CN101936937A - Micro-cantilever gas sensor and manufacturing method thereof - Google Patents
Micro-cantilever gas sensor and manufacturing method thereof Download PDFInfo
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Abstract
The invention discloses a micro-cantilever gas sensor comprising sensing units and is characterized in that each group of sensing units comprises two micro-cantilevers, wherein the two micro-cantilevers can be a measuring cantilever and a reference cantilever, and a Wheaston bridge is formed by the measuring cantilever and the reference cantilever and two matching resistors; the measuring cantilever and the reference cantilever are connected to adjacent bridge arms of the Wheastone bridge, and the surface of the measuring cantilever is provided with a pressure-sensitive layer and an air-sensitive layer; a layer of polyelectrolyte polydiene propyl ammonium chloride film is deposited on the surface of the reference cantilever; and a photosensitive polyimide is used as a sacrifice layer material to connect an upper electrode with a lower electrode of each sensing unit through an inverse-splay window. The sensor has the advantages of simple structure, higher test sensitivity, and has wide application prospect in fields, such as environment monitoring, food safety, military and the like.
Description
Technical field
The present invention relates to microelectromechanical systems gas sensor and organic-inorganic nanocomposite field, be specifically related to a kind of micro-cantilever gas sensor based on the organic/inorganic nano laminated film and preparation method thereof.
Background technology
In recent years, gas sensor has all obtained in fields such as environmental monitoring, food industry and military affairs using widely, and traditional gas detecting instrument volume is big, costs an arm and a leg, and therefore development has high performance microminiaturization, integrated gas sensor is imperative.Along with the develop rapidly of MEMS technology (Micro Electro-MechanicalSystem) and in the application of sensor field, with the micro-cantilever research focus and the difficult point that gas sensor that the basis constitutes becomes sensor field.The mass-sensitive effect detection that the advantage of such sensor is to utilize micro-cantilever is to the mass change that flies to restrain magnitude, and therefore, micro-cantilever has extraordinary application prospect being in the gas sensor of basic sensitive mechanism with intermolecular specific adsorption.
Micro-cantilever beam sensor is compared with traditional sensor, mainly contains two big advantages: sensitivity and array technique.(useful area as little beam is about 10 of other mass sensor because the quality of little beam itself and size are very little
-5Doubly), therefore, its sensitivity can improve 2 more than the order of magnitude; Simultaneously, small size also means some other advantage: response time weak point, low cost of manufacture, the research ability of microenvironment is strengthened, be convenient to rig-site utilization more and carry, this real-time detection to trace/trace gas is very favourable.And utilize microelectronics and micro-processing technology, little beam can make array easily, and can be integrated into SOC (system on chip) with measuring and analysis system, and the size of integrated back array system is relatively also less.
