CN102661979B - Method for preparing comb-like nanostructure zinc oxide gas sensitive sensor - Google Patents
Method for preparing comb-like nanostructure zinc oxide gas sensitive sensor Download PDFInfo
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- CN102661979B CN102661979B CN2012101241330A CN201210124133A CN102661979B CN 102661979 B CN102661979 B CN 102661979B CN 2012101241330 A CN2012101241330 A CN 2012101241330A CN 201210124133 A CN201210124133 A CN 201210124133A CN 102661979 B CN102661979 B CN 102661979B
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- zinc oxide
- gas sensor
- pectination
- quartzy
- gas
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 14
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 10
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910002091 carbon monoxide Inorganic materials 0.000 claims abstract description 19
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 7
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052737 gold Inorganic materials 0.000 claims abstract description 4
- 239000010931 gold Substances 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 67
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 30
- 229910052757 nitrogen Inorganic materials 0.000 claims description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 12
- 239000001301 oxygen Substances 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 12
- 239000003708 ampul Substances 0.000 claims description 9
- 238000005259 measurement Methods 0.000 claims description 9
- 239000010453 quartz Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 238000009434 installation Methods 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000011521 glass Substances 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- 239000000758 substrate Substances 0.000 claims description 7
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 238000001507 sample dispersion Methods 0.000 claims description 3
- 238000001338 self-assembly Methods 0.000 claims description 3
- 238000013022 venting Methods 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 230000035945 sensitivity Effects 0.000 abstract description 7
- 239000004065 semiconductor Substances 0.000 abstract description 6
- 239000013078 crystal Substances 0.000 abstract description 4
- 238000012858 packaging process Methods 0.000 abstract description 2
- 238000004806 packaging method and process Methods 0.000 abstract 1
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical compound [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 6
- 244000126211 Hericium coralloides Species 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002121 nanofiber Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000567 combustion gas Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
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Abstract
The invention belongs to the technical field of one-dimensional nanostructure semiconductor oxide gas sensitive sensor preparation and relates to a method for preparing a comb-like nanostructure zinc oxide gas sensitive sensor capable of detecting carbon monoxide under the condition of room temperature by utilizing a chemical vapor deposition method. The method for preparing the comb-like nanostructure zinc oxide gas sensitive sensor comprises the following steps of: firstly, selecting the growth condition of a crystal as needed; preparing comb-like nanostructure zinc oxide by utilizing the improved chemical vapor deposition method; then, dispersing the comb-like nanostructure zinc oxide to a gold cell array; connecting two adjacent cells in which the zinc oxide exists by using microelectrodes; and packaging in a shell by adopting a conventional semiconductor packaging process to prepare the zinc oxide gas sensitive sensor. The sensor works at normal temperature and is simple in structure, is low in power consumption, simple in preparation process and low in cost. The growing zinc oxide crystal is high in purity and good in completeness; the surface area of a gas contact reaction is big; the contact resistance is low; actions of gathering and conducting current are performed by the zinc oxide at the combed parts; and the sensor is high in sensitivity.
Description
Technical field:
The invention belongs to one-dimensional nano structure conductor oxidate gas sensor preparing technical field, relate to a kind of method of utilizing the chemical gaseous phase depositing process preparation can detect at ambient temperature the pectination nanostructured zinc oxide gas sensor of carbon monoxide.
Background technology:
Gas sensor is a kind of senser element that detects specific gas, for example combustion gas leaks and the event of anthracemia happens occasionally in using the carbon monoxide process, usually, the adult stays in the environment of content 400ppm carbon monoxide, toxicity symptom in 2 hours is front metopodynia, will be in peril of one's life after 3 hours; So the detection to the qualitative or quantitative detection of inflammable gas and poisonous gas, monitoring, warning is essential.Present numerous Oxide Gas Sensors used, working temperature, usually at 200-400 ℃, need to arrange heating element, causes its complicated structure and power consumption larger.For example, Chinese patent (application number 200810116300.0) has been put down in writing a kind of WO
3Gas sensor, and provided under 300 ℃ and 350 ℃ response curve to CO gas.ZnO is a kind of multi-function metal oxide semiconductor material, has good physical and chemical stability, is one of research and application gas sensitive the earliest, has just successfully developed the ZnO semiconductor gas sensor in 1962 as Seiyama; The research of the gas sensor of relevant ZnO is mainly the gas-sensitive property of ZnO pottery, thick film, film, form of nanofibers.In order to improve the performance of ZnO gas sensor, the way that adopts at present is a lot, such as by the ZnO semiconductor is adulterated (unit of doping have Co, Cu, Pd, Sn etc.), thereby regulate Fermi surface position, promote the absorption of molecule on surface, perhaps change the microscopic appearance structure of ZnO, increase specific surface area.Adopt the pectination Nano ZnO gas sensitive of chemical vapour deposition technique preparation, compare with traditional ZnO material have larger specific surface area, larger surfactivity and stronger adsorptive power, can accelerate and gas reaction, its gas sensor of making can improve sensitivity and the response speed of gas sensor, can at room temperature carry out work, do not need heating element, but the technology of preparing of this material also not yet has disclosed more perfect overall technical architecture at present, and inquire into and this technical scheme is provided, will be main task of the present invention.
