CN101799446A - Room-temperature alcohol thin film gas sensor and preparation method thereof - Google Patents
Room-temperature alcohol thin film gas sensor and preparation method thereof Download PDFInfo
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- CN101799446A CN101799446A CN 201010148726 CN201010148726A CN101799446A CN 101799446 A CN101799446 A CN 101799446A CN 201010148726 CN201010148726 CN 201010148726 CN 201010148726 A CN201010148726 A CN 201010148726A CN 101799446 A CN101799446 A CN 101799446A
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Abstract
The invention discloses a room-temperature alcohol thin film gas sensor and a preparation method thereof, and relates to a gas sensor and a preparation method thereof. The invention solves the problems of long response and recovery time, poor gas selectivity, high working temperature, and high lowest detection limit for alcohol gases of conventional sensitive elements for measuring alcohol gases. The room-temperature alcohol thin film gas sensor consists of a gold interdigital glass substrate and an oxide film. The preparation method comprises the following steps: 1, preparing an oxide sol; 2, processing the gold interdigital glass substrate; 3, repeatedly operating for ten times according to the order in the step 2; and 4, sintering the gold interdigital glass substrate processed by the step 3 to obtain the room-temperature alcohol thin film gas sensor. The room-temperature alcohol thin film gas sensor has short response and recovery time, can selectively respond to the alcohol gases, and can detect the alcohol gases with the concentration of 2ppm at room temperature.
Description
Technical field
The present invention relates to a kind of gas sensor and preparation method thereof.
Background technology
Sensor of chemical gas uses conductor oxidate as sensing material at present, and this sensor general work temperature needs to consume lot of energy, so limited its practical application in portable field at 300~500 degree.Press for low-power consumption in safety in production field and Portable, personal sensor field at present, the low-cost sensor of working and room temperature.Metal oxide alcohols sensing element material after deliberation mainly concentrates on the SnO of doping
2, In
2O
3, ZnSnO
3And SmFeO
3, and detection gas is main mainly with alcohol gas.The SnO that bibliographical information Ag and Sb mix
2Sensing element is respectively 5 and 48 to the sensitivity of the alcohol gas of 50ppm under the heating voltage of 6V; SmFeO
3Be 370 when spending in operating temperature, the sensitivity of 50ppm alcohol gas is reached about 55; And composite oxides sensor ZrO
2-Fe
2O
3And SnO
2-Fe
2O
3, 200 degree during work the sensitivity to the alcohol gas of 1000ppm reach more than 20; Above-mentioned material is all very high to alcohols gas detectable concentration.The SnO that Sb mixes
2Sensing element be 48 to the sensitivity of the alcohol gas of 50ppm, but response and recovery time is long under the heating voltage of 6V, all in a few minutes scopes; SnO
2-Fe
2O
3Sensing element 200 degree during work the sensitivity to the alcohol gas of 1000ppm reach more than 20 but selectively relatively poor to other alcohols gases; Because methyl alcohol, ethanol are very similar to the character of propyl alcohol, these materials are very poor to the selective response of alcohols gas, and the practical operation temperature is also higher, and very high to the lowest detection line of alcohols gas, and this brings difficulty to practical application.
Summary of the invention
Goal of the invention of the present invention is for the response of the sensitive element existence that solves existing measurement alcohols gas and release time is long, poor, the working temperature height of gas-selectively, lowest detectable limit problem of higher to alcohols gas provides a kind of room-temperature alcohol thin film gas sensor and preparation method thereof.
Room-temperature alcohol thin film gas sensor of the present invention is made up of the interdigital glass substrate of gold and sull, and the oxide general formula that consists of sull is M
xO
y, wherein M is Cr, Ti, Zn, Fe, W or V, 1≤x≤2,1≤y≤5 wherein, and x, y are integer.The preparation method of room-temperature alcohol thin film gas sensor is as follows: one, preparation oxide sol: with M (NO
3)
yBe dissolved in the deionized water, obtaining concentration is the M (NO of 0.01mol/L
3)
ySolution, adding concentration is the concentrated hydrochloric acid of 6mol/L, gets mixed liquor, M (NO in the mixed liquor
3)
yWith the concentration ratio of hydrochloric acid be 2~4 ﹕ 1, in 110 ℃ heating jacket, reflux then, heating mixed liquor 2~8 hours, obtain M
xO
yOxide sol, 1≤x≤2,1≤y≤5 wherein, x, y are integer; Two, with the speed immersion M of the interdigital glass substrate of gold with 20~40 mm/min
xO
yStopped in the oxide sol 2~5 minutes, and mentioned with the speed of 20~40 mm/min again, then with the interdigital glass substrate oven dry of gold; Three, the reiteration according to step 2 operates ten times; Four, the golden interdigital glass substrate that will process through step 3 sintering 1 hour in 500 ℃ Muffle furnace namely gets room-temperature alcohol thin film gas sensor.
