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GOIN 11116 (2006.01) (52) U.S. Cl. .................... 73/54.41; 73/53.05; 73/64.42 (58) Field of Classification Search ............... 73/24.06, 73/31.06,30.04,32 A, 54.24, 54.38, 54.41, 73/61.49, 61.75; 422/68.1 See application file for complete search history. (57) ABSTR<\CT A method for analyzing a fluid contained within a machine, comprising the steps of providing a machine including a passage for containing a fluid; placing a sensor including a mechanical resonator in the passage; operating the resonator to have a portion thereof translate through the fluid; and monitoring the response of the resonator to the fluid in the passage. 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Iijima, Electrolytis Determination of Nanomolar Concentrations of Silver in Solution with a Piezoelectric Quartz Crystal:, Analytiea Chimica Aeta, 1981, pp. 97-102,131, Elsevier Scientific Publishing Company. U.S. App!. No. 09/174,856 entitled "Graphic Design of Combinatorial Material Libraries" (Lacy, et al.) filed on Oct. 19, 1998. Ulbricht, Helmar, Eningen, Crimpen-eine ausgereifte AnschluBtechnik, XP-000902731. International Search Report dated Jul. 12,2004 (PCTIUS031 32983), 7 pages. * cited by examiner u.s. Patent May 16, 2006 US 7,043,969 B2 Sheet 1 of 5 100 ~ 102 106 104 108 lFig-1 I I I I I I II I __________ . . __ JI 110 112 120 \ , -', , - 1'-118.-/ ", "\ , \ I "\ ,,- I / ,-, / I i/ \ I \\ \ \ I ,, \ , l"- ,, I I / / \\ I \\ I " I \ lFig-2 16 u.s. Patent May 16, 2006 US 7,043,969 B2 Sheet 2 of 5 !Fig-3A 128 !Fig-3B 138 138 lFig-3C .. .. !Fig-3D u.s. Patent May 16, 2006 US 7,043,969 B2 Sheet 3 of 5 200 204 204 [ 206 ~ 206 202 [200 lFi~-3E 204 204 I I \ I \ \ 206 206 I \ \, \ \ \ \ \ ____ IV' ,,/' 202 ,~- \ ,, ,, I I \ -- -1 [200 204 204 lFi9.- 3F I ..--~ I \ I I 206 I I I 206 u ~ lFi~-3G u.s. Patent May 16, 2006 US 7,043,969 B2 Sheet 4 of 5 0.257..------------------------, 0.256+-----------------------., o SAE30 0.255 i--------,~~1r--__j + SAE40 /l SAE50 1----..., 0.254 +----------r' ~ 2 0.253 +------;1 ~ <::( 0.252 - ! - - - - - j [ ; H j Jll.-'*'------~--~-__&n=::...,~'----____I 0.251 0.25+--------------"IlIiIflCi----------i 0.249 +---.--------.-------,---------r----,-----,--.-----,----,----., 27000 27500 28000 28500 29000 29500 30000 30500 31000 31500 32000 FREQUENCY (Hz) IF"ig-4A 0.151-,--------------------------, 0.15 + - - - - - - - - - - - - I I F - ' : u r . - - - l 0 0 0 IOW·30NEW 1OW.30 USED 0.149 +---------:-:~~---4------___:_:rm1lfl\lUll 0.148 +-----,rnoI.1iVF"----------t--~'-"-----___I Lu § I- ~ 0.147+----------- <::( 0.146 +-------~* O.145+---.....,,:j)ji 0.144~---------------------f 0.143 +-------r-j- - - - . . , - - - - - - - , - - - - - , - - - - - - - , - - - . - - - - - 1 29000 32000 26000 27000 28000 31000 30000 FREQUENCY (Hz) lFig-4B u.s. Patent May 16, 2006 Sheet 5 of 5 Z(00) lFig-7 US 7,043,969 B2 US 7,043,969 B2 1 2 MACHINE FLUID SENSOR AND METHOD resonator to have a portion thereof translate through the fluid; and monitoring the response of the resonator to the fluid in the passage or reservoir. One embodiment of the invention is a method for analyzing a fluid contained within a vehicle. A tuning fork resonator is operated at a frequency of less than 1 MHz while the resonator is in contact with the fluid contained within the vehicle. A response of the resonator is monitored. Yet another method of the present invention is for analyzing a fluid of an automotive vehicle. A mechanical resonator on a substrate having circuitry thereon is operated at a frequency of less than about 1 MHz while the resonator is in contact with the fluid of the automotive vehicle to have a portion of the resonator translate through the fluid. A response of the resonator is monitored. Still another method of the invention is for analyzing a circulating oil of a vehicle engine. An input signal is applied to a tuning fork resonator on a substrate having circuitry thereon at a frequency of less than about 100 kHz while the resonator is in contact with the oil of the automotive vehicle engine. A response of the resonator is monitored. According to one preferred embodiment of the method, a mechanical transducer is operated in a non-resonant mode with at least a portion of the transducer being translated through the fluid while a property such as mechanical impedance or the like is measured preferably using the monitored response. The monitoring that occurs in the method above may also employ suitable hardware package or configuration for monitoring the change of frequency of the mechanical resonator while maintaining the input signal to the resonator as a constant. It may alternatively employ the monitoring of the change in electrical feedback from the resonator while maintaining a constant frequency. In a particularly preferred embodiment wherein the input signal is a variable frequency input signal and the monitoring step includcs varying the frequency of a variablc frcquency input sigual over a predetennined frequency range to obtain a frequency-dependent resonator response of the mechanical resonator. Though other stmctures may be employed, in one highly preferred embodiment the mechanical resonator is configured generally as a tuning fork, and thus preferably includes at least two opposing free-ended tines that share a C01111110n base. The systems, methods and apparatus of the prcsent invention may further comprise other components, such as a computer, a micro controller, an energy source (e.g., a power, stimulus or excitation source) (e.g., for providing a variable frequency input signal to the resonators), a device for converting a signal drawn from a power source of a vehicle into a variable frequency input sigual or the like. CLAIM OF BENEFIT OF FILING DATE The present application claims the benefit of the filing date of U.S. Provisional Application Ser. No. 60/419,404 (filed Oct. 18, 2002), hereby incorporated by reference. TECHNICAL FIELD 10 The present invention generally relates to the field of fluid sensors and more particularly to an automotive fluid sensor incorporating a mechanical resonator. BACKGROUND OF THE INVENTION The use of a quartz oscillator in a sensor has been described in U.S. Pat. No. 6,223,589. U.S. Pat. No. 5,741, 961 also discloses a quartz resonator for use in an engine oil sensor. Yet another piezoelectric