CN108375498A - Integrated device of gas concentration sensing and preparation method thereof - Google Patents
Integrated device of gas concentration sensing and preparation method thereof Download PDFInfo
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- CN108375498A CN108375498A CN201810120026.8A CN201810120026A CN108375498A CN 108375498 A CN108375498 A CN 108375498A CN 201810120026 A CN201810120026 A CN 201810120026A CN 108375498 A CN108375498 A CN 108375498A
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Abstract
The invention discloses a kind of gas concentrations to sense integrated device and preparation method thereof.Integrated device is metal-oxide gas transducer, annular insulating layer, annular platinum micro-heater, annular insulating layer and the annular gas inspissator that surface is covered with the connection electrode being equipped with successively on the silicon chip of mesoporous thermal insulation layer, wherein, width≤1 μm of annular platinum micro-heater, 200 500nm of thickness, electrode respectively with platinum micro-heater and power electric connection；Method is repeatedly in applying electron sensitive resist on the silicon chip that surface is covered with mesoporous thermal insulation layer, by electron beam exposure method depict the figure of corresponding device on electron sensitive resist, after being sputtered on figure or corresponding device is deposited out, in growth gasses inspissator on annular insulating layer, purpose product is made.It has a compact-sized, small power consumption, the advantage that detectable limit is high, real-time and convenient, is extremely easy to be widely used in the high sensitivity detection to gas, makes it wearable or can be embedded in the fields such as intelligent terminal and have a wide range of applications.
Description
Technical field
The present invention relates to a kind of integrated device and preparation method, especially a kind of gas concentration sensing one device and its system
Preparation Method.
Background technology
Trace gas in indoor and outdoor surroundings carries environment and the relevant important information of health, and research and development are wearable or can be embedding
Frontier development in the Internet of things era is had wide market to answer by the micro semiconductor gas sensor for entering intelligent terminal
Use foreground.In the recent period, people are in order to further promote the detection limit of oxide semiconductor gas sensor, effectively to promote it
Application in the fields such as trace contamination gas, breathing gas detection, has made some good tries and effort, such as entitled
“UItratrace Measurement of Acetone from Skin Using Zeol ite:Toward
Development of a Wearable Monitor of Fat Metabol ism ", Analytical Chemistry, 87
(2015) 7588-7594 (" uses the trace acetone of zeolite detection skin release：Develop wearable fat metabolism monitoring sensing
Device ",《Analytical chemistry》2015 the 7588-7594 pages of volume 87) article.The monitoring sensor referred in this article is vial
In be equipped with acetone sensor and its side be arranged the outer gas concentrator for twining platinum heating wire, wherein acetone sensor and platinum electricity
The both ends of heated filament are respectively connected with electrode, and gas concentrator is zeolite, and electrode is connect with the power supply outside bottle；When measurement, first make glass
Bottleneck covers skin area to be measured for a period of time, so that zeolite fully adsorbs the acetone molecules in area to be measured, then passes through platinum electric heating
Silk heating zeolite, makes the acetone molecules being enriched on zeolite rapidly be desorbed, and be spread in the surface of acetone sensor, reaches promotion
Acetone sensor detects the purpose of limit.Though this monitoring sensor can be used for the detection of trace acetone gas, but also there is not
Foot place, first, bulky, the volume for placing the vial of a whole set of concentration measurement device is up to 16.9ml, can not be integrated into
The intelligent terminals such as mobile phone；Next, acetone sensor farther out, is centimetres, seriously weakens at a distance from gas concentrator
The concentrated effect of gas concentrator；Again, the volume of the platinum heating wire of heating zeolite gas concentrator is excessive --- and 300 × 300
×500μm3, the power consumption for not only resulting in platinum heating wire is larger, also causes the thermal relaxation time of acetone sensor and gas concentrator
It is longer, it is unfavorable for carrying out quick sampling test.
Invention content
The technical problem to be solved in the present invention is to overcome shortcoming in the prior art, provides a kind of compact-sized, work(
Consume small, the detection easily integrated device of gas concentration sensing.
The invention solves another technical problem be that a kind of preparation of the integrated device of above-mentioned gas concentration sensing is provided
Method.
To solve the technical problem of the present invention, used technical solution is that the integrated device of gas concentration sensing is by positioning
Gas sensor, gas concentrator, electric heater and electrode in shell form, and the power supply being connect with electrode, especially：
The positioning shell is the silicon chip that surface is covered with mesoporous thermal insulation layer；
The gas sensor is metal-oxide gas transducer, and the metal-oxide gas transducer invests described
Surface is covered on the silicon chip of mesoporous thermal insulation layer；
The gas concentrator is annular, and the annular gas inspissator invests the metal-oxide gas transducer
Periphery；
The electric heater is wide≤1 μm, platinum (Pt) micro-heater of thickness 200-500nm, and the platinum micro-heater is located at institute
It states under annular gas inspissator；
Between the platinum micro-heater and the periphery of metal-oxide gas transducer between annular gas inspissator
It is equipped with annular insulating layer；
The electrode is electrically connected with metal-oxide gas transducer, platinum micro-heater respectively.
Being further improved for integrated device is sensed as gas concentration：
Preferably, a length of 3-5 μm of metal-oxide gas transducer, width be 0.3-1.5 μm, thickness 100-200nm,
In metal oxide be stannic oxide (SnO2) or indium oxide (In2O3) or gallium oxide (Ga2O3) or tungstic acid
(WO3) or molybdenum trioxide (MoO3) or copper oxide (CuO) or nickel oxide (NiO) or chromium oxide (Cr2O3)。
Preferably, annular gas inspissator is annular shape, and concentrically with metal-oxide gas transducer, and its inner ring
Radius is 4-6 μm, outer shroud radius is 8-12 μm, thickness 500-1000nm, and the material of annular gas inspissator is organic mesoporous material
Material or inorganic mesoporous material or oxidate nano linear array.
