CN106093137A - A kind of based on α Fe2o3acetone gas sensor of multi-pore micron flower sensitive material and preparation method thereof - Google Patents
A kind of based on α Fe2o3acetone gas sensor of multi-pore micron flower sensitive material and preparation method thereof Download PDFInfo
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- CN106093137A CN106093137A CN201610439141.2A CN201610439141A CN106093137A CN 106093137 A CN106093137 A CN 106093137A CN 201610439141 A CN201610439141 A CN 201610439141A CN 106093137 A CN106093137 A CN 106093137A
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- 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
Abstract
A kind of based on α Fe2O3Acetone gas sensor of multi-pore micron flower sensitive material and preparation method thereof, belongs to conductor oxidate gas sensor technical field.The novel preparation means that present invention incorporates solvent-thermal method and calcination method is prepared for α Fe2O3Multi-pore micron flower sensitive material.Utilize α Fe2O3Loose porous, the feature such as favorable dispersibility, basic-cell dimensions are less of multi-pore micron flower, effectively monitors acetone gas.Additionally, sensor construction of the present invention is by the commercially available Al with 2 annular gold electrodes2O3Insulating ceramics pipe, it is coated in annular gold electrode and Al2O3Quasiconductor sensitive material on insulating ceramics pipe and through Al2O3The nichrome heating coil composition of insulating ceramics pipe.Device technology is simple, and volume is little, is suitable to produce in enormous quantities, thus has broad application prospects in terms of content of acetone in detection microenvironment.
Description
Technical field
The invention belongs to conductor oxidate gas sensor technical field, be specifically related to a kind of based on α-Fe2O3Porous is micro-
Acetone gas sensor of popped rice sensitive material and preparation method thereof.
Background technology
Acetone has another name called dimethyl ketone, is a kind of colourless, transparent, active, inflammable, volatile and has the liquid of acrid odors.
Industrially act not only as producing explosive, plastics, the important solvent of rubber, be also used as synthesizing ketenes, iodoform, asphalt mixtures modified by epoxy resin
The important source material of the materials such as fat.But, it being similar to other organic solvents, it has feature inflammable, volatile, meets naked light, height
Thermoae easy firing explodes, and its explosion limit is 2.55%~12.8%.Further, acetone not only has bigger fire risk,
Also the central nervous system of people is had anesthetic action when low concentration, make the nervous system of human body, liver, kidney, pancreas etc.
Impaired organ, results even in people's stupor and death when high concentration.Therefore, the detection for acetone gas has particularly significant
Meaning.
Resistor-type gas sensing utensil in the gas sensor of huge number, with conductor oxidate as sensitive material
There are the advantages such as highly sensitive, Monitoring lower-cut is low, selectivity good, respond and resume speed is fast, manufacture method is simple, cost is relatively low,
It it is one of current most widely used gas sensor.Along with the development of nanometer science and technology, regulate and control into receive by gas sensitive
Rice structure can be greatly enhanced the specific surface area of material, increases avtive spot, gas-sensitive property can be made to be improved.
α-Fe2O3Being the n-type semiconductor of a kind of broad stopband, owing to it is nontoxic, aboundresources etc. is widely used in gas
Body sensing aspect.But, although many different-shape, various sizes of α-Fe2O3Material is developed, but most of α-
Fe2O3When detecting VOC (VOC) gas, all show relatively low sensitivity and higher detection temperature.
Further, since their manufacture method is the harshest, so utilizing straightforward procedure preparation graduation α-Fe2O3Gas sensitive, passes through
Regulate and control its size and pattern feature, thus it is most important to promote its air-sensitive performance.
Summary of the invention
It is an object of the invention to provide a kind of based on α-Fe2O3Multi-pore micron flower sensitive material acetone gas sensor and
Its preparation method.
