CN106370706B - A kind of Pd base variable capacitance type hydrogen gas sensor and preparation method thereof - Google Patents
A kind of Pd base variable capacitance type hydrogen gas sensor and preparation method thereof Download PDFInfo
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- CN106370706B CN106370706B CN201610937801.XA CN201610937801A CN106370706B CN 106370706 B CN106370706 B CN 106370706B CN 201610937801 A CN201610937801 A CN 201610937801A CN 106370706 B CN106370706 B CN 106370706B
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- 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
- G01N27/22—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance
- G01N27/227—Sensors changing capacitance upon adsorption or absorption of fluid components, e.g. electrolyte-insulator-semiconductor sensors, MOS capacitors
Abstract
The invention discloses a kind of Pd base variable capacitance type hydrogen gas sensors and preparation method thereof.The thermal oxide growth SiO on doped single crystal Si substrate2Layer, in SiO2It is provided in layer through SiO2The deposition hole of layer deposits movable electrode Pd sill in deposition hole；In SiO2The upper surface of layer is provided with the air channel being connected to deposition hole, and stationary electrode conducting plate is bonded to SiO2On layer.In the presence of hydrogen, the Pd base movable electrode in sensor absorbs hydrogen generation reversible volumetric expansion, makes/stationary electrode hypotelorism, and capacitor increases, to realize the monitoring to density of hydrogen.The deposition hole of sensor provided by the invention, which has, laterally limits effect, so that the volume expansion of Pd base movable electrode is added to short transverse, increases sensing response, effectively shortens the response time of sensor.Meanwhile sensor is made of standard Si base micro fabrication, cost and power consumption are lower, can be mass, and have broad mass market prospect.
Description
Technical field
The invention belongs to gas sensing techniques fields, and in particular to a kind of Pd base variable capacitance type hydrogen gas sensor and its system
Preparation Method.
Background technique
Hydrogen is important the raw material of industry, is widely used in the industry such as chemical industry, electronics, metallurgy, food, aerospace and section
Grind field.Especially in today that the problems such as environmental pollution, energy crisis gets worse, to renewable and clean energy resources such as hydrogen
Development and utilization becomes especially urgent.In recent years, using photolysis water hydrogen, hydrogen fuel cell as the exploitation of the hydrogen energy source of representative, utilization
Technology achieves rapid progress, and the automobile of hydrogen fuel cell driving has also emerged with portable unit.However, the hair of hydrogen sensing technology
Zhan Ze falls behind relatively, hinders the universal of hydrogen energy source significantly.The main technical requirements of hydrogen gas sensor are as follows: highly sensitive, short sound
Between seasonable, highly selective, high stability, miniaturization, low-power consumption and low cost.Hydrogen gas sensor on the market has electrification at present
Type, four major class of catalytic combustion-type, metal oxide resistor type and heat-conduction-type.These sensors have one common to lack
Falling into --- poor selectivity also has stronger response to common gas such as carbon monoxide, methane, acetylene, ethyl alcohol, therefore sensor is easy
Wrong report.
Metal Palladium (Pd) is the hydrogen catalyst being most widely used, and has natural selectivity to hydrogen, is that current hydrogen passes
Feel the hot spot material of research.Hydrogen molecule can be split as hydrogen atom when encountering hydrogen by Pd, and is absorbed part hydrogen atom and caused resistance
Rate increases and volume expansion.Under room temperature and an atmospheric pressure, when density of hydrogen is less than 1%, it is solid that Pd forms Pd-H in conjunction with H
Solution, resistivity maximal increment are 5%, and volume maximal increment is 0.3%.When density of hydrogen is 1~2%, Pd-H solid solution phase
Gradually it is changed into hydride phase, resistivity maximal increment is 70%, and dilatation is up to 10.4%.Hereafter, due to phase transformation
It completes, density of hydrogen further increases, and resistivity and volume are basically unchanged.Generation solid solution → hydrogen can be regulated and controled by adjusting temperature
Density of hydrogen needed for compound phase transformation and phase transition process.