Preferably, thickness >=80nm of annular insulating layer, for annular silicon dioxide insulating layer, or annular alumina insulation
Layer, or annular zirconium dioxide insulating layer.
To solve another technical problem of the present invention, another used technical solution is that above-mentioned gas concentration passes
The preparation method of the integrated device of sense includes that electron beam exposure method, especially key step are as follows：
Step 1, it is covered with prior to surface after applying electron sensitive resist on the silicon chip of mesoporous thermal insulation layer, passes through electron beam exposure
Method depicts sensor pattern on it, and sputtering metal oxide gas using magnetron sputtering method in sensor pattern passes
After sensor, places it in and remove electron sensitive resist in dimethyl formamide solution, be covered with metal oxide gas thereon
The surface of sensor is covered with the silicon chip of mesoporous thermal insulation layer；
Step 2, the first surface for being covered with metal-oxide gas transducer thereon, which is covered on the silicon chip of mesoporous thermal insulation layer, applies
After applying electron sensitive resist, electrode pattern is depicted at the both ends of metal-oxide gas transducer by electron beam exposure method,
It after electrode evaporation on electrode pattern, places it in and removes electron sensitive resist in dimethyl formamide solution, obtain thereon
The surface for being covered with the metal-oxide gas transducer of connection electrode is covered with the silicon chip of mesoporous thermal insulation layer；
Step 3, the surface for the metal-oxide gas transducer for being first covered with connection electrode thereon is covered with mesoporous thermal insulation layer
Silicon chip on coating electron sensitive resist after, depicted on the periphery of metal-oxide gas transducer by electron beam exposure method
Annular places it in after sputtering insulating layer using magnetron sputtering method in annular and removes electronics in dimethyl formamide solution
Beam resist, the surface for obtaining the metal-oxide gas transducer for being covered with connection electrode successively thereon and annular insulating layer are covered with
The silicon chip of mesoporous thermal insulation layer；
Step 4, first it is covered with the table of the metal-oxide gas transducer and annular insulating layer of connection electrode successively thereon
Face is covered on the silicon chip of mesoporous thermal insulation layer after coating electron sensitive resist, is portrayed at annular insulating layer by electron beam exposure method
Go out platinum micro-heater figure, after platinum micro-heater is deposited on platinum micro-heater figure, it is molten to place it in dimethylformamide
Electron sensitive resist is removed in liquid, obtains being covered with the metal-oxide gas transducer of connection electrode, annular insulation successively thereon
The surface of layer and annular platinum micro-heater is covered with the silicon chip of mesoporous thermal insulation layer；
Step 5, the metal-oxide gas transducer, annular insulating layer and annular of connection electrode are first covered with successively thereon
The surface of platinum micro-heater is covered on the silicon chip of mesoporous thermal insulation layer after coating electron sensitive resist, by electron beam exposure method in ring
Depict annular at shape platinum micro-heater, in annular using magnetron sputtering method sputtering insulating layer after, growth gasses thereon
Inspissator then places it in and removes electron sensitive resist in dimethyl formamide solution, and gas concentration is made and senses integrated device
Part.
Being further improved for the preparation method of integrated device is sensed as gas concentration：
Preferably, electron sensitive resist is ZEP 520A electron sensitive resists or polymethyl methacrylate (PMMA) electricity
Beamlet resist.
Preferably, it is 80- that sputtering power when magnetron sputtering method sputtered metal oxide gas sensor is used in step 1
120W, sputtering time 10-60min, a length of 3-5 μm of metal-oxide gas transducer, width be 0.3-1.5 μm, thickness is
100-200nm, metal oxide therein are stannic oxide (SnO2) or indium oxide (In2O3) or gallium oxide (Ga2O3), or
Tungstic acid (WO3) or molybdenum trioxide (MoO3) or copper oxide (CuO) or nickel oxide (NiO) or chromium oxide (Cr2O3)。
Preferably, the vapor deposition of electrode and platinized platinum is magnetron sputtering or d.c. sputtering or electron beam evaporation.
Preferably, thickness >=80nm of annular insulating layer, for annular silicon dioxide insulating layer, or annular alumina insulation
Layer, or annular zirconium dioxide insulating layer.
Preferably, the growth course of gas concentrator is, first to being covered with the metal oxide gas of connection electrode successively thereon
Body sensor, annular insulating layer, annular platinum micro-heater and the surface of annular insulating layer and electron sensitive resist are covered with mesoporous
The silicon chip of thermal insulation layer carries out oxygen plasma cleaning, then is dipped in the zinc nitrate methanol solution and 35- of 15-25mmol/L
20-40min is stood in the mixed solution of the 2-methylimidazole methanol solution of 45mmol/L, obtains point being located on annular insulating layer
Son sieve inspissator；Wherein, oxygen plasma clean when radio-frequency power be 80-120W, oxygen pressure be 0.5-1.5Torr, cleaning when
Between for >=20s, the volume ratio of zinc nitrate methanol solution and 2-methylimidazole methanol solution is 0.8-1.2 in mixed solution：0.8-
1.2。
Preferably, the growth course of gas concentrator is first to be covered with the metal oxide gas of connection electrode successively thereon
Body sensor, annular insulating layer, annular platinum micro-heater and the surface of annular insulating layer and electron sensitive resist are covered with mesoporous
The zinc oxide seed layer that thickness is 1-20nm is sputtered on the silicon chip of thermal insulation layer, reuses solwution method in being grown in zinc oxide seed layer
Zinc oxide nano-wire array；Wherein, it is 0.8-1.2 that the precursor solution in solwution method, which is volume ratio,：The 0.4- of 0.8-1.2
Zinc nitrate (Zn (the NO of 0.6mmol/L3)2) solution and 0.4-0.6mmol/L hexamethylene tetraammonia solution mixed solution, it is raw
Temperature when long is 90-100 DEG C, time 1-3h.
