CN102359980A - Resistance-type gas sensor with two support suspension beams and four-layer structure and method - Google Patents
Resistance-type gas sensor with two support suspension beams and four-layer structure and method Download PDFInfo
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Abstract
The invention relates to a resistance-type gas sensor with two support suspension beams and a four-layer structure and a manufacturing method for the sensor. The sensor comprises a substrate frame, a heat insulation cavity, a heating membrane area, a transition area, the support suspension beams, a heating resistance wire, a power supply lead, a power supply electrode, interdigital electrodes, a detection lead, a detection electrode and a sensitive membrane. The resistance-type gas sensor is characterized in that: the heating membrane area positioned above the heat insulation cavity is connected with the substrate frame by the transition area and the support suspension beams; the heating resistance wire is arranged on the heating membrane area in a mode of a crease line and is connected with the power supply electrode on the substrate frame through the power supply lead; the interdigital electrodes are arranged in a gap of the heating resistance wire and are connected with the detection electrode by the detection lead; and the sensitive membrane is positioned on the heating membrane area to cover the integral heating resistance wire and the interdigital electrodes, and is electrically connected with the interdigital electrodes.
Description
Technical field
The present invention relates to a kind of resistance-type gas sensor and method for making with two support overarm four-layer structures, the method for having used micro fabrication and chemical synthesis process to combine belongs to microelectromechanical systems (MEMS) and gas sensory field.
Background technology
Gas sensor has been obtained widely in industrial, civilian and environmental monitoring three big main fields and has been used.At present the ways and means of detected gas is very many, mainly comprises catalytic combustion type, electric chemical formula, heat-conducted, infrared absorption type and semiconductor-type gas sensor etc.Because advantages such as that the resistance-type semiconductor transducer has are highly sensitive, easy to operate, volume is little, with low cost, response time and release time are short, therefore use the most extensive, especially to flammable explosive gas (like CH
4, H
2Deng) and toxic and harmful (like CO, NO
xDeng) detection in play an important role.
In order to improve the performance of sensor, in the evolution of decades, semiconductor gas sensor has bigger development on device architecture in the past.Device architecture mainly is divided into slug type, thick-film type, film-type and silica-base film type.Sintering-type gas sensor mainly comprises directly-heated type and heater-type.The element discreteness is big because directly-heated type exists, interchangeability is poor, and the sensor of this structure is replaced by heater-type gradually gradually.The heater-type sensor is with gas sensitive and little binder mixed grinding, processes slurry then and is applied on the ceramic pipe that has contact conductor, at heating resistor of ceramic pipe positioned inside, provides working sensor required temperature.For example: Duan Chunming, " characteristic of heater-type semiconductor gas sensor and influence factor thereof ", the sensor world, 1999 (10), 23-26.The thick-film type gas sensor is to be made up of substrate, electrode and gas sensitive; Manufacturing process is that gas sensitive is mixed with a certain proportion of bonding agent; And the adding appropriate amount of catalysts is processed pasty state; Print to then on the ceramic substrate that electrode and heating element are installed in advance, dry, high-temperature calcination forms.For example: Zhang Weida, " α-Fe
2O
3The research of air-sensitive pottery ", functional material, 1994 (5), 426-431.Thin film gas sensor configuration is similar with thick film.The gas sensitive that different is above the potential electrode be utilize vacuum sputtering, reaction to steam to cross, thin film that methods such as chemical vapor deposition, spray pyrolysis, sol-gel are crossed.For example: Gao Shengguo, Zhan Zili, clock gram wound, centre forward still, the Peng Chunhua, " SnO of sol-gel process preparation
2The film gas-sensitive characteristic research ", Light Engineering Institutes Of Zhengzhou's journal (natural science edition), 2002 (17), 11-13.The film-type gas sensor has that material usage is low, the physical strength of the repeatability between each sensor, sensor advantage preferably, but the manufacture process of film-type sensor needs complicacy, expensive process equipment, strict environmental baseline, and cost is higher.Silica-based microstructure film type gas sensor is based on the novel resistance-type gas sensor of microheater, and present main flow is based on the microheater of sealing membrane type or four overarm formulas, and power consumption is relatively still higher.For example: John S.Suehle, Richard E.Cavicchi, Michael Gaitan; Steve Semancik; " Tin oxide gas sensor fabricated using CMOS micro-hotplates and in-situ processing ", IEEE Electron Device Letters, vol.14; 1993, pp.118-120.
