CN1015936B - Fabrication of zinc metastannate (or zinc stannate) gas-sensitive devices - Google Patents
Fabrication of zinc metastannate (or zinc stannate) gas-sensitive devicesInfo
- Publication number
- CN1015936B CN1015936B CN86106681.2A CN86106681A CN1015936B CN 1015936 B CN1015936 B CN 1015936B CN 86106681 A CN86106681 A CN 86106681A CN 1015936 B CN1015936 B CN 1015936B
- Authority
- CN
- China
- Prior art keywords
- gas
- zinc
- type
- semiconductor
- sensitive
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 239000011701 zinc Substances 0.000 title claims description 12
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims description 4
- 229910052725 zinc Inorganic materials 0.000 title claims description 4
- 238000004519 manufacturing process Methods 0.000 title description 11
- BNEMLSQAJOPTGK-UHFFFAOYSA-N zinc;dioxido(oxo)tin Chemical compound [Zn+2].[O-][Sn]([O-])=O BNEMLSQAJOPTGK-UHFFFAOYSA-N 0.000 title description 2
- 239000004065 semiconductor Substances 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims description 13
- 229910018626 Al(OH) Inorganic materials 0.000 claims description 4
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 229910052573 porcelain Inorganic materials 0.000 claims 1
- 239000010935 stainless steel Substances 0.000 claims 1
- 239000007789 gas Substances 0.000 abstract description 59
- 238000005516 engineering process Methods 0.000 abstract description 12
- 238000001514 detection method Methods 0.000 abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 9
- 239000001257 hydrogen Substances 0.000 abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 8
- 229910001868 water Inorganic materials 0.000 abstract description 8
- 239000003915 liquefied petroleum gas Substances 0.000 abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 3
- 238000000227 grinding Methods 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 abstract description 3
- 239000000945 filler Substances 0.000 abstract description 2
- 238000007650 screen-printing Methods 0.000 abstract description 2
- 238000007738 vacuum evaporation Methods 0.000 abstract description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 2
- 229910007694 ZnSnO3 Inorganic materials 0.000 abstract 1
- 239000000853 adhesive Substances 0.000 abstract 1
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- 239000010408 film Substances 0.000 abstract 1
- 238000010422 painting Methods 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 238000004544 sputter deposition Methods 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 239000010409 thin film Substances 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 229910007717 ZnSnO Inorganic materials 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 5
- 150000002431 hydrogen Chemical class 0.000 description 5
- 230000035945 sensitivity Effects 0.000 description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 230000018109 developmental process Effects 0.000 description 4
- 239000002360 explosive Substances 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 208000005156 Dehydration Diseases 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910006404 SnO 2 Inorganic materials 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- NSEQHAPSDIEVCD-UHFFFAOYSA-N N.[Zn+2] Chemical compound N.[Zn+2] NSEQHAPSDIEVCD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 239000002800 charge carrier Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010291 electrical method Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000002737 fuel gas Substances 0.000 description 1
- 239000003502 gasoline Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- -1 oxonium ion Chemical class 0.000 description 1
- KYKLWYKWCAYAJY-UHFFFAOYSA-N oxotin;zinc Chemical compound [Zn].[Sn]=O KYKLWYKWCAYAJY-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000012113 quantitative test Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
Images
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- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The present invention uses ZnSnO3 or Zn2Sn4 as a filling agent or an adhesive agent by adding certain SiO2 and Al (OH) 3. Semiconductor gas sensing elements of a directly-heated type, an indirectly-heated type, etc. can be fabricated through the technologies of grinding, painting, sintering, etc. A semiconductor gas sensing element of a thick film type or a thin film type can also be fabricated by a screen printing technology, a vacuum evaporation technology and a sputtering technology. Indicated by testing, the gas sensing elements fabricated by the materials and technologies are sensitive to gas, such as hydrogen, water gas, etc., and have higher stability and selectivity, and the gas sensing elements can be used for the detection and the alarm of hydrogen, water gas, liquefied petroleum gas, etc.
Description
The invention belongs to gas detection device technical field.
