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Manipulation of confined bubbles in a thin microchannel: Drag and acoustic Bjerknes forces

Manipulation of confined bubbles in a thin microchannel: Drag and acoustic Bjerknes forces
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  Manipulation of confined bubbles in a thin microchannel:Drag and acoustic Bjerknes forces David Rabaud, Pierre Thibault, Jan-Paul Raven, Olivier Hugon,Eric Lacot, and Philippe Marmottant a  UMR 5588, Laboratoire Interdisciplinaire Physique, CNRS and Université de Grenoble,F-38402 Grenoble, France  Received 3 September 2010; accepted 17 March 2011; published online 18 April 2011  Bubbles confined between the parallel walls of microchannels experience an increased dragcompared to freestanding bubbles. We measure and model the additional friction from the walls,which allows the calibration of the drag force as a function of velocity. We then develop a setup toapply locally acoustic waves and demonstrate the use of acoustic forces to induce the motion of bubbles. Because of the bubble pulsation, the acoustic forces—called Bjerknes forces—are muchhigher than for rigid particles. We evaluate these forces from the measurement of bubble driftvelocity and obtain large values of several hundreds of nanonewtons. Two applications have beendeveloped to explore the potential of these forces: asymmetric bubble breakup to produce very wellcontrolled bidisperse populations and intelligent switching at a bifurcation. ©  2011 American Institute of Physics .   doi:10.1063/1.3579263  I. INTRODUCTION Recent years have seen the rise of digital microfluidics,in which tiny droplets or bubbles are handled as discretevolumes of fluids. 1 We focus in the present work on mi-crobubbles generated in flow focusing devices, bubbles char-acterized by very reproducible volumes. 2,3 These mi-crobubbles may act as tiny samples in lab-on-a-chipdevices. 4,5 Microbubbles can also act as simple spacers be-tween droplet samples, to avoid any contact and contamina-tion between them. 6 Another application is their collectionout of the microfluidic chip to obtain contrast agents 7 or tofabricate new porous materials.We further consider bubbles which diameters may ex-ceed the height of the microchannel geometry, defined by thetwo parallel plates and a rectangular cross-section. Underconfinement, bubbles will therefore loose their sphericity soas to adopt a shape that may be assimilated to a “frenchcheese” or “pancake.” This geometrical confinement has tobe contrasted with the confinement of bubbles inside tubes of circular cross-section, which have drawn a lot of attention ontheir vibrations. 8 In the perspective of developing noncontact handlingmethods so as to avoid any contamination of the operator, thecontrol of bubble trajectories is of major importance, andpossibly with selective control. This would, for instance, al-low to sort bubbles, to control reactions   thermal, chemical,biological   to perform on lab-on-chips.We propose to take advantage of acoustic waves to ma-nipulate bubbles. The generator of acoustic waves, a piezo-electric element, can be miniaturized and integrated in achip. Such devices have been developed to sort solidparticles 9,10 and biological cells 11 using acoustic radiationforces. However, the specificity of bubbles is their pulsationnear a resonance frequency, giving rise to Bjerknesforces 12–14 that are much larger than radiation forces onpoorly compressible particles. For instance, these forces arehelpful to act on bubbles rising in a liquid pool. 15 In order to evaluate the efficiency of the applied acousticforces, one can estimate the resisting drag forces. This wayof reasoning is close to the one developed in the famouselectrical force measurement on oil droplets by Millikan. 16 However, in Millikan’s experiment the droplet is in plain airand the Stokes drag formula is valid, while in the presentmicrofluidic configuration, the bubble is confined betweenwalls and the drag is increased by friction with the walls. Oursystem is therefore close to that of a bubble in a typicalHele–Shaw configuration, studied by Maruvada  et al. 17 Theauthors of this study assume a specific frictional behavior,that of a pure liquid, and do not take into account the pres-ence of surfactants. Nevertheless, these surfactants are nec-essarily added in solution to prevent any undesirable bubblecoalescence, when the bubble concentration is high: becausesurfactants can rigidify the interface, their impact