CN106841314A - One kind is based on nano-TiO2Low-power consumption micro-nano gas sensor and preparation method - Google Patents

One kind is based on nano-TiO2Low-power consumption micro-nano gas sensor and preparation method Download PDF

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CN106841314A
CN106841314A CN201710198653.9A CN201710198653A CN106841314A CN 106841314 A CN106841314 A CN 106841314A CN 201710198653 A CN201710198653 A CN 201710198653A CN 106841314 A CN106841314 A CN 106841314A
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CN106841314B (en
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王海容
王梦雅
王博
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Xian Jiaotong University
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/12Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
    • G01N27/125Composition of the body, e.g. the composition of its sensitive layer
    • G01N27/127Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles

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Abstract

Nano-TiO is based on the invention discloses one kind2Low-power consumption micro-nano gas sensor and preparation method, the sensor from bottom to top be respectively SiO2‑Si3N4Masking layer, silicon base, SiO2‑Si3N4‑SiO2‑Si3N4Composite insulation layer, electrode layer, sensitive material.By arranging thermometric electrode, the chip center of measurement in real time temperature.Most Si are removed by wet etching under Si substrates, SiO is formed2‑Si3N4‑SiO2‑Si3N4Compound suspension structures, are the heating electrode and sensitive electrode by Central Symmetry, screw arrangement on outstanding film.Sensitive material is located on sensitive electrode, and TiO is sputtered successively in sensitive material region2Film, wherein Ti films, TiO2Film is used to define the vitellarium of follow-up nanometer rods, and Ti sources are oxidized to TiO by hot hydrochloric acid vapour method2Nanometer rods prepare sensitive layer, make TiO2Nanorod growth is in TiO2On film.Nanometer rods bridge joint of the present invention is connected, with high specific surface area and more preferable gas response characteristic;The mechanical performance of outstanding film is optimized, heat transfer, temperature controllable precise is reduced.Simplify operation, it is to avoid the generation of parasitic fields.

Description

One kind is based on nano-TiO2Low-power consumption micro-nano gas sensor and preparation method
Technical field
Nano-TiO is based on the present invention relates to one kind2Low-power consumption micro-nano gas sensor configuration and preparation method.
Background technology
All there is extensive demand in many fields of national product life to the detection of gaseous species and concentration.Such as, family Air quality in the confined spaces such as residence, cubicle, compartment directly affects the comfort level of people, if toxic and harmful cannot Timely detect, trigger alarm, or even the life security that people can be threatened.In field of industrial production, such as petrochemical industry, pharmacy, rubber, skin Leather etc., particularly produce poisonous inflammable or foul gas workplace, it is necessary to all kinds of toxic gases in production are detected, Monitoring and alarm.And in agriculture field, the content of oxygen or carbon dioxide can directly affect the growth of crop.
Gas sensor is the effective means of gas detection, it is possible to achieve real-time monitoring to specific gas and to gas Analysis of composition etc., huge application potential is had in national product life association area.From semiconductor alloy oxygen in 1962 Since compound ceramic gas sensor comes out, it is most universal, most practical that semiconductor gas sensor has become current application One class gas sensor of value.Semiconductor gas sensor is the element made using metal oxide semiconductor material, Under uniform temperature, adsorption or reaction are produced when being interacted with gas, cause the electrical conductivity being characterized with carrier moving Or C-V characteristic or surface potential change.So, metal-oxide gas transducer typically by metal oxide sensing element and Heating element heater is constituted.
Wherein sensing element is changed into the thick film form based on screen printing technique from initial bulk forms, to nowadays base In the film morphology of MEMS technology, the specific surface area of sensitive material is set constantly to increase, gas response characteristic gradually strengthens.Especially The metal oxide nano-material of the various forms of recent researches, such as nanometer rods, nanosphere, nano wire, by countless nanometers The thin-film material of monomer bridge joint has high gas-sensitive property.
The direction that heating element heater also constantly reduces towards volume, each structure height is integrated is developed, by heating element heater, sensitive unit Part etc. is integrated on a device for micron level, realizes the functions such as quick heating, Quick resistance measurement, and adiabatic by discharging Groove forms cantilever beam or suspension structures etc. to reduce power consumption, compared with ordinary sensors, it is easier to meet current all trades and professions pair Portable, low pow consumption gas sensor requirement.But the micro-heater being made up of each layer film should due to the complicated and film of technique Easily there is rupture in power, reduces the yield rate of device.