Advantageous effect compared with the existing technology is：
First, after using such cramped construction, the present invention both has planar dimension≤(100 × 100) μm2, it is thick≤5 μm
Advantage, so that it is extremely easy to meet integrated and wearable sensors part the requirement of chip；Again because metal oxide gas senses
The peripheral ring of device is around annular gas inspissator, and the space length of the two is very small, and only≤10 μm, pole is conducive to annular gas
The gas molecule being enriched on inspissator keeps the molecule for diffusing into metal-oxide gas transducer region logical when heating desorption
Amount is in maximum, has fully played effect of the gas concentrator in terms of trace gas molecules enrichment；Due also to silicon chip
The mesoporous thermal insulation layer that surface is covered with, and the size of each device and spacing that are arranged thereon are smaller, to not only greatly drop
The low size and power consumption of platinum micro-heater, extremely shortens the heat of metal-oxide gas transducer and gas concentrator
Relaxation time --- it is only Millisecond, pole is conducive to the present invention and carries out rapidly sampling test；More because of organic mesoporous material or inorganic
Mesoporous material or oxidate nano linear array can be used as the material of gas concentrator, in conjunction with to applicable metal oxide gas
The selection of body sensor makes the specific aim of detection gas type of the present invention obtain great promotion.
Second, preparation method science, efficiently.Compact-sized, small power consumption is not only made, easily purpose is produced for detection
Object --- the integrated device of gas concentration sensing；Also there is it high to the detectable limit of gas, real-time and convenient；In turn
So that purpose product is extremely easy to be widely used in high sensitivity detection to gas, makes it wearable or intelligent terminal can be embedded in
Equal fields have a wide range of applications.
Description of the drawings
Fig. 1 is a kind of scanning electron microscope (SEM) image of basic structure of the present invention.
Fig. 2 is to use 4200 characteristic of semiconductor analysis system of Keithley (Keithley) to the platinum micro-heater in the present invention
One of the result characterized with scanning electron microscope.Wherein, a figures in Fig. 2 are to analyze to be using 4200 characteristic of semiconductor of Keithley
The result figure of unified test examination, since the resistance of platinum micro-heater is increased with temperature and increases, and can pass through the temperature-coefficient of electrical resistance of platinum
0.003K-1The temperature for estimating micro-heater under different input power, the temperature of the micro-heater provided by secondary coordinate it is found that
Platinum micro-heater highest can be heated to 500 DEG C, when its input power is 23mW, can be heated to 300 DEG C；B schemes and c figure difference
It is heated to the SEM image before and after 500 DEG C for platinum micro-heater, can be seen that by it, the platinum micro-heater after hot operation is without apparent
Degeneration.
Specific implementation mode
The preferred embodiment of the present invention is described in further detail below in conjunction with the accompanying drawings.
It buys from market or is voluntarily made first：
ZEP 520A electron sensitive resists and polymethyl methacrylate electron sensitive resist as electron sensitive resist；
As the stannic oxide of metal oxide, indium oxide, gallium oxide, tungstic acid, molybdenum trioxide, copper oxide, oxidation
Nickel and chromium oxide；
Silica, aluminium oxide and zirconium dioxide as annular insulating layer material；
Organic mesoporous material, inorganic mesoporous material and the oxidate nano linear array of material as gas concentrator.
Wherein：
The growth course of molecular sieve inspissator is, first to being covered with the metal oxide gas of connection electrode successively thereon
Sensor, annular insulating layer, annular platinum micro-heater and the surface of annular insulating layer and electron sensitive resist be covered with it is mesoporous every
The silicon chip of thermosphere carries out oxygen plasma cleaning, then is dipped in the zinc nitrate methanol solution and 35- of 15-25mmol/L
20-40min is stood in the mixed solution of the 2-methylimidazole methanol solution of 45mmol/L, obtains point being located on annular insulating layer
Son sieve inspissator；Wherein, oxygen plasma clean when radio-frequency power be 80-120W, oxygen pressure be 0.5-1.5Torr, cleaning when
Between for >=20s, the volume ratio of zinc nitrate methanol solution and 2-methylimidazole methanol solution is 0.8-1.2 in mixed solution：0.8-
1.2。
The growth course of zinc oxide nano-wire array gas concentrator is first to be covered with the metal of connection electrode successively thereon
The surface of oxide gas sensor, annular insulating layer, annular platinum micro-heater and annular insulating layer and electron sensitive resist
It is covered with the zinc oxide seed layer for sputtering that thickness is 1-20nm on the silicon chip of mesoporous thermal insulation layer, reuses solwution method in zinc oxide seed
Growth of zinc oxide nano linear array on layer；Wherein, it is 0.8-1.2 that the precursor solution in solwution method, which is volume ratio,：0.8-1.2's
The mixed solution of the zinc nitrate solution of 0.4-0.6mmol/L and the hexamethylene tetraammonia solution of 0.4-0.6mmol/L, when growth
Temperature is 90-100 DEG C, time 1-3h.
