CN104316575A - Full-silicon MEMS (micro-electromechanical system) methane sensor, gas detection application and preparation method of full-silicon MEMS methane sensor - Google Patents
Full-silicon MEMS (micro-electromechanical system) methane sensor, gas detection application and preparation method of full-silicon MEMS methane sensor Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/14—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of an electrically-heated body in dependence upon change of temperature
- G01N27/16—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of an electrically-heated body in dependence upon change of temperature caused by burning or catalytic oxidation of surrounding material to be tested, e.g. of gas
Abstract
The invention discloses a full-silicon MEMS (micro-electromechanical system) methane sensor, gas detection application and a preparation method of the full-silicon MEMS methane sensor, is suitable for being used under an industrial and mining environment, belongs to a methane sensor as well as a preparation method and a detection method thereof, and particularly belongs to a methane sensor adopting an MEMS processing technology and a methane detection method thereof. The full-silicon MEMS sensor is prepared from a heating material with monocrystalline silicon serving as a heating element; the heating element is also used as a methane sensitive element; furthermore, the detection on low-concentration methane can be realized without a catalyst carrier and a catalyst material. The full-silicon MEMS methane sensor is processed by taking an SOI (silicon on insulator) silicon slice as a substrate and adopting an MEMS technology; the processing technology is compatible with a CMOS technology (complementary metal oxide semiconductor) technology. The full-silicon MEMS methane sensor has the characteristics of low power consumption, high sensitivity, no influence from oxygen deficit, and no influence of carbon deposition, poisoning and the like from catalysts.
Description
Technical field
The present invention relates to methane transducer and gas management application and preparation method, be particularly useful for a kind of industrial and mineral produce in gas prevention in use total silicon MEMS methane transducer and gas management application and preparation method.
Background technology
The current catalytic combustion type methane transducer heated based on traditional platinum filament is still in underground coal mine widespread use.Its principle is the catalyst combustion reaction heat release effect based on methane gas, there is its shortcomings owing to using catalyzer.As short in the adjustment cycle, carbon distribution, poisoning, activation etc. are fundamentally come to use catalyzer and catalyst support.Existing catalytic combustion type methane transducer adopts the coil of the noble metal coilings such as platinum filament as heating element, is difficult to mass production and consistance is poor, and power consumption is larger.Therefore, the application demand of Internet of Things to methane transducer is not well positioned to meet.Existing heat-conducted firedamp sensor at underground coal mine for detecting the methane gas based on methane of high concentration, low due to sensitivity lower than the methane gas based on methane of 4% for low concentration, cannot detection alarm be used for.
Summary of the invention
Technical matters: the object of this invention is to provide a kind of structure simple, do not use catalyzer, can detect that concentration is lower than 4% methane gas based on methane, and adopt cmos compatible MEMS technology, produce total silicon MEMS methane transducer and gas management application and preparation method easily.
Technical scheme: total silicon MEMS methane transducer of the present invention comprises silicon cell, stiff end and silicon frame bearing; Described silicon frame bearing is SOI substrate, and comprise silicon substrate, establish top layer silicon on buried regions monox on a silicon substrate and buried regions monox, top layer silicon is monocrystalline silicon;
On the buried regions monox of described stiff end on silicon frame bearing; Described stiff end comprises the silicon oxide layer outside silicon layer, silicon layer and is used as the metal level that electricity draws pad Pad; The silicon layer of stiff end is located on buried regions monox; Doped silicon layer is provided with in the support silicon layer of described stiff end; The metal level that described electricity draws pad Pad is located on the silicon oxide layer on silicon layer; Metal level directly contacts with the doped silicon layer of stiff end and forms Ohmic contact, and the two contact portion does not have silicon oxide layer;
Described silicon cell comprises silicon oxide layer outside silicon layer, silicon layer and passivation protection layer, described silicon cell be provided with silicon well heater, two symmetrically arranged for supporting silicon well heater and providing the silicon cantilever of electrical connection, the length at least 300um of described silicon cantilever for silicon well heater; One end of described single silicon cantilever is connected with silicon well heater, and the other end is connected with the stiff end on silicon frame bearing, and silicon well heater is suspended from air by two silicon cantilevers; Two silicon cantilevers are preferably and parallelly form U-shaped cantilever design side by side, with silicon overall heater; Silicon well heater can be the parallel connection of multiple silicon fire-bar, to have larger surface area; Described passivation protection layer is monox, or hafnia, or silica/alumina composite bed, or hafnia/aluminum oxide composite layers, or hafnia/silicon nitride composite bed, or aluminium oxide/silicon nitride composite bed, or monox/silicon nitride composite bed, or the composite bed that monox, hafnia, aluminium oxide, silicon nitride different materials are combined to form; The wherein thickness of monox at least 10nm, the thickness of hafnia is at least 5um, aluminium oxide thickness at least 6nm, and silicon nitride thickness is 10nm at least, and the thickness of whole passivation protection layer is no more than 1um;
The silicon layer of described silicon cell and the silicon layer of stiff end are both a part for the top layer silicon of SOI substrate, and be namely both a part for the top layer silicon of silicon frame bearing, shaped by top layer silicon, thickness is identical; But be not connected with other top layer silicon of silicon frame bearing; Only be connected with the silicon layer of silicon cell between the silicon layer of two stiff ends.
