CN102661978A - Plane methane gas sensor with double-sensitive layer structure and manufacturing method thereof - Google Patents
Plane methane gas sensor with double-sensitive layer structure and manufacturing method thereof Download PDFInfo
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- CN102661978A CN102661978A CN2012100910328A CN201210091032A CN102661978A CN 102661978 A CN102661978 A CN 102661978A CN 2012100910328 A CN2012100910328 A CN 2012100910328A CN 201210091032 A CN201210091032 A CN 201210091032A CN 102661978 A CN102661978 A CN 102661978A
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Abstract
The invention discloses a plane methane gas sensor with a double-sensitive layer structure and a manufacturing method thereof, and belongs to the technical field of gas sensors. The existing methane gas sensor does not have high selectivity, high sensitivity, fast response recovery and long-term stability simultaneously. The plane methane gas sensor with a double-sensitive layer structure is characterized in that methane gas sensitive layers of the plane methane gas sensor comprise a nanofiber sensitive layer and a particle coating sensitive layer, wherein the nanofiber sensitive layer is sandwiched between a signal electrode and the particle coating sensitive layer; the nanofiber sensitive layer is composed of a gas sensitive material of SnO2 doped with In and Pd, wherein mass of doped In is 5 to 7% of total mass of In2O3, PdO and SnO2 and mass of doped Pd is 5 to 7% of total mass of In2O3; and the particle coating sensitive layer is composed of a Co3O4-WO3 composite material which is a gas sensitive material. In the preparation method of the plane methane gas sensor, the nanofiber sensitive layer composed of SnO2 doped with In and Pd is prepared at a side of the signal electrode and then the particle coating sensitive layer composed of the Co3O4-WO3 composite material is prepared on the nanofiber sensitive layer so that a whole plane methane gas sensor is obtained; and the whole plane methane gas sensor is cut into the plane methane gas sensor which is a single chip having the area of 1*1 to 10*10mm<2>. The plane methane gas sensor provided by the invention has excellent four performances.
Description
Technical field
The present invention relates to a kind of plane formula methane gas sensor and manufacturing approach thereof with two sensitive layer structures, said sensor has high selectivity, is used for the methane gas sensing, belongs to the gas sensor technical field.
Background technology
Gas sensor is that information translation one-tenth such as a kind of composition with gas, concentration can be by the device of the information of utilizations such as personnel, instrument and meter, computing machine.Gas sensor is widely used in fields such as Industry Control, agricultural production, national defense safety, health care.Particularly based on the sensor of chemical gas of metal oxide gas sensitive; Because volume is little, simple in structure, with low cost; On distributed gas sensor network and portable gas detecting devices, important use is arranged, become and have the call, use one type of the widest sensor in the domestic gas sensor.
The parameter that the research institute of gas sensor is pursued comprises: sensitivity, i.e. the variable quantity of sensor electrical signal, be defined as sensor in air with the ratio of resistance value in seized gas; Response recovery time comprises response time and release time, refers to that all change in electric reaches the time of 95% total variation; Selectivity, the characteristics that do not respond to the response of certain gas and to other gas; Stability, the sensitivity of several months to several years is elegant.In these parameters, selectivity is the core research object of sensor exploitation as one of most important index of gas sensor always.Particularly,,, make it reach practicability so need improve selectivity through methods such as various doping, finishinges because metal oxide is responsive to multiple gases usually based on the sensor of chemical gas of metal oxide gas sensitive.For some inactive gas, like CO
2, CH
4Deng, even, get rid of the interference of other gas with multiple gases sensor composition sensor array.Yet this element manufacturing difficulty is quite big, and testing process is very complicated.