sensor for engine oil is disclosed in Hammond, ct aI., "An Acoustic Automotivc Engine Oil Quality Sensor", Proceedings of the 1997 IEEE International Frequency Control Symposium, IEEE Catalog No. 97CH36016, pp. 72-80, May 28-30, 1997. An improved system for measuring characteristics of fluids using mechanical resonators is disclosed in commonly-owned U.S. Pat. Nos. 6,401,519; 6,393,895; 6,336, 353; and 6,182,499. The use of acoustic sensors has been addressed in applications such as viscosity measurement in "Acoustic Wave Microsensors," 1. W. Grate, et at, Anal. Chem. 65, 940A-948A (1993)); "Viscosity and Density Sensing with Ultrasonic Plate Waves", B. A. Martin, S. W. Wenzel, and R. M. White, Sensors and Actuators, A21-A23 (1990), 704-708; "Preparation of chemically etched piezoelectric resonators for density meters and viscorneters", S. Trolier, Q. C. Xu, R. E. Newnham, Mat.Res. Bull. 22, 1267-74 (1987); "On-line Sensor for Density and Viscosity Measurement of a Liquid or Slurry for Process Control in the Food Industry", Margaret S. Greenwood, Ph. D. James R. Skorpik, Judith Ann Bamberger, P. E. Sixth Conference on Food Engineering, 1999 AIChE A.l1llual Meeting, Dallas, Texas; U.S. Pat. Nos. 5,708,191; 5,886,250; 6,082,180; 6,082,181; and 6,311,549; and "Micromachined viscosity sensor for real-time polymerization monitoring", O. Brand, 1. M. English, S. A. Bidstrup, M. G. Allen, Transducers '97, 121-124 (1997). Notwithstanding the above, there remains a need in the art for alternative or improved sensors for analyzing fluids used in machines (such as those in automotive systems), particularly for measuring changes in fluid amounts, changes in fluid quality or combinations thereof. 15 20 25 30 35 40 45 50 SUMMARY OF THE INVENTION BRIEF DESCRIPTION OF THE DRAWINGS 55 The present invention meets the above need by providing an improved fluid sensor and method of using the same, premised upon the employment of sensitive mechanical resonators, whose resonance performance can be monitored and corrclated with fluid characteristics. One embodiment of the present invention is an improved method for analyzing a fluid contained within a machine, comprising the steps of providing an machine including a passage or rescrvoir for containing a fluid; placing a sensor including a mechanical resonator in the passage or reservoir, a size of the resonator preferably being substantially smaller than a wave length of an acoustic wave; operating the 60 65 FIG. 1 shows a schematic view of one preferred system of the present invention. FIG. 2 shows a view of an illustrative resonator element of the present invention. FIGS. 3A-3G illustrate alternative stmctures for a resonator according to the present invention. FIGS. 4A and 4B depicts an illustrative graphical display of data in accordance with the present invention. FIG. 5 is a schematic of one system employing a sensor according to the present invention. FIG. 6 is a schematic of an alternative system employing a sensor according to the present invention. US 7,043,969 B2 3 4 FIG. 7 illustrates au example of an equivalent circuit in accordance with the present invention. frequency of the mechauical resonator while maintaining the input signal to the resonator as a constant. In another embodiment, the monitoring step includes monitoring the change in electrical feedback from the resonator while maintaining a constant frequency. In yet auother instance, the monitoring can be in the substantial absence of a signal, where for example, the frequency change, the amplitude decay or both of a resonator is observed over a period of time after an input signal has been terminated. The monitoring step will typically be guided by the nature of any input signal. In one highly preferred embodiment, for example, the monitoring step includes varying the frequency of a variable frequency input signal over a predetermined frequency rauge to obtain a frequency-dependent resonator response of the mechanical resonator. The sensor of the present invention preferably includes at least one mechanical resonator, stillmore preferably one that is capable of operating at a frequency range less than 1 MHz. For example, a highly preferred resonator according to the present invention is operated at a frequency of less than 500 kHz, more preferably less than 100 kHz, and even still more preferably less than 75 kHz. A particularly preferred operational range is from about 1 kHz to about 50 kHz aud more preferably about 5 to about 40 kHz. One highly preferred embodiment operates at about 20 to about 35 kHz. Though other resonators are also possible, a preferred resonator is selected from the group consisting of tuning forks, cantilevers, bimorphs, and unimorphs. A highly preferred resonator is a tuning fork resonator. The resonator may be uncoated or coated or otherwise surface treated over some or all of its exterior surface. A preferred coating is a metal, plastic, ceramic or composite thereof, in which the coating material is substautially resistant to degradation from the fluid to which it is to be exposed or to surface build-up, over a temperature range of about -10° to 100° c., and more preferably over a temperature range of about -40° to 125 or 150 0 C. The structure of the resonator may be any suitable structure taking into account the specific environment into which it is to be introduced. As indicated, a preferred resonator is a tuning fork, and thus will include a plurality of tines projecting from a common base wherein the tines and base may be arranged in a variety of configurations. It will be also appreciated that the resonator ofthe present invention, though potentially free standing, will generally be carried by a suitable support medium, such as a connector device for cOlmecting the resonator with a source of an input signal, a device for monitoring the response of the resonator to the signal, or both. The nature of the connector device may vary from application to application. In one embodiment, it is a molded plastic (e.g., polyamide or the like) device into which electrical wires cau be inserted in electrical communication with an inserted resonator. The connector may itself be configured for providing a suitable attachment (e.g., using a quick-cOlmect mechanism) to a surface of the machine into which it is introduced. Alternatively, the connector may be adapted for