A kind of total silicon MEMS methane transducer CH_4 detection application process: make silicon cell work in operating point regions in current-resistance family curve on the left of turning point by applying voltage or pass to electric current on two stiff ends of the silicon cell of described total silicon MEMS methane transducer, the silicon well heater of silicon cell is generated heat, heating-up temperature more than 500 degrees Celsius, the power consumption about 80 ~ 90mW during work of single silicon cell, described turning point is that electrical resistance curtage increases the point of greatest resistance occurred, when curtage continues to increase, resistance no longer continues to increase and reduces on the contrary, when there being methane gas to occur, the temperature of the silicon well heater of total silicon MEMS methane transducer reduces, and the resistance of silicon cell is changed, use the silicon cell of the total silicon MEMS methane transducer described in two to form Wheatstone bridge and detect brachium pontis detection methane concentration, the silicon cell of one of them total silicon MEMS methane transducer contacts with surrounding air, the silicon cell of another total silicon MEMS methane transducer is air-tight packaging, gas in encapsulation and surrounding air are isolated to be sealed, when there is methane gas, the output voltage of favour stone detection electric bridge changes because the silicon cell resistance contacted with surrounding air reduces, the output voltage that favour stone detects electric bridge increases with methane concentration and reduces, realize the detection to methane gas, 10mV/CH can be reached to the detection sensitivity of low-concentration methane gas (0 ~ 4%)
4%, the response time can reach about 40ms.
The preparation method of total silicon MEMS methane transducer as claimed in claim 1, comprises three kinds of preparation methods, is specially:
The step of preparation method () is:
The first step, the top layer silicon on SOI substrate front prepares silicon oxide layer;
Second step, the silicon oxide layer on graphical top layer silicon, forms doping or the window needed for ion implantation;
3rd step, doping or ion implantation form doped silicon layer;
4th step, forms metal level by deposit, sputtering or evaporation on SOI substrate front;
5th step, the metal level that graphical 4th step is formed, forms the metal Pad that electricity draws pad, forms Ohmic contact after annealing;
6th step, photoetching forms front etching window figure, etch the silicon oxide layer got rid of in the etching window figure of front, adopt RIE (Reactive Ion Etching subsequently, reactive ion etching) method dry etching continues to get rid of top layer silicon, etching stopping is in buried regions monox, on buried regions silicon oxide layer, silicon cell is formed after etching, the structure graph of stiff end, and etch the remaining silicon oxide layer and top layer silicon got rid of in the window corresponding with back-etching window, the silicon cell formed and connected two stiff ends are not connected with all the other top layer silicon on buried regions silicon oxide layer, two stiff ends of same silicon cell are not connected with all the other top layer silicon on silicon frame bearing, also be not connected by all the other top layer silicon on silicon frame bearing,
7th step, etch-protecting layer is prepared in the front of SOI substrate, and adopt photoresist or PSG (phosphorosilicate glass) as etch-protecting layer, described etch-protecting layer covers the front of whole soi wafer;
8th step, after the photoetching of SOI substrate back forms back-etching graph window, adopt wet etching or ICP (Inductively Coupled Plasma, sense coupling) or DRIE (Deep Reactive Ion Etching, deep reaction ion etching) etc. dry etching method etching get rid of the silicon substrate of the SOI substrate that back-etching window exposes, etching stopping is in buried regions monox; Described back-etching window and front etching window coincide at the centre of figure of SOI silicon chip rear projection, and back-etching window is greater than front etching window;
9th step, the buried regions silicon oxide layer adopting hydrofluoric acid solution or hydrofluorite aerosol wet etching to expose from SOI substrate back, discharges silicon cell;
Tenth step, removes the etch-protecting layer prepared by the 7th step, dry;
11 step, is oxidized the silicon exposed, and forms oxide thin layer silicon layer;
12 step, adopt protective seam to cover the front of SOI substrate, described protective seam covers the SOI substrate front remainder except silicon cell; Can photoresist as protective seam; The preparation after accurately locating of micro-spray printing device can be adopted to be used as the photoresist of protective seam; Also the version of sheltering covering SOI substrate front can be used to adopt the described photoresist being used as protective seam of the method for spraying preparation, described in shelter version and only expose silicon cell, and remaining masked version in SOI substrate front portion shelters from;
13 step, ALD method is adopted to prepare hafnia film, or prepare aluminum oxide film, or prepare hafnia/alumina composite film, or prepare monox/hafnia/alumina composite film, form passivation protection layer by the 11 step and this step or by one of them step in the 11 step and this step; The passivation protection layer of preparation covers silicon cell outside surface;
14 step, removes the protective seam that the 12 step uses, dry;
15 step, carries out scribing along marking groove to SOI substrate, obtains a large amount of methane transducer of the present invention after sliver;
Or the step of preparation method (two) is:
The first step, the top layer silicon on SOI substrate front prepares silicon oxide layer;
Second step, the silicon oxide layer on graphical top layer silicon, forms doping or the window needed for ion implantation;
3rd step, doping or ion implantation form doped silicon layer;
4th step, photoetching forms front etching window figure, etch the silicon oxide layer got rid of in the etching window figure of front, RIE etching is adopted to continue to get rid of top layer silicon subsequently, etching stopping is in buried regions monox, on buried regions silicon oxide layer, silicon cell is formed after etching, the structure graph of stiff end, and etch the remaining silicon oxide layer and top layer silicon got rid of in the window corresponding with back-etching window, the silicon cell formed and connected two stiff ends are not connected with all the other top layer silicon on buried regions silicon oxide layer, two stiff ends of same silicon cell are not connected with all the other top layer silicon on silicon frame bearing, also be not connected by all the other top layer silicon on silicon frame bearing,