Additionally, it is the difficulty for nowadays preparing micro-nano gas sensor that nano film material is integrated with micro- heating plate of low-power consumption Point.How will be blended with highly sensitive nano film material and the technique for preparing the micro- heating plate of low-power consumption is the heat studied Point.
The content of the invention
The technical problems to be solved by the invention are to overcome nano material to prepare and traditional MEMS technique incompatibility problem, Nano sensitive material is set to position homoepitaxial on the premise of higher sensitivity is kept.Meanwhile, improve the outstanding film of gas sensor Mechanical property, and temperature control electrode is set, thus a kind of metal-oxide gas transducer and preparation method are provided, simplify and pass Sensor integrated technique, prepares the low pow consumption gas sensor that can be mass-produced of accurate temperature controlling.
To achieve the above objectives, the present invention is adopted the following technical scheme that and is achieved:
One kind is based on nano-TiO2Low-power consumption micro-nano gas sensor preparation method, comprise the steps:
(1) at Si substrate front surfaces and the back side, thermal oxide is respectively adopted and Low Pressure Chemical Vapor Deposition prepares SiO2-Si3N4 Double-layer compound film;
(2) in front SiO2-Si3N4On double-layer compound film, sunk successively using plasma reinforced chemical vapour deposition method Product SiO2And Si3N4, and anneal at a certain temperature;
(3) on the insulating barrier of front, by spin coating photoetching process, sensitive electrode and lead wire tray, heating electrode are obtained and is drawn The figure of drum and thermometric electrode and lead wire tray;
(4) Cr is sputtered on heating electrode and lead wire tray, sensitive electrode and lead wire tray and thermometric electrode and lead wire tray figure Adhesive linkage, then sputters Au layers on adhesive linkage;
(5) by stripping technology, sensitive electrode and lead wire tray, heating electrode and lead wire tray and thermometric electrode and lead are obtained Disk, and made annealing treatment;
(6) on the rectangular area that sensitive electrode is surrounded, sensitive layer pattern is obtained by photoetching process;
(7) TiO is sputtered on sensitive layer pattern2Film, defines follow-up nanorod growth position;In TiO2Sputtered on film Ti films, there is provided titanium source;
(8) TiO is prepared using hot hydrochloric acid vapour method2Nanometer rods;
(9) take and obtain Si backside of substrate insulation tanks with step (3) identical spin coating photoetching process, that is, complete low-power consumption micro- Receive the making of gas sensor.
Further scheme in above-mentioned technique is also resided in:
In the step (1), SiO2-Si3N4The middle SiO of double-layer compound film2Film thickness is 500nm, Si3N4Film is thick It is 150nm to spend.
In the step (2), SiO is sequentially depositing2Thickness is 500nm and Si3N4Thickness is 150nm, and 500 DEG C -600 Anneal 5-7h at DEG C.
In the step (4), sputtering Cr thickness of adhibited layer is 50nm, and sputtering Au thickness degree is 250nm.
In the step (5), anneal 10-30min at 260 DEG C-300 DEG C.
In the step (7), TiO is sputtered2Film thickness is 30nm;Sputtering Ti film thicknesses are 300nm.
In the step (8), TiO is prepared2The method of nanometer rods is as follows:
Sputtering 8a) there is into TiO2On the chain-wales that film, the chip of Ti films are placed in high-pressure hydrothermal reaction kettle, by hydrochloric acid With deionized water by volume 1:Added after 10 mixing in reactor, 3.5h is incubated at 150 DEG C;
8b) after cooling, chip is taken out, removal chip surface debris, 100 DEG C of bakings is cleaned successively with ethanol and deionized water Dry 0.5h, obtains TiO2Nano-rod film.
In the step (9), Si backside of substrate is prepared insulation tank and is comprised the steps:
9a) by photoetching process, photoresist dispels the Si at notch window by deep dry etching as masking layer3N4- SiO2Layer, photoresist is removed using lift-off techniques, obtains the insulated tank figure below silicon base;
9b) in chip front side spin coating photoresist, after 90 DEG C of drying, PDMS is dropwise dropped in into chip front side, until by front Drop is full, 70 DEG C of drying 1h, by chip front side patch on the glass sheet, and chip back foreign aid painting one is enclosed into PDMS, makes chip firmly Patch is on the glass sheet;
Chip 9c) is put into sheet glass concentration together in 25% TMAH TMAH solution, 85 DEG C of temperature Lower corrosion 16h forms insulation tank;PDMS is gently torn, with acetone soak, photoresist and remnants PDMS, 100 DEG C of drying is removed 1h, obtains sensor.