Summary of the invention:
the object of the invention is to overcome the shortcomings such as gas sensor working temperature height that prior art exists, seek to provide a kind of method for preparing carbon monoxide transducer, when having a certain amount of carbon monoxide toxic gas in environment, this sensor can detect at normal temperatures and the variation by current signal responds fast, gas sensor with the making of zinc paste pectination nanostructured fibers, grow regularly arranged branch on the vertical direction of single nanofiber, pattern is similar to comb tooth, increase the contact area of test gas and zinc paste, improve sensitivity and the response time of sensor.
To achieve these goals, the present invention first selects the growth conditions of crystal as required, utilizes modified chemical vapor deposition process (MCVD) to prepare the pectination nanostructured zinc oxide; Again the pectination nanostructured zinc oxide is distributed on golden array of cells, the two adjacent cells that have zinc paste are connected with microelectrode, adopt conventional semiconductor packaging process encapsulation in the enclosure, prepare the zinc paste gas sensor; Its concrete steps comprise:
(1) prepare the pectination nanostructured zinc oxide with modified chemical vapor deposition process (MCVD): first quartzy bottle is lain in a horizontal plane in the horizontal quartz ampoule in quick anneal oven, quartzy bottleneck towards identical with airflow direction, put into the zinc powder of purity 99.9% on the position at the quartzy bottle end; Area load has the silicon chip of gold nano grain or glass sheet to be placed on quartzy bottleneck; Produce the environment of rich zinc in quartzy bottle, the oxygen that enters with quartzy bottleneck, at quartzy bottleneck generation chemical reaction, grows ZnO nano-structure on the substrate of silicon chip or glass sheet; Again quartz ampoule is evacuated to 10-2Torr, passes into nitrogen and remain on 1 standard atmospheric pressure; Then be rapidly heated, in annealing furnace, temperature was elevated to 700 ℃ in 10 minutes, and keeping simultaneously flow velocity is the logical argon gas of 90sccm; After 20 minutes, pass into the oxygen flow that 2% oxygen and 98% argon gas mix in quartz ampoule, kept 30 minutes; Close finally oxygen flow, pass into nitrogen, make annealing furnace naturally cool to room temperature; Take out the substrate of silicon chip or glass sheet from quartzy bottle, its surface is covered by the ZnO of white nanostructured, uses scanning electron microscopic observation, by the scanning electron microscope sem photo, sees the pectination nanostructured zinc oxide sample that self assembly forms;
(2) assembling of pectination Nano ZnO gas sensor: in the air-sensitive proving installation that routine is used, with pectination nanostructured zinc oxide sample dispersion to the golden array electrode of processing in advance with traditional micro-processing technology, each golden cell is of a size of 5 * 5 μ m, then connect respectively golden cell with two microelectrodes, as both positive and negative polarity, and with power supply and current measurement instrument, join, namely form pectination nanostructured zinc oxide gas sensor sample;
(3) gas sensor is tested the carbon monoxide sensing capabilities: before measurement, first the air-sensitive proving installation to routine is filled with nitrogen, other gases in remover, be filled with atmospheric CO to be measured again in the air-sensitive proving installation after the gas sensor sample current is stable, gas sensor sample measurement voltage is 20 volts, the inflation/deflation cycle is 8 minutes, wherein inflates and exits each 4 minutes; During inflation, close nitrogen, be filled with carbon monoxide; During venting, close carbon monoxide, be filled with nitrogen; 2-15 cycle so repeatedly; Use simultaneously computer recording gas sensor sample current curve over time, be the response curve of pectination nanostructured zinc oxide gas sensor, when carbon monoxide gas concentration was 250ppm, the electric current of gas sensor increased; After closing CO gas, electric current reduces.
