CN105717167B - A kind of preparation method and application of the ammonia gas sensor based on the nano combined nano material of two-dimensional magnetic - Google Patents
A kind of preparation method and application of the ammonia gas sensor based on the nano combined nano material of two-dimensional magnetic Download PDFInfo
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- CN105717167B CN105717167B CN201610101673.5A CN201610101673A CN105717167B CN 105717167 B CN105717167 B CN 105717167B CN 201610101673 A CN201610101673 A CN 201610101673A CN 105717167 B CN105717167 B CN 105717167B
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001514 detection method Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 8
- 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
- 229910052742 iron Inorganic materials 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
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-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
- 238000010438 heat treatment Methods 0.000 claims description 10
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 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
- 239000000919 ceramic Substances 0.000 claims description 9
- 230000008569 process Effects 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
- 230000015572 biosynthetic process Effects 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
- 238000000227 grinding Methods 0.000 claims description 5
- 239000004570 mortar (masonry) Substances 0.000 claims description 5
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 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
- 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
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-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
- 239000001099 ammonium carbonate Substances 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
- 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
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 3
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 3
- 229910000360 iron(III) sulfate Inorganic materials 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
- 229910000329 aluminium sulfate Inorganic materials 0.000 claims description 2
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 2
- 229910052573 porcelain Inorganic materials 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 9
- 230000004044 response Effects 0.000 abstract description 5
- 230000005540 biological transmission Effects 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000012544 monitoring process Methods 0.000 abstract description 3
- 239000010409 thin film Substances 0.000 abstract description 2
- 229910002546 FeCo Inorganic materials 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 19
- 229910021529 ammonia Inorganic materials 0.000 description 9
- 230000035945 sensitivity Effects 0.000 description 6
- 238000001354 calcination Methods 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 239000002055 nanoplate Substances 0.000 description 4
- 238000007689 inspection Methods 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
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000009614 chemical analysis method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 230000007794 irritation Effects 0.000 description 2
- -1 pharmacy Substances 0.000 description 2
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229910003087 TiOx Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 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
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000007084 catalytic combustion reaction Methods 0.000 description 1
- 238000012512 characterization method 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
- 229910052738 indium Inorganic materials 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
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 239000000618 nitrogen fertilizer Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 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
- 238000001179 sorption measurement Methods 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
- HLLICFJUWSZHRJ-UHFFFAOYSA-N tioxidazole Chemical compound CCCOC1=CC=C2N=C(NC(=O)OC)SC2=C1 HLLICFJUWSZHRJ-UHFFFAOYSA-N 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 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
Abstract
The present invention relates to a kind of preparation method of ammonia gas sensor, specifically based on the gas sensor constructed by the magnetic Nano material of two-dimensional sheet, available for ammonia gas content in detection environment.Belong to Nano-function thin films and environmental monitoring technology field.The method comprises the steps of firstly, preparing a kind of iron and the nitrogen-doped titanium dioxide nanometer sheet FeCo N@TiO of cobalt dual-metal In-situ reaction2, changed using the big specific surface area of the material, mesoporous high gas absorption characteristic and electron transmission by material surface gas and influence sensitive many characteristics, realize the structure that there is sensitive, quick response gas sensor to ammonia gas.
Description
Technical field
The present invention relates to a kind of preparation methods of ammonia gas sensor.Belong to Nano-function thin films and environmental monitoring
Technical field.
Background technology
Ammonia is industrially often used to manufacture ammonium hydroxide, nitrogenous fertilizer（Urea, ammonium bicarbonate etc.）Deng also some inorganic salt containing nitrogens and having
Machine object intermediate etc. is also all needed directly using ammonia as raw material.Therefore, ammonia is in fields such as chemical industry, light industry, chemical fertilizer, pharmacy, synthetic fibers
Tool has been widely used.But ammonia exists in gaseous form at normal temperatures and pressures, that is, ammonia.Ammonia is that one kind has
The colourless gas of intense irritation smell has stimulation, effect of burning to the mucous membrane of the skin of people, eyes and respiratory apparatus,
If sucking is excessive, lung swelling can be caused, so that it is dead.Although the irritation of ammonia is reliable adverse concentration alarm signal,
But due to olfactory fatigue, the ammonia of low concentration can be difficult to discover after Long Term Contact, and form potential danger.
At present, mainly there are chemical analysis method and instrument testing method for the detection method of ammonia.Though chemical analysis method operates
Simply, but sensitivity is not high and the shortcomings of can not reuse；Instrument testing method mainly detects instrument pair using ammonia gas
Ammonia gas concentration in air carries out quantitative detection, has many advantages, such as high sensitivity, reusable, high degree of automation,
And it is widely applied in industrial production.