Methane is the simplest organism, also is the hydrocarbon of carbon content minimum (hydrogen content is maximum).Methane is very wide in distributed in nature, is one of principal ingredient of rock gas, biogas, hole gas and coal gas.Methane can be used as fuel, also as the raw material of making materials such as hydrogen, carbon monoxide, carbon black, acetylene, hydrogen cyanide and formaldehyde.Methane has positive tetrahedron shape non-polar molecule; Therefore stability is very high; Sensor of chemical gas is not high usually to the sensitivity of methane, and, in practical application, also need get rid of interference to hydrogen with extremely strong reductibility; Therefore, have high selectivity, to have highly sensitive methane gas sensor simultaneously be one of focus of paying close attention to of scientific research and market always.
Prior art is applied to gas sensor with the particle coating mode or with the nanofiber mode with the metal oxide gas sensitive.So-called particle coating mode is meant that methods such as adopting chemical colloidal sol or mechanical lapping prepares gas sensitive, is coated on the substrate.This mode productive rate height, good uniformity, cost are extremely low, mix easily, and selectivity is good.But this mode metal oxide gas sensitive is reunited easily, and the gas absorption ability is not high, and sensitivity is low, response recovers slow.So-called nanofiber mode is meant that the employing method of electrostatic spinning prepares gas sensitive, and its length-diameter ratio is big, specific surface area is high, and can be formed naturally the reticulate texture sensitive layer, seized gas high adsorption capacity, and highly sensitive, response recovers fast.But; Because method of electrostatic spinning doping difficulty is higher than prepare particle shape gas sensitive doping difficulty with methods such as chemical colloidal sol or mechanical lappings; In a single day particularly add multiple adulterant, the pattern of fiber and structure will be difficult to keep, and be difficult to use in methane gas sensor.
In addition, because of the substrate form is different, sensor of chemical gas also is divided into Figaro formula and plane formula, and big, the temperature control out of true of the former volume is not suitable for producing in enormous quantities.
Summary of the invention
The objective of the invention is to; Obtain a kind of methane gas sensor; Has high selectivity for methane gas; Keep good sensitivity, response restorability and stability simultaneously, and can produce in batches, we have invented a kind of plane formula methane gas sensor and manufacturing approach thereof with two sensitive layer structures for this reason.
The present invention's the plane formula methane gas sensor with two sensitive layer structures is furnished with heating electrode and signal electrode respectively on silicon substrate two side insulation layers; The methane gas sensitive layer is positioned on the signal electrode; It is characterized in that; The methane gas sensitive layer comprises nanofiber sensitive layer and particle coating sensitive layer, and the nanofiber sensitive layer is between signal electrode and particle coating sensitive layer; Nanofiber sensitive layer gas sensitive is the SnO that mixes In and Pd
2, the incorporation of In and Pd respectively accounts for In
2O
3, PdO, SnO
25～7% of three kinds of oxide gross masses, particle coating sensitive layer gas sensitive is Co
3O
4-WO
3Compound substance.
The present invention's the plane formula methane gas sensor manufacturing approach with two sensitive layer structures is substrate with the silicon chip; Make insulation course in the silicon chip both side surface; On two side insulation layers, make some groups of heating electrodes and signal electrode more respectively; Heating electrode in one group and signal electrode position are corresponding up and down, it is characterized in that, make the SnO that mixes In and Pd earlier in signal electrode one side
2The nanofiber sensitive layer is made Co again on said nanofiber sensitive layer
3O
4-WO
3Compound substance particle coating sensitive layer obtains the full wafer sensor, obtains 1 * 1mm through cutting
2To 10 * 10mm
2Monolithic sensor.
Its technique effect of such scheme is, mixes the SnO of In and Pd
2The nanofiber sensitive layer makes the present invention's sensor have characteristics highly sensitive, that the response recovery is fast; Co
3O
4-WO
3Compound substance particle coating sensitive layer can be got rid of the interference of gases such as hydrogen, ethanol, makes sensor have very high selectivity.The sensor that is obtained simultaneously has advantages of higher stability.Compared with prior art, when having high sensitivity, fast-response recovery and high stability, has very high selectivity.
