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    • 专利摘要:
    A device (1) for fractionating particles (P) contained in a liquid (M) according to their masses comprises a plurality of cantilevers (2, 2.1, 2.2, 2.3) which are each mounted on one side and have a free end (2a) , wherein each cantilever (2, 2.1, 2.2, 2.3) has a, in particular U-shaped, fluid channel (3, 3.1, 3.2, 3.3) and the fluid channels of the cantilevers are connected in series. The cantilevers (2, 2.1, 2.2, 2.3) can be set in vibration by at least one vibration generator (5, 5 ', 5 "). The centrifugal forces (Fcent) and / or frictional forces (Fdrag) exerted by the vibrations of the respective cantilever (2, 2.1, 2.2, 2.3) on the particle-laden liquid (M) flowing in the fluid channel are for each cantilever (2, 2.1, 2.2, 2.3 ) set differently.
    公开号:AT514855A1
    申请号:T50641/2013
    申请日:2013-10-04
    公开日:2015-04-15
    发明作者:
    申请人:Tech Universität Wien；
    IPC主号:
    专利说明:

    T17731
    Device for fractionating particles contained in a liquid
    The invention relates to a device for fractionating particles contained in a liquid according to their masses, comprising a plurality of cantilevers, which are each mounted on one side and have a free end, each cantilever has a, in particular U-shaped, fluid channel and the fluid channels of the Cantilever are connected in series, wherein the cantilevers are set by at least one vibration generator in oscillation.
    The term cantilever as used herein means cantilevered and cantilevered components.
    The invention serves to fractionate small particles into different size classes and optionally to measure the total mass of the accumulated particles, the particles being in a liquid medium which is allowed to flow continuously or in discrete steps through the fluid channels of the cantilevers. The invention is generally applicable to particles which can be distinguished from the liquid medium by their higher density. These may be, for example, metallic wear particles or other inorganic or organic particles, biological cells, etc. As a medium, e.g. Water or engine oil in question.
    Coulter counter methods are known for measuring the presence of particles in a liquid medium based on a change in the electrical resistance of the medium in the presence of a particle. However, these methods are not applicable if the medium is poor or not conductive, such as oil. Small particle sizes (<1 pm) would also require a very small electrode geometry for resistance measurement and thus impractically small channels for flow through the particle-loaded medium.
    Optical measuring methods, such as obscuring the sprue path through particles between e.g. A fiber and a photodetector disposed on opposite sides of a flow path are only possible for particles> lpm and require that the liquid in which the particles are contained be at rest and transparent. According to the invention, however, such a restriction should be avoided.
    So-called Suspended MicroChannel Resonators (SMR) have proven to be useful and sensitive for detecting the mass of individual particles in liquid medium, which are vibration-excited, microfabricated cantilevers with embedded channels. Particles that flow through an SMR and pass its tip create a momentary change in the frequency of oscillation that can be measured. The basic structure and use of SMRs are described, for example, in documents WO 2008/045988 A1 and US 2010 / 288043A1. The latter document also explains that a particle which oscillates against the channel walls will tend to move towards higher oscillations, i. Towards the SMR tip, and depending on the flow rate and vibration amplitude, the vibration-induced centrifugal forces push the particle against the channel wall so as to generate sufficient frictional force to overcome the flow and trap the particle against the channel wall.
    It is known from the document US 2010/0154535 A1 to serially connect two or more identical suspended microchannel resonators (SMRs) in cantilever form so that the flow of a particle-laden liquid through the SMRs takes place sequentially. In this case, the first SMR is supplied with a liquid laden with a particle having a first density and a resonator measurement is carried out while the particle is in the fluid channel of the first SMR. Between the resonators, the density of the liquid is changed, preferably by mixing the liquid in a defined ratio with another liquid having a second density different from the first one. Thus, a fluid of other density flows through the second SMR than in the first SMR, and the resonator measurement is repeated when the particle is in the second SMR. Assuming that the SMRs are the same, and any inequalities are calibrated out, thereby causing identical behavior of the SMRs, the measurement of buoyancy of each cantilever can be used to determine the density, volume and absolute mass of the particle ,
    However, this known cantilever SMR arrangement can not be used to separate a plurality of particles of different mass from each other. Rather, it assumes that there is only one particle (or cell) in a cantilever.
    It is therefore an object of the present invention to further develop the initially mentioned apparatus for fractionating particles contained in a liquid according to their masses in such a way that the particles can be divided into different mass classes by means of the cantilever arrangement. The particle fractionation preferably takes place continuously. In a further aspect of the invention, the total masses of the fractionated particles are to be measured and recorded class by class, whereby the size distribution of the particles can be determined.
    The invention achieves the stated object by further developing the apparatus mentioned above for fractionating particles contained in a liquid according to their masses by setting the centrifugal forces and / or frictional forces exerted by the vibrations of the respective cantilever on the particle-laden liquid flowing in the fluid channel differently for each cantilever are. This makes it possible to "capture" particles of different mass from the liquid in each cantilever, to classify, to take measurements on it and, if appropriate, to discharge the captured, fractionated particles from the cantilevers.