Then：
Embodiment 1
Prepare the specific steps are：
Step 1, it is covered with prior to surface after applying electron sensitive resist on the silicon chip of mesoporous thermal insulation layer, passes through electron beam exposure
The sensor pattern that method depicts a length of 3 μm on it, width is 1.5 μm；Wherein, electron sensitive resist is ZEP 520A electron beams
Resist.After sputtering metal-oxide gas transducer using magnetron sputtering method in sensor pattern, two are placed it in
Electron sensitive resist is removed in methylformamide solution, the surface for being covered with metal-oxide gas transducer thereon is covered with Jie
The silicon chip of hole thermal insulation layer；Sputtering power when wherein, using magnetron sputtering method sputtered metal oxide gas sensor be 80W,
Sputtering time is 60min, and the thickness of metal-oxide gas transducer is 200nm, and metal oxide therein is stannic oxide.
Step 2, the first surface for being covered with metal-oxide gas transducer thereon, which is covered on the silicon chip of mesoporous thermal insulation layer, applies
After applying electron sensitive resist, electrode pattern is depicted at the both ends of metal-oxide gas transducer by electron beam exposure method；
Wherein, electron sensitive resist is ZEP 520A electron sensitive resists.After electrode evaporation on electrode pattern, diformazan is placed it in
Electron sensitive resist is removed in base formamide solution, is covered with the table of the metal-oxide gas transducer of connection electrode thereon
Face is covered with the silicon chip of mesoporous thermal insulation layer；Wherein, it is deposited as electron beam evaporation.
Step 3, the surface for the metal-oxide gas transducer for being first covered with connection electrode thereon is covered with mesoporous thermal insulation layer
Silicon chip on coating electron sensitive resist after, depicted on the periphery of metal-oxide gas transducer by electron beam exposure method
Annular.After the insulating layer for sputtering 80nm thickness using magnetron sputtering method in annular, place it in dimethyl formamide solution
Electron sensitive resist is removed, the metal-oxide gas transducer for being covered with connection electrode successively thereon and annular insulating layer are obtained
Surface is covered with the silicon chip of mesoporous thermal insulation layer；Wherein, the material of annular insulating layer is silica.
Step 4, first it is covered with the table of the metal-oxide gas transducer and annular insulating layer of connection electrode successively thereon
Face is covered on the silicon chip of mesoporous thermal insulation layer after coating electron sensitive resist, is portrayed at annular insulating layer by electron beam exposure method
Go out wide 0.2 μm of platinum micro-heater figure；Wherein, electron sensitive resist is ZEP 520A electron sensitive resists.Then at platinum it is micro- plus
After the platinum micro-heater of thickness 500nm is deposited on hot device figure, it is against corrosion to place it in stripping electron beam in dimethyl formamide solution
Agent obtains being covered with the metal-oxide gas transducer of connection electrode, annular insulating layer and annular platinum micro-heater successively thereon
Surface be covered with the silicon chip of mesoporous thermal insulation layer；Wherein, it is deposited as electron beam evaporation.
Step 5, the metal-oxide gas transducer, annular insulating layer and annular of connection electrode are first covered with successively thereon
The surface of platinum micro-heater is covered on the silicon chip of mesoporous thermal insulation layer after coating electron sensitive resist, by electron beam exposure method in ring
Annular is depicted at shape platinum micro-heater；Wherein, electron sensitive resist is ZEP 520A electron sensitive resists.Make in annular
After the insulating layer for sputtering 80nm thickness with magnetron sputtering method, growth inner ring radius is 4 μm thereon, outer shroud radius is 12 μm, thickness is
The gas concentrator of 500nm；Wherein, the material of annular insulating layer is silica, and gas concentrator is zinc-oxide nano linear array
Row gas concentrator.Then, it places it in and removes electron sensitive resist in dimethyl formamide solution, be made and be similar to Fig. 1 institutes
The integrated device of gas concentration sensing shown.
Embodiment 2
Prepare the specific steps are：
Step 1, it is covered with prior to surface after applying electron sensitive resist on the silicon chip of mesoporous thermal insulation layer, passes through electron beam exposure
The sensor pattern that method depicts a length of 3.5 μm on it, width is 1.2 μm；Wherein, electron sensitive resist is ZEP 520A electronics
Beam resist.After sputtering metal-oxide gas transducer using magnetron sputtering method in sensor pattern, place it in
Electron sensitive resist is removed in dimethyl formamide solution, the surface for being covered with metal-oxide gas transducer thereon is covered with
The silicon chip of mesoporous thermal insulation layer；Sputtering power when wherein, using magnetron sputtering method sputtered metal oxide gas sensor is
The thickness of 90W, sputtering time 48min, metal-oxide gas transducer are 175nm, and metal oxide therein is titanium dioxide
Tin.
Step 2, the first surface for being covered with metal-oxide gas transducer thereon, which is covered on the silicon chip of mesoporous thermal insulation layer, applies
After applying electron sensitive resist, electrode pattern is depicted at the both ends of metal-oxide gas transducer by electron beam exposure method；
Wherein, electron sensitive resist is ZEP 520A electron sensitive resists.After electrode evaporation on electrode pattern, diformazan is placed it in
Electron sensitive resist is removed in base formamide solution, is covered with the table of the metal-oxide gas transducer of connection electrode thereon
Face is covered with the silicon chip of mesoporous thermal insulation layer；Wherein, it is deposited as electron beam evaporation.
