CN100401548C - Method for making ferric oxide/stannic oxide bilaminar membrane alcohol sensitive element - Google Patents
Method for making ferric oxide/stannic oxide bilaminar membrane alcohol sensitive element Download PDFInfo
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- CN100401548C CN100401548C CNB2003101092708A CN200310109270A CN100401548C CN 100401548 C CN100401548 C CN 100401548C CN B2003101092708 A CNB2003101092708 A CN B2003101092708A CN 200310109270 A CN200310109270 A CN 200310109270A CN 100401548 C CN100401548 C CN 100401548C
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- iron oxide
- tin ash
- tin
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Abstract
The present invention relates to a method for manufacturing an alcohol sensing element with an iron oxide/tin dioxide double-layer thin film, which belongs to the technical field of the manufacturing technology of semiconductor sensors and sensing elements. In the present invention, a sol-gel technology is mainly adopted. The present invention is characterized in that firstly, a tin dioxide layer is dipped and coated on an aluminium oxide substrate; then, an iron oxide layer is prepared on the surface of the tin dioxide layer. An alcohol sensing element with an iron oxide/tin dioxide double-layer thin film is formed by heat treatment. The alcohol sensing element with an iron oxide / tin dioxide double-layer thin film, which is prepared by the method of the present invention has the advantages of high stability performance, high sensitivity, simple technology and low cost. The present invention can be used for detecting whether drivers drink wine excessively, and the problem of driving a car after drinking can be controlled.
Description
Technical field
The present invention relates to the manufacture method of a kind of iron oxide/tin ash bilayer film ethanol sensor, belong to semiconductor transducer and senser manufacturing process technology field.
Background technology
Semiconductor gas sensor is meant semi-conducting material is added the gas sensor that top electrode and heating resistor are prepared from.Because the variation of environmental gas composition causes the electrical property of semiconductor gas sensor and changes the kind and the concentration of the gas that exists in the testing environment by the resistance of measuring semiconductor gas sensor.
As everyone knows, whether ethanol sensor can be used to detect the driver excessive consumption of alcohol, can control and driving a car under the influence of alcohol.Present ethanol sensor signal drift is bigger, and poor stability is difficult to guarantee monitoring accuracy when using for a long time.
Summary of the invention
The purpose of this invention is to provide a kind of high stability iron oxide/tin ash bilayer film ethanol sensor and manufacture method thereof.
The manufacture method of a kind of iron oxide of the present invention/tin ash bilayer film ethanol sensor mainly adopts sol-gel technology, it is characterized in that it includes following each processing step:
A. at first prepare base-material tin ash colloidal sol, butter of tin is dissolved in forms solution in the ethanol, reflux 4-6 hour, in 60 ℃ of-80 ℃ of water-baths, wore out 24 hours then, obtain tin ash colloidal sol;
B. the alumina substrate with set gold electrode and ruthenium oxide resistance zone of heating immerses in the above-mentioned tin ash colloidal sol, takes out after 10 minutes, and dries under 110 ℃ of temperature;
C. repeat the immersion-drying course among above-mentioned steps b 10-20 time is obtained the tin ash sol pellicle;
D. then this sol pellicle was handled 1 hour down at 500 ℃-550 ℃, can be made this sol pellicle be converted into the tin ash gel film, its thickness is the 300-800 nanometer;
E. then prepare the iron oxide base-material, ferric trichloride is dissolved in forms solution in the ethanol, reflux 6-8 hour, in 60 ℃ of-80 ℃ of water-baths, wore out 24 hours then, get iron oxide colloidal sol;
F. the alumina substrate with the above-mentioned tin ash gel film that has prepared immerses in the iron oxide colloidal sol again, takes out after 10 minutes, and dries under 110 ℃ of temperature;
G. repeat immersion-drying course 10-20 time among the above-mentioned steps f, handled 1 hour down at 500 ℃-550 ℃ then, can get the gel sull, its thickness is the 300-800 nanometer;
H. last with the above-mentioned iron oxide that obtains/tin ash bilayer film 700 ℃ of following heat treatments 30 minutes, make bilayer film go out one deck iron tin composite oxides transition zone to interface growth, finally make iron oxide/tin ash bilayer film ethanol sensor.