insertion into, or otherwise may comprise, au integrated portion of a receptacle within the machine. It is also contemplated that the connector device, the receptacle or both may include a chip (e.g., a computer chip) for assisting in the communication of date to other components described herein. The present invention is not limited to the use of a single resonator, but rather a plurality of resonators may be used. There may be plural resonators that are operational over the same or a different range of frequencies. There may be a plurality of resonators each of a different material or having DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS As will be appreciated from the description herein, the present invention is directed primarily for analyzing one or more fluids that are contained (whether in a sealed system, an unsealed system or a combination thereof) in machines. One highly preferred use of the present invention is the analysis of one or more fluids (aud particularly the viscosity, density or dielectric properties of one or more fluids) that are used in transportation vehicles (including, but not limited to, motorcycles, scooters, trucks, automobiles, construction equipment, locomotives, airplaues, boats, ships, fann machinery aud/or spacecraft), such as-fluids that are part of a sealed and/or self-contained operating system, and more preferably fluids that are part of a circulating or reservoir fluid system, such as engine oiL fueL transmission oiL radiator fluid, power steering oil, hydraulic fluid, refrigerant, gear oil, brake fluid or the like. Accordingly, though illustrated herein in connection with such highly preferred use as in a transportation vehicle, the present invention has a wide variety of uses and the description is not intended to limit the invention herein disclosed. Tl1e present invention is particularly attractive because of its ability to yield reproducible aud reliable fluid analysis, particularly over a broad range of operation temperatures. It also affords a relatively low cost alternative to other existing sensors. In one particularly preferred embodiment, though not required in every embodiment, the sensors of the present invention cau be operated with success at a relatively low frequency rauge. One embodiment of the present invention is an improved method for analyzing a fluid contained within a machine. The method comprises the steps of providing a machine including a passage or reservoir for containing a fluid; placing a sensor including a mechauical resonator in the passage or reservoir; operating the resonator to have a portion thereof translate through the fluid; and monitoring the response of the resonator to the fluid in the passage or reservoir. In another embodiment, the present invention is directed to a method for sensing a fluid in a circulating or reservoir fluid system, and includes the steps of providing a sealed circulating or reservoir fluid system; incorporating a mechanical resonator into the system, the mechauical resonator being in electrical communication with a source of an input signal; coupling the mechanical resonator with diagnostics hardware; exposing the fluid of the circulating or reservoir fluid system to the mechauical resonator; optionally applying an input signal; aud monitoring a response of the mechanical resonator to the fluid with the diagnostics hardware. When employed, the input signal for the sensors of the present invention may be any suitable signal. It may be generated from a direct current source or an alternating current source. It can be a constant frequency or a varying frequency. In one highly preferred embodiment, the signal is a varying frequency input signal. In another embodiment, the signal is a result of a voltage spike, sine wave burst, mechanical shock, pressure impulse, combinations thereof or the like. The step of monitoring may be performed under any of a variety of different conditions. For example, in one embodiment, the monitoring step includes monitoring the change of 10 15 20 25 30 35 40 45 50 55 60 65 US 7,043,969 B2 5 6 a different coating or surface treatment. Plural resonators may be carried by a COllllllon carrier, or by separate carriers. Further, the resonators may be placed in the same general or proximate region of the machine or at remote locations relative to each other. An array of at least three resonators on a common carrier may also be employed. One particularly preferred embodiment involves the incorporation of an oil sensor according to the present invention into an automotive vehicle engine. Thus, one possible approach is to locate the sensor in an engine oil pan. However, a sensor may be located in any other suitable oil passage in the engine. The sensors of the present invention may be used continuously. Alternatively, a sensor can be disposable, so that at predetermined intervals it is removed and replaced with a different sensor. Tl1e nature of the sensing that is performed by the sensor can be varied depending upon the parameter or condition that is desired to be monitored. Among the various applications are the use of the sensors herein for detecting the presence or absence of a fluid, the level of a fluid, the physical properties of a fluid, the presence of a contaminant in the fluid, the fluid pressure, the fluid flow rate, the fluid temperature, a change in physical property, condition or parameter of a fluid or a combination thereof. Of course, basic conditions of the fluid such as viscosity, density, dielectric constant, conductivity or a combination thereof may also be monitored and reported, and in a highly preferred embodiment these are the properties that are analyzed. It is also possible that one of these latter basic conditions is monitored using one or more of the present sensors and the data output is processed by a suitable processing lmit, which may apply an algoritlllll for correlating the outputted data with the presence or absence of a fluid, the level of a fluid, the replacement of a fluid, the presence of a contaminant in the fluid, the fluid pressure, the fluid flow rate, the fluid temperature, a change in the physical property, condition or parameter of a fluid or a combination thereof. The step of monitoring may be performed under normal operating conditions of the machine into which the present sensor is placed. The present invention