CN105717167A - Preparation method and application of ammonia gas sensor based on two-dimensional magnetic composite nanomaterial - Google Patents
Preparation method and application of ammonia gas sensor based on two-dimensional magnetic composite nanomaterial Download PDFInfo
- Publication number
- CN105717167A CN105717167A CN201610101673.5A CN201610101673A CN105717167A CN 105717167 A CN105717167 A CN 105717167A CN 201610101673 A CN201610101673 A CN 201610101673A CN 105717167 A CN105717167 A CN 105717167A
- Authority
- CN
- China
- Prior art keywords
- ammonia gas
- preparation
- gas sensor
- salt
- feco
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 8
- 239000002131 composite material Substances 0.000 title abstract 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000010941 cobalt Substances 0.000 claims abstract description 6
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 6
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000011065 in-situ storage Methods 0.000 claims abstract description 5
- 229910052751 metal Inorganic materials 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims abstract description 5
- 238000001514 detection method Methods 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 150000003863 ammonium salts Chemical class 0.000 claims description 10
- 150000001868 cobalt Chemical class 0.000 claims description 10
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 10
- 150000002505 iron Chemical class 0.000 claims description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 6
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 6
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 239000002585 base Substances 0.000 claims description 5
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 5
- 239000000919 ceramic Substances 0.000 claims description 5
- 229910052571 earthenware Inorganic materials 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000004570 mortar (masonry) Substances 0.000 claims description 5
- 235000011837 pasties Nutrition 0.000 claims description 5
- 229910052697 platinum Inorganic materials 0.000 claims description 5
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 5
- 239000012498 ultrapure water Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 159000000013 aluminium salts Chemical class 0.000 claims description 4
- 229910000329 aluminium sulfate Inorganic materials 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 3
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 3
- 235000019270 ammonium chloride Nutrition 0.000 claims description 3
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 3
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 3
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 3
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 3
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 3
- 229940097267 cobaltous chloride Drugs 0.000 claims description 3
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 3
- 229910000358 iron sulfate Inorganic materials 0.000 claims description 3
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 3
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 2
- 239000001099 ammonium carbonate Substances 0.000 claims description 2
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 9
- 230000035945 sensitivity Effects 0.000 abstract description 5
- 230000008859 change Effects 0.000 abstract description 4
- 238000012544 monitoring process Methods 0.000 abstract description 3
- 229910052742 iron Inorganic materials 0.000 abstract 1
- 239000008204 material by function Substances 0.000 abstract 1
- 239000002135 nanosheet Substances 0.000 abstract 1
- 230000027756 respiratory electron transport chain Effects 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 20
- 229910021529 ammonia Inorganic materials 0.000 description 10
- 230000000694 effects Effects 0.000 description 5
- 239000002055 nanoplate Substances 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000009614 chemical analysis method Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- -1 pharmacy Substances 0.000 description 2
- JJEJDZONIFQNHG-UHFFFAOYSA-N [C+4].N Chemical compound [C+4].N JJEJDZONIFQNHG-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Chemical class [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 description 1
- 235000013877 carbamide Nutrition 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000007084 catalytic combustion reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 210000004877 mucosa Anatomy 0.000 description 1
- 239000000618 nitrogen fertilizer Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000241 respiratory effect Effects 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000011540 sensing material Substances 0.000 description 1
- 238000011896 sensitive detection Methods 0.000 description 1
- 230000035943 smell Effects 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention relates to a preparation method of an ammonia gas sensor, in particular to a gas-sensitive sensor established based on a two-dimensional flaky magnetic nanomaterial and belongs to the technical field of novel nano functional materials and environment monitoring. The sensor can be used for detecting the content of ammonia gas in an environment. An iron and cobalt bi-metal in-situ composite nitrogen-doped titanium dioxide nanosheet FeCo-N@TiO2 is prepared firstly. Through the characteristics that the material has the large specific area, and high mesoporous gas adsorption and multiple characteristics that electron transfer affects sensitivity due to the material surface gas change, the gas-sensitive sensor which is sensitive to and rapidly responds to the ammonia gas is established.