    In a first preferred embodiment, the cantilevers are excited to different vibration frequencies and / or vibration amplitudes. Different vibration frequencies and / or vibration amplitudes exert different degrees of acceleration on the particles contained in the liquid. The greater the mass of the particles, the stronger the resulting centrifugal forces and the lower the accelerations required for the separation of the particles from the liquid. By applying this principle, particles with different masses can be fractionated in the individual cantilevem.
    In one embodiment of the invention, the cantilevers have different natural frequencies, which are preferably due to differences in material and / or geometrical differences, e.g. Cantileverlänge or wall thicknesses are set. This embodiment is useful on the one hand, if only a single vibration generator for excitation of all cantilevers is used, since the different natural frequencies of the cantilevers lead to different moods against the vibration generator, which in turn result in different vibration frequencies and / or vibration amplitudes of the cantilevers. If, on the other hand, each cantilever is assigned its own vibration generator, then this can be operated to achieve a maximum vibration amplitude at the natural frequency of the cantilever assigned to it.
    In a further preferred embodiment of the invention, the fluid channels of the cantilevers have different channel geometries, e.g. Channel height, channel width,
    Channel cross-sectional area, channel cross-sectional shape and / or channel wall textures. The term "different channel geometries" also includes differently shaped deflection regions and asymmetries of the channel guidance. This configuration of the device according to the invention, the flow velocity of the liquid can be changed by the respective fluid channel. A reduced flow rate reduces the fluid friction, in particular the friction between liquid and particles. Reduced fluid friction causes particles of lower mass to be eliminated. Different channel wall nature or coating also includes functionalizing the channel wall with certain chemical groups, which can lead to different fluid friction / adhesion not only of the medium but also adhesion / repulsion (e.g., electrostatic) of the particles. This can prevent or cause attachment if desired.
    The at least one oscillation generator provided in the device according to the invention is preferably designed according to one of the following basic principles: The at least one oscillation generator comprises piezo elements arranged on the cantilevers and a resonant circuit driving the piezo elements. The at least one vibration generator comprises coils arranged on the cantilevers, the deflection of the cantilevers being effected by the Forentz force. The at least one vibration generator periodically electrostatically attracts and / or repels the cantilevers.
    If each cantilever is assigned a separate vibration generator, this vibration generator can be optimally adapted to the natural frequency of the associated cantilever or each cantilever can be variably excited.
    The at least one vibration generator should excite the cantilevers to vibrate transversely to their catch axes in order to exert maximum centrifugal force on the particle-laden fluid.
    In one embodiment of the invention, the cantilevers or the channels connecting the fluid channels of the cantilevers have branch connections, preferably branch valves
    Discharging fractionated particles. This allows the fractionated particles to be subjected to measurements outside the device.
    Due to their masses, the accumulation of the fractionated particles in the cantilevers leads to a detuning of the oscillating circuit formed by the vibration generator and cantilever, which manifests itself in a change in the vibration frequencies and / or amplitudes of the cantilevers. In one aspect, the invention provides a vibration meter for measuring the vibration frequencies and / or amplitudes of the cantilevers, thereby providing a measure of the mass of the particles accumulated in the cantilevem. It is thus possible to carry out particle mass measurements directly and continuously in the device according to the invention.
    The vibration measuring device may comprise piezoresistors arranged on the cantilevers, the output signals of which represent a measure of the oscillation frequency and amplitude of the cantilevers.
    Alternatively, the vibration meter may comprise light-deflecting elements, which are irradiated with light, arranged on the cantilevers, the deflected light beams being applied to photosensitive components, e.g. Photoresistors, impinges, whose output signals represent a measure of the vibration frequency and amplitude of the cantilever.
    In a further alternative embodiment, the vibration measuring device detects the detuning of an excitation oscillation circuit of the vibration generator.
    In a further embodiment of the device according to the invention, a particle measuring device for measuring the number of accumulated particles is implemented, wherein the particle measuring device preferably comprises a light beam, preferably a laser beam, which can be coupled into the fluid channels by means of waveguide structures, and a detector unit which at a transparent position of the cantilevers either the Particles directly or through the particle-laden liquid passing light of the light beam or detected by the particles caused scattered light of the light beam. Herein, either an electromagnetic wave diffraction or scattering imaging method or a spectroscopic method (e.g., XRF) based on adsorption or emission of electromagnetic waves may preferably be used for estimating the number of particles or particulate matter.
    A pump is expediently provided in the device according to the invention which pumps the liquid laden with the particles to be fractionated or, if appropriate, reversible, a cleaning liquid through the serially connected fluid channels. This embodiment makes it possible on the one hand to set defined flow rates and profiles of the liquid being pumped, and on the other hand to clean the fluid channels by increasing the flow or generating pressure surges and / or flushing with cleaning liquid. If the pumping rate of the pump is variable, wherein the pumping rate is preferably reducible to zero, particularly accurate mass measurements of the fractionated particles can be carried out. For particularly accurate measurements and adjustments, a flow measuring device for measuring the flow rate of the particle-laden liquid flowing through the fluid channels is provided on the device according to the invention.