At present such sensor application is had wide coverage in all kinds of volatile organic compoundses and mineral-type gas.The micro-cantilever gas sensor with high selectivity of people such as typical report as T.A.Betts in 2000 and U.S.'s Oak Ridge National Laboratory cooperation research and development, this sensor adopts the static deformation of laser acquisition V-type micro-cantilever, with polymer film as sensitive layer, tested it to pentane, toluene, aniline, ethanol, the response characteristic of gases such as water vapor (T.A.Betts, C.A.Tripple, Selectivity of chemical sensors based onmicro-cantilevers coated with thin polymer films, Analytica Chimica Acta, 2000,422 (1): 89-99).2004, the L.Fadel of France and group thereof adopt the electric magnetization mode, the method of utilization spin coating has prepared polyether polyurethane (PEUT) sensitive membrane, obtained the good linear relation (L.Fadel of the frequency change and the alcohol gas concentration of sensor, F.Lochon, I.Dufour, O.Francais, Chemicalsensing:millimeter size resonant microcantilever performance, Journal ofMicromechanics and Microengineering, 2004,14:S23-S30).Simultaneously, because the single polymers film has the cross sensitivity characteristic to the response of gas, people begin preparation and research micro-cantilever array sensor.2007, the H.P.Lang of Switzerland and group thereof integrate the formation micro-cantilever array with 8 micro-cantilevers, and it is combined with principal component analysis (PCA) (PCA), formed electric nasus system, this Electronic Nose can successfully be distinguished steam, ethylene dichloride, ethanol and toluene (H.P.Lang, J.P.Ramseyer, W.Grange, T.Braum, D.Schmid, P.Hunziker, C.Jung, M.Hegner, C.Gerber, An artificial nosebased on microcantilever array sensors, Journal of Physics:Conference Series, 2007,61:663-667).2008, people such as the Z.em ann M of Switzerland have showed the pressure resistance type gas sensor that can be used for detecting volatile organic gas, this sensor is integrated in 4 micro-cantilever arrays and self-sustained oscillation loop on the chip, can realize the feeble signal of microvolt level is realized amplification (the Z.em ann M of the low skew of low noise, T.Volden, K.irstein, A CMOS-based intergrated-system architecture for a staticcantilever array, Sensors and Actuators B, 2008,131:254-264).
In recent years, domestic research for the micro-cantilever gas sensor has also obtained fast development.2003, Fudan University has made the micro-cantilever resonant transducer that adopts PZT to drive, smeared the molecular sieve sensitive material on its little beam, detectable Cmin is the Freon gas (J.Zhou of 10ppm, P.Li, Zeolite-modified microcantilever gas sensor for indoor air control, Sensors andActuators B, 2003,94 (3): 337-342).2007, Shanghai Communications University and Shanghai micro-system are designed, and a kind of high-resolution pressure drag detected formula silicon dioxide micro-cantilever resonant transducer, through Cu
2+The micro-cantilever beam sensor of/thin basic undecanoic acid self assembly layer modification has quick response (P.Li, X.X Li, A single-sided micromachined piezoresistive SiO to dimethyl methyl phosphonate (DMMP) gas
2Cantileversensor for ultra-sensitive detection of gaseous chemicals, Journal of Micromechanicsand Microengineering, 2006,16:2539-2546); Utilize same structure after 6-MNA SAM modifies, also can realize detection (G.Zuo, X.X.Li, P.Li, Trace TNT vapor detection withan SAM function piezoresistive SiO to TNT
2Microcantilever, Ananlytica Chemical Acta, 2006,580:123-127).2009, Tsing-Hua University has designed the micro-cantilever resonator that a kind of electric heating excitation pressure drag detects, after sensitive layer on the semi-girder adsorbs specific gas, can draw the concentration (D.Ying of gas to be measured by the measurement semi-girder change of resonance frequency that mass change caused, G.Wei, Y.Zheng, Thermally-excited MEMS cantilever resonator for gas sensing, Nanotechnology andPrecision Engineering, 2009,7 (2): 119-122), but this work mainly concentrates on theoretical analysis and to the simulating, verifying aspect of device architecture.Aspect application for a patent for invention, application for a patent for invention prospectus CN1536335A and CN 1719240A have reported micro-cantilever beam sensor that a kind of semi-girder takes the shape of the letter U and a kind of micro-cantilever resonant mode phthalein mountain valley with clumps of trees and bamboo zinc thin film gas sensor and preparation method thereof respectively.
At present, the precision of micro-cantilever gas sensor can compare favourably with other traditional gas detection mode, and array is based on such sensor incomparable advantage, and it can improve accuracy of detection, measures when can also be used to realizing multiple gases.The subject matter that present stage restricts the development of such sensor is choosing of micro-cantilever sensitive layer material and prepares, the present invention prepares the micro-cantilever gas sensor as gas sensing layer and varistor layer simultaneously with Organic, for new approach is started in the research of micro-cantilever gas sensor, this research has not yet to see report, does not also have the application of related invention patent.