How under the prerequisite that guarantees good sensitivity, selectivity and stability, can realize low cost again, the sensor of low-power consumption and batch process is the technical barrier that those skilled in the art thirst for solving, thereby also is guided out the object of the invention.
Summary of the invention
The object of the present invention is to provide a kind of resistance-type gas sensor and preparation method thereof with two overarm four-layer structures, reduce cost with power consumption in, can improve the sensitivity and the selectivity of sensor again.
Structurally, resistance-type gas sensor of the present invention is one and can be divided into four layers of device with difference in functionality from bottom to top.Ground floor (orlop) is the silicon substrate framework, wherein comprises a heat insulation cavity.The second layer is that the heating film region that is positioned at heat insulation cavity top is hung oneself from a beam with supporting, and they are made up of the multilayer complex films of monox and silicon nitride.The 3rd layer is resistive heater, power supply lead-in wire, interdigital electrode and detection leads.Being arranged in resistive heater on the heating film region with broken line form, to be converted into heat energy to electric energy be that sensor provides suitable working temperature.Interdigital electrode is positioned at the heating film region place, and the interdigital gap that is arranged in resistive heater will be used to connect sensitive membrane.When characteristic gas contacted with gas sensitive, the resistance value of gas sensitive can change, and just can realize detection of gas through the resistance variations of measuring between exploring electrode.The 4th layer (the superiors) are the sensitive membrane that is used for detection of gas, and sensitive membrane is positioned at the heating film region place and with interdigital electrode good electrical contact is arranged, and is the sensing unit of sensor.
In sum, a kind of structure of resistance-type gas sensor with two overarm four-layer structures provided by the invention is as shown in Figure 1, comprising: substrate framework 1, heat insulation cavity 2; Heating film region 3, zone of transition 4 supports overarm 5, resistive heater 6; Power supply lead-in wire 7, transmitting electrode 8, interdigital electrode 9; Detection leads 10, exploring electrode 11 and sensitive membrane 12.Its architectural feature is:
1. the heat insulation cavity in the substrate framework can have multiple shape according to the difference of implementing process; A kind of is to be down structure trapezoidal or " V " font through the xsect that front anisotropic silicon wet etching forms, and another kind is the structure that is circular arc through the xsect that isotropy release corrosion or isotropic dry etch form.
2. the two ends of heating film region link to each other with an end that supports overarm through a zone of transition respectively, and the other end that supports overarm connects substrate framework and plays the effect of support, and is suspended on the heat insulation cavity.
3. resistive heater is arranged on the heating film region with the form of broken line, and links to each other with transmitting electrode on the substrate framework through two power supply lead-in wires that support in the overarm.
4. interdigital electrode is positioned at the heating film region place, in the interdigital gap that is arranged in resistive heater, and links to each other with exploring electrode on the substrate framework through detection leads.
5. sensitive membrane is positioned on the heating film region, covers whole resistive heater and interdigital electrode, and with interdigital electrode good electrically connecting is arranged.
6. the broken line form resistive heater of arranging links to each other with transmitting electrode on the substrate framework through two power supply lead-in wires that support in the overarm.
7. interdigital electrode links to each other with the exploring electrode of substrate framework through detection leads.
8. described heating film region is shaped as rectangular configuration.
Described zone of transition be shaped as isosceles trapezoidal structure, and trapezoidal bottom links to each other with the short rib of rectangle heating film region, trapezoidal last base with support overarm and link to each other.