The present invention's method adopts semiconductor technology, in view of the characteristics of semiconductor technology, can produce sensor in batches, after adopting the commercially available 4 inches silicon wafer to manufacture full wafer sensors of a slice, can obtain hundreds of monolithic sensors through cutting.
Description of drawings
Fig. 1 is the present invention's the plane formula methane gas sensor structural representation with two sensitive layer structures, and this figure double as is a Figure of abstract.Fig. 2 is the present invention's the plane formula methane gas sensor heating electrode figure with two sensitive layer structures.Fig. 3 is the present invention's the plane formula methane gas sensor signal electrode figure with two sensitive layer structures.Fig. 4 is the present invention's the plane formula methane gas sensor manufacturing approach synoptic diagram with two sensitive layer structures.Fig. 5 is the present invention's plane formula methane gas sensor with two sensitive layer structures and the comparison diagram of existing sensor on selectivity.Fig. 6 is the present invention's the plane formula methane gas sensor response recovery curve with two sensitive layer structures.Fig. 7 is the present invention's the plane formula methane gas sensor stability curve with two sensitive layer structures.
Embodiment
The present invention's the plane formula methane gas sensor with two sensitive layer structures is furnished with heating electrode 1 and signal electrode 5 respectively on 3 liang of side insulation layers of silicon substrate, see shown in Figure 1.Substrate 3 is the commercially available 4 inches silicon chips of < 100>crystal orientation twin polishing, and thickness is 0.2～3mm.Insulation course is SiO
2Layer, thickness is 50～200nm, comprises following insulation course 2, goes up insulation course 4.Heating electrode 1 is attached to down on the insulation course 2, and signal electrode 5 is attached on the insulation course 4, and the material of heating electrode 4 and signal electrode 5 is Pt, and thickness is 50～200nm.The structure of heating electrode 1 is annular parallel connection, see shown in Figure 3, conducting film width 5 μ m to 0.5mm, heating electrode 1 resistance 1～50 Ω.Signal electrode 5 structures are interdigital structure, see shown in Figure 4, conducting film width 5 μ m to 0.5mm, each interdigital length is 0.5～20mm.The methane gas sensitive layer is positioned on the signal electrode 5.The methane gas sensitive layer comprises nanofiber sensitive layer 6 and particle coating sensitive layer 7, and nanofiber sensitive layer 6 is between signal electrode 5 and particle coating sensitive layer 7.Nanofiber sensitive layer 6 gas sensitives are the SnO that mixes In and Pd
2, the incorporation of In and Pd respectively accounts for In
2O
3, PdO, SnO
25～7% of three kinds of oxide gross masses, nanofiber mean diameter 50～200nm, length 1～10mm.Particle coating sensitive layer 7 gas sensitives are Co
3O
4-WO
3Compound substance, particle coating sensitive layer 7 thickness are 0.05～0.3mm.Heating electrode lead-in wire 8 connects power supply, and signal electrode lead-in wire 9 connects metering circuit.Heating electrode lead-in wire 8 is Pt silk or Au silk with signal electrode lead-in wire 9.
The present invention's the plane formula methane gas sensor manufacturing approach with two sensitive layer structures is a substrate 3 with commercially available 4 inches < 100>crystal orientation twin polishing silicon chips.Make insulation course in the silicon chip both side surface, comprise following insulation course 2, go up insulation course 4, be SiO
2Layer generates through thermal oxidation method in the lump.Again respectively following insulation course 2, on make some groups of heating electrodes 1 and signal electrode 5 through magnetron sputtering, photoetching, corrosion each item technology successively on the insulation course 4; Heating electrode 1 in one group is corresponding up and down with signal electrode 5 positions, and the material of heating electrode 4 and signal electrode 5 is Pt.High annealing is to improve the physical strength and the stability of substrate 3.Adopt the method for electrostatic spinning deposition to mix the SnO of In and Pd earlier in signal electrode 5 one sides
2Nanofiber sensitive layer 6, In, Pd replace part SnO
2In Sn after with In
2O
3, the PdO form exists, the incorporation of In and Pd respectively accounts for In
2O
3, PdO, SnO
25～7% of three kinds of oxide gross masses.With Co
3O
4, WO
3Material mechanical grinds to form slurry, is spin-coated on the nanofiber sensitive layer 6, forms Co
3O
4-WO
3Compound substance particle coating sensitive layer 7 is seen shown in Figure 4ly, obtains the full wafer sensor, obtains 1 * 1mm through cutting
2To 10 * 10mm
2Monolithic sensor.Adopt the heating electrode lead-in wire 8 of Pt silk or Au silk respectively heating electrode 1 and signal electrode 5 to be caused external power supply and metering circuit with signal electrode lead-in wire 9.