Room-temperature alcohol thin film gas sensor response of the present invention and release time are short, and the sample granularity of room-temperature alcohol thin film gas sensor of the present invention is evenly distributed, and particle is elliposoidal, and particle diameter is in 12~15nm scope.Room-temperature alcohol thin film gas sensor at room temperature has good sensitive property to low concentration alcohols gas.Room-temperature alcohol thin film gas sensor has the ability the low concentration propyl alcohol gas in the environment is carried out selective response.Particularly the propyl alcohol gas to the 2ppm low concentration detects, and the sensitivity of room-temperature alcohol thin film gas sensor reaches 3.1.Room-temperature alcohol thin film gas sensor of the present invention can optionally respond alcohols gas, and can detectable concentration be the alcohols gas of 2ppm promptly at room temperature.
Description of drawings
Fig. 1 is the micro-structure diagram of the room-temperature alcohol thin film gas sensor of preparation in the embodiment 12; Fig. 2 is response and the recovery characteristics curve map of the room-temperature alcohol thin film gas sensor of preparation in the embodiment 12 to different concentration ethanol gas; Fig. 3 is to the sensitivity curve of alcohol gas under the room-temperature alcohol thin film gas sensor room temperatures of embodiment ten, 11 and 12 preparations, under the room-temperature alcohol thin film gas sensor room temperature of-■-expression embodiment ten preparations to the sensitivity curve of alcohol gas, under the room-temperature alcohol thin film gas sensor room temperature of-▲-expression embodiment 11 preparations to the sensitivity curve of alcohol gas ,-● and under the room-temperature alcohol thin film gas sensor room temperature of-expression embodiment 12 preparations to the sensitivity curve of alcohol gas; Fig. 4 is to the sensitivity curve of propyl alcohol gas under the room-temperature alcohol thin film gas sensor room temperatures of embodiment ten, 11 and 12 preparations, under the room-temperature alcohol thin film gas sensor room temperature of-■-expression embodiment ten preparations to the sensitivity curve of propyl alcohol gas, under the room-temperature alcohol thin film gas sensor room temperature of-▲-expression embodiment 11 preparations to the sensitivity curve of propyl alcohol gas ,-● and under the room-temperature alcohol thin film gas sensor room temperature of-expression embodiment 12 preparations to the sensitivity curve of propyl alcohol gas.
Embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises any combination between each specific embodiment.
The specific embodiment one: room-temperature alcohol thin film gas sensor of the present invention is made up of the interdigital glass substrate of gold and sull, and the oxide general formula that consists of sull is M
xO
y, wherein M is Cr, Ti, Zn, Fe, W or V, 1≤x≤2,1≤y≤5 wherein, and x, y are integer.
The specific embodiment two: present embodiment and the specific embodiment one are different is that the oxide general formula that consists of sull is CrO
3Other is identical with embodiment one.
The specific embodiment three: present embodiment and the specific embodiment one are different is that the oxide general formula that consists of sull is TiO
2Other is identical with embodiment one.
Embodiment four: present embodiment and embodiment one are different is that the oxide general formula that constitutes sull is ZnO.Other is identical with embodiment one.
The specific embodiment five: present embodiment and the specific embodiment one are different is that the oxide general formula that consists of sull is Fe
2O
3Other is identical with embodiment one.
The specific embodiment six: present embodiment and the specific embodiment one are different is that the oxide general formula that consists of sull is WO
3Other is identical with embodiment one.
The specific embodiment seven: present embodiment and the specific embodiment one are different is that the oxide general formula that consists of sull is V
2O
5Other is identical with embodiment one.
