CN103675048A - Metal-oxide gas sensor based on MEMS (Micro-Electro-Mechanic System) and preparation technology thereof - Google Patents
Metal-oxide gas sensor based on MEMS (Micro-Electro-Mechanic System) and preparation technology thereof Download PDFInfo
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Abstract
The invention discloses a metal-oxide gas sensor based on MEMS (Micro-Electro-Mechanic System) and a preparation technology thereof. The gas sensor is characterized by comprising an Si substrate, an insulating layer, two thin-film resistor heating elements, a rectangular micro array, a pair of sensitive electrodes and a metallic oxide three-dimensional multi-level nano-structure produced on the rectangular micro array, wherein partial Si at the lower part of the Si base is removed in an anisotropic manner through wet etching; at the front of the gas sensor, the heating elements and the sensitive electrodes are arranged in a central symmetry and spiral manner, the rectangular micro array is arranged in the center, and the heating elements, the sensitive electrodes and the rectangular micro array are positioned on the same layer; the heating elements can also serve as temperature detecting elements. According to the invention, the nano-structure synthetized by adopting a hydrothermal method can realize the bridge type electrical connection through the mutually crossed dendritic structures, and is finally connected with the sensitive electrodes; the arrangement manner of the rectangular micro array is changed, and nano-materials of different types are replaced, so that the metal-oxide nano gas sensor based on different measuring circuits and sensitive materials of different types can be processed.
Description
Technical field
The present invention relates to a kind of based on MEMS(Micro-Electro-Mechanic System MEMS (micro electro mechanical system)) metal-oxide gas transducer structure and the preparation method of technique.
Background technology
For public safety with healthy, the composition in efficient detection indusrial toxic gas, flammable explosion hazard gases, chemical weapons and with the chemical composition of disease association, seem very important.And develop there is hypersensitivity, high selectivity, fast the speed of response, short release time, can long-term stable operation (being so-called 4S index, Sensitivity, Selectivity, Speed, Stability) chemical sensor be also the target that researchers pursue always.
Nineteen fifty-two Brattain and Bardeen have found the gas-sensitive property of semiconductor Germanium (Ge) first, and this characteristic is also found in metal oxide by Seiyama subsequently.After this, the semiconductor gas sensor based on metal oxide is developed out.It is to be noted, metal oxide only has at a certain temperature just can have good gas-sensitive property, therefore the gas sensor based on this kind of sensitive material all can an integrated heating element, and this heating element energy consumption accounts for absolute specific gravity in the power consumption of whole device.For the needs that improve aforesaid what is called " 4S " index, reduction device power consumption, the all constantly evolution along with the development of technology of sensitive materials form, heating element form and the integration mode of the two, such gas sensor technology has roughly experienced following 3 developing stage:
1. classical Taguchi metal-oxide gas transducer pattern;
2. the metal-oxide gas transducer pattern based on thick-film technique (serigraphy);
3. the metal-oxide gas transducer pattern based on MEMS thin-film technique.
Aspect sensitive material, there is in recent years metal oxide nanostructure (as nano wire), because it has extraordinary sensitivity characteristic and response speed, higher selectivity and stability, lower working temperature and power consumption, possesses the possibility of the radio communication of realizing, and be expected to become gas sensor high-performance sensitive material of future generation.Yet nano material volume is small, synthetic method is special, cause its picking up, transfer, regularly arrange, mechanics adhesion, electricity connects and the aspect such as process compatible exists many difficult problems.Although the experimental prototype of nano gas sensor occurs, the relevant device that it need to be expensive and complicated technological process, this is also not suitable with large-scale production cheaply.
Aspect heating element, the sheet resistance based on MEMS technique remains main flow heating source.
Aspect sensitive element (containing sensitive material and sensitive electrode) and heating element integrated, traditional mode that the two lamination is placed has increased process complexity, and thereupon membrane stress has also reduced the yield rate of device.