The above-mentioned set gold electrode and the alumina substrate of ruthenium oxide resistance zone of heating, its preparation method is: respectively draw a horizontal line with gold paste at the two ends of the front and back of substrate earlier being of a size of on the alumina substrate of 3 * 5mm, have four, 950 ℃ of sintering temperatures 10 minutes, form four gold electrodes; Ruthenium-oxide slurry in substrate back printing 600 ℃ of sintering temperatures 30 minutes, forms the ruthenium oxide resistance zone of heating, get final product the alumina substrate crossed through processed.
Among the present invention, the transition zone at iron oxide/tin ash bilayer film and interface is a key technology of the present invention.The existence of transition zone is that iron oxide/tin ash bilayer film has the reason of high stability.
Iron oxide/tin ash bilayer film the ethanol sensor of the inventive method preparation have higher stable performance and sensitivity, and technology is easy, and is with low cost.The semiconductor transducer gas sensor of detection ethanol of the present invention, whether have excessive consumption of alcohol, can control the problem of drivining a car under the influence of alcohol if can be used for detecting the driver.
Description of drawings
Fig. 1 is iron oxide of the present invention/tin ash bilayer film ethanol sensor structural representation.
Fig. 2 is the stability curve of iron oxide/tin ash bilayer film ethanol sensor.
In the above-mentioned accompanying drawing 1, the meaning that each code name is represented is as follows:
1-oxidation nail zone of heating 2-alumina substrate 3-gold electrode 4-iron oxide layer 5-iron tin-oxide transition zone 6-tin ash layer
Embodiment
Now in conjunction with the accompanying drawings and embodiments the present invention further is described in the back:
Embodiment one: adopt sol-gel technology to prepare the tin ash base-material earlier.Butter of tin is dissolved in forms solution in the ethanol, reflux 4 hours in 60 ℃ of water-baths aging 24 hours then, obtains tin ash colloidal sol.Alumina substrate with preprocessed gold and ruthenium oxide resistance zone of heating immerses in the tin ash colloidal sol then, takes out after 10 minutes, and dries under 110 ℃ of temperature.Repeat to immerse---the process of oven dry 10 times, 500 ℃ of following heat treatments 1 hour, make colloidal sol be converted into gel then, its thickness is the 300-400 nanometer.
Then adopt same sol-gel technology to prepare the iron oxide base-material, ferric trichloride is dissolved in forms solution in the ethanol, refluxed 6 hours, in 60 ℃ of water-baths, wore out 24 hours then, obtain iron oxide colloidal sol.The above-mentioned alumina substrate for preparing the tin ash layer is immersed in the iron oxide colloidal sol, take out after 10 minutes, and under 110 ℃ of temperature, dry.Repeat to immerse---the process of oven dry 10 times, then 500 ℃ of following heat treatments 1 hour.Can get the gel iron oxide layer, its thickness is the 300-400 nanometer.700 ℃ of following heat treatments 30 minutes, make the bilayer film interface growth go out one deck iron tin composite oxides transition zone the above-mentioned iron oxide that obtains/tin ash bilayer film.Finally obtain high stability iron oxide/tin ash bilayer film ethanol sensor.
The alumina substrate of resistance heating layer is treated in described set gold electrode and oxidation, its preparation method is: respectively draw a horizontal line with gold paste at the two ends of the front and back of end liner earlier being of a size of on the alumina substrate of 3 * 5mm, have four, 950 ℃ of sintering temperatures 10 minutes, form four gold electrodes; Oxidation nail slurry in substrate back printing 600 ℃ of sintering temperatures 30 minutes, forms oxidation nail resistance heating layer, can obtain the alumina substrate of crossing through processed.
