CN1719240A - Micro cantilever resonant type zinc phthalocynate film gas sensor and its preparation method - Google Patents
Micro cantilever resonant type zinc phthalocynate film gas sensor and its preparation method Download PDFInfo
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- CN1719240A CN1719240A CN 200510010248 CN200510010248A CN1719240A CN 1719240 A CN1719240 A CN 1719240A CN 200510010248 CN200510010248 CN 200510010248 CN 200510010248 A CN200510010248 A CN 200510010248A CN 1719240 A CN1719240 A CN 1719240A
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Abstract
The present invention relates to a micro cantilever beam resonant phthalocyanin zinc film gas sensor and its preparation method. Said sensor is formed from micro cantilever beam, piezoresistance vibration pick-upbridge and thermostimulated resistor. Its preparation method includes the following steps: A. integrating piezoresistance vibration pick-upbridge and thermostimulated resistor on the silicon chip; B. preparing micro cantilever beam structure; C. preparing phthalocyanin zinc gas sensing film; and D. making the phthalocyanin zinc gas sensing film be vacuum-deposited on the micro cantilever beam.
Description
Technical field:
The present invention relates to microelectromechanical systems gas sensor and preparation method thereof.
Background technology:
Along with MEMS (microelectromechanical systems) technology rapid development, the miniaturization of sensor, the integrated direction that has become the sensor development.Gas sensor can detect the composition and the concentration of all gases as the Sensitive Apparatus to all gases, is widely used in surveying various toxic and harmfuls, various inflammable gass, greenhouse gases and contaminated environment gas.At present, the MEMS gas sensor comprises MOSFET type, solid electrolyte type, metal oxide type and resonant mode etc.Wherein resonance declines beam sensor because highly sensitive, and advantages such as good stability become one of important directions of gas sensor development and research.
In recent years, more and more for the research of resonant transducer.People such as French Johann Mertens had studied HF (hydrogen fluoride) beam type detector in 2004, adopted piezoelectric excitation/optics pick-up method to detect the concentration of HF gas; The same year U.S. Northern Arizona university A.Kooser, R.L.Gunter, people such as W.D.Delinger, a kind of new gas sensor that adopted EPM (embedded piezoresistivemicrocantilever) technical research.Adopt the resistance pressure type cantilever beam structure, contain the condensate sensitive material of Ni, detect CO gas.At home, the bright grade of the Liu Yue of Xi'an University of Technology people adopts electric heating excitation/piezoelectricity pick-up method that the resonance performance of silicon micromachine cantilever beam has been carried out experimental study, has successfully realized the experiment test to first three first order mode of silicon micro-cantilever resonator.People such as the Zhou Jia of Fudan University have developed piezo-electric resonance type micro-cantilever gas sensor, are a kind of piezoelectric effects of the PZT of utilization piezoelectric membrane, realize the resonant-type tiny cantilever beam device of resonant excitation under the effect of alternating voltage.Form uniform molecular screen membrane on the micro-cantilever surface, the mass change that is caused by molecular sieve adsorption freon molecule converts the change of mechanical resonant frequency to, and then with electric signal output, the content of detection of freon.(referring to 1, JohannMertens, Eric Finot et al, Detection of gas trace of hydrofluoric acidusing microcantilever, Sensors and Actuators B 99 (2004) 58-65; 2, A.Kooser, R.L.Gunter, W.D.Delinger, et al, Gas sensing usingembedded piezoresistive microcantilever sensors, Sensors and ActuatorsB 99 (2004) 474-479; 3, Liu Yueming, Tian Weijian, Liu Junhua, the electricity of silicon micro-cantilever resonator swash electricity and pick up method research, semiconductor optoelectronic, 2003,24 (6): 289-391; 4, Zhou Jia, Li Po, yellow suitable equality, piezo-electric resonance type micro-cantilever gas sensor, piezoelectricity and acousto-optic, 2003.10,25 (5): 359～361.)
At present, in the resonant mode gas sensor, adopt resonant element in conjunction with specific gas sensitization membrane structure more.Difference is, the difference of resonant element, sensitive membrane and excitation/pick-up mode.The resonant element side of generally comprising film, the little beam of two fixed ends and microbridge and micro-cantilever etc.Now, static excitation: need two electrodes, control is had relatively high expectations to electrode separation, and the capacitance detecting difficulty is big.Electric magnetization: must utilize magnetic field, be difficult to realize microminiaturized.Piezoelectric excitation: processing technology and integrated circuit technology are incompatible, are unfavorable for problems such as integrated and intellectuality.