Compared with prior art, sensor is worked at normal temperatures in the present invention, and it is simple in structure, and power consumption is little; Preparation technology is simple, and cost is low, and the zincite crystal purity of growth is high, integrality good; The pectination of zinc oxide nano fiber, increased and the catalytic surface area of gas; Parallel to each other between the pectination nanometer rods, can reduce contact resistance, the zinc paste at the place of combing dry plays a part to collect, conduction current, the sensitivity that improves sensor.
Description of drawings:
Fig. 1 is pectination nanostructured zinc oxide scanning electron microscopy electromicroscopic photograph of the present invention.
Fig. 2 is the structural principle schematic picture that gas sensor of the present invention carries out electrical testing, wherein, and 1 and 2 two adjacent golden cells of expression; 3 and 4 expression microelectrode lead-in wires, the arrow indication is across the pectination nanostructured zinc oxide between adjacent golden cell gap.
Fig. 3 is the response curve of gas sensor sample of the present invention to CO gas.
Fig. 4 is the sensing capabilities principle schematic of gas sensor of the present invention.
Embodiment:
Also be described further by reference to the accompanying drawings below by embodiment.
Embodiment:
The concrete steps of the present embodiment comprise:
(1) prepare the pectination nanostructured zinc oxide with modified chemical vapor deposition process (MCVD): first quartzy bottle is lain in a horizontal plane in the horizontal quartz ampoule in quick anneal oven, quartzy bottleneck towards identical with airflow direction, the zinc powder of purity 99.9% is put in quartzy bottle position, the end, and area load has the substrate (comprising silicon chip or glass sheet) of gold nano grain to be placed on the bottleneck position; The effect of quartzy bottle is to produce the environment of a rich zinc in bottle, and the oxygen that enters with bottleneck, at bottleneck generation chemical reaction, grows ZnO nano-structure on substrate; Again quartz ampoule is evacuated to 10
-2Torr, pass into nitrogen and remain on 1 standard atmospheric pressure; Then be rapidly heated, in stove, temperature was elevated to 700 ℃ in 10 minutes, and keeping simultaneously flow velocity is the logical argon gas of 90sccm; After 20 minutes, pass into the oxygen flow that 2% oxygen and 98% argon gas mix in quartz ampoule, kept 30 minutes; Close finally oxygen flow, pass into nitrogen, make stove naturally cool to room temperature; Take out substrate from quartzy bottle, its surface is covered by whiteness, observe with scanning electron microscope, can see that whiteness is the ZnO of nanostructured, its scanning electron microscope sem photo can be known the pectination nanostructured zinc oxide sample (as shown in Figure 1) of seeing that self assembly forms;
(2) assembling of pectination Nano ZnO gas sensor: in the air-sensitive proving installation that routine is used, with pectination nanostructured zinc oxide sample dispersion to (as shown in Figure 2) on the golden array electrode of processing in advance with traditional micro-processing technology, each golden cell is of a size of 5 * 5 μ m, then with two microelectrodes connect respectively golden cell as both positive and negative polarity and respectively with power supply and the current measurement instrument rear formation gas sensor sample that joins;
(3) gas sensor is tested the carbon monoxide sensing capabilities: before measurement, first to the air-sensitive proving installation, be filled with nitrogen, other gases in remover, be filled with atmospheric CO to be measured again in device after sample current is stable, sample measurement voltage is 20 volts, the inflation/deflation cycle is 8 minutes, wherein inflates and exits each 4 minutes; During inflation, close nitrogen, be filled with carbon monoxide; During venting, close carbon monoxide, be filled with nitrogen; So repeatedly 2-15 cycle, use simultaneously computer recording sample current curve over time, be the response curve of pectination nanostructured zinc oxide gas sensor, as shown in Figure 3; As seen, when carbon monoxide gas concentration was 250ppm, the electric current of sensor obviously increased; After closing CO gas, electric current reduces rapidly, can see that this sensor has high sensitivity, good repeatability and good stability.
Common airborne oxygen molecule O
2Be adsorbed to the ZnO surface and form multiple negative ion, for example O
-, O
2 -And O
2-, these negative ions can react while with carbon monoxide CO molecule, meeting, and form carbon dioxide CO
2Molecule, the electronics that discharges is got back in ZnO, participates in conduction, has increased electric current; Pectination zinc paste to the high sensitivity principle of gas sensing as shown in Figure 4, can find out, compare with ganoid nano wire, the nanostructured comb tooth has largely increased the contact area with the CO gas molecule; And what form between comb tooth is parallel circuit, and the electric current on each tooth converges on combing dry, increased total current; So pectination nanostructured zinc oxide sensor just shows higher sensitivity to CO gas at ambient temperature.