Utilize α-Fe2O3Multi-pore micron flower as sensitive material, on the one hand α-Fe2O3As typical Semiconductor gas sensors material
Material, has the features such as nontoxic, aboundresources and is widely studied;On the other hand α-Fe2O3Graded structure there is specific surface area
Greatly, the feature such as loose porous, it is possible to the reaction efficiency of gas and sensitive material is greatly improved, and then improves the sensitive of sensor
Degree.Additionally, composition α-Fe2O3α-the Fe that elementary cell is small size, 10~20nm of multi-pore micron flower2O3Nano-particle, nanometer
The exclusive activity of granule can reduce the required energy of reaction, such that it is able to reduce the operating temperature of device.Meanwhile, nano-particle
Between exist pile up hole be conducive to the transmission of gas to spread, it is possible to effectively reduce response time.Of the present invention commercially available
Tubular structure sensor manufacturing process is simple, and volume is little, the most industrial batch production, therefore has important using value.
Of the present invention based on α-Fe2O3Multi-pore micron flower sensitive material acetone gas sensor, by outer surface with
Article two, the Al of gold electrode parallel, ring-type and separate2O3Earthenware substrate, it is coated in Al2O3Earthenware outer surface and gold electricity
The sensitive material extremely gone up, it is placed in Al2O3NI-G heating coil composition in earthenware;It is characterized in that: sensitive material be α-
Fe2O3Multi-pore micron flower, and prepared by following steps,
First by 0.10~0.18g Fe2(SO4)3·xH2O (x ≈ 7~9) is dissolved in the dehydrated alcohol of 20~40mL,
And be kept stirring for until solution is homogeneous under 40~60 DEG C of water-baths;
2. by above-mentioned mixed solution hydro-thermal reaction 20~26 hours at 130~160 DEG C, will generate after being cooled to room temperature
Precipitation ethanol repeatedly eccentric cleaning, calcines 2~4 hours after being then dried at room temperature at 600~700 DEG C again, thus
To α-Fe2O3Multi-pore micron pollen end.
One of the present invention is based on α-Fe2O3The preparation side of the acetone gas sensor of multi-pore micron flower sensitive material
Method, its step is as follows:
1. by α-Fe2O3Multi-pore micron pollen end mixes with deionized water in mass ratio 3~5:1, grinds and forms pasty state slurry
Material, then dips a small amount of slurry and is uniformly coated on commercially available outer surface from the Al with 2 annular gold electrodes2O3Earthenware table
Face, and make sensitive material that annular gold electrode is completely covered, form the sensitive material film of 10~30 μ m-thick, a length of the 4 of earthenware
~4.5mm, external diameter is 1.2~1.5mm, and internal diameter is 0.8~1.0mm;
2. toast 30~45 minutes under infrared lamp, treat that sensitive material is dried, Al2O3Earthenware is at 400~450 DEG C
Lower calcining 2~3 hours;Then the NI-G heating coil that resistance value is 30~40 Ω is passed Al2O3Ceramic tube inside is as heating
Silk, finally welds by above-mentioned device according to general heater-type gas sensor and encapsulates, thus obtain α-Fe2O3Oxide half
Conductor acetone sensor.
The present invention prepare based on α-Fe2O3The acetone gas sensor of multi-pore micron flower sensitive material has the advantage that
1. preparation method is simple, it is not necessary to adding surfactant and special solvent, preparation condition is relatively mild.
2. the material scatter of preparation is good, loose porous;There is good repeatability.Sensitivity to acetone is good, and material
The optimum working temperature of material is relatively low, and response speed is very fast simultaneously.Have broad application prospects in terms of detection content of acetone;
3. using commercially available tubular type sensor, device technology is simple, and volume is little, is suitable to produce in enormous quantities.
Accompanying drawing explanation
Fig. 1: α-Fe2O3Multi-pore micron flower SEM shape appearance figure, wherein the amplification of (a) figure is 1000 times, and (b) figure is single
The pattern of micro-flowers, amplification is 2000 times;
Fig. 2: α-Fe2O3The XRD figure of multi-pore micron flower;
Fig. 3: based on α-Fe2O3The acetone sensor structural representation of multi-pore micron flower sensitive material;
Fig. 4: embodiment 1 sensor sensitivity curve to 100ppm acetone gas at a temperature of different operating;
Fig. 5: embodiment 1 sensor response recovery curve to 100ppm acetone gas at 210 DEG C;
Fig. 6: embodiment 1 sensor sensitivity-acetone concentration characteristic curve at 210 DEG C.