Summary of the invention
The technical problem to be solved in the present invention be to overcome nanostructured described in background technology picking up, transfer, regularly arrange, mechanics adhesion, electricity connects and process compatible aspect difficulty, utilize MEMS technology with the machining path of top-down, to realize the accurate location of nanostructured, utilize the hydro-thermal method of simple and easy cheapness with the machining path of bottom-up, to realize the growth in situ of metal oxide three-dimensional multistage nanostructured.Meanwhile, sensitive element and heating element are placed in to same layer, simplify the integrated technique of sensor.
For achieving the above object, the present invention takes following technical scheme to be achieved:
A kind of metal-oxide gas transducer based on MEMS, be respectively masking layer, Si substrate, insulation course from bottom to top, wherein Si substrate back has insulated tank, it is characterized in that, on described insulation course, be provided with a pair of heating element and lead wire tray, a pair of sensitive electrode and lead wire tray, rectangle microarray, described rectangle microarray is positioned at the central area on insulation course, on this rectangle microarray, growth has metal oxide three-dimensional multistage nanostructured, this structure to realize electricity by cross one another dendritic overlap joint to connect.
In such scheme, described a pair of heating element is according to Central Symmetry, spiral way layout, and a rectangular area is vacated in the two relative center; In this rectangular area and inside heating element, according to Central Symmetry, spiral way, be furnished with a pair of sensitive electrode, the two relative center forms interior rectangle region, wherein arranges rectangle microarray; Described two heating elements are respectively containing a pair of independent lead wire tray, are distributed in insulation course upper surface near the position of four jiaos; Each own lead wire tray of each sensitive electrode, is symmetrically distributed in insulation course upper surface near the position of an opposite side.
Described heating element, sensitive electrode and rectangle microarray all adopt Ti-Pt film to make; Described metal oxide is TiO
2.Described masking layer, insulation course are by SiO
2-Si
3n
4be composited.
A preparation technology for aforementioned metal oxide gas sensor, is characterized in that, comprises the steps:
(1) in Si backside of substrate, front, adopt respectively thermal oxide, LPCVD depositing operation to prepare masking layer and insulation course;
(2), on the insulation course of front, by photoetching, magnetron sputtering technique processing, make heating element and lead wire tray, sensitive electrode and the lead wire tray thereof that thickness is not less than 300nm;
(3) by photoetching, magnetron sputtering technique center region processing on insulation course, go out thickness and be not less than 300nm rectangle microarray; Repeat photoetching process, define the growth array of metal oxide three-dimensional multistage nanostructured;
(4) by photoetching, wet-etching technology, remove masking layer and the Si substrate itself of Si backside of substrate, form the silicon chip with insulated tank;
(5), on the growth array of step (3) definition, utilize hydrothermal synthesis method to grow by cross one another dendritic overlap joint and realize the metal oxide three-dimensional multistage nanostructured that electricity connects.
In said method, the mass concentration of described hydrochloric acid is 37%.
Describedly utilize hydrothermal synthesis method to grow the concrete technology of realizing the metal oxide three-dimensional multistage nanostructured that electricity connects by cross one another dendritic overlap joint to be:
A, by butyl titanate, hydrochloric acid, oleic acid by volume 1:1:5 mix, after magnetic agitation, put into high-pressure hydrothermal reaction kettle;
B, will remove Si backside of substrate masking layer and Si substrate itself, formation is put into the reactor described in step a with the silicon chip of insulated tank, in 200 degrees Celsius of following insulations, after at least 4 hours, take out, with absolute ethyl alcohol, clean and remove unnecessary organism for several times, with acetone, wash away unnecessary photoresist, after being dried, obtain TiO
2nano gas sensor.
Wherein, described dry be to bake and bank up with earth 4 hours under 80 degrees Celsius, air ambient.
Compared with prior art, the present invention has the following advantages:
1, in technology intersection aspect, the present invention combines the advantage separately of MEMS technology and nanometer technology, the former provides each element of sensor accurate location of (comprising the nanostructured as sensitive material), the sensitive material of the latter provides cheap, easy nanostructured synthetic method and high-performance (being good " 4S " index).