is particularly advantageous in that it is believed operable over a broad range of temperatures. Thus it is contemplated that the monitoring step occurs at a temperature below -40 0 C. or possibly the monitoring step occurs at a temperature above 125 or 1500 C. Generally the monitoring will occur between these extremes. It is also possible that during or following a monitoring step the response of the sensor is compared against a known reference value for the fluid. For example, in the context of an automotive engine oil, fresh oil can be analyzed upon its introduction into an engine. The observed response may then be stored in memory or otherwise recorded. Data about a particular fluid may be stored in memory of a suitable processor, which can be retrieved in response to a triggering event, such as input from a technician or reading of an engine oil type by an optical detector, such as a bar code scauner. As the oil is used over a period of time, further analysis can be made and the response compared with that of the fresh oil. The identification of a diJl'erence between responses could then be used as a trigger or other output signal for communicating with diagnostics hardware, such as one or both of an on-board diagnostic device or operator interface (e.g., a dashboard display, an on board computer or the like), which would provide an audible or visual signal to the operator. It is also possible that a signal is outputted to a remote telemetry device, such as one located external of the vehicle. Thus, the signal that is outputted may be a radio frequency signal or another wireless signal. In one preferred embodiment, an output signal triggers an engine control unit to alter one or more functions (e.g, air intake; timing, or the like) of the engine or a combination thereof. Comparison of the response of the sensor to a reference value from the original fluid is not the only approach for generating a cOllllllunication to a user about the fluid condition. Certain expected values may be pre-progralllllled into a device, which then compares the real-time values obtained to the expected values. Moreover, it is possible that no comparisons are made between real-time values and expected values, but rather upon obtaining a certain threshold response, an output signal is generated for triggering a user notification, for triggering an engine control unit to alter one or more functions of the engine or a combination thereof. It is also contemplated that a sensor in a controlled fluid sample may be employed as an internal reference. It is also possible that the response obtained from the monitoring is stored in a memory, with or without communicating the response to the user. In this manner, a service technician can later retrieve the data for analysis. Though illustrated in comlection with an automotive vehicle, as with all such examples herein, it should be appreciated that such illustrations are not limited only to automotive vehicles, but that, as with the example just provided, like steps can be performed with other machines and motorized vehicles for transportation, hauling, lifting or perfornling mechanized work. Referring to FIG. 1, there is illustrated one preferred system 100 of the present invention. The system 100 includes a component 102 having passages 104 therein through which a fluid is passed. Disposed within one of the passages 104 is at least one sensor 106, which is in signaling conllllunication with a computer, controller or other like device 108. Preferably the sensor is also in signaling communication with a suitable power source 110. Diagnostics hardware 112 optionally may be incorporated into the device 108, or maintained separately from it. Suitable readout electronics may optionally be employed as part of or separate from the diagnostics hardware, e.g., including a readout board for interfacing between the computer and the resonator. Alternatively, a readout device may be associated with an instrument panel, such as for visual display to the operator of the machine or vehicle. It will be appreciated that the above configuration permits the use of one or more measurement modes (which can be measured using electrical techniques, optical techniques or a combination thereof) such as excitation at one or more frequencies around resonance, passive oscillations due to ambient noise, vibrations, EMI or the time decay of oscillation after an electrical or mechanical impulse (e.g., a voltage spike). It should be appreciated that, by use of the ternl "passage" herein, it is not intended to limit to strnctures that would be defined by walls of a conduit. Passage may include a reservoir, a well, an open-channel, a closed-chaunel, a container, or the like. Thus, generally the term "passage" herein contemplates any structure into which a fluid may be introduced, contained temporarily, contained permanently, passed through, removed from or otherwise. Incorporation of a sensor into an automotive vehicle is in accordance with the inventive principles herein. It will be appreciated that the location of the resonator, or plurality of 10 15 20 25 30 35 40 45 50 55 60 65 US 7,043,969 B2 7 8 resonators, may be any snitable location for the intended measurement, such as (among others) an engine oil pan, an oil sump, a pump, an oil filter device, an engine head, an engine block, a transfer case differential housing, a fluid line or hose, a heat exchanger, a dipstick, a drain plug, a sensor housing, or any other suitable location. Preferably the resonator is surface mounted, suspended or both, and positioned so that is analytical capability is not substantially compromised by fluid velocity, turbulence, mechanical oscillations, harmonics, vibrations or other extreme operating conditions. If it is necessary to subject a sensor to an extreme operating condition, then preferably the resonator will be suitably housed (e.g., in an enclosed chamber) or otherwise shielded as described herein. Diagnostics hardware for use in monitoring the response of a resonator according to the present invention may comprise any suitable art-disclosed hardware, and the discussion herein is not intended as limiting. Without limitation, it is possible to employ hardware such as disclosed in commonly owned u.s. Pat. Nos. 6,401,519; 6,393,895; 6,336,353; and 6,182,499, hereby incorporated by reference. Another