Description
Technical field
The present invention relates to the preparation method of a kind of ammonia gas sensor.Belong to Nano-function thin films and environmental monitoring technology field.
Background technology
Ammonia is the most often used to manufacture ammonia, nitrogenous fertilizer (carbamide, carbon ammonium etc.) etc., also has some inorganic salt containing nitrogen and orgnnic comopounds etc. the most all to need directly with ammonia as raw material.Therefore, ammonia has been widely used at field tools such as chemical industry, light industry, chemical fertilizer, pharmacy, synthetic fibers.But, ammonia exists the most in gaseous form, namely ammonia.Ammonia is a kind of colourless gas with intense stimulus abnormal smells from the patient, and the mucosa of skin, eyes and the respiratory apparatus of people is had stimulation, the effect of burning, if sucked too much, can cause lung swelling, so that dead.Although the zest of ammonia is reliable adverse concentration alarm signal, but due to olfactory fatigue, after Long Term Contact, the ammonia to low concentration can be difficult to discover, and forms potential danger.
Detection method currently for ammonia mainly has chemical analysis method and instrument testing method.Though chemical analysis method is simple to operate, but the shortcoming such as sensitivity is the highest and cannot reuse；Instrument testing method, main use ammonia gas instrumentation carries out detection by quantitative to the ammonia gas concentration in air, has highly sensitive, reusable, automaticity advantages of higher, and be widely applied in the middle of commercial production.
The ammonia gas detector used for instrument testing method, most crucial parts are the gas sensors to ammonia gas with qualitative, quantitative response, are namely coated with the gas sensor of different nano-functional material.Gas sensor is a kind of sensor detecting specific gas, and principle is velocity of wave based on SAW device and frequency can be drifted about with the change of external environment.It mainly includes semiconductor gas sensor, catalytic combustion type gas sensor and Electro-chemical Gas Sensor etc., and wherein most are semiconductor gas sensors.
Sensitivity is the important sign of gas sensor gas-sensitive property.Sensitivity definition is sensor resistance value in air atmosphereR a With sensor resistance value in certain density tested gas atmosphereR g Ratio, i.e.
Therefore, probe into that adsorptivity is strong, stability good, catalysis activity is high, have specific recognition to ammonia gas and can the gas sensing materials of detection by quantitative, and then preparation have highly sensitive, response quickly, the ammonia gas sensor of the characteristic such as recovery time is short has important using value to commercial production, human health, is also emphasis and the difficult point of environmental monitoring technology area research simultaneously.
Summary of the invention
It is an object of the invention to provide a kind of prepare simple, highly sensitive, detect quickly available in the preparation method of gas sensor of ammonia gas detection, prepared sensor, can be used for quick, the Sensitive Detection of ammonia gas.Based on this purpose, the method comprises the steps of firstly, preparing the nitrogen-doped titanium dioxide nanometer sheet FeCo-N@TiO of the magnetic Nano material of a kind of two-dimensional sheet, i.e. ferrum and cobalt dual-metal In-situ reaction2, utilize the specific surface area that this material is big, mesoporous high gas absorption characteristic and electron transmission to be affected many characteristics of sensitivity by the change of material surface gas, it is achieved that to have the structure of the gas sensor of response sensitive, quick to ammonia gas.