2, aspect heating element, the present invention uses two centrosymmetric sheet resistances, a symmetrical homogeneous temperature field can be provided, compare some asymmetric arrangement mode, reduce because temperature field is asymmetric, the risk of the excessive film breaks causing of extra heat stress.
3, aspect sensitive element, (comprise sensitive material, sensitive electrode structure), in the present invention as the metal oxide three-dimensional multistage nanostructured original position life of sensitive materials on described rectangle microarray and regulated and controled by it, between nanostructured, by cross one another dendritic morphology, realizing bridge-type electricity connects, avoided general nano gas sensor required pick up, the processing step such as transfer, and nanostructured regular arranged, mechanics adhesion, electricity connect also and automatically realize in process.In addition, by changing rectangle microarray arrangement mode, changing different types of nano material, can process based on different measuring path (series-parallel or other complex forms), based on variety classes sensitive materials (TiO
2, SnO
2, ZnO, CuO etc.) metal oxide nano gas sensor.
4, aspect heating element and sensitive element integrated, the present invention is arranged in same layer by the two by Central Symmetry, spiral way, has simplified processing technology, can reduce the not high risk of yield rate causing because of the existence of multilayer film complex stress.
Accompanying drawing explanation
Below in conjunction with the drawings and the specific embodiments, the present invention is described in further detail.
Fig. 1 is the structural representation of metal oxide nano gas sensor of the present invention.Wherein (a) figure is each layer of section of sensor; In figure: 1, Si
3n
4masking layer; 2, SiO
2masking layer; 3, Si substrate; 4, SiO
2insulation course; 5, Si
3n
4insulation course; 6, Ti ?Pt lead wire tray; 7, heating element (Ti ?Pt sheet resistance); 8, Ti ?Pt sensitive electrode; 9, Ti ?Pt rectangle microarray; 10, three-dimensional multistage nanostructured; 11, insulated tank; 12, rectangular area; 13, interior rectangle region.(b) figure is sensor three-dimensional structure, visible Si substrate, six lead wire tray (four of diagonal position is heating element lead wire tray, and relative two in center are sensitive element lead wire tray).(c) figure is the two plane figure of heating element, sensitive element (containing sensitive electrode, rectangle microarray, nano-structure array).(d) figure be long on rectangle microarray, cross one another nanostructured.
Fig. 2 is the heating element [(a) figure] of sensor of the present invention, the planar structure of sensitive electrode [(b) figure].
Fig. 3 is for realizing the sensitive element schematic diagram of series connection Measure Channel.
Fig. 4 is the sensitive element schematic diagram of realizing Measure Channel in parallel.
Fig. 5 is for realizing the sensitive element schematic diagram of string duplex measurement path.
Embodiment
The metal oxide sensitive materials of gas sensor of the present invention are with TiO
2for example, but be not limited to TiO
2, can be also SnO
2, ZnO, CuO.By changing the kind of metal oxide, or multiple material compound use, the gas sensor of different kinds can be made.
As shown in Figure 1, a kind of metal oxide nano gas sensor based on MEMS, is respectively the Si of wet etching from bottom to top
3n
4masking layer 1, SiO
2masking layer 2, Si substrate 3, SiO
2insulation course 4, Si
3n
4the heating element 7 that insulation course 5, a pair of Ti-Pt sheet resistance are made and Ti-Pt sensitive electrode 8 and Ti-Pt rectangle microarray 9, wherein, on rectangle microarray 9, regrowth has one deck TiO
2three-dimensional multistage nanostructured 10.The Si of Si substrate 3 back certain areas
3n
4, SiO
2masking layer and Si are removed and form insulated tank 11[Fig. 1 (a) by wet etching].
With reference to figure 2(a), a pair of Ti-Pt heating element 7 is according to Central Symmetry, spiral way layout, and 12, two of the rectangular areas heating element of 220 μ m*150 μ m is vacated respectively containing a pair of independent lead wire tray 6 in the two relative center, is distributed in silicon chip Si
3n
4insulation course upper surface is near the position of four jiaos.With reference to figure 2(b), in heating element and inner side, rectangular area, according to Central Symmetry, spiral way, be furnished with a pair of Ti-Pt sensitive electrode 8, each own lead wire tray of each sensitive electrode.Rectangle region 13 in forming between sensitive electrode, wherein arranges Ti-Pt rectangle microarray 9.With reference to figure 1(c), Fig. 1 (d), on rectangle microarray 9, growth has a TiO
2three-dimensional multistage nanostructured 10, this nanostructured is by cross one another dendritic overlap joint, to realize electricity to connect.
