A kind of huge pressure drag double resonance mass sensor and preparation method thereof
Technical field
The present invention relates to a kind of huge pressure drag double resonance mass sensor and preparation method thereof, belong to micro-nano electronic mechanical system (MEMS/NEMS) technical field.
Background technology
In recent years, micro-nano mechanical resonator has been widely developed as highly sensitive mass sensor, this kind of sensor, mainly by the change of additional quality or pressure is converted to the change of respective resonant frequencies, then draws object under test mass value by the relation of frequency with quality or pressure.In biochemical sensitive field, the QCM (QCM) having been put into using is exactly to have used this principle: the change of quartz crystal oscillator electrode surface quality is converted into the frequency change of the quartz crystal oscillator circuit output signal of telecommunication, and then obtain high-precision data by other auxiliary equipments such as computers, it is the sensitiveest a kind of quality testing instrument.
But there are the following problems for current resonant mode mass sensor: (1), in liquid detecting environment, sensor electrical signal is under the influence of electrolyte solution, and its clean output voltage is very restricted.Further, since the effect of fluid damping, its energy ezpenditure can increase, and ultimately results in too high dynamic electric resistor, the degree of accuracy that impact is measured;(2) change in resistance of pressure drag is by additional quality (pressure) and the double influence of environment temperature, and especially in ultramicron detects, environment temperature is bigger on the impact of result, and current resonant mode mass sensor the most all lacks temperature-compensating measure;(3) tradition is less by the coefficient of strain of the silicon piezo-resistance of doping process, along with diminishing of moment sensor size, the piezo-resistance of Traditional dopant technique can not meet the requirement of modern high sensitivity detection, the requirement of the especially biochemical class ultrafast detection of pressure sensor ultramicron.
Summary of the invention
The technical problem to be solved is the defect overcoming prior art, it is provided that a kind of huge pressure drag double resonance mass sensor and preparation method thereof.
For solving above-mentioned technical problem, the present invention provides a kind of huge pressure drag double resonance mass sensor and preparation method thereof, including sensor chip and external circuit, it is characterized in that, described sensor chip includes two resonant transducer chips being connected by thin nano rod and temperature compensation means chip, described resonant transducer chip includes the sensitive structure of resonant transducer, silicon bottom, insulating silicon oxide layer, silicon top layer, aluminium top layer, exciting electrode, exciting electrode exit electrode and detecting electrode, described silicon bottom, insulating silicon oxide layer, silicon top layer sets gradually from bottom to up;Described aluminium top layer and silicon top layer are in the zones of different of same layer, described exciting electrode exit electrode and detecting electrode are arranged on aluminium top layer, described exciting electrode is arranged on silicon top layer, the sensitive structure of described resonant transducer is arranged on silicon top layer, the sensitive structure of described resonant transducer includes monocrystalline silicon nm harmonic film and T-shaped nano rod, described monocrystalline silicon nm harmonic film is anchored on silicon top layer center by T-shaped nano rod, described exciting electrode exit electrode is connected with exciting electrode by the wire of silica surface, described detecting electrode is connected with described T-shaped nano rod;Described external circuit includes that modulate circuit and control circuit, described modulate circuit electrically connect sensor chip and control circuit, and described control circuit and sensor chip electrically connect.
Further, described modulate circuit includes electrically connecting successively discharge circuit, filter circuit, analog oscilloscope;Analog-digital converter that described control circuit includes electrically connecting successively, DC/DC isolator, microprocessor, liquid crystal display, described control circuit also includes digital to analog converter and the linear power supply electrically connected respectively with microprocessor;Wherein the analog oscilloscope of modulate circuit electrically connects with the analog-digital converter of control circuit;Wherein the reverse input end of discharge circuit electrically connects with a detecting electrode of one of them described resonant transducer chip, the positive input of discharge circuit electrically connects with a detecting electrode of described temperature compensation means chip, and digital to analog converter electrically connects with the exit electrode of this resonant transducer chip above-mentioned.
