CN108663420A - The methane gas sensor and preparation method of tin mud supported palladium in a kind of tin plating technique - Google Patents

The methane gas sensor and preparation method of tin mud supported palladium in a kind of tin plating technique Download PDF

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CN108663420A
CN108663420A CN201810440026.6A CN201810440026A CN108663420A CN 108663420 A CN108663420 A CN 108663420A CN 201810440026 A CN201810440026 A CN 201810440026A CN 108663420 A CN108663420 A CN 108663420A
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tin
gas sensor
porous
nanosolids
methane gas
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CN108663420B (en
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李建中
徐浩元
付玉
尹远洪
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Shenzhen Aiduoke Sensor Technology Co Ltd
Northeastern University China
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Shenzhen Sai Fling Technology Co Ltd
Northeastern University China
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Abstract

The methane gas sensor and preparation method of tin mud supported palladium, belong to semiconductor gas sensor and environmental monitoring technology field in a kind of tin plating technique.The present invention is directed to the waste problem of the tin mud of the generation in tin plating technique, and the modifications such as washing, pore-creating, sintering have been carried out to tin mud, and has carried out Metal Palladium load on this basis and be prepared for methane sensitive material.Prepared gas sensor is to CH4Higher sensitivity is shown when gas detection and preferably responds recovery characteristics.Material preparation of the present invention and gas sensor preparation process have many advantages, such as that simple for process, cost of material is low, short preparation period, can be used for industrializing, produce in enormous quantities.Meanwhile the comprehensive utilization of resource is realized in terms of raw material sources.Thus the sensor has broad application prospects in methane gas context of detection.

Description

The methane gas sensor and preparation method of tin mud supported palladium in a kind of tin plating technique
Technical field
The invention belongs to conductor oxidate gas sensors and environmental monitoring technology field, and in particular to one kind is based on plating Tin mud in process of tin is modified and the methane gas sensor and preparation method thereof of supported palladium.
Background technology
Methane is a kind of colorless and odorless, flammable explosive gas, and aerial explosion is limited to 5%~15% (volume point Number).Methane is the main component of biogas, natural gas and combustible ice, the energy supply being widely used in life and industry.But Methane is also to cause one of predominant gas of greenhouse effects, and with methane in people's lives universal, caused by its leakage Safety accident it is also more and more.Therefore monitoring in real time and early warning are carried out accurately and rapidly reducing caused by it methane Safety accident is vital.Currently used for methane gas detection sensor type mainly include catalytic type, thermal conductivity type with And spectral absorption type.Wherein, catalytic type sensor becomes because of its simple in structure, at low cost and good CH_4 detection characteristic Current most popular methane gas sensor.
In sensitive material used in catalytic type methane gas sensor, nano SnO2Because it is with good physical chemistry Performance and air-sensitive performance and be widely studied.Currently, nano SnO2Preparation method mainly include sol-gal process, hydro-thermal method And chemical precipitation method.Above method is in production nano SnO2All there is low production efficiency when material, be unable to industrial mass The problems such as.Meanwhile although pure nano SnO2Sensitive material has methane gas certain response characteristic, but there are sensitivity The problems such as low and stability is poor.To nano SnO2It is the most effective side for improving its air-sensitive performance that material, which carries out precious metal doping, Method.Wherein, metal Pd is to methane oxidation because having good catalytic effect, and doping process is simple, good cycle and by It is widely used in nano SnO2Study on the modification in.
In process of tin is electroplated, predominantly divalent tin ion participates in electroplating process, but part is had in electroplating process Bivalent Tin is oxidized to tetravalent tin on anode, or when electrolyte splash is in air, and the Bivalent Tin in electrolyte is by oxygen Change and forms tetravalent tin.In acidic electrolysis bath, tetravalent tin does not participate in electrolyting precipitation process, when its content in the electrolytic solution is more than When 10g/L, tin mud will be generated and be precipitated out from electrolyte, be deposited on electrolyte accumulator tank slot bottom.The main component of tin mud For SnO2, wherein also containing a small amount of sulfonate and sulfur-bearing and containing sulfonic compound.The generation of tin mud not only increases life Cost is produced, the loss for also resulting in cathode tin increases, and a large amount of depositions also affect being normally carried out for plating process of tin.Currently, The tin mud generated during tin plating is not reasonably utilized, therefore this patent has studied and is modified processing system to tin mud Standby methane sensitive material to realize the comprehensive utilization of resource, and reduces production cost.