As it is shown in figure 1, (a) figure can be seen that α-Fe2O3Graded structure is flower-like nanostructure, favorable dispersibility;
B () figure is found out α-Fe2O3Multi-pore micron flower is to be made up of the nano-particle of 10~about 20nm, and the diameter of micro-flowers is about 2 μ
m;
As in figure 2 it is shown, α-Fe2O3Multi-pore micron flower is pure phase α-Fe2O3Structure;Corresponding XRD spectra JCPDS is 33-
0664.
As it is shown on figure 3, device is by Al2O3Earthenware 1, quasiconductor sensitive material 2, nickel-cadmium coil 3, annular gold electrode 4
Form with platinum line 5;
As shown in Figure 4, the optimum working temperature of embodiment is respectively 210 DEG C, now sensitive to 100ppm acetone of device
Degree is 14.5;
As it is shown in figure 5, when device is operated in optimum working temperature 210 DEG C, acetone gas concentration is under 100ppm, embodiment
It is respectively provided with good repeatability;Its corresponding speed is very fast, and about 1s i.e. can reach steady statue.
As shown in Figure 6, when embodiment device is at operating temperature is 210 DEG C, and the sensitivity of device is along with acetone concentration
Increase and increase, embodiment is respectively 3.5 to the sensitivity of 10,20,40,60,80,100 and 200ppm acetone, 5.2,8.5,
10.2,12.0,14.5 and 19.4, its Monitoring lower-cut can reach 1ppm, and corresponding Sensitirity va1ue is 1.44.
Note: the sensitivity (n-type semiconductor) of device is defined as its resistance value in atmosphere in test reducibility gas
With the ratio of resistance value size in tested gas, it is S=Ra/Rg.In test process, static test system is used to survey
Examination.Device is placed in the gas tank of 50~80L, inwardly injects a certain amount of organic gas to be measured, observe and record its resistance and become
Change, by being calculated corresponding sensitivity number.
Detailed description of the invention:
Embodiment:
With α-Fe2O3Multi-pore micron flower makes acetone sensor as sensitive material, its concrete manufacturing process:
First by the Fe of 0.12g2(SO4)3·xH2O is dissolved in the middle of the dehydrated alcohol of 30mL, and protects under 50 DEG C of water-baths
Hold constantly stirring until solution is homogeneous;
2., by above-mentioned mixed solution hydro-thermal reaction 24 hours at 150 DEG C, it is cooled to the precipitation second of generation after room temperature
Alcohol repeatedly eccentric cleaning, calcines 2 hours at 650 DEG C after being then dried at room temperature for again, thus obtains α-Fe2O3Multi-pore micron
Pollen end.Its quality is about 30mg, and specific surface area is 22m2g-1;
3. α-the Fe that will obtain2O3Multi-pore micron flower sensitive material powder mixes with deionized water 5:1 in mass ratio, and grinds
Mill forms pasty slurry, then dips a small amount of slurry with brush and is uniformly coated on commercially available outer surface from 2 annular gold
The Al of electrode2O3Earthenware surface, forms the sensitive material film of 30 μ m-thick, a length of 4mm of earthenware, and external diameter is 1.2mm, interior
Footpath is 0.8mm, and makes sensitive material that annular gold electrode is completely covered;
4. toast 3 minutes under infrared lamp, treat that sensitive material is dried, Al2O3It is little that earthenware calcines 2 at 400 DEG C
Time;Then the nickel-cadmium coil that resistance value is 30 Ω is passed Al2O3Ceramic tube inside is as heater strip, finally by above-mentioned device
Part welds according to general heater-type gas sensor and encapsulates, thus obtains α-Fe2O3The acetone of multi-pore micron flower sensitive material
Gas sensor.
Claims (2)
1. one kind based on α-Fe2O3Multi-pore micron flower sensitive material acetone gas sensor, by outer surface with two parallel,
The Al of gold electrode ring-type and separate2O3Earthenware substrate, it is coated in Al2O3Quick on earthenware outer surface and gold electrode
Feel material, be placed in Al2O3NI-G heating coil composition in earthenware;It is characterized in that: sensitive material is α-Fe2O3Porous is micro-
Popped rice, and prepared by following steps,
First by 0.10~0.18g Fe2(SO4)3·xH2O is dissolved in the dehydrated alcohol of 20~40mL, and at 40~60 DEG C of water
It is kept stirring for until solution is homogeneous under bath;
2. by above-mentioned mixed solution hydro-thermal reaction 20~26 hours at 130~160 DEG C, the precipitation that will generate after being cooled to room temperature
By ethanol repeatedly eccentric cleaning, calcine 2~4 hours at 600~700 DEG C again after being then dried at room temperature for, thus obtain α-
Fe2O3Multi-pore micron pollen end.