    To compensate for drift of the cantilever, a reference cantilever can be provided whose oscillation frequency and / or oscillation amplitude is used as a reference for a drift compensation of the other cantilevers, the reference cantilever either not flowing at all or passing only particle-free liquid. The drift compensation is performed by calibration measurements at specific time intervals.
    In an embodiment of the device according to the invention which can be produced in a simple and very miniaturized manner, at least one of the cantilevers has or comprises a curved capillary defining the fluid channel.
    To achieve high vibration frequencies, the cantilevers can be operated in higher vibration modes.
    The invention will now be explained in more detail by way of non-limiting embodiments with reference to the drawings.
    Fig. 1 shows schematically a first embodiment of the device according to the invention in plan view.
    Fig. 2 shows a selected cantilever of the device according to the invention in side view.
    Fig. 3 shows the selected cantilever in section.
    Fig. 4 shows schematically a variant of the embodiment of Fig. 1 with a reference cantilever.
    Fig. 5 shows schematically a further variant of the embodiment of Fig. 1 with a branch valve in the fluid channel.
    Figures 6A, 6B, 6C show an embodiment of a cantilever in three sectional views. FIGS. 7A, 7B, 7C show a further embodiment of a cantilever in three sectional views.
    FIGS. 8A and 8B show an arrangement according to the invention of two cantilevers.
    FIGS. 9A and 9B show a further arrangement according to the invention of two cantilevers. 10 shows schematically a vibration generator with piezo elements used in the device according to the invention.
    Fig. 11 shows schematically a vibration generator used in the fiction, contemporary device on the principle of electrostatic attraction and repulsion.
    Fig. 12 shows schematically a vibration generator used in the fiction, contemporary device with arranged on the Cantilevem current-carrying coils and excitation by the Lorentz force.
    Fig. 13 shows schematically a vibration measuring device used in the fiction, contemporary device on piezoresistive basis.
    Fig. 14 shows schematically a vibration measuring device according to the optical-lever principle used in the device according to the Invention.
    Fig. 15 shows schematically a vibration measuring device used in the fiction, contemporary device utilizing the Lorentz force.
    16 shows schematically a particle measuring device used on the optical basis in the device according to the invention.
    FIGS. 17, 18, 19, 20 show diagrams with comparisons of centrifugal forces and frictional forces on particles in cantilevers with different geometries.
    In Fig. 1, a first embodiment of a device according to the Invention 1 for fractionation of particles contained in a liquid M is shown schematically in plan view according to their masses. The device 1 comprises a plurality of cantilevers 2.1, 2.2, 2.3, which are each mounted on one side on a base 4 and have a free end 2a. Each cantilever 2.1, 2.2, 2.3 has a U-shaped fluid channel 3.1, 3.2, 3.3. The fluid channels 3.1, 3.2, 3.3 of all cantilevers 2.1, 2.2, 2.3 are connected in series, so that all fluid channels are flowed through one behind the other by the particle-laden liquid M. The cantilevers 2.1, 2.2, 2.3 are fabricated as a series arrangement of micro-cantilevers with microchannels embedded therein, e.g. in Si, S1O2 or polymers. The particle-laden liquid M is pumped by a pump 6 with variable pumping rate and thus variable flow rate through the fluid channels, wherein for the implementation of measurements, the pumping rate is preferably reduced to zero. In this embodiment of the device 1 according to the invention, a cleaning liquid R can be pumped from the pump 6 through the serially connected fluid channels 3.1, 3.2, 3.3 alternately to the liquid M loaded with the particles P to be fractionated. As a cleaning liquid R, the liquid M can also serve if it is not loaded with particles P. For precise settings of the pumping rate of the pump 6 and for performing highly accurate measurements is a flow meter 9.
    The cantilevers 2.1, 2.2, 2.3 are set in vibration by a vibration generator 5. In this first embodiment of the device 1, a single vibration generator 5 for vibrational excitation of all cantilevers 2.1, 2.2, 2.3 is provided. Hereinafter, embodiments of the invention are presented in which each cantilever is assigned its own vibration generator. The device according to the invention is characterized in that the centrifugal forces Fcent and / or frictional forces Fdrag exerted by the vibrations of the respective cantilever 2.1, 2.2, 2.3 on the particle-laden liquid M flowing in the fluid channel are set differently for each cantilever 2.1, 2.2, 2.3.