Invention content
For existing nano SnO2In the problem of preparation process and tin plating technique the problems such as the waste of tin mud, The present invention proposes a kind of technology of tin mud comprehensive utilization.Based on this purpose, the tin mud generated in tin plating technique is carried out first Modification, and carried out precious metal palladium load to it on this basis and be prepared for methane sensitive material, prepared methane gas Body sensor, which can be realized, fast and accurately detects methane.
Technical scheme of the present invention:
The methane gas sensor of tin mud supported palladium in a kind of tin plating technique, which is plate armature, with ceramics As substrate, the front of ceramic substrate is arranged interdigital gold-plated electrode, sensitive material film is applied on interdigital gold-plated electrode substrate, quick Sense material is that the tin mud that generates is modified and the Porous nanosolids of carried metal palladium in tin plating technique, and the back side of ceramic substrate is set Set Micro high-temperature heating plate.
The Porous nanosolids are by the SnO of grain size about 10~20nm2Near-spherical bulky grain made of little particle is reunited.
The thickness of the sensitive material film is 0.2~0.5mm.A length of 3.8~4mm of the ceramic substrate, width be 3~ 3.2mm, thickness are 0.6~0.8mm.
The preparation method of the methane gas sensor of tin mud supported palladium, includes the following steps in a kind of tin plating technique:
(1) modification of tin mud prepares Porous nanosolids
It dries tin mud deionized water and absolute ethyl alcohol filtering and washing and in air;Take the tin mud after drying in ball milling In tank, polyethylene glycol and polyvinyl alcohol is added as pore creating material, obtained mixture is packed into autoclave by mechanical ball mill mixing In, it is heated to 160~200 DEG C after sealing, cooled to room temperature after 3~5h of constant temperature;By autoclave treated porous nano Solid takes out, and after being sintered 2~4h at 400~600 DEG C in air, obtains the modified Porous nanosolids of tin mud;It is described Porous nanosolids be by the SnO of grain size about 10~20nm2Near-spherical bulky grain made of little particle is reunited, after the drying Tin mud, polyvinyl alcohol and polyethylene glycol mass ratio be 5:1~3:7~9.
(2) PdCl is prepared2The Porous nanosolids gas sensitive of load
By PdCl2It is dissolved in the mixed solution of deionized water and absolute ethyl alcohol, adds Porous nanosolids and as drop Mixed liquor is placed in 2~4h of heat treatment at 400~480 DEG C, obtains PdCl by the antimony oxide of resist, uniform stirring2Load Porous nanosolids gas sensitive;The PdCl2, as friction reducer antimony oxide and Porous nanosolids quality it Than being 5~20:1:100, PdCl2A concentration of 0.5~2mg/ml in ionized water and absolute ethyl alcohol mixed solution.
(3) methane gas sensor is prepared
The PdCl that step (2) is prepared2The Porous nanosolids gas sensitive of load and deionized water in mass ratio 1 ~3:After 1 mixing, slurry is made in grinding, slurry is coated uniformly on the interdigital gold-plated electrode on ceramic substrate, naturally dry Working electrode and heating electrode welding are obtained into methane gas sensor on gas sensor pedestal afterwards.
The drying temperature of tin mud described in step (1) is 80~120 DEG C, and drying time is 8~12 hours.
Polyethylene glycol described in step (1) is polyethylene glycol 400.
Deionized water and the volume ratio of absolute ethyl alcohol are 1 in mixed solution described in step (2):1.
Beneficial effects of the present invention:
(1) waste problem of the present invention for the tin mud generated in tin plating technique, it is proposed that sensitive with the clay standby methane of tin Material realizes the comprehensive utilization of resource.
