CN109187662A - Work in the metal oxide base ethyl alcohol gas sensor preparation method of room temperature - Google Patents

Work in the metal oxide base ethyl alcohol gas sensor preparation method of room temperature Download PDF

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Publication number
CN109187662A
CN109187662A CN201811007612.8A CN201811007612A CN109187662A CN 109187662 A CN109187662 A CN 109187662A CN 201811007612 A CN201811007612 A CN 201811007612A CN 109187662 A CN109187662 A CN 109187662A
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China
Prior art keywords
tio
znsno
nano
znsn
gas sensor
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CN201811007612.8A
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Chinese (zh)
Inventor
王秀宇
李�亨
朱宣同
夏梦真
傅惠
刘颜鹏
丁伯楠
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Tianjin University
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Tianjin University
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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

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  • Chemical & Material Sciences (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 present invention discloses a kind of metal oxide base ethyl alcohol gas sensor preparation method for working in room temperature, and key step includes: to prepare the flower-shaped ZnSnO of 3D first3Presoma ZnSn (OH)6, and dried at 40 DEG C；Successively weigh ZnSn (OH)6And nano-TiO2, deionized water is added, first magnetic agitation, then ultrasonic disperse both make uniformly mixing, and finally the magnetic agitation again at 40 DEG C, makes water volatilization concentration at paste；Then above-mentioned paste is coated in interdigital electrode using lacquering technique, makes its film forming, is then dried under the conditions of 40 DEG C；Finally above-mentioned membrane coated electrode is heat-treated in high temperature, presoma ZnSn (OH)6Dehydration forms ZnSnO at high temperature3, during the dehydration process and and nano-TiO2Chemisorption is bonded together to form, nano-TiO is formed2/ZnSnO3Compound.