Summary of the invention:
The objective of the invention is to be difficult to realize microminiaturization, integrated and intelligent and manufacture craft and the incompatible problem of integrated circuit technology in order to solve existing microelectromechanical systems gas sensor, a kind of micro cantilever resonant type zinc phthalocynate film gas sensor and preparation method thereof is provided, and the concrete technical scheme that addresses the above problem is as follows:
Micro cantilever resonant type zinc phthalocynate film gas sensor of the present invention, it is made up of micro-cantilever 1, pressure drag pick-up electric bridge 2, heat-excitation resistance 3, root and free end at micro-cantilever 1 are impregnated with pressure drag pick-up electric bridge 2 and heat-excitation resistance 3 respectively, evaporation has Phthalocyanine Zinc gas sensitization film 4 on the upper surface of the micro-cantilever 1 that is impregnated with heat-excitation resistance 3 places, and Phthalocyanine Zinc gas sensitization film 4 is covered above the heat-excitation resistance 3 fully.
The preparation method's of micro cantilever resonant type zinc phthalocynate film gas sensor of the present invention step is as follows:
A, with pressure drag pick-up electric bridge 2 and heat-excitation resistance 3, adopt diffusion technique to be produced in the root and the free end of micro-cantilever silicon chip;
B, will adopt anisotropic corrosion technique,, form the structure of micro-cantilever 1 through anticaustic through the silicon chip of the making micro-cantilever of the diffusion region that pressure drag pick-up electric bridge 2 and heat-excitation resistance 3 are arranged that steps A forms;
C, preparation Phthalocyanine Zinc gas sensitization film 4;
D, the Phthalocyanine Zinc gas sensitization film 4 that will make through step C, adopt vacuum deposition method with Phthalocyanine Zinc gas sensitization film 4 evaporations on the upper surface of the micro-cantilever 1 at heat-excitation resistance 3 places, and Phthalocyanine Zinc gas sensitization film 4 is covered above the heat-excitation resistance 3 that infiltrates micro-cantilever 1 fully.
The present invention has following characteristics: output quantity be frequency signal, easily with computer system interface, to adsorb the mass resolution height, to NO
2Gas have good selectivity, manufacture craft can with ic process compatibility, it is low, integrated, microminiaturized also to have a cost.
Description of drawings:
Fig. 1 is the side cross-sectional view of micro cantilever resonant type zinc phthalocynate film gas sensor.
Embodiment:
Embodiment one: present embodiment is made up of micro-cantilever 1, pressure drag pick-up electric bridge 2, heat-excitation resistance 3, root and free end at micro-cantilever 1 are impregnated with pressure drag pick-up electric bridge 2 and heat-excitation resistance 3 respectively, evaporation has Phthalocyanine Zinc gas sensitization film 4 on the upper surface of the micro-cantilever 1 at heat-excitation resistance 3 places, and Phthalocyanine Zinc gas sensitization film 4 is covered above the heat-excitation resistance 3 fully.
Heat-excitation resistance 3 of this sensor and pressure drag pick-up electric bridge 2 are finished the pick-up of electric heating excitation/pressure drag, make sensor form self-sustained oscillation loop and output quantity detection, when tested gas molecule was attracted on the Phthalocyanine Zinc gas sensitization film 4, (the organic compound Phthalocyanine Zinc was to make the ideal material of nitrogen dioxide gas sensor to the increase of silicon beam quality.When organic compound Phthalocyanine Zinc (ZnPc) film 4 is exposed to tested gas NO
2When middle, gas can be adsorbed by sensitive membrane, cause the variation of micro-cantilever resonator 5 quality, influence the resonance frequency of beam), the resonance frequency of micro-cantilever resonator 5 is changed, because the resonance frequency variable quantity is directly proportional with the concentration of adsorbate, so by detecting the size that resonance frequency can calculate gas concentration.
Electric heating excitation is a kind of method of simple in structure and easy control.It is based on the thermal expansion phenomenon of micro-cantilever.The heat that heat-excitation resistance 3 produces, in the length direction and the normal direction formation temperature gradient of beam, the normal direction thermograde causes beam thermal expansion gradient on normal direction, makes beam produce flexural deformation, increases its amplitude, makes arousal effect better.Therefore, on heat-excitation resistance 3, apply alternating voltage, produce the temperature stress of alternation on the beam, drive semi-girder and vibrate, when vibration frequency is consistent with its natural frequency, promptly produce resonance.The resonance frequency of micro-cantilever is:
λ in the formula
iBe a parameter that has nothing to do with physical dimension, E is the Young modulus of micro-cantilever, and I is the cross section inertia square of beam, and ρ is the density of beam, and A is the cross-sectional area of beam, and L is the length of beam.
