CN106841314B - One kind being based on nano-TiO2Low-power consumption micro-nano gas sensor and preparation method - Google Patents
One kind being based on nano-TiO2Low-power consumption micro-nano gas sensor and preparation method Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating 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
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
Abstract
The invention discloses one kind to be based on nano-TiO2Low-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, real-time measurement chip center temperature.Most Si are removed by wet etching under Si substrate, form SiO2‑Si3N4‑SiO2‑Si3N4Compound suspension structures hang on film for by the heating electrode and sensitive electrode of central symmetry, screw arrangement.Sensitive material is located on sensitive electrode, successively sputters TiO in sensitive material region2Film, Ti film, wherein TiO2Film is used to define the vitellarium of subsequent nanometer rods, and the source Ti is 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, and has high specific surface area and better gas response characteristic；The mechanical performance of outstanding film is optimized, heat transmitting, temperature controllable precise are reduced.Process is simplified, the generation of parasitic fields is avoided.
Description
Technical field
The present invention relates to one kind to be based on nano-TiO2Low-power consumption micro-nano gas sensor configuration and preparation method.
Background technique
All there is extensive demand in many fields of national product life to the detection of gaseous species and concentration.For example, family
Air quality in the confined spaces such as residence, cubicle, compartment directly affects the comfort level of people, if toxic and harmful gas cannot get
It timely detects, cause alarm, or even the life security of people can be threatened.In field of industrial production, such as petrochemical industry, pharmacy, rubber, skin
Leather etc., especially generates toxic inflammable or foul gas workplace, need to detect toxic gases all kinds of in production,
Monitoring and alarm.And in agriculture field, the content of oxygen or carbon dioxide will have a direct impact on the growth of crop.
Gas sensor is the effective means of gas detection, be may be implemented to the real-time monitoring of specific gas and to gas
The analysis etc. of ingredient, in national product life related fields, there is huge application potentials.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
A kind of gas sensor of value.Semiconductor gas sensor is the element being made into using metal oxide semiconductor material,
Adsorption is generated under certain temperature, when interacting with gas or is reacted, and the conductivity characterized by carrier moving is caused
Or C-V characteristic or surface potential change.So metal-oxide gas transducer generally by metal oxide sensing element and
Heating element composition.
Wherein sensing element becomes the thick film form based on screen printing technique from initial bulk forms, to nowadays base
In the film morphology of MEMS technology, increase the specific surface area of sensitive material constantly, gas response characteristic gradually increases.Especially
The metal oxide nano-material of the various forms of recent researches, such as nanometer rods, nanosphere, nano wire, by countless nanometers
Thin-film material made of monomer bridge joint has high gas-sensitive property.
The direction that heating element also constantly reduces towards volume, each structure height is integrated is developed, by heating element, sensitive member
Part etc. is integrated on the device of a micron level, realizes the functions such as quickly heating, Quick resistance measurement, and pass through release insulation
Slot 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 of each layer film is answered due to the complexity and film of technique
Power is easy to appear rupture, reduces the yield rate of device.
In addition, it is the difficulty for nowadays preparing micro-nano gas sensor that nano film material and micro- heating plate of low-power consumption, which are integrated,
Point.How will there is the technique of highly sensitive nano film material and the preparation micro- heating plate of low-power consumption to blend is the heat of research
Point.
Summary of the invention
Technical problem to be solved by the present invention lies in overcome nano material preparation with traditional MEMS technique incompatibility problem,
Nano sensitive material is set to position homoepitaxial under the premise of keeping higher sensitivity.Meanwhile improving gas sensor and hanging film
Thus mechanical property, and temperature control electrode is arranged provides a kind of metal-oxide gas transducer and preparation method, simplifies 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, which adopts the following technical scheme that, is achieved:
One kind being based on nano-TiO2Low-power consumption micro-nano gas sensor preparation method, include the following steps:
(1) at Si substrate front surface and the back side, thermal oxide and Low Pressure Chemical Vapor Deposition preparation SiO is respectively adopted2-Si3N4
Double-layer compound film；
(2) in positive SiO2-Si3N4On double-layer compound film, successively sunk using plasma reinforced chemical vapour deposition method
Product SiO2And Si3N4, and anneal at a certain temperature；
(3) on the insulating layer of front, by spin coating photoetching process, sensitive electrode and lead wire tray, heating electrode is 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
Then adhesive layer sputters Au layers on adhesive layer；
(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 surrounds, sensitive layer pattern is obtained by photoetching process；
(7) TiO is sputtered on sensitive layer pattern2Film defines subsequent nanorod growth position；In TiO2It is sputtered on film
Ti film, provides titanium source；
(8) TiO is prepared using hot hydrochloric acid vapour method2Nanometer rods；
(9) the identical spin coating photoetching process with step (3) is taken to obtain Si backside of substrate insulation tank, i.e. completion low-power consumption is micro-
Receive the production of gas sensor.