(2) a kind of tin mud modification treatment technology proposed by the present invention, prepared Porous nanosolids have smaller grain Diameter (10~20nm), and particle dispersion is preferable, is conducive to the diffusion of gas molecule, with higher sensitivity and preferably Response-recovery characteristic.
(3) present invention is directed to pure SnO2The method of the problems of gas sensitive, proposition precious metal doping improves it Comprehensive performance.Noble metal can largely improve the air-sensitive performance of sensitive material to the activation of object gas, and increase The stability of strong methane gas sensor, reduces null offset.
(4) present invention uses the tin mud in tin plating technique to prepare gas sensitive as raw material, and cost of material is low, and solves Current SnO2The problems such as low production efficiency in the presence of preparation.
(5) material preparation process of the present invention has many advantages, such as simple for process, short preparation period, can be used for industry Change, produce in enormous quantities.
Description of the drawings
Fig. 1 is scanning electron microscope (SEM) photo of modified tin mud;
Fig. 2 is the structural schematic diagram of the methane gas sensor of tin mud supported palladium;
In figure:1 ceramic substrate;2 interdigital gold-plated electrodes;3 Micro high-temperature heating plates;4 sensitive material films.
Fig. 3 is sensor in the embodiment of the present invention 2 to the CH of various concentration4The sensitivity of gas, and to 2000ppm The response-recovery curve (small figure) of methane gas;
In figure:The sensitivity S of gas sensor is defined as:S=Ra/Rg, RaAnd RgRespectively sensor is in air and first Resistance value when in alkane gas between interdigital electrode;
Specific implementation mode
It is prepared by the methane gas sensor of 1 tin mud supported palladium of embodiment
Take 5g it is washed, it is dry after tin mud in ball grinder, and be added 8g polyethylene glycol 400s and 2g polyvinyl alcohol into Row mechanical ball mill, the mixture that ball milling is obtained in autoclave after 160 DEG C of constant temperature 4h, take out and at 500 DEG C in air by cooling Middle sintering 3h obtains the modified Porous nanosolids of tin mud.By the PdCl of 0.1g2It is dissolved in 10ml deionized waters and absolute ethyl alcohol Mixed solution in, and 1g Porous nanosolids and 10mg antimony oxides are added, after uniform stirring 3h, at 450 DEG C in sky It is heat-treated 2h in gas, obtains PdCl2The Porous nanosolids gas sensitive of load.By PdCl2The Porous nanosolids material of load With deionized water in mass ratio 2:After 1 mixing, grinding is made slurry and is coated uniformly on ceramic substrate, carries out after natural drying Electrode welding obtains methane gas sensor.
It is prepared by the methane gas sensor of 2 tin mud supported palladium of embodiment
Take 5g it is washed, it is dry after tin mud in ball grinder, and be added 8g polyethylene glycol 400s and 2g polyvinyl alcohol into Row mechanical ball mill, the mixture that ball milling is obtained in autoclave after 180 DEG C of constant temperature 4h, take out and at 500 DEG C in air by cooling Middle sintering 3h obtains the modified Porous nanosolids of tin mud.By the PdCl of 0.1g2It is dissolved in 10ml deionized waters and absolute ethyl alcohol Mixed solution in, and 1g Porous nanosolids and 10mg antimony oxides are added, after uniform stirring 3h, at 450 DEG C in sky It is heat-treated 2h in gas, obtains PdCl2The Porous nanosolids gas sensitive of load.By PdCl2The Porous nanosolids material of load With deionized water in mass ratio 2:After 1 mixing, grinding is made slurry and is coated uniformly on ceramic substrate, carries out after natural drying Electrode welding obtains methane gas sensor.
It is prepared by the methane gas sensor of 3 tin mud supported palladium of embodiment
Take 5g it is washed, it is dry after tin mud in ball grinder, and be added 8g polyethylene glycol 400s and 2g polyvinyl alcohol into Row mechanical ball mill, the mixture that ball milling is obtained in autoclave after 200 DEG C of constant temperature 4h, take out and at 500 DEG C in air by cooling Middle sintering 3h obtains the modified Porous nanosolids of tin mud.By the PdCl of 0.1g2It is dissolved in 10ml deionized waters and absolute ethyl alcohol Mixed solution in, and 1g Porous nanosolids and 10mg antimony oxides are added, after uniform stirring 3h, at 450 DEG C in sky It is heat-treated 2h in gas, obtains PdCl2The Porous nanosolids gas sensitive of load.By PdCl2The Porous nanosolids material of load With deionized water in mass ratio 2:After 1 mixing, grinding is made slurry and is coated uniformly on ceramic substrate, carries out after natural drying Electrode welding obtains methane gas sensor.
