CN103364449B - A kind of surface covers the TiO of Pt electrode2nano-tube array room-temperature hydrogen sensor - Google Patents
A kind of surface covers the TiO of Pt electrode2nano-tube array room-temperature hydrogen sensor Download PDFInfo
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 48
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 48
- 125000004435 hydrogen atom Chemical class [H]* 0.000 title abstract 5
- 239000002071 nanotube Substances 0.000 claims abstract description 38
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 18
- 239000011888 foil Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 15
- 230000003647 oxidation Effects 0.000 claims abstract description 15
- 230000035945 sensitivity Effects 0.000 claims abstract description 13
- 230000008569 process Effects 0.000 claims abstract description 12
- 230000004044 response Effects 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims abstract description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 31
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 29
- 150000002431 hydrogen Chemical class 0.000 claims description 25
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000000137 annealing Methods 0.000 claims description 6
- 238000011084 recovery Methods 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 239000010949 copper Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000012360 testing method Methods 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 238000007743 anodising Methods 0.000 claims description 4
- 238000010790 dilution Methods 0.000 claims description 4
- 239000012895 dilution Substances 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 238000004544 sputter deposition Methods 0.000 claims description 4
- 238000005516 engineering process Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 claims description 2
- 230000008025 crystallization Effects 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000011056 performance test Methods 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000000523 sample Substances 0.000 description 10
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 238000012271 agricultural production Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention discloses a kind of room-temperature hydrogen sensor, be specifically related to surface and cover the TiO of Pt electrode2The preparation of nano-tube array hydrogen-sensitive element detects with performance.The preparation method of hydrogen-sensitive element of the present invention is: suitable for cutting high-purity technical Ti paillon foil is placed on ammonium fluoride and glycol water Anodic Oxidation processes 3h through strict cleaning, prepare surface uniformly, the TiO of high-sequential2Nano-tube array.Surface is used to cover the TiO of Pt electrode2Nano-tube array, as hydrogen-sensitive element, improves transducer sensitivity, response speed, reduces operating temperature.
Description
Technical field
The present invention relates to a kind of room-temperature hydrogen sensor, be specifically related to surface in hydrogen gas sensor and cover the TiO of Pt electrode2The preparation of nano-tube array hydrogen-sensitive element detects with performance.
Background technology
Hydrogen is a kind of inexhaustible clean energy resource.As the preferable novel energy of one, it has a wide range of applications in terms of the industrial and agricultural productions such as chemistry, food, electronics.During being guaranteed in various hydrogeneous industrial and agricultural production, the use of hydrogen as energy source, shifting and the safety of the application aspect such as storage, research and development have the problem that the hydrogen gas sensor of the quick performance of good hydrogen has become as people's growing interest.Metal current oxide semiconductor (SnO2、WO3, ZnO) hydrogen gas sensor become the focus of research, it is to utilize the resistance of quasiconductor hydrogen-sensitive element or conductance change under a hydrogen atmosphere to detect hydrogen.But at present the operating temperature of sensors with auxiliary electrode compared with high, sensitivity is relatively low, power consumption is big, safety is low, strongly limit its range of application.TiO2Being the functional material of a kind of green, the physicochemical characteristics of its excellence makes it have wide using value at numerous areas such as storage and utilization, photocatalytic degradation, photochromic, the gas sensors of solar energy.Utilize TiO2Physicochemical properties caused by the small size of nano-tube array and high-specific surface area change and the catalytic action of Pt electrode, are expected to solve the technical bottleneck of metal semiconductor oxide hydrogen gas sensor working and room temperature, improve the sensitivity of sensor simultaneously.
Summary of the invention
It is an object of the invention to: for the deficiencies in the prior art, the present invention provides a kind of room-temperature hydrogen sensor, is specifically related to surface in hydrogen gas sensor and covers the TiO of Pt electrode2The preparation of nano-tube array hydrogen-sensitive element detects with performance.With TiO2Nano-tube array, as hydrogen-sensitive element, improves the performance of sensor；By TiO2The surface of nano-tube array deposits one layer of Pt electrode and can improve sensitivity, shorten response time, reduction operating temperature.