For ammonia gas detector used in instrument testing method, most crucial component is with qualitative to ammonia gas
The gas sensor of quantitative response, that is, the gas sensor coated with different nano-functional materials.Gas sensor is a kind of
The sensor of specific gas is detected, principle is that velocity of wave based on SAW device and frequency can be sent out with the variation of external environment
Raw drift.It mainly includes semiconductor gas sensor, catalytic combustion type gas sensor and Electro-chemical Gas Sensor etc.,
It is middle it is most be semiconductor gas sensor.
Sensitivity is the important characterization of gas sensor gas-sensitive property.Sensitivity definition is sensor in air atmosphere
Resistance valueR a With resistance value of the sensor in certain density tested gas atmosphereR g Ratio, i.e.,
Therefore, probe into that strong adsorption, stability are good, catalytic activity is high, have specific recognition and can to ammonia gas
The gas sensing materials quantitatively detected, and then prepare the ammonia gas with the characteristics such as high sensitivity, response quickly, recovery time be short
Body sensor has important application value to industrial production, human health, while is also environmental monitoring technology area research
Key points and difficulties.
Invention content
Prepare that simple, high sensitivity, detection is quickly available is examined in ammonia gas the purpose of the present invention is to provide a kind of
The preparation method of the gas sensor of survey, prepared sensor, quick, Sensitive Detection available for ammonia gas.Based on this
Purpose, the method comprises the steps of firstly, preparing a kind of magnetic Nano material of two-dimensional sheet, i.e. the nitrogen of iron and cobalt dual-metal In-situ reaction is mixed
Miscellaneous titanium dioxide nanoplate FeCo-N@TiO2, passed using the big specific surface area of the material, mesoporous high gas absorption characteristic and electronics
It passs and is changed by material surface gas and influence sensitive many characteristics, realize to ammonia gas with sensitive, quick response
The structure of gas sensor.
The technical solution adopted by the present invention is as follows：
1. a kind of preparation method of the ammonia gas sensor based on the nano combined nano material of two-dimensional magnetic, described
The nano combined nano material of two-dimensional magnetic is iron and the nitrogen-doped titanium dioxide nanometer sheet FeCo-N@of cobalt dual-metal In-situ reaction
TiO2；
It is characterized in that, the preparation method includes following preparation process：
（1）FeCo-N@TiO2Preparation；
（2）The preparation of ammonia gas sensor；
Wherein, step（1）Prepare FeCo-N@TiO2The specific steps are：
First, 0.8 mmol molysite, 0.8 ~ 1.2 mmol cobalt salts and 1 mmol ammonium salts is taken to be added to 5 mL butyl titanates
In, in whipping process, 0.5 ~ 0.8 mL hydrofluoric acid is slowly added to, is reacted in a kettle at 160 ~ 200 DEG C 18 ~ 24 hours, it is cold
But to after room temperature, with ultra-pure water and absolute ethyl alcohol centrifuge washing three times after, be dried in vacuo at 50 DEG C；Then, by the powder of grinding
It is put into Muffle furnace, heating rate is 1 ~ 3 DEG C/min, at 480 ~ 560 DEG C under nitrogen protection, calcines 10 ~ 60 min；Finally,
Powder after calcining is cooled to room temperature, obtains FeCo-N@TiO2；
The molysite is selected from one of following：Ferric sulfate, iron chloride, ferric nitrate；
The cobalt salt is selected from one of following：Cobaltous sulfate, cobalt chloride, cobalt nitrate；
The ammonium salt is selected from one of following：Ammonium sulfate, ammonium chloride, ammonium nitrate, ammonium carbonate；
Step（2）Prepare ammonia gas sensor the specific steps are：
First, step is taken（1）The FeCo-N@TiO of middle preparation2100 mg and 0.5 ~ 2.0 mmol aluminium salts are placed in mortar,
Absolute ethyl alcohol is added in, insulating ceramics pipe surface formation film is coated uniformly on after being ground to paste, dries at room temperature；Then,
The platinum filament of ceramic tube both sides and heater strip are welded with pedestal；Finally, the element being welded is placed on detecting instrument
In, burin-in process is carried out to 4.22V by adjusting heating voltage, obtains ammonia gas sensor；
The aluminium salt is selected from one of following：Aluminum sulfate, aluminium chloride, aluminum nitrate.