approach herein for measurement hardware is to employ an electrical readout system in communication with a computer and any resonators. For example, one or more hard-wired circuits may be employed, or more preferably, one or a plurality of printed circuit boards are employed to comprise the readout board, thereby affording a compact and reliable structure. It should be appreciated that the discussion herein, in conformance with the drawings is specifically addressed to a system including one sensor adapted for analysis of a single fluid. However, the invention is not intended to be limited thereby, and it will be appreciated that the present invention also covers the use of a plurality of different sensors for measuring one fluid or a plurality of different fluids. FIG. 2 illustrates one preferred resonator comprising a resonator element 114. The resonator element 114 preferably includes a base 116 that has at least two tines 118 having tips 120 that project from the base. The shape of the tines and their orientation relative to each other on the base may vary depending upon the particular needs of an application. For example, in one embodiment, the tines 118 are generally parallel to each other. In another embodiment the tines diverge away from each other as the tips are approached. In yet another embodiment, the tines converge toward each other. The tines may be generally straight, curved, or a combination thereof. They may be of constant cross sectional thickness, of varying thickness progressing along the length of the tine, or a combination thereof. Resonator elements are suitably positioned in an element holder that is built into the component 102. Alternatively, the elements (with or without a holder) may be securably attached to a wall or other surface defining one of the passages 104. In yet another embodiment, the element is suitably suspended within a passage 104, such as by a wire, screen, or other suitable structure. Element holders may partially or fully surround the resonator elements as desired. Suitable protective shields, baffles, sheaths or the like may also be employed, as desired, for protection of the resonator elements from sudden changes in fluid flow rate, pressure or velocity, electrical or mechanical bombardment or the like. It should be appreciated that resonator elements may be fabricated from suitable materials or in a suitable mauner such that they may be re-useable or disposable. One or both of the resonator element holders preferably is configured with suitable hardware so that the resonator can be counected in signaling comlllunication with an input signal source, an output analyzer or a combination thereof. One preferred construction thus contemplates a device in which an exposed resonator is formed integrally with or attached to a chip or like surface mountable substrate that optionally has suitable circuitry built thereon. The chip, in turn, may also include other sensing elements, or may be attached in signaling comlllunication with another substrate having sensing elements associated with it. For exanlple, an existing device if or sensing fluid temperature, fluid level or both, may be adapted so that the sensor of the present invention (such as one for sensing oil condition) is housed along with the other sensing elements. All of the elements may connect to a common carrier or substrate, or be enclosed in a common housing (e.g., an enclosure having one or more openings to allow a fluid to pass through the enclosure). Of course, the sensor can also be employed as a stand-alone sensor, and not need to be housed with other sensing elements. The materials of the resonators of the present invention preferably are selected from at least one of piezoelectric materials, electrostrictive materials, magstostrictive materials, piezoresistive materials, elasto-optic materials, anisotropic materials, or combinations thereof. By way of example, the particular material may be a metallic material, a crystalline material, a ceramic material or a combination thereof. Examples of suitable materials include, without limitation, quartz, lithillll1 niobate, zinc oxide, lead zirconate titanate (PZT) or the like. Any suitable technique may be used to manufacture the resonator. For example, in one aspect, the resonators are prepared by art-disclosed processing techniques, such as are practiced in the semiconductor device fabrication industry. Thus, a wafer may be provided, one or more layers deposited thereon (e.g., by vapor deposition, sputtering, spin coating, curtain coating, laminating wafer bonding, or the like). Steps may be performed for shaping the resonator, such as photo lithography, laser cutting, etching, dicing or the like. Other fabrication techniques, such as casting, molding, or the like may also be used. A highly preferred embodiment of the present invention contemplates employing a tuning fork as a resonator. Preferably a two tine tuning fork is employed as the resonator. However, the method and system of the present invention can use any type of tuning fork resonator, such as a trident (three-prong) tuning fork or tuning forks of different sizes, without departing from the spirit and scope of the invention. As indicated, the present invention is not intended to be limited to tlming fork resonators. Other types of resonators can be used, such as tridents, cantilevers, torsion bars, bimorphs, membrane resonators, torsion resonators, unimorphs or combinations thereof. Still other types of resonators can be used if modified from their conventional art disclosed forms or if they are used in combination with a preferred resonator. Examples of such resonators include thickness shear mode resonators, length extension resonators, various surface acoustic wave devices or combinations thereof. A plurality of the same type or different types of resonators can be used in combination. For example, a low frequency resonator may be employed with a high frequency resonator. In this malmer, it may be possible to obtain a wider range of responses for a given sample. Specifically it is preferred that the resonator of the sensors of the present invention are mechanical resonators, and more preferably flexural resonators, torsional resonators or a com- 10 15 20 25 30 35 40 45 50 55 60 65 US 7,043,969 B2 9 10 bination thereof. In one embodiment, preferred resonators may be