The technical solution used in the present invention is as follows:
1. a preparation method for ammonia gas sensor based on the nano combined nano material of two-dimensional magnetic, the nano combined nano material of described two-dimensional magnetic is the nitrogen-doped titanium dioxide nanometer sheet FeCo-N TiO of ferrum and cobalt dual-metal In-situ reaction2；
It is characterized in that, described preparation method includes following preparation process:
(1) FeCo-N@TiO2Preparation；
(2) preparation of ammonia gas sensor；
Wherein, step (1) prepares FeCo-N@TiO2Concretely comprise the following steps:
First, take 0.8 mmol iron salt, 0.8 ~ 1.2
Mmol cobalt salt and 1 mmol ammonium salt join in 5 mL butyl titanates, in whipping process, are slowly added to 0.5 ~ 0.8 mL Fluohydric acid., and 160 ~ 200
React in a kettle. at DEG C 18 ~ 24 hours, after being cooled to room temperature, after ultra-pure water and dehydrated alcohol centrifuge washing three times, be vacuum dried at 50 DEG C；Then, putting in Muffle furnace by the powder of grinding, programming rate is 1 ~ 3 DEG C/min, at 480 ~ 560 DEG C under nitrogen protection, calcines 10 ~ 60 min；Finally, the powder after calcining is cooled to room temperature, i.e. prepares FeCo-N@TiO2；
Described iron salt is selected from one of following: iron sulfate, iron chloride, ferric nitrate；
Described cobalt salt is selected from one of following: cobaltous sulfate, cobaltous chloride, cobalt nitrate；
Described ammonium salt is selected from one of following: ammonium sulfate, ammonium chloride, ammonium nitrate, ammonium carbonate；
Step (2) prepares concretely comprising the following steps of ammonia gas sensor:
First, the FeCo-N@TiO of preparation in step (1) is taken2
100 mg and 0.5 ~ 2.0 mmol aluminium salt are placed in mortar, add dehydrated alcohol, are coated uniformly on insulating ceramics tube-surface and form film, at room temperature dry after being ground to pasty state；Then, platinum filament and the heater strip of earthenware both sides are welded with base；Finally, the element welded is placed in detecting instrument, carries out burin-in process by regulation heating voltage to 4.22V, i.e. prepare ammonia gas sensor；
Described aluminium salt is selected from one of following: aluminum sulfate, aluminum chloride, aluminum nitrate.
The application of the ammonia gas sensor prepared by preparation method the most of the present invention, it is characterised in that can apply to the detection of ammonia gas, detection is limited to 0.02 mg/m3。
The useful achievement of the present invention
(1) ammonia gas sensor of the present invention preparation is simple, easy to operate, it is achieved that the selective enumeration method quick, sensitive, high to ammonia gas, has market development prospect；
(2) present invention is prepared for New Two Dimensional lamellar light-sensitive material FeCo-N TiO first2Fully contact with titanium dioxide nanoplate due to growth in situ on titanium dioxide nanoplate of ferrum, cobalt, utilize ferrum, the metal surface plasma body effect of cobalt and the mutual promoting action of the two, it is effectively increased semiconductor substrate electron transmission ability and catalysis activity, solve that although titanium dioxide nanoplate specific surface area is bigger and mesoporous high gas absorption characteristic is applicable to air-sensitive host material, but the technical problem that gas-sensitive activity is the highest and impedance variation is unstable；Simultaneously because the doping of nitrogen and make titanium dioxide nanoplate preferably strengthen layer gap spacing and fully dispersed, greatly increase the exposure of high energy crystal face of titanium dioxide nanoplate, electron transmission and fully dispersed, greatly increase electron transmission ability, solve the technical problem that air-sensitive host material impedance quickly responds with gas change；And, by aluminum ions doping, solve the technical problem of specific detection ammonia gas.Therefore, effective preparation of this material, there is important scientific meaning and using value.
Detailed description of the invention
Embodiment 1 FeCo-N@TiO2Preparation
First, 0.8 mmol iron salt and 0.8 is taken
Mmol cobalt salt and 1 mmol ammonium salt join in 5 mL butyl titanates, in whipping process, are slowly added to 0.5 mL Fluohydric acid., react in a kettle. at 160 DEG C 24 hours, after being cooled to room temperature, after ultra-pure water and dehydrated alcohol centrifuge washing three times, it is vacuum dried at 50 DEG C；Then, putting in Muffle furnace by the powder of grinding, programming rate is 1 DEG C/min, calcines 60 min at 480 DEG C；Finally, the powder after calcining is cooled to room temperature, i.e. prepares FeCo-N@TiO2；
Described iron salt is iron sulfate；
Described cobalt salt is cobaltous sulfate；
Described ammonium salt is ammonium sulfate.