On manufacture craft, resistance-type gas sensor of the present invention can be divided into two parts.Utilize MEMS technology to realize the making of parts such as microheater and interdigital electrode earlier, utilize traditional handicraft to act on the sensitive membrane of detection of gas at the heating film region positioning again.The concrete making step of method for making of a kind of resistance-type gas sensor with two overarm four-layer structures provided by the invention is following:
1. selection substrate.When discharging film and adopt the anisotropic wet etching, the silicon chip that must adopt (100) face is as substrate, when discharge that film adopts be isotropy wet etching or isotropic dry etch the time, the crystal orientation of silicon substrate is not required.
2. making composite membrane.Composite membrane is used to form heating film region, and zone of transition is hung oneself from a beam with supporting, and is produced on the described substrate of step 1.Composite membrane is composited by the monox and the silicon nitride of single or multiple lift.Can adopt oxidation, plasma reinforced chemical vapour deposition (PECVD) or the preparation of low-pressure chemical vapor deposition methods such as (LPCVD).
3. make resistive heater, power supply lead-in wire, transmitting electrode, interdigital electrode, detection leads and exploring electrode.Adopt metal material,, utilize lift-off (peeling off) technology or wet corrosion technique to make like platinum, gold etc.
4. open the film release window.Utilize reactive ion etching (RIE) or ion beam etching (Ion-beam) the thoroughly monox and the silicon nitride composite membrane of etching exposure, expose substrate silicon and form the film release window.
5. release film.A kind of method is to use the anisotropic wet corrosive liquid, like TMAH (TMAH) or potassium hydroxide (KOH) etc.; Another kind method is to use the isotropy wet method rotten, as, hydrofluorite (HF)+nitric acid (HNO
3)+water (H
2O) etc. or isotropic dry etch gas, like XeF
2Deng.The substrate silicon of emptying below the composite membrane through these two kinds of methods can discharge membrane structure.
6. making sensitive membrane.Can adopt common vapor phase method, liquid phase method or solid phase method are made sensitive membrane.
A kind of resistance-type gas sensor with two overarm four-layer structures provided by the invention and preparation method thereof is compared with resistance-type gas sensor in the past, and its advantage is:
1. make based on MEMS technology, device volume is little, and cost is low, is easy to produce in batches.
2. the microheater that adopts two overarms to support is that sensor provides work required high temperature, is beneficial to the reduction power consumption, improves temperature homogeneity, and is easy to improve through adjusting and Control work temperature the performance of sensor.
3. the structure of this two overarm sensors is very simple, and the physical strength under the high temperature is higher, and the release of structure can have multiple choices.
4. utilize MEMS technology to make microheater and interdigital electrode earlier, make sensitive membrane again, substep is accomplished, and effectively avoids semiconductor technology to the active influence of sensitive membrane.
5. resistive heater and interdigital electrode are in same one deck, are evenly distributed on the heating film region, have reduced the film number of plies, utilize the physical strength that improves thin film region.
Description of drawings
Fig. 1 is a kind of structural representation with resistance-type gas sensor of two overarm four-layer structures provided by the invention.
Fig. 2 is second to the 4th layer a decomposing schematic representation of sensor.
Fig. 3 is a kind of process flow diagram with resistance-type gas sensor method for making of two overarm four-layer structures provided by the invention, and wherein (a) is for selecting substrate, (b) for making composite membrane; (c) for making resistive heater, power supply lead-in wire, transmitting electrode; Interdigital electrode, detection leads, and exploring electrode; (d) for opening the film release window, (e) for discharging film, (f) for making sensitive membrane.
Fig. 4 is the structural representation of embodiment 2, and wherein (a) is vertical view, (b) is sectional view.
Fig. 5 is the structural representation of embodiment 3, and wherein (a) is vertical view, (b) is sectional view.
1 is framework among the figure, and 2 is heat insulation cavity, and 3 is heating film region, and 4 is zone of transition, and 5 for supporting overarm, and 6 is resistive heater, and 7 are the power supply lead-in wire, and 8 is transmitting electrode, and 9 is interdigital electrode, and 10 is detection leads, and 11 is exploring electrode, and 12 is sensitive membrane.