has to beincluded in the analysis for the friction. Note that Fuerstman et al. 18 have studied the pressure drop of a flowing bubble ina thin microchannel, but for the case where the bubble takesthe whole width of the channel, touching the four walls of thin channels with a rectangular cross-section.This paper is organized as follows. The materials andmethods are given in Sec. II with two configurations of mi-crofluidic channels: the first for the study of the drag forcethat we calibrate with the buoyancy force, and the other onefor acoustic forcing. We present in Sec. III measurements of the drag force and introduce a new model for this force,which takes into account the diverse behavior of surfactantsand is validated by measurements. Then we evaluate theacoustic force experienced by deviated bubbles in Sec. IV.Section V is devoted to the description of applications we a  Electronic mail: PHYSICS OF FLUIDS  23 , 042003   2011  1070-6631/2011/23  4   /042003/9/$30.00 © 2011 American Institute of Physics 23 , 042003-1 Author complimentary copy. Redistribution subject to AIP license or copyright, see  have specifically developed: size sorting, automated switch-ing, and asymmetric breakup at a bifurcation. II. THE ACOUSTOMICROFLUIDIC DEVICEA. Experimental setup Acoustically operated microfluidic circuits are built us-ing soft-lithography techniques. 19 The circuit consists of twolayers. The first layer includes the channel and liquid plusgas inlets which are molded in a polydimethylsiloxane  PDMS   Sylgard 184, Dow Corning   so as to create a flowfocusing geometry as shown in Fig. 1. The second layer of the circuit includes the acoustic generator consisting of aglass rod   cut from a microscope slide   molded and coveredby a thin 100    m layer of PDMS. A piezoelectric ceramic  PIC151, 1 mm thick, Piezo-Instruments   is glued with ep-oxy to one end of the glass rod. The two layers are finallybonded by air plasma exposure   Harrick Plasma   with therod perpendicular to the channel, as shown on Fig. 1. Thisresults in a glass rod which is therefore not in direct contactwith the channel, but separated by the thin 100    m layer of PDMS.The gas thread flowing through the flow-focusing orificeis symmetrically pinched by water, creating microbubblesfurther dragged by the liquid. The liquid is de-ionized waterwith 10% commercial dishwashing detergent   Dreft, Procterand Gamble  . A syringe pump   11 Pico Plus, Harvard Appa-ratus   is used to push the liquid in the channel. The gas   purenitrogen   is under controlled pressure. The liquid flow rate  Q l and the gas pressure  P g  are the control parameters for theproduction and the flow of the bubbles. The standard valuesare around 120    l min −1 for  Q l  and 7 kPa for  P g . The pro-duced bubbles are flowing in channels whose thickness varybetween  h =50    m and  h =100    m. They are always incontact with top and bottom channel walls, and their aspectratio varies in the range 1.3–5.2.The bubble flow is recorded with a CMOS-camera   Mar-lin F131B, AVT   through an inverted microscope   IX70,Olympus  . Post-treatment of images is used to extract thebubbles’ characteristics such as their radii  R  and their longi-tudinal and transverse velocities  U   x   and  U   y . The average liq-uid velocity  V  , along  x  , is obtained by dividing the flow rate Q l  by the cross section of the channel: height  h   between 10and 100    m   times its width  w   1000    m in all our experi-ments  .An efficient coupling between the bubble flow and theultrasound field is obtained by integrating the acoustic sourceinto the microcircuit, limiting excess attenuation from thePDMS polymer matrix. The choice of a glass rod put per-pendicular to the main flow is advantageous as it possesseswell-defined resonance modes when excited from the piezo-electric transducer for certain frequencies. The signal sent tothe transducer is produced by a function generator  AFG3102, Tektronik    and is amplified   7600M, Krohn Hite  up to 50 V. B. Characterization of the resonance modes of theglass rod The resonance modes along the main axis   the  y -axis inFig. 