Pd base hydrogen gas sensor mainly has three classes at present.One is Pd based resistance type hydrogen gas sensor, such sensor is logical
Cross the resistance variations detection density of hydrogen of monitoring Pd sill.The response time of this kind of sensor is typically larger than 60s, is unable to satisfy
The requirement of hydrogen leak detection.The second is Pd base nano gap type hydrogen gas sensor, the sensitive material of this kind of sensor be containing
The Pd sill of nano gap.After meeting hydrogen, the volume expansion of Pd sill makes original interstice become smaller or even be closed, device resistance
It decreases, to detect hydrogen.Extremely rapid due to inhaling hydrogen-expansion process, this kind of sensor response time is usually less than
10s.But since nano gap is unstable, with increasing for detection times, sensor performance decaying is very fast.The third is Pd base grid
Pole Metal-oxide-semicondutor (MOS) capacitive hydrogen gas sensor, this kind of sensor is by the hydrogen atom of involvement Pd in Pd base
The electric dipole formed at grid and oxide interface changes the capacitance of MOS capacitor to detect hydrogen.This kind of sensor is surveyed
It is high to try precision, measurement range is 15ppm~1%, but complex manufacturing technology, higher cost.The sold production unit cost of H2SCAN Corp.
At 2000 dollars or so, it is usually only used in high-end field.Booming bite of hydrogen energy source needs big quantity high performance, low cost, low function
The portable hydrogen sensor of consumption is to ensure with hydrogen safety.
Summary of the invention
The present invention is directed to overcome the shortcomings of the prior art, provide that a kind of selectivity is good, performance is stable, inexpensive, low
Pd base variable capacitance type hydrogen gas sensor of power consumption and preparation method thereof.
Realize that the technical solution of the object of the invention is to provide a kind of Pd base variable capacitance type hydrogen gas sensor, structure are as follows:
The thermal oxide growth SiO on doped single crystal Si substrate2Layer, in SiO2It is provided in layer through SiO2The deposition hole of layer, in deposition hole
Deposit movable electrode Pd sill；In SiO2The upper surface of layer is provided with the air channel being connected to deposition hole, and stationary electrode conduction is flat
Plate is bonded to SiO2On layer；The resistivity of the doped single crystal Si substrate is 10-3~102Ω·cm；SiO2Layer with a thickness of
0.5~1.5 micron；The air channel distributes as net shape, and groove depth is 0.1~0.5 micron；The Pd sill is pure metal Pd
Or Pd alloy, the height of the movable electrode Pd sill of deposition are SiO2The 50%~90% of thickness.
Technical solution of the present invention further includes a kind of preparation method of Pd base variable capacitance type hydrogen gas sensor, including walks as follows
It is rapid:
1, use thermal oxidation process in resistivity for 10-3~102The doped single crystal Si substrate surface of Ω cm grows one layer
0.5~1.5 micron of thick SiO2；
2, lithography and etching technique is first used, in the SiO of thermal oxide growth2The net that upper production depth is 0.1~0.5 micron
Trellis air channel, then use lithography and etching technique in the SiO of thermal oxide growth2Upper production runs through SiO2The deposition hole of layer；Or first
Using lithography and etching technique thermal oxide growth SiO2Upper production runs through SiO2The deposition hole of layer, then use lithography and etching
SiO of the technique in thermal oxide growth2The latticed air channel that upper production depth is 0.1~0.5 micron；
3, movable electrode of the Pd sill as variable capacitance hydrogen gas sensor, the Pd substrate are deposited in deposition hole
Material is pure metal Pd or its alloy；Pd sill height is between SiO2The 50%~90% of thickness；
4, first production is had and is bonded conducting plate material on the doped single crystal Si substrate of Pd sill movable electrode, conduction is flat
Stationary electrode of the plate material as variable capacitance hydrogen gas sensor, reusing slice tool will make on same single crystalline Si substrate
Sensor separation；Or production is first had to using slice tool the doped single crystal Si substrate separation of Pd sill movable electrode, then
It is bonded conducting plate material respectively on isolated single crystalline Si substrate；
5, welding electrode lead obtains a kind of Pd base variable capacitance type hydrogen gas sensor.
