CN110243880A - A kind of preparation method and application for the gas sensitive detecting ammonia - Google Patents
A kind of preparation method and application for the gas sensitive detecting ammonia Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method and application of gas sensitive for detecting ammonia, function of dominant material, sensing technology and environmental monitoring technology fields.The present invention prepares MoS respectively2And g-C3N4Material prepares g-C with sol method3N4/MoS2Nanocomposite detects ammonia as gas sensitive；G-C will be coated3N4/MoS2Resistance wire is passed through inside it after the gas sensor aging of nanocomposite, is later welded 6 pillars of 6 filaments and gas sensor pedestal on ceramic tube with tin to get the sensor gas sensor of required detection ammonia is arrived.Gas sensor obtained has many advantages, such as the detection of ammonia highly sensitive, highly selective, can be used for detecting the ammonia in industrial environment.
Description
Technical field
The present invention relates to a kind of gas sensitive and preparation method and application for detecting ammonia, function of dominant nano material prepares skill
Art and gas sensing detection technical field.
Background technique
Eighties of last century the '30s, foreign countries begin one's study and develop gas sensor successively, until eighties of last century mid-term, passes
Sense field rapidly develop, wherein semiconductor transducer, solid-state electrolyte sensor and humidity sensor it is certain country
Realize commercialization.Nowadays, hundreds of gas sensor is developed successively.In recent years, by the way that gas sensitive is made
Film or nanostructure improve its air-sensitive performance, because the adsorption capacity of gas sensitive, specific surface area and active site etc. are
The main reason for influencing its selectivity and sensitivity.So how to improve the response speed of gas sensor, sensitivity and choosing
Selecting property becomes the Main way studied now.
Since metal-oxide semiconductor (MOS) has its unique feature performance benefit, such as the response time is short, sensitivity is high, Hen Duoqi
Quick investigation of materials personnel are using metal oxide as main study subject, but the operating temperature that metal oxide gas sensitive requires
It is higher, it will be typically higher than 200 DEG C, and can also require the heating condition of auxiliary, this makes metal oxide gas sensitive power consumption
Greatly, stability is bad.And determinand is also possible to thermal degradation can occur because of higher operating temperature, can thus make to detect
As a result it is greatly affected.Metal sulfide semiconductor material is very sensitive to the variation of surface electrical properties, because of its surface state
Density is relatively low, therefore has the great potential as highly sensitive resistor-type gas sensor.And metal sulfide semiconductor is received
Rice material has many advantages, such as that large specific surface area, surface state are controllable, preparation process also comparative maturity, in recent years in gas sensing side
The application in face starts to receive significant attention.
Semiconductor gas sensor includes resistance value, operating temperature, sensitivity, selectivity and stability and response speed
Multiple performance parameters such as degree, response/recovery time.Wherein the sensitivity (S) of gas sensor is gas sensor in clean sky
The ratio of resistance value (Ra) and the resistance value (Rg) in the environment full of tested gas in compression ring border, formula are as follows: S=Ra/Rg.
Sensitivity reflects gas sensor to the size of the sensitivity of tested gas, is the important parameter of detection gas sensor performance
And test index.Its application value in production and life of the usual higher gas sensitive of sensitivity is higher.
Response time is gas sensor and tested gas mutually encounter that resistance value reaches stable this period from beginning 90%.
It embodies gas sensor to the response speed of the under test gas in environment, and the response time of usual gas sensor is shorter to be turned out
Its response performance is better.Similarly, recovery time be gas sensor escape to from tested gas resistance value reach in cleaned air
Resistance value identical this period 90%.It embodies the speed that gas sensor is detached from tested gas, usual gas sensor
Shorter to turn out its restorability better recovery time.
The characteristic that two-dimentional (2D) nano structural material has due to it, thickness and big specific surface area such as nanoscale,
Make two-dimension nano materials that there is outstanding adsorption capacity to various chemical gas molecules, shows that they have good gas sensing
Performance.Molybdenum disulfide (MoS2) have unique two-dimensional layered structure, high-specific surface area, adjustable band-gap (1.2~1.8eV),
The advantages that nontoxicity, high mobility, high electric current of make-and-break are than with excellent mechanical strength is that there is high-performance sensing material under low temperature
The candidate material of future.
