CN108956708A - A kind of alcohol gas sensor and preparation method thereof based on zinc ferrite nano sensitive material - Google Patents
A kind of alcohol gas sensor and preparation method thereof based on zinc ferrite nano sensitive material Download PDFInfo
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- CN108956708A CN108956708A CN201810495618.8A CN201810495618A CN108956708A CN 108956708 A CN108956708 A CN 108956708A CN 201810495618 A CN201810495618 A CN 201810495618A CN 108956708 A CN108956708 A CN 108956708A
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
Abstract
The invention belongs to oxide semiconductor gas sensor technical fields, provide a kind of alcohol gas sensor and preparation method thereof based on zinc ferrite nano sensitive material.The present invention is using zinc salt, molysite, organic ligand, organic solvent as raw material, after mixture ultrasonic disperse, carries out solvent-thermal method reaction, product is washed, it is dry, the zinc ferrite nano sensitive material of hollow fusellal fabric is obtained after high-temperature burning process；The alcohol gas sensor of external-heat is finally constructed using zinc ferrite nano sensitive material.The invention has the benefit that raw material is easy to get, low in cost, method is simple；Zinc ferrite nano sensitive material is hollow structure, has higher specific surface area, and there is absorption oxygen functional group abundant on its surface, can be improved the air-sensitive performance of material；Alcohol gas sensor operating temperature is low, is a kind of alcohol gas sensor of low energy consumption.
Description
Technical field
The invention belongs to oxide semiconductor gas sensor technical field, it is related to a kind of based on hollow fusellal fabric
ZnFe2O4Alcohol gas sensor of nano sensitive material and preparation method thereof.
Background technique
Ethyl alcohol is defended as a kind of inflammable, volatile colourless transparent liquid in people's lives and national defence chemical industry, medical treatment
Life, food industry are widely applied in industrial and agricultural production.Its steam is easy to form explosive mixture with air.In addition, being based on second
The alcohol breath detection analysis instrument of alcohol sensor gradually replaces conventional method identification to drive when intoxicated, to avoid casualties and property
Heavy losses.Therefore, in order to prevent the generations of various accidents, carry out in time, accurately that monitoring and alarm are very to ethyl alcohol
It is necessary.Presently, there are ethanol sensor mainly include feulcell prototype (catalytic combustion type), MOS type,
Infra red type, gas chromatographic analysis type, than colour pattern etc..It is most common that metal is aoxidized from easy to use and in price consider
Object semi-conductor type.The gas sensor of the type is low, small in size with price, structure is simple, performance stable sensitivity is high and easy
With a large amount of concerns the advantages that semiconductor technology compatibility and by scholar.
The core of metal-oxide semiconductor (MOS) gas sensor is semiconductor sensitive material, at present Fe2O3And SnO2Material is
It is produced for large batch of gas sensor, can be used to detect and forecast hydrogen, methane, carbon monoxide, nitrogen dioxide, hydrogen sulfide
Etc. various fuel gas, toxic gas and environmental pollution gas.But this kind of Semiconductor gas sensors material there is also poor selectivity,
The disadvantages of operating temperature is high.Poor selectivity will lead to the easy interference by other gases in environment of sensor；Operating temperature is high,
It is high to lead to sensor energy consumption, and brings potential danger to the detection of inflammable gas.
It, can also be using advanced material synthesis technology to existing other than exploring new material in order to promote air-sensitive performance
Some gas sensitives are into improvement.ZnFe2O4Composite oxides Ferrite Material is to have excellent selectivity as gas sensitive
And stability.Researcher utilize different material synthesis methods, by change surface state, lattice defect, doping metals from
Son etc., to promote the air-sensitive performance of material.In recent years, researcher starts to consider hollow structure to improve material grains surface
Utilization rate simultaneously accelerates the diffusion velocity of gas molecule on the surface of the material.A kind of emerging crystalline state with periodic network structure is more
It is hollow porous to prepare that the metal organic framework compound (MOFs) of pore structure can be used as a kind of general template or presoma
The function nano material of structure.This structure has high specific surface area and is not susceptible to the regular texture reunited.Organic ligand
Type, the dosage of additive and materials synthesis temperature class lead to the air-sensitive performances such as sensitivity, selectivity and operating temperature
Generate significant difference.