To achieve these goals, the technical scheme is that
A kind of surface that the present invention provides covers the TiO of Pt electrode2Nano-tube array room-temperature hydrogen sensor, using the high-purity technical after cleaning with Ti paillon foil as substrate, uses direct anodizing to prepare TiO2Nano-tube array, then by magnetically controlled DC sputtering at one layer of Pt electrode of its surface portion area deposition, step is as follows:
1, the cleaning of Ti paillon foil:
1) the industrial Ti paillon foil that purity is 99.99% is cut into rectangle, then uses fine sandpaper to polish；
2) the rectangle Ti paillon foil after polishing is successively used each ultrasonic cleaning 30min under acetone, ethanol and deionized water high power, and 80 DEG C of drying in air ambient.
2, use direct anodizing, grow TiO in Ti foil surfaces2Nano-tube array, idiographic flow and process conditions are as follows；
1) the rectangle Ti paillon foil after cleaning is placed in the side of the Multifunctional anodic oxidation device of the glycol water equipped with 0.2wt% ammonium fluoride, accesses positive pole of stabilized voltage supply with wire；Negative electrode copper sheet is placed in anodic oxidation device opposite side, accesses regulated power supply negative pole with wire；
2) anode oxidation process: use 45V constant voltage oxidation 3h to obtain TiO under room temperature (15 DEG C～25 DEG C) environment2Nano-tube array；
3) surface processes: by the TiO after anodic oxidation2Sample first uses a large amount of deionized water repeatedly to rinse, and is subsequently placed in low power ultrasound in Fluohydric acid. and cleans；
3, annealing crystallization processes: the TiO after cleaning2Sample is placed in tubular annealing stove flat-temperature zone, is incubated 3h, is then shut off heater, naturally cools to room temperature in air ambient after rising to 500 DEG C with the heating rate of 10 DEG C/min.
4, a kind of surface covers the TiO of Pt electrode2Nano-tube array room-temperature hydrogen sensor, the preparation process of its surface Pt electrode is:
1) TiO prepared in aforementioned manners2Nano-tube array, as hydrogen-sensitive element, makes electrode pattern mask plate in advance on its surface；
2) magnetically controlled DC sputtering technology is used, at TiO2The zone line on nano-tube array surface prepares rectangle Pt electrode；
Test sensor hydrogen sensitivity energy at room temperature, is connected the probe of data acquisition unit (MASTECH MS8218) with copper pressing wire, is fixed by sample pressing and be placed on the top, closed metal chamber that can flow a gas over.A kind of surface using the present invention covers the TiO of Pt electrode2Nano-tube array room-temperature hydrogen sensor performance detecting step is as follows:
1) before performance test, it is passed through high purity argon, until stable resistance signal occurs in this hydrogen gas sensor；
2) it is continually fed into the hydrogen after argon-dilution until signal curve no longer declines and tends to be steady, resistance signal now is denoted as RH, then pass to air until signal curve no longer rises and tends towards stability, resistance signal now be denoted as R0And repeatable operation is repeatedly；
3) response time of the definition quick test of hydrogen is the time that resistance declines required for 90%, and definition recovery time is 90% required time that resistance returns to initial value.Response and the recovery time of different hydrogen concentration determination after argon-dilution are carried out record；
4) data process, and definition sensitivity S is (R0-RH)/RH, and carry out data scanning and collection.
Advantages of the present invention:
1) direct anodic oxidation on high-purity technical Ti paillon foil is used to prepare TiO2Nano-tube array, its technique is simple, cost is relatively low.
2) TiO is used2Nano-tube array is conducive to surface electronic to migrate as hydrogen-sensitive element, bigger specific surface area；The catalytic action of surface Pt electrode advantageously reduces the operating temperature of sensor.
3) use the hydrogen-sensitive element prepared by the present invention that nitrogen atmosphere at room temperature shows response speed, stable restorability and higher sensitivity faster.
Accompanying drawing explanation
Fig. 1 is the TiO that surface covers Pt electrode2Nano-tube array hydrogen gas sensor configuration schematic diagram.
Fig. 2 is the TiO that surface covers Pt electrode2The nano-tube array hydrogen gas sensor room temperature response curve to variable concentrations hydrogen.
Fig. 3 is the TiO that surface covers Pt electrode2The nano-tube array hydrogen gas sensor sensitivity curve to variable concentrations hydrogen.
Fig. 4 is the TiO that surface covers Pt electrode2Nano-tube array hydrogen gas sensor is to the response of variable concentrations hydrogen and curve recovery time.
Detailed description of the invention
Below by embodiment, and combine accompanying drawing, technical scheme is further described in detail.