2. the application of the ammonia gas sensor prepared by preparation method of the present invention, which is characterized in that Ke Yiying
For 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 is prepared simply, easy to operate, is realized to the fast of ammonia gas
Fast, sensitive, highly selective detection has market development prospect；
（2）The present invention is prepared for New Two Dimensional sheet light-sensitive material FeCo-N TiO for the first time2, since iron, cobalt are in titanium dioxide
Growth in situ in titanium nanometer sheet and fully contacted with titanium dioxide nanoplate, the metal surface plasma body of iron, cobalt is utilized to make
With and the two mutual promoting action, effectively increase semiconductor substrate electron transmission ability and catalytic activity, solve two
Although TiOx nano piece specific surface area is bigger and mesoporous high gas absorption characteristic is suitable for air-sensitive host material, air-sensitive
The technical issues of not high and impedance variations of activity are unstable；Simultaneously because the doping of nitrogen and cause titanium dioxide nanoplate it is better
Increase layer gap spacing and fully dispersed, greatly increase the exposure of the high energy crystal face of titanium dioxide nanoplate, electron transmission and
It is fully dispersed, electron transmission ability is greatly increased, the impedance of air-sensitive host material is solved and changes and quick response with gas
The technical issues of；Moreover, by aluminum ions doping, solves the technical issues of specific detection ammonia gas.Therefore, the material
Effective preparation of material has important scientific meaning and application value.
Specific embodiment
1 FeCo-N@TiO of embodiment2Preparation
First, 0.8 mmol molysite and 0.8 mmol cobalt salts and 1 mmol ammonium salts is taken to be added in 5 mL butyl titanates,
In whipping process, 0.5 mL hydrofluoric acid is slowly added to, is reacted in a kettle at 160 DEG C 24 hours, after being cooled to room temperature, used
Ultra-pure water and absolute ethyl alcohol centrifuge washing three times after, be dried in vacuo at 50 DEG C；Then, the powder of grinding is put into Muffle furnace,
Heating rate is 1 DEG C/min, and 60 min are calcined at 480 DEG C；Finally, the powder after calcining is cooled to room temperature, obtained
FeCo-N@TiO2；
The molysite is ferric sulfate；
The cobalt salt is cobaltous sulfate；
The ammonium salt is ammonium sulfate.
2 FeCo-N@TiO of embodiment2Preparation
First, 0.8 mmol molysite and 1.0 mmol cobalt salts and 1 mmol ammonium salts is taken to be added in 5 mL butyl titanates,
In whipping process, 0.65 mL hydrofluoric acid is slowly added to, is reacted in a kettle at 180 DEG C 21 hours, after being cooled to room temperature, used
Ultra-pure water and absolute ethyl alcohol centrifuge washing three times after, be dried in vacuo at 50 DEG C；Then, the powder of grinding is put into Muffle furnace,
Heating rate is 2 DEG C/min, and 30 min are calcined at 520 DEG C；Finally, the powder after calcining is cooled to room temperature, obtained
FeCo-N@TiO2；
The molysite is iron chloride；
The cobalt salt is cobalt chloride；
The ammonium salt is ammonium chloride.
3 FeCo-N@TiO of embodiment2Preparation
First, 0.8 mmol molysite and 1.2 mmol cobalt salts and 1 mmol ammonium salts is taken to be added in 5 mL butyl titanates,
In whipping process, 0.8 mL hydrofluoric acid is slowly added to, is reacted in a kettle at 200 DEG C 18 hours, after being cooled to room temperature, used
Ultra-pure water and absolute ethyl alcohol centrifuge washing three times after, be dried in vacuo at 50 DEG C；Then, the powder of grinding is put into Muffle furnace,
Heating rate is 3 DEG C/min, and 10 min are calcined at 560 DEG C；Finally, the powder after calcining is cooled to room temperature, obtained
FeCo-N@TiO2；
The molysite is ferric nitrate；
The cobalt salt is cobalt nitrate；
The ammonium salt is ammonium nitrate.