selected from the group consisting of tuning forks, cantilevers, unimorphs, bimorphs, disc benders, and combinations thereof. The size of the resonators can be varied. However, it should be appreciated that one advantage of the present invention is the ability to fabricate a very small sensor using the present resonators. For example, one preferred resonator has its largest dimension smaller than about 2 cm, and more preferably smaller than about 1 cm. One preferred resonator has length and width dimensions of about 2 nnn by 5 nnn, and possibly as small as about 1 lll111 by 2.5 mm. It is thus seen that a preferred resonator is configured for movement of a body through a fluid. Thus, for example, as seen in FIG. 2, the resonator 114 may have a base 116 and one or a plurality of tines 118 projecting from the base. It is preferred in one aspect that any tine 118 has at least one free tip 120 that is capable of displacement in a fluid relative to the base 116. FIG. 3A illustrates a cantilever 122 having a base 124 and a free tip 126. Other possible structures, seen in FIGS. 3B and 3C contemplate having a disk 128, a plate 130 or the like that is adapted so that one portion of it is displaceable relative to one or more variable or fixed locations (e.g., 132 in FIG. 3B) (e.g. 132' in FIG. 3C). As seen in FIG. 3D, in yet another embodiment a resonator 134 is contemplated in which a shear surface 136 of the resonator has one or more projections 138 of a suitable configuration in order that the resonator may be operated in shear mode while still functioning consistent with the flexural or torsional resonators of the present invention, by passing the projections through a fluid. In still other embodiments, and referring to FIGS. 3E~3G, it is contemplated that a resonator 200 may include an elongated member 202 supported on its sides 204 by a pair of arms 206. As shown respectively in FIGS. 3E~3G, the elongated member may be configured to oscillate side-toside, back and forth, in twisting motions or combinations thereof. The embodiment of FIG. 3B may be constructed as a monolithic device. Yet another structure of the present invention contemplates the employment of a lanlinate or other multi-layer body that employs dissimilar materials in each of at least a first layer and a second layer, or a laminate comprised of layers of piezoelectric material of different orientations or configurations. According to this approach, upon subjecting one or more of the layers to a stimulus such as temperature change, an electrical signal or other stimulus, one of the materials will respond differently than the other and the difference in responses will, in turn, result in the flexure of the resonator. As can be seen, the selection of the specific resonator material, structure, or other characteristic will likely vary depending upon the specific intended application. Nonetheless, it is preferred that for each application, the resonator is such that one or a combination of the following features (and in one highly preferred embodiment, a combination of all features) is present: 1) a coating placed upon the resonator in thickness greater than about O.lmicron that will not substantially detract from resonance performance; 2) the resonator is operable and is operated at a frequency of less than about 1 MHz, and more preferably less than about 100 kHz; 3) the resonator is substantially resistant to contaminants proximate to the sensor surface; 4) the resonator operates to displace at least a portion of its body through a fluid; or 5) the resonator responses are capable of de-convolntion for measuring one or more individual properties of density, viscosity, or dielectric constant. Also as discussed, in certain instances it is preferable for the resonator to be optionally coated with a material to change the performance characteristics of the resonator. For example, the material can be a coating, such as to protect the resonator from corrosion, degradation or other factors potentially affecting resonator performance. Alternatively, it may be a specialized "functionalization" coating that changes the resonator's response if a selected substance is present in the composition being tested by the resonator. For example, adding a hydrophobic or hydrophilic functionality to a resonator tine allows the tine to attract or repel selected substances in the fluid being analyzed, changing the mass, effective mass, geometry or a combination thereof of the tuning fork and thereby changing its resonance frequency. Thus, in one particularly preferred embodiment the resonators used in the present invention include a surface that is substantially resistant to contaminant build-up (e.g., impurities, soot, varnish, sludge, or the like) over all or a portion thereof. Accordingly, it is preferred that at least a portion of the resonator surface includes a material or texture that exhibits a relatively low affinity to a contaminant, a relatively high affinity to the fluid under test, a relatively high degree of hydrophobicity, or a combination thereof. Under separate circumstances, however, it may be desirable that the resonator surface include a material or texture that exhibits a relatively high affinity to a contaminant, and a relatively high degree of hydrophillicity. It is possible to achieve this by the selection of a resonator material that meets this requirement. Alternatively, a resonator may be suitably coated over at least a portion of its surface with a coating for exhibiting high hydrophobicity, a low coefficient of friction, or a combination thereof. Examples of suitable coating materials include, for example, fluoropolymers (e.g., PTFE), polyolefins (e.g., HDPE, HDPP or the like), silicones, silanes, siloxanes, ceramics (e.g., silicon nitride), diamond, or the like. Coating thickness is not critical for most contemplated applications. However, a preferred coating thickness ranges from about O.l microns to about 10 microns. One embodiment contemplates a thickness of about 1 micron. The resonators can also be functionalized with a polymer layer or other selective absorbing layer to detect the presence of specific molecules. The coating or functionality can be applied onto the resonator using any known method, such as physical vapor deposition (PVD), chemical vapor deposition (CVD), plasma enhanced chemical vapor deposition (PECVD), pulsed laser deposition (PLD), spraying or dipping. Further, the specific material selected for the coating or functionality will depend on the specific application in which the tuning fork resonator is to be used. A single resonator may be coated or functionalized. Alternatively, multiple resonators having the same or a different structure but different coatings and/or functionalities can be incorporated into one sensor. For example, a plurality of resonators may have the same structure bnt have different functionalities, each functionality designed to, for example, bond with a different target molecule. When the sensor is used in such an application, one resonator can, for example, be fi.mctionalized with a material designed to bond with a first substance while another resonator can be functionalized with a material designed to bond with second substance. The presence of either one of these substances in the sample composition being tested will cause the corresponding resonator to change its resonance frequency. It is 10 15 20 25 30 35 40 45 50 55 60 65 US 7,043,969 B2 11 12 also possible to employ one or more sensors in which one resonator is coated, and another is not coated. As discussed elsewhere, the manner of operating the sensors of the present invention may vary. In one embodiment, the sensor is operated continuously. In another, it may be intermittently operated. In other embodiments, the sensor may be operated only in preselected conditions, such as prior to starting vehicle operation, upon starting vehicle operation, during vehicle operation upon concluding vehicle operation, while the vehicle travels at a substantially constant velocity, while the vehicle accelerates or decelerates, or otherwise. Under any or all of the above conditions, it will be recognized that the integrity of the measurement may be impaired as a result of some environmental condition, such as temperature. The present invention thus also contemplates as one of its embodiments, the employment of an envirOlmlent conditioner, pursuant to which at least the environment proximate the location of the sensor is monitored or controlled to a predetennined condition. For example, it may be preferred with certain sensors to maintain the optimal sensing capability to be within a certain range of temperatures. A fluid that is outside of that range preferably will be detected and a temperature regulating device will heat or cool the fluid appropriately so that it can be efficiently sensed by the resonators of the present invention. It is also possible that the environmental conditioner is operated to maintain the environment in a constant condition. In this mamler, it can be seen, for example, that it is possible to employ a sensor of the present invention with a suitable heater for heating a frigid fluid to a certain temperature and preferably maintaining the fluid at that temperature for the duration of a measurement. The use of an environmental conditioner also offers the advantage that certain properties of the sensed fluid that are sensitive to environmental conditions (e.g., viscosity, which is sensitive to temperature) will be relatively unaffected during measurements, and provide a more reproducible and reliable data. Accordingly, in one preferred embodiment, the present invention contemplates operation of the sensor while the temperature of the sensed fluid is controlled at a substantially constant temperature by natural heat generated during nonnal vehicle operation, operation with local heating ofthe fluid or otherwise. In certain instances, it is contemplated that data obtaining from the sensors may be graphically displayed, such as on a video display screen (e.g., a desk-top screen, a hand-held screen, or both). It may also be outputted in printed format. FIGS. 4A and 4B are exemplary displays of data obtained in accordance with the present invention. Though illustrating results comparing new and used engine oils, and different types of oils, like results are believed possible for other fluids, and at other frequencies. Examples of suitable systems that may be employed herein include the systems illustrated in FIGS. 5 and 6. FIG. 5 illustrates a system 140 that employs a sweep oscillator 142 in signaling conllllunication with a resonator 144. The signal generated from the resonator is transmitted to an analog-to-digital converter 146. Data from another sensor 148 (e.g., a temperature sensor) may also be sent to the converter 146. The converter 146, the sweep oscillator 142 or both connnunicate with a suitable processor 150 (e.g., an embedded microcontroller), which in tum is in signaling communication with one or both of an internal bus 152 or external bus 154, via for example a suitable interface 156 (e.g., a CAN interface). FIG. 6 is substantially identical as FIG. 5 (with like parts denoted by like reference numerals), but fllrther includes a suitable environmental conditioner 158 driven by a suitable driver 160 in conllllunication with the processor 150. It will be appreciated from the foregoing that, in one preferred embodiment, the present invention is employed for sensing viscosity of a machine fluid, and is founded upon analysis of changes in resonance characteristics that occur when the resonator is in contact with a fluid. The response is thus correlated with one or more fluid properties. Without intending to be bound by theory, to help with such a correlation, in a highly preferred embodiment, applicable for highly preferred resonators in accordance herewith, a mathematical or equivalent electrical circuit model can be constmcted that includes the mechanical and electrical characteristics of the resonator, the properties of the surrounding fluid, and the coupling between resonator and fluid. Comparison of the model to measured data can help to yield the properties of interest. The parameters of the model can be found by fitting to the measured response using standard data fitting methods, such as (without limitation) least squares minimization. In one procedure, the parameters corresponding to the resonator alone are first detennined by calibration in air or vacunm. A second calibration in a liquid of known properties such as viscosity, density, dielectric constant or a combination thereof, gives parameters for mechanical and electrical coupling between resonator and liquid. With the