The iron oxide of the detection ethanol that finally makes/tin ash bilayer film sensitive element structure as shown in Figure 1.
Embodiment two: present embodiment and the foregoing description are identical, just some technological parameter difference: butter of tin is dissolved in forms solution in the ethanol earlier, reflux 6 hours wore out 24 hours in 80 ℃ of water-baths then, obtained tin ash colloidal sol.The alumina substrate of preprocessed gold and oxidation nail resistance heating layer is immersed in the tin ash colloidal sol, take out after 10 minutes, and under 110 ℃ of temperature, dry.Repeat to immerse---the process of oven dry 20 times, 550 ℃ of following heat treatments 1 hour, make colloidal sol be converted into gel then, its thickness is the 700-800 nanometer.
Then adopt same sol-gel technology to prepare the iron oxide base-material, ferric trichloride is dissolved in forms solution in the ethanol, refluxed 8 hours, in 80 ℃ of water-baths, wore out 24 hours then, obtain iron oxide colloidal sol.The above-mentioned alumina substrate for preparing the tin ash layer is immersed in the iron oxide colloidal sol, take out after 10 minutes, and under 110 ℃ of temperature, dry.Repeat to immerse---the process of oven dry 20 times, then 550 ℃ of following heat treatments 1 hour.Can get the gel iron oxide layer, its thickness is the 700-800 nanometer.700 ℃ of following heat treatments 30 minutes, make the bilayer film interface growth go out one deck iron tin composite oxides transition zone the above-mentioned iron oxide that obtains/tin ash bilayer film.Finally obtain high stability iron oxide/tin ash bilayer film ethanol sensor.
Above-mentioned set gold electrode is identical with embodiment one with the preparation method of the alumina substrate of oxidation nail resistance heating layer.
About the sample of embodiment one and embodiment two, i.e. the stability of iron oxide/tin ash bilayer film ethanol sensor, the stability curve of Fig. 2 in the visible accompanying drawing, this stability curve has shown stably and advantages of higher stability.
This semiconductor transducer gas sensor of the present invention is when reality is used, when promptly in containing the ethanol environment, detecting, because variation has taken place the electrical property of the iron oxide/tin ash bilayer film sensitive layer on the gas sensor, therefore just can learn the concentration of alcohol gas in the environment by the measuring resistance size.Also essential in when work by the gold electrode input direct voltage, oxidation nail resistance heating layer is under 200 ℃ the working temperature, make the transducer can operate as normal.
Claims (2)
1. the manufacture method of iron oxide/tin ash bilayer film ethanol sensor mainly adopts sol-gel technology, it is characterized in that it includes following each processing step:
A. at first prepare base-material tin ash colloidal sol, butter of tin is dissolved in forms solution in the ethanol, reflux 4-6 hour, in 60 ℃ of-80 ℃ of water-baths, wore out 24 hours then, obtain tin ash colloidal sol;
B. the alumina substrate with preprocessed gold and ruthenium oxide resistance zone of heating immerses in the above-mentioned tin ash colloidal sol, takes out after 10 minutes, and dries under 110 ℃ of temperature;
C. repeat immersion-drying course 10-20 time among the above-mentioned steps b, obtain the tin ash sol pellicle;
D. then this sol pellicle was handled 1 hour down at 500 ℃-550 ℃, can be made this sol pellicle be converted into the tin ash gel film, its thickness is the 300-800 nanometer;
E. then prepare base-material iron oxide colloidal sol, ferric trichloride is dissolved in forms solution in the ethanol, reflux 6-8 hour, in 60 ℃ of-80 ℃ of water-baths, wore out 24 hours then, get iron oxide colloidal sol;
F. the alumina substrate with the above-mentioned tin ash gel film that has prepared immerses in the iron oxide colloidal sol again, takes out after 10 minutes, and dries under 110 ℃ of temperature;
G. repeat immersion-drying course 10-20 time among the above-mentioned steps f, handled 1 hour down at 500 ℃-550 ℃ then, can get the gel sull, its thickness is the 300-800 nanometer;
H. last with the above-mentioned iron oxide that obtains/tin ash bilayer film 700 ℃ of following heat treatments 30 minutes, make the bilayer film interface growth go out one deck iron tin composite oxides transition zone, finally make iron oxide/tin ash bilayer film ethanol sensor.