The specific embodiment eight: the preparation method of room-temperature alcohol thin film gas sensor is as follows in the present embodiment: one, preparation oxide sol: with M (NO
3)
yBe dissolved in the deionized water, obtaining concentration is the M (NO of 0.01mol/L
3)
ySolution, adding concentration is the concentrated hydrochloric acid of 6mol/L, gets mixed liquor, M (NO in the mixed liquor
3)
yWith the concentration ratio of hydrochloric acid be 2~4 ﹕ 1, in 110 ℃ heating jacket, reflux then, heating mixed liquor 2~8 hours, obtain M
xO
yOxide sol, 1≤x≤2,1≤y≤5 wherein, x, y are integer; Two, with the speed immersion M of the interdigital glass substrate of gold with 20~40 mm/min
xO
yStopped in the oxide sol 2~5 minutes, and mentioned with the speed of 20~40 mm/min again, then with the interdigital glass substrate oven dry of gold; Three, the reiteration according to step 2 operates ten times; Four, the golden interdigital glass substrate that will process through step 3 sintering 1 hour in 500 ℃ Muffle furnace namely gets room-temperature alcohol thin film gas sensor.
Golden interdigital glass substrate used in the present embodiment is produced by Harbin sensitive technology research institute.
The specific embodiment nine: the preparation method of room-temperature alcohol thin film gas sensor is as follows in the present embodiment: one, preparation oxide sol: with M (NO
3)
yBe dissolved in the deionized water, obtaining concentration is the M (NO of 0.01mol/L
3)
ySolution, adding concentration is the concentrated hydrochloric acid of 6mol/L, gets mixed liquor, M (NO in the mixed liquor
3)
yWith the concentration ratio of hydrochloric acid be 2 ﹕ 1, in 110 ℃ heating jacket, reflux then, heating mixed liquor 4 hours, obtain M
xO
yOxide sol, 1≤x≤2,1≤y≤5 wherein, wherein x, y are integer; Two, with the speed immersion M of the interdigital glass substrate of gold with 30 mm/min
xO
yStopped 3 minutes in the oxide sol, mention with the speed of 30 mm/min again, then the interdigital glass substrate of gold is dried in 80 ℃ baking oven; Three, the reiteration according to step 2 operates ten times; Four, the golden interdigital glass substrate that will process through step 3 sintering 1 hour in 500 ℃ Muffle furnace namely gets room-temperature alcohol thin film gas sensor.
Embodiment ten: the preparation method of room-temperature alcohol thin film gas sensor is as follows in the present embodiment: one, preparation oxide sol: with ZnNO
3Be dissolved in the deionized water, obtain the ZnNO that concentration is 0.01mol/L
3Solution, adding concentration is the concentrated hydrochloric acid of 6mol/L, gets mixed liquor, ZnNO in the mixed liquor
3With the concentration ratio of hydrochloric acid be 2 ﹕ 1, in 110 ℃ heating jacket, reflux then, heating mixed liquor 4 hours, obtain the ZnO oxide sol; Two, with stopping 3 minutes in the speed immersion ZnO oxide sol of the interdigital glass substrate of gold with 30 mm/min, mention with the speed of 30 mm/min again, then the interdigital glass substrate of gold is dried in 80 ℃ baking oven; Three, operate ten times according to the reiteration of step 2; Four, the golden interdigital glass substrate that will handle through step 3 sintering 1 hour in 500 ℃ muffle furnace promptly gets the ZnO room-temperature alcohol thin film gas sensor.
The specific embodiment 11: the preparation method of room-temperature alcohol thin film gas sensor is as follows in the present embodiment: one, preparation oxide sol: with Ti (NO
3)
2Be dissolved in the deionized water, obtaining concentration is the Ti (NO of 0.01mol/L
3)
2Solution, adding concentration is the concentrated hydrochloric acid of 6mol/L, gets mixed liquor, Ti (NO in the mixed liquor
3)
2With the concentration ratio of hydrochloric acid be 2 ﹕ 1, in 110 ℃ heating jacket, reflux then, heating mixed liquor 4 hours, obtain TiO
2Oxide sol; Two, with the speed immersion TiO of the interdigital glass substrate of gold with 30 mm/min
2Stopped 3 minutes in the oxide sol, mention with the speed of 30 mm/min again, then the interdigital glass substrate of gold is dried in 80 ℃ baking oven; Three, the reiteration according to step 2 operates ten times; Four, the golden interdigital glass substrate that will process through step 3 sintering 1 hour in 500 ℃ Muffle furnace namely gets TiO
2Room-temperature alcohol thin film gas sensor.