Step 3, the surface for the metal-oxide gas transducer for being first covered with connection electrode thereon is covered with mesoporous thermal insulation layer
Silicon chip on coating electron sensitive resist after, depicted on the periphery of metal-oxide gas transducer by electron beam exposure method
Annular.After the insulating layer for sputtering 90nm thickness using magnetron sputtering method in annular, place it in dimethyl formamide solution
Electron sensitive resist is removed, the metal-oxide gas transducer for being covered with connection electrode successively thereon and annular insulating layer are obtained
Surface is covered with the silicon chip of mesoporous thermal insulation layer；Wherein, the material of annular insulating layer is silica.
Step 4, first it is covered with the table of the metal-oxide gas transducer and annular insulating layer of connection electrode successively thereon
Face is covered on the silicon chip of mesoporous thermal insulation layer after coating electron sensitive resist, is portrayed at annular insulating layer by electron beam exposure method
Go out wide 0.4 μm of platinum micro-heater figure；Wherein, electron sensitive resist is ZEP 520A electron sensitive resists.Then at platinum it is micro- plus
After the platinum micro-heater of thickness 425nm is deposited on hot device figure, it is against corrosion to place it in stripping electron beam in dimethyl formamide solution
Agent obtains being covered with the metal-oxide gas transducer of connection electrode, annular insulating layer and annular platinum micro-heater successively thereon
Surface be covered with the silicon chip of mesoporous thermal insulation layer；Wherein, it is deposited as electron beam evaporation.
Step 5, the metal-oxide gas transducer, annular insulating layer and annular of connection electrode are first covered with successively thereon
The surface of platinum micro-heater is covered on the silicon chip of mesoporous thermal insulation layer after coating electron sensitive resist, by electron beam exposure method in ring
Annular is depicted at shape platinum micro-heater；Wherein, electron sensitive resist is ZEP 520A electron sensitive resists.Make in annular
After the insulating layer for sputtering 90nm thickness with magnetron sputtering method, growth inner ring radius is 4.5 μm thereon, outer shroud radius is 11 μm, thick
For the gas concentrator of 625nm；Wherein, the material of annular insulating layer is silica, and gas concentrator is zinc oxide nanowire
Array gas concentrator.Then, it places it in and removes electron sensitive resist in dimethyl formamide solution, be made and be similar to Fig. 1
Shown in the integrated device of gas concentration sensing.
Embodiment 3
Prepare the specific steps are：
Step 1, it is covered with prior to surface after applying electron sensitive resist on the silicon chip of mesoporous thermal insulation layer, passes through electron beam exposure
The sensor pattern that method depicts a length of 4 μm on it, width is 0.9 μm；Wherein, electron sensitive resist is ZEP 520A electron beams
Resist.After sputtering metal-oxide gas transducer using magnetron sputtering method in sensor pattern, two are placed it in
Electron sensitive resist is removed in methylformamide solution, the surface for being covered with metal-oxide gas transducer thereon is covered with Jie
The silicon chip of hole thermal insulation layer；Sputtering power when wherein, using magnetron sputtering method sputtered metal oxide gas sensor be 100W,
Sputtering time is 35min, and the thickness of metal-oxide gas transducer is 150nm, and metal oxide therein is stannic oxide.
Step 2, the first surface for being covered with metal-oxide gas transducer thereon, which is covered on the silicon chip of mesoporous thermal insulation layer, applies
After applying electron sensitive resist, electrode pattern is depicted at the both ends of metal-oxide gas transducer by electron beam exposure method；
Wherein, electron sensitive resist is ZEP 520A electron sensitive resists.After electrode evaporation on electrode pattern, diformazan is placed it in
Electron sensitive resist is removed in base formamide solution, is covered with the table of the metal-oxide gas transducer of connection electrode thereon
Face is covered with the silicon chip of mesoporous thermal insulation layer；Wherein, it is deposited as electron beam evaporation.
Step 3, the surface for the metal-oxide gas transducer for being first covered with connection electrode thereon is covered with mesoporous thermal insulation layer
Silicon chip on coating electron sensitive resist after, depicted on the periphery of metal-oxide gas transducer by electron beam exposure method
Annular.After the insulating layer for sputtering 100nm thickness using magnetron sputtering method in annular, place it in dimethyl formamide solution
Electron sensitive resist is removed, the metal-oxide gas transducer for being covered with connection electrode successively thereon and annular insulating layer are obtained
Surface is covered with the silicon chip of mesoporous thermal insulation layer；Wherein, the material of annular insulating layer is silica.
Step 4, first it is covered with the table of the metal-oxide gas transducer and annular insulating layer of connection electrode successively thereon
Face is covered on the silicon chip of mesoporous thermal insulation layer after coating electron sensitive resist, is portrayed at annular insulating layer by electron beam exposure method
Go out wide 0.6 μm of platinum micro-heater figure；Wherein, electron sensitive resist is ZEP 520A electron sensitive resists.Then at platinum it is micro- plus
After the platinum micro-heater of thickness 350nm is deposited on hot device figure, it is against corrosion to place it in stripping electron beam in dimethyl formamide solution
Agent obtains being covered with the metal-oxide gas transducer of connection electrode, annular insulating layer and annular platinum micro-heater successively thereon
Surface be covered with the silicon chip of mesoporous thermal insulation layer；Wherein, it is deposited as electron beam evaporation.
Step 5, the metal-oxide gas transducer, annular insulating layer and annular of connection electrode are first covered with successively thereon
The surface of platinum micro-heater is covered on the silicon chip of mesoporous thermal insulation layer after coating electron sensitive resist, by electron beam exposure method in ring
Annular is depicted at shape platinum micro-heater；Wherein, electron sensitive resist is ZEP 520A electron sensitive resists.Make in annular
After the insulating layer for sputtering 100nm thickness with magnetron sputtering method, growth inner ring radius is 5 μm thereon, outer shroud radius is 10 μm, thickness is
The gas concentrator of 750nm；Wherein, the material of annular insulating layer is silica, and gas concentrator is zinc-oxide nano linear array
Row gas concentrator.Then, it places it in and removes electron sensitive resist in dimethyl formamide solution, be made as shown in Figure 1
The integrated device of gas concentration sensing.