It is prepared by the methane gas sensor of 4 tin mud supported palladium of embodiment
Take 5g it is washed, it is dry after tin mud in ball grinder, and be added 8g polyethylene glycol 400s and 2g polyvinyl alcohol into Row mechanical ball mill, the mixture that ball milling is obtained in autoclave after 180 DEG C of constant temperature 3h, take out and at 500 DEG C in air by cooling Middle sintering 3h obtains the modified Porous nanosolids of tin mud.By the PdCl of 0.1g2It is dissolved in 10ml deionized waters and absolute ethyl alcohol Mixed solution in, and 1g Porous nanosolids and 10mg antimony oxides are added, after uniform stirring 3h, at 450 DEG C in sky It is heat-treated 2h in gas, obtains PdCl2The Porous nanosolids gas sensitive of load.By PdCl2The Porous nanosolids material of load With deionized water in mass ratio 2:After 1 mixing, grinding is made slurry and is coated uniformly on ceramic substrate, carries out after natural drying Electrode welding obtains methane gas sensor.
It is prepared by the methane gas sensor of 5 tin mud supported palladium of embodiment
Take 5g it is washed, it is dry after tin mud in ball grinder, and be added 8g polyethylene glycol 400s and 2g polyvinyl alcohol into Row mechanical ball mill, the mixture that ball milling is obtained in autoclave after 180 DEG C of constant temperature 5h, take out and at 500 DEG C in air by cooling Middle sintering 3h obtains the modified Porous nanosolids of tin mud.By the PdCl of 0.1g2It is dissolved in 10ml deionized waters and absolute ethyl alcohol Mixed solution in, and 1g Porous nanosolids and 10mg antimony oxides are added, after uniform stirring 3h, at 450 DEG C in sky It is heat-treated 2h in gas, obtains PdCl2The Porous nanosolids gas sensitive of load.By PdCl2The Porous nanosolids material of load With deionized water in mass ratio 2:After 1 mixing, grinding is made slurry and is coated uniformly on ceramic substrate, carries out after natural drying Electrode welding obtains methane gas sensor.
It is prepared by the methane gas sensor of 6 tin mud supported palladium of embodiment
Take 5g it is washed, it is dry after tin mud in ball grinder, and be added 8g polyethylene glycol 400s and 2g polyvinyl alcohol into Row mechanical ball mill, the mixture that ball milling is obtained in autoclave after 180 DEG C of constant temperature 4h, take out and at 400 DEG C in air by cooling Middle sintering 3h obtains the modified Porous nanosolids of tin mud.By the PdCl of 0.1g2It is dissolved in 10ml deionized waters and absolute ethyl alcohol Mixed solution in, and 1g Porous nanosolids and 10mg antimony oxides are added, after uniform stirring 3h, at 450 DEG C in sky It is heat-treated 2h in gas, obtains PdCl2The Porous nanosolids gas sensitive of load.By PdCl2The Porous nanosolids material of load With deionized water in mass ratio 2:After 1 mixing, grinding is made slurry and is coated uniformly on ceramic substrate, carries out after natural drying Electrode welding obtains methane gas sensor.