Human comings and goings all is to carry out in the environment of atmosphere, produces and the also too busy to get away certain atmosphere of life activity.The situation of atmosphere has tremendous influence for human existence.
Along with science and technology development, industrial kind and scale enlarge gradually, and gaseous species that produces in gas raw material of Shi Yonging and the production run and quantity are also increasing aborning.It much is inflammable and explosive having in these gases.They leak in the air not only contaminated environment seriously, but also might cause fire and explosion accident, give to produce and life security is brought danger.In addition, because the development and the growth in the living standard of producing, liquefied petroleum gas (LPG), town gas and rock gas etc. are popularized rapidly as family's fuel, because of blast and fire failure that the leakage of these inflammable gass causes also increasing.Therefore, in order to guarantee safety in production and life, prevent the generation of the various accidents that cause thus, what help producing and living normally carries out, various inflammable and explosive property gases are detected, in time take preventive measures, become one of important process in the gas detection.
The gas detection method of present existing practicality mainly contains electrochemical method; Light source method (comprising luminous); Several different methods such as electrical method.Utilizing the semiconductor gas sensing device to come the method for detected gas, is a kind of method of electrical detection gas.Aspect the inflammable and explosive property gas of detection, the semiconductor gas sensing device has easy to use, low price, highly sensitive, advantages such as good reliability.Therefore, be one of better method of detecting inflammable and explosive property gas.
Electronics industry science and technology committee sensitive element consulting group: " sensitive element special edition ", (1983); Clear, the little long well of high bridge is sincere: " セ Application サ I レ Network ト ロ ニ Network ス ", documents such as (1984, clear rolling hall) shows that semiconductor gas sensor zinc oxide films membrane module the earliest is to succeed in developing at the initial stage in the sixties.It is to utilize under heating condition, and the zinc oxide films film resistance descends with the increase of the concentration of the inflammable gas of contact, thereby realizes N
2The detection of O and CO gas.Develop SnO later on again
2Series, r-Fe
2O
3Gas sensors such as series.Semiconductor gas sensor is divided into resistor-type and non-resistor-type, and resistor-type generally is to measure tested gas with its resistance value with the variation of gas concentration, and device architecture mostly is porous sintered article.Non-resistor-type is to utilize gas absorption to influence semi-conductive work function to change and come detected gas.Existing SnO commonly used
2, r-Fe
2O
3The type gas sensor, general fabrication cycle is longer, needs to add noble metals such as pt, pd and makes catalyzer, and constant temperature time needs several hours and even tens hours.
Because semiconductor gas sensor has highly sensitive characteristics such as of many uses.Therefore obtained development rapidly in recent decades.Further carrying out the research of many kinds semiconductor air-sensitive new material and element thereof, is one of the important topic in current semiconductor gas sensor gas detection technology field.
In order to seek new semiconductor air-sensitive material and the element made from this material thereof, reduce and use price, enlarge measurement range, promote the development of China's semiconductor air-sensitive material and device research.Department of physics of Yunnan University has succeeded in developing and has used ZnSnO
3Make gas sensor.Primary Study shows that it does not resemble SnO commonly used now
2, r-Fe
2O
3The type gas sensor need add noble metals such as pt, pd when making and make catalyzer, only needs to add low-cost SiO
2, Al(OH)
3As filling agent and bonding agent; Manufacture craft is simple, and constant temperature time is short, can shorten fabrication cycle, saves the energy and manpower; Can be made into directly-heated type, multiple structures such as heater-type, film, thick film; The heating-up temperature of control element can obtain the susceptibility of gas with various.After tested and analyze, all responsive to gases such as hydrogen, carbon monoxide, water gas.By selected prescription with improve manufacturing process, also can make it have higher selectivity and stability, can be used for liquefied petroleum gas (LPG), household fuel gas, etc. detection and warning.
The present invention is through the World Patent Index 74-86.16 phase, " chemical abstracts " 74-86(104,1-8 volume), Chinese thematic information retrieval in 86 years shows, finds manufacture craft and the element identical with the present invention as yet.