2. the one described in claim 1 is based on α-Fe2O3The preparation side of the acetone gas sensor of multi-pore micron flower sensitive material
Method, its step is as follows:
1. by α-Fe2O3Multi-pore micron pollen end mixes with deionized water in mass ratio 3~5:1, grinds and forms pasty slurry, so
After dip a small amount of slurry and be uniformly coated on outer surface from the Al of 2 annular gold electrodes2O3Earthenware surface, and make sensitivity
Material is completely covered annular gold electrode, forms the sensitive material film of 10~30 μ m-thick;
2. toast 30~45 minutes under infrared lamp, treat that sensitive material is dried, Al2O3Earthenware is forged at 400~450 DEG C
Burn 2~3 hours;Then the NI-G heating coil that resistance value is 30~40 Ω is passed Al2O3Ceramic tube inside as heater strip,
Finally above-mentioned device is welded according to general heater-type gas sensor and encapsulates, thus obtain based on α-Fe2O3Multi-pore micron
The acetone gas sensor of flower sensitive material.
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Cited By (13)
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CN106770497A (en) * | 2017-01-09 | 2017-05-31 | 吉林大学 | One kind is based on Pt/ α Fe2O3Acetone gas sensor of porous nanoparticles sensitive material and preparation method thereof |
CN107651706A (en) * | 2017-11-03 | 2018-02-02 | 安徽工业大学 | A kind of preparation method of bismuthic acid lanthanum nanometer rods |
CN107673413A (en) * | 2017-11-03 | 2018-02-09 | 安徽工业大学 | A kind of preparation method of nickel antimonide nanometer rods |
CN107673414A (en) * | 2017-11-03 | 2018-02-09 | 安徽工业大学 | A kind of preparation method of nickel acid manganese nanometer sheet |
CN107720831A (en) * | 2017-10-09 | 2018-02-23 | 福州大学 | Ferric oxide nano-material and its application based on solvent-thermal method controlledly synthesis |
CN108828017A (en) * | 2018-03-20 | 2018-11-16 | 武汉科技大学 | A kind of gas sensor and preparation method thereof towards acetone gas detection |
CN108828025A (en) * | 2018-06-22 | 2018-11-16 | 吉林大学 | One kind being based on hollow CdFe2O4The acetone gas sensor and preparation method thereof of nanocages sensitive material |
CN109001264A (en) * | 2018-06-22 | 2018-12-14 | 吉林大学 | One kind being based on porous C uFe2O4The acetone gas sensor and preparation method thereof of microballoon sensitive material |
CN109338466A (en) * | 2018-09-02 | 2019-02-15 | 景德镇陶瓷大学 | It is a kind of to prepare monocrystalline Fe2O3The method of nano-particles self assemble elliptical shape ball micro nano structure |
CN110988052A (en) * | 2019-12-30 | 2020-04-10 | 吉林大学 | Based on Fe2O3Acetone sensor of sensitive material and preparation method thereof |
CN111579616A (en) * | 2020-05-29 | 2020-08-25 | 吉林大学 | Based on YSZ and Fe2TiO5-TiO2Acetone sensor of sensitive electrode, preparation method and application thereof |
CN111638251A (en) * | 2020-05-15 | 2020-09-08 | 苏州新傲信息技术有限公司 | Nano material, synthesis method thereof, gas sensor, preparation method and application thereof |
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CN110988052A (en) * | 2019-12-30 | 2020-04-10 | 吉林大学 | Based on Fe2O3Acetone sensor of sensitive material and preparation method thereof |
CN111638251A (en) * | 2020-05-15 | 2020-09-08 | 苏州新傲信息技术有限公司 | Nano material, synthesis method thereof, gas sensor, preparation method and application thereof |
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Application publication date: 20161109 |