Summary of the invention
Problem to be solved by this invention is: how a kind of micro-cantilever gas sensor and preparation method thereof is provided, and this sensor construction is simple, and measurement sensitivity is higher, all is with a wide range of applications in fields such as environmental monitoring, food security and military affairs.
Technical matters proposed by the invention is to solve like this: a kind of micro-cantilever gas sensor is provided, it comprises sensing unit 1, it is characterized in that, every group of sensing unit 1 comprises two micro-cantilevers, be respectively and measure semi-girder 2 and, described measurement semi-girder 2 and with reference to semi-girder 3 and two build-out resistors composition Wheatstone bridges 4 with reference to semi-girder 3; Measure semi-girder 2 and be connected on the adjacent brachium pontis of Wheatstone bridge 4 with reference to semi-girder 3, described measurement semi-girder surface is provided with pressure-sensitive and gas sensing layer 5; Described with reference to semi-girder surface deposition one deck polyelectrolyte polydiene propyl ammonium chloride film 6; Adopt light-sensitive polyimide as sacrificial layer material, carry out the sensor upper/lower electrode by the window of falling the Eight characters and connect.
According to micro-cantilever gas sensor provided by the present invention, it is characterized in that described varistor layer and gas sensing layer are the organic/inorganic nano laminated film.
According to micro-cantilever gas sensor provided by the present invention, it is characterized in that described measurement semi-girder 2 and be arranged on the both sides of sensing unit 1 with reference to the position of semi-girder 3.
According to micro-cantilever gas sensor provided by the present invention, it is characterized in that described upper/lower electrode is Ti/Au duplicature or Al monofilm.
According to micro-cantilever gas sensor provided by the present invention, it is characterized in that described micro-cantilever beam length 50-200 μ m, wide 10-50 μ m, thick 1-2 μ m.
A kind of method for making of micro-cantilever gas sensor is characterized in that, may further comprise the steps:
1. adopt the silicon chip with oxide layer, single-crystal silicon device layer as substrate, the column criterion of going forward side by side is cleaned;
2. adopt magnetron sputtering method depositing Ti/Au duplicature or Al monofilm, and chemical wet etching lead-in wire electrode, this lead-in wire electrode is a bottom electrode;
3. adopt spin coating proceeding to apply the light-sensitive polyimide sacrifice layer, and make the herringbone window by lithography;
4. the heat growth silicon dioxide layer exposes bottom electrode as the micro cantilever structure layer and carry out chemical wet etching;
5. adopt magnetron sputtering method depositing Ti/Au duplicature or Al monofilm, and chemical wet etching lead-in wire electrode, this lead-in wire electrode is a top electrode;
6. heat growth silicon dioxide dielectric layer, and chemical wet etching contact hole exposes top electrode;
7. adopt the oxygen plasma dry etch process to discharge the light-sensitive polyimide layer, make micro-cantilever unsettled;
8. adopt self assembly, spin coating or drip and be coated with technology and on micro-cantilever, deposit organic/inorganic nano combined film;
9. deposition polyelectrolyte polydiene propyl ammonium chloride film on the sensitive thin film layer on reference semi-girder surface is verified with reference to the influence of semi-girder to eliminate undetected object.
Method for making according to micro-cantilever gas sensor provided by the present invention is characterized in that, wherein step 2. with 5. described Ti/Au duplicature of step or Al monofilm, its thickness is 300-500nm.
Method for making according to micro-cantilever gas sensor provided by the present invention is characterized in that, wherein the 3. described light-sensitive polyimide layer thickness of step is 1-2 μ m.
Method for making according to micro-cantilever gas sensor provided by the present invention is characterized in that, the 6. described silica dioxide medium layer thickness of step is 50-150nm, and its contact hole is a bar hole.