1   of the glass rod are studied as they are responsible forthe transverse acoustic forces on the bubbles. In order tokeep a unidimensional vibration pattern, the allowed fre-quencies are limited to  l  / 2   L , where   = c /  f   is thewavelength of sound in glass, and where  l  and  L  are thewidth and length of the glass rod. For  l =3.7 mm,  L =25 mm, and  c  of the order of 1000 m s −1  as measured,see Fig. 2  b  , the frequency is indeed contained between 20and 140 kHz.The acoustic pressure on the surface of the glass rod ismeasured by a needle hydrophone   NP10–3, Dapco  . Thisuncalibrated hydrophone is used to detect the position of thenodes and antinodes at each frequency, rather than absoluteacoustic amplitude. A sweep between 20 and 140 kHz hasbeen performed to identify the resonance modes. For a spa-tial exploration, a homemade micropositioning system with10    m of precision has been used to perform steps of 0.1 mm along the  y -axis. The lubricated needle is in contactwith a free glass rod, not molded in the PDMS matrix.We measure the wave number  k   of the vibration patterns  Fig. 2  a   along the  y -axis, taking into account the fact thatthe wavelength of the pattern is half of the vibration wave-length, because the needle hydrophone gives only the abso-lute value of the acoustic signal. We have access to the speedof the standing wave through the relation  c =   / k  , and we PDMSPDMS  channelglassrod 100 µzy (a)(b)(c) FIG. 1.   Color online   a   Schematic geometry of an acoustically coupledmicrochannel: the channel is filled with water and the main bubble flow isalong the  x   direction. The channel is very thin in the  z  direction. These axesare attached to the channel. Light gray: the glass rod, separated from thechannel by a thin layer of elastomer.   b   Photograph of a cut section of thePDMS perpendicular to the microchannel  x  -axis. The position of the glassrod is above the thin channel, separated by a 100    m PDMS layer.   c  Photograph of the circuit, along  z  direction, without the acoustic glass rod.Here it was tilted by 90° around the main axis for the drag force calibration,with gravity vector along  y -axis. For acoustic measurements, the channelwas horizontal, and gravity vector along the  z -axis. 042003-2 Rabaud  et al.  Phys. Fluids  23 , 042003   2011  Author complimentary copy. Redistribution subject to AIP license or copyright, see  find that  c  varies from 450 to 1000 m s −1 between 20 and120 kHz   Fig. 2  b  . These values are typical of the firstantisymmetric Lamb waves, in agreement with the work of Haake. 10 The vibrations emitted by the glass rod propagate tothe channel and liquid, the PDMS attenuation being small.We measured an attenuation of longitudinal waves inbulk PDMS of 7 dB cm −1 MHz −1 , 20 meaning an attenuationby propagation of 0.007 dB   through 100    m at 100 kHz  ,much smaller than the transmission coefficient at the glass/ PDMS and PDMS/water interfaces. The wavevector for thevibration of the liquid in the channel is therefore  k  = k  Lamb ,and thus slightly different from the wavevector in water  k  w .We measured the vibration of the channel wall  in situ ,with a distant vibrometer based on a LOFI system   LaserOptical Feedback Interferometer  , 21 in order to check that thevibrations are localized near the glass rod. The system, basedon an autodyne interferometer, is particularly efficient andeasy to implement. Its main features are that it is self-alignedand extremely sensitive, thanks to a signal resonance ampli-fication phenomenon. For this study, the setup was composedof a Nd:YAG   neodymium-doped yttrium aluminum garnet  microlaser whose beam was frequency shifted by acousto-optic modulators and then injected into a microscope. Whenthe beam is focused on a scattering interface, we let thebackscattered light be reinjected into the laser, causing itsintensity to be modulated at the shift frequency. If the inter-face under investigation is vibrating, there is a modulation of this frequency by the Doppler effect, generating sidebandsaround the shift frequency in the laser power spectrum. Thevibration amplitude of the interface is then gathered fromthose sideband amplitude using a Bessel analysis.The results obtained for the amplitude of vibration of thechannel   here filled with air   just below the glass rod aresummarized in Fig. 2  c  . The vibration amplitude is muchattenuated out of the borders of the glass rods. In conclusion,the vibration is localized in the channel, and the variation inacoustic amplitude follows that of the glass rod. III. DRAG FORCE FOR A CONFINED BUBBLEIN HELE–SHAW CONFIGURATIONA. Bubble shape in the surfactant solution The shape of a bubble confined in a microchannel isillustrated in Fig. 3: near the top and bottom channel walls, itpossesses almost flat faces lubricated by thin liquid films,while the side surface is curved. Because of the