5th step, prepares etch-protecting layer in the front of SOI substrate, and adopt photoresist or PSG (phosphorosilicate glass) as etch-protecting layer, described etch-protecting layer covers the front of whole soi wafer;
6th step, after the photoetching of SOI substrate back forms back-etching graph window, adopt the dry etching method such as wet etching or ICP or DRIE etching to get rid of the silicon substrate of the SOI substrate that back-etching window exposes, etching stopping is in buried regions monox;
7th step, the buried regions silicon oxide layer adopting hydrofluoric acid solution or hydrofluorite aerosol wet etching to expose from silicon substrate, discharges unsettled silicon cell;
8th step, removes the etch-protecting layer that the 5th step is formed;
9th step, is oxidized the silicon exposed, and forms oxide thin layer silicon layer;
Tenth step, adopt protective seam to cover the front of SOI substrate, described protective seam covers the SOI substrate front remainder except unsettled silicon cell; Can photoresist as protective seam; The preparation after accurately locating of micro-spray printing device can be adopted to be used as the photoresist of protective seam; Also the version of sheltering covering SOI substrate front can be used to adopt the photoresist being used as protective seam described in the method preparation of spraying; Described version of sheltering only exposes silicon cell, and remaining masked version in SOI substrate front portion shelters from;
11 step, adopts ALD method to prepare aluminium oxide or hafnia film at the outside surface of silicon cell;
12 step, adopts PECVD to prepare silicon nitride at the outside surface of unsettled silicon cell 400 ~ 450 DEG C time; Monox/silicon nitride laminated film is prepared into by the combination of the 9th step, the 11 step and this step or above-mentioned three steps, or silica/alumina/silicon nitride laminated film, or hafnia/silicon nitride laminated film, or monox/hafnia/aluminium oxide/silicon nitride meets film, form passivation protection layer; The passivation protection layer of preparation covers silicon cell outside surface;
13 step, removes the protective seam that the tenth step uses, dry;
14 step, prepares photoresist in SOI substrate front, forms the figure that electricity draws the metal Pad of pad after photoetching;
15 step, prepares metal level by sputtering or depositing;
16 step, removes photoresist prepared by described 14 step, only at the upper metal Pad (22) forming electricity extraction pad of stiff end (102), dry, forms Ohmic contact after annealing;
17 step, carries out scribing along marking groove to SOI substrate, obtains a large amount of methane transducer of the present invention after sliver;
Or the step of preparation method (three) is:
The first step to the 13 step with the first step of preparation method to the 13 step,
14 step, version is sheltered in preparation, described in shelter the figure of version identical with the figure that the on-chip electricity of SOI draws the metal Pad of pad;
15 step, preparation electricity draws the metal Pad of pad, to be placed on SOI substrate front and splash-proofing sputtering metal after aiming at, only on stiff end, to form sheltering version described in the 14 step the metal Pad that electricity draws pad, forming Ohmic contact after annealing;
16 step, carries out scribing along marking groove to SOI substrate, obtains the methane transducer of One's name is legion of the present invention after sliver.
Beneficial effect: the silicon cell of total silicon MEMS methane transducer of the present invention and silicon well heater take silicon as heating material, not use metal as heating material, its silicon well heater by the support of silicon cantilever away from silicon substrate hang in atmosphere can electrified regulation to the high temperature of more than 500 DEG C, do not use catalyzer, the MEMS processing technology of employing and CMOS compatible.Owing to have employed such scheme, there is following effective effect:
The silicon well heater discharged from soi wafer is outstanding in atmosphere, well reduces the thermal loss by soi wafer, silicon well heater can be heated to the high temperature of more than 500 DEG C with lower power; Methane transducer of the present invention is not containing catalyzer and catalytic carrier, and therefore, the performance of sensor, by the impact of catalyzer, does not exist catalyst activity and reduces the problems such as the sensitivity decrease caused, poisoning, activation; Significantly for low-concentration methane gas; Methane transducer of the present invention has higher sensitivity, can reach 10mV/CH
4%, such sensitivity directly can promote instrument, reaches the requirement of national standard.
1, total silicon MEMS methane transducer of the present invention take silicon cell as heating element and methane detection element, does not use catalyzer can realize the detection of low-concentration methane gas (0 ~ 5%); The structure of silicon well heater of the present invention is the parallel form of multiple silicon fire-bar, has the larger pyrometric scale area contacted with air, can with high sensitivity technique low-concentration methane; The sensitivity of total silicon MEMS methane transducer of the present invention can reach 10mV/CH
4%, directly can promote instrument, meets national standard requirement.
2, methane transducer of the present invention is not containing catalyzer and catalytic carrier, and therefore, the performance of sensor, by the impact of catalyzer, does not exist catalyst activity and reduces the problems such as the sensitivity decrease caused, poisoning, activation; Further, the detection of methane transducer of the present invention to methane participates in without the need to oxygen, therefore not by the impact of oxygen in air;
3, the silicon well heater of total silicon MEMS methane transducer of the present invention is outstanding in atmosphere and away from silicon substrate by the support of silicon cantilever, distance is greater than more than 300um, silicon well heater can be heated to the high temperature of more than 500 DEG C with lower power, therefore there is advantage low in energy consumption, power consumption about 80 ~ 90mW during single silicon cell work.