Further, described discharge circuit is the discharge circuit of difference-mode input, described filter circuit is bandwidth-limited circuit, described analog-digital converter is the ADS8319 analog-digital converter of 16, described DC/DC isolator be model be the DC/DC isolator of ADUM5000, described microprocessor be the S3C2410 microprocessor of Samsung, described liquid crystal display be 2.8 cun of TFTLCD liquid crystal displays, described digital to analog converter be the DAC8531 digital to analog converter of 16, described linear power supply is LD0 linear power supply.
Further, described monocrystalline silicon nm harmonic film is square, and described exciting electrode four limits corresponding with monocrystalline silicon nm harmonic film are in being equally spaced.
Further, described monocrystalline silicon nm harmonic film surface plasma Ba and Hf carries out technique modification.
Further, the size of described temperature compensation means chip is as material and resonant transducer chip.
Further, realizing frequency by two thin nano rod and couple between two monocrystalline silicon nm harmonic films of said two resonant transducer chip, four angles of resonance film are extended and compression campaign along T-shaped nano rod in a plane.
Further, the preparation method of a kind of huge pressure drag double resonance mass sensor, it is characterized in that, comprise the steps:
Step one: selecting the material that the Si in N-type 110 crystal orientation is prepared as sensor chip, a length of 150-300 m of the most square resonance film, thickness is 50-200nm;
Step 2: respectively rinse Si silicon chip about 15 minutes with sulfuric acid with hydrogen peroxide mixed solution and deionization DI water respectively;
Step 3: at the silicon top layer of Si silicon with 5-9 ° of angle of inclination, 20keV energy injection 1016-1017The As ion of every cubic centimetre of dosage, the time is 10 minutes, is then placed into the 25-35 second in high-temperature annealing furnace so that As uniform ion is distributed;
Step 4: at silicon top layer spin coating photoresist, is designed with nm harmonic Thinfilm pattern by electron beam exposure, T-shaped nano rod pattern, electrode pattern, the mask plate of wire pattern carry out photoetching;
Step 5: then at SF6/N2Under environment, by ICP dry etching Si silicon upper surface, it is carved into silicon dioxide layer and stops;
Step 6: using silicon as mask, by the silica under BOE solution wet etching transducer sensitive structure, is carved into substrate silicon and stops, discharging transducer sensitive structure;
Step 7: utilize plasma Ba and Hf to be spaced 20-40 minute and successively film surface is carried out twice injection bombardment, film surface is made to form the defect of roughness and charged impurity, in film, form bigger residual stress simultaneously, effectively modulate the huge piezoresistive characteristic of monocrystalline silicon nm harmonic film.
The beneficial effect that the present invention is reached:
1) coupled by two thin nano rod between double resonator, quality induction zone is spatially separated from signal detection district come, the optimization achieving biochemical response and physical conduction of maximum possible, maximization reduces in liquid measure environment, the electrolyte solution impact on measurement result;
2) in order to eliminate the environment temperature impact on pressure drag change in resistance, devise a material in the present invention identical, outward appearance and the most differentiated temperature compensation means of resonator, the difference of the signal of telecommunication that the signal of telecommunication of its output exports with resonator, as the differential input signal of discharge circuit, effectively raises the degree of accuracy of measurement result;
3) the pressure drag array that the present invention selects is that a kind of novel surface modification processes that utilizes processed, with bigger residual stress, the resistor-strain coefficient of its huge piezoresistive effect characterized is up to 4000-5000, ratio high 2-3 the order of magnitude of resistor-strain coefficient of the silicon pressure drag of conventional bulk processing, the huge piezoresistive effect that pressure drag array produces under pressure can be greatly improved detection sensitivity and the resolution ratio of sensor.It is easily achieved trace detection;
4) signal of telecommunication of detecting electrode output passes through conditioning and the control of external circuit, can more stablize, effectively feeding back to exciting electrode, the value of the signal of telecommunication can directly be read by LCDs, and the output waveform of the signal of telecommunication can also be found out from analog oscilloscope intuitively.Voltage waveform need not be drawn by the data matching in later stage again, substantially increase efficiency;
5) this patent design increases substantially sensitivity and the resolution ratio of double resonance mass sensor, greatly reduces the impact on measurement result of liquid environment and environment temperature simultaneously, improves precision and the reliability of detection data.