    The principle according to the invention will now be explained with reference to FIGS. 2 and 3. Fig. 2 shows a side view of any of the series arrangement of cantilevers 2.1, 2.2, 2.3 selected cantilever, designated by the general reference numeral 2. Fig. 3 shows this selected Cantilever in section, in which the U-shaped course of the general Reference numeral 3 designated fluid channel 3 detects. The fluid channel 3 is traversed by the liquid M, which is loaded with the particles P to be fractionated of different mass (or different size, if the density of the particles P is the same). The cantilever 2 is excited by the vibration generator, not shown, to oscillate transversely to the catch axis FA with an oscillation frequency f and an amplitude A, which represents the maximum instantaneous deflection. Due to the vibrations of the cantilever 2, centrifugal forces Fcent are exerted in the direction of the catching axis FA on the particles P present in the fluid channel 3. These can be estimated to a first approximation, when the movement of the free end 2a of the cantilever 2 describes an arc with the base 4 of the cantilever 2 as the center.
    With periodic excitation, there is an angle change according to
    where L represents the length of the cantilever 2 and A the amplitude of the vibrating free end 2a of the cantilever 2, and f the frequency with which the cantilever 2 oscillates, and t the time. Here, sin (0 (t)) ~ 0 (t) is approximated for small angles. The angular velocity results in the derivative
    and thus at the free end 2a of the cantilever 2 an acceleration of
    For a single oscillation cycle, the acceleration is average
    and thus the centrifugal force Fcent on a mass at the free end 2a of the cantilever 2 in the direction of the z-axis
    Since the particles P in the fluid channel 3 of the cantilever are maximally at a somewhat smaller longitudinal coordinate z = L-AL, the centrifugal force Fcent is reduced to
    where AF is between the wall thickness d and d + w, with w the width of the fluid channel 3 at the free end 2a. For spherical particles P with radius R in a viscous liquid M results in a frictional force (Fdrag) of
    η represents the dynamic viscosity, Vf the flow rate of the medium, and vp the velocity of the particle P. In laminar flow ratios (Reynolds number <1), particles P follow the liquid paths when no external forces are applied to them (i.e., vp =
    Vf). If a centrifugal force Fcent now acts on a particle P in the direction of the longitudinal axis, then it is contrasted with the liquid friction force Fdrag, with Fcent acting in the opposite direction as an Fdrag and therefore having to be provided with a negative sign, and obtained
    If the centrifugal force Fcent is so large that the amount of the additional velocity component vcent of the particle P induced thereby exceeds the flow velocity Vf (lvcentl> lvfl) and is opposite in the direction of liquid flow, then this particle will move outward in the longitudinal axis direction LA and be held at the free end 2a of the cantilever 2. Smaller and thus lighter particles P will, however, follow the flow and flow out of the cantilever because they are valued at lvcentl <lvfl. The deflection of the cantilever 2 up and down (x-axis) also causes a movement of particles proportional to the deflection, which is zero on average and thus has no effect on the centrifugal forces acting Fcent and the resulting particle movement in the direction of the longitudinal axis LA ,
    The velocity of a spherical particle with the mass mp = pp-4nR / 3 due to the centrifugal forces Fcent is thus approximately proportional to the squares of particle radius R, vibration frequency f and amplitude A and indirectly proportional to the viscosity η of the fluid M and the length L of cantilever 2:
    The channel wall nature or coating, such as functionalization with certain chemical groups, can result in different fluid friction / adhesion not only of the medium but also adhesion / repulsion (e.g., electrostatic) of the particles. This would also prevent or cause attachment if desired.
    In general, the effect of the centrifugal forces Fcent is greater, the heavier and larger the particles P are and the less viscous the liquid M is. The oscillation frequency f depends on the geometry of the cantilever, which should be operated at its resonant frequency, to allow for large vibration amplitudes.
    Based on this principle, an essential point of the invention is an arrangement of several such cantilevers 2, all of which can be excited to different vibrations (ie, different frequency f and / or amplitude A) to be able to exert different centrifugal forces Fcent and thus different ones Particle clays of different mass to be separated. An embodiment has already been described above with reference to FIG. 1; further embodiments will be described below. When the liquid M loaded with particles P is pumped through the device 1, in the first cantilever 2.1, the larger, i.e. trapped heavier particles while smaller particles flow to the next cantilever 2.2. There are due to higher vibration frequency f and / or amplitude A at the free end of the cantilever 2.2 stronger centrifugal forces induced so that the next smaller particle class is deposited. In the next cantilever 2.3 and further cantilevem as required, this fractionation process of particles for further classes will continue. If only one vibration generator 5 is used for all cantilevers, then different vibrations of the cantilevers can be caused by setting different natural frequencies. The adjustment of the respective natural frequency may be due to material differences of the cantilevers and / or geometric differences, such as e.g. Cantileverlänge L or the Cantileverwandstärken be made.
    Figures 6A, 6B, 6C show an embodiment of a cantilever 2 with a large ratio between length L and width B, and a small rectangular cross-sectional area (channel height h, channel width b) of the fluid channel 3. The channel width S in the deflection region of the fluid channel is compared to remaining channel width b increased. The reference signs dl-d4 denote the wall thicknesses at different locations of the cantilever.