4, the monocrystalline silicon of the employing stable performance of the silicon cell of total silicon MEMS methane transducer of the present invention obtains through MEMS technology processing, and this makes methane transducer of the present invention under hot operation state, have good stability and long life-span.The shortcomings such as the high temperature of the METAL HEATING PROCESS such as platinum, tungsten material more than 500 degrees Celsius easily volatilizees, distils this is because monocrystalline silicon does not exist, migration, also do not exist polysilicon resistance at high temperature grain boundary resistance be easy to the shortcoming that changes, cannot control.Meanwhile, the passivation layer arranged at the outside surface of silicon cell of the present invention also reduces the impact of external environment on above-mentioned components and parts, thus further increases the stability of methane transducer performance of the present invention.
5, the silicon cell of total silicon MEMS methane transducer of the present invention obtains through MEMS processing with silicon, processing technology is unified, simple, with SOI-CMOS process compatible, there is the advantage that production cost is low.
6, total silicon MEMS methane transducer size of the present invention is little, low in energy consumption, and fast response time, can reach about 40ms, linearity of output signal is good.
7, methane transducer of the present invention can adopt CMOS technology to produce in batches, can have good consistance and interchangeability, also can calibrate in batches, therefore can improve sensor performance further and reduce the cost of pick up calibration link.
Advantage: total silicon MEMS methane transducer provided by the invention has highly sensitive response signal to low-concentration methane, its preparation method can be compatible with CMOS technology, low, the easy batch production of cost and calibration, there is good consistance, interchangeability, methane transducer size of the present invention is little, fast response time, biosensor power consumption are low, highly sensitive, linearity of output signal is good, the life-span is long; Sensor performance, not by catalysts influence, need not consider the complex effects of catalyzer, simple when the performance of sensor is carried out to complex optimum and compensated.
Accompanying drawing explanation
Fig. 1 is that total silicon MEMS firedamp sensor of the present invention is in the on-chip schematic top plan view of SOI.
Fig. 2 is the schematic top plan view of the total silicon MEMS firedamp sensor of the present invention after scribing.
Fig. 3 is the A-A cross-sectional view in Fig. 1, Fig. 2 of the present invention.
Fig. 4 is a kind of structural representation of silicon well heater of the present invention.
Fig. 5 is the current-resistance family curve of the silicon cell of total silicon MEMS methane transducer of the present invention.
Fig. 6 is the methane resonse characteristic of total silicon MEMS methane transducer of the present invention.
In figure: 101-silicon cell, 102-stiff end, 103-silicon frame bearing; 104-front etching window, 105-back-etching window, 106-is along marking groove; 1011-silicon well heater, 1012-silicon cantilever, 1013-silicon fire-bar; 21-silicon layer, 22-electricity draws the metal of pad, 23-silicon oxide layer; 24-doped silicon layer, 25-passivation protection layer, 31-silicon substrate; 32-buried regions monox, 33-top layer silicon.
Embodiment
Below in conjunction with accompanying drawing, embodiments of the invention are further described:
Embodiment: in Fig. 1, Fig. 2, Fig. 3, this total silicon MEMS methane transducer comprises silicon cell 101, stiff end 102 and silicon frame bearing 103; Described silicon frame bearing 103 is SOI substrate, and comprise silicon substrate 31, be located at the buried regions monox 32 on silicon substrate 31 and the top layer silicon 33 on buried regions monox 32, top layer silicon 33 is monocrystalline silicon;
On the buried regions monox 32 of described stiff end 102 on silicon frame bearing 103; Described stiff end 102 comprises the silicon oxide layer 23 outside silicon layer 21, silicon layer 21 and is used as the metal Pad 22 that electricity draws pad; The silicon layer 21 of stiff end 102 is located on buried regions monox 12; Doped silicon layer 24 is provided with in the support silicon layer 21 of described stiff end 102; The metal Pad 22 that described electricity draws pad is located on the silicon oxide layer 23 on silicon layer 21; Metal level 22 directly contacts with the doped silicon layer 24 of stiff end 102 and forms Ohmic contact, and the two contact portion does not have silicon oxide layer 23;
Described silicon cell 101 comprises silicon oxide layer 23 outside silicon layer 21, silicon layer 21 and passivation protection layer 25, it is symmetrically arranged for supporting silicon well heater 1011 and providing the silicon cantilever 1012 of electrical connection, the length at least 300um of described silicon cantilever 1012 for silicon well heater 1011 that described silicon cell 101 is provided with silicon well heater 1011, two; One end of described single silicon cantilever 1012 is connected with silicon well heater 1011, and the other end is connected with the stiff end 102 on silicon frame bearing 103, and silicon well heater 1011 is suspended from air by two silicon cantilevers 1012; Two silicon cantilevers 1012 are preferably and parallelly form U-shaped cantilever design side by side, with silicon well heater 1011 entirety; Described passivation protection layer 25 is monox, or hafnia, or silica/alumina composite bed, or hafnia/aluminum oxide composite layers, or hafnia/silicon nitride composite bed, or aluminium oxide/silicon nitride composite bed, or monox/silicon nitride composite bed, or the composite bed that monox, hafnia, aluminium oxide, silicon nitride different materials are combined to form; The wherein thickness of monox at least 10nm, the thickness of hafnia is at least 5um, aluminium oxide thickness at least 6nm, and silicon nitride thickness is 10nm at least, and the thickness of whole passivation protection layer is no more than 1um;
Silicon layer 21 and the silicon layer 21 of stiff end 102 of described silicon cell 101 are both a part for the top layer silicon 33 of SOI substrate, and be namely both a part for the top layer silicon 33 of silicon frame bearing 103, shaped by top layer silicon 33, thickness is identical; But be not connected with other top layer silicon 33 of silicon frame bearing 103; Only be connected with the silicon layer 21 of silicon cell between the silicon layer 21 of two stiff ends 102.