Embodiment 2 FeCo-N@TiO2Preparation
First, 0.8 mmol iron salt and 1.0 is taken
Mmol cobalt salt and 1 mmol ammonium salt join in 5 mL butyl titanates, in whipping process, are slowly added to 0.65 mL Fluohydric acid., react in a kettle. at 180 DEG C 21 hours, after being cooled to room temperature, after ultra-pure water and dehydrated alcohol centrifuge washing three times, it is vacuum dried at 50 DEG C；Then, putting in Muffle furnace by the powder of grinding, programming rate is 2 DEG C/min, calcines 30 min at 520 DEG C；Finally, the powder after calcining is cooled to room temperature, i.e. prepares FeCo-N@TiO2；
Described iron salt is iron chloride；
Described cobalt salt is cobaltous chloride；
Described ammonium salt is ammonium chloride.
Embodiment 3 FeCo-N@TiO2Preparation
First, 0.8 mmol iron salt and 1.2 is taken
Mmol cobalt salt and 1 mmol ammonium salt join in 5 mL butyl titanates, in whipping process, are slowly added to 0.8 mL Fluohydric acid., react in a kettle. at 200 DEG C 18 hours, after being cooled to room temperature, after ultra-pure water and dehydrated alcohol centrifuge washing three times, it is vacuum dried at 50 DEG C；Then, putting in Muffle furnace by the powder of grinding, programming rate is 3 DEG C/min, calcines 10 min at 560 DEG C；Finally, the powder after calcining is cooled to room temperature, i.e. prepares FeCo-N@TiO2；
Described iron salt is ferric nitrate；
Described cobalt salt is cobalt nitrate；
Described ammonium salt is ammonium nitrate.
Embodiment 4The preparation of ammonia gas sensor
First, the FeCo-N@TiO of preparation in Example 12
100 mg and 0.5 mmol aluminum sulfate are placed in mortar, add dehydrated alcohol, are coated uniformly on insulating ceramics tube-surface and form film, at room temperature dry after being ground to pasty state；Then, platinum filament and the heater strip of earthenware both sides are welded with base；Finally, being placed in detecting instrument by the element welded, carry out burin-in process by regulation heating voltage to 4.22V, i.e. prepare ammonia gas sensor, be applied to the detection of ammonia gas, detection is limited to 0.02 mg/m3。
Embodiment 5 The preparation of ammonia gas sensor
First, the FeCo-N@TiO of preparation in Example 22
100 mg and 1.2 mmol aluminum chloride are placed in mortar, add dehydrated alcohol, are coated uniformly on insulating ceramics tube-surface and form film, at room temperature dry after being ground to pasty state；Then, platinum filament and the heater strip of earthenware both sides are welded with base；Finally, being placed in detecting instrument by the element welded, carry out burin-in process by regulation heating voltage to 4.22V, i.e. prepare ammonia gas sensor, be applied to the detection of ammonia gas, detection is limited to 0.02 mg/m3。
Embodiment 6 The preparation of ammonia gas sensor
First, the FeCo-N@TiO of preparation in Example 32
100 mg and 2.0 mmol aluminum nitrates are placed in mortar, add dehydrated alcohol, are coated uniformly on insulating ceramics tube-surface and form film, at room temperature dry after being ground to pasty state；Then, platinum filament and the heater strip of earthenware both sides are welded with base；Finally, being placed in detecting instrument by the element welded, carry out burin-in process by regulation heating voltage to 4.22V, i.e. prepare ammonia gas sensor, be applied to the detection of ammonia gas, detection is limited to 0.02 mg/m3。
Claims (2)
1. a preparation method for ammonia gas sensor based on the nano combined nano material of two-dimensional magnetic, the nano combined nano material of described two-dimensional magnetic is the nitrogen-doped titanium dioxide nanometer sheet FeCo-N TiO of ferrum and cobalt dual-metal In-situ reaction2；
It is characterized in that, described preparation method includes following preparation process:
(1) FeCo-N@TiO2Preparation；
(2) preparation of ammonia gas sensor；
Wherein, step (1) prepares FeCo-N@TiO2Concretely comprise the following steps:
First, take 0.8 mmol iron salt, 0.8 ~ 1.2 mmol cobalt salt and 1 mmol ammonium salt and join in 5 mL butyl titanates, in whipping process, it is slowly added to 0.5 ~ 0.8 mL Fluohydric acid., react in a kettle. at 160 ~ 200 DEG C 18 ~ 24 hours, after being cooled to room temperature, after ultra-pure water and dehydrated alcohol centrifuge washing three times, it is vacuum dried at 50 DEG C；Then, putting in Muffle furnace by the powder of grinding, programming rate is 1 ~ 3 DEG C/min, at 480 ~ 560 DEG C under nitrogen protection, calcines 10 ~ 60 min；Finally, the powder after calcining is cooled to room temperature, i.e. prepares FeCo-N@TiO2；
Described iron salt is selected from one of following: iron sulfate, iron chloride, ferric nitrate；
Described cobalt salt is selected from one of following: cobaltous sulfate, cobaltous chloride, cobalt nitrate；
Described ammonium salt is selected from one of following: ammonium sulfate, ammonium chloride, ammonium nitrate, ammonium carbonate；
Step (2) prepares concretely comprising the following steps of ammonia gas sensor:
First, the FeCo-N@TiO of preparation in step (1) is taken2100 mg and 0.5 ~ 2.0 mmol aluminium salt are placed in mortar, add dehydrated alcohol, are coated uniformly on insulating ceramics tube-surface and form film, at room temperature dry after being ground to pasty state；Then, platinum filament and the heater strip of earthenware both sides are welded with base；Finally, the element welded is placed in detecting instrument, carries out burin-in process by regulation heating voltage to 4.22V, i.e. prepare ammonia gas sensor；
Described aluminium salt is selected from one of following: aluminum sulfate, aluminum chloride, aluminum nitrate.
2. the application of the ammonia gas sensor prepared by preparation method as claimed in claim 1, it is characterised in that can apply to the detection of ammonia gas, detection is limited to 0.02 mg/m3。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610101673.5A CN105717167B (en) | 2016-02-25 | 2016-02-25 | A kind of preparation method and application of the ammonia gas sensor based on the nano combined nano material of two-dimensional magnetic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610101673.5A CN105717167B (en) | 2016-02-25 | 2016-02-25 | A kind of preparation method and application of the ammonia gas sensor based on the nano combined nano material of two-dimensional magnetic |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105717167A true CN105717167A (en) | 2016-06-29 |
| CN105717167B CN105717167B (en) | 2018-06-22 |
Family
ID=56157031
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610101673.5A Expired - Fee Related CN105717167B (en) | 2016-02-25 | 2016-02-25 | A kind of preparation method and application of the ammonia gas sensor based on the nano combined nano material of two-dimensional magnetic |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105717167B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102249299A (en) * | 2011-05-27 | 2011-11-23 | 新疆大学 | Method for preparing TiO2 overlong micro rod in NaCl molten salt system |
| CN103949232A (en) * | 2014-04-30 | 2014-07-30 | 上海师范大学 | TiO2 photocatalyst with mesoporous structure, as well as preparation method and applications of photocatalyst |
| CN104233206A (en) * | 2014-06-30 | 2014-12-24 | 左娟 | Preparation method and application of Fe-doped nanotube array membrane |
| CN105126886A (en) * | 2015-07-01 | 2015-12-09 | 宁波工程学院 | Preparation method of TiO<2>/WO<3>/g-C<3>N<4> thoroughly mesoporous nanofibers |
| CN105301062A (en) * | 2015-10-29 | 2016-02-03 | 东北大学 | Gas sensor based on graded porous WO3 microspheres and preparation method thereof |
-
2016
- 2016-02-25 CN CN201610101673.5A patent/CN105717167B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102249299A (en) * | 2011-05-27 | 2011-11-23 | 新疆大学 | Method for preparing TiO2 overlong micro rod in NaCl molten salt system |
| CN103949232A (en) * | 2014-04-30 | 2014-07-30 | 上海师范大学 | TiO2 photocatalyst with mesoporous structure, as well as preparation method and applications of photocatalyst |
| CN104233206A (en) * | 2014-06-30 | 2014-12-24 | 左娟 | Preparation method and application of Fe-doped nanotube array membrane |
| CN105126886A (en) * | 2015-07-01 | 2015-12-09 | 宁波工程学院 | Preparation method of TiO<2>/WO<3>/g-C<3>N<4> thoroughly mesoporous nanofibers |