The specific embodiment 12: the preparation method of room-temperature alcohol thin film gas sensor is as follows in the present embodiment: one, preparation oxide sol: with Fe (NO
3)
3Be dissolved in the deionized water, obtaining concentration is the Fe (NO of 0.01mol/L
3)
3Solution, adding concentration is the concentrated hydrochloric acid of 6mol/L, gets mixed liquor, Fe (NO in the mixed liquor
3)
3With the concentration ratio of hydrochloric acid be 2 ﹕ 1, in 110 ℃ heating jacket, reflux then, heating mixed liquor 4 hours, obtain Fe
2O
3Oxide sol; Two, with the speed immersion Fe of the interdigital glass substrate of gold with 30 mm/min
2O
3Stopped 3 minutes in the oxide sol, mention with the speed of 30 mm/min again, then the interdigital glass substrate of gold is dried in 80 ℃ baking oven; Three, the reiteration according to step 2 operates ten times; Four, the golden interdigital glass substrate that will process through step 3 sintering 1 hour in 500 ℃ Muffle furnace namely gets Fe
2O
3Room-temperature alcohol thin film gas sensor.
The sample granularity of being found out present embodiment gained room-temperature alcohol thin film gas sensor by Fig. 1 is evenly distributed, and particle is elliposoidal, and particle diameter is in 12~15nm scope.
Curve among Fig. 2 be under the present embodiment gained room-temperature alcohol thin film gas sensor room temperature when the alcohol gas of test 30ppm, the response of its sensitivity and recover indicatrix.The ratio of the room-temperature alcohol thin film gas sensor Sensitivity calculation formula definition resistance value that is room-temperature alcohol thin film gas sensor in test atmosphere and resistance value in air is defined as response time and release time the 90% needed time of change in resistance maximal value that reaches.Present embodiment gained room-temperature alcohol thin film gas sensor is 11.2 to the sensitivity of alcohol gas as can be seen from Figure 2, is respectively the response time of room-temperature alcohol thin film gas sensor and release time 20s and 48s, and the response time is shorter than corresponding release time.This diagram shows present embodiment gained room-temperature alcohol thin film gas sensor is placing after alcohols gas responds, when coming back to air ambient, rapidly convalescence regime values, show good stability.
By finding out when ethanol gas concentration is 10ppm Fe among Fig. 3
2O
3Room-temperature alcohol thin film gas sensor, ZnO room-temperature alcohol thin film gas sensor and TiO
2The sensitivity of room-temperature alcohol thin film gas sensor is respectively 5.1,2.7 and 1.9.And Fe under identical test concentrations
2O
3The sensitivity of room-temperature alcohol thin film gas sensor will be apparently higher than other room-temperature alcohol thin film gas sensors.Illustrate that room-temperature alcohol thin film gas sensor at room temperature has good sensitive property to low concentration alcohols gas.
By finding out Fe when concentration reaches 5ppm among Fig. 4
2O
3The sensitivity of room-temperature alcohol thin film gas sensor and the sensitivity difference of other sensing elements reach 5.8, illustrate that room-temperature alcohol thin film gas sensor has the ability the low concentration propyl alcohol gas in the environment is carried out selective response.Particularly the propyl alcohol gas to the 2ppm low concentration detects Fe
2O
3The sensitivity of room-temperature alcohol thin film gas sensor reaches 3.1, illustrates that this material is a kind of desirable detection low concentration alcohols gas sensitive material, and under identical test concentrations Fe
2O
3The sensitivity of room-temperature alcohol thin film gas sensor will be apparently higher than other sensing elements.
This shows that room-temperature alcohol thin film gas sensor can optionally respond alcohols gas, and can detectable concentration be the alcohols gas of 2ppm promptly at room temperature.Therefore it is well suited for as sensing element, and the alcohols gas concentration in real work and the living environment is monitored.
Claims (8)
1. room-temperature alcohol thin film gas sensor is characterized in that room-temperature alcohol thin film gas sensor is made up of the interdigital glass substrate of gold and sull, and the oxide general formula that consists of sull is M
xO
y, wherein M is Cr, Ti, Zn, Fe, W or V, 1≤x≤2,1≤y≤5 wherein, and x, y are integer.