Silicon well heater 1011 is as shown in Figure 4 parallel connections of multiple silicon fire-bar 1013, and to increase the pyrometric scale area contacted with air, silicon well heater 1011 also can be toroidal.
Fig. 5 is the current-resistance family curve of total silicon MEMS methane transducer of the present invention.
A kind of CH_4 detection application process of total silicon MEMS methane transducer, silicon cell 101 is made to work in operating point regions in current-resistance family curve on the left of turning point by applying voltage or pass to electric current on two stiff ends 102 of the silicon cell 101 of described total silicon MEMS methane transducer, the silicon well heater 1011 of silicon cell 101 is generated heat, heating-up temperature more than 500 degrees Celsius, power consumption about 80 ~ 90mW when single silicon cell 101 works, described turning point is that electrical resistance curtage increases the point of greatest resistance occurred, when curtage continues to increase, resistance does not increase in continuation and reduces on the contrary, when there being methane gas to occur, the temperature of the silicon well heater 1011 of total silicon MEMS methane transducer reduces, the resistance of silicon cell 101 is changed, use the silicon cell 101 of the total silicon MEMS methane transducer described in two to form Wheatstone bridge and detect brachium pontis detection methane concentration, the silicon cell 101 of one of them total silicon MEMS methane transducer contacts with surrounding air, the silicon cell 101 of another total silicon MEMS methane transducer is air-tight packaging, gas in encapsulation and surrounding air are isolated to be sealed, when there is methane gas, the output voltage of favour stone detection electric bridge changes because silicon cell 101 resistance contacted with surrounding air reduces, the output voltage that favour stone detects electric bridge increases with methane concentration and reduces, realize the detection to methane gas, 10mV/CH can be reached to the detection sensitivity of low-concentration methane gas (0 ~ 4%)
4%, the response time can reach about 40ms.
Fig. 6 is the methane resonse characteristic of total silicon MEMS methane transducer of the present invention.
The preparation method of total silicon MEMS methane transducer, comprises three kinds of preparation methods, is specially:
The step of preparation method () is:
The first step, the top layer silicon 33 on SOI substrate front prepares silicon oxide layer 23;
Second step, the silicon oxide layer 23 on graphical top layer silicon 33, forms doping or the window needed for ion implantation;
3rd step, doping or ion implantation form doped silicon layer 24;
4th step, forms metal level by deposit, sputtering or evaporation on SOI substrate front;
5th step, the metal level that graphical 4th step is formed, forms the metal Pad 22 that electricity draws pad, forms Ohmic contact after annealing;
6th step, photoetching forms front etching window 104 figure, etch the silicon oxide layer 23 got rid of in front etching window 104 figure, RIE dry etching is adopted to continue to get rid of top layer silicon 33 subsequently, etching stopping is in buried regions monox 32, on buried regions silicon oxide layer 32, silicon cell 101 is formed after etching, the structure graph of stiff end 102, and etch the remaining silicon oxide layer 23 and top layer silicon 33 got rid of in the window corresponding with back-etching window, the silicon cell 101 formed and connected two stiff ends 102 are not connected with all the other top layer silicon on buried regions silicon oxide layer 32, two stiff ends 102 of same silicon cell 101 are not connected with all the other top layer silicon on silicon frame bearing 103, also be not connected by all the other top layer silicon on silicon frame bearing 103,
7th step, etch-protecting layer is prepared in the front of SOI substrate, and adopt photoresist or PSG (phosphorosilicate glass) as etch-protecting layer, described etch-protecting layer covers the front of whole soi wafer;
8th step, after the photoetching of SOI substrate back forms back-etching window 105 figure, adopt the dry etching method such as wet etching or ICP or DRIE etching to get rid of the silicon substrate 31 of the SOI substrate that back-etching window exposes, etching stopping is in buried regions monox 32; Described back-etching window 105 coincides at the centre of figure of SOI silicon chip rear projection with front etching window 104, and back-etching window 105 is greater than front etching window 104;
9th step, the buried regions silicon oxide layer 32 adopting hydrofluoric acid solution or hydrofluorite aerosol wet etching to expose from SOI substrate back, discharges silicon cell 101;
Tenth step, removes the etch-protecting layer prepared by the 7th step, dry;
11 step, is oxidized the silicon exposed, and forms oxide thin layer silicon layer;
12 step, adopt protective seam to cover the front of SOI substrate, described protective seam covers the SOI substrate front remainder except silicon cell 101; Can photoresist as protective seam; The preparation after accurately locating of micro-spray printing device can be adopted to be used as the photoresist of protective seam; Also the version of sheltering covering SOI substrate front can be used to adopt the described photoresist being used as protective seam of the method for spraying preparation, described in shelter version and only expose silicon cell 101, and remaining masked version in SOI substrate front portion shelters from;
13 step, ALD Atomic layer deposition method is adopted to prepare hafnia film, or prepare aluminum oxide film, or prepare hafnia/alumina composite film, or prepare monox/hafnia/alumina composite film, form passivation protection layer 25 by the 11 step and this step or by one of them step in the 11 step and this step; The passivation protection layer 25 of preparation covers silicon cell 101 outside surface;
14 step, removes the protective seam that the 12 step uses, dry;
15 step, carries out scribing along marking groove 106 pairs of SOI substrates, obtains a large amount of methane transducer of the present invention after sliver.