| CN105301062A (en) * | 2015-10-29 | 2016-02-03 | 东北大学 | Gas sensor based on graded porous WO3 microspheres and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 姜洪泉，王城英等: "N掺杂TiO2纳米粉体的表面特性及可见光活性", 《材料科学与工程学报》 * |
| 戴振清、孙以材等: "金属氧化物掺杂对TiO2气敏特性的影响", 《传感器世界》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105717167B (en) | 2018-06-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Rahman et al. | Carbon black co-adsorbed ZnO nanocomposites for selective benzaldehyde sensor development by electrochemical approach for environmental safety | |
| CN105717168B (en) | A kind of preparation method and application of the these hydrogen sulfide gas sensor based on titanium dioxide nanoplate carried noble metal | |
| Queralto et al. | Detecting cancer by breath volatile organic compound analysis: a review of array-based sensors | |
| CN105699439B (en) | A kind of preparation method and application of the methanol gas sensor based on carbonitride carried metal and metal oxide composite | |
| Yang et al. | One-pot synthesis of SnO2 hollow microspheres and their formaldehyde sensor application | |
| Wu et al. | VOCs gas sensor based on MOFs derived porous Au@ Cr2O3-In2O3 nanorods for breath analysis | |
| Sun et al. | Chemiresistive sensor arrays based on noncovalently functionalized multi-walled carbon nanotubes for ozone detection | |
| CN109342522B (en) | Polypyrrole/graphene composite material-based resistance type NH3Sensor, preparation method and application thereof | |
| CN105158303A (en) | Precious metal/base metal oxide/graphene ternary composite gas sensitive material and preparation method thereof | |
| Zou et al. | Sensitive and selective n-butanol gas detection based on ZnO nanocrystalline synthesized by a low-temperature solvothermal method | |
| Cheng et al. | High performance ammonia gas detection based on TiO2/WO3· H2O heterojunction sensor | |
| CN105158412B (en) | The preparation method of the aromatic hydrocarbons gas sensor that a kind of bimetallic alloy nano composite material based on molybdenum bisuphide load builds | |
| Tian et al. | Trace level detection of hydrogen gas using birnessite-type manganese oxide | |
| CN105606655B (en) | A kind of preparation method and application of the acetone gas sensor based on two-dimentional porous nano composite material supported palladium | |
| CN104502415B (en) | A kind of preparation method of the ammonia gas sensor based on noble metal composite-material structure | |
| CN109437329A (en) | A kind of Co3O4/ graphene composite material and its preparation method and application | |
| Tang et al. | Cataluminescence gas sensor for ketones based on nanosized NaYF4: Er | |
| CN105021656B (en) | A kind of preparation method of chloroform gas sensor | |
| CN105628745A (en) | Preparation method and application for nitrogen dioxide gas sensor based on titanium-dioxide-based porous nanocomposite | |
| CN105699438A (en) | Method for preparing explosive sensor array based on manganese-doped zinc sulfide nano-crystal | |
| CN105717167A (en) | Preparation method and application of ammonia gas sensor based on two-dimensional magnetic composite nanomaterial | |
| Xu et al. | High efficiency triethylamine gas sensor based on SmVO4 nano octahedron granules | |
| CN105758994B (en) | A kind of preparation method and application of the formaldehyde gas sensor based on carbonitride load additive Mn two-dimensional nano composite | |
| CN105572176B (en) | A kind of preparation method and application of the toluene gas sensor based on base metal doped and compounded material | |
| CN105572175B (en) | A kind of preparation method and application of the dimethylbenzene gas sensor based on titanium dioxide nanoplate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20230116 Address after: No. 37, Jingwu Road, Huaiyin District, Jinan City, Shandong Province, 250001 Patentee after: Luyan Engineering Technology Consulting Co.,Ltd. Address before: No. 336, West Road, South Xin Zhuang, Shandong, Shandong Patentee before: University of Jinan |
|
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20180622 |