As shown in Fig. 3, Fig. 4, Fig. 5, the growth position of nanostructured 10 is subject to 9 regulation and control of rectangle microarray, by changing the arrangement mode of rectangle dimension array, realizes electricity access paths different between nanostructured, finally realizes multi-form Measure Channel.For Fig. 3, to be that M * 1 is single-row arrange rectangular array, forms with sensitive electrode the Measure Channel of connecting; For Fig. 4, rectangular array is that 1 * N single file is arranged, and every the rectangle being listed as, is directly connected with same electrode, is prong shape, finally forms Measure Channel in parallel; For Fig. 5, rectangular array is that M * N arranges, and each little rectangle is connected by nanostructured with adjacent four rectangles, forms the also Measure Channel (above m, n are all greater than 1) of mixed form of string with sensitive electrode.
When heating element is worked (as produced the temperature field of 200 degrees Celsius), if certain specific gas (as oxygen) concentration changes in the environment of sensor place, can there is marked change in the resistivity of nanostructured, the especially resistance of the bridge-type junction of intersection, by measuring the resistance variations between sensitive electrode, can indirectly measure the concentration of ambient atmos.
The preparation technology of the metal oxide nano gas sensor shown in Fig. 1 is as follows:
(1) SiO of Si substrate 3 Double-side hot oxidation 500nm
2masking layer 2, SiO
2insulation course 4, LPCVD(Low Pressure Chemical Vapor Deposition) Si of deposition 150nm
3n
4masking layer 1, Si
3n
4insulation course 5;
(2) at positive Si
3n
4on insulation course 5, by photoetching, magnetron sputtering technique processing, make Ti-Pt thin film resistive layer (heating element 7) and lead wire tray, Ti-Pt sensitive electrode 8 and lead wire tray thereof, thickness is greater than 300nm;
(3) by the Si of rectangle region 13 in photoetching, magnetron sputtering technique are between sensitive electrode
3n
4on insulation course, process Ti-Pt rectangle microarray 9, Ti thickness is 50nm, and Pt thickness is 250nm, repeats photoetching process, defines TiO
2the growth array of three-dimensional multistage nanostructured 10;
(4) by photoetching process, ICP(plasma etching) remove the Si at back
3n
4masking layer, removes the SiO at back with wet-etching technology (as hydrofluorite)
2masking layer, then form insulated tank 11 with the Si substrate of wet-etching technology one side etching back;
(5) butyl titanate, hydrochloric acid (mass concentration 37%), oleic acid 1:1:5 mixing by volume, magnetic agitation is put into after 30 minutes containing teflon-lined high-pressure hydrothermal reaction kettle;
(6) silicon chip obtaining in (4) is put into reactor described in (5), be placed in after being incubated 4 hours under 180 degrees Celsius and take out, with absolute ethyl alcohol, clean and to remove unnecessary organism for several times, with acetone, wash away unnecessary photoresist, under 80 degrees Celsius, air ambient, bake and bank up with earth 4 hours.
Claims (8)
1. the metal-oxide gas transducer based on MEMS, be respectively masking layer, Si substrate, insulation course from bottom to top, wherein Si substrate back has insulated tank, it is characterized in that, on described insulation course, be provided with a pair of heating element and lead wire tray, a pair of sensitive electrode and lead wire tray, rectangle microarray, described rectangle microarray is positioned at the central area on insulation course, on this rectangle microarray, growth has metal oxide three-dimensional multistage nanostructured, this structure to realize electricity by cross one another dendritic overlap joint to connect.