Illustrate the present invention below, see shown in Figure 4.
1, be 0.4mm's at commercially available 4 inch thickness<100>Crystal orientation twin polishing silicon chip substrate 3 two sides, through thermal oxidation method under 1000 ℃ of temperature respectively oxidation go out the thick SiO of 100nm
2Following insulation course 2 and last insulation course 4.
2, be sputtering source with the Pt target; Plant capacity 120W is under 300 ℃ the condition at the Ar of air pressure 1Pa compression ring border, underlayer temperature, sputter 2h; Following insulation course 2, on obtain the Pt layer that thickness is 100nm respectively on the insulation course 3, respectively as heating electrode layer, signal electrode layer.
3, the GP18 photoresist is coated on the heating electrode layer, 2400 rev/mins of whirl coating rotating speeds, 60 ℃ of preceding down baking 30min form photoresist layer; The mask plate of parallelly connected figure ringwise is covered on the photoresist layer, uv-exposure 15s, through developing also at 150 ℃ of baking 1h down, photoresist layer has the annular parallelly connected figure of heating electrode 1, sees shown in Figure 2 subsequently.
4, the GP18 photoresist is coated on the signal electrode layer 2400 rev/mins of whirl coating rotating speeds, 60 ℃ of preceding down baking 30min; Form photoresist layer, the mask plate that will be interdigital figure is covered on the photoresist layer, uv-exposure 15s; Subsequently through developing and toasting 1h down at 150 ℃; Photoresist layer has the interdigital figure of signal electrode 5, sees shown in Figure 3ly, and each signal electrode 5 is all corresponding on the position with a heating electrode 1.
5, the using plasma etching technics is in the Ar atmosphere of 5Pa at pressure, plant capacity 90W, and etching 30min under the normal temperature removes the heating electrode layer, the signal electrode layer that do not receive photoresist layer and cover; Subsequently, silicon chip is put into acetone soln soak 20min, remove, obtain heating electrode 1 and signal electrode 5 respectively, the conducting film width 0.25mm of heating electrode 3, length 90mm, resistance value 36 Ω by the photoresist layer of mask; Signal electrode 4 have 6 pairs interdigital, conducting film width 0.25mm, single interdigital length 8mm.
6, in quick anneal oven, annealing in process 10h under 600 ℃ of temperature passes to N therebetween
2As blanket gas.
7, adopt the method for electrostatic spinning deposition to mix the SnO of In (indium) and Pd (palladium) earlier in signal electrode 5 one sides
2Nanofiber sensitive layer 6; Process is following: 0.4g stannous chloride, 0.04g palladium bichloride, 0.05g indium trichloride, 4.42g dimethyl formamide (DMF) and 4.42g alcohol are mixed; And magnetic agitation 6h; The polyvinylpyrrolidone (PVP) that adds 0.8g then is magnetic agitation 6h once more, obtains spinning liquid; Spinning liquid is imported in the syringe of electrospinning device, metal electrode probes in the front end kapillary; Receiving range is as the criterion like 20cm with the distance of capillary tip and dash receiver; Apply the voltage of 10kV then, on signal electrode 5, deposit 10h, form nanofiber sensitive layer 6, nanofiber mean diameter 100nm, length 4mm.