Method for making according to micro-cantilever gas sensor provided by the present invention, it is characterized in that, wherein in the 8. described organic/inorganic nano laminated film of step, organic phase is polyaniline or poly-(3,4-vinyl dioxy thiophene)/poly-(styrene sulfonate) etc., inorganic is nano titanium oxide, tin ash, barium titanate or carbon nano-tube etc. mutually.
The present invention is owing to take above technical scheme, have following characteristic and advantage: (1) utilizes the gas-sensitive property and the pressure drag characteristic of organic/inorganic nano laminated film, with gas sensing layer and the voltage dependent resistor (VDR) of organic/inorganic nano laminated film while as the micro-cantilever gas sensor, and do not need to make separately polysilicon or doped monocrystalline silicon voltage dependent resistor (VDR) layer, simplify preparation section greatly, and improved sensitivity; (2) adopt light-sensitive polyimide as sacrificial layer material, and the utilization oxygen plasma carries out dry method and discharge, realized the monolateral manufacturing of micro-cantilever, thereby wet etching and back-etching technology when having avoided micro-cantilever discharged have improved device performance; (3) the present invention is arranged on two resistance in the Wheatstone bridge on two adjacent micro-cantilevers, and semi-girder is measured in a conduct, and another one has been eliminated the influence of noise signal to measurement result as the reference semi-girder; (4) according to the function and the characteristics of device, designed metal interconnection line and bar shaped contact hole structure, realized the electric interconnected and signal output of device, increased the contact area of electrode and sensitive thin film simultaneously; (5) can or apply different organic/inorganic composite films by self assembly on micro-cantilever, thereby realize measurement gas with various.The present invention combines nano composite material, thin-film technique with MEMS technology, simplified device preparation technology, has improved device performance, for new approach has been opened up in the preparation and the application of micro-cantilever gas sensor.
Description of drawings
Fig. 1 is a micro-cantilever chip structure synoptic diagram provided by the present invention;
Fig. 2 is a Wheatstone bridge synoptic diagram provided by the present invention;
Fig. 3 is a process flow diagram provided by the present invention.
Wherein, 1, sensing unit, 2, measure semi-girder, 3, with reference to semi-girder, 4, Wheatstone bridge, 5, gas sensing layer and varistor layer, 6, polyelectrolyte polydiene propyl ammonium chloride film.
Embodiment
Below in conjunction with accompanying drawing the present invention is further described:
As shown in Figure 1 and Figure 2, the invention belongs to piezoresistance type microcantilever beam sensor, it comprises sensing unit 1, and every group of sensing unit 1 comprises two micro-cantilevers, is respectively to measure semi-girder 2 and with reference to semi-girder 3; Two micro-cantilevers and build-out resistor R
1And R
2Form Wheatstone bridge 4.Measure semi-girder 2 and be connected on the adjacent brachium pontis of Wheatstone bridge 4, the Rs resistance and the Rr resistance of corresponding electric bridge 4 respectively with reference to semi-girder 3.With reference to semi-girder 3 mainly is in order to eliminate the influence of noise signal to measurement result.According to the difference of measuring object, can or drip by self assembly, spin coating and be coated in the different organic/inorganic nano laminated film of semi-girder surface deposition as varistor layer and gas sensing layer 5; Simultaneously, in order to eliminate the influence of measuring object, deposit one deck polyelectrolyte polydiene propyl ammonium chloride film 6 again on the surface of reference semi-girder 3 to reference semi-girder 3.
In the foregoing description, micro-cantilever 2 and 3 long 50-200 μ m, wide 10-50 μ m, thick 1-2 μ m.Behind the air-sensitive film adsorption gas molecule on micro-cantilever 2 surfaces, the micro-cantilever deformation that bends produces stress on the beam surface; STRESS VARIATION causes the resistance of voltage dependent resistor (VDR) to change, and tests the detection that can realize gas by the output of Wheatstone bridge 4.The detection principle of its foundation is as follows:
According to Ohm law, the resistance of conductor or semiconductor material is:
R＝ρL/A (1)
In the formula: ρ is the resistivity of material;
L is a conductor length;
A is conductor or semi-conductive cross-sectional area.