In technical solution of the present invention, the Pd sill deposition method is electroplating deposition or masking film sputtering sedimentation；
The conducting plate material is 10 selected from resistivity-3~102Doped single crystal Si piece, stainless steel substrates, copper sheet or the aluminium of Ω cm
One of piece.
The principle of foundation of the present invention is: Pd sill in sensor deposition hole and with conducting plate material respectively as can
Moving electrode and stationary electrode constitute a variable capacitance type hydrogen gas sensor.When thering is hydrogen to occur in environment, Pd sill
Hydrogen can be absorbed and reversible volume expansion occurs.Due to the restriction effect of deposition hole, Pd base movable electrode can not lateral expansion,
Its dilatation is all added to the short transverse of deposition hole, so that the spacing between Pd base movable electrode and stationary electrode contracts
Short, sensor capacitance increases with it.The volume of Pd base movable electrode is with extraneous density of hydrogen monotonic increase, monitoring sensor capacitor
Extraneous density of hydrogen can be detected.
Sensor provided by the invention, when hydrogen occurs, Pd base movable electrode absorbs hydrogen generation reversible volumetric expansion,
So that the hypotelorism between movable electrode and stationary electrode, sensor capacitance increases, and realizes the monitoring to density of hydrogen.Due to
Pd suction hydrogen-expansion process is extremely rapid, and the typical response time of sensor was less than 10 seconds.Further, since the limitation of deposition hole is made
With, Pd base movable electrode can not lateral expansion, dilatation is all added to the short transverse in hole, increases the sound of sensor
It answers, capacitance variations are up to 10 times or more before and after inhaling hydrogen.
Compared with prior art, the invention has the advantages that
1, since Pd inhales, hydrogen-expansion process is extremely rapid, and the sensor response time is smaller than 10s, being capable of effective guarantee hydrogen
Safety.
2, due to the restriction effect of deposition hole, Pd sill is all added to height side in the dilatation of three dimensions
To, increase sensor response.
3, metal Pd there is natural selectivity and performance to stablize hydrogen, therefore this sensor selectivity is good and in high temperature
Under still have stable performance.
4, this sensor using standard semi-conductor processes make, material and process costs it is low and be suitable for batch production, therefore
Cost is relatively low for sensor, is suitble to promote the use of.
5, this sensor is lower without leakage current, power consumption in the standby state, is suitable for wireless sensor network, portable gas
Sensing etc. needs the application field of low-power consumption sensor.
Detailed description of the invention
Fig. 1 is the perspective three dimensional structural schematic diagram of Pd base variable capacitance type hydrogen provided by the invention sensing；
Fig. 2 is a kind of operation principle schematic diagram of Pd base variable capacitance type hydrogen gas sensor provided by the invention.
Fig. 3 is that the production that the embodiment of the present invention 1 provides has the doped single crystal Si substrate of sensor chip and another conduct
Three dimensional structure diagram when being bonded to the doped monocrystalline silicon sheet of electrode；
In figure: 1, as the doped single crystal Si substrate of substrate；2, the SiO of thermal oxide growth2；3, air channel；4, deposition hole；
5, as the Pd sill of movable electrode；6, as the conducting plate material of stationary electrode；7, the biography made on single crystalline Si substrate
Sensor.
Specific embodiment
Technical solution of the present invention is further elaborated in the following with reference to the drawings and specific embodiments.
