CN108680609A - It is a kind of using p-type delafossite structure oxide as room temperature ammonia gas sensor of sensitive material and preparation method thereof - Google Patents
It is a kind of using p-type delafossite structure oxide as room temperature ammonia gas sensor of sensitive material and preparation method thereof Download PDFInfo
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- CN108680609A CN108680609A CN201810212137.1A CN201810212137A CN108680609A CN 108680609 A CN108680609 A CN 108680609A CN 201810212137 A CN201810212137 A CN 201810212137A CN 108680609 A CN108680609 A CN 108680609A
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- room temperature
- sensitive
- gas sensor
- ammonia gas
- delafossite structure
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
Abstract
The invention discloses a kind of using p-type delafossite structure oxide as room temperature ammonia gas sensor of sensitive material and preparation method thereof.For the first time p-type delafossite structure AgAlO2As the sensitive material of ammonia gas sensor, a kind of resistance-type room temperature ammonia gas sensor of function admirable is constructed.The sensor takes full advantage of simple semiconductor resistance-type sensing material high sensitivity, at low cost, device, being easily integrated, is easily achieved live the advantages of continuously detecting and AgAlO2At room temperature to ammonia high selectivity the characteristics of, construct can working and room temperature and to ammonia respond it is sensitive（Monitoring lower-cut can reach million ranks）, selectivity is good, stability is good and economic and environment-friendly resistance sensor, while being also that ammonia gas sensor has found a kind of good sensitive material, more p-type broad-band gap delafossite structure oxide opens a kind of new application field.
Description
Technical field
The invention belongs to sensitive material and sensor technical fields, and in particular to a kind of to be aoxidized with p-type delafossite structure
Object is the room temperature ammonia gas sensor and preparation method thereof of sensitive material.
Background technology
Ammonia has been widely used in the fields such as chemical industry, light industry, chemical fertilizer, pharmacy, synthetic fibers tool, is often used to manufacture ammonia
Water, nitrogenous fertilizer（Urea, ammonium bicarbonate etc.）Deng, also some inorganic salt containing nitrogens and orgnnic comopounds etc. also all need directly with ammonia be original
Material.Ammonia exists in gaseous form at normal temperatures and pressures, referred to as ammonia.Ammonia is a kind of colourless with intense irritation smell
Gas has stimulation, effect of burning to the mucous membrane of the skin of people, eyes and respiratory apparatus, if sucking is excessive, can cause lung
Swelling, so that it is dead.Metal semiconductor material is a kind of material for being applied to ammonia gas sensor earliest, mainly by contact ammonia
Conductivity variations before and after gas are detected, and have many advantages, such as of low cost, high sensitivity, easy to carry.But current ammonia passes
Sensor is there are poor selectivity, the response-recovery time is long, need to be in high temperature（>150℃）The shortcomings of work.
Invention content
The present invention in view of the above-mentioned deficiencies in the prior art, provides a kind of, selectivity high to ammonia response sensitivity
It is good, stability is strong, the response-recovery time is short and in the novel ammonia gas sensor and preparation method thereof of working and room temperature.
In order to achieve the above objectives, the present invention uses following technical scheme：
It is a kind of using p-type delafossite structure oxide as the room temperature ammonia gas sensor of sensitive material, including gas sensitive close substrate, institute
It states gas sensitive and is coated uniformly on the substrate surface, the gas sensitive ingredient is p-type delafossite structure AgAlO2Nanometer
Grain, the gas sensitive coating thickness are 500 nm-100 μm.
The p-type delafossite structure AgAlO2The particle size range of nano particle is 20 nm-600nm.
The substrate is the Al with Pt, Au or Al electrode2O3Substrate.
It is a kind of using p-type delafossite structure oxide as the preparation method of the room temperature ammonia gas sensor of sensitive material, including with
Lower step：
Step 1 prepares p-type delafossite structure AgAlO2Nano particle：
By Al (NO3)3·9H2O and AgNO3It is dissolved in deionized water, NaOH is added after dissolving, above-mentioned solution is poured into polytetrafluoro
In ethylene liner, liner compactedness is 60%-70%, and autoclave is put into 24-64 hours postcoolings of 190-230 DEG C of reaction in baking oven
It takes out, silvery white powder is washed using 1M/L weak aqua ammonias, 1M/L dust technologies, deionized water, dried for standby to room temperature；
Step 2 prepares gas sensitive slurry：
By p-type delafossite structure AgAlO2Nano particle and absolute ethyl alcohol, ethyl cellulose, terpinol mixing, magnetic agitation are equal
It is even, obtain gas sensitive slurry；
Step 3 prepares ammonia gas sensor：
The gas sensitive slurry of above-mentioned preparation is coated on substrate and forms air-sensitive film, the gas sensitive coating thickness is 1 μ
m-100μm；Air-sensitive film is sintered 1-4 hours at 300-500 DEG C, final gained is AgAlO2Ammonia gas sensor.