8, spin coating Co on nanofiber sensitive layer 6
3O
4-WO
3Compound substance particle coating sensitive layer 7; Process is following: 0.35g cobalt oxide, 0.25g tungsten oxide, 0.24g palladium bichloride, 0.05g tetraethoxysilance and 02g pyrrolidone are mixed, and mechanical lapping 2h forms slurry; Under the condition of 1000rpm, be spin-coated on slurry above the nanofiber sensitive layer 6; Form particle coating sensitive layer 7, thickness 0.1mm obtains the full wafer sensor.The introducing of palladium bichloride can replenish nanofiber sensitive layer 6 and lose because of the ease of palladium and cause the minimizing of mixing.
9, will obtain the full wafer sensor at 600 ℃ of following sintering 4h, form firm two sensitive layer structures.
10, the full wafer sensor is cut into 2 * 4mm
2Monolithic sensor.
11, heating electrode lead-in wire 8 and signal electrode lead-in wire 9 are the Pt silk, adopt the gold paste welding compound respectively heating electrode lead-in wire 8 and signal electrode lead-in wire 9 to be received power supply and metering circuit in the intelligent air-sensitive analytic system.
The CGS-8 intelligence air-sensitive analytic system that said intelligent air-sensitive analytic system such as Beijing Ai Lite Science and Technology Ltd. produce; This system can provide the present invention's sensor required heating current; And its air-sensitive performance of multianalysis; As heating current 60mA is set, and the selectivity of detecting sensor, response recovery curve and linearity curve steady in a long-term, measurement result is seen Fig. 5～shown in Figure 7.Sensitivity definition among the figure be sensor in air with the ratio of resistance value in seized gas.
The present invention's sensor selectivity testing result is following, sees shown in Figure 5ly, and No. 0 gas is methane among the figure; No. 1 gas is hydrogen, and No. 2 gases are ethanol, and No. 3 gases are acetone; The black post is the present invention's transducer sensitivity for existing transducer sensitivity, white post, and is visible; The present invention's sensor reaches 21.6 for the sensitivity of methane, and is very approaching with existing sensor, still; Then far below existing sensor, show extremely strong selectivity for the sensitivity of other interference gas such as hydrogen, ethanol, acetone.Data are tested under the 60mA heating current among the figure, and concentration of methane gas is 100ppm.
The present invention's sensor response recovery time testing result is following; See shown in Figure 6ly, can find out that it is in the 100ppm methane gas time that sensor as the present invention is exposed to concentration, sensor signal reaches balance about 6s; When sensor is exposed in the air again; Sensor signal is recovered initial value about 10s, therefore, have only the present invention's sensor's response time and release time 6s and 10s respectively.
The present invention's sensor stability testing result is following, sees shown in Figure 7ly, and be 180 days detection time; Detecting number of times is 13 times; Testing result is for the present invention's transducer sensitivity minimum value is 19, maximal value is 23, and is very approaching with mean value 21.6, and still remains on this mean value in the result who detects for the 180th day the 13rd time; It is thus clear that the sensitivity of the present invention's sensor does not still have tangible relaxation phenomenon, explain that the present invention's sensor has good long term stability.
Above presentation of results, the present invention's the plane formula methane gas sensor with two sensitive layer structures has high selectivity for methane gas, keeps good sensitivity, response restorability and stability simultaneously.
Claims (6)
1. plane formula methane gas sensor with two sensitive layer structures; On silicon substrate two side insulation layers, be furnished with heating electrode and signal electrode respectively; The methane gas sensitive layer is positioned on the signal electrode; It is characterized in that the methane gas sensitive layer comprises nanofiber sensitive layer and particle coating sensitive layer, the nanofiber sensitive layer is between signal electrode and particle coating sensitive layer; Nanofiber sensitive layer gas sensitive is the SnO that mixes In and Pd
2, the incorporation of In and Pd respectively accounts for In
2O
3, PdO, SnO
25～7% of three kinds of oxide gross masses, particle coating sensitive layer gas sensitive is Co
3O
4-WO
3Compound substance.