Embodiment 1:
Referring to attached drawing 1, it is a kind of Pd base variable capacitance type hydrogen gas sensor provided by the invention.The main portion of the sensor
Part includes: resistivity between 10-3~102The doped single crystal Si substrate 1 of Ω cm, the SiO of thermal oxide growth2Layer 2, in SiO2Layer
Upper production air channel 3, in SiO2What is made on layer runs through SiO2The deposition hole 4 of layer, what is deposited in deposition hole is used as sensor can
The Pd sill 5 of moving electrode, the conducting plate material 6 as sensor stationary electrode.Its specific structure are as follows: in doped single crystal
Thermal oxide growth SiO on Si substrate 12Layer 2, SiO2Layer with a thickness of 0.5~1.5 micron；In SiO2It is provided in layer through SiO2Layer
Deposition hole 4, movable electrode Pd sill 5 is deposited in deposition hole, the height of the movable electrode Pd sill of deposition is SiO2
The 50%~90% of thickness；In SiO2The upper surface of layer is provided with the air channel 3 to distribute as net shape being connected to deposition hole 4, groove depth
It is 0.1~0.5 micron；Stationary electrode conducting plate 6 is bonded to SiO2On layer.In the present invention, the material of Pd sill can be
Pure metal Pd or its alloy；The preferred material of conducting plate material is resistivity between 10-3~102The doped single crystal Si of Ω cm
One of piece, stainless steel substrates, copper sheet or aluminium flake.
Referring to attached drawing 2, it is a kind of work original of Pd base variable capacitance type hydrogen gas sensor sensor provided by the invention
Manage schematic diagram.As shown in attached drawing 2(a), Pd sill in deposition hole and make respectively with the conducting plate material at the top of deposition hole
A variable capacitance type hydrogen gas sensor is constituted for movable electrode and stationary electrode, it is ring in formula that capacitance, which is C=A/d,
The dielectric constant of border gas, A are the sectional area of deposition hole, distance of the d between Pd base movable electrode and stationary electrode.Such as attached drawing 2
(b) shown in, when having hydrogen to occur in environment, Pd sill can absorb hydrogen and reversible volumetric expansion, V occursPdIncrease.Due to
The restriction effect of deposition hole, Pd base movable electrode can not lateral expansion, dilatation is all added to the height side of deposition hole
To so that the spacing d between Pd base movable electrode and stationary electrode shortens, sensor capacitance C is increased with it.Pd base movable electrode
Volume with extraneous density of hydrogen monotonic increase, monitoring sensor capacitor can detect extraneous density of hydrogen.
The present embodiment provides a kind of production methods of Pd base variable capacitance type hydrogen gas sensor, and steps are as follows:
(1) use thermal oxidation process in resistivity for 5 × 10-34 inches of doped single crystal Si substrate surfaces of Ω cm are grown
One layer of 1 micron of thick SiO2；
(2) use positive photoresist ultraviolet photolithographic and plasma etch process in the SiO of thermal oxide growth2Upper production depth is
0.1 micron of latticed air channel；
(3) use positive photoresist ultraviolet photolithographic and method for etching plasma in the SiO of thermal oxide growth2Upper production diameter is 1
Millimeter and run through SiO2The deposition hole of layer, so that conduction Si substrate is exposed in air；
(4) electric plating method depositing pure gold in deposition hole is used to belong to Pd as the movable electrode of sensor, Pd base is movably electric
High degree is 0.89 micron；
(5) referring to attached drawing 3, it for production provided in this embodiment have the doped single crystal Si substrate of sensor chip with it is another
Three dimensional structure diagram when piece is bonded as the doped monocrystalline silicon sheet to electrode；Taking another piece of resistivity is 5 × 10-3
4 inches of doped single crystal Si pieces 6 of Ω cm are bonded with the sensor 7 made on single crystalline Si substrate, make sensor；
(6) sensor is separated with scribing machine；
(7) there is the Si substrate of device in production and as the Si on piece welding electrode lead of stationary electrode, finally obtain one
Kind Pd base variable capacitance type hydrogen gas sensor.