The present invention so give according to above-mentioned process make one kind be based on nano-TiO2Low-power consumption micro-nano gas Body sensor, including Si substrates, the back side of Si substrates are provided with insulated tank, and SiO is followed successively by Si backside of substrate2Masking layer and Si3N4 Masking layer, front is by SiO2-Si3N4-SiO2-Si3N4The insulating barrier that four-level membrane is composited, on insulating barrier set a pair it is quick Sense electrode and its lead wire tray, two pairs of heating electrode and its lead wire tray, two pairs of thermometric electrodes and its lead wire tray, each electrode is located at same Plane, is prepared using the same technique of identical material, and sensitive material is located at centre sensitive electrode top, sensitive layer by film and Nanorod structure is constituted.
Further scheme is also resided in said structure:
The sensitive material is rectangular arrangement heart position in the sensor, a pair is led on sensitive electrode and symmetrical is in The electrode wires of zigzag shape, and to contact conductor disk;Sensitive electrode is interdigital structure, is fully contacted with sensitive layer, heats electrode Along sensitive electrode side lead to two pairs it is symmetrical in double-stranded heater strip, and to heating element heater lead wire tray;Around quick Sense electrode, temperature detecting resistance is respectively provided at both sides, and each electrode respectively has independent lead wire tray, is distributed in both sides, and sensor owns Electrode and lead wire tray are and are centrosymmetrically arranged.
The sensitive layer is by TiO2Film and TiO2Nanometer rods two parts are constituted, and insulating barrier is by SiO2-Si3N4-SiO2-Si3N4 Four-level membrane is composited, and masking layer is by SiO2-Si3N4Bilayer film is composited.Sensitive electrode, heating electrode, temperature detecting resistance And each lead wire tray is made of Cr-Au films.
Compared with prior art, the present invention has advantages below:
1st, by sputtering TiO2Ti sources are oxidized to TiO by film, Ti films, hot hydrochloric acid vapour method2Nanometer rods prepare sensitive Layer, makes TiO2Nanorod growth is in TiO2On film.Compared with simple sputtered film, the specific surface area of sensitive material is increased, made Have more preferable gas response characteristic;With TiO is grown on electrode merely2Nanometer rods are compared, in one layer of very thin TiO2Film Upper growth preferably located TiO2The growth position of nanometer rods, makes nanometer rods concentrate on positioning area, is allowed to controllability, right For production in enormous quantities, being capable of being consistent property.
2nd, insulating barrier is from bottom to top by SiO2-Si3N4-SiO2-Si3N4Four-level membrane constitute, after wet etching insulated tank into To hang film.Ground floor SiO is prepared by thermal oxidation method2, reduce due to directly in conjunction with the intrinsic stress for producing, as Si and Si3N4 Between cushion, recycle PECVD deposition SiO2、Si3N4Layer, on the one hand using PECVD method deposition film high mechanical strengths Advantage, increase outstanding film strength.On the other hand, the generation of stress between four layers of film successively staggeredly, suppression four-level membrane, and The residual stress between four-level membrane is greatly eliminated using annealing.This kind of method optimizes the mechanical performance of outstanding film.
3rd, centrosymmetric temperature element is provided with, by the temperature for measuring the resistance of temperature detecting resistance to determine sensitizing range Degree obtains during working sensor accurately temperature control.
4th, heating element heater, sensing element, temperature element are arranged on same layer, and each figure is once splashed to using identical material In shape, operation has been simplified, it is to avoid the generation of parasitic fields.
5th, gas sensor size of the invention is only 2 × 2mm, and heat is reduced by Si substrates back wet etching insulated tank Transmission, extremely low power can be reached during by conducting self-heating heated by electrodes, meet need of the present market to low-power consumption sensor Ask.
Brief description of the drawings
Fig. 1 is the section of structure of low-power consumption micro-nano gas sensor of the present invention.
Fig. 2 (a), Fig. 2 (b) are respectively heating electrode, sensitive electrode, the thermometric of low-power consumption micro-nano gas sensor of the present invention The planar structure of electrode.