Accompanying drawing explanation
Fig. 1 is the monocrystalline silicon nm harmonic film surface pressure drag distributed model figure by technique modified;
Fig. 2 (a), (b), (c), (d), (e) are huge pressure drag double resonance mass sensor chip preparation flow top views;
Fig. 2 (f) is the explanatory diagram in huge pressure drag double resonance mass sensor chip preparation flow top view;
Fig. 3 is huge pressure drag double resonance mass sensor and external circuit connection diagram.
1-10 in figure is exciting electrode exit electrode, and 11-22 is detecting electrode, and 23-34 is T-shaped nano rod, and 35,36 is thin nano rod.
Detailed description of the invention
The invention will be further described below in conjunction with the accompanying drawings.Following example are only used for clearly illustrating technical scheme, and can not limit the scope of the invention with this.
Two resonant transducer chip hereinafter referred to as resonator I resonator II.
As shown in Figure 1, owing to single crystal silicon material is anisotropic, its piezoresistance coefficient is relevant with crystal orientation, in stress sensitive device designs, the orientation of crystal mainly has<110>,<100>crystal face two kinds, and when when being oriented in<110>crystal orientation of pressure drag, piezoresistance coefficient is maximum, therefore in the present invention, the pressure drag of monocrystalline silicon nm harmonic film surface is distributed along<110>crystal orientation.The just equivalence of monocrystalline silicon nano thin-film surface now thinks that the diagonal at T-shaped nano rod 24 and 26 place is arranged numerous pressure drag unit, pressure drag unit these series connection and in parallel constitutes a regular pressure drag array, and symmetrical with the diagonal both sides at detecting electrode 14 place along detecting electrode 12, on diagonal, the pressure drag unit of distribution is most.By finite element simulation, the piezoresistance coefficient that now monocrystalline silicon nano thin-film is symbolized is maximum.When there being dynamic excitation signal function, nm harmonic film will make extension and the compression motion of certain frequency in a plane along T-shaped nano rod 23 ~ 26, inside black arrow represents inward compression motion, outside black arrow represents outward expansion motion, wherein, total resistance of equivalence pressure drag array is Rr, total resistance of four T-shaped nano rod is Rt。
As shown in Fig. 2 (a), (b), (c), (d), (e), the preparation method of a kind of huge pressure drag double resonance mass sensor, it is characterised in that: comprise the steps:
Step one: as shown in Figure 2 (a) shows, selects the material that the Si in N-type 110 crystal orientation is prepared as sensor chip, and a length of 150-300 m of the most square nm harmonic film, thickness is 50-200nm;
Step 2: respectively rinse Si silicon chip about 15 minutes with sulfuric acid with hydrogen peroxide mixed solution and deionization DI water respectively;
Step 3: as shown in Fig. 2 (b), at the silicon top layer of Si silicon with 5-9 ° of angle of inclination, 20keV energy injection 1016The As ion of every cubic centimetre of dosage, the time is 10 minutes, is then placed into the 25-35 second in high-temperature annealing furnace so that As uniform ion is distributed;
Step 4: at silicon top layer spin coating photoresist, as shown in Figure 2 (c), is designed with nm harmonic Thinfilm pattern by electron beam exposure, T-shaped nano rod pattern, electrode pattern, the mask plate of wire pattern carry out photoetching;
Step 5: then at SF6/N2Under environment, by ICP dry etching Si silicon upper surface, it is carved into silicon dioxide layer and stops;
Step 6: using silicon as mask, by the silica under BOE solution wet etching transducer sensitive structure, is carved into substrate silicon and stops, discharging transducer sensitive structure, as shown in Figure 2 (d) shows;
Step 7: utilize plasma Ba and Hf to be spaced 20-40 minute and successively silicon pressure drag array surface is carried out twice injection bombardment, pressure drag array surface is made to form the defect of roughness and charged impurity, in film, form bigger residual stress simultaneously, effectively modulate the huge piezoresistive characteristic of silicon pressure drag array;