Embodiment
Embodiment 1:
The structural representation of this embodiment is referring to shown in Figure 1, and concrete method for making is following:
1. selection substrate.The silicon chip of 4 inches twin polishings of choosing N type (100) face is as substrate, and resistivity 3-8 Ω cm, silicon wafer thickness are 350 ± 10 microns, the angular error of side cut＜1%.
2. making composite membrane.Adopt the individual layer composite membrane, utilizing the method for low-pressure chemical vapor deposition (LPCVD) layer thickness of growing successively is the silicon nitride that 0.5 micron monox and a layer thickness is 0.3 micron.
3. making resistive heater, power supply lead-in wire, transmitting electrode, interdigital electrode, detection leads and exploring electrode.Adopt stripping technology (lift-off) to make.Thin glue photoetching (photoresist thickness is 2.0 microns) defines resistive heater, the power supply lead-in wire, and transmitting electrode, interdigital electrode, the figure of detection leads and exploring electrode, the titanium platinum of sputter one deck 0.2 micron thick gets final product after last acetone removes photoresist then.
4. open the film release window.Positive photoetching defines and is used to discharge heating film region and the corrosion window graphics that supports overarm, the monox and the silicon nitride composite membrane that under the protection of photoresist, utilize the thorough etching of ion beam etching (Ion-beam) to expose.
5. release film.Utilize the TMAH corrosive liquid through film release window corrosion substrate silicon, and the central mode district with support overarm below form and fall trapezoidal heat insulation cavity.
6. making sensitive membrane.Adopt vapor phase method to make the gas sensitization film.
Embodiment 2:
The structural representation of this embodiment is referring to shown in Figure 4, and concrete method for making is following:
1. selection substrate.The silicon chip of 4 inches twin polishings of choosing P type (100) face is as substrate, and resistivity 3-8 Ω cm, silicon wafer thickness are 350 ± 10 microns, the angular error of side cut＜1%.
2. making composite membrane.Adopt the individual layer composite membrane, utilizing the method for plasma reinforced chemical vapour deposition (PECVD) layer thickness of growing successively is the silicon nitride that 0.4 micron monox and a layer thickness is 0.6 micron.
3. making resistive heater, power supply lead-in wire, transmitting electrode, interdigital electrode, detection leads and exploring electrode.Adopt stripping technology (li ft-off) to make.Thin glue photoetching (photoresist thickness is 2.0 microns) defines resistive heater, the power supply lead-in wire, and transmitting electrode, interdigital electrode, the figure of detection leads and exploring electrode, the titanium platinum of sputter one deck 0.3 micron thick gets final product after last acetone removes photoresist then.
4. open the film release window.Positive photoetching defines and is used to discharge heating film region and the corrosion window graphics that supports overarm, the monox and the silicon nitride composite membrane that under the protection of photoresist, utilize the thorough etching of reactive ion etching (RIE) to expose.
5. release film.Utilize the KOH corrosive liquid through film release window corrosion substrate silicon, and the central mode district with support overarm below form and fall trapezoidal heat insulation cavity.
6. making sensitive membrane.Adopt liquid phase method to make the gas sensitization film.
Embodiment 3:
The structural representation of this embodiment is referring to shown in Figure 5, and concrete method for making is following:
1. selection substrate.The silicon chip of 4 inches twin polishings of selection P type (111) face is as substrate, and resistivity 3-8 Ω cm, silicon wafer thickness are 350 ± 10 microns, the angular error of side cut＜1%.
2. making composite membrane.Adopt multilayer complex films; Utilizing the method for low-pressure chemical vapor deposition (LPCVD) to deposit a layer thickness successively earlier is the silicon nitride that 0.2 micron monox and a layer thickness is 0.2 micron, and utilizing the method for plasma reinforced chemical vapour deposition (PECVD) to deposit a layer thickness successively again is the silicon nitride that 0.2 micron monox and a layer thickness is 0.2 micron.