Fig. 3 (a), Fig. 3 (b) are that the sensitive material nanorod growth of low-power consumption micro-nano gas sensor of the present invention is being defined TiO2Schematic diagram on film.
Fig. 4 (a)-Fig. 4 (m) is the preparation technology flow chart of low-power consumption micro-nano gas sensor of the present invention.
In figure:1、Si3N4Masking layer;2、SiO2Masking layer;3rd, Si substrates;4、SiO2Insulating barrier I;5、Si3N4Insulating barrier I; 6、SiO2Insulating barrier II;7、Si3N4Insulating barrier II;8th, Cr-Au heating electrode;9、TiO2Nano thin-film;10、TiO2Nanometer rods;11、 Cr-Au sensitive electrodes;12nd, lead wire tray;13rd, insulated tank;14th, thermometric electrode;15th, sensitive material.
Specific embodiment
The invention will be described in further detail with reference to the accompanying drawings and examples, but is not intended as doing any limit to invention The foundation of system.
(a), (b) are shown as shown in Figure 1, Figure 2, and the present invention is based on nano-TiO2Low-power consumption micro-nano gas sensor, including Si Substrate 3, the back side of Si substrates 3 is provided with insulated tank 13, and SiO is followed successively by the back side of Si substrates 32Masking layer 2 and Si3N4Masking layer 1, Front is by SiO2The 4-Si of insulating barrier I3N4The 5-SiO of insulating barrier I2The 6-Si of insulating barrier II3N4The four-level membrane of insulating barrier II 7 is composited Insulating barrier, 12, the two couples of Cr-Au of a pair of Cr-Au sensitive electrodes 11 and its lead wire tray heating electrodes 8 are set on insulating barrier and its are drawn 12, two pairs of thermometric electrodes 14 of drum and its lead wire tray 12, each electrode is generally aligned in the same plane, using the same technique system of identical material Standby, sensitive material 15 is located at centre sensitive electrode top, and sensitive layer is by TiO2Nano thin-film 9 and TiO2The structure of nanometer rods 10 Composition.
As shown in Fig. 2 (a), (b), sensitive material 15 is rectangular arrangement heart position, Cr-Au sensitive electrodes 11 in the sensor On lead to a pair electrode wires of symmetrical helically wire, and to contact conductor disk;Cr-Au sensitive electrodes 11 are interdigital knot Structure, is fully contacted with sensitive layer, Cr-Au heat electrode 8 along the side of Cr-Au sensitive electrodes 11 lead to two pairs it is symmetrical in double spiral shells The heater strip of structure is revolved, and to heating element heater lead wire tray;Around Cr-Au sensitive electrodes 11, thermometric electrode 14 is separately positioned on two Side, each electrode respectively has independent lead wire tray, is distributed in both sides, and all electrodes of sensor and lead wire tray are Central Symmetry cloth Put.
Sensitive layer is by TiO2Film 9 and TiO2The two parts of nanometer rods 10 are constituted, and insulating barrier and masking layer are by SiO2-Si3N4It is double Layer film is composited;Sensitive electrode, heating electrode and temperature detecting resistance and each lead wire tray are made of Cr-Au films.
Reference picture 2 (a), heater strip and sensitive electrode are Central Symmetry, spiral way arrangement, and sensitive electrode is heated silk Surround, sensitive material is in sensitive electrode top.Reference picture 2 (b), a pair of Cr-Au heater strip inner rings sizes are the μ of 145 μ m 240 M, heater strip width is 12 μm, and gap is 40 μm.Cr-Au sensitive electrodes, a width of 15 μm of electrode, gap is 10 μm, such as Fig. 2 (b) Shown, sensitive material is located in the region of wire frame 14, and sensitive electrode top, size is 100 μm of 100 μ m.
As shown in Fig. 3 (a), (b), nanorod growth is in the TiO for defining2Bridged on film, between nanometer rods and be connected, Form the nano-rod film with high specific surface area.
Reference picture 4, low-power consumption metal-oxide gas transducer preparation method of the invention is as follows:
Embodiment 1
(1) as shown in Fig. 4 (a), at Si substrate front surfaces and the back side, thermal oxide and Low Pressure Chemical Vapor Deposition is respectively adopted Prepare SiO2-Si3N4Double-layer compound film;The two-sided thermal oxide 500nm SiO of silicon chip2Layer, (low pressure chemical phase sinks two-sided LPCVD Form sediment) deposition 150nm Si3N4
(2) as shown in Fig. 4 (b), in front SiO2-Si3N4On double-layer compound film, front is sequentially depositing using PECVD 500nm SiO2、150nm Si3N4, anneal 7h at 500 DEG C.