    FIGS. 7A, 7B, 7C show a further embodiment of a cantilever 2 with a ratio of approximately 1: 1 between length L and width B, as well as a substantially larger channel width b of the fluid channel 3 than in the previous embodiment. By forming such cantilevers with different geometric shapes Parameters and / or wall materials on a Partikelfraktioniervorrichtung different vibrations of the cantilevers can be generated.
    8A and 8B show an arrangement according to the invention of two cantilevers 2.1 and 2.2 with different lengths LI, L2, but fluid channels 3.1 and 3.2 with the same channel width b and channel height h.
    In a second aspect of the invention-as an alternative or in addition to the variation of the centrifugal forces Fcent-for fractionating particles of different mass classes in the cantilevers, the fluid friction forces Fdrag prevailing therein are set differently. This can be achieved by providing the fluid channels 3, 3.1, 3.2, 3.3 of the cantilevers 2, 2.1, 2.2, 2.3 with different channel geometries, e.g. different channel height, channel width, channel cross-sectional area, channel cross-sectional shape. This leads to a change in the flow velocity vf, which brings about a different fluid friction. The above-explained embodiments of cantilever 2 according to FIGS. 6A-6C on the one hand and FIGS. 7A-7C on the other hand have significantly different channel widths b and thus different cross-sectional areas leading to different flow velocities, a larger cross-sectional area causing a reduction in the flow velocity.
    9A and 9B show an inventive arrangement of two cantilevers 2.1 and 2.2 with the same catches F, but fluid channels 3.1 and 3.2 of different channel widths bl, b2 and channel heights hl, h2.
    Another means to achieve different fluid friction in the fluid channels of the cantilevers is the variation of the channel wall textures (roughness, protrusions, materials or wall coatings with different adhesion to the liquid M and to the particles P).
    10 schematically shows a vibration generator 5 used in the device according to the invention with piezo elements 5a arranged on the base 4 of the cantilever, which are driven by a resonant circuit 5a '.
    Fig. 11 shows schematically a vibration generator 5 'used in the fiction, contemporary device on the principle of electrostatic attraction and repulsion. A at the free end 2a of the cantilever 2 electrode 5b and a remote therefrom counter electrode 5c are connected to an AC power source 5d and pull each other periodically electrostatically to repel each other periodically.
    Fig. 12 shows schematically a vibration generator 5 "used in the device according to the Invention arranged with a Cantilever 2, powered by a DC power source 5g, current-carrying coil 5f a spaced apart electromagnet 5e for excitation by the Forentz force.
    Each aforementioned vibration generator is either each associated with a single cantilever, or alternatively assigned to several or all cantilevers.
    Prerequisites for a quantitative definition of the particle classes are a known viscosity of the liquid M, which can be ensured by prior measurement of the viscosity of the liquid M, and known mass density of the particles P. If the latter is not known, one obtains a mass equivalent diameter as a function of particle density and -large and viscosity of the liquid M.
    In the case of metallic wear particles in lubricating oil, one can previously magnetically separate and reuse the iron particles present in the oil. In order to further improve the separation of the particles from the liquid, the temperature of the device 1 with an external heating element can also be increased, whereby the viscosity of the liquid M flowing through the fluid channels 3.1, 3.2, 3.3 is reduced. Also, instead or additionally, dilution of the liquid M with suitable solvents is conceivable (e.g., heptane).
    Since the particles P are pressed by the centrifugal forces Fcent in the direction of the free end 2a of the cantilevers 2.1, 2.2, 2.3, it is possible that there form agglomerates in the fluid channels 3.1, 3.2, 3.3 or adhere particles to the channel walls. Furthermore, by varying the channel wall properties (roughness, protrusions, materials or wall coatings), a different adhesion to the liquid M and to the particles P can be produced. Should this be a problem for any subsequent measurements, then e.g. With the help of ultrasound these accumulated particles solve again from each other or tear loose by high generated by the pump 6 flow rates of the liquid M adhering to walls particles. In the case of engine oil as a medium, additives are also present which prevent the deposition and agglomeration of particles.
    Calibration measurements at specific time intervals can also compensate for measurement drift due to accumulated particles. For this purpose, as shown in Fig. 4, a reference Cantilever 2.R, which is not flowed through by liquid provided. The oscillation frequency and / or oscillation amplitude of the reference cantilever 2.R is used as a reference for a drift compensation of the other cantilevers 2.1, 2.2. As an alternative to non-flow through, the reference cantilever 2.R could only be traversed by particle-free liquid.
    detection
    After the particle fractionation, the particles can be discharged in class from the individual cantilevers, if the cantilevers 2.1, 2.2, 2.3 or the channels 8.1, 8.2, connecting the fluid channels 3.1, 3.2, 3.3 of the cantilevers, 8.2 branch connections 7.1, 7.2, e.g. preferably branch valves, as shown schematically in Fig. 5. The discharged particles may then be subjected to arbitrary measurements outside the device or used as desired.