Embodiment 4
Prepare the specific steps are：
Step 1, it is covered with prior to surface after applying electron sensitive resist on the silicon chip of mesoporous thermal insulation layer, passes through electron beam exposure
The sensor pattern that method depicts a length of 4.5 μm on it, width is 0.6 μm；Wherein, electron sensitive resist is ZEP 520A electronics
Beam resist.After sputtering metal-oxide gas transducer using magnetron sputtering method in sensor pattern, place it in
Electron sensitive resist is removed in dimethyl formamide solution, the surface for being covered with metal-oxide gas transducer thereon is covered with
The silicon chip of mesoporous thermal insulation layer；Sputtering power when wherein, using magnetron sputtering method sputtered metal oxide gas sensor is
The thickness of 110W, sputtering time 23min, metal-oxide gas transducer are 125nm, and metal oxide therein is titanium dioxide
Tin.
Step 2, the first surface for being covered with metal-oxide gas transducer thereon, which is covered on the silicon chip of mesoporous thermal insulation layer, applies
After applying electron sensitive resist, electrode pattern is depicted at the both ends of metal-oxide gas transducer by electron beam exposure method；
Wherein, electron sensitive resist is ZEP 520A electron sensitive resists.After electrode evaporation on electrode pattern, diformazan is placed it in
Electron sensitive resist is removed in base formamide solution, is covered with the table of the metal-oxide gas transducer of connection electrode thereon
Face is covered with the silicon chip of mesoporous thermal insulation layer；Wherein, it is deposited as electron beam evaporation.
Step 3, the surface for the metal-oxide gas transducer for being first covered with connection electrode thereon is covered with mesoporous thermal insulation layer
Silicon chip on coating electron sensitive resist after, depicted on the periphery of metal-oxide gas transducer by electron beam exposure method
Annular.After the insulating layer for sputtering 110nm thickness using magnetron sputtering method in annular, place it in dimethyl formamide solution
Electron sensitive resist is removed, the metal-oxide gas transducer for being covered with connection electrode successively thereon and annular insulating layer are obtained
Surface is covered with the silicon chip of mesoporous thermal insulation layer；Wherein, the material of annular insulating layer is silica.
Step 4, first it is covered with the table of the metal-oxide gas transducer and annular insulating layer of connection electrode successively thereon
Face is covered on the silicon chip of mesoporous thermal insulation layer after coating electron sensitive resist, is portrayed at annular insulating layer by electron beam exposure method
Go out wide 0.8 μm of platinum micro-heater figure；Wherein, electron sensitive resist is ZEP 520A electron sensitive resists.Then at platinum it is micro- plus
After the platinum micro-heater of thickness 275nm is deposited on hot device figure, it is against corrosion to place it in stripping electron beam in dimethyl formamide solution
Agent obtains being covered with the metal-oxide gas transducer of connection electrode, annular insulating layer and annular platinum micro-heater successively thereon
Surface be covered with the silicon chip of mesoporous thermal insulation layer；Wherein, it is deposited as electron beam evaporation.
Step 5, the metal-oxide gas transducer, annular insulating layer and annular of connection electrode are first covered with successively thereon
The surface of platinum micro-heater is covered on the silicon chip of mesoporous thermal insulation layer after coating electron sensitive resist, by electron beam exposure method in ring
Annular is depicted at shape platinum micro-heater；Wherein, electron sensitive resist is ZEP 520A electron sensitive resists.Make in annular
After the insulating layer for sputtering 110nm thickness with magnetron sputtering method, growth inner ring radius is 5.5 μm thereon, outer shroud radius is 9 μm, thick
For the gas concentrator of 875nm；Wherein, the material of annular insulating layer is silica, and gas concentrator is zinc oxide nanowire
Array gas concentrator.Then, it places it in and removes electron sensitive resist in dimethyl formamide solution, be made and be similar to Fig. 1
Shown in the integrated device of gas concentration sensing.
Embodiment 5
Prepare the specific steps are：
Step 1, it is covered with prior to surface after applying electron sensitive resist on the silicon chip of mesoporous thermal insulation layer, passes through electron beam exposure
The sensor pattern that method depicts a length of 5 μm on it, width is 0.3 μm；Wherein, electron sensitive resist is ZEP 520A electron beams
Resist.After sputtering metal-oxide gas transducer using magnetron sputtering method in sensor pattern, two are placed it in
Electron sensitive resist is removed in methylformamide solution, the surface for being covered with metal-oxide gas transducer thereon is covered with Jie
The silicon chip of hole thermal insulation layer；Sputtering power when wherein, using magnetron sputtering method sputtered metal oxide gas sensor be 120W,
Sputtering time is 10min, and the thickness of metal-oxide gas transducer is 100nm, and metal oxide therein is stannic oxide.
Step 2, the first surface for being covered with metal-oxide gas transducer thereon, which is covered on the silicon chip of mesoporous thermal insulation layer, applies
After applying electron sensitive resist, electrode pattern is depicted at the both ends of metal-oxide gas transducer by electron beam exposure method；
Wherein, electron sensitive resist is ZEP 520A electron sensitive resists.After electrode evaporation on electrode pattern, diformazan is placed it in
Electron sensitive resist is removed in base formamide solution, is covered with the table of the metal-oxide gas transducer of connection electrode thereon
Face is covered with the silicon chip of mesoporous thermal insulation layer；Wherein, it is deposited as electron beam evaporation.