Further scheme in above-mentioned technique also resides in:
In the step (1), SiO2-Si3N4The middle SiO of double-layer compound film2Film thickness is 500nm, Si3N4Film
With a thickness of 150nm.
In the step (2), it is sequentially depositing SiO2With a thickness of 500nm and Si3N4With a thickness of 150nm, and 500 DEG C -600
Anneal 5-7h at DEG C.
In the step (4), sputtering Cr thickness of adhibited layer is 50nm, sputters Au layers with a thickness of 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 thickness is 300nm.
In the step (8), TiO is prepared2The method of nanometer rods is as follows:
Sputtering 8a) there is into TiO2Film, Ti film chip be placed on the chain-wales in high-pressure hydrothermal reaction kettle, by hydrochloric acid
It is added in reaction kettle with after deionized water 1:10 mixing by volume, keeps the temperature 3.5h at 150 DEG C；
8b) after cooling, chip is taken out, is successively cleaned with ethyl alcohol and deionized water and removes chip surface sundries, 100 DEG C
0.5h is dried, TiO is obtained2Nano-rod film.
In the step (9), Si backside of substrate is prepared insulation tank and is included the following steps:
9a) by photoetching process, photoresist dispels the Si at notch window by deep dry etching as masking layer3N4-
SiO2Layer removes photoresist using lift-off technique, obtains the insulated tank figure below silicon base；
9b) after chip front side spin coating photoresist, 90 DEG C of drying, PDMS is dripped dropwise in chip front side, until will be positive
Drop is full, 70 DEG C of drying 1h, on the glass sheet by chip front side patch, and chip back foreign aid is applied a circle PDMS, makes chip firmly
Patch is on the glass sheet；
It is 85 DEG C of temperature in 25% tetramethylammonium hydroxide TMAH solution that chip, which 9c) is put into togerther concentration with sheet glass,
Lower corrosion 16h forms insulation tank；PDMS is gently torn, with acetone soak, removes photoresist and remnants PDMS, 100 DEG C of drying
1h obtains sensor.
The present invention gives in turn is based on nano-TiO according to one kind of above-mentioned process production2Low-power consumption micro-nano gas
Body sensor, including Si substrate, the back side of Si substrate are provided with insulated tank, are followed successively by SiO in Si backside of substrate2Masking layer and
Si3N4Masking layer, front is by SiO2-Si3N4-SiO2-Si3N4The insulating layer that four-level membrane is combined is arranged one on insulating layer
Sensitive electrode and its lead wire tray, two pairs of heating electrodes and its lead wire tray, two pairs of thermometric electrodes and its lead wire tray, each electrode are located at
Same plane is prepared using the same technique of identical material, and sensitive material is located above the sensitive electrode of centre, and sensitive layer is by thin
Film and nanorod structure composition.
Further embodiment also resides in above structure:
The sensitive material is rectangular arrangement heart position in the sensor, leads on sensitive electrode and a pair of symmetrical is in
The electrode wires of zigzag shape, and to contact conductor disk；Sensitive electrode is interdigital structure, is come into full contact with sensitive layer, and electrode is heated
It is symmetrical in double-stranded heater strip that two pairs are led to along sensitive electrode side, and to heating element lead wire tray；Around quick
Sense electrode, temperature detecting resistance are respectively provided at both sides, and each electrode respectively has independent lead wire tray, are distributed in two sides, and sensor is all
Electrode and lead wire tray are to be centrosymmetrically arranged.
The sensitive layer is by TiO2Film and TiO2Nanometer rods two parts composition, insulating layer is by SiO2-Si3N4-SiO2-
Si3N4Four-level membrane is combined, and masking layer is by SiO2-Si3N4Bilayer film is combined.Sensitive electrode, heating electrode, thermometric
Resistance and each lead wire tray are made of Cr-Au film.
Compared with prior art, the invention has the following advantages that
1, pass through sputtering TiO2The source Ti is oxidized to TiO by film, Ti film, hot hydrochloric acid vapour method2Nanometer rods preparation is sensitive
Layer, makes TiO2Nanorod growth is in TiO2On film.Compared with simple sputtered film, the specific surface area of sensitive material is increased, is made
Have better gas response characteristic；With grow TiO on the 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, right with controllability
For mass production, it is able to maintain consistency.