Wherein, Al (NO in the step 13)3·9H2O、AgNO3Molar ratio with NaOH is 1：（0.8-1.5）：（2-
6）.
Wherein, the p-type delafossite structure AgAlO in the step 22The weight ratio of powder, ethyl cellulose, terpinol
It is 1：（0.5-2）：（0.5-2）.
Wherein, air-sensitive film sintering atmosphere can be air, vacuum or N in the step 32, Ar inert atmospheres.
Ammonia gas sensor of the present invention is Gas Sensors of Electric Resistance Semiconductors, mainly according to the electricity before and after element adsorbed gas
Resistive is detected, and is physically or chemically inhaled, is desorbed on sensitive material using under test gas, causes material resistance etc.
Change in electrical properties is to reach testing goal.Ammonia gas sensor operating temperature of the present invention is within the scope of room temperature；Sensor resistance
Changing in moving air and using air as the ammonia gas of background in the environment of makes sensor signal generate；Sensor it is real-time
Monitoring signals are the variations of sensor resistance.
Compared with prior art, the present invention has the following advantages：
1, ammonia gas sensor manufacture craft of the invention is simple and convenient to operate.
2, p-type delafossite structure AgAlO of the invention2Nano particle has high sensitivity to ammonia response（Monitoring lower-cut
It can reach million ranks）, response recovery time is short and stability is good advantage；Also it is that ammonia gas sensor has found one kind very simultaneously
Good sensitive material, more p-type broad-band gap delafossite structure oxide open a kind of new application field.
3, the sensor prepared by the present invention has good selectivity to ammonia, for other common gas（As methanol,
Toluene, acetone, absolute ethyl alcohol etc.）It is insensitive, it can quickly and effectively detect ammonia in numerous mixed gas.
4, the ammonia gas sensor that the present invention prepares is operated in room temperature, is not necessarily to heater element and temperature measuring device, eliminates attached
Add structure, and avoids integral device aging or damage under long-time hot operation.
Description of the drawings
Fig. 1 is p-type delafossite structure AgAlO in embodiment 12The X-ray diffractogram of nano particle；
Fig. 2 is p-type delafossite structure AgAlO in embodiment 12The stereoscan photograph of nano particle；
Fig. 3 is p-type delafossite structure AgAlO in embodiment 12The x-ray photoelectron spectroscopy of nano particle；
Fig. 4 is that ammonia gas sensor prepared by the embodiment of the present invention 1 at room temperature becomes the resistance of several escaping gas of 100 ppm
Change response diagram；
Fig. 5 is ammonia gas sensor of the present invention at room temperature to 20-100 ppm NH3Resistance variations response diagram；Ra is sensor
Aerial resistance value, Rg are resistance value of the sensor in tested gas.
Specific implementation mode
Below in conjunction with the accompanying drawings and the present invention is discussed in detail in specific embodiment.But embodiment below is only limitted to explain this hair
Bright, protection scope of the present invention should include the full content of claim, be not limited only to the present embodiment.
Embodiment 1
It is a kind of using p-type delafossite structure oxide as the room temperature ammonia gas sensor of sensitive material, including gas sensitive and substrate, gas
Quick material is coated uniformly on substrate surface, and gas sensitive coating thickness is 10 μm, and gas sensitive is p-type delafossite structure AgAlO2
Nano particle, particle diameter 200nm-500nm；
Preparation method includes the following steps：
Step 1 prepares p-type delafossite structure AgAlO2Nano particle：By 0.015mol Al (NO3)3·9H2O and 0.015mol
AgNO3It is dissolved in 70 ml deionized waters, 2.4 g NaOH is added after dissolving, above-mentioned solution is poured into 100ml polytetrafluoroethylene (PTFE)
In lining, autoclave is put into 210 DEG C of 64 hours postcoolings of reaction to room temperature in baking oven and is taken out, silvery white powder is dilute using 1M/L
Ammonium hydroxide, 1M/L dust technologies, deionized water washing, dried for standby；
Step 2 prepares gas sensitive slurry：By 0.2 g p-type delafossite structures AgAlO2Nano particle and the anhydrous second of 3 ml
Alcohol, 0.05g M9 ethyl celluloses, the mixing of 0.2 g terpinols, magnetic agitation is uniform, obtains gas sensitive slurry；
Step 3 prepares ammonia gas sensor：It is thin that the gas sensitive slurry of above-mentioned preparation is coated uniformly on formation air-sensitive on substrate
Film, the gas sensitive coating thickness are 4 μm.Air-sensitive film is sintered 4 hours at 400 DEG C, final gained is AgAlO2Ammonia
Gas sensor.