    However, it is provided in a preferred embodiment of the invention to quantify the amount of particles present in the liquid within the device by measuring the mass of the accumulated particles in the free ends 2a of the cantilevers 2.1, 2.2, 2.3. The principle is based on shifting the resonant frequency of a cantilever as its mass changes
    The resonance frequency of an unloaded cantilever results from the geometry and the material parameters and determines the sensitivity S ~ fres / (2m) of a cantilever against small mass changes Af = S-Am. This displacement Δf on a cantilever is detected, for example, by means of the optical lever method or integrated piezoresistive elements.
    FIG. 13 schematically shows a vibration measuring device 10 for a cantilever 2 with a piezoresistor 11 arranged on the cantilever 2, the output signals of which are detected by an evaluation circuit 10 a and represent a measure of the oscillation frequency and oscillation amplitude of the cantilever 2.
    14 schematically shows a vibration measuring device 10 ', in which a light deflecting element 12, which is irradiated with light from a light source 10b, is arranged on a cantilever 2. The light beams deflected by the light deflecting element 12 strike a photosensitive device 13, e.g. a photoresistor whose output signals represent a measure of the oscillation frequency and oscillation amplitude of the cantilever 2.
    Fig. 15 discloses a vibration measuring device 10 "based on the action of the Lorentz force. In this case, by means of a measuring circuit 106, the detuning of a
    Excitation resonant circuit of the vibration generator, comprising the coils 5e and 5f measured.
    In the case of the present invention, fractionation of the particles may be carried out for a certain time to subsequently reduce the flow rate completely and to measure the mass of the particles accumulated in the individual cantilevers. Thereafter, fractionation is again performed, etc. The parameters for the excitation may also be different for both modes. Of course, essential for both modes is a high quality of the resonator, such as by vibration in the air or vacuum, and thus low attenuation, e.g. would be possible by suitable packaging.
    With the help of these alternating operating modes, it is possible to record the increase in mass over time and thus to draw conclusions about the mass distribution of the particles present overall to the individual size classes.
    In addition, assuming an optically transparent medium, it is possible to use transparent cantilevers (e.g., S1O2) and to track the movement of larger particles (> lpm) by a Fichte microscope. 16 schematically shows a particle measuring device 20 in the form of the sprue microscope with integrated camera, which is directed onto a transparent point 2b of the cantilever.
    Due to their scattered light, particles of <1 pm can be detected by coupling fiber through waveguide structures at suitable points in order to record scattered light from these particles by means of a microscope and a camera. This can be used to count particles and thus gain additional information about the number per size class.
    Technical realization and estimation
    The fabrication of SMRs has been described in several publications of the group of Manalis, e.g. in WO 2005/029042 A2. Also conceivable would be production methods analogous to deBoer et al., J. Micromech. Microeng., 2000, 9, or the fabrication of channels in polymer cantilevers.
    When the excitation is via an external piezo element, the excitation frequency and amplitude are the same for all cantilevers of the array, i. the actual oscillation amplitude of the individual cantilevers results from their geometry. As soon as the excitation frequency deviates from the natural frequency of a cantilever, its deflection is reduced, as a result of which at least one parameter, namely the oscillation amplitude, can be influenced.
    Separate excitation, i. Setting the oscillation frequency and amplitude for each cantilever of the array is usually possible by means of Lorentz force by modulation of the excitation current, which requires the structuring of current paths on the cantilever and an external magnet (or vice versa). For electrostatic excitation, an additional counter electrode, for example, on the substrate below the cantilever, is necessary.
    Different channel dimensions per cantilever influence the flow velocity and thus also the separation areas. For mass measurement, the frequency change of a cantilever may e.g. be detected by optical fever method or integrated piezoresistors. In addition, one should implement at least one reference cantilever to compensate for any drift.
    In order to achieve greater centrifugal forces and thus separation of smaller, lighter particles, both the vibration frequency of a cantilever and the peak deflection at the free end of the cantilever must be sufficiently large. Shorter cantilevers have a higher resonant frequency, but at the expense of maximum peak excursion. Thus, the height of a cantilever and thus of the channel is limited (in addition to technological Fimits). In contrast, the width has no influence on the resonance frequency and only a small influence on the peak amplitude, but on the modes of the resonator.