Summary of the invention
In view of the problems of the existing technology, a kind of zinc ferrite nano sensitive material based on hollow fusellal fabric of the present invention
Alcohol gas sensor and preparation method thereof, realize that the low-power consumption to alcohol gas detects.
For most of above-mentioned purposes, the technical solution of the present invention is as follows:
A kind of alcohol gas sensor of the zinc ferrite nano sensitive material based on hollow fusellal fabric, the ethanol gas
Body sensor is external-heat structure, including ZnFe2O4Nano sensitive material layer, Al2O3Ceramic tube, Pt conducting wire, two gold electrodes,
Heating wire, wherein ZnFe2O4Nano sensitive material is hollow fusellal fabric.
The Al2O3Ceramic tube inside penetrates heating wire, and both ends coat gold electrode, each gold electrode with Pt conducting wire phase
Connection；The ZnFe2O4Nano sensitive material layer is coated on Al2O3The outer surface of ceramic tube, and by the outer surface of ceramic tube and
Cyclic annular Au electrode is completely covered, and reserves Pt lead, obtains testing element, and testing element is welded on pedestal by pin, through sealing
Alcohol gas sensor is obtained after dress, aging.The ZnFe2O4Nano sensitive material layer is with a thickness of 8~30um.Described
Al2O3Ceramic tube is insulating layer, and a length of 3~5mm, internal diameter are 0.7~0.9mm, outer diameter is 1.1~1.3mm.
The preparation method of the above-mentioned alcohol gas sensor based on zinc ferrite nano sensitive material, with zinc salt, molysite, organic
Ligand, organic solvent are raw material, after mixture ultrasonic disperse, carry out solvent-thermal method reaction, product is washed, dry, high temperature is forged
The zinc ferrite nano sensitive material of hollow fusellal fabric is obtained after burning process；Using ZnFe2O4Nano sensitive material constructs ethanol gas
Body sensor.The following steps are included:
The first step prepares persursor material
1.1) at room temperature, by zinc nitrate hexahydrate, six nitric hydrate iron, fumaric acid according to 3~4:6 of mass ratio~7:25~
35 are dissolved in n,N-Dimethylformamide DMF, by this mixed solution ultrasound to uniform.
1.2) homogeneous solution for obtaining step 1.1) moves into reaction kettle, the heating reaction 6 under the conditions of 100~140 DEG C
It after~8 hours, is cooled to room temperature, after obtained product is successively cleaned multiple times with detergent, is put into vacuum tank, 50~
90 DEG C drying 6~10 hours, obtain persursor material.The detergent is DMF, ethyl alcohol or both mixture.
Second step prepares ZnFe2O4Nano sensitive material
The persursor material that step 1.2) is obtained is placed in Muffle furnace, the high-temperature calcination 2~6 under the conditions of 350~550 DEG C
Hour, obtain ZnFe2O4Nano sensitive material.
Third step prepares alcohol gas sensor
3.1) by ZnFe2O4It is suitable to obtain viscosity for grinding after nano sensitive material is mixed with deionized water 4~6:1 in mass ratio
In slurry, slurry is evenly applied to by Al using fine, soft fur brush2O3The outer surface of ceramic tube, and by the outer surface of ceramic tube and ring
Dress Au electrode is completely covered, and reserves Pt lead, obtains testing element.
3.2) it by after testing element drying, is welded on pedestal by six pins, obtains ethanol gas after encapsulated, aging
Body sensor, the aging temperature are 200~350 DEG C, and ageing time is 48~96 hours.