Taken the logarithm in formula (1) both sides, can get behind the differential:
Poisson ratio (being the ratio of transverse strain and longitudinal strain) expression formula is introduced and can be got:
Have simultaneously
Bring (2) formula into:
Again because
:
In the formula: π is a piezoresistance coefficient; σ is a stress;
E is an elastic modulus; μ is a Poisson ratio;
ε is strain; K=(π E+1+2 μ) is a sensitivity coefficient.
The present invention utilizes the gas-sensitive property and the pressure drag characteristic of organic/inorganic nano laminated film, and the organic/inorganic nano laminated film simultaneously as the gas sensing layer and the voltage dependent resistor (VDR) of micro-cantilever gas sensor, has been simplified preparation section greatly, and improved sensitivity.Below in conjunction with process flow diagram Fig. 3 (comprising sectional view and vertical view) making embodiment of the present invention is described:
(1) adopt have oxide layer, single-crystal silicon device layer soi wafer as substrate, the column criterion of going forward side by side is cleaned (shown in Fig. 3 a);
(2) adopt magnetron sputtering method depositing Ti/Au duplicature or Al monofilm, and chemical wet etching lead-in wire bottom electrode (shown in Fig. 3 b), thickness of electrode 300-500nm; For the Ti/Au duplicature, Ti film thickness 20-50nm wherein, Au film 280-450nm;
(3) adopt spin coating proceeding to apply the light-sensitive polyimide sacrifice layer, and make herringbone window (shown in Fig. 3 c) by lithography; The aperture is 2-3 μ m under the herringbone window, and last aperture is 5-6 μ m.
(4) the heat growth silicon dioxide layer exposes bottom electrode (shown in Fig. 3 d) as the micro cantilever structure layer and carry out chemical wet etching; Silicon dioxide layer thickness 1-2 μ m.
(5) adopt magnetron sputtering method depositing Ti/Au duplicature or Al monofilm, and chemical wet etching lead-in wire top electrode (shown in Fig. 3 e); Thickness of metal film is with embodiment step (2).
(6) heat growth silicon dioxide dielectric layer (shown in Fig. 3 f), the thickness of silica dioxide medium layer is 50-150nm; The chemical wet etching contact hole exposes top electrode (shown in Fig. 3 g) then, and contact hole is a bar hole.
(7) adopt the oxygen plasma dry etch process to discharge the light-sensitive polyimide layer, make micro-cantilever unsettled (shown in Fig. 3 h);
(8) adopt self assembly, spin coating or drip and be coated with technology and on micro-cantilever, deposit organic/inorganic nano combined film (shown in Fig. 3 i);
(9) deposition polyelectrolyte polydiene propyl ammonium chloride film on the sensitive thin film layer on reference semi-girder surface is verified with reference to the influence (shown in Fig. 3 j) of semi-girder to eliminate undetected object.
In the said method, step 8 wherein, when preparing the organic/inorganic nano laminated film as voltage dependent resistor (VDR) and sensitive layer, can select polyaniline (PANI) or poly-(3,4-vinyl dioxy thiophene)/poly-(styrene sulfonate) (PEDT/PSS) waiting is organic phase, and nano titanium oxide, tin ash, barium titanate and carbon nano-tube etc. are inorganic phase; Preparing Organic by chemical oxidative polymerization, promptly is the polyreaction that nuclear carries out organic polymer with the inorganic nano-particle.Under the situation that inorganic nano-particle exists, nano particle at first evenly disperses in polymer monomer, trigger monomer carries out polymerization under the effect of oxygenant again, and polymkeric substance carries out limited growth around inorganic nano-particle, forms Organic then.Aspect the organic/inorganic nano laminated film prepares, can realize by original position self-assembling technique or spin coating proceeding.The advantage of self-assembling technique is that the film of its generation is even, fine and close, stable.Employing polyelectrolyte polydiene propyl ammonium chloride (PDDA) and poly-(sodium p styrene sulfonate) (PSS) composite self-assembly thin film system are introduced polar group at substrate surface, and utilization original position self-assembling technique prepares organic/inorganic nano composite air-sensitive film.The utilization spin coating proceeding prepares laminated film then more report, and technology is ripe, does not do detailed description at this.