2, insulating layer is from bottom to top by SiO2-Si3N4-SiO2-Si3N4Four-level membrane composition, after wet etching insulated tank at
To hang film.First layer SiO is prepared by thermal oxidation method2, the intrinsic stress due to binding directly generation is reduced, as Si and Si3N4
Between buffer layer, recycle PECVD deposit SiO2、Si3N4On the one hand layer utilizes PECVD method deposition film high mechanical strength
The advantages of, increase outstanding film strength.On the other hand, four layers of successively staggered film inhibit the generation of stress between four-level membrane, and
The residual stress between four-level membrane is greatly eliminated using annealing.Such method optimizes the mechanical performance of outstanding film.
3, it is provided with centrosymmetric temperature element, determines the temperature of sensitizing range by measuring the resistance value of temperature detecting resistance
Degree, come accurately temperature controls when obtaining working sensor.
4, heating element, sensing element, temperature element are arranged in same layer, are once splashed to each figure using identical material
In shape, process has been simplified, has avoided the generation of parasitic fields.
5, gas sensor size of the invention is only 2 × 2mm, reduces heat by Si substrate back wet etching insulated tank
Transmitting, by can achieve extremely low power when conducting self-heating heated by electrodes, meets present market to the need of low-power consumption sensor
It asks.
Detailed description of the invention
Fig. 1 is the cross-sectional view of the 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 defining
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；3, Si substrate；4,SiO2Insulating layer I； 5,Si3N4Insulating layer I；
6、SiO2Insulating layer II；7,Si3N4Insulating layer II；8, Cr-Au heats electrode； 9,TiO2Nano thin-film；10,TiO2Nanometer rods；
11, Cr-Au sensitive electrode；12, lead wire tray；13, insulated tank；14, thermometric electrode；15, 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 invention any limit
The foundation of system.
(a), (b) are shown as shown in Figure 1, Figure 2, and the present invention is based on nano-TiOs2Low-power consumption micro-nano gas sensor, including Si
Substrate 3, the back side of Si substrate 3 are provided with insulated tank 13, are followed successively by SiO at 3 back side of Si substrate2Masking layer 2 and Si3N4Masking layer 1,
Front is by SiO2I 4-Si of insulating layer3N4I 5-SiO of insulating layer2II 6-Si of insulating layer3N4II 7 four-level membrane of insulating layer is combined
Insulating layer, be arranged on insulating layer 12, two couples of Cr-Au of a pair of Cr-Au sensitive electrode 11 and its lead wire tray heat electrodes 8 and its
12, two pairs of thermometric electrodes 14 of lead wire tray and its lead wire tray 12, each electrode are generally aligned in the same plane, using the same technique system of identical material
Standby, sensitive material 15 is located above the sensitive electrode of centre, and sensitive layer is by TiO2Nano thin-film 9 and TiO210 structure of nanometer rods
Composition.
As shown in Fig. 2 (a), (b), sensitive material 15 is rectangular arrangement heart position in the sensor, Cr-Au sensitive electrode
Lead to a pair of symmetrical helically linear electrode wires on 11, and to contact conductor disk；Cr-Au sensitive electrode 11 is fork
Refer to structure, come into full contact with sensitive layer, Cr-Au heat electrode 8 along 11 side of Cr-Au sensitive electrode lead to two pairs it is symmetrical
In double-stranded heater strip, and to heating element lead wire tray；Around Cr-Au sensitive electrode 11, thermometric electrode 14 is set respectively
Set in two sides, each electrode respectively has independent lead wire tray, be distributed in two sides, all electrodes of sensor and lead wire tray it is equal centered on it is right
Claim arrangement.
Sensitive layer is by TiO2Film 9 and TiO210 two parts of nanometer rods composition, insulating layer and masking layer are by SiO2-Si3N4It is double
Layer film is combined；Sensitive electrode, heating electrode and temperature detecting resistance and each lead wire tray are made of Cr-Au film.
Referring to Fig. 2 (a), heater strip and sensitive electrode are central symmetry, spiral way arrangement, and sensitive electrode is heated silk
It surrounds, sensitive material is in above sensitive electrode.Referring to Fig. 2 (b), a pair of of Cr-Au heater strip inner ring is having a size of 145 μ m, 240 μ
M, heater strip width are 12 μm, and gap is 40 μm.Cr-Au sensitive electrode, electrode width are 15 μm, and gap is 10 μm, such as Fig. 2 (b)
Shown, sensitive material is located in 14 region of wire frame, above sensitive electrode, having a size of 100 μm of 100 μ m.