Material technology of the present invention is that the employing chemical preparation process is the synthetic ZnSnO of wet method
3Concrete grammar be with zinc salt and pink salt as base stock, at first make zinc ammonium complex ion Zn(NH
3)
4, the hydrate Zn (Sn(OH) of synthetic again zinc tin oxide), through the calcination dehydration, then can be made into ZnSnO
3The implementation step of object lesson is:
Get a certain amount of ZnSO
4Solution, the certain density ammoniacal liquor of agitation and dropping under the room temperature generates white precipitate, continues dropping ammonia, clarifies until solution.Its reaction is
In above-mentioned solution, add equimolar SnCl
4Solution stirs above-mentioned solution at a certain temperature, generates white precipitate Zn (Sn(OH) immediately
6) ↓.Its reaction can be shown:
Gained solution is filtered washing, the white precipitate Zn (Sn(OH) that obtains
6) put into platinum crucible, to 400 degree calcination dehydrations, then can be made into ZnSnO at 380 degree Celsius
3Its reaction is:
When being heated to 800 degree Celsius during the left and right sides, can obtain Zn
2SnO
4
Ultimate principle of the present invention is ZnSnO
3The semiconductor sensitive material is a kind of senior high-frequency insulation material, is heated to Celsius approximately 800 when spending in high temperature, ZnSnO
3Can resolve into Zn
2SnO
4And SnO
2, form three's composite material.Because SnO
2, Zn
2SnO
4It also all is the semiconductor sensitive material, oxonium ion in these material lattice, acid ion take place vacant, and it is less and when losing the gas molecule in electronics or hole easily, carrier concentration increases to run into dissociation energy, resistance reduces, thereby responsive especially to gases such as hydrogen, water gas.It is generally acknowledged that because the semiconductor surface adsorption gas molecule is filled the omission in the lattice, discharge electronics or hole, charge carrier increases in the crystal thereby make, resistivity decreased.When gas molecule was overflowed, resistivity was recovered initial value again.So just can connect the content of change in resistance and test gas by a simple test circuit.By quantitative test, just can measure the gas of variable concentrations.
Element manufacture craft of the present invention is to adopt directly-heated type, heater-type, thick-film type structure and sintering process.With the directly-heated type structure is that the manufacture craft of example is earlier at ZnSnO
3Add SiO in the material
2, Al(OH)
3Acid-washed asbestos is through grinding, sintering, add technology such as welded tube seat and make element.
Concrete technology is to press ZnSnO
390～95%, SiO
22～5%, Al(OH)
3The material that 2～5% prescription weighs up grinds alms bowl with bowl mill or agate and grinds, and is thin more good more.The electrode diameter is 0.04～0.09 millimeter, and resistance is that 4～20 ohm platinum wire is made, the coiling tubulose, and about about 10 circles, spiral pipe is about 1 millimeter.
With ground matrix material, the furnishing starchiness is coated in the good and sound electrode die, thereby wants all topped firmly helix electrode to make tube core.
Tube core with coating after air dry, is placed on the special carriage, puts sintering in the sintering furnace into.The condition of sintering is: heat to 500～800 degree Celsius, constant temperature 5～30 minutes (heating rate be 1-4 degree Celsius/minute) is cooled to room temperature rapidly behind the constant temperature.
With the energising heating tube core behind the sintering is worn out then; Tube core is welded on the base, puts into special-purpose agingtable energising and wear out.Time is more than 100 hours, so that improve the performance of device, increases stability, makes pottery and eliminates unacceptable product.
Device after aging is carried out the measurement of parameters,, seal, check after tested, qualified packing warehouse-in with 100 order double-layer stainless steels with qualified tube core.
Directly-heated type structure and heater-type structural detail sintering process flow process are as follows:
Weighing → grinding → coating → add electrode → sintering → welded tube seat → preliminary survey.
With above-mentioned directly-heated type or heater-type structure sintering process, utilize screen printing technique, heating material adopts RuO, and electrode material adopts Au, can be made into the thick-film type element.