presence of surfactant molecules in water, the wetting of the channel sur-faces is always satisfactory, meaning a vanishing contactangle. The shape of the bubble is parametrized by the chan-nel thickness  h , and the outer radius  R , easy to measure onthe image of the bubble when projected perpendicularly tothe planes. B. Measurements under flow and transverse appliedforce The drag force  F drag  in such a confined geometry differsnotably from the Stokes expression for a sphere in the bulk of a fluid  F Stokes =6      R  V − U  , where     is the dynamic vis-cosity of the liquid,  R  the radius of the bubble,  V  the averagespeed of the fluid, and  U  the bubble speed.We measured the bubble velocity in a fluid stream  V  under a transverse applied force  F   y . To obtain a controlledapplied force, we just used the buoyancy force: in the ab-sence of ultrasound, the circuit is inclined with a variableangle      from 0° to 90°   around the  x  -axis. The gravity vec-tor  g  being perpendicular to the flow   see Fig. 1  b  , thebubbles undergo the buoyancy force and are pulled up in thetransverse direction. This external force is given by F  applied,  y =     R 2 hg  sin    , where     is the difference of den-sity between air and water, and where we assume cylindricalbubbles as an approximation of their real shape, shown inFig. 3. Due to the low Reynolds number   between 0.1 and 1  ,a steady state of the velocity is quickly reached so that 20 40 60 80 100 12005001000f(kHz)     c     (    m     /    s     ) 0 0.5 1 1.5 2 2.5050100 x(mm)      A     (    n    m     ) (a)(b)(c) FIG. 2.   Color online   Vibration of the free glass rod, before molding inPDMS:   a   spatial-frequency diagram of the resonating rod.  y =0 corre-sponds to the free end, the forced end   the piezoelectric   is approximately at  y =25 mm. The color bar indicates the zero to peak voltage values measuredon the hydrophone.   b   Wave speed obtained with the spatial Fourier trans-form, same scale of the abscisses as in   a  ;   c   internal vibration of the topchannel wall, after molding and assembly of the circuit, measured just belowthe glass rod whose limits are shown by dotted lines, along the channel   x  -axis  . Each point is an average of the vibration in the width of the channel   f  =62 kHz  . RU x U y Vh FIG. 3.   Color online   Sketch of the shape of the bubbles confined by theupper and lower faces of the channel. 042003-3 Manipulation of confined bubbles in a thin microchannel Phys. Fluids  23 , 042003   2011  Author complimentary copy. Redistribution subject to AIP license or copyright, see  F drag + F applied =0. The drag force components are therefore F  drag,  x  =0 and  F  drag,  y =− F   y . For a Stokes drag we would thusobtain  U   x  = V   and  U   y = F   y / 6      R .The measurements displayed in Fig. 4 show that this isnot the case:  U   x  / V   and  U   y / F   y    R  are not the expected con-stants 1 and 1 / 6   , but depend on the bubble velocity. Herewe have nondimensionalized the bubble velocity usingCa=   U    the capillary number, constructed with the norm of thebubble velocity  U  =  U   x  2 + U   y 2  1 / 2 and the surface tension     measured to be approximately equal to 35  10 −3 N m −1 forour surfactant solutions  . A first phenomenological descrip-tion of the effect of the capillary number is to fit the mea-sured values with power laws, which is shown on Fig. 4. Theeffect of bubble size and of channel height will be treated inthe following section. C. Model for the drag force In the present configuration, we model the drag force asthe sum of a viscous drag   of the liquid on the bubbles   anda friction force   between the bubbles and the walls of thechannel  , so that the total drag is F drag =  a fluid 12      R 2 h  2 V  −  U   −  a wall   h   h R  3 Ca    −1 U ,  1  where  h  is the height of the channel and Ca=   U  /    is thecapillary number based on the norm of the bubble velocityvector.The first term of the right-hand side is the friction fromthe bulk fluid. This equation has been used by Maruvada  et al. , 17 who derived an expression for the Stokes drag for acylindrical bubble, with slip conditions, following the analy-sis of Taylor and Saffman in Hele–Shaw configuration. 