Graphite phase carbon nitride (g-C3N4) forbidden bandwidth it is moderate, electronics and hole can be improved with a variety of semiconductor couplings
Separative efficiency, be conducive to the transfer of electronics.By g-C3N4With MoS2It is compound, prepare g-C3N4/MoS2Gas sensor is realized
Material is integrated with function, plays the advantage of two kinds of materials, and the sensing capabilities for improving material are of great significance.
Ammonia is widely used in various industries production, but it is a kind of easy explosion and inflammable pernicious gas.It connects for a long time
Touching ammonia can cause very major injury to human body, therefore, prepare the ammonia gas biography of quick one kind, reliable, high sensitivity and selectivity
Sensor be currently there is an urgent need to.
Summary of the invention
The technical problem to be solved by the present invention is to for how quick, reliable, high sensitivity the inspection of above-mentioned existing issue
It surveys ammonia dangerous in industry production and a kind of preparation method of gas sensitive for detecting ammonia is provided, comprising the following steps:
(1) 1.30g ammonium molybdate and 2.30g thiocarbamide are taken and 35mL deionized water is added, is placed on magnetic stirring apparatus and stirs
30min forms homogeneous solution；
(2) solution in step (1) is transferred in 50mL reaction kettle, is kept for 24 hours in 180 DEG C of thermostatic drying chambers, later
Make reaction system cooled to room temperature, obtains reaction product A；
(3) the reaction product A in step (2) is collected by centrifugation, is washed repeatedly with water and dehydrated alcohol to neutrality, obtains product
B；
(4) the product B in step (3) is put into crucible, puts in a drying box drying 24 hours at 60 DEG C, obtains black
Color powder body material, saves backup；
(5) it takes 5g melamine to be placed in the crucible of capping, is forged with 2 DEG C/min heating rate to 500 DEG C in Muffle furnace
After burning 2h, it is continuously heating to 520 DEG C of calcining 2h, after cooled to room temperature, by product C3N4Grind into powder；
(6) 1g C is taken3N4It is placed in the crucible not covered, it is hot at 520 DEG C with 2 DEG C/min heating rate in Muffle furnace
4h is handled, g-C is obtained3N4Material, by gained sample grind into powder；
(7) g-C that concentration is 0.92mg/mL is respectively configured3N4The MoS of ethanol solution and 10mg/mL2Ethanol solution, ultrasound
30min is handled, colloidal solution is formed；
(8) g-C of 1~5mL is taken3N4Ethanol solution be added drop-wise to the MoS of 10mL2Ethanol solution in, mixed solution is existed
Magnetic agitation is heated for 24 hours at 60 DEG C, and product is collected by centrifugation, calcines 3h at 300 DEG C, is prepared into g-C3N4With MoS2Mass ratio is
0.92~4.60% g-C3N4/MoS2Composite material.
Gas sensor is prepared based on above-mentioned material the present invention also provides one kind and is used for ammonia detection method, including following step
It is rapid:
(1) with deionized water by g-C3N4/MoS2It is tuned into paste, g-C3N4/MoS2Mass ratio with deionized water is 1:
(0.5-1.5), then be coated in outside the ceramic tube equipped with platinum filament and two gold electrodes with fine, soft fur brush, the ceramics that will be coated later
Pipe puts in a drying box at 100 DEG C aging for 24 hours；
(2) take out aging ceramic tube, by resistance wire pass through its inside, later with tin by ceramic tube 6 filaments with
6 pillars one-to-one correspondence of gas sensor pedestal welds to get required gas sensor is arrived.
The present invention also provides application of the above-mentioned gas sensor in ammonia detection.
Positive beneficial effect of the invention is embodied in:
(1) preparation process is simple, environmental-friendly, and organic solvent-free is at low cost, it is easy to accomplish mass production.
(2) sensor gas sensor uses a certain amount of C3N4With MoS2Nano material compound method improves air-sensitive material
Expect the sensitivity and selectivity to ammonia.1.84% g-C3N4/MoS2At 120 DEG C of optimum working temperature, to the ammonia of 50ppm
Gas sensitivity reaches 21.2.
(3) sensor realizes detection hazardous gas ammonia quickly, reliable, highly sensitive, realizes portability and low function
Consumption.
Detailed description of the invention
C prepared by Fig. 1, embodiment 13N4/MoS2The transmission electron microscope figure of nanocomposite.
The detection sensitivity of sensor prepared by Fig. 2, Examples 1 to 5 to 50ppm ammonia.
Sensor prepared by Fig. 3, embodiment 1 is under the conditions of 120 DEG C to the response recovery curve of 50ppm ammonia.