The step of preparation method (two) is:
The first step, the top layer silicon 33 on SOI substrate front prepares silicon oxide layer 23;
Second step, the silicon oxide layer 23 on graphical top layer silicon 33, forms doping or the window needed for ion implantation;
3rd step, doping or ion implantation form doped silicon layer 24;
4th step, photoetching forms front etching window 104 figure, etch the silicon oxide layer 23 got rid of in front etching window 104 figure, RIE dry etching is adopted to continue to get rid of top layer silicon 33 subsequently, etching stopping is in buried regions monox 32, on buried regions silicon oxide layer 32, silicon cell 101 is formed after etching, the structure graph of stiff end 102, and etch the remaining silicon oxide layer 23 and top layer silicon 33 got rid of in the window corresponding with back-etching window, the silicon cell 101 formed and connected two stiff ends 102 are not connected with all the other top layer silicon on buried regions silicon oxide layer 32, two stiff ends 102 of same silicon cell 101 are not connected with all the other top layer silicon on silicon frame bearing 103, also be not connected by all the other top layer silicon on silicon frame bearing 103,
5th step, prepares etch-protecting layer on the front top layer silicon of SOI substrate, and adopt photoresist or PSG (phosphorosilicate glass) as etch-protecting layer, described etch-protecting layer covers the front of whole soi wafer;
6th step, after the photoetching of SOI substrate back forms back-etching window 105 figure, adopt the dry etching method such as wet etching or ICP or DRIE etching to get rid of the silicon substrate 31 of the SOI substrate that back-etching window exposes, etching stopping is in buried regions monox 32;
7th step, the buried regions silicon oxide layer 32 adopting hydrofluoric acid solution or hydrofluorite aerosol wet etching to expose from silicon substrate 31, discharges unsettled silicon cell 101;
8th step, removes the etch-protecting layer that the 5th step is formed;
9th step, is oxidized the silicon exposed, and forms oxide thin layer silicon layer;
Tenth step, adopt protective seam to cover the front of SOI substrate, described protective seam covers the SOI substrate front remainder except unsettled silicon cell 101; Can photoresist as protective seam; The preparation after accurately locating of micro-spray printing device can be adopted to be used as the photoresist of protective seam; Also the version of sheltering covering SOI substrate front can be used to adopt the photoresist being used as protective seam described in the method preparation of spraying; Described version of sheltering only exposes silicon cell 101, and remaining masked version in SOI substrate front portion shelters from;
11 step, adopts ALD Atomic layer deposition method to prepare aluminium oxide or hafnia film at the outside surface of silicon cell 101;
12 step, adopts PECVD (Plasma Enhanced Chemical Vapor Deposition, plasma enhanced chemical vapor deposition method) to prepare silicon nitride at the outside surface of unsettled silicon cell 101 400 ~ 450 DEG C time; Monox/silicon nitride laminated film is prepared into by the combination of the 9th step, the 11 step and this step or above-mentioned three steps, or silica/alumina/silicon nitride laminated film, or hafnia/silicon nitride laminated film, or monox/hafnia/aluminium oxide/silicon nitride meets film, form passivation protection layer 25; The passivation protection layer 25 of preparation covers silicon cell 101 outside surface;
13 step, removes the protective seam that the tenth step uses, dry;
14 step, prepares photoresist in SOI substrate front, forms the figure that electricity draws the metal Pad 22 of pad after photoetching;
15 step, prepares metal level by sputtering or depositing;
16 step, removes photoresist prepared by described 14 step, only at the upper metal Pad (22) forming electricity extraction pad of stiff end (102), dry, forms Ohmic contact after annealing;
17 step, carries out scribing along marking groove 106 pairs of SOI substrates, obtains a large amount of methane transducer of the present invention after sliver.
The step of preparation method (three) is:
The first step to the first step of the same preparation method of the 13 step (two) to the 13 step,
14 step, version is sheltered in preparation, described in shelter the figure of version identical with the figure that the on-chip electricity of SOI draws the metal Pad 22 of pad;
15 step, preparation electricity draws the metal Pad 22 of pad, to be placed on SOI substrate front and splash-proofing sputtering metal after aiming at, only on stiff end 102, to form sheltering version described in the 14 step the metal Pad 22 that electricity draws pad, forming Ohmic contact after annealing;
16 step, carries out scribing along marking groove 106 pairs of SOI substrates, obtains the methane transducer of One's name is legion of the present invention after sliver.