2. the metal-oxide gas transducer based on MEMS as claimed in claim 1, is characterized in that, described a pair of heating element is according to Central Symmetry, spiral way layout, and a rectangular area is vacated in the two relative center; In this rectangular area and inside heating element, according to Central Symmetry, spiral way, be furnished with a pair of sensitive electrode, the two relative center forms interior rectangle region, wherein arranges rectangle microarray; Described two heating elements are respectively containing a pair of independent lead wire tray, are distributed in insulation course upper surface near the position of four jiaos; Each own lead wire tray of each sensitive electrode, is symmetrically distributed in insulation course upper surface near the position of an opposite side.
3. the metal-oxide gas transducer based on MEMS as claimed in claim 1, is characterized in that, described heating element, sensitive electrode and rectangle microarray all adopt Ti-Pt film to make; Described metal oxide is TiO
2.
4. the metal-oxide gas transducer based on MEMS as claimed in claim 1, is characterized in that, described masking layer, insulation course are by SiO
2-Si
3n
4be composited.
5. a preparation technology for the metal-oxide gas transducer based on MEMS claimed in claim 1, is characterized in that, comprises the steps:
(1) in Si backside of substrate, front, adopt respectively thermal oxide, LPCVD depositing operation to prepare masking layer and insulation course;
(2), on the insulation course of front, by photoetching, magnetron sputtering technique processing, make heating element and lead wire tray, sensitive electrode and the lead wire tray thereof that thickness is not less than 300nm;
(3) by photoetching, magnetron sputtering technique center region processing on insulation course, go out thickness and be not less than 300nm rectangle microarray; Repeat photoetching process, define the growth array of metal oxide three-dimensional multistage nanostructured;
(4) by photoetching, wet-etching technology, remove masking layer and the Si substrate itself of Si backside of substrate, form the silicon chip with insulated tank;
(5), on the growth array of step (3) definition, utilize hydrothermal synthesis method to grow by cross one another dendritic overlap joint and realize the metal oxide three-dimensional multistage nanostructured that electricity connects.
6. the preparation technology of the metal-oxide gas transducer based on MEMS as claimed in claim 5, is characterized in that, the mass concentration of described hydrochloric acid is 37%.
7. the preparation technology of the metal-oxide gas transducer based on MEMS as claimed in claim 5, it is characterized in that, describedly utilize hydrothermal synthesis method to grow the concrete technology of realizing the metal oxide three-dimensional multistage nanostructured that electricity connects by cross one another dendritic overlap joint to be:
A, by butyl titanate, hydrochloric acid, oleic acid by volume 1:1:5 mix, after magnetic agitation, put into high-pressure hydrothermal reaction kettle;
B, will remove Si backside of substrate masking layer and Si substrate itself, formation is put into the reactor described in step a with the silicon chip of insulated tank, in 200 degrees Celsius of following insulations, after at least 4 hours, take out, with absolute ethyl alcohol, clean and remove unnecessary organism for several times, with acetone, wash away unnecessary photoresist, after being dried, obtain TiO
2nano gas sensor.
8. the preparation technology of the metal-oxide gas transducer based on MEMS as claimed in claim 7, is characterized in that, described dry be to bake and bank up with earth 4 hours under 80 degrees Celsius, air ambient.
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| CN109212329A (en) * | 2018-10-24 | 2019-01-15 | 清华大学 | Based on piezoelectricity-magnetic anisotropy coupled structure electric field measurement MEMS sensing device |
| CN109212329B (en) * | 2018-10-24 | 2020-12-18 | 清华大学 | Electric field measurement MEMS sensing device based on piezoelectric-magnetic anisotropic coupling structure |
| CN112083047A (en) * | 2020-08-11 | 2020-12-15 | 西安交通大学 | Portable gas detection device and detection method |
| CN112179956A (en) * | 2020-09-29 | 2021-01-05 | 西安交通大学 | Preparation method of MEMS formaldehyde sensor based on aluminum-doped zinc oxide porous nano film |
| CN112179956B (en) * | 2020-09-29 | 2021-11-19 | 西安交通大学 | Preparation method of MEMS formaldehyde sensor based on aluminum-doped zinc oxide porous nano film |
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