Also can be made into the film-type element with vacuum evaporation or the low-priced technology of penetrating.
Fig. 1 is ZnSnO
3The gas sensor resistance value is with the variation of all gases concentration.As seen from the figure, when the concentration of hydrogen was increased to 1000PPm gradually, its resistance can change to several kilo-ohms by last megaohm, and its variation range is that hundred times arrives nearly thousand times.As seen its sensitivity is very high, and water gas can reach nearly a hundred times.Though also responsive to methane, its variation only is about twice.
In addition, measure and to show that also the response time of this kind element and release time are also fast.
Utilize ZnSnO
3The semiconductor gas sensor of making has following characteristic: the working temperature of element is 100～350 degree Celsius.Show that after tested inflammable gass such as hydrogen, carbon monoxide, water gas, oil liquefied gas, alkanes gas, gasoline, acetone, alcohol are had sensitivity in various degree, but especially with the most responsive to hydrogen.With regard to hydrogen, methane, water gas, oil liquefied gas, heating power is 1 watt-hour, sensitivity β 0.5=(R
A)/(R
0.5) be respectively 150～350,1.5～2.5,35～45,10～12.R wherein
ABe the resistance of sample in the clean air, R
0.5Resistance when containing percent 0.5 tested gases in the air.With regard to the SnO that surpasses far away with regard to the sensitivity of hydrogen
2Series of elements and Fe
2O
3Series of elements, with regard to regard to water gas also than other two class components sensitivity.
Utilize Zn
2SnO
4, adopt similar above-mentioned prescription also to can be made into the gas sensor of similar said structure and characteristic.
Claims (3)
1, a kind of semiconductor gas sensor, make by sintering process, its structure can be directly-heated type or heater-type (containing thick-film type), comprise electrode, sensitive material, base, the stainless steel guard, heater-type also comprises porcelain body, and the main body that it is characterized in that described gas sensitive is a zinc metastannate, and an amount of in addition SiO
2And Al (OH)
3
2, gas sensor according to claim 1 is characterized in that consisting of of described gas sensitive:
100 parts of zinc metastannates
SiO
22～5 parts
Al(OH)
32～5 parts
3, gas sensor according to claim 1 and 2, the sintering range that it is characterized in that described element is 500～800 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN86106681.2A CN1015936B (en) | 1986-10-09 | 1986-10-09 | Fabrication of zinc metastannate (or zinc stannate) gas-sensitive devices |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN86106681.2A CN1015936B (en) | 1986-10-09 | 1986-10-09 | Fabrication of zinc metastannate (or zinc stannate) gas-sensitive devices |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN86106681A CN86106681A (en) | 1987-10-21 |
| CN1015936B true CN1015936B (en) | 1992-03-18 |
Family
ID=4803319
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN86106681.2A Expired CN1015936B (en) | 1986-10-09 | 1986-10-09 | Fabrication of zinc metastannate (or zinc stannate) gas-sensitive devices |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1015936B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100360423C (en) * | 2006-01-09 | 2008-01-09 | 浙江理工大学 | Process for synthesizing spinel zine stannate nano rod |
| CN101251508B (en) * | 2008-04-01 | 2011-06-22 | 重庆大学 | Method for manufacturing gas sensor for testing hydrogen |
| CN109187662A (en) * | 2018-08-31 | 2019-01-11 | 天津大学 | Work in the metal oxide base ethyl alcohol gas sensor preparation method of room temperature |
| CN108709915B (en) * | 2018-09-01 | 2021-11-19 | 山东多瑞电子科技有限公司 | Harmful gas detection device in car |
| CN110108758B (en) * | 2019-05-13 | 2022-05-24 | 上海理工大学 | Formaldehyde sensitive material, sensitive element and preparation method thereof |
| CN116380997B (en) * | 2023-05-26 | 2023-08-15 | 深圳市道合顺传感实业有限公司 | Gas-sensitive material, preparation method and application thereof |
-
1986
- 1986-10-09 CN CN86106681.2A patent/CN1015936B/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| CN86106681A (en) | 1987-10-21 |
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