(3) as shown in Fig. 4 (c), on the insulating barrier of front, by spin coating photoetching process obtain sensitive electrode and lead wire tray, The figure of heating electrode and lead wire tray, thermometric electrode and lead wire tray, photoresist uses positive glue EPG535.
(4) as shown in Fig. 4 (d), Cr bondings are sputtered on heating electrode and lead wire tray and sensitive electrode and lead wire tray figure Layer, then sputters Au layers on adhesive linkage;Sputter 50nm Cr, 250nm Au successively using sputter.
(5) such as Fig. 4 (e), photoresist is removed using lift-off (stripping) technique, obtains each electrode and lead wire tray, 300 DEG C Lower annealing 10min.
(6) as shown in Fig. 4 (f), on the rectangular area that sensitive electrode is surrounded, take and step (3) identical spin coating light Carving technology obtains sensitive material pattern.
(7) TiO is sputtered on sensitive layer pattern2Film, defines follow-up nanorod growth position;In TiO2Sputtered on film Ti films, there is provided titanium source;Sputter 30nm TiO successively using sputter2, 300nm Ti, shown in such as Fig. 4 (g).
(8) TiO is prepared using hot hydrochloric acid vapour method2Nanometer rods;Photoresist is removed using lift-off techniques, sensitivity is obtained Patterns of material such as Fig. 4 (h).
Sputtering there is into TiO2Film, the chip of Ti films as the chain-wales in high-pressure hydrothermal reaction kettle on, by hydrochloric acid and Deionized water by volume 1:10 mixing, add in reactor, are put into drying oven and are incubated 3.5h at 150 DEG C.After cooling, Reactor is taken out from drying oven, chip is taken out immediately, surface irregularities, 100 DEG C of drying are cleaned according to this with ethanol, deionized water 0.5h, obtains TiO2Nano-rod film.As shown in Fig. 4 (i).
(9) take and obtain back side notch window pattern, such as Fig. 4 (j) with step (3) identical spin coating photoetching process.
(9a) photoresist dispels the Si at notch window by deep dry etching as masking layer3N4-SiO2Layer, during etching Between 13min.Photoresist is removed using lift-off techniques, window such as Fig. 4 (k) is obtained.
PDMS after 90 DEG C of drying, is dropwise dropped in chip front side in chip front side spin coating photoresist by (9b), until by front Drop is full, shown in 70 DEG C of drying 1h, such as Fig. 4 (l), chip front side is pasted on the glass sheet, and chip back foreign aid is applied into one and enclosed PDMS, makes chip firmly paste on the glass sheet.
With sheet glass be put into chip together in TMAH (concentration is 25% TMAH) solution by (9c), 85 DEG C, Corrosion 16h forms insulation tank.PDMS is gently torn, with acetone soak, photoresist and remnants PDMS, 100 DEG C of drying 1h is removed, Obtain sensor such as Fig. 4 (m).
Embodiment 2
(1) at Si substrate front surfaces and the back side, thermal oxide is respectively adopted and Low Pressure Chemical Vapor Deposition prepares SiO2-Si3N4 Double-layer compound film;The two-sided thermal oxide 500nm SiO of silicon chip2Layer, two-sided LPCVD (low pressure chemical phase precipitation) deposits 150nm Si3N4
(2) in front SiO2-Si3N4On double-layer compound film, front is sequentially depositing 500nm SiO using PECVD2、 150nm Si3N4, anneal 5h at 600 DEG C.
(3) on the insulating barrier of front, sensitive electrode and lead wire tray, heating electrode and lead are obtained by spin coating photoetching process The figure of disk, thermometric electrode and lead wire tray, photoresist uses positive glue EPG535.
(4) Cr adhesive linkages are sputtered on heating electrode and lead wire tray and sensitive electrode and lead wire tray figure, then in bonding Au layers is sputtered on layer;Sputter 50nm Cr, 250nm Au successively using sputter.