It is prepared by the methane gas sensor of 7 tin mud supported palladium of embodiment
Take 5g it is washed, it is dry after tin mud in ball grinder, and be added 8g polyethylene glycol 400s and 2g polyvinyl alcohol into Row mechanical ball mill, the mixture that ball milling is obtained in autoclave after 180 DEG C of constant temperature 4h, take out and at 600 DEG C in air by cooling Middle sintering 3h obtains the modified Porous nanosolids of tin mud.By the PdCl of 0.1g2It is dissolved in 10ml deionized waters and absolute ethyl alcohol Mixed solution in, and 1g Porous nanosolids and 10mg antimony oxides are added, after uniform stirring 3h, at 450 DEG C in sky It is heat-treated 2h in gas, obtains PdCl2The Porous nanosolids gas sensitive of load.By PdCl2The Porous nanosolids material of load With deionized water in mass ratio 2:After 1 mixing, grinding is made slurry and is coated uniformly on ceramic substrate, carries out after natural drying Electrode welding obtains methane gas sensor.
It is prepared by the methane gas sensor of 8 tin mud supported palladium of embodiment
Take 5g it is washed, it is dry after tin mud in ball grinder, and be added 8g polyethylene glycol 400s and 2g polyvinyl alcohol into Row mechanical ball mill, the mixture that ball milling is obtained in autoclave after 180 DEG C of constant temperature 4h, take out and at 500 DEG C in air by cooling Middle sintering 2h obtains the modified Porous nanosolids of tin mud.By the PdCl of 0.1g2It is dissolved in 10ml deionized waters and absolute ethyl alcohol Mixed solution in, and 1g Porous nanosolids and 10mg antimony oxides are added, after uniform stirring 3h, at 450 DEG C in sky It is heat-treated 2h in gas, obtains PdCl2The Porous nanosolids gas sensitive of load.By PdCl2The Porous nanosolids material of load With deionized water in mass ratio 2:After 1 mixing, grinding is made slurry and is coated uniformly on ceramic substrate, carries out after natural drying Electrode welding obtains methane gas sensor.
It is prepared by the methane gas sensor of 9 tin mud supported palladium of embodiment
Take 5g it is washed, it is dry after tin mud in ball grinder, and be added 8g polyethylene glycol 400s and 2g polyvinyl alcohol into Row mechanical ball mill, the mixture that ball milling is obtained in autoclave after 180 DEG C of constant temperature 4h, take out and at 500 DEG C in air by cooling Middle sintering 4h obtains the modified Porous nanosolids of tin mud.By the PdCl of 0.1g2It is dissolved in 10ml deionized waters and absolute ethyl alcohol Mixed solution in, and 1g Porous nanosolids and 10mg antimony oxides are added, after uniform stirring 3h, at 450 DEG C in sky It is heat-treated 2h in gas, obtains PdCl2The Porous nanosolids gas sensitive of load.By PdCl2The Porous nanosolids material of load With deionized water in mass ratio 2:After 1 mixing, grinding is made slurry and is coated uniformly on ceramic substrate, carries out after natural drying Electrode welding obtains methane gas sensor.
It is prepared by the methane gas sensor of 10 tin mud supported palladium of embodiment
Take 5g it is washed, it is dry after tin mud in ball grinder, and be added 8g polyethylene glycol 400s and 2g polyvinyl alcohol into Row mechanical ball mill, the mixture that ball milling is obtained in autoclave after 180 DEG C of constant temperature 3h, take out and at 500 DEG C in air by cooling Middle sintering 3h obtains the modified Porous nanosolids of tin mud.By the PdCl of 0.05g2It is dissolved in 10ml deionized waters and absolute ethyl alcohol Mixed solution in, and 1g Porous nanosolids and 10mg antimony oxides are added, after uniform stirring 3h, at 450 DEG C in sky It is heat-treated 2h in gas, obtains PdCl2The Porous nanosolids gas sensitive of load.By PdCl2The Porous nanosolids material of load With deionized water in mass ratio 2:After 1 mixing, grinding is made slurry and is coated uniformly on ceramic substrate, carries out after natural drying Electrode welding obtains methane gas sensor.