Description

Work in the metal oxide base ethyl alcohol gas sensor preparation method of room temperature
Technical field
It is the invention belongs to semiconductor gas sensor field, in particular to a kind of to work at room temperature and air-sensitive performance is excellent Good metal oxide base ethyl alcohol gas sensor preparation method.
Background technique
The environment of human lives and surrounding air are closely bound up, some hazardous gases (such as coal gas, natural gas, liquefied gas) To people life bring great convenience while, safety also can not be ignored, hazardous gas cause explosion, fire, in The accidents such as poison it is watchful importance of the people to effective monitoring and the prevention of hazardous gas.Gas sensor can help people It monitors the particular risk gas in environment, prevents the generation of peril；And Metal Oxide Semiconductor Gas Sensing sensor because Gas sensitive is easier to the advantages that preparation, environmental protection by extensive concern both domestic and external and research.
Zinc metastannate (ZnSnO3) it is a kind of ternary composite metal oxide semiconductor with perovskite structure, it has both ZnO and SnO2The advantages of two kinds of materials, shows excellent air-sensitive performance and thermal stability.But it is partly led with binary metal oxide Body (such as WO3、ZnO、SnO2) material is the same, ZnSnO3Gas sensor, which must work, is just able to achieve good air-sensitive at 200 DEG C or more Performance, this severely limits its applications in the hazardous gases such as inflammable, explosive.For this problem, the present invention is in ZnSnO3 It is middle to introduce ultraviolet light-sensitive material nano-TiO2, and under action of ultraviolet light, by changing the gas sensing mechanism of prepared sensor, Develop a kind of ethanol sensor that can be worked at room temperature.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of metal oxide base second for working in room temperature Alcohol gas sensor preparation method reduces ZnSnO3The operating temperature of gas sensor.
The present invention is proposes in solution background technique the technical issues of, the technical solution adopted is that: work in the gold of room temperature Belong to oxide-base ethyl alcohol gas sensor preparation method, includes the following steps:
1) the flower-shaped ZnSnO of 3D is prepared3Presoma ZnSn (OH)6, and dried at 40 DEG C；
2) ZnSn (OH) is successively weighed6And nano-TiO2, deionized water is added, first magnetic agitation, then ultrasonic disperse makes The two uniformly mixes, finally the magnetic agitation again at 40 DEG C, makes water volatilization concentration at paste；
3) above-mentioned paste is coated in interdigital electrode using lacquering technique, makes its film forming, is then dried under the conditions of 40 DEG C；
4) above-mentioned membrane coated electrode is heat-treated in high temperature, presoma ZnSn (OH)6Dehydration forms ZnSnO at high temperature3, During the dehydration process and and nano-TiO2Chemisorption is bonded together to form, nano-TiO is formed2/ZnSnO3Compound.
Nano-TiO in step 2) of the present invention2With ZnSn (OH)6Powder quality ratio m2/m1It is 20%.
The utility model has the advantages that
1, the nano-TiO in ultraviolet light interdigital electrode2/ZnSnO3Compound changes ZnSnO3The air-sensitive of sensor Mechanism makes it just have good air-sensitive performance at room temperature.
2, the present invention reduces ZnSnO3The operating temperature of gas sensor, and gas sensor can obtain at room temperature compared with Good air-sensitive performance.
Detailed description of the invention
Fig. 1 is gas sensor schematic diagram (a) and gas-sensitive sensor structure schematic diagram (b) in the present invention；
Fig. 2 is the gas response curve of the present invention at room temperature, and illustration is nano-TiO used in the gas sensor2/ ZnSnO3Compound shape appearance figure；
Fig. 3 is air-sensitive performance of the gas sensor of the present invention in working and room temperature:
(a) the response-recovery characteristic curve in different ethanol concentration environment
(b) the response-recovery characteristic curve when concentration of alcohol is 10ppm；
Specific embodiment
Below in conjunction with specific embodiments and the drawings, the present invention will be further described.
With the flower-shaped ZnSnO of 3D3As gas sensitive, with ultraviolet light-sensitive material nano-TiO2, it is modified, is prepared (25 DEG C) are just with the ethyl alcohol gas sensor of excellent air-sensitive performance at room temperature.
(1) the flower-shaped ZnSnO of 3D is prepared according to the method in this seminar patent of invention CN201810304991.03Presoma ZnSn(OH)6Powder；
(2) m in mass ratio1:m2:m3=5:1:250 weighs the flower-shaped ZnSn of 3D (OH) respectively6Powder, nano-TiO2, go from Sub- water is placed in a beaker, and then magnetic agitation 20min is uniformly mixed, subsequent re-ultrasonic dispersion 30min, finally in a heated condition (40 DEG C) magnetic agitation again makes the excessive moisture in mixed liquor volatilize concentration into paste；
(3) paste in step (2) is coated uniformly in gold thread interdigital electrode using lacquering technique (speed 50r/s), And film forming is dried under the conditions of 40 DEG C；
(4) by the film forming interdigital electrode in step (3) at 500 DEG C high-temperature heat treatment 2h, in the process, presoma ZnSn(OH)6Dehydration forms ZnSnO at high temperature3, and and nano-TiO2Chemisorption is bonded together to form, nano-TiO is formed2/ ZnSnO3Compound, as shown in Fig. 2 illustration, the flower-shaped ZnSnO of prepared 3D3Particle is micron order.It is coated with TiO2/ZnSnO3It is multiple The interdigital electrode for closing object is the core component of gas sensor, as shown in Fig. 1 (a).
(5) gas-sensitive sensing element made from step (4) is assembled by Fig. 1 (b), the LED of medium wavelength 365nm is ultraviolet Lamp and gas-sensitive sensing element distance are 2cm；Gas sensor element is connect into 100V voltage, LED ultraviolet lamp according to shown in Fig. 1 (b) 5V voltage is connect, ultraviolet signal controlled switch is opened, prepared sensor can work.
TiO2/ZnSnO3The test of compound gas sensor shows: working as nano-TiO2With the flower-shaped ZnSn of 3D (OH)6Powder matter Amount compares m2/m1When being 20%, under 1000ppm ethanol gas concentration, response R of the gas sensor in room temperaturea/RgIt reaches It is 36.6 to maximum, as shown in Fig. 2, mass ratio at this time is optimum proportioning；For TiO2/ZnSnO3When compound optimum proportioning Gas sensor, further test show response-recovery of the gas sensor under different ethanol gas concentrations when room temperature Shown in characteristic such as Fig. 3 (a), and in most 10ppm, prepared gas sensor response and recovery time are respectively 4s and 17s, As shown in Fig. 3 (b).
In conclusion in ultraviolet light-sensitive material nano-TiO2Under the assistance of ultraviolet light, ZnSnO can be reduced3Gas sensing The operating temperature of device makes it just have good air-sensitive performance at room temperature.This method can be applied to other low temperature gas Dependent sensor.