Claims (1)
1. the preparation method of a pectination nanostructured zinc oxide gas sensor is characterized in that concrete steps comprise:
(1) prepare the pectination nanostructured zinc oxide with modified chemical vapor deposition process (MCVD): first quartzy bottle is lain in a horizontal plane in the horizontal quartz ampoule in quick anneal oven, quartzy bottleneck towards identical with airflow direction, put into the zinc powder of purity 99.9% on the position at the quartzy bottle end; Area load has the silicon chip of gold nano grain or glass sheet to be placed on quartzy bottleneck; Produce the environment of rich zinc in quartzy bottle, the oxygen that enters with quartzy bottleneck, at quartzy bottleneck generation chemical reaction, grows ZnO nano-structure on the substrate of silicon chip or glass sheet; Again quartz ampoule is evacuated to 10
-2Torr, pass into nitrogen and remain on 1 standard atmospheric pressure; Then be rapidly heated, in annealing furnace, temperature was elevated to 700 ℃ in 10 minutes, and keeping simultaneously flow velocity is the logical argon gas of 90sccm; After 20 minutes, pass into the oxygen flow that 2% oxygen and 98% argon gas mix in quartz ampoule, kept 30 minutes; Close finally oxygen flow, pass into nitrogen, make annealing furnace naturally cool to room temperature; Take out the substrate of silicon chip or glass sheet from quartzy bottle, its surface is covered by the ZnO of white nanostructured, uses scanning electron microscopic observation, by the scanning electron microscope sem photo, sees the pectination nanostructured zinc oxide sample that self assembly forms;
(2) assembling of pectination Nano ZnO gas sensor: in the air-sensitive proving installation that routine is used, with pectination nanostructured zinc oxide sample dispersion to the golden array electrode of processing in advance with traditional micro-processing technology, each golden cell is of a size of 5 * 5 μ m, then connect respectively golden cell with two microelectrodes, as both positive and negative polarity, and with power supply and current measurement instrument, join, namely form pectination nanostructured zinc oxide gas sensor sample;
(3) gas sensor is tested the carbon monoxide sensing capabilities: before measurement, first the air-sensitive proving installation to routine is filled with nitrogen, other gases in remover, be filled with atmospheric CO to be measured again in the air-sensitive proving installation after the gas sensor sample current is stable, gas sensor sample measurement voltage is 20 volts, the inflation/deflation cycle is 8 minutes, wherein inflates and exits each 4 minutes; During inflation, close nitrogen, be filled with carbon monoxide; During venting, close carbon monoxide, be filled with nitrogen; 2-15 cycle so repeatedly; Use simultaneously computer recording gas sensor sample current curve over time, be the response curve of pectination nanostructured zinc oxide gas sensor, when carbon monoxide gas concentration was 250ppm, the electric current of gas sensor increased; After closing CO gas, electric current reduces.
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| CN109813760A (en) * | 2019-02-28 | 2019-05-28 | 江苏理工学院 | A kind of zinc oxide nanowire gas sensor and preparation method thereof |
| CN113155915B (en) * | 2021-05-07 | 2023-02-24 | 山东鲁泰控股集团有限公司石墨烯高分子复合材料研发中心 | Titanium mesh supported cobalt-based metal organic framework graphene nanosheet array and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101329357A (en) * | 2008-06-27 | 2008-12-24 | 中国科学院合肥物质科学研究院 | SnO2 thin film of vehicle mounted ethanol detection and preparation method thereof |
| CN102288648A (en) * | 2011-07-07 | 2011-12-21 | 刘文超 | Zinc oxide nanostructure gas sensor and manufacturing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101329357A (en) * | 2008-06-27 | 2008-12-24 | 中国科学院合肥物质科学研究院 | SnO2 thin film of vehicle mounted ethanol detection and preparation method thereof |
| CN102288648A (en) * | 2011-07-07 | 2011-12-21 | 刘文超 | Zinc oxide nanostructure gas sensor and manufacturing method thereof |
Non-Patent Citations (4)
| Title |
|---|
| 《ZnO纳米结构制备及其器件研究》;冯怡等;《中国科技论文在线》;20090331;第4卷(第3期);157-169页 * |
| 《磁控溅射制备In掺杂ZnO薄膜及NO2气敏特性分析》;方亮等;《重庆大学学报》;20090930;第32卷(第9期);1002-1005,1015 * |
| 冯怡等.《ZnO纳米结构制备及其器件研究》.《中国科技论文在线》.2009,第4卷(第3期), |
| 方亮等.《磁控溅射制备In掺杂ZnO薄膜及NO2气敏特性分析》.《重庆大学学报》.2009,第32卷(第9期), |
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