Embodiment 2
The structure such as embodiment 1 of Pd base variable capacitance type hydrogen gas sensor provided in this embodiment.The production side of sensor
Method are as follows:
(1) thermal oxidation process is used to grow one layer 1.5 in resistivity for 4 inches of doped single crystal Si piece surfaces of 10 Ω cm
The thick SiO of micron2；
(2) use negtive photoresist ultraviolet photolithographic and hydrofluoric acid wet etching method in the SiO of thermal oxide growth2Upper production diameter is
1 centimetre and run through SiO2The deposition hole of layer, so that conduction Si substrate is exposed in air；
(3) use positive photoresist ultraviolet photolithographic and plasma etching industrial in the SiO of thermal oxide growth2Upper production depth is 0.2
The latticed air channel of micron；
(4) stainless steel exposure mask is aided with using double target co-sputtering, it is selective that 80%Pd/20%Ni alloy is deposited in deposition hole
As the movable electrode of sensor, Pd base movable electrode height is 1.2 microns；
(5) sensor is separated with scribing machine；
(6) individual devices upper surface bonding polishing stainless steel plate after singulation is as sensor stationary electrode；
(7) it is bonded contact conductor on Si substrate and stainless steel plate, finally obtains a kind of Pd base variable capacitance type hydrogen biography
Sensor.
Embodiment 3
The structure such as embodiment 1 of Pd base variable capacitance type hydrogen gas sensor provided in this embodiment.The production side of sensor
Method are as follows:
(1) use thermal oxidation process in resistance rate for 5 × 10-24 inches of doped single crystal Si substrate surfaces growth one of Ω cm
0.5 micron of thick SiO of layer2；
(2) use positive photoresist ultraviolet photolithographic and plasma etch process in the SiO of thermal oxide growth2Upper production depth is
0.1 micron of latticed air channel；
(3) use positive photoresist ultraviolet photolithographic and method for etching plasma in the SiO of thermal oxide growth2Upper production diameter is
0.1 millimeter and run through SiO2The deposition hole of layer, so that conduction Si substrate is exposed in air；
(4) stainless steel exposure mask is aided with using double target co-sputtering, it is selective that pure 90%Pd/10%Ag conjunction is deposited in deposition hole
Movable electrode of the gold as sensor, Pd sill height are 0.45 micron；
(5) taking another piece of resistivity is 5 × 10-34 inches of doped single crystal Si pieces of Ω cm and production have the Si base of device
Piece bonding, the stationary electrode as sensor；
(6) sensor is separated with scribing machine；
(7) in substrate Si piece and as the Si on piece welding electrode lead of stationary electrode, it is variable to finally obtain a kind of Pd base
Capacitive hydrogen gas sensor.
Table 1 provides the sensor structure of the offer of the embodiment of the present invention 1~3 and functional parameter summarizes.
Table 1
As it can be seen from table 1 when select table in canonical parameter when, sensor before and after inhaling hydrogen capacitance variations up to 10 times
More than, the response time is smaller than 10s.
Pd base variable capacitance type hydrogen gas sensor of the present invention, can significantly promote hydrogen detection efficiency, have compared with
Good selectivity and stability and lower cost and power consumption, provide new approaches for hydrogen detection, be hydrogen energy source popularization and
It is universal to provide safety guarantee.
Claims (5)
1. a kind of Pd base variable capacitance type hydrogen gas sensor, it is characterised in that its structure are as follows: on doped single crystal Si substrate (1)
Thermal oxide growth SiO2Layer (2), in SiO2It is provided in layer through SiO2The deposition hole (4) of layer, deposits movable electrode in deposition hole
Pd sill (5)；In SiO2The upper surface of layer is provided with the air channel (3) being connected to deposition hole (4), stationary electrode conducting plate
(6) it is bonded to SiO2On layer；The resistivity of the doped single crystal Si substrate (1) is 10-3~102Ω·cm；SiO2Layer (2)
With a thickness of 0.5~1.5 micron；The air channel (3) distributes as net shape, and groove depth is 0.1~0.5 micron；The Pd sill
It (5) is pure metal Pd or Pd alloy, the height of the movable electrode Pd sill of deposition is SiO2The 50%~90% of thickness.
2. a kind of Pd base variable capacitance type hydrogen gas sensor according to claim 1, it is characterised in that: stationary electrode is conductive
The material of plate is 10 selected from resistivity-3~102One in the doped single crystal Si piece of Ω cm, stainless steel substrates, copper sheet or aluminium flake
Kind.