Beneficial effects of the present invention: (1) present invention uses MOF for the porous ZnFe of precursor preparation2O4Nano material, raw material
It is easy to get, low in cost, method is simple；(2) the porous ZnFe in the present invention2O4Nano material has hollow structure, has higher
Specific surface area；(3) the porous ZnFe in the present invention2O4Nano-material surface has absorption oxygen functional group abundant, significantly improves material
The air-sensitive performance of material；(4) ZnFe based on hollow fusellal fabric in the present invention2O4The alcohol gas of nano sensitive material senses
Device, operating temperature is low, is a kind of alcohol gas sensor of low energy consumption.
Detailed description of the invention
Fig. 1 is Zn prepared by embodiment 1, the scanning electron microscope (SEM) photograph (SEM) of Fe-MOF nano material.
Fig. 2 is ZnFe prepared by embodiment 12O4The scanning electron microscope (SEM) photograph (SEM) of nano material.
Fig. 3 is ZnFe prepared by embodiment 12O4The X-ray diffractogram (XRD) of nano material.
Fig. 4 is that embodiment 1 prepares gas sensitive device for the dynamic response recovery curve of ethyl alcohol.
Specific embodiment
Below in conjunction with attached drawing and technical solution, a specific embodiment of the invention is further illustrated.
Embodiment 1
The preparation method of alcohol gas sensor based on zinc ferrite nano sensitive material, comprising the following steps:
(1) presoma Zn, Fe-MOF nano material are prepared
By zinc nitrate hexahydrate (74.4mg), Fe(NO3)39H2O (202mg), fumaric acid (928.6mg) is dissolved in 10mL
N,N-dimethylformamide (DMF) solution is simultaneously ultrasonic to uniform.Said mixture is stirred into 10min at room temperature, is then incited somebody to action
To solution be transferred in 20mL reaction kettle and heat 8h at 100 DEG C, after the centrifugation of obtained product, successively use DMF and ethyl alcohol
It is cleaned, is put into 60 DEG C of vacuum oven dry 8h later, obtains presoma Zn, Fe-MOF nano material.Use scanning electron
The pattern of the Zn that microscopic characterization obtains, Fe-MOF nano material.As shown in Figure 1, resulting Zn, Fe-MOF nano material are in spinning
Hammer structure into shape, partial size is in 200nm or so.
(2) ZnFe is prepared2O4Nano material
By (1) resulting Zn, Fe-MOF nano material (100mg) is put into crucible and is placed in Muffle furnace, in air atmosphere
Lower carry out high-temperature calcination.Calcination temperature is 450 DEG C, calcination time 2h, 1 DEG C/min of heating rate.
Its structure is analyzed with x-ray diffractometer, as shown in Fig. 2, nano material is the ZnFe of spinel structure2O4Nanometer material
Material.The ZnFe characterized with scanning electron microscope2O4The pattern of nano material.As shown in Fig. 2, resulting ZnFe2O4Nanometer
Material is in fusellal fabric, and the scanning electron microscope image of calcining front and back sample is compared it is found that material is sent out after firing
A degree of contraction is given birth to, length-width ratio is significantly increased.
(3) alcohol gas sensor and the test of air-sensitive property are prepared
By ZnFe obtained in (2)2O4Nano material (10mg) is mixed to form uniform muddy with deionized water and mixes
Then muddy mixture is uniformly coated on the ceramic tube comprising two gold electrodes and four platinum filaments by object with small brushes.
After sample is dried overnight at room temperature, four Pt leads of ceramic tube are welded on pedestal and are inserted into nichrome resistance wire,
The effect of nichrome resistance wire is to be controlled by changing current control to temperature.By the sensor made at 200 DEG C
Air in after aging 72 hours, be inserted on the socket of air-sensitive tester, then taken using micro syringe a certain amount of to be measured
Solvent injects evaporating dish, and making solvent volatilization is steam to be measured.Air atmosphere and vapor atmosphere to be measured are tested by air-sensitive tester
Under resistance value, the sensitivity of gas detection is indicated with ratio.ZnFe2O4Nano material is at a temperature of different operating, to difference
The results are shown in Table 1 for gas air-sensitive property.