    The following example illustrates the dependence of the separation efficiency on the geometry of a cantilever. The dimensions of a Si cantilever (ESi = 170GPa) were chosen: catches F = 500pm, width B = 200pm, height H = 10pm. This results in a resonant frequency of fres = 48kHz for a solid cantilever. Comparisons with the literature on SMR show that the frequency of an SMR is 15-26% lower than that of a comparable filled cantilever, while COMSOF simulations give a 5% higher frequency (the reason might be due to different material parameters or manufacturing). A Forentz force excitation with I = 10mA, Bmag = 0.3T, Fcurrent = 0.9B gives a force F at the tip of the cantilever towards the plane of F = Bmag · I · Fcurrent = 0.54 μΝ which causes a static peak excursion of dTip = 4FF3 / (ESiBH3) = 0.01 pm. A value of Q of the SMRs of 1000 is assumed, which is a practically achievable value for vibrations in vacuums or vacuums. Thus, the amplitude of the cantilever at resonance can be estimated as 2 2 -4 A = Q-dTip = 10pm. The centrifugal acceleration is thus proportional to Q -F LH ~. With fluid channel dimensions of 80pm x 8pm (length x width), a flow rate of v = lmm / s (0.64nL / s), a viscosity η = 1 OmPas, and a particle density of p = 5.17g / cm (iron oxide) a comparison of the centrifugal forces Fcent with the fluid friction Fdrag and an estimate up to which diameter D particles would be caught in the cantilever. This comparison for the parameters Q = 1000, Cantileverlänge L = 500pm, Cantileverhöhe = 10pm, amplitude A = lOpm and oscillation frequency f = 48kHz can be seen in the bar graph of Fig. 17, in which the abscissa the particle diameter D in pm and the ordinate the centrifugal forces Fcent and fluid friction Fdrag represent. FIGS. 18-20 illustrate comparative examples having varying values of Q, L, H, and the resulting vibration amplitude A and vibration frequency f. FIG. 18 shows a diagram for a cantilever with the parameters: quality Q = 5000, cantilever length L = 500 pm, cantilever height = 10 pm, amplitude A = 52 pm and oscillation frequency f = 48 kHz. 19 shows a diagram for a cantilever with the parameters: quality Q = 5000, cantilever length L = 100 rpm, cantilever height = 10 pm, amplitude A = 415 pm and oscillation frequency f = 12 kHz. 20 shows a diagram for a cantilever with the parameters: quality Q = 5000, cantilever length L = 100 rpm, cantilever height = 20 pm, amplitude A = 52 pm and oscillation frequency f = 24 kHz.
    权利要求:
    Claims (21)
    [1]
    Claims 1. A device (1) for fractionating particles (P) contained in a liquid (M) according to their masses, comprising a plurality of cantilevers (2, 2.1, 2.2, 2.3) each supported on one side and a free end (2a), wherein each cantilever (2, 2.1, 2.2, 2.3) has a, in particular U-shaped, fluid channel (3, 3.1, 3.2, 3.3) and the fluid channels of the cantilevers are connected in series, wherein the cantilevers (2 , 2.1, 2.2, 2.3) by at least one vibration generator (5, 5 ', 5 ") are set into vibration, characterized in that by the vibrations of the respective cantilever (2, 2.1, 2.2, 2.3) flowing in the fluid channel particle-laden liquid (M) applied centrifugal forces (Fcent) and / or frictional forces (Fdrag) for each Cantilever (2, 2.1, 2.2, 2.3) are set differently.
    [2]
    2. Apparatus according to claim 1, characterized in that the cantilevers (2, 2.1, 2.2, 2.3) to different vibration frequencies (f) and / or vibration amplitudes (A) are excited.
    [3]
    3. A device according to claim 2, characterized in that the cantilevers (2, 2.1, 2.2, 2.3) have different natural frequencies, which are preferably due to material differences and / or geometric differences, such as. Cantileverlänge (L) or wall thicknesses (dl-d4), are set.
    [4]
    4. Device according to one of the preceding claims, characterized in that the fluid channels (3, 3.1, 3.2, 3.3) of the cantilevers (2, 2.1, 2.2, 2.3) different channel geometries, such. Have channel height, channel width, channel cross-sectional area, channel cross-sectional shape, and / or channel wall textures.
    [5]
    5. Device according to one of the preceding claims, characterized in that the at least one vibration generator (5) arranged on the cantilever piezoelectric elements (5a) and a piezoelectric elements driving the resonant circuit (5a ').
    [6]
    6. Device according to one of claims 1 to 4, characterized in that the at least one vibration generator (5 ") arranged on the cantilevers current-carrying coil (5f) and the deflection of the cantilever is effected by the Lorentz force.
    [7]
    7. Device according to one of claims 1 to 4, characterized in that the at least one vibration generator (5 ') periodically electrostatically attracts and / or repels the cantilevers.
    [8]
    8. Device according to one of the preceding claims, characterized in that each cantilever (2, 2.1, 2.2, 2.3) is associated with a separate vibration generator (5).
    [9]
    9. Device according to one of the preceding claims, characterized in that the at least one vibration generator (5) excites the cantilevers (2, 2.1, 2.2, 2.3) to vibrate transversely to their longitudinal axes.
    [10]
    10. Device according to one of the preceding claims, characterized in that the cantilevers (2, 2.1, 2.2, 2.3) or the fluid channels (3, 3.1, 3.2, 3.3) of the cantilever connecting channels (8.1, 8.2) Abzweiganschlüsse (7.1, 7.2), preferably branch valves, for discharging fractionated particles.
    [11]
    11. Device according to one of the preceding claims, characterized by a vibration measuring device (10, 10 ', 10 ") for measuring the vibration frequencies (f) and / or vibration amplitudes (A) of the cantilevers (2, 2.1, 2.2, 2.3).