The p-type delafossite structure AgAlO obtained in the present embodiment2Nano particle, through X-ray diffraction and scanning electron microscopy
Mirror characterizes, and obtained result is shown in Fig. 1, Fig. 2 and Fig. 3 in attached drawing.
Embodiment 2
It is a kind of using p-type delafossite structure oxide as the room temperature ammonia gas sensor of sensitive material, including gas sensitive and substrate, gas
Quick material is coated uniformly on substrate surface, and gas sensitive coating thickness is 50 μm, and gas sensitive is p-type delafossite structure AgAlO2
Nano particle, particle diameter are 1 μm -3 μm；
Preparation method includes the following steps：
Step 1 prepares p-type delafossite structure AgAlO2Nano particle：By 0.015mol Al (NO3)3·9H2O and
0.01575mol AgNO3It is dissolved in 70 ml deionized waters, 3 g NaOH is added after dissolving, above-mentioned solution is poured into 100ml and is gathered
In tetrafluoroethene liner, autoclave is put into 220 DEG C of 64 hours postcoolings of reaction to room temperature in baking oven and is taken out, by silvery white powder
It is washed using 1M/L weak aqua ammonias, 1M/L dust technologies, deionized water, dried for standby；
Step 2 prepares gas sensitive slurry：By 0.2 g p-type delafossite structures AgAlO2Nano particle and the anhydrous second of 2 ml
Alcohol, 0.05g M9 ethyl celluloses, the mixing of 0.2 g terpinols, magnetic agitation is uniform, obtains gas sensitive slurry；
Step 3 prepares ammonia gas sensor：It is thin that the gas sensitive slurry of above-mentioned preparation is coated uniformly on formation air-sensitive on substrate
Film, the gas sensitive coating thickness are 50 μm.Air-sensitive film is sintered 4 hours at 350 DEG C, final gained is AgAlO2
Ammonia gas sensor.
Embodiment 3
It is a kind of using p-type delafossite structure oxide as the room temperature ammonia gas sensor of sensitive material, including gas sensitive and substrate, gas
Quick material is coated uniformly on substrate surface, and gas sensitive coating thickness is 100 μm, and gas sensitive is p-type delafossite structure
AgAlO2Nano particle, particle diameter range 200nm-500nm；
Preparation method includes the following steps：
Step 1 prepares p-type delafossite structure AgAlO2Nano particle：By 0.015mol Al (NO3)3·9H2O and 0.015mol
AgNO3It is dissolved in 70 ml deionized waters, 2.4 g NaOH is added after dissolving, above-mentioned solution is poured into 100ml polytetrafluoroethylene (PTFE)
In lining, autoclave is put into 220 DEG C of 64 hours postcoolings of reaction to room temperature in baking oven and is taken out, silvery white powder is dilute using 1M/L
Ammonium hydroxide, 1M/L dust technologies, deionized water washing, dried for standby；
Step 2 prepares gas sensitive slurry：By 0.3 g p-type delafossite structures AgAlO2Nano particle and the anhydrous second of 2 ml
Alcohol, 0.05g M9 ethyl celluloses, the mixing of 0.2 g terpinols, magnetic agitation is uniform, obtains gas sensitive slurry；
Step 3 prepares ammonia gas sensor：It is thin that the gas sensitive slurry of above-mentioned preparation is coated uniformly on formation air-sensitive on substrate
Film, the gas sensitive coating thickness are 100 μm.Air-sensitive film is sintered 4 hours at 500 DEG C, final gained is AgAlO2
Ammonia gas sensor.