When micro-cantilever resonator 5 placed tested gas, the relational expression between the quality m of the resonance frequency f of silicon beam and the adsorbed gas on it was:
ρ in the formula
1Be the density of silicon, ρ
2Be the density of gas sensitization film, h
1Be silicon cantilever thickness, h
2Be the gas sensitization film thickness, b is a deck-siding, and l is a beam length, f
0The natural resonance frequency of beam when being zero for the gas absorption amount.By measuring the variable quantity of silicon beam resonance frequency f, just can obtain the adsorbance of gas molecule, thereby obtain the concentration value of tested gas.
The organic compound Phthalocyanine Zinc is to make the ideal material of nitrogen dioxide gas sensor.When organic compound Phthalocyanine Zinc (ZnPc) film 4 is exposed to tested gas NO
2When middle, gas can be adsorbed by sensitive membrane, causes the variation of micro-cantilever resonator 1 quality, influences the resonance frequency of beam.NO
2Molecular adsorption back on sensitive membrane is difficult to automatic desorption, therefore at the heat-excitation resistance 3 that designs below the gas sensitization film in the excitation resonator vibration, also make the gas sensitization film be heated, make NO
2Molecule has enough energy desorptions, has guaranteed that sensor has good repeatability.When the absorption of gas molecule and desorption process reached balance, it is stable that the resonance frequency of resonator keeps.When tested gas concentration changed, the absorption quality of gas sensitization film changed, and resonance frequency also changes thereupon.Therefore, can detect the concentration of tested gas in real time by the change of resonance frequency that detects micro-cantilever resonator 5.
Embodiment two: the preparation method of the micro cantilever resonant type zinc phthalocynate film gas sensor of present embodiment adopts following steps:
A, adopt twin polishing N type (100) crystal orientation silicon chip, clean this silicon chip after, adopt heat growth method to carry out two-sided oxidation, on two planes of silicon chip, grow certain thickness SiO
2Layer carries out a photoetching, carves the diffusion region figure, injects by the boron ion at silicon face and spreads, in the diffusion region that the root and the free end of micro-cantilever forms pressure drag pick-up electric bridge 2 and heat-excitation resistance 3;
B, will adopt the secondary photoetching through the silicon chip of the making micro-cantilever of the diffusion region that pressure drag pick-up electric bridge 2 and heat-excitation resistance 3 are arranged that steps A forms, and carve the fairlead figure, evaporation of aluminum anti-carves aluminium, forms the aluminium electrode, adopts the PECVD method, two-sided growth Si
3N
4Layer; Carry out third photo etching, etch back side silicon cup window, be that 40% KOH etchant solution carries out anisotropic etch with concentration under 85 ℃～120 ℃, forming thickness is the silicon cup of 40 ~ 70um, and four photoetching etch front semi-girder window, KOH solution with 40% corrodes once more, finally form the thick micro-cantilever 1 of 20 ~ 35um, remove the protective seam at electrode place, expose the aluminium electrode;
C, preparation Phthalocyanine Zinc gas sensitization film 4,0.50g (3.35mmol) anhydrous zinc chloride, 1.90g (15.1mmol) phthalonitrile, 2.88ml (3.35mmol) DBU agitating heating in 80ml n-amyl alcohol solvent refluxed, and (proportionate relationship of said components was constant in 6 hours, can multiply by certain multiple), cooled and filtered, to filter product that the back obtains successively with the ethanol washing of n-amyl alcohol, 3% hydrochloric acid, water and 100%, with getting the mazarine powder behind the chloroform extraction, be 2.5 * 10 in vacuum tightness with this mazarine powder
-3Pa, temperature is under 400～500 ℃ of conditions, gets the Phthalocyanine Zinc powder behind the employing vacuum sublimation method purifying; Adopt the heating vacuum vaporation coating machine, the Phthalocyanine Zinc evaporation on substrate, before the deposition, is carried out cleaning surfaces to used substrate and handles, the Phthalocyanine Zinc powder is placed in the silica crucible in the vacuum system, and the bottom of crucible disposes resistance heater and controls heating-up temperature; Regulate the resistance wire electric current Phthalocyanine Zinc powder is carried out evaporation, underlayer temperature is a room temperature, and the system pressure during evaporation is 2 * 10
-4Pa to 4 * 10
-4Between the Pa, evaporation time was controlled at 15～30 minutes, made thick Phthalocyanine Zinc (ZnPc) the distillation film of 0.8～1.2 μ m.