3. making resistive heater, power supply lead-in wire, transmitting electrode, interdigital electrode, detection leads and exploring electrode.The employing wet corrosion technique is made.The titanium platinum of elder generation's sputter one deck 0.2 micron thick approaches glue photoetching (photoresist thickness is 2.0 microns) again and defines resistive heater, the figure of power supply lead-in wire and transmitting electrode; Last wet etching forms resistive heater, power supply lead-in wire, transmitting electrode; Interdigital electrode, detection leads, and exploring electrode.
4. open the film release window.Positive photoetching defines and is used to discharge heating film region and the corrosion window graphics that supports overarm, the monox and the silicon nitride composite membrane that under the protection of photoresist, utilize the thorough etching of reactive ion etching (RIE) to expose.
5. release film.Utilize XeF
2Gas passes through film release window etched substrate silicon, and below central mode district and support overarm, forms the heat insulation cavity of circular arc.
6. making sensitive membrane.Adopt solid phase method to make the gas sensitization film.
Claims (9)
1. resistance-type gas sensor with two brace summer four-layer structures; It is characterized in that described resistance-type gas sensor is one and is divided into four layers from bottom to top and has the difference in functionality structure; Wherein the orlop ground floor is the silicon substrate framework, wherein comprises a heat insulation cavity; The second layer is that the heating film region that is positioned at heat insulation cavity top is hung oneself from a beam with supporting, and is made up of the multilayer complex films of monox and silicon nitride; The 3rd layer is resistive heater, power supply lead-in wire, interdigital electrode and detection leads; Resistive heater is arranged on the heating film region with broken line form; Interdigital electrode is arranged in the gap of resistive heater and is connected with the 4th layer of sensitive membrane that is used for detection of gas topmost; Sensitive membrane is positioned on the heating film region, covers whole resistive heater and interdigital electrode, and with interdigital electrode good electrical connection is arranged.
2. by the described sensor of claim 1, the two ends that it is characterized in that being positioned at the heating film region of heat insulation cavity top link to each other through a zone of transition and the end that supports overarm respectively, support the other end connection substrate framework of overarm, and are suspended on the heat insulation cavity.
3. by claim 1 or 2 described sensors, it is characterized in that the shape of said heat insulation cavity a kind of be to be down trapezoidal or the V-shape structure through the xsect that front anisotropic silicon wet etching forms; Another kind is the structure that is circular arc through the xsect that isotropy release corrosion or isotropic dry etch form.
4. by the described sensor of claim 1, it is characterized in that resistive heater that broken line form arranges links to each other with transmitting electrode on the substrate framework through two power supply lead-in wires that support in the overarm.
5. by the described sensor of claim 1, it is characterized in that interdigital electrode passes through detection leads and link to each other with the exploring electrode of substrate framework.
6. by the described sensor of claim 1, it is characterized in that the rectangular configuration that is shaped as of described heating film region.
7. by the described sensor of claim 2, it is characterized in that the isosceles trapezoidal structure that is shaped as of described zone of transition, and trapezoidal bottom linking to each other with the short rib of rectangle heating film region, hangs oneself from a beam with support and links to each other in trapezoidal last base.