As it is shown in figure 1, present embodiment discloses a kind of surface to cover the TiO of Pt electrode2Nano-tube array room-temperature hydrogen sensor, its structure includes that two pieces of thickness that surface covers are 30nm, and a length of 15mm, a width of 2mm are spaced apart the rectangle Pt electrode 1 of 5mm, Ti substrate 2, TiO2Nano-tube array 3.
Specific embodiment is
1, direct anodizing is used to prepare TiO on high-purity technical Ti paillon foil2Nano-tube array:
1) press aforesaid operations step, Ti sheet is cut into the rectangular-shaped pieces of 3cm × 1cm, be carried out by the method for operating procedure one after fine sandpaper is polished；
2) the rectangle Ti paillon foil after cleaning is placed in the side of the Multifunctional anodic oxidation device of the glycol water equipped with 0.2wt% ammonium fluoride, accesses positive pole of stabilized voltage supply with wire；Negative electrode copper sheet is placed in the opposite side of anodic oxidation device, accesses regulated power supply negative pole with wire；
3) 45V is transferred in regulated power supply output, constant voltage anodic oxidation 3h at room temperature 20 DEG C.First using a large amount of deionized water repeatedly to rinse in the sample after oxidation, be subsequently placed in the Fluohydric acid. of 0.08wt%, low power ultrasound cleans 30s, and the residual substance that after removing anodic oxidation, sample surfaces covers, obtaining aperture is 100nm, the TiO of a length of 2 μm2Nano-tube array.
4) by the TiO after anodic oxidation2Sample is placed in the flat-temperature zone of tubular annealing stove and makes annealing treatment.It is incubated 3h after rising to 500 DEG C with the heating rate of 10 DEG C/min in air ambient, is then shut off heater, naturally cools to room temperature.
2, at TiO2Nano-tube array surface coverage mask plate, room temperature, 120W, 0.5Pa parameter under to use magnetically controlled DC sputtering deposition techniques thickness be 30nm, a length of 15mm, a width of 2mm, be spaced apart the two block lengths square Pt electrode of 5mm.Surface covers the TiO of Pt electrode2The hydrogen-sensitive element structure that nano-tube array is constituted is as shown in Figure 1.
3, at room temperature the hydrogen sensitivity of sample can be tested, probe and the copper pressing wire of data acquisition unit (MASTECH MS8218) be connected, then sample pressing is fixed on the top, closed metal chamber that can flow a gas over.Testing to (4) by performance detecting step (1), result is as shown in Figure 2,3, 4.Fig. 2 illustrates that surface covers the TiO of Pt electrode2Nano-tube array all has response to the hydrogen of bigger concentration range.Fig. 3 shows that this hydrogen-sensitive element has higher sensitivity, and under low density of hydrogen (100-500ppm), sensitivity can reach 102To 103；It is up to 10 when density of hydrogen reaches its sensitivity of 2000ppm7.Fig. 4 shows that this hydrogen-sensitive element has very fast response time and stable recovery time, and when density of hydrogen reaches 2000ppm, response time is only 13s the soonest.
Claims (4)
1. the TiO of a surface covering Pt electrode2The preparation method of nano-tube array room-temperature hydrogen sensor, it is characterised in that step
Suddenly it is:
1) cleaning of Ti paillon foil:
The industrial Ti paillon foil that purity is 99.99% is cut into rectangle by a, then uses fine sandpaper polishing；
Rectangle Ti paillon foil after polishing is successively used acetone, ethanol and the most each ultrasonic cleaning of deionized water by b
30min, and 80 DEG C of drying in air ambient；
2) use direct anodizing, grow TiO in Ti foil surfaces2Nano-tube array, idiographic flow and process conditions
As follows:
Rectangle Ti paillon foil after a will clean is placed in the multi-functional anodic oxygen of the glycol water equipped with 0.2wt% ammonium fluoride
Gasifying device side, accesses positive pole of stabilized voltage supply with wire；Negative electrode copper sheet is placed in the opposite side of anodic oxidation device and uses wire
Access regulated power supply negative pole；
B anode oxidation process: use 45V constant voltage oxidation 3h to obtain TiO under room temperature environment2Nano-tube array；
C surface processes: by the TiO after oxidation2Sample first uses a large amount of deionized water repeatedly to rinse, and is subsequently placed in Fluohydric acid.