Step 8: as shown in Fig. 2 (e), with temperature 400-450 DEG C, the time is 35-45 minute sputtered aluminum as resonator and the detecting electrode of temperature compensation means and exciting electrode exit electrode, wire;
As it is shown on figure 3, the concrete structure of sensor chip is as follows: whole sensor chip is divided into three bulks: resonator I, resonator II, temperature compensation means;On resonator I, exciting electrode exit electrode 1 ~ 3, they are connected with exciting electrode by the wire of silica surface, and the monocrystalline silicon nm harmonic film on resonator I is anchored on silicon face by T-shaped nano rod 23 ~ 26, and detecting electrode 11 ~ 14 and T-shaped nano rod 23 ~ 26 connect together;On resonator II, exciting electrode exit electrode 4 ~ 6, they are connected with exciting electrode by the wire of silica surface, and the monocrystalline silicon nm harmonic film on resonator II is anchored on silicon face by T-shaped nano rod 27 ~ 30, and detecting electrode 15 ~ 18 and T-shaped nano rod 27 ~ 30 connect together;It is connected by thin nano rod 35 ~ 36 between resonator I with resonator II, thus realizes mechanical couplings resonance;On temperature compensation means, exciting electrode exit electrode 7 ~ 10, they are connected with exciting electrode by the wire of silica surface, and temperature compensation means is anchored on silicon face by T-shaped nano rod 31 ~ 34, and detecting electrode 19 ~ 22 and T-shaped nano rod 31 ~ 34 connect together.
As it is shown on figure 3, the concrete measuring method of this sensor is as follows: resonator II is as quality induction zone, and resonator I is vibrational excitation and signal detection district, and resonator I is m with the proper mass of resonator II0, intrinsic frequency is f0, the resistance value of pressure drag array is Rr, total resistance of four T-shaped nano rod is Rt.The detecting electrode 12 of resonator I connects the reverse input end of differential operation circuit, and the detecting electrode 19 of temperature compensation means connects the positive input of differential operation circuit, thus realizes environment temperature error compensation by this Differential Input.In present case, when there being additional quality m on resonator IIcTime, also there is elastic deformation in the film of the resonator I being mechanically coupled together, due to the effect of huge piezoresistive effect, the resistance of the pressure drag array on nano thin-film surface occurs notable change, and the value of its change in resistance is Δ Rr1, under the effect of external dc power supply Vd, input current Im ≈ (Vd/R) * (the Δ R of the reverse input end of computing circuitr1/Rr), wherein R=Rr+Rt, the electric current of positive input input is In ≈ (Vd/R) * (Δ Rr2/Rr), wherein Rr2For the resistance of the pressure drag array changing value under the influence of temperature, differential input signal is through the process output AC voltage V of discharge circuit0, wherein V0=|V0|cosw0T, alternating voltage V0After filtered circuit filters off surface ripples, analog oscilloscope demonstrates stable voltage waveform, the binary number of 16 is converted to through A/D analog-digital converter ADS8319, real-time magnitude of voltage shows on TFTLCD, and the digital quantity collected sends D/A digital to analog converter DAC8531 to through microprocessor S3C2410 and is converted to analog voltage V2, wherein V2≈V0, the V of output2Feed back on the exciting electrode exit electrode 1 ~ 3 of resonator I, constitute closed loop autonomous system.Capacitor C3 is at additional alternating voltage V2With DC offset voltage V1Effect under, producing a size is F0Electrostatic force, wherein F0=1/2*(C/ X) * (V1+V2)2, wherein C is condenser capacity, and X is the distance between capacitor plate.Resonator I and resonator II are at electrostatic force F0Producing vibration under effect, now the vibration frequency after mass change becomes f1, by formula mc =-2m0Δf / f0Just additional quality m can be obtainedcSize, wherein Δ f=f1-f0。
The above is only the preferred embodiment of the present invention; it should be pointed out that, for those skilled in the art, on the premise of without departing from the technology of the present invention principle; can also make some improvement and deformation, these improve and deformation also should be regarded as protection scope of the present invention.