As shown in Fig. 3 (a), (b), nanorod growth is in the TiO defined2On film, bridges and is connected between nanometer rods,
Form the nano-rod film with high specific surface area.
Referring to Fig. 4, low-power consumption metal-oxide gas transducer of the invention the preparation method is as follows:
Embodiment 1
(1) as shown in Fig. 4 (a), at Si substrate front surface 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 wafer2Layer, (low pressure chemical phase is heavy by two-sided LPCVD
Form sediment) deposition 150nm Si3N4。
(2) as shown in Fig. 4 (b), in positive SiO2-Si3N4On double-layer compound film, front is successively sunk using PECVD
Product 500nm SiO2、150nm Si3N4, anneal at 500 DEG C 7h.
(3) as shown in Fig. 4 (c), on the insulating layer of front, by spin coating photoetching process obtain sensitive electrode and lead wire tray,
The figure of electrode and lead wire tray, thermometric electrode and lead wire tray is heated, photoresist uses positive photoresist EPG535.
(4) as shown in Fig. 4 (d), the sputtering Cr bonding on heating electrode and lead wire tray and sensitive electrode and lead wire tray figure
Then layer sputters Au layers on adhesive layer；50nm Cr, 250nm Au are successively sputtered using sputter.
(5) such as Fig. 4 (e), each electrode and lead wire tray are obtained using lift-off (removing) technique removal photoresist, 300 DEG C
Lower annealing 10min.
(6) as shown in Fig. 4 (f), on the rectangular area that sensitive electrode surrounds, the identical spin coating light with step (3) is taken
Carving technology obtains sensitive material pattern.
(7) TiO is sputtered on sensitive layer pattern2Film defines subsequent nanorod growth position；In TiO2It is sputtered on film
Ti film, provides titanium source；30nm TiO is successively sputtered using sputter2, 300nm Ti, as shown in Fig. 4 (g).
(8) TiO is prepared using hot hydrochloric acid vapour method2Nanometer rods；Photoresist is removed using lift-off technique, obtains sensitivity
Patterns of material such as Fig. 4 (h).
Sputtering there is into TiO2Film, Ti film chip as the chain-wales in high-pressure hydrothermal reaction kettle on, by hydrochloric acid and
1:10 is mixed deionized water by volume, is added in reaction kettle, is put into drying oven and keeps the temperature 3.5h at 150 DEG C.After cooling,
Reaction kettle is taken out from drying oven, takes out chip immediately, with ethyl alcohol, deionized water clean the surface sundries according to this, 100 DEG C of drying
0.5h obtains TiO2Nano-rod film.As shown in Fig. 4 (i).
(9) the identical spin coating photoetching process with step (3) is taken to obtain back side notch window pattern, such as Fig. 4 (j).
(9a) photoresist dispels the Si at notch window by deep dry etching as masking layer3N4-SiO2Layer, when etching
Between 13min.Photoresist is removed using lift-off technique, obtains window such as Fig. 4 (k).
(9b) drips PDMS after chip front side spin coating photoresist, 90 DEG C of drying in chip front side dropwise, until will be positive
Drop is full, 70 DEG C of drying 1h, as shown in Fig. 4 (l), on the glass sheet by chip front side patch, and chip back foreign aid is applied a circle
PDMS pastes chip firmly on the glass sheet.
Chip is put into togerther in TMAH (concentration is 25% tetramethylammonium hydroxide) solution by (9c) with sheet glass, and 85 DEG C,
Corrode 16h and forms insulation tank.PDMS is gently torn, with acetone soak, removes photoresist and remnants PDMS, 100 DEG C of drying 1h,
Obtain sensor such as Fig. 4 (m).
Embodiment 2
(1) at Si substrate front surface and the back side, thermal oxide and Low Pressure Chemical Vapor Deposition preparation SiO is respectively adopted2-
Si3N4Double-layer compound film；The two-sided thermal oxide 500nm SiO of silicon wafer2Layer, two-sided LPCVD (low pressure chemical phase precipitating) deposition
150nm Si3N4。
(2) in positive SiO2-Si3N4On double-layer compound film, front is sequentially depositing 500nm SiO using PECVD2、
150nm Si3N4, anneal at 600 DEG C 5h.
(3) on the insulating layer 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 use positive photoresist EPG535.