    [12]
    12. The device according to claim 11, characterized in that the vibration measuring device (10) arranged on the cantilever piezoresistors (11) whose output signals are a measure of the oscillation frequency (f) and oscillation amplitude (A) of the cantilever (2, 2.1, 2.2, 2.3).
    [13]
    13. The device according to claim 11, characterized in that the vibration measuring device (10 ') on the cantilevers (2, 2.1, 2.2, 2.3) arranged light-deflecting elements (12) which are irradiated with light and the deflected light beams on photosensitive devices ( 13), eg Photoresistors, impact whose output signals represent a measure of the oscillation frequency (f) and oscillation amplitude (A) of the cantilevers (2, 2.1, 2.2, 2.3).
    [14]
    14. The device according to claim 11, characterized in that the vibration measuring device (10 ") detects the detuning of an excitation resonant circuit (5e, 5f, 10e) of the vibration generator (5).
    [15]
    15. Device according to one of the preceding claims, characterized by a particle measuring device (20) for measuring the number of accumulated particles, wherein the particle measuring device preferably comprises a means of waveguide structures in the fluid channels einkoppelbaren light beam, preferably a laser beam, and a detector unit, which at a transparent location the cantilever (2, 2.1, 2.2, 2.3) detects either the particles directly or the light of the light beam passing through the particle-laden liquid or the scattered light or diffracted light of the light beam caused by the particles or comprises spectroscopic means based on adsorption or emission of electromagnetic waves.
    [16]
    16. Device according to one of the preceding claims, characterized by a pump (6), which loaded with the particles to be fractionated liquid (M) or, optionally, a cleaning fluid (R) through the serially connected fluid channels (3, 3.1, 3.2 , 3.3) pumps.
    [17]
    17. The apparatus according to claim 16, characterized in that the pumping rate of the pump (6) is variable, wherein the pumping rate is preferably reduced to zero.
    [18]
    18. Device according to one of the preceding claims, characterized by a flow measuring device (9) for measuring the flow rate of the fluid channels (3, 3.1, 3.2, 3.3) flowing, particle-laden liquid (M).
    [19]
    19. Device according to one of the preceding claims, characterized by a reference cantilever (2.R) whose vibration frequency and / or oscillation amplitude is used as a reference for a drift compensation of the other cantilevers (2.1, 2.2), wherein the reference cantilever (2 .R) either not at all or only by particle-free liquid flows through.
    [20]
    20. Device according to one of the preceding claims, characterized in that at least one of the cantilevers (2, 2.1, 2.2, 2.3) has a fluid channel (3, 3.1, 3.2, 3.3) defining curved capillary or consists thereof.
    [21]
    21. Device according to one of the preceding claims, characterized in that the cantilevers (2, 2.1, 2.2, 2.3) are operated in higher vibration modes.
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    同族专利:
    公开号 | 公开日
    AT514855B1|2015-08-15|
    WO2015049301A1|2015-04-09|
    DE112014004564A5|2016-08-04|
    引用文献:
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    WO2001001121A1|1999-06-29|2001-01-04|Ut-Battelle, Llc|Multi-modal analysis of micromechanical structures for sensing applications|
    US20040038426A1|2002-08-22|2004-02-26|Scott Manalis|Measurement of concentrations and binding energetics|
    US20080194012A1|2007-02-08|2008-08-14|Cellasic Corporation|Microfluidic particle analysis method, device and system|
    WO2009035125A1|2007-09-13|2009-03-19|Fujifilm Corporation|Cantilever-type sensor, as well as a substance sensing system and a substance sensing method that use the sensor|
    WO2008043040A2|2006-10-05|2008-04-10|Massachusetts Institute Of Technology|Integrated microfluidic device for preconcentration and detection of multiple biomarkers|
    US8631685B2|2008-10-15|2014-01-21|Massachusetts Institute Of Technology|Method and apparatus for extended time and varying environment measurements of single particles in microfluidic channels|
    US8312763B2|2008-10-15|2012-11-20|Massachusetts Institute Of Technology|Method and apparatus for trapping single particles in microfluidic channels|
    EP2602608B1|2011-12-07|2016-09-14|Imec|Analysis and sorting of biological cells in flow|US20210255082A1|2020-02-19|2021-08-19|Tdk Corporation|Methods and Devices for Detecting Particles Using a Cantilever Sensor|
    法律状态:
    2020-08-15| MM01| Lapse because of not paying annual fees|Effective date: 20191004 |
    优先权:
    申请号 | 申请日 | 专利标题
    ATA50641/2013A|AT514855B1|2013-10-04|2013-10-04|Device for fractionating particles contained in a liquid|ATA50641/2013A| AT514855B1|2013-10-04|2013-10-04|Device for fractionating particles contained in a liquid|
    DE112014004564.0T| DE112014004564A5|2013-10-04|2014-10-01|Device for fractionating particles contained in a liquid|
    PCT/EP2014/071066| WO2015049301A1|2013-10-04|2014-10-01|Device for fractionating particles contained in a liquid|
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