Table 1.ZnFe2O4Nano material air-sensitive performance test result
Embodiment 2
(1) Zn is prepared, Fe-MOF nano material step is same as Example 1.
(2) ZnFe is prepared2O4Nano material
By the resulting Zn of embodiment 1, Fe-MOF nano material (100mg) is put into crucible, is placed in Muffle furnace, in air
High-temperature calcination is carried out under atmosphere.Calcination temperature is 550 DEG C, heating rate 1 DEG C/min, calcination time 2h.ZnFe2O4Nanometer material
The structure of material, morphology characterization are similar to Example 1.
(3) it is same as Example 1 to prepare alcohol gas sensor step.
Embodiment 3
(1) Zn, Fe-MOF nano material are prepared
At room temperature, zinc nitrate hexahydrate (82mg), six nitric hydrate iron (130mg), fumaric acid (935mg) are dissolved in 12ml
In n,N-Dimethylformamide DMF, by this mixed solution ultrasound to uniform.Homogeneous solution is moved into reaction kettle, in 120 DEG C of items
Under part after heating reaction 7 hours, it is cooled to room temperature, after obtained product is successively cleaned multiple times with DMF and ethyl alcohol, is put into
Vacuum tank, it is 6 hours dry at 80 DEG C, obtain persursor material.
(2) ZnFe is prepared2O4Nano material
By resulting Zn, Fe-MOF nano material (100mg) is put into crucible, is placed in Muffle furnace, in air atmosphere
Carry out high-temperature calcination.Calcination temperature is 350 DEG C, calcination time 6h.ZnFe2O4Structure, morphology characterization and the implementation of nano material
Example 1 is similar.
(3) it is same as Example 1 to prepare alcohol gas sensor step, wherein aging temperature is 300 DEG C, ageing time
It is 85 hours.
Embodiment 4
(1) Zn-Fe-MOF nano material is prepared
At room temperature, zinc nitrate hexahydrate (60mg), six nitric hydrate iron (174mg), fumaric acid (625mg) are dissolved in
In 8mlN, dinethylformamide DMF, by this mixed solution ultrasound to uniform.Homogeneous solution is moved into reaction kettle, 135
Under the conditions of DEG C after heating reaction 6 hours, it is cooled to room temperature, after obtained product is successively cleaned multiple times with DMF and ethyl alcohol,
It is put into vacuum tank, it is 10 hours dry at 50 DEG C, obtain persursor material.
(2) ZnFe is prepared2O4Nano material
By resulting Zn, Fe-MOF nano material (100mg) is put into crucible, is placed in Muffle furnace, in air atmosphere
Carry out high-temperature calcination.Calcination temperature is 500 DEG C, calcination time 2h.ZnFe2O4Structure, morphology characterization and the implementation of nano material
Example 1 is similar.
(3) it is same as Example 1 to prepare alcohol gas sensor step, wherein aging temperature is 350 DEG C, ageing time
It is 50 hours.
Embodiments of the present invention above described embodiment only expresses, but it cannot be understood as special to the present invention
The limitation of the range of benefit, it is noted that for those skilled in the art, without departing from the inventive concept of the premise,
Various modifications and improvements can be made, these are all belonged to the scope of protection of the present invention.
Claims (9)
1. a kind of preparation method of the alcohol gas sensor based on zinc ferrite nano sensitive material, it is characterised in that following step
It is rapid:
The first step prepares persursor material
1.1) at room temperature, that zinc nitrate hexahydrate, six nitric hydrate iron, fumaric acid is molten according to 3~4:6 of mass ratio~7:25~35
In n,N-Dimethylformamide DMF, by this mixed solution ultrasound to uniform；
1.2) homogeneous solution for obtaining step 1.1) moves into reaction kettle, and heating reaction 6~8 is small under the conditions of 100~140 DEG C
Shi Hou is cooled to room temperature, and after washed dose of obtained product cleaning, is put into vacuum tank and is dried to obtain persursor material；
Second step prepares ZnFe2O4Nano sensitive material
The persursor material that step 1.2) is obtained obtains ZnFe high-temperature calcination 2~6 hours under the conditions of 350~550 DEG C2O4It receives
Rice sensitive material；
Third step prepares alcohol gas sensor
3.1) by ZnFe2O4Grinding obtains the slurry of modest viscosity after nano sensitive material is mixed with deionized water, and slurry is uniform
Coated on Al2O3The outer surface of ceramic tube, and the outer surface of ceramic tube and ring-type Au electrode are completely covered, Pt lead is reserved, is obtained
To testing element；
3.2) it is welded on pedestal after testing element is dry, obtains alcohol gas sensor after encapsulated, aging.