It is prepared by the methane gas sensor of 11 tin mud supported palladium of embodiment
Take 5g it is washed, it is dry after tin mud in ball grinder, and be added 8g polyethylene glycol 400s and 2g polyvinyl alcohol into Row mechanical ball mill, the mixture that ball milling is obtained in autoclave after 180 DEG C of constant temperature 3h, take out and at 500 DEG C in air by cooling Middle sintering 3h obtains the modified Porous nanosolids of tin mud.By the PdCl of 0.2g2It is dissolved in 10ml deionized waters and absolute ethyl alcohol Mixed solution in, and 1g Porous nanosolids and 10mg antimony oxides are added, after uniform stirring 3h, at 450 DEG C in sky It is heat-treated 2h in gas, obtains PdCl2The Porous nanosolids gas sensitive of load.By PdCl2The Porous nanosolids material of load With deionized water in mass ratio 2:After 1 mixing, grinding is made slurry and is coated uniformly on ceramic substrate, carries out after natural drying Electrode welding obtains methane gas sensor.

Claims (8)

1. the methane gas sensor of tin mud supported palladium in a kind of tin plating technique, which is characterized in that the sensor is flat knot Structure, using ceramic substrate as substrate, interdigital gold-plated electrode is arranged in the front of ceramic substrate, and sensitive material is applied on interdigital gold-plated electrode Expect film, sensitive material is that the tin mud that generates is modified and the Porous nanosolids of carried metal palladium in tin plating technique, ceramic base Micro high-temperature heating plate is arranged in the back side of piece.
2. the methane gas sensor of tin mud supported palladium in a kind of tin plating technique according to claim 1, which is characterized in that The Porous nanosolids are by the SnO of grain size about 10~20nm2Near-spherical bulky grain made of little particle is reunited.
3. the methane gas sensor of tin mud supported palladium, feature exist in a kind of tin plating technique according to claim 1 or claim 2 In the thickness of the sensitive material film is 0.2~0.5mm;A length of 3.8~4mm of the ceramic substrate, width be 3~ 3.2mm, thickness are 0.6~0.8mm.
4. the preparation method of the methane gas sensor of tin mud supported palladium in any tin plating techniques of claim 1-3, special Sign is that steps are as follows:
(1) modification of tin mud prepares Porous nanosolids
It dries tin mud deionized water and absolute ethyl alcohol filtering and washing and in air;Take the tin mud after drying in ball grinder In, and polyethylene glycol and polyvinyl alcohol is added as pore creating material, obtained mixture is packed into autoclave by mechanical ball mill mixing In, it is heated to 160~200 DEG C after sealing, cooled to room temperature after 3~5h of constant temperature;By autoclave treated porous nano Solid takes out, and after being sintered 2~4h at 400~600 DEG C in air, obtains the modified Porous nanosolids of tin mud;It is described The mass ratio of tin mud, polyvinyl alcohol and polyethylene glycol after drying is 5:1~3:7~9;
(2) PdCl is prepared2The Porous nanosolids gas sensitive of load
By PdCl2It is dissolved in the mixed solution of deionized water and absolute ethyl alcohol, adds Porous nanosolids and as friction reducer Mixed liquor is placed in 2~4h of heat treatment at 400~480 DEG C, obtains PdCl by antimony oxide, uniform stirring2The porous of load receives Rice solid gas sensitive;The PdCl2, as friction reducer antimony oxide and Porous nanosolids mass ratio be 5 ~20:1:100, PdCl2A concentration of 0.5~2mg/ml in ionized water and absolute ethyl alcohol mixed solution;
(3) methane gas sensor is prepared
The PdCl that step (2) is prepared2The Porous nanosolids gas sensitive of load and deionized water in mass ratio 1~3:1 After mixing, slurry is made in grinding, slurry is coated uniformly on the interdigital gold-plated electrode on ceramic substrate, after natural drying by work Make electrode and heat electrode welding on gas sensor pedestal, obtains methane gas sensor.
5. the preparation method of the methane gas sensor of tin mud supported palladium in a kind of tin plating technique according to claim 4, It is characterized in that, the drying temperature of the tin mud described in step (1) is 80~120 DEG C, drying time is 8~12 hours.
6. the preparation side of the methane gas sensor of tin mud supported palladium in a kind of tin plating technique according to claim 4 or 5 Method, which is characterized in that the polyethylene glycol described in step (1) is polyethylene glycol 400.
7. the preparation side of the methane gas sensor of tin mud supported palladium in a kind of tin plating technique according to claim 4 or 5 Method, which is characterized in that deionized water and the volume ratio of absolute ethyl alcohol are 1 in the mixed solution described in step (2):1.