model parameters then established, the properties of other liquids can be determined. Data acquisition and analysis can be simplified for incorporation in a fluid monitoring system. An example of one such analysis is set forth in L. F. Matsiev, "Application of Flexural Mechanical Resonators to Simultaneous Measurements of Liquid Density and Viscosity", IEEE Ultrasonics Symposium Proceedings, pp. 457-460 (1999), hereby incorporated by reference. By way of illustration, for the equivalent circuit depicted in FIG. 7, it is assumed that Cs , Ro, are equivalent characteristics of a preferred resonator in a vacuum, Cp is the equivalent parallel capacitance, p is the liquid density, 11 is liquid viscosity, CD is oscillation frequency. Accordingly, it can be seen that viscosity and density can be de-convoluted by the following: 10 15 20 25 30 35 40 45 50 55 60 65 M=Ap. AZ=B'!P1l The above is not intended as limiting of the present invention. Other alternative models might be derived with reference to publications such as "Frequency response of cantilever beams immersed in viscous fluids with applications to the atomic force microscope", 1. E. Sader, 1. App!. Phys. 84, 64-76 (1998); "Resonance response of scanning force microscopy cantilever", G. Y. Chen, R. 1. Warnlack, T. Thundat, and D. P. Allison, Rev. Sci. Instrum. 65, 2532-2537 (1994); and "Lecture notes on shear and friction force detection with quartz tuning forks" Work presented at the "Ecole Thematique du CNRS" on near-field optics, March 2000, La Londe les Maures, France by Khaled Karrai, Center for Nanoscience, Section Physik der LudwigMaximilians-Universitat Miinchen D-80539 Munchen, Germany, the teachings of which are hereby incorporated by reference. US 7,043,969 B2 13 14 Further, it will also be appreciated that the above protocol need not be performed in every instance. For example, where the specifics of the resonator geometry and electronics are accurately known, a reduced set of measurements, such as the frequency and amplitude of the resonance peak and minimum could suffice to determine particular liquid properties. In this case, simplified detector electronics and analysis methods advantageously might be employed to facilitate incorporation in a system for on-line or real time fluid condition monitoring, which is also contemplated herein. The sensors in accordance with the present invention advantageously provide excellent performance characteristics. Without limitation, for example, the sensors herein require less than 5V AC of excitation voltage, and on the order of less than 1 micro-amp current (e.g., about 0.1 micro-amps). Accurate measurements are obtainable in less than one second, and often less than about 0.25 seconds. The measurement range for viscosity is from about 0 to at least about 20 cPs (and possibly as high as at least about 5000 cPs) at 1 g/cm3. The measurement range for density is from about 0 to at least about 20 g/cm3 at 1 cPo Dielectric constants are measurable over at least the range of about 1 to about 100. Resolution (density,viscosity) values of less than 1% are also possible. It will be further appreciated that functions or structures of a plurality of components or steps may be combined into a single component or step, or the functions or structures of one step or component may be split among plural steps or components. The present invention contemplates all of these combinations. It is understood that the above description is intended to be illustrative and not restrictive. Many embodiments as well as many applications besides the examples provided will be apparent to those of skill in the art upon reading the above description. The scope of the invention should, therefore, be detennined not with reference to the above description, but should instead be determined with reference to the appended claims, along with the full scope of equivalents to which such claims are entitled. The disclosures of all articles and references, including patent applications and publications, are incorporated by reference for all purposes. What is claimed is: 1. A method for analyzing a fluid contained within a vehicle, the method comprising the steps of: a) operating a !lUling fork resonator at a frequency of less than 1 MHz while the resonator is in contact with said fluid contained within said vehicle; and b) monitoring a response of the resonator. 2. The method of claim 1 wherein said monitoring step comprises monitoring the change of frequency of the tuning fork resonator while maintaining an input signal to the resonator as a constant. 3. The method of claim 1, wherein said monitoring step comprises monitoring a change in electrical feedback from the tuning fork resonator. 4. The method of claim 1. further comprising operating said tuning fork resonator in a non-resonant mode wherein at least a portion of the tuning fork resonator is translated through said fluid. 5. The method of claim 1, wherein the response is at least related to the viscosity of the fluid. 6. The method of claim 1. wherein the vehicle is an automotive vehicle. 7. The method of claim 1. wherein the tuning fork resonator is located in an engine oil pan of the vehicle. 8. The method of claim 1 further comprising the step of mounting a sensor comprising said tuning fork resonator on the vehicle. 9. The method of claim 1, wherein the operating step comprises applying a variable frequency input signal to the tuning fork resonator. 10. The method of claim 9, wherein said operating step further comprises varying the frequency of the input signal over a predetermined frequency range, and wherein said monitoring step comprises obtaining a frequency-dependent resonator response of the tuning fork resonator. 11. The method of claim 1 wherein the resonator comprises a resonator element made of a material selected from piezoelectric materials, electrostrictive material, magneto restrictive materials, piezoresistive materials, elasto-optic materials, anisotropic material, or combinations thereof. 12. The method of claim 11. wherein the monitoring step comprises monitoring a response of the tuning fork resonator while the resonator is located in a temperature controlled region. 13. The method of claim 11, wherein said resonator element comprises a piezoelectric material. 10 15 20 25 30 35 40 * * * * *
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