Claims (9)
1. micro-cantilever gas sensor, it comprises sensing unit, it is characterized in that, every group of sensing unit comprises two micro-cantilevers, be respectively and measure semi-girder and, described measurement semi-girder and with reference to semi-girder and two build-out resistors composition Wheatstone bridges with reference to semi-girder; Measure semi-girder and be connected on the adjacent brachium pontis of Wheatstone bridge with reference to semi-girder, described measurement semi-girder surface is provided with pressure-sensitive and gas sensing layer; Described with reference to semi-girder surface deposition one deck polyelectrolyte polydiene propyl ammonium chloride film; Adopt light-sensitive polyimide as sacrificial layer material, carry out the sensor upper/lower electrode by the window of falling the Eight characters and connect.
2. micro-cantilever gas sensor according to claim 1 is characterized in that, described pressure-sensitive and gas sensing layer is the organic/inorganic nano laminated film.
3. micro-cantilever gas sensor according to claim 1 is characterized in that, described measurement semi-girder and be arranged on the both sides of sensing unit with reference to the position of semi-girder.
4. micro-cantilever gas sensor according to claim 1 is characterized in that, described upper/lower electrode is Ti/Au duplicature or Al monofilm.
5. micro-cantilever gas sensor according to claim 1 is characterized in that, described micro-cantilever beam length 50-200 μ m, wide 10-50 μ m, thick 1-2 μ m.
6. the method for making of a micro-cantilever gas sensor is characterized in that, may further comprise the steps:
1. adopt the silicon chip with oxide layer, single-crystal silicon device layer as substrate, the column criterion of going forward side by side is cleaned;
2. adopt magnetron sputtering method depositing Ti/Au duplicature or Al monofilm, and chemical wet etching lead-in wire electrode, this lead-in wire electrode is a bottom electrode;
3. adopt spin coating proceeding to apply the light-sensitive polyimide sacrifice layer, and make the herringbone window by lithography;
4. the heat growth silicon dioxide layer exposes bottom electrode as the micro cantilever structure layer and carry out chemical wet etching;
5. adopt magnetron sputtering method depositing Ti/Au duplicature or Al monofilm, and chemical wet etching lead-in wire electrode, this lead-in wire electrode is a top electrode;
6. heat growth silicon dioxide dielectric layer, and chemical wet etching contact hole exposes top electrode;
7. adopt the oxygen plasma dry etch process to discharge the light-sensitive polyimide layer, make micro-cantilever unsettled;
8. adopt self assembly, spin coating or drip and be coated with technology and on micro-cantilever, deposit organic/inorganic nano combined film;
9. deposition polyelectrolyte polydiene propyl ammonium chloride film on the sensitive thin film layer on reference semi-girder surface is verified with reference to the influence of semi-girder to eliminate undetected object.
7. the method for making of micro-cantilever gas sensor according to claim 6 is characterized in that, wherein step 2. with 5. described Ti/Au duplicature of step or Al monofilm, its thickness is 300-500nm.
8. the method for making of micro-cantilever gas sensor according to claim 6 is characterized in that, wherein the 3. described light-sensitive polyimide layer thickness of step is 1-2 μ m.
9. the method for making of micro-cantilever gas sensor according to claim 6 is characterized in that, the 6. described silica dioxide medium layer thickness of step is 50-150nm, and its contact hole is a bar hole.
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