2. room-temperature alcohol thin film gas sensor according to claim 1, the oxide general formula that it is characterized in that consisting of sull is CrO
3
3. room-temperature alcohol thin film gas sensor according to claim 1, the oxide general formula that it is characterized in that consisting of sull is TiO
2
4. room-temperature alcohol thin film gas sensor according to claim 1, the oxide general formula that it is characterized in that constituting sull is ZnO.
5. room-temperature alcohol thin film gas sensor according to claim 1, the oxide general formula that it is characterized in that consisting of sull is Fe
2O
3
6. room-temperature alcohol thin film gas sensor according to claim 1, the oxide general formula that it is characterized in that consisting of sull is WO
3
7. room-temperature alcohol thin film gas sensor according to claim 1, the oxide general formula that it is characterized in that consisting of sull is V
2O
5
8. the preparation method of the described room-temperature alcohol thin film gas sensor of claim 1 is characterized in that the preparation method of room-temperature alcohol thin film gas sensor is as follows: one, preparation oxide sol: with M (NO
3)
yBe dissolved in the deionized water, obtaining concentration is the M (NO of 0.01mol/L
3)
ySolution, adding concentration is the concentrated hydrochloric acid of 6mol/L, gets mixed liquor, M (NO in the mixed liquor
3)
yWith the concentration ratio of hydrochloric acid be 2~4 ﹕ 1, in 110 ℃ heating jacket, reflux then, heating mixed liquor 2~8 hours, obtain M
xO
yOxide sol, 1≤x≤2,1≤y≤5 wherein, x, y are integer; Two, with the speed immersion M of the interdigital glass substrate of gold with 20~40 mm/min
xO
yStopped in the oxide sol 2~5 minutes, and mentioned with the speed of 20~40 mm/min again, then with the interdigital glass substrate oven dry of gold; Three, the reiteration according to step 2 operates ten times; Four, the golden interdigital glass substrate that will process through step 3 sintering 1 hour in 500 ℃ Muffle furnace namely gets room-temperature alcohol thin film gas sensor.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103250121A (en) * | 2010-12-21 | 2013-08-14 | 日本写真印刷株式会社 | Sensor integrated with glass cover |
CN105651835A (en) * | 2014-11-12 | 2016-06-08 | 长沙理工大学 | Methanol gas sensor and preparation method thereof |
CN106744667A (en) * | 2015-11-23 | 2017-05-31 | 天津大学 | The tungsten oxide of vertical orientation/cupric oxide heterojunction nano-wire array gas sensor and its application in ethanol is detected |
CN112326735A (en) * | 2020-10-14 | 2021-02-05 | 滕州创感电子科技有限公司 | Preparation method of room-temperature semiconductor gas sensing material and sensor |
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CN101140254A (en) * | 2007-10-16 | 2008-03-12 | 上海大学 | Method for enhancing air-sensitive performance of metal oxide semiconductor material |
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CN101140254A (en) * | 2007-10-16 | 2008-03-12 | 上海大学 | Method for enhancing air-sensitive performance of metal oxide semiconductor material |
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《Sensors and Actuators B》 20071231 Guangzhong Xie et al. Gas sensing characteristics of WO3 vacuum deposited thin films 第909-914页 1-8 , 第123期 * |
《功能材料》 20051231 李莉等 V2O5薄膜在传感器上的研究进展 第1482页 2 V2O5薄膜在气体传感器上的研究进展 3,5-7 第36卷, 第10期 * |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103250121A (en) * | 2010-12-21 | 2013-08-14 | 日本写真印刷株式会社 | Sensor integrated with glass cover |
CN103250121B (en) * | 2010-12-21 | 2014-09-17 | 日本写真印刷株式会社 | Sensor integrated with glass cover |
CN105651835A (en) * | 2014-11-12 | 2016-06-08 | 长沙理工大学 | Methanol gas sensor and preparation method thereof |
CN106744667A (en) * | 2015-11-23 | 2017-05-31 | 天津大学 | The tungsten oxide of vertical orientation/cupric oxide heterojunction nano-wire array gas sensor and its application in ethanol is detected |
CN112326735A (en) * | 2020-10-14 | 2021-02-05 | 滕州创感电子科技有限公司 | Preparation method of room-temperature semiconductor gas sensing material and sensor |
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