Low power ultrasound cleans；
D annealing crystallization processes: the sample after anodic oxidation is placed in tubular annealing stove flat-temperature zone, with 10 DEG C in air ambient
The heating rate of/min is incubated 3h after rising to 500 DEG C, is then shut off heater, naturally cools to room temperature；
3) a kind of surface covers the TiO of Pt electrode2Nano-tube array room-temperature hydrogen sensor, the preparation step of its surface Pt electrode
Suddenly it is:
The TiO that a is prepared in aforementioned manners2Nano-tube array hydrogen-sensitive element, makes electrode pattern mask plate in advance on its surface；
B uses magnetically controlled DC sputtering technology, at TiO2The zone line on nano-tube array surface prepares rectangle Pt electrode, institute
State Pt electrode be two block gaps be 5mm, thickness is 30nm, a length of 15mm, a width of 2mm rectangular electrodes.
A kind of surface the most according to claim 1 covers the TiO of Pt electrode2The system of nano-tube array room-temperature hydrogen sensor
Preparation Method, it is characterised in that in step (2), surface processes the Fluohydric acid. mass fraction used is 0.08wt%, and ultrasonic time is
30s。
A kind of surface the most according to claim 1 covers the TiO of Pt electrode2The system of nano-tube array room-temperature hydrogen sensor
Preparation Method, it is characterised in that in step (3), the preparation parameter of Pt electrode is room temperature, 100～150W, 0.5Pa.
The surface that the most according to claim 1, preparation method obtains covers the TiO of Pt electrode2Nano-tube array room temperature hydrogen passes
The method for testing performance of sensor, the steps include:
1) before performance test, it is passed through high purity argon, until stable resistance signal occurs in this hydrogen gas sensor；
2) hydrogen after argon-dilution it is continually fed into until signal curve no longer declines and tends to be steady, by resistance signal now
It is denoted as RH, then pass to air until signal curve no longer rises and tends towards stability, resistance signal now be denoted as R0And it is anti-
Multiple operation is repeatedly；
3) response time of the definition quick test of hydrogen is the time that resistance declines required for 90%, and definition recovery time is that resistance recovers
To 90% required time of initial value, and response and the recovery time of different hydrogen concentration determination after argon-dilution are carried out record；
4) data process, and definition sensitivity S is (R0-RH)/RH, and carry out data scanning and collection.
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| CN103760196B (en) * | 2014-02-19 | 2016-01-20 | 中国工程物理研究院化工材料研究所 | A kind of Birnessite type manganese dioxide nanosheet hydrogen sensor and preparation method thereof |
| CN103926285B (en) * | 2014-04-17 | 2016-04-27 | 武汉大学 | Precious metal doping titanic oxide nano prepares the method for hydrogen gas sensor |
| CN104316461B (en) * | 2014-10-29 | 2017-06-13 | 武汉理工大学 | The Optical Fider Hybrogen Sensor of multi-layer nano membrana granulosa enhanced sensitivity |
| CN106198648B (en) * | 2016-09-14 | 2020-12-01 | 扬州大学 | Preparation method of room temperature hydrogen sensor |
| 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 |
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| CN102180518A (en) * | 2011-01-25 | 2011-09-14 | 湖北大学 | Large-scale preparation method of niobium pentoxide nanowires and hydrogen-sensitive element thereof |
| CN202064019U (en) * | 2011-01-10 | 2011-12-07 | 湖北大学 | Multifunctional anodic oxidation device |
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| US6969900B2 (en) * | 2003-03-17 | 2005-11-29 | National Cheng Kung University | Semiconductor diode capable of detecting hydrogen at high temperatures |
| US20060105141A1 (en) * | 2004-11-18 | 2006-05-18 | General Electric Company | Mesoporous nano-crystalline titania structures for hydrogen sensing |
| US8790502B2 (en) * | 2007-02-21 | 2014-07-29 | Northeastern University | Titania nanotubes prepared by anodization in chloride-containing electrolytes |
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| CN202064019U (en) * | 2011-01-10 | 2011-12-07 | 湖北大学 | Multifunctional anodic oxidation device |
| CN102180518A (en) * | 2011-01-25 | 2011-09-14 | 湖北大学 | Large-scale preparation method of niobium pentoxide nanowires and hydrogen-sensitive element thereof |
Non-Patent Citations (1)
| Title |
|---|
| "TiO2纳米管和纳米管阵列的制备、形貌及机理研究";周成凤;《中国优秀硕士学位论文全文数据库》;20111215(第S2期);第10页第1.6.1节、第38页第4.4节及第39页第1-3段、第44页第4.6.3节第1、2段 * |
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