2. the manufacture method of a kind of iron oxide according to claim 1/tin ash bilayer film ethanol sensor, it is characterized in that, the alumina substrate of described set gold electrode and ruthenium oxide resistance zone of heating, its preparation method is: respectively draw a horizontal line with gold paste at the two ends of the front and back of substrate earlier being of a size of on the alumina substrate of 3 * 5mm, have four, 950 ℃ of sintering temperatures 10 minutes, form four gold electrodes; Ruthenium-oxide slurry in substrate back printing 600 ℃ of sintering temperatures 30 minutes, forms the ruthenium oxide resistance zone of heating, get final product the alumina substrate crossed through processed.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2003101092708A CN100401548C (en) | 2003-12-11 | 2003-12-11 | Method for making ferric oxide/stannic oxide bilaminar membrane alcohol sensitive element |
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| CNB2003101092708A CN100401548C (en) | 2003-12-11 | 2003-12-11 | Method for making ferric oxide/stannic oxide bilaminar membrane alcohol sensitive element |
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| CN100401548C true CN100401548C (en) | 2008-07-09 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101201333B (en) * | 2006-04-21 | 2010-08-25 | 湖南大学 | Method for preparing ITO nanometer line and gas sensor thereof |
| CN100465635C (en) * | 2006-12-21 | 2009-03-04 | 广州大学 | Coating type ammonia sensor nano film and method for preparing same |
| CN101182188B (en) * | 2007-11-23 | 2010-08-11 | 福州大学 | Method for preparing nano-grade rutile phase RuO2-SnO2 oxide |
| CN104977320B (en) * | 2015-06-03 | 2017-11-14 | 安徽兰兮工程技术开发有限公司 | A kind of ceramic gas sensor for alcohol detection |
| CN105866189A (en) * | 2016-04-12 | 2016-08-17 | 吉林大学 | Cobalt doped tin dioxide semiconductor ethanol sensor, and making method and application thereof |
| CN108802112B (en) * | 2018-04-02 | 2020-12-15 | 中国科学院合肥物质科学研究院 | Platinum particle modified tin oxide-iron oxide nano composite particle and preparation method and application thereof |
| CN113088873B (en) * | 2021-03-15 | 2021-12-21 | 中南大学 | Ethanol steam and gap sensitive element and development method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1007193B (en) * | 1988-01-18 | 1990-03-14 | 中国科学院长春应用化学研究所 | Sensing element for combustible gas |
| CN1012016B (en) * | 1989-07-29 | 1991-03-13 | 吉林大学 | Double sensitive film air sensor for both gases of alcohol nitrogen dioxide |
| WO2003042681A1 (en) * | 2001-11-14 | 2003-05-22 | Matsushita Electric Industrial Co., Ltd. | Gas sensor, and production method for gas sensor |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1007193B (en) * | 1988-01-18 | 1990-03-14 | 中国科学院长春应用化学研究所 | Sensing element for combustible gas |
| CN1012016B (en) * | 1989-07-29 | 1991-03-13 | 吉林大学 | Double sensitive film air sensor for both gases of alcohol nitrogen dioxide |
| WO2003042681A1 (en) * | 2001-11-14 | 2003-05-22 | Matsushita Electric Industrial Co., Ltd. | Gas sensor, and production method for gas sensor |
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