(5) photoresist is removed using lift-off (stripping) technique, obtains each electrode and lead wire tray, annealed at 260 DEG C 30min。
(6) on the rectangular area that sensitive electrode is surrounded, take and obtain sensitivity with step (3) identical spin coating photoetching process Patterns of material.
(7) TiO is sputtered on sensitive layer pattern2Film, defines follow-up nanorod growth position;In TiO2Sputtered on film Ti films, there is provided titanium source;Sputter 30nm TiO successively using sputter2、300nm Ti。
(8) TiO is prepared using hot hydrochloric acid vapour method2Nanometer rods;Photoresist is removed using lift-off techniques, sensitivity is obtained Patterns of material.
Sputtering there is into TiO2Film, the chip of Ti films as the chain-wales in high-pressure hydrothermal reaction kettle on, by hydrochloric acid and Deionized water by volume 1:10 mixing, add in reactor, are put into drying oven and are incubated 3.5h at 150 DEG C.After cooling, Reactor is taken out from drying oven, chip is taken out immediately, surface irregularities, 100 DEG C of drying are cleaned according to this with ethanol, deionized water 0.5h, obtains TiO2Nano-rod film.
(9) take and obtain back side notch window pattern with step (3) identical spin coating photoetching process.
(9a) photoresist dispels the Si at notch window by deep dry etching as masking layer3N4-SiO2Layer, during etching Between 13min.Photoresist is removed using lift-off techniques, window is obtained.
PDMS after 90 DEG C of drying, is dropwise dropped in chip front side in chip front side spin coating photoresist by (9b), until by front Drop is full, 70 DEG C of drying 1h, by chip front side patch on the glass sheet, and chip back foreign aid painting one is enclosed into PDMS, makes chip firmly Patch is on the glass sheet.
With sheet glass be put into chip together in TMAH (concentration is 25% TMAH) solution by (9c), 85 DEG C, Corrosion 16h forms insulation tank.PDMS is gently torn, with acetone soak, photoresist and remnants PDMS, 100 DEG C of drying 1h is removed, Obtain sensor.
The invention is not limited in above-described embodiment, on the basis of technical scheme disclosed by the invention, the skill of this area Art personnel are according to disclosed technology contents, it is not necessary to which performing creative labour just can make one to some of which technical characteristic A little to replace and deform, these are replaced and deform within the scope of the present invention.

Claims (10)

1. it is a kind of to be based on nano-TiO2Low-power consumption micro-nano gas sensor preparation method, it is characterised in that including following steps Suddenly:
(1) at Si substrate front surfaces and the back side, thermal oxide is respectively adopted and Low Pressure Chemical Vapor Deposition prepares SiO2-Si3N4It is double-deck Laminated film;
(2) in front SiO2-Si3N4On double-layer compound film, it is sequentially depositing using plasma reinforced chemical vapour deposition method SiO2And Si3N4, and anneal at a certain temperature;
(3) on the insulating barrier of front, by spin coating photoetching process, sensitive electrode and lead wire tray, heating electrode and lead wire tray are obtained With thermometric electrode and the figure of lead wire tray;
(4) Cr bondings are sputtered on heating electrode and lead wire tray, sensitive electrode and lead wire tray and thermometric electrode and lead wire tray figure Layer, then sputters Au layers on adhesive linkage;
(5) by stripping technology, sensitive electrode and lead wire tray, heating electrode and lead wire tray and thermometric electrode and lead wire tray are obtained, And made annealing treatment;
(6) on the rectangular area that sensitive electrode is surrounded, sensitive layer pattern is obtained by photoetching process;
(7) TiO is sputtered on sensitive layer pattern2Film, defines follow-up nanorod growth position;In TiO2Ti is sputtered on film thin Film, there is provided titanium source;
(8) TiO is prepared using hot hydrochloric acid vapour method2Nanometer rods;
(9) take and obtain Si backside of substrate insulation tanks with step (3) identical spin coating photoetching process, that is, complete low-power consumption micro-nano gas The making of body sensor.
2. according to claim 1 based on nano-TiO2Low-power consumption micro-nano gas sensor preparation method, its feature exists In, in the step (1), SiO2-Si3N4The middle SiO of double-layer compound film2Film thickness is 500nm, Si3N4Film thickness is 150nm。
3. according to claim 1 based on nano-TiO2Low-power consumption micro-nano gas sensor preparation method, its feature exists In in the step (2), being sequentially depositing SiO2Thickness is 500nm and Si3N4Thickness is 150nm, and at 500 DEG C -600 DEG C Annealing 5-7h;
In the step (5), anneal 10-30min at a temperature of 260 DEG C-300 DEG C.