(4) Cr adhesive layer is sputtered on heating electrode and lead wire tray and sensitive electrode and lead wire tray figure, is then being bonded
Au layers are sputtered on layer；50nm Cr, 250nm Au are successively sputtered using sputter.
(5) photoresist is removed using lift-off (removing) technique, obtains each electrode and lead wire tray, anneals at 260 DEG C
30min。
(6) on the rectangular area that sensitive electrode surrounds, the identical spin coating photoetching process with step (3) is taken to obtain sensitivity
Patterns of material.
(7) TiO is sputtered on sensitive layer pattern2Film defines subsequent nanorod growth position；In TiO2It is sputtered on film
Ti film, provides titanium source；30nm TiO is successively sputtered using sputter2、300nm Ti。
(8) TiO is prepared using hot hydrochloric acid vapour method2Nanometer rods；Photoresist is removed using lift-off technique, obtains sensitivity
Patterns of material.
Sputtering there is into TiO2Film, Ti film chip as the chain-wales in high-pressure hydrothermal reaction kettle on, by hydrochloric acid and
1:10 is mixed deionized water by volume, is added in reaction kettle, is put into drying oven and keeps the temperature 3.5h at 150 DEG C.After cooling,
Reaction kettle is taken out from drying oven, takes out chip immediately, with ethyl alcohol, deionized water clean the surface sundries according to this, 100 DEG C of drying
0.5h obtains TiO2Nano-rod film.
(9) the identical spin coating photoetching process with step (3) is taken to obtain back side notch window pattern.
(9a) photoresist dispels the Si at notch window by deep dry etching as masking layer3N4-SiO2Layer, when etching
Between 13min.Photoresist is removed using lift-off technique, obtains window.
(9b) drips PDMS after chip front side spin coating photoresist, 90 DEG C of drying in chip front side dropwise, until will be positive
Drop is full, 70 DEG C of drying 1h, on the glass sheet by chip front side patch, and chip back foreign aid is applied a circle PDMS, makes chip firmly
Patch is on the glass sheet.
Chip is put into togerther in TMAH (concentration is 25% tetramethylammonium hydroxide) solution by (9c) with sheet glass, and 85 DEG C,
Corrode 16h and forms insulation tank.PDMS is gently torn, with acetone soak, removes photoresist and remnants PDMS, 100 DEG C of drying 1h,
Obtain sensor.
The present invention is not limited to the above embodiments, on the basis of technical solution disclosed by the invention, the skill of this field
For art personnel according to disclosed technology contents, one can be made to some of which technical characteristic by not needing creative labor
A little replacements and deformation, these replacements and deformation are within the scope of the invention.
Claims (8)
1. one kind is based on nano-TiO2Low-power consumption micro-nano gas sensor preparation method, which is characterized in that including following steps
It is rapid:
(1) at Si substrate front surface and the back side, thermal oxide and Low Pressure Chemical Vapor Deposition preparation SiO is respectively adopted2-Si3N4It is double-deck
Laminated film constitutes masking layer；
(2) in positive SiO2-Si3N4On double-layer compound film, it is sequentially depositing using plasma reinforced chemical vapour deposition method
SiO2And Si3N4, form SiO2-Si3N4-SiO2-Si3N4Four layers of laminated film constitute insulating layer, and move back at a certain temperature
Fire；
(3) on the insulating layer of front, by spin coating photoetching process, sensitive electrode and lead wire tray, heating electrode and lead wire tray are obtained
With the figure of thermometric electrode and lead wire tray；
(4) the sputtering Cr bonding on heating electrode and lead wire tray, sensitive electrode and lead wire tray and thermometric electrode and lead wire tray figure
Then layer sputters Au layers on adhesive layer；
(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 it is made annealing treatment；
(6) on the rectangular area that sensitive electrode surrounds, sensitive layer pattern is obtained by photoetching process；
(7) TiO is sputtered on sensitive layer pattern2Film defines subsequent nanorod growth position；In TiO2It is thin that Ti is sputtered on film
Film provides titanium source；
(8) TiO is prepared using hot hydrochloric acid vapour method2Nanometer rods constitute sensitive layer；
(9) the identical spin coating photoetching process with step (3) is taken to obtain Si backside of substrate insulation tank, i.e. completion low-power consumption micro-nano gas
The production of body sensor；
In the step (1), SiO2-Si3N4The middle SiO of double-layer compound film2Film thickness is 500nm, Si3N4Film thickness is
150nm；
In the step (2), it is sequentially depositing SiO2With a thickness of 500nm and Si3N4With a thickness of 150nm, and at 500 DEG C -600 DEG C
Anneal 5-7h；
In the step (5), anneal 10-30min at a temperature of 260 DEG C-300 DEG C.