Step 3, the surface for the metal-oxide gas transducer for being first covered with connection electrode thereon is covered with mesoporous thermal insulation layer
Silicon chip on coating electron sensitive resist after, depicted on the periphery of metal-oxide gas transducer by electron beam exposure method
Annular.After the insulating layer for sputtering 120nm thickness using magnetron sputtering method in annular, place it in dimethyl formamide solution
Electron sensitive resist is removed, the metal-oxide gas transducer for being covered with connection electrode successively thereon and annular insulating layer are obtained
Surface is covered with the silicon chip of mesoporous thermal insulation layer；Wherein, the material of annular insulating layer is silica.
Step 4, first it is covered with the table of the metal-oxide gas transducer and annular insulating layer of connection electrode successively thereon
Face is covered on the silicon chip of mesoporous thermal insulation layer after coating electron sensitive resist, is portrayed at annular insulating layer by electron beam exposure method
Go out wide 1 μm of platinum micro-heater figure；Wherein, electron sensitive resist is ZEP 520A electron sensitive resists.Then at the micro- heating of platinum
After the platinum micro-heater of thickness 200nm is deposited on device figure, places it in and removes electron sensitive resist in dimethyl formamide solution,
Obtain being covered with the metal-oxide gas transducer of connection electrode, the table of annular insulating layer and annular platinum micro-heater successively thereon
Face is covered with the silicon chip of mesoporous thermal insulation layer；Wherein, it is deposited as electron beam evaporation.
Step 5, the metal-oxide gas transducer, annular insulating layer and annular of connection electrode are first covered with successively thereon
The surface of platinum micro-heater is covered on the silicon chip of mesoporous thermal insulation layer after coating electron sensitive resist, by electron beam exposure method in ring
Annular is depicted at shape platinum micro-heater；Wherein, electron sensitive resist is ZEP 520A electron sensitive resists.Make in annular
After the insulating layer for sputtering 120nm thickness with magnetron sputtering method, growth inner ring radius is 6 μm thereon, outer shroud radius is 8 μm, thickness is
The gas concentrator of 1000nm；Wherein, the material of annular insulating layer is silica, and gas concentrator is zinc-oxide nano linear array
Row gas concentrator.Then, it places it in and removes electron sensitive resist in dimethyl formamide solution, be made and be similar to Fig. 1 institutes
The integrated device of gas concentration sensing shown.
Select ZEP 520A electron sensitive resists or the polymethyl methacrylate electricity as electron sensitive resist respectively again
Beamlet resist, as the stannic oxide or indium oxide or gallium oxide or tungstic acid or molybdenum trioxide of metal oxide or oxidation
Copper or nickel oxide or chromium oxide, vapor deposition selects magnetron sputtering or d.c. sputtering or electron beam evaporation, as annular insulating layer material
Silica or aluminium oxide or zirconium dioxide, the organic mesoporous material or inorganic mesoporous material of the material as gas concentrator
Or oxidate nano linear array, above-described embodiment 1-5 is repeated, gas concentration biography shown in FIG. 1 has equally been made as or has been similar to
The integrated device of sense.
Obviously, those skilled in the art can to integrated device of gas concentration sensing of the present invention and preparation method thereof into
The various modification and variations of row are without departing from the spirit and scope of the present invention.If in this way, to these modifications and changes of the present invention
Within the scope of the claims of the present invention and its equivalent technology, then the present invention is also intended to exist comprising these modification and variations
It is interior.
Claims (10)
1. a kind of integrated device of gas concentration sensing, by gas sensor, gas concentrator, electric heater and the electrode in positioning shell
It forms, and the power supply being connect with electrode, it is characterised in that：
The positioning shell is the silicon chip that surface is covered with mesoporous thermal insulation layer；
The gas sensor is metal-oxide gas transducer, and the metal-oxide gas transducer invests the surface
It is covered on the silicon chip of mesoporous thermal insulation layer；
The gas concentrator is annular, and the annular gas inspissator invests the week of the metal-oxide gas transducer
Side；
The electric heater is wide≤1 μm, platinum micro-heater of thickness 200-500nm, and the platinum micro-heater is located at the annular gas
Under body inspissator；
It is equipped between annular gas inspissator between the platinum micro-heater and the periphery of metal-oxide gas transducer
Annular insulating layer；
The electrode is electrically connected with metal-oxide gas transducer, platinum micro-heater respectively.
2. the integrated device of gas concentration sensing according to claim 1, it is characterized in that metal-oxide gas transducer
A length of 3-5 μm, width be 0.3-1.5 μm, thickness 100-200nm, metal oxide therein be stannic oxide or indium oxide, or
Gallium oxide or tungstic acid or molybdenum trioxide or copper oxide or nickel oxide or chromium oxide.
3. the integrated device of gas concentration sensing according to claim 1, it is characterized in that annular gas inspissator is annular shape,
And concentrically with metal-oxide gas transducer, and its inner ring radius is 4-6 μm, outer shroud radius is 8-12 μm, thickness 500-
The material of 1000nm, annular gas inspissator are organic mesoporous material or inorganic mesoporous material or oxidate nano linear array.
4. the integrated device of gas concentration sensing according to claim 1, it is characterized in that thickness >=80nm of annular insulating layer,
It is annular silicon dioxide insulating layer, or annular alumina insulating layer, or annular zirconium dioxide insulating layer.