The preparation of 4 ammonia gas sensor of embodiment
First, the FeCo-N@TiO prepared in Example 12100 mg and 0.5 mmol aluminum sulfate are placed in mortar, are added
Enter absolute ethyl alcohol, be coated uniformly on insulating ceramics pipe surface formation film after being ground to paste, dry at room temperature；Then, will
Platinum filament and heater strip and the pedestal of ceramic tube both sides are welded；Finally, the element being welded is placed in detecting instrument,
Burin-in process is carried out to 4.22V by adjusting heating voltage, obtains ammonia gas sensor, the inspection applied to ammonia gas
It surveys, detection is limited to 0.02 mg/m3。
The preparation of 5 ammonia gas sensor of embodiment
First, the FeCo-N@TiO prepared in Example 22100 mg and 1.2 mmol aluminium chloride are placed in mortar, are added
Enter absolute ethyl alcohol, be coated uniformly on insulating ceramics pipe surface formation film after being ground to paste, dry at room temperature；Then, will
Platinum filament and heater strip and the pedestal of ceramic tube both sides are welded；Finally, the element being welded is placed in detecting instrument,
Burin-in process is carried out to 4.22V by adjusting heating voltage, obtains ammonia gas sensor, the inspection applied to ammonia gas
It surveys, detection is limited to 0.02 mg/m3。
The preparation of 6 ammonia gas sensor of embodiment
First, the FeCo-N@TiO prepared in Example 32100 mg and 2.0 mmol aluminum nitrates are placed in mortar, are added
Enter absolute ethyl alcohol, be coated uniformly on insulating ceramics pipe surface formation film after being ground to paste, dry at room temperature；Then, will
Platinum filament and heater strip and the pedestal of ceramic tube both sides are welded；Finally, the element being welded is placed in detecting instrument,
Burin-in process is carried out to 4.22V by adjusting heating voltage, obtains ammonia gas sensor, the inspection applied to ammonia gas
It surveys, detection is limited to 0.02 mg/m3。
Claims (2)
1. a kind of preparation method of the ammonia gas sensor based on the nano combined nano material of two-dimensional magnetic, the two-dimensional magnetic
Property nitrogen-doped titanium dioxide nanometer sheet FeCo-N@TiO of the nano combined nano material for iron and cobalt dual-metal In-situ reaction2；
It is characterized in that, the preparation method includes following preparation process：
（1）FeCo-N@TiO2Preparation；
（2）The preparation of ammonia gas sensor；
Wherein, step（1）Prepare FeCo-N@TiO2The specific steps are：
First, 0.8 mmol molysite, 0.8 ~ 1.2 mmol cobalt salts and 1 mmol ammonium salts is taken to be added in 5 mL butyl titanates, is stirred
During mixing, 0.5 ~ 0.8 mL hydrofluoric acid is slowly added to, reacts 18 ~ 24 hours, is cooled in a kettle at 160 ~ 200 DEG C
After room temperature, with ultra-pure water and absolute ethyl alcohol centrifuge washing three times after, be dried in vacuo at 50 DEG C；Then, the powder of grinding is put into
In Muffle furnace, heating rate is 1 ~ 3 DEG C/min, at 480 ~ 560 DEG C under nitrogen protection, calcines 10 ~ 60 min；Finally, it will forge
Powder after burning is cooled to room temperature, and obtains FeCo-N@TiO2；
The molysite is selected from one of following：Ferric sulfate, iron chloride, ferric nitrate；
The cobalt salt is selected from one of following：Cobaltous sulfate, cobalt chloride, cobalt nitrate；
The ammonium salt is selected from one of following：Ammonium sulfate, ammonium chloride, ammonium nitrate, ammonium carbonate；
Step（2）Prepare ammonia gas sensor the specific steps are：
First, step is taken（1）The FeCo-N@TiO of middle preparation2100 mg and 0.5 ~ 2.0 mmol aluminium salts are placed in mortar, are added in
Absolute ethyl alcohol is coated uniformly on insulating ceramics pipe surface formation film after being ground to paste, dries at room temperature；Then, it will make pottery
Platinum filament and heater strip and the pedestal of porcelain tube both sides are welded；Finally, the element being welded is placed in detecting instrument, led to
It overregulates heating voltage and carries out burin-in process to 4.22V, obtain ammonia gas sensor；
The aluminium salt is selected from one of following：Aluminum sulfate, aluminium chloride, aluminum nitrate.
2. the application of the ammonia gas sensor prepared by preparation method as described in claim 1, which is characterized in that Ke Yiying
For 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 |
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| Publication Number | Publication Date |
|---|---|
| CN105717167A CN105717167A (en) | 2016-06-29 |
| CN105717167B true CN105717167B (en) | 2018-06-22 |
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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 |
-
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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 |
|---|
| N掺杂TiO2纳米粉体的表面特性及可见光活性;姜洪泉，王城英等;《材料科学与工程学报》;20110430;第29卷(第2期);161-166页 * |
| 金属氧化物掺杂对TiO2气敏特性的影响;戴振清、孙以材等;《传感器世界》;20030930(第9期);10-14页 * |
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