22 Weadd a free parameter  a fluid  to account for a deviation from apurely cylindrical bubble and to account for the influence of surfactants that would change the slip conditions.The second term of the right-hand side, the friction withthe walls, is a correction to the formula 17 and extends it forthe presence of surfactants. This presence modifies the varia-tion of the friction forces with velocity. We introduce phe-nomenological coefficients  a wall  and    , depending on the na-ture of the surfactant. In the following we present aderivation of the equation we use for this friction force withthe walls.Such a phenomenological approach is classical in slip-ping foam studies with different types of surfactants, but herewe feel it is necessary to recall its foundations. First, weintroduce the phenomenological exponent    . A dimensionalanalysis shows that the friction force scales like  F  wall     U  / h F    A F  , 23 where  h F   is the film thickness and  A F   is thearea of friction   see Fig. 5  . In the case of a free interface  pure water   or an interface with very mobile surfactant mol-ecules, the Bretherton theory 24 states that the film thicknessincreases with bubble velocity   “aquaplaning” effect orLandau–Levich lubrication   so that  h F   h Ca 2 / 3 , while thefriction area varies like  A F   h 2 Ca 1 / 3 . The friction forcetherefore may be expressed as  F  wall    h Ca −1 / 3 U    and is thusproportional to  U  2 / 3  . This is in contradiction to the analysisof Maruvada  et al. 17 where the friction area  A F   was incor-rectly set to be a constant   this yields a force proportional to U  1 / 3  . In the case of immobile surfactants, the surface isrigid, and it has been shown 23 that  h F   h Ca 1 / 2 , while thefriction area is constant, so that  F  wall    h Ca −1 / 2 U   U  1 / 2 .See Table I for a summary.These two cases, mobile and immobile surfactants, canbe extrapolated to any type of surfactants by postulating thatthe force may be expressed as  F  wall    h Ca   −1 U    force pro-portional to  U     , the value of     , between 1/2 and 2/3, reflect- 10 −4 10 −3 10 −2 10 −2 10 −1 10 0  U x  /VU y  µ  R /FyCa FIG. 4.   Color online   Measurements of the axial bubble velocity  U   x   in-duced by the stream velocity  V   and deviation velocity  U   y  induced by atransverse force  F   y , as a function of the capillary number based on the normof the bubble velocity. Dashes: Saffman–Taylor model for a bubble in purewater, which neglects wall friction   a wall =0  . Several channel thicknessesare tested:   ,  h =50    m;   , 70    m;   , 100    m. The bubble radii varyfrom 40 to 80    m for all thicknesses. Power-law fits are plotted as dashedlines, with exponents of 0.52 for the scaled  U   x   and 0.56 for the scaled  U   y . U h r  Plateau  h F   A F  (a)(b) FIG. 5.   Color online   Cross-section of    a   one isolated bubble; in white thegas.   b   Comparison with a foam composed of one layer of bubbles. Theinsert is an enlargement on the liquid corners where dissipation is localizedin both cases.TABLE I. Summary of the friction models with mobile and immobile sur-factants.Surfactant Film thickness Friction area Friction forceMobile a h F   h Ca 2 / 3  A F   h 2 Ca 1 / 3 F  wall    h Ca −1 / 3 U  Immobile b h F   h Ca 1 / 2  A F   cst  F  wall    h Ca −1 / 2 U  a Reference 24. b Reference 23. 042003-4 Rabaud  et al.  Phys. Fluids  23 , 042003   2011  Author complimentary copy. Redistribution subject to AIP license or copyright, see  ing the mobility of the surfactant. This variable exponent iswidely used in slipping foam studies, 25 as well as in foamdrainage or rheology characterization. 26 Second, we have also introduced the influence of theratio of the thickness to the bubble size  h /  R . We are inspiredby the predictions of Terriac  et al. 27 for bubbles in contact  thus forming a foam   in Hele–Shaw cells. They considerthat dissipation is actually localized within liquid corners,and this is the radius of the liquid corners that counts   seeinset of Fig. 5  . In the case of foams, the liquid corner as aradius equal to the radius of the Plateau border, i.e., the me-niscus joining liquid to walls   see Fig. 5  b   for the definitionof   r  Plateau  . Here the liquid corner has a radius equal to half of the channel height  r  Plateau = h / 2. Equivalently, the bubbles ina foam have the same shape as isolated bubbles when r  Plateau = h / 2. Setting this value for the liquid corner size, theanalysis of Terriac for a bubble of spanwise diameter 2  R  since the spanwise width of the liquid corner at the wallssets the total friction 28   yields a friction force  F  wall  2  R    h /  R  −2  h /  R  3 Ca       h  h /  R  3 Ca    −1 U  , that we usein Eq.   1  .In conclusion, the total drag force is given by Eq.   1  , inwhich the phenomenological coefficients     ,  a fluid , and  a wall  will be adjusted in experiments.The projections of Eq.   1   onto the  x  - and  y -axes give thebubble velocity components  U   x   and  U   y  as a function of theexternal flow  V    here along the  x  -axis   and transverse force F  applied,  y   along the  y -axis  , U   x  V    24     Rh  2 a fluid a wall   h R  3 Ca  1−   ,   2    hU   y F  applied,  y =1 a wall   h R  3 Ca  1−   .   