3N4；
Described cerium salt is cerous sulfate;
Described cobalt salt is cobaltous sulfate.
Embodiment 2CeCo-TiO2/g-C3N4Preparation
First, get 0.8mmol cerium salt and 1.0mmol cobalt salt and join in 5mL butyl titanate, in whipping process, slowly addEnter 0.65mL hydrofluoric acid, reaction kettle for reaction 21 hours, be cooled to after room temperature, with ultra-pure water and absolute ethyl alcohol at 180 DEG CAfter centrifuge washing three times, vacuum drying at 50 DEG C; Secondly, get the dried solid of 200mg and mix with 400mg melamine,And grind into powder; Then, the powder of grinding is put into Muffle furnace, programming rate is 2 DEG C/min, calcining at 520 DEG C2 hours; Finally, the powder after calcining is cooled to room temperature, makes CeCo-TiO2/g-C3N4；
Described cerium salt is cerium chloride;
Described cobalt salt is cobalt chloride.
Embodiment 3CeCo-TiO2/g-C3N4Preparation
First, get 0.8mmol cerium salt and 1.2mmol cobalt salt and join in 5mL butyl titanate, in whipping process, slowly addEnter 0.8mL hydrofluoric acid, reaction kettle for reaction 18 hours, be cooled to after room temperature, with ultra-pure water and absolute ethyl alcohol at 200 DEG CAfter centrifuge washing three times, vacuum drying at 50 DEG C; Secondly, get the dried solid of 250mg and mix with 400mg melamine,And grind into powder; Then, the powder of grinding is put into Muffle furnace, programming rate is 3 DEG C/min, calcining at 560 DEG C0.5 hour; Finally, the powder after calcining is cooled to room temperature, makes CeCo-TiO2/g-C3N4；
Described cerium salt is cerous nitrate;
Described cobalt salt is cobalt nitrate.
The preparation of embodiment 4 acetone gas sensors
First, get the CeCo-TiO of preparation in embodiment 12/g-C3N4100mg and 0.5mmol palladium bichloride are placed in mortar, addEnter absolute ethyl alcohol, be ground to and be evenly coated in insulating ceramics tube-surface after pasty state and form film, at room temperature dry; Then, willThe platinum filament of earthenware both sides and heater strip and base weld; Finally, the element having welded is placed in detecting instrument,By regulating heating voltage to carry out burin-in process to 4.22V, make acetone gas sensor, be applied to the inspection of acetone gasSurvey, detect and be limited to 0.001mg/m3。
The preparation of embodiment 5 acetone gas sensors
First, get the CeCo-TiO of preparation in embodiment 22/g-C3N4100mg and 1.2mmol palladium bichloride are placed in mortar, addEnter absolute ethyl alcohol, be ground to and be evenly coated in insulating ceramics tube-surface after pasty state and form film, at room temperature dry; Then, willThe platinum filament of earthenware both sides and heater strip and base weld; Finally, the element having welded is placed in detecting instrument,By regulating heating voltage to carry out burin-in process to 4.22V, make acetone gas sensor, be applied to the inspection of acetone gasSurvey, detect and be limited to 0.001mg/m3。
The preparation of embodiment 6 acetone gas sensors
First, get the CeCo-TiO of preparation in embodiment 32/g-C3N4100mg and 2.0mmol palladium bichloride are placed in mortar, addEnter absolute ethyl alcohol, be ground to and be evenly coated in insulating ceramics tube-surface after pasty state and form film, at room temperature dry; Then, willThe platinum filament of earthenware both sides and heater strip and base weld; Finally, the element having welded is placed in detecting instrument,By regulating heating voltage to carry out burin-in process to 4.22V, make acetone gas sensor, be applied to the inspection of acetone gasSurvey, detect and be limited to 0.001mg/m3。
Claims (2)
1. a preparation method for the acetone gas sensor based on two-dimentional porous nano composite supported palladium, described two dimensionPorous nano composite is that the titanium dioxide nanoplate original position composite nitride carbon two-dimensional nano of cerium and cobalt dual-metal codope is multipleCondensation material CeCo-TiO2/g-C3N4, described palladium is Pd nano particle;
It is characterized in that, described preparation method comprises following preparation process:
（1）CeCo-TiO2/g-C3N4Preparation;
(2) preparation of acetone gas sensor;
Wherein, step (1) is prepared CeCo-TiO2/g-C3N4Concrete steps be:
First, get 0.8mmol cerium salt and 0.8 ~ 1.2mmol cobalt salt and join in 5mL butyl titanate, in whipping process, slowSlowly add 0.5 ~ 0.8mL hydrofluoric acid, reaction kettle for reaction 18 ~ 24 hours, be cooled to after room temperature, with super at 160 ~ 200 DEG CAfter pure water and absolute ethyl alcohol centrifuge washing three times, vacuum drying at 50 DEG C; Secondly, get the dried solid of 150 ~ 250mg with400mg melamine mixes, and grind into powder; Then, the powder of grinding is put into Muffle furnace, programming rate is 1 ~ 3DEG C/min, at 480 ~ 560 DEG C, calcine 0.5 ~ 5 hour; Finally, the powder after calcining is cooled to room temperature, makes CeCo-TiO2/g-C3N4；
It is one of following that described cerium salt is selected from: cerous sulfate, cerium chloride, cerous nitrate;
It is one of following that described cobalt salt is selected from: cobaltous sulfate, cobalt chloride, cobalt nitrate;
The concrete steps that step (2) is prepared acetone gas sensor are:
First, get the CeCo-TiO of preparation in step (1)2/g-C3N4100mg and 0.5 ~ 2.0mmol palladium bichloride are placed in mortarIn, add absolute ethyl alcohol, be ground to and be evenly coated in insulating ceramics tube-surface after pasty state and form film, at room temperature dry; SoAfter, the platinum filament of earthenware both sides and heater strip and base are welded; Finally, the element having welded is placed on to detectorIn device, by regulating heating voltage to carry out burin-in process to 4.22V, make acetone gas sensor.
2. the application of the prepared acetone gas sensor of preparation method as claimed in claim 1, is characterized in that Ke YiyingFor the detection of acetone gas, detect and be limited to 0.001mg/m3。
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Cited By (3)
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| CN108889325A (en) * | 2018-06-28 | 2018-11-27 | 陕西科技大学 | A kind of synthetic method of Pt nanoparticle catalyst |
| CN110711863A (en) * | 2019-11-06 | 2020-01-21 | 郑州大学 | AuPd alloy nanoparticle loaded 3DOM WO3Preparation method of (1) |
| CN112844436A (en) * | 2021-01-27 | 2021-05-28 | 宁波方太厨具有限公司 | Catalyst for removing formaldehyde and carbon monoxide by catalysis and preparation method thereof |
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| CN110711863A (en) * | 2019-11-06 | 2020-01-21 | 郑州大学 | AuPd alloy nanoparticle loaded 3DOM WO3Preparation method of (1) |
| CN112844436A (en) * | 2021-01-27 | 2021-05-28 | 宁波方太厨具有限公司 | Catalyst for removing formaldehyde and carbon monoxide by catalysis and preparation method thereof |
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