4 ammonia gas sensor performance test of embodiment
Sensor prepared by embodiment 1-3 is placed under air environment, operating temperature is room temperature, ambient air humidity 35%RH,
Then NH is introduced3Gas molecule.By multimeter measurement sensor in air and using air as the various concentration NH of background3Ring
Resistance variations under border, the signal as sensor.By taking the ammonia gas sensor that embodiment 1 is prepared as an example, compares figure 4 is subject to
Illustrate, Fig. 4 gives prepared sensor for several escaping gas such as ethyl alcohol, methanol, propyl alcohol and NH3At room temperature
Electrical response compares, it can be found that the sensor is to NH3Response be other gases several times, show the sensor to NH3Sound
Answer sensitivity higher.Fig. 5 give prepared sensor 20 ~ 100ppm NH3Under environment, the variation feelings of sensor resistance
Condition.In the NH of 100ppm3Under environment, the response time of sensor is 29s, recovery time 49s.Relative to other similar sensings
Device, inventive sensor is to NH3Response and resume speed it is fast.
It should be noted that according to the various embodiments described above of the present invention, those skilled in the art are that this hair may be implemented completely
Bright independent claims and the full scope of appurtenance, realize process and the same the various embodiments described above of method；And the present invention is not
It elaborates and partly belongs to techniques well known.
The above, part specific implementation mode only of the present invention, but scope of protection of the present invention is not limited thereto, appoints
In the technical scope disclosed by the present invention, the change or replacement that can be readily occurred in should all be covered what those skilled in the art
Within protection scope of the present invention.
Claims (7)
1. it is a kind of using p-type delafossite structure oxide as the room temperature ammonia gas sensor of sensitive material, including gas sensitive conjunction substrate,
The gas sensitive is coated uniformly on the substrate surface, which is characterized in that the gas sensitive ingredient is p-type delafossite structure
AgAlO2Nano particle, the gas sensitive coating thickness are 500nm-100 μm.
2. it is according to claim 1 a kind of using p-type delafossite structure oxide as the room temperature ammonia gas sensor of sensitive material,
It is characterized in that, the p-type delafossite structure AgAlO2The particle size range of nano particle is 20 nm-600nm.
3. according to claim 1 or 2 a kind of using p-type delafossite structure oxide as the room temperature ammonia of sensitive material sensing
Device, which is characterized in that the substrate is the Al with Pt, Au or Al electrode2O3Substrate.
4. a kind of using p-type delafossite structure oxide as the preparation method of the room temperature ammonia gas sensor of sensitive material, feature exists
In including the following steps：
Step 1 prepares p-type delafossite structure AgAlO2Nano particle：
By Al (NO3)3·9H2O and AgNO3It is dissolved in deionized water, NaOH is added after dissolving, above-mentioned solution is poured into polytetrafluoroethyl-ne
In alkene liner, liner compactedness is 60%-70%, and autoclave is put into baking oven and reacts 24-64 hours postcoolings extremely for 190-230 DEG C
Room temperature is taken out, and silvery white powder is washed using 1M/L weak aqua ammonias, 1M/L dust technologies, deionized water, dried for standby；
Step 2 prepares gas sensitive slurry：
By p-type delafossite structure AgAlO2Nano particle and absolute ethyl alcohol, ethyl cellulose, terpinol mixing, magnetic agitation are equal
It is even, obtain gas sensitive slurry；
Step 3 prepares ammonia gas sensor：
The gas sensitive slurry of above-mentioned preparation is coated on substrate and forms air-sensitive film, the gas sensitive coating thickness is 1 μ
m-100μm；Air-sensitive film is sintered 1-4 hours at 300-500 DEG C, final gained is AgAlO2Ammonia gas sensor.
5. the preparation method of room temperature ammonia gas sensor according to claim 4, which is characterized in that Al in the step 1
(NO3)3·9H2O、AgNO3Molar ratio with NaOH is 1：（0.8-1.5）：（2-6）.
6. the preparation method of room temperature ammonia gas sensor according to claim 4, which is characterized in that the p in the step 2
Type delafossite structure AgAlO2Powder, ethyl cellulose, terpinol weight ratio be 1：（0.5-2）：（0.5-2）.
7. the preparation method of room temperature ammonia gas sensor according to claim 4, which is characterized in that air-sensitive in the step 3
Film sintered atmosphere can be air, vacuum or N2, Ar inert atmospheres.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113376221A (en) * | 2021-06-15 | 2021-09-10 | 上海航天科工电器研究院有限公司 | Acetone gas sensor and preparation method thereof |
| CN114577862A (en) * | 2022-02-16 | 2022-06-03 | 中国科学院合肥物质科学研究院 | Ozone gas sensor and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113376221A (en) * | 2021-06-15 | 2021-09-10 | 上海航天科工电器研究院有限公司 | Acetone gas sensor and preparation method thereof |
| CN114577862A (en) * | 2022-02-16 | 2022-06-03 | 中国科学院合肥物质科学研究院 | Ozone gas sensor and preparation method and application thereof |
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