Claims (2)

1. working in the metal oxide base ethyl alcohol gas sensor preparation method of room temperature, which comprises the steps of:
1) the flower-shaped ZnSnO of 3D is prepared3Presoma ZnSn (OH)6, and dried at 40 DEG C；
2) ZnSn (OH) is successively weighed6And nano-TiO2, deionized water is added, first magnetic agitation, then ultrasonic disperse makes the two Uniformly mixing, finally the magnetic agitation again at 40 DEG C, makes water volatilization concentration at paste；
3) above-mentioned paste is coated in interdigital electrode using lacquering technique, makes its film forming, is then dried under the conditions of 40 DEG C；
4) above-mentioned membrane coated electrode is heat-treated in high temperature, presoma ZnSn (OH)6Dehydration forms ZnSnO at high temperature3, de- During water and and nano-TiO2Chemisorption is bonded together to form, nano-TiO is formed2/ZnSnO3Compound.
2. the metal oxide base ethyl alcohol gas sensor preparation method according to claim 1 for working in room temperature, special Sign is, nano-TiO in the step 2)2With ZnSn (OH)6Powder quality ratio m2/m1It is 20%.
CN201811007612.8A 2018-08-31 2018-08-31 Work in the metal oxide base ethyl alcohol gas sensor preparation method of room temperature Pending CN109187662A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110208326A (en) * 2019-06-25 2019-09-06 天津大学 Work in the preparation method of the metal composite oxide base ethyl alcohol gas sensor under low temperature
CN111077189A (en) * 2019-12-10 2020-04-28 天津大学 Preparation method of high-performance ethanol gas sensor working at low temperature

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN86106681A (en) * 1986-10-09 1987-10-21 云南大学 The making of zinc metastannate (zinc stannate) gas sensor
CN101251508B (en) * 2008-04-01 2011-06-22 重庆大学 Method for manufacturing gas sensor for testing hydrogen
KR101364138B1 (en) * 2012-03-13 2014-02-18 인하대학교 산학협력단 ZnSnO3 nanorods coated with palladium particles, a preparation method thereof, and gas sensor using the same
CN104418382A (en) * 2013-09-09 2015-03-18 天津大学 Method for preparing zinc metastannate by hydrothermal method
CN107064235A (en) * 2016-11-02 2017-08-18 景德镇学院 A kind of Pt nanoparticles modify ZnSnO3The preparation method of nanosheet gas-sensitive material

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN86106681A (en) * 1986-10-09 1987-10-21 云南大学 The making of zinc metastannate (zinc stannate) gas sensor
CN101251508B (en) * 2008-04-01 2011-06-22 重庆大学 Method for manufacturing gas sensor for testing hydrogen
KR101364138B1 (en) * 2012-03-13 2014-02-18 인하대학교 산학협력단 ZnSnO3 nanorods coated with palladium particles, a preparation method thereof, and gas sensor using the same
CN104418382A (en) * 2013-09-09 2015-03-18 天津大学 Method for preparing zinc metastannate by hydrothermal method
CN107064235A (en) * 2016-11-02 2017-08-18 景德镇学院 A kind of Pt nanoparticles modify ZnSnO3The preparation method of nanosheet gas-sensitive material

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
XIUYU WANG等: "Synthesis of 3D flower-like ZnSnO3 and improvement of ethanol-sensing properties at room temperature based on nano-TiO2 decoration and UV radiation", 《SENSORS AND ACTUATORS B: CHEMICAL》 *
刘焕林等: "偏锡酸锌气敏材料敏感机理的研究", 《功能材料》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110208326A (en) * 2019-06-25 2019-09-06 天津大学 Work in the preparation method of the metal composite oxide base ethyl alcohol gas sensor under low temperature
CN111077189A (en) * 2019-12-10 2020-04-28 天津大学 Preparation method of high-performance ethanol gas sensor working at low temperature

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Application publication date: 20190111