8. make the method for sensor according to claim 1 or claim 2, it is characterized in that utilizing earlier MEMS technology to realize microheater and interdigital electrode making, utilizing traditional handicraft to make sensitive membrane in the heating film region location, concrete steps are:
(a) select substrate: when discharging film and adopt the anisotropic wet corrosion, the silicon chip that adopts (100) face is as substrate, when discharge that film adopts be isotropy wet etching or isotropic dry etch the time, the crystal orientation of silicon substrate is not required;
(b) make composite membrane: composite membrane is used to form heating film region, and zone of transition is hung oneself from a beam with supporting; Composite membrane is composited by the monox and the silicon nitride of single or multiple lift, adopts oxidation, plasma reinforced chemical vapour deposition or low-pressure chemical vapor deposition method preparation;
(c) make resistive heater, power supply lead-in wire, transmitting electrode, interdigital electrode, detection leads and exploring electrode; Adopt platinum or golden metal material, utilize stripping technology or wet corrosion technique to make;
(d) open the film release window: the monox and the silicon nitride composite membrane that utilize reactive ion etching or ion beam etching etching to expose, expose substrate silicon and form the film release window;
(e) discharge film: a kind of method is to use TMAH or potassium hydroxide anisotropic wet corrosive liquid, and another kind of method is to use (hydrofluorite+nitric acid+water) isotropy wet method rotten, perhaps XeF
2Isotropic dry etch gas, the substrate silicon of emptying below the composite membrane through these two kinds of methods can discharge membrane structure;
(f) make sensitive membrane: adopt vapor phase method, liquid phase method or solid phase method are made sensitive membrane.
9. by the described method of claim 8, it is characterized in that:
1) described individual layer composite membrane is that one deck monox and one deck silicon nitride are composited;
Or 2) described multilayer complex films deposits one deck monox and one deck silicon nitride with the LPCVD method earlier successively, and then utilizes PECVD method deposition one deck monox and one deck silicon nitride.
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| CN104058360A (en) * | 2013-03-19 | 2014-09-24 | 罗伯特·博世有限公司 | Sensor Device And Method For Producing Sensor Device |
| CN105940295A (en) * | 2013-12-06 | 2016-09-14 | 罗伯特·博世有限公司 | Semiconductor sensor having suspended structure and its manufacturing method |
| CN108318547A (en) * | 2018-05-11 | 2018-07-24 | 合肥微纳传感技术有限公司 | A kind of single suspension beam type gas sensor and sensor array with coiled structure |
| CN108519409A (en) * | 2018-05-11 | 2018-09-11 | 合肥微纳传感技术有限公司 | A kind of single suspension beam type gas sensor, preparation method and the sensor array of warpage |
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| WO2021189718A1 (en) * | 2020-03-26 | 2021-09-30 | 合肥微纳传感技术有限公司 | Mems gas sensor and array thereof, and gas detection and preparation method |
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| CN103675015A (en) * | 2012-09-19 | 2014-03-26 | 原子能和替代能源委员会 | Heat flux sensor with increased resolution |
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| CN105940295A (en) * | 2013-12-06 | 2016-09-14 | 罗伯特·博世有限公司 | Semiconductor sensor having suspended structure and its manufacturing method |
| CN108519409A (en) * | 2018-05-11 | 2018-09-11 | 合肥微纳传感技术有限公司 | A kind of single suspension beam type gas sensor, preparation method and the sensor array of warpage |
| CN108318547A (en) * | 2018-05-11 | 2018-07-24 | 合肥微纳传感技术有限公司 | A kind of single suspension beam type gas sensor and sensor array with coiled structure |
| WO2019214228A1 (en) * | 2018-05-11 | 2019-11-14 | 合肥微纳传感技术有限公司 | Gas sensor, sensor preparation method, and sensor array |
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| CN108318547B (en) * | 2018-05-11 | 2024-01-23 | 微纳感知(合肥)技术有限公司 | Single cantilever type gas sensor with curled structure and sensor array |
| CN108519409B (en) * | 2018-05-11 | 2024-05-07 | 微纳感知(合肥)技术有限公司 | Warp single cantilever type gas sensor, preparation method and sensor array |
| CN110143564A (en) * | 2019-04-02 | 2019-08-20 | 上海交通大学 | The connection structure and preparation method of temperature sensor, electrode and temperature-sensitive membrane |
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| CN113514498A (en) * | 2020-04-10 | 2021-10-19 | 中国石油化工股份有限公司 | Common-chip heating array type gas detection microchip and preparation method thereof |
| CN113514499A (en) * | 2020-04-10 | 2021-10-19 | 中国石油化工股份有限公司 | Embedded three-dimensional structure micro-heating plate, preparation method and gas sensor |
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Application publication date: 20120222 |