The sensitivity of sensor prepared by Fig. 4, embodiment 1 under the conditions of 120 DEG C to the multiple gases of various concentration.
Specific embodiment
The present invention is further explained in the light of specific embodiments, but the present invention is not limited thereto.
Experimental method described in following embodiments is unless otherwise specified conventional method；The material, reagent etc., such as
Without specified otherwise, commercially obtain.
Embodiment 1
(1) 1.30g ammonium molybdate and 2.30g thiocarbamide are taken and 35mL deionized water is added, is placed on magnetic stirring apparatus and stirs
30min forms homogeneous solution；
(2) solution in step (1) is transferred in 50mL reaction kettle, is kept for 24 hours in 180 DEG C of thermostatic drying chambers, later
Make reaction system cooled to room temperature；
(3) product in step (2) is collected by centrifugation, is washed repeatedly with water and dehydrated alcohol to neutrality；
(4) product in step (3) is put into crucible, puts in a drying box drying 24 hours at 60 DEG C, obtains black
Powder body material saves backup；
(5) it takes 5g melamine to be placed in the crucible of capping, is forged with 2 DEG C/min heating rate to 500 DEG C in Muffle furnace
After burning 2h, it is continuously heating to 520 DEG C of calcining 2h, after cooled to room temperature, by product C3N4Grind into powder；
(6) 1g C is taken3N4It is placed in the crucible not covered, it is hot at 520 DEG C with 2 DEG C/min heating rate in Muffle furnace
4h is handled, g-C is obtained3N4Material, by gained sample grind into powder；
(7) g-C that concentration is 0.92mg/mL is respectively configured3N4The MoS of ethanol solution and 10mg/mL2Ethanol solution, ultrasound
30min is handled, colloidal solution is formed；
(8) g-C of 2mL is taken3N4Ultrasonic solution is added drop-wise to the MoS of 10mL2In solution, mixed solution is heated at 60 DEG C
For 24 hours, product is collected by centrifugation in magnetic agitation, calcines 3h at 300 DEG C, is prepared into g-C3N4With MoS2The g- that mass ratio is 1.84%
C3N4/MoS2Material.
Embodiment 2
Preparation method is substantially with embodiment 1, and being a difference in that for embodiment 1:
The g-C of 1mL is taken in step (8)3N4Ultrasonic solution is added drop-wise to the MoS of 10mL2In solution, it is prepared into g-C3N4With MoS2
The g-C that mass ratio is 0.92%3N4/MoS2Material.
Embodiment 3
Preparation method is substantially with embodiment 1, and being a difference in that for embodiment 1:
The g-C of 3mL is taken in step (8)3N4Ultrasonic solution is added drop-wise to the MoS of 10mL2In solution, it is prepared into g-C3N4With MoS2
The g-C that mass ratio is 2.76%3N4/MoS2Material.
Embodiment 4
Preparation method is substantially with embodiment 1, and being a difference in that for embodiment 1:
The g-C of 5mL is taken in step (8)3N4Ultrasonic solution is added drop-wise to the MoS of 10mL2In solution, it is prepared into g-C3N4With MoS2
The g-C that mass ratio is 4.60%3N4/MoS2Material.
Comparative example 1
Preparation method is substantially with embodiment 1, and being a difference in that for embodiment 1:
Step does not take g-C in (8)3N4Ultrasonic solution is added drop-wise to the MoS of 10mL2In solution, it is prepared into and does not add g-C3N4's
MoS2Material.
The present invention also provides a kind of based on above-mentioned material prepares gas sensor and for detecting different gas
(1) with deionized water by g-C3N4/MoS2It is tuned into paste, g-C3N4/MoS2Mass ratio with deionized water is 1:
(0.5-1.5), then be coated in outside the ceramic tube equipped with platinum filament and two gold electrodes with fine, soft fur brush, the ceramics that will be coated later
Pipe puts in a drying box at 100 DEG C aging for 24 hours.
(2) take out aging ceramic tube, by resistance wire pass through its inside, later with tin by ceramic tube 6 filaments with
6 pillars one-to-one correspondence of gas sensor pedestal welds to get required gas sensor is arrived.
(3) gas sensor is put into air chest, different amounts of gas, gas sensitive element to be detected is then added in air chest
After part resistance value is stablized, with S=Ra/Rg formula meter sensitivity, the detection sensitivity of gas with various is obtained.