D, the Phthalocyanine Zinc gas sensitization film 4 that will make through step C, adopt vacuum deposition method, Phthalocyanine Zinc gas sensitization film 4 evaporations on the upper surface of the heat-excitation resistance 3 that is impregnated with micro-cantilever 1, and cover Phthalocyanine Zinc gas sensitization film 4 to infiltrate on the upper surface of heat-excitation resistance 3 of micro-cantilever 1 fully.Promptly make micro cantilever resonant type zinc phthalocynate film gas sensor of the present invention.
Claims (5)
1, micro cantilever resonant type zinc phthalocynate film gas sensor, it is made up of micro-cantilever (1), pressure drag pick-up electric bridge (2), heat-excitation resistance (3), root and free end at micro-cantilever (1) are impregnated with pressure drag pick-up electric bridge (2) and heat-excitation resistance (3) respectively, it is characterized in that evaporation has Phthalocyanine Zinc gas sensitization film (4) on the upper surface that is impregnated with the micro-cantilever (1) that heat-excitation resistance (3) locates, and make Phthalocyanine Zinc gas sensitization film (4) cover fully heat-excitation resistance (3) above.
2, micro cantilever resonant type zinc phthalocynate film gas sensor according to claim 1, the thickness that it is characterized in that Phthalocyanine Zinc gas sensitization film (4) are 0.8～1.2 μ m.
3, the preparation method of micro cantilever resonant type zinc phthalocynate film gas sensor is characterized in that this preparation method's step is as follows:
A, with pressure drag pick-up electric bridge (2) and heat-excitation resistance (3), adopt diffusion technique to be produced in the root and the free end of micro-cantilever silicon chip;
B, will adopt anisotropic corrosion technique,, form the structure of micro-cantilever (1) through anticaustic through the silicon chip of the making micro-cantilever of the diffusion region that pressure drag pick-up electric bridge (2) and heat-excitation resistance (3) are arranged that steps A forms;
C, preparation Phthalocyanine Zinc gas sensitization film (4);
D, the Phthalocyanine Zinc gas sensitization film (4) that will make through step C, adopt vacuum deposition method with Phthalocyanine Zinc gas sensitization film (4) evaporation on the upper surface of the micro-cantilever (1) that heat-excitation resistance (3) is located, and Phthalocyanine Zinc gas sensitization film (4) is covered above the heat-excitation resistance (3) that infiltrates micro-cantilever (1) fully.
4, the preparation method of micro cantilever resonant type zinc phthalocynate film gas sensor according to claim 3, the method for making that it is characterized in that Phthalocyanine Zinc gas sensitization film (4) is: refluxed 6 hours by 0.50g anhydrous zinc chloride, 1.90g phthalonitrile, 2.88mlDBU agitating heating in 80ml n-amyl alcohol solvent, cooled and filtered, to filter product that the back obtains successively with the ethanol washing of n-amyl alcohol, 3% hydrochloric acid, water and 100%, with getting the mazarine powder behind the chloroform extraction, be 2.5 * 10 in vacuum tightness with this mazarine powder
-3Pa, temperature is under 400～500 ℃ of conditions, gets the Phthalocyanine Zinc powder behind the employing vacuum sublimation method purifying; Adopt the heating vacuum vaporation coating machine, the Phthalocyanine Zinc evaporation on substrate, before the deposition, is carried out cleaning surfaces to used substrate and handles, the Phthalocyanine Zinc powder is placed in the silica crucible in the vacuum system, and the bottom of crucible disposes resistance heater and controls heating-up temperature; Regulate the resistance wire electric current Phthalocyanine Zinc powder is carried out evaporation, underlayer temperature is a room temperature, and the system pressure during evaporation is 2 * 10
-4Pa to 4 * 10
-4Between the Pa, evaporation time was controlled at 15～30 minutes, made the thick Phthalocyanine Zinc gas sensitization film (4) of 0.8～1.2 μ m.
5, the preparation method of micro cantilever resonant type zinc phthalocynate film gas sensor according to claim 3, the corrosion temperature that it is characterized in that micro-cantilever (1) is 85～120 ℃.
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