4. according to claim 1 based on nano-TiO2Low-power consumption micro-nano gas sensor preparation method, its feature exists In in the step (4), sputtering Cr thickness of adhibited layer is 50nm, and sputtering Au thickness degree is 250nm.
5. according to claim 1 based on nano-TiO2Low-power consumption micro-nano gas sensor preparation method, its feature exists In, in the step (7), sputtering TiO2Film thickness is 30nm;Sputtering Ti film thicknesses are 300nm.
6. according to claim 1 based on nano-TiO2Low-power consumption micro-nano gas sensor preparation method, its feature exists In, in the step (8), preparation TiO2The method of nanometer rods is as follows:
Sputtering 8a) there is into TiO2On the chain-wales that film, the chip of Ti films are placed in high-pressure hydrothermal reaction kettle, hydrochloric acid and will go Ionized water by volume 1:Added after 10 mixing in reactor, 3.5h is incubated at 150 DEG C;
8b) after cooling, chip is taken out, removal chip surface debris, 100 DEG C of drying is cleaned successively with ethanol and deionized water 0.5h, obtains TiO2Nano-rod film.
7. according to claim 1 based on nano-TiO2Low-power consumption micro-nano gas sensor preparation method, its feature exists In in the step (9), Si backside of substrate is prepared insulation tank and comprised the steps:
9a) by photoetching process, photoresist dispels the Si at notch window by deep dry etching as masking layer3N4-SiO2 Layer, photoresist is removed using lift-off techniques, obtains the insulated tank figure below silicon base;
9b) in chip front side spin coating photoresist, after 90 DEG C of drying, PDMS is dropwise dropped in into chip front side, until front drop is full, 70 DEG C of drying 1h, by chip front side patch on the glass sheet, and apply a circle PDMS by chip back foreign aid, chip is firmly attached to glass On glass piece;
Chip 9c) is put into sheet glass concentration together in 25% TMAH TMAH solution, it is rotten at a temperature of 85 DEG C Erosion 16h forms insulation tank;PDMS is gently torn, with acetone soak, photoresist and remnants PDMS, 100 DEG C of drying 1h is removed, obtained To sensor.
8. it is a kind of to be based on nano-TiO2Low-power consumption micro-nano gas sensor, it is characterised in that including Si substrates, the back of the body of Si substrates Face is provided with insulated tank, and SiO is followed successively by Si backside of substrate2Masking layer and Si3N4Masking layer, front is by SiO2-Si3N4-SiO2- Si3N4The insulating barrier that four-level membrane is composited, sets a pair of sensitive electrodes and its lead wire tray, two pairs of heating electrodes on insulating barrier And its lead wire tray, two pairs of thermometric electrodes and its lead wire tray, each electrode is generally aligned in the same plane, using the same technique system of identical material Standby, sensitive material is located at centre sensitive electrode top, and sensitive layer is made up of film and nanorod structure.
9. according to claim 8 a kind of based on nano-TiO2Low-power consumption micro-nano gas sensor, it is characterised in that institute It is rectangular arrangement heart position in the sensor to state sensitive material, and a pair symmetrical helically wire are led on sensitive electrode Electrode wires, and to contact conductor disk;Sensitive electrode is interdigital structure, is fully contacted with sensitive layer, and heating electrode is along sensitive electrode Side lead to two pairs it is symmetrical in double-stranded heater strip, and to heating element heater lead wire tray;Around sensitive electrode, thermometric Resistance is respectively provided at both sides, and each electrode respectively has independent lead wire tray, is distributed in both sides, all electrodes of sensor and lead wire tray It is and is centrosymmetrically arranged.
10. according to claim 8 a kind of based on nano-TiO2Low-power consumption micro-nano gas sensor, it is characterised in that institute Sensitive layer is stated by TiO2Film and TiO2Nanometer rods two parts are constituted, and insulating barrier is by SiO2-Si3N4-SiO2-Si3N4Four-level membrane is answered Conjunction is formed, and masking layer is by SiO2-Si3N4Bilayer film is composited;Sensitive electrode, heating electrode and temperature detecting resistance and each lead Disk is made of Cr-Au films.
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