Fig. 1 is 1.84%g-C3N4/MoS2The transmission electron microscope photo of sample, by observing g-C3N4/MoS2TEM
Picture confirms that sample is lamellar structure.
Fig. 2 is the g-C of different quality ratio3N4/MoS2Sensitivity of the sensor to 50ppm ammonia is surveyed under the conditions of 120 DEG C
Static volumetric method is used, with the g-C of different quality ratio3N4/MoS2Gas sensor is measured to 50ppm ammonia sensitivity.Its
The g-C of middle mass ratio 1.84%3N4/MoS2(embodiment 1) sensitivity reaches 22.1, is individual MoS2Sensor (comparative example 1)
6.94 times of sensitivity.
The g-C that Fig. 3 is 1.84%3N4/MoS2Sensor can learn its sound to the response recovery curve of 50ppm ammonia
Answer/recovery time is 19.4s and 28.5s, show that prepared gas sensor is preferable to the response speed of ammonia.
Fig. 4 is 1.84% g-C3N4/MoS2Sensor is under the conditions of 120 DEG C to the sensitive of the multiple gases of various concentration
It spends, gained 1.84%g-C is shown in figure3N4/MoS2Gas sensor is at 120 DEG C to methanol (50ppm), dehydrated alcohol
The sensitivity of (50ppm, 100ppm), acetic acid (50ppm), acetone (50ppm), corresponding sensitivity is respectively 0.88,0.90,
4.02,4.56 and 3.25, and 5.02 and 22.10 are had reached to the sensitivity of ammonia 20ppm, 50ppm.Obviously, 1.84% g-
C3N4/MoS2To the reaction of ammonia than more significant, 5~25 times higher than the reaction sensitivity that other are tested gas or so.
Claims (3)
1. a kind of preparation method for the gas sensitive for detecting ammonia, which comprises the following steps:
(1) 1.30g ammonium molybdate and 2.30g thiocarbamide are taken and 35mL deionized water is added, is placed on magnetic stirring apparatus and stirs 30min,
Form homogeneous solution；
(2) solution in step (1) is transferred in 50mL reaction kettle, is kept for 24 hours in 180 DEG C of thermostatic drying chambers, made later anti-
System cooled to room temperature is answered, reaction product A is obtained；
(3) the reaction product A in step (2) is collected by centrifugation, is washed repeatedly with water and dehydrated alcohol to neutrality, obtains product B；
(4) the product B in step (3) is put into crucible, puts in a drying box drying 24 hours at 60 DEG C, obtains black powder
Body material, saves backup；
(5) 5g melamine is taken to be placed in the crucible of capping, with 2 DEG C/min heating rate to 500 DEG C of calcining 2h in Muffle furnace
Afterwards, 520 DEG C of calcining 2h are continuously heating to, after cooled to room temperature, by product C3N4Grind into powder；
(6) 1g C is taken3N4It is placed in the crucible not covered, is heat-treated at 520 DEG C in Muffle furnace with 2 DEG C/min heating rate
4h obtains g-C3N4Material, by gained sample grind into powder；
(7) g-C that concentration is 0.92mg/mL is respectively configured3N4With the MoS of 10mg/mL2Ethanol solution is ultrasonically treated 30min, shape
At colloidal solution；
(8) g-C of 1~5mL is taken3N4Ethanol solution be added drop-wise to the MoS of 10mL2Ethanol solution in, the mixed solution that will obtain
Magnetic agitation is heated for 24 hours at 60 DEG C, and product is collected by centrifugation, calcines 3h at 300 DEG C, is prepared into g-C3N4With MoS2Mass ratio
For 0.92~4.60% g-C3N4/MoS2Composite material.
2. gas sensor made from a kind of preparation method of the gas sensitive of detection ammonia according to claim 1, special
Sign is, comprising the following steps:
(1) g-C that claim 1 is prepared with deionized water3N4/MoS2It is tuned into paste, g-C3N4/MoS2With deionized water
Mass ratio be 1:(0.5-1.5), then be coated in outside the ceramic tube equipped with platinum filament and two gold electrodes with fine, soft fur brush, later
The ceramic tube coated is put in a drying box at 100 DEG C aging for 24 hours；
(2) ceramic tube for taking out aging, resistance wire is passed through inside it, later with tin by 6 filaments and gas on ceramic tube
6 pillars one-to-one correspondence of sensor base welds to get required gas sensor is arrived.
3. application of the gas sensor according to claim 2 in ammonia detection.
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