2. a kind of preparation side of alcohol gas sensor based on zinc ferrite nano sensitive material according to claim 1
Method, which is characterized in that drying temperature is 50~90 DEG C in the second step, and drying time is 6~10 hours.
3. a kind of preparation of alcohol gas sensor based on zinc ferrite nano sensitive material according to claim 1 or 2
Method, which is characterized in that the third step 3.2) in aging temperature be 200~350 DEG C, ageing time be 48~96 hours.
4. a kind of preparation of alcohol gas sensor based on zinc ferrite nano sensitive material according to claim 1 or 2
Method, which is characterized in that the third step 3.1) in ZnFe2O4Nano sensitive material and deionized water quality ratio are 4~6:1.
5. a kind of preparation side of alcohol gas sensor based on zinc ferrite nano sensitive material according to claim 3
Method, which is characterized in that the third step 3.1) in ZnFe2O4Nano sensitive material and deionized water quality ratio are 4~6:1.
6. a kind of system of the alcohol gas sensor based on zinc ferrite nano sensitive material described according to claim 1 or 2 or 5
Preparation Method, which is characterized in that detergent is DMF, ethyl alcohol or both mixture in the second step.
7. a kind of preparation side of alcohol gas sensor based on zinc ferrite nano sensitive material according to claim 3
Method, which is characterized in that detergent is DMF, ethyl alcohol or both mixture in the second step.
8. a kind of preparation side of alcohol gas sensor based on zinc ferrite nano sensitive material according to claim 4
Method, which is characterized in that detergent is DMF, ethyl alcohol or both mixture in the second step.
9. a kind of ethyl alcohol based on zinc ferrite nano sensitive material that any preparation method of claim 1-8 is prepared
Gas sensor, which is characterized in that the alcohol gas sensor is external-heat structure, including ZnFe2O4Nano sensitive material
Layer, Al2O3Ceramic tube, Pt conducting wire, two gold electrodes, heating wire, wherein ZnFe2O4Nano sensitive material is hollow fusellal fabric；
The Al2O3Ceramic tube inside penetrates heating wire, and both ends coat gold electrode, and each gold electrode is connected with Pt conducting wire；
The ZnFe2O4Nano sensitive material layer is coated on Al2O3The outer surface of ceramic tube, and by the outer surface of ceramic tube and ring-type
Au electrode is completely covered, and reserves Pt lead, obtains testing element, and testing element is welded on pedestal by pin, encapsulated, old
Alcohol gas sensor is obtained after change；The ZnFe2O4Nano sensitive material layer is with a thickness of 8~30um；The Al2O3Pottery
Porcelain tube is insulating layer, and a length of 3~5mm, internal diameter are 0.7~0.9mm, outer diameter is 1.1~1.3mm.
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| CN109946348A (en) * | 2019-03-18 | 2019-06-28 | 中国药科大学 | A kind of foamed metal oxide is preparing the application in gas sensor |
| CN110887871A (en) * | 2019-11-27 | 2020-03-17 | 哈尔滨师范大学 | Oxygen-enriched defect zinc stannate material, synthesis method thereof and hydrogen sulfide early warning sensor |
| CN111115694A (en) * | 2020-01-21 | 2020-05-08 | 河南科技大学 | Preparation method of hollow Co-Fe LDH material |
| CN111157590A (en) * | 2020-01-21 | 2020-05-15 | 复旦大学 | Semiconductor type carbon monoxide sensor |
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