3. a kind of preparation method of Pd base variable capacitance type hydrogen gas sensor, it is characterised in that include the following steps:
(1) use thermal oxidation process in resistivity for 10-3~102The doped single crystal Si substrate surface of Ω cm grows one layer 0.5
~1.5 microns of thick SiO2；
(2) lithography and etching technique is first used, in the SiO of thermal oxide growth2Upper production depth is 0.1~0.5 micron latticed
Air channel, then use lithography and etching technique in the SiO of thermal oxide growth2Upper production runs through SiO2The deposition hole of layer；Or it first uses
SiO of the lithography and etching technique in thermal oxide growth2Upper production runs through SiO2The deposition hole of layer, then use lithography and etching technique
In the SiO of thermal oxide growth2The latticed air channel that upper production depth is 0.1~0.5 micron；
(3) movable electrode of the Pd sill as variable capacitance type hydrogen gas sensor, the Pd substrate are deposited in deposition hole
Material is pure metal Pd or its alloy；Pd sill height is between SiO2The 50%~90% of thickness；
(4) first production is had and is bonded conducting plate material, conducting plate on the doped single crystal Si substrate of Pd sill movable electrode
Stationary electrode of the material as variable capacitance type hydrogen gas sensor, reusing slice tool will make on same single crystalline Si substrate
Sensor separation；Or production is first had to using slice tool the doped single crystal Si substrate separation of Pd sill movable electrode, then
It is bonded conducting plate material respectively on isolated single crystalline Si substrate；
(5) welding electrode lead obtains a kind of Pd base variable capacitance type hydrogen gas sensor.
4. a kind of preparation method of Pd base variable capacitance type hydrogen gas sensor according to claim 3, it is characterised in that: institute
The Pd sill deposition method stated is electroplating deposition or masking film sputtering sedimentation.
5. a kind of preparation method of Pd base variable capacitance type hydrogen gas sensor according to claim 3, it is characterised in that: institute
The conducting plate material stated is 10 selected from resistivity-3~102Doped single crystal Si piece, stainless steel substrates, copper sheet or the aluminium flake of Ω cm
One of.
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| JP6926040B2 (en) * | 2018-09-10 | 2021-08-25 | 株式会社東芝 | Hydrogen sensor, hydrogen detection method and program |
| CN113406147B (en) * | 2021-05-08 | 2022-11-29 | 中北大学 | Hydrogen sensitive element and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US7389675B1 (en) * | 2006-05-12 | 2008-06-24 | The United States Of America As Represented By The National Aeronautics And Space Administration | Miniaturized metal (metal alloy)/ PdOx/SiC hydrogen and hydrocarbon gas sensors |
| CN203551501U (en) * | 2013-10-16 | 2014-04-16 | 华东师范大学 | High-sensitivity gas sensor based on micro-channel plate three-dimensional structure |
| CN105424768A (en) * | 2015-11-30 | 2016-03-23 | 中国电子科技集团公司第四十八研究所 | Dielectric material for hydrogen sensor core, hydrogen sensor core and preparation method and application thereof |
| CN205562452U (en) * | 2015-12-11 | 2016-09-07 | 中国电子科技集团公司第四十八研究所 | Hydrogen sensor is dielectric material , hydrogen sensor core for core |
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| US9618465B2 (en) * | 2013-05-01 | 2017-04-11 | Board Of Trustees Of Northern Illinois University | Hydrogen sensor |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7389675B1 (en) * | 2006-05-12 | 2008-06-24 | The United States Of America As Represented By The National Aeronautics And Space Administration | Miniaturized metal (metal alloy)/ PdOx/SiC hydrogen and hydrocarbon gas sensors |
| CN203551501U (en) * | 2013-10-16 | 2014-04-16 | 华东师范大学 | High-sensitivity gas sensor based on micro-channel plate three-dimensional structure |
| CN105424768A (en) * | 2015-11-30 | 2016-03-23 | 中国电子科技集团公司第四十八研究所 | Dielectric material for hydrogen sensor core, hydrogen sensor core and preparation method and application thereof |
| CN205562452U (en) * | 2015-12-11 | 2016-09-07 | 中国电子科技集团公司第四十八研究所 | Hydrogen sensor is dielectric material , hydrogen sensor core for core |
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