5. the preparation method of the integrated device of gas concentration sensing described in a kind of claim 1, including electron beam exposure method, feature
It is that key step is as follows：
Step 1, it is covered with prior to surface after applying electron sensitive resist on the silicon chip of mesoporous thermal insulation layer, is existed by electron beam exposure method
Sensor pattern is depicted thereon, and metal-oxide gas transducer is sputtered using magnetron sputtering method in sensor pattern
Afterwards, it places it in and removes electron sensitive resist in dimethyl formamide solution, be covered with metal oxide gas sensing thereon
The surface of device is covered with the silicon chip of mesoporous thermal insulation layer；
Step 2, the surface for being first covered with metal-oxide gas transducer thereon is covered with coating electricity on the silicon chip of mesoporous thermal insulation layer
After beamlet resist, electrode pattern is depicted at the both ends of metal-oxide gas transducer by electron beam exposure method, then at
On electrode pattern after electrode evaporation, places it in and remove electron sensitive resist in dimethyl formamide solution, be covered with thereon
The surface of the metal-oxide gas transducer of connection electrode is covered with the silicon chip of mesoporous thermal insulation layer；
Step 3, the surface for the metal-oxide gas transducer for being first covered with connection electrode thereon is covered with the silicon of mesoporous thermal insulation layer
After on piece coats electron sensitive resist, ring is depicted on the periphery of metal-oxide gas transducer by electron beam exposure method
Shape places it in after sputtering insulating layer using magnetron sputtering method in annular and removes electron beam in dimethyl formamide solution
Resist, the surface for obtaining the metal-oxide gas transducer for being covered with connection electrode successively thereon and annular insulating layer are covered with Jie
The silicon chip of hole thermal insulation layer；
Step 4, it covers on the surface of the metal-oxide gas transducer and annular insulating layer that are first covered with connection electrode successively thereon
Have after applying electron sensitive resist on the silicon chip of mesoporous thermal insulation layer, platinum is depicted at annular insulating layer by electron beam exposure method
Micro-heater figure places it in after platinum micro-heater is deposited on platinum micro-heater figure in dimethyl formamide solution
Remove electron sensitive resist, obtain being covered with successively thereon the metal-oxide gas transducer of connection electrode, annular insulating layer and
The surface of annular platinum micro-heater is covered with the silicon chip of mesoporous thermal insulation layer；
Step 5, the metal-oxide gas transducer, annular insulating layer and annular platinum for being first covered with connection electrode successively thereon are micro-
The surface of heater is covered on the silicon chip of mesoporous thermal insulation layer after coating electron sensitive resist, by electron beam exposure method in annular platinum
Annular is depicted at micro-heater, after sputtering insulating layer using magnetron sputtering method in annular, growth gasses concentrate thereon
Device then places it in and removes electron sensitive resist in dimethyl formamide solution, and the integrated device of gas concentration sensing is made.
6. the preparation method of the integrated device of gas concentration sensing according to claim 5, it is characterized in that electron sensitive resist
For ZEP 520A electron sensitive resists or polymethyl methacrylate (PMMA) electron sensitive resist.
7. the preparation method of the integrated device of gas concentration sensing according to claim 5, it is characterized in that using magnetic in step 1
Control sputtering method sputtered metal oxide gas sensor when sputtering power be 80-120W, sputtering time 10-60min, metal
A length of 3-5 μm of oxide gas sensor, width be 0.3-1.5 μm, thickness 100-200nm, metal oxide therein is two
Tin oxide or indium oxide or gallium oxide or tungstic acid or molybdenum trioxide or copper oxide or nickel oxide or chromium oxide.
8. the preparation method of the integrated device of gas concentration sensing according to claim 5, it is characterized in that annular insulating layer
Thickness >=80nm, for annular silicon dioxide insulating layer, or annular alumina insulating layer, or annular zirconium dioxide insulating layer.
9. the preparation method of the integrated device of gas concentration sensing according to claim 5, it is characterized in that gas concentrator
Growth course is, first micro- to being covered with the metal-oxide gas transducer, annular insulating layer, annular platinum of connection electrode successively thereon
The silicon chip progress oxygen plasma that heater and the surface of annular insulating layer and electron sensitive resist are covered with mesoporous thermal insulation layer is clear
It washes, then is dipped in the mixed of the zinc nitrate methanol solution of 15-25mmol/L and the 2-methylimidazole methanol solution of 35-45mmol/L
It closes and stands 20-40min in solution, obtain the molecular sieve inspissator being located on annular insulating layer；Wherein, when oxygen plasma cleans
Radio-frequency power be 80-120W, oxygen pressure is 0.5-1.5Torr, scavenging period is >=20s, zinc nitrate methanol is molten in mixed solution
The volume ratio of liquid and 2-methylimidazole methanol solution is 0.8-1.2：0.8-1.2.
10. the preparation method of the integrated device of gas concentration sensing according to claim 5, it is characterized in that gas concentrator
Growth course is that the first metal-oxide gas transducer for being covered with connection electrode successively thereon, annular insulating layer, annular platinum are micro-
It is 1- that heater and the surface of annular insulating layer and electron sensitive resist, which are covered on the silicon chip of mesoporous thermal insulation layer and sputter thickness,
The zinc oxide seed layer of 20nm reuses solwution method in growth of zinc oxide nano linear array in zinc oxide seed layer；Wherein, solution
Precursor solution in method is that volume ratio is 0.8-1.2：The zinc nitrate solution and 0.4- of the 0.4-0.6mmol/L of 0.8-1.2
The mixed solution of the hexamethylene tetraammonia solution of 0.6mmol/L, temperature when growth is 90-100 DEG C, time 1-3h.
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