2. the plane formula methane gas sensor with two sensitive layer structures according to claim 1 is characterized in that SnO
2Nanofiber mean diameter 50～200nm, length 1～10mm.
3. the plane formula methane gas sensor with two sensitive layer structures according to claim 1 is characterized in that, particle coating sensitive layer (7) thickness is 0.05～0.3mm.
4. plane formula methane gas sensor manufacturing approach with two sensitive layer structures; With the silicon chip is substrate; Make insulation course in the silicon chip both side surface, on two side insulation layers, make some groups of heating electrodes and signal electrode more respectively, the heating electrode in a group and signal electrode position be correspondence up and down; It is characterized in that, make the SnO that mixes In and Pd earlier in signal electrode one side
2The nanofiber sensitive layer is made Co again on said nanofiber sensitive layer
3O
4-WO
3Compound substance particle coating sensitive layer obtains the full wafer sensor, obtains 1 * 1mm through cutting
2To 10 * 10mm
2Monolithic sensor.
5. the plane formula methane gas sensor manufacturing approach with two sensitive layer structures according to claim 4 is characterized in that, adopts the method for electrostatic spinning deposition to mix the SnO of In and Pd
2Nanofiber sensitive layer (6).
6. the plane formula methane gas sensor manufacturing approach with two sensitive layer structures according to claim 4 is characterized in that, with Co
3O
4, WO
3Material mechanical grinds to form slurry, is spin-coated on the nanofiber sensitive layer (6), forms Co
3O
4-WO
3Compound substance particle coating sensitive layer (7).
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| CN107228927A (en) * | 2017-06-22 | 2017-10-03 | 云南大学 | A kind of high sensitivity methane gas sensitive material and preparation method and application |
| CN108195888A (en) * | 2017-12-27 | 2018-06-22 | 长春理工大学 | Impedance type dew cell using the compound wet sensory material of cross-linked polymer and preparation method thereof |
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| CN109621854A (en) * | 2018-10-31 | 2019-04-16 | 青岛大学 | A kind of compound hollow microballoon preparation method improving triethylamine detection performance |
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| CN105353016A (en) * | 2015-12-10 | 2016-02-24 | 河南工程学院 | Methane gas thin-layer medium electrochemical biosensor and preparing method thereof |
| CN105353016B (en) * | 2015-12-10 | 2017-11-21 | 河南工程学院 | A kind of methane gas thin-layered medium electrochemica biological sensor and preparation method thereof |
| CN106198631A (en) * | 2016-06-27 | 2016-12-07 | 京东方科技集团股份有限公司 | A kind of quasiconductor hydrogen gas sensor and preparation method thereof |
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| CN107228927B (en) * | 2017-06-22 | 2019-08-13 | 云南大学 | A kind of high sensitivity methane gas sensitive material and the preparation method and application thereof |
| CN107228927A (en) * | 2017-06-22 | 2017-10-03 | 云南大学 | A kind of high sensitivity methane gas sensitive material and preparation method and application |
| CN108195888A (en) * | 2017-12-27 | 2018-06-22 | 长春理工大学 | Impedance type dew cell using the compound wet sensory material of cross-linked polymer and preparation method thereof |
| CN108387625A (en) * | 2018-02-24 | 2018-08-10 | 东北大学 | A kind of double coating methane gas sensors and preparation method thereof of anti-organosilicon poisoning |
| CN108387625B (en) * | 2018-02-24 | 2019-06-18 | 东北大学 | A kind of double coating methane gas sensors and preparation method thereof of anti-organosilicon poisoning |
| CN109621854A (en) * | 2018-10-31 | 2019-04-16 | 青岛大学 | A kind of compound hollow microballoon preparation method improving triethylamine detection performance |
| CN109621854B (en) * | 2018-10-31 | 2021-09-14 | 青岛大学 | Preparation method of composite hollow microspheres for improving triethylamine detection performance |
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Application publication date: 20120912 |