Claims (3)
1. a total silicon MEMS methane transducer, is characterized in that: it comprises silicon cell (101), stiff end (102) and silicon frame bearing (103); Described silicon frame bearing (103) is SOI substrate, and comprise silicon substrate (31), be located at the buried regions monox (32) on silicon substrate (31) and the top layer silicon (33) on buried regions monox (32), top layer silicon (33) is monocrystalline silicon;
Described stiff end (102) is located on the buried regions monox (32) on silicon frame bearing (103); Described stiff end (102) comprises silicon layer (21), silicon layer (21) silicon oxide layer outward (23) and is used as the metal Pad(22 that electricity draws pad); The silicon layer (21) of stiff end (102) is located on buried regions monox (12); Doped silicon layer (24) is provided with in the silicon layer (21) of described stiff end (102); Described electricity draws the metal Pad(22 of pad) be located on silicon layer (21) silicon oxide layer (23) on; Metal level (22) directly contacts with the doped silicon layer (24) of stiff end (102) and forms Ohmic contact, and the two contact portion does not have silicon oxide layer (23);
Described silicon cell (101) comprises silicon layer (21), silicon layer (21) silicon oxide layer outward (23) and passivation protection layer (25), described silicon cell (101) be provided with silicon well heater (1011), two symmetrically arranged for supporting silicon well heater (1011) and providing the silicon cantilever (1012) of electrical connection, the length at least 300um of described silicon cantilever (1012) for silicon well heater (1011); One end of described single silicon cantilever (1012) is connected with silicon well heater (1011), and the other end is connected with the stiff end (102) on silicon frame bearing (103), and silicon well heater (1011) is suspended from air by two silicon cantilevers (1012); Two silicon cantilevers (1012) are preferably and parallelly form U-shaped cantilever design side by side, with silicon well heater (1011) entirety; Described passivation protection layer (25) is monox, or hafnia, or silica/alumina composite bed, or hafnia/aluminum oxide composite layers, or hafnia/silicon nitride composite bed, or aluminium oxide/silicon nitride composite bed, or monox/silicon nitride composite bed, or the composite bed that monox, hafnia, aluminium oxide, silicon nitride different materials are combined to form; The wherein thickness of monox at least 10nm, the thickness of hafnia is at least 5um, aluminium oxide thickness at least 6nm, and silicon nitride thickness is 10nm at least, and the thickness of whole passivation protection layer is no more than 1um;
The silicon layer (21) of described silicon cell (101) and the silicon layer (21) of stiff end (102) are both a part for the top layer silicon (33) of SOI substrate, namely a part for the top layer silicon (33) of silicon frame bearing (103) is both, shaped by top layer silicon (33), thickness is identical; But be not connected with other top layer silicon (33) of silicon frame bearing (103); Only be connected with the silicon layer (21) of silicon cell between the silicon layer (21) of two stiff ends (102).
2. a total silicon MEMS methane transducer CH_4 detection application process, it is characterized in that: by making silicon cell (101) work in operating point regions in current-resistance family curve on the left of turning point at upper voltage or the electric current of applying of two stiff ends (102) of described total silicon MEMS methane transducer, the silicon well heater (1011) of silicon cell (101) is generated heat, and heating-up temperature is more than 500 degrees Celsius, described turning point is that electrical resistance curtage increases the point of greatest resistance occurred, when curtage continues to increase, resistance no longer continues to increase and reduces on the contrary, when there being methane gas to occur, the temperature of the silicon well heater (1011) of total silicon MEMS methane transducer reduces, and the resistance of silicon cell is changed, use the silicon cell (101) of the total silicon MEMS methane transducer described in two to form Wheatstone bridge and detect brachium pontis detection methane concentration, the silicon cell (101) of one of them total silicon MEMS methane transducer contacts with surrounding air, the silicon cell (101) of another total silicon MEMS methane transducer is air-tight packaging, gas in encapsulation and surrounding air are isolated to be sealed, when there is methane gas, the output voltage of favour stone detection electric bridge changes because silicon cell (101) resistance contacted with surrounding air reduces, the output voltage that favour stone detects electric bridge increases with methane concentration and reduces, realize the detection to methane gas.
3. the preparation method of total silicon MEMS methane transducer as claimed in claim 1, is characterized in that comprising three kinds of preparation methods;
The step of preparation method () is:
The first step, the top layer silicon (33) on SOI substrate front prepares silicon oxide layer (23);
Second step, the silicon oxide layer (23) on graphical top layer silicon (33), forms doping or the window needed for ion implantation;
3rd step, doping or ion implantation form doped silicon layer (24);
4th step, forms metal level by deposit, sputtering or evaporation on SOI substrate front;
5th step, the metal level that graphical 4th step is formed, forms the metal Pad(22 that electricity draws pad), form Ohmic contact after annealing;
6th step, photoetching forms front etching window (104) figure, etch the silicon oxide layer (23) got rid of in front etching window (104) figure, adopt RIE(Reactive Ion Etching subsequently, reactive ion etching) method dry etching continues to get rid of top layer silicon (33), etching stopping is in buried regions monox (32), on buried regions silicon oxide layer (32), silicon cell (101) is formed after etching, the structure graph of stiff end (102), and etch the remaining silicon oxide layer (23) and top layer silicon (33) got rid of in the window corresponding with back-etching window, the silicon cell (101) formed and connected two stiff ends (102) are not connected with all the other top layer silicon on buried regions silicon oxide layer (32), two stiff ends (102) of same silicon cell (101) are not connected with all the other top layer silicon on silicon frame bearing (103), also be not connected by all the other top layer silicon on silicon frame bearing (103),
7th step, etch-protecting layer is prepared in the front of SOI substrate, and described etch-protecting layer covers the front of whole soi wafer;