3  To obtain Eq.   2  , we have assumed  U   x   V  .We plot in Fig. 6 the measured bubble velocity compo-nents  U   x   and  U   y  scaled by  V   24     R / h  2 and  F  applied,y /   h ,respectively, versus   h /  R  3 Ca. All the points collapse onpower law curves as expected from Eqs.   2   and   3  , for awide range of conditions:  h  ranges from 50 to 100    m,  R from 34 to 83    m, and  V   from 7 to 33 mm s −1 . With thisnew rescaling, data points are slightly less dispersed than inFig. 4. The dispersion in the values of the scaled  U   y  dropsfrom   29% down to   27%. Additionally, the range of thescaled data is larger by one order of magnitude. We thereforeuse this new scaling designed to describe large range of variations in channel thickness and bubble radius. So we areable to adjust the parameters    ,  a wall , and  a fluid  in Eqs.   2  and   3  .We now discuss the value of     , the exponent of theCapillary number in Eq.   3  . According to Denkov  et al. , 23 this exponent reflects the nature of the tangential mobility of the surfactant molecules on the surface of the bubbles. Thevalue    =0.51 corresponds to tangentially immobile surfac-tants. This may be due to large Marangoni stresses. Here theconcentration of surfactant in the solution is high, 40 timesthe critical micellar concentration, and the surface tensiondrops down to    =35  10 −3 N / m, instead of     w =73  10 −3 N / m for a clean interface. Surfactants can thereforecreate Marangoni surface stresses up to     =   w −   =38  10 −3 N / m. The ratio of these stresses to viscous stressesmay be expressed as     /   U  =    /    Ca −1 . In the presentexperiment this ratio is always above 500   value at largestvelocity  , meaning that surfactants create surface stressesthat are high enough to immobilize the surface in front of viscous stresses.This phenomenon is important because it governs thenature of the friction on the walls of the channel. The valueof the coefficient  a fluid =4.53, that gives the friction from theflow around the bubble see Eq.   1  , is substantially higherthan 1, which also suggests that instead of a slip velocitythere is an immobile velocity at the surface.In conclusion, we have calibrated the friction force act-ing on confined bubbles. We are thus able to deduce thevalue of any transverse external force acting on the bubblesfrom the measurement of their drift velocity   any externalforce is equal and opposite to the transverse drag  . Accordingto Eq.   1   and from several calibrations, we end up with anempirical formula that may be expressed as  F  applied,  y  10.9   h  h /  R  3 Ca  −0.49 U   y . IV. THE ACOUSTIC BJERKNES FORCEFOR A CONFINED BUBBLEA. Measurements from deviation velocityin the acoustic field A measurement of acoustic force applied to the bubblesis obtained when considering the acoustic deviation velocity U   y  of the bubbles in the absence of gravity effects   horizon-tal channel   and during the emission of an ultrasonic stand-ing wave.We plot in Fig. 7 the results obtained for the acousticforce as a function of the bubble radius under constant acous-tic conditions   frequency of 91 kHz, amplitude of the electricsignal sent to the piezo-50 V  . The first striking feature is thelarge amplitude of the acoustic forces: they amount to nearly200 nN, enough to counteract the friction forces that are high 10 −4 10 −3 10 −2 10 −3 10 −2 10 −1 U x  /V /(24 π (R/h) 2 )U y  µ  h /Fy(h/R) 3 Ca FIG. 6.   Color online   Adimensioned velocity components  U   x    top   and  U   y  bottom  , as a function of    h /  R  3 Ca, proportional to the total bubble velocity U  . Lines: power fits with Eqs.   2   and   3   are    =0.51,  a wall =10.9, and a fluid =4.0. Only the values  U   x  / V   0.5 are fitted. Same symbols than inFig. 4. 042003-5 Manipulation of confined bubbles in a thin microchannel Phys. Fluids  23 , 042003   2011  Author complimentary copy. Redistribution subject to AIP license or copyright, see
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