2. according to claim 1 be based on nano-TiO2Low-power consumption micro-nano gas sensor preparation method, feature exists
In in the step (4), sputtering Cr thickness of adhibited layer is 50nm, sputters Au layers with a thickness of 250nm.
3. according to claim 1 be based on nano-TiO2Low-power consumption micro-nano gas sensor preparation method, feature exists
In, in the step (7), sputtering TiO2Film thickness is 30nm；Sputtering Ti film thickness is 300nm.
4. according to claim 1 be based on nano-TiO2Low-power consumption micro-nano gas sensor preparation method, feature exists
In, in the step (8), preparation TiO2The method of nanometer rods is as follows:
Sputtering 8a) there is into TiO2Film, Ti film chip be placed on the chain-wales in high-pressure hydrothermal reaction kettle, hydrochloric acid and will go
It is added in reaction kettle after ionized water 1:10 mixing by volume, keeps the temperature 3.5h at 150 DEG C；
8b) after cooling, chip is taken out, successively cleans removal chip surface sundries, 100 DEG C of drying with ethyl alcohol and deionized water
0.5h obtains TiO2Nano-rod film.
5. according to claim 1 be based on nano-TiO2Low-power consumption micro-nano gas sensor preparation method, feature exists
In in the step (9), Si backside of substrate is prepared insulation tank and included the following steps:
9a) by photoetching process, photoresist dispels the Si at notch window by deep dry etching as masking layer3N4-SiO2
Layer removes photoresist using lift-off technique, obtains the insulated tank figure below silicon base；
9b) after chip front side spin coating photoresist, 90 DEG C of drying, PDMS is dripped dropwise in chip front side, until front drop is full,
Chip back foreign aid on the glass sheet by chip front side patch, and is applied a circle PDMS, chip is made firmly to be attached to glass by 70 DEG C of drying 1h
Glass on piece；
It is corruption at a temperature of 85 DEG C in 25% tetramethylammonium hydroxide TMAH solution that chip, which 9c) is put into togerther concentration with sheet glass,
It loses 16h and forms insulation tank；PDMS is gently torn, with acetone soak, removes photoresist and remnants PDMS, 100 DEG C of drying 1h are obtained
To sensor.
6. a kind of claim 1-5 is described in any item to be based on nano-TiO2Low-power consumption micro-nano gas sensor, feature exists
In, including Si substrate, the back side of Si substrate is provided with insulated tank, is followed successively by SiO in Si backside of substrate2Masking layer and Si3N4Masking
Layer, front is by SiO2-Si3N4-SiO2-Si3N4A pair of of sensitive electrical is arranged on insulating layer for the insulating layer that four-level membrane is combined
Pole and its lead wire tray, two pairs of heating electrodes and its lead wire tray, two pairs of thermometric electrodes and its lead wire tray, each electrode are located at same flat
Face is prepared using the same technique of identical material, and sensitive material is located above the sensitive electrode of centre, and sensitive layer is by film and receives
Rice stick structure composition.
7. according to claim 6 a kind of based on nano-TiO2Low-power consumption micro-nano gas sensor, which is characterized in that institute
Stating sensitive material is rectangular arrangement heart position in the sensor, and a pair of symmetrical helically threadiness is led on sensitive electrode
Electrode wires, and to contact conductor disk；Sensitive electrode is interdigital structure, is come into full contact with sensitive layer, heats electrode along sensitive electrode
It is symmetrical in double-stranded heater strip that side leads to two pairs, and to heating element 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 two sides, all electrodes of sensor and lead wire tray
It is to be centrosymmetrically arranged.
8. according to claim 6 a kind of based on nano-TiO2Low-power consumption micro-nano gas sensor, which is characterized in that institute
Sensitive layer is stated by TiO2Film and TiO2Nanometer rods two parts composition, insulating layer is by SiO2-Si3N4-SiO2-Si3N4Four-level membrane is multiple
It closes, masking layer is by SiO2-Si3N4Bilayer film is combined；Sensitive electrode, heating electrode and temperature detecting resistance and each lead
Disk is made of Cr-Au film.
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| CN113405685B (en) * | 2021-05-17 | 2022-12-16 | 清华大学 | Temperature sensor based on PEDOT-ZnO nano heterojunction and preparation method thereof |
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