8. the preparation method of the methane gas sensor of tin mud supported palladium in a kind of tin plating technique according to claim 6, It is characterized in that, deionized water and the volume ratio of absolute ethyl alcohol are 1 in mixed solution described in step (2):1.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109181641A (en) * 2018-11-09 2019-01-11 东北大学 A kind of SnO preparing NiO doping using tin mud as raw material2The method of porous nano particle
CN111017987A (en) * 2019-12-31 2020-04-17 深圳爱多科传感技术有限公司 Method for preparing CO sensitive material by purifying and doping modification of tin anode slime
CN112142098A (en) * 2019-06-28 2020-12-29 东北大学 Ag coated SnO2Preparation of SO2Method for sensing material
CN113651611A (en) * 2021-07-13 2021-11-16 广东迈能欣科技有限公司 Ceramic gas sensor porous structure sensitive slurry and preparation method of ceramic gas sensor
CN116183682A (en) * 2023-02-23 2023-05-30 广州海谷电子科技有限公司 Patch type VOC sensor and manufacturing method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1284474A (en) * 1999-08-17 2001-02-21 惠春 Tin dioxide-base nanometer crystal gas-sensitive material and its preparation
CN101571504A (en) * 2009-06-04 2009-11-04 哈尔滨工程大学 Noble metal doped SnO2 composite material and preparation method thereof
CN104843770A (en) * 2015-03-30 2015-08-19 中国钢研科技集团有限公司 Method of resource utilization of tin sludge
CN105092659A (en) * 2015-08-28 2015-11-25 云南大学 Pt-doped SnO2 mesoporous thin film-based gas sensor preparation method
CN205506741U (en) * 2016-03-16 2016-08-24 哈尔滨理工大学 AlN thermal insulation bilateral structure low -grade fever board gas sensor

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1284474A (en) * 1999-08-17 2001-02-21 惠春 Tin dioxide-base nanometer crystal gas-sensitive material and its preparation
CN101571504A (en) * 2009-06-04 2009-11-04 哈尔滨工程大学 Noble metal doped SnO2 composite material and preparation method thereof
CN104843770A (en) * 2015-03-30 2015-08-19 中国钢研科技集团有限公司 Method of resource utilization of tin sludge
CN105092659A (en) * 2015-08-28 2015-11-25 云南大学 Pt-doped SnO2 mesoporous thin film-based gas sensor preparation method
CN205506741U (en) * 2016-03-16 2016-08-24 哈尔滨理工大学 AlN thermal insulation bilateral structure low -grade fever board gas sensor

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
宋明歆: "SnO2气敏性能与微观结构", 《中国优秀硕士学位论文全文数据库(工程科技I辑)》 *
栾春红: "二氧化锡多孔纳米固体的制备及性质研究", 《中国博士学位论文全文数据库(工程科技I辑)》 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109181641A (en) * 2018-11-09 2019-01-11 东北大学 A kind of SnO preparing NiO doping using tin mud as raw material2The method of porous nano particle
CN109181641B (en) * 2018-11-09 2021-09-07 东北大学 NiO-doped SnO prepared from tin mud2Method for producing porous nanoparticles
CN112142098A (en) * 2019-06-28 2020-12-29 东北大学 Ag coated SnO2Preparation of SO2Method for sensing material
CN111017987A (en) * 2019-12-31 2020-04-17 深圳爱多科传感技术有限公司 Method for preparing CO sensitive material by purifying and doping modification of tin anode slime
CN111017987B (en) * 2019-12-31 2022-05-13 深圳爱多科传感技术有限公司 Method for preparing CO sensitive material by purifying and doping modification of tin anode slime
CN113651611A (en) * 2021-07-13 2021-11-16 广东迈能欣科技有限公司 Ceramic gas sensor porous structure sensitive slurry and preparation method of ceramic gas sensor
CN116183682A (en) * 2023-02-23 2023-05-30 广州海谷电子科技有限公司 Patch type VOC sensor and manufacturing method thereof

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