8th step, after the photoetching of SOI substrate back forms back-etching window (105) figure, adopt wet etching or ICP (Inductively Coupled Plasma, sense coupling) or DRIE(Deep Reactive Ion Etching, deep reaction ion etching) etc. dry etching method etching get rid of the silicon substrate (31) of the SOI substrate that back-etching window exposes, etching stopping is in buried regions monox (32); Described back-etching window (105) and front etching window (104) coincide at the centre of figure of SOI silicon chip rear projection, and back-etching window (105) is greater than front etching window (104);
9th step, the buried regions silicon oxide layer (32) adopting hydrofluoric acid solution or hydrofluorite aerosol wet etching to expose from SOI substrate back, discharges silicon cell (101);
Tenth step, removes the etch-protecting layer prepared by the 7th step, dry;
11 step, is oxidized the silicon exposed, and forms oxide thin layer silicon layer;
12 step, adopt protective seam to cover the front of SOI substrate, described protective seam covers the SOI substrate front portion except silicon cell (101);
13 step, adopting ALD(ald) method prepares hafnia film, or prepare aluminum oxide film, or prepare hafnia/alumina composite film, or prepare monox/hafnia/alumina composite film, form passivation protection layer (25) by the 11 step and this step or by one of them step in the 11 step and this step; The passivation protection layer (25) of preparation covers silicon cell (101) outside surface;
14 step, removes the protective seam that the 12 step uses, dry;
15 step, carries out scribing along marking groove (106) to SOI substrate, obtains a large amount of methane transducer of the present invention after sliver;
Or the step of preparation method (two) is:
The first step, the top layer silicon (33) on SOI substrate front prepares silicon oxide layer (23);
Second step, the silicon oxide layer (23) on graphical top layer silicon (33), forms doping or the window needed for ion implantation;
3rd step, doping or ion implantation form doped silicon layer (24);
4th step, photoetching forms front etching window (104) figure, etch the silicon oxide layer (23) got rid of in front etching window (104) figure, adopt RIE(Reactive Ion Etching subsequently, reactive ion etching) method dry etching continues to get rid of top layer silicon (33), etching stopping is in buried regions monox (32), on buried regions silicon oxide layer (32), silicon cell (101) is formed after etching, the structure graph of stiff end (102), and etch the remaining silicon oxide layer (23) and top layer silicon (33) got rid of in the window corresponding with back-etching window, the silicon cell (101) formed and connected two stiff ends (102) are not connected with all the other top layer silicon on buried regions silicon oxide layer (32), two stiff ends (102) of same silicon cell (101) are not connected with all the other top layer silicon on silicon frame bearing (103), also be not connected by all the other top layer silicon on silicon frame bearing (103),
5th step, prepare etch-protecting layer in the front (above top layer silicon) of SOI substrate, described etch-protecting layer covers the front of whole soi wafer;
6th step, after the photoetching of SOI substrate back forms back-etching window (105) figure, adopt wet etching or ICP (Inductively Coupled Plasma, sense coupling) or DRIE(Deep Reactive Ion Etching, deep reaction ion etching) etc. dry etching method etching get rid of the silicon substrate (31) of the SOI substrate that back-etching window exposes, etching stopping is in buried regions monox (32);
7th step, the buried regions silicon oxide layer (32) adopting hydrofluoric acid solution or hydrofluorite aerosol wet etching to expose from silicon substrate (31), discharges unsettled silicon cell (101);
8th step, removes the etch-protecting layer that the 5th step is formed;
9th step, is oxidized the silicon exposed, and forms oxide thin layer silicon layer;
Tenth step, adopt protective seam to cover the front of SOI substrate, described protective seam covers the SOI substrate front portion except unsettled silicon cell (101)
11 step, adopts ALD(ald) method prepares aluminium oxide or hafnia film at the outside surface of silicon cell (101);
12 step, adopts PECVD (Plasma Enhanced Chemical Vapor Deposition, plasma enhanced chemical vapor deposition method) to prepare silicon nitride at the outside surface of unsettled silicon cell (101) 400 ~ 450 DEG C time; Monox/silicon nitride laminated film is prepared into by the combination of the 9th step, the 11 step and this step or above-mentioned three steps, or silica/alumina/silicon nitride laminated film, or hafnia/silicon nitride laminated film, or monox/hafnia/aluminium oxide/silicon nitride meets film, form passivation protection layer (25); The passivation protection layer (25) of preparation covers silicon cell (101) outside surface;
13 step, removes the protective seam that the tenth step uses, dry;
14 step, prepares photoresist in SOI substrate front, forms electricity and draw the metal Pad(22 of pad after photoetching) figure;
15 step, prepares metal level by sputtering or depositing;
16 step, removes photoresist prepared by described 14 step, only at the upper metal Pad(22 forming electricity extraction pad of stiff end (102)), dry, form Ohmic contact after annealing;
17 step, carries out scribing along marking groove (106) to SOI substrate, obtains a large amount of methane transducer of the present invention after sliver;
Or the step of preparation method (three) is:
The first step to the first step of the same preparation method of the 13 step (two) to the 13 step,
14 step, version is sheltered in preparation, described in shelter version figure and the on-chip electricity of SOI draw the metal Pad(22 of pad) figure identical;
15 step, preparation electricity draws the metal Pad(22 of pad), to be placed in sheltering version described in the 14 step on SOI substrate front and splash-proofing sputtering metal after aiming at, only on stiff end (102), to form the metal Pad(22 that electricity draws pad), form Ohmic contact after annealing;
16 step, carries out scribing along marking groove (106) to SOI substrate, obtains the methane transducer of One's name is legion of the present invention after sliver.
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| PCT/CN2015/093096 WO2016066106A1 (en) | 2014-10-31 | 2015-10-28 | All-silicon mems methane sensor, fuel gas detection application, and manufacturing method |
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| CN109844511A (en) * | 2016-11-04 | 2019-06-04 | Msa技术有限公司 | Combustible gas sensor and the method for identifying fuel gas type for the pulse operation via combustible gas sensor |
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