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Experimental Thermal and Fluid Science 35 (2011) 849–865 Contents lists available at ScienceDirect Experimental

Contents lists available at ScienceDirect

Experimental Thermal and Fluid Science

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Science journal homepage: www.else vier.com/locate/etfs A critical review of the measurement techniques for the

A critical review of the measurement techniques for the analysis of gas microflows through microchannels

Gian Luca Morini , Yahui Yang, Habib Chalabi, Marco Lorenzini

Dipartimento di Ingegneria Energetica, Nucleare e del Controllo Ambientale, Alma Mater Studiorum, Università di Bologna, Viale Risorgimento 2, I- 40136 Bologna, Italy

article info

Article history:

Received 12 November 2010 Received in revised form 21 February 2011 Accepted 21 February 2011 Available online 25 February 2011

Keywords:

Microfluidics Microconvection Friction factors in microchannels Rarefied gases Compressible gases

abstract

In Microfluidics, a large deviation in the published experimental data on the dynamic and thermal behav- ior of microflows has been observed with respect to the classical theory but, from a chronological analysis of these experimental results, it can be realized how the deviations in the behavior of fluid flows through microchannels from that through large-sized channels are decreasing. Today, it seems to be clear that some of the inconsistencies in the data were originated from the experimental methods used for the investigation of convective microflows. This fact highlights the need for the development of specific mea- surement techniques for Microfluidics. In this work, we explore and categorize different approaches found in literature for measuring microflow characteristics, especially for gas flows, and the geometry of the microchannels pointing out the advantages and disadvantages inherent to each experimental tech- nique. Starting from the operative definition of friction factor, the main parameters that must be checked in an experimental work in order to characterize the flow are reviewed. A discussion based on uncer- tainty analysis will be presented in order to individuate the main operative parameters that one must be able to measure accurately to determine pressure drop in the microchannels with a low level of uncer- tainty. In the paper each measurement technique is critically analysed to evidence the important issues which may have been overlooked in previous researches. The main goal of this study is to give a summary of experimental procedure and a useful guideline for experimental research in Microfluidics. 2011 Elsevier Inc. All rights reserved.

1. Introduction

During the last 10 years a rapid development of new microflow devices (MFD) in several scientific fields has taken place. Nowa- days, the manufacture of MFDs, like micropumps, microvalves, microcold plates, microheat exchangers, and other microcompo- nents and sensors used in chemical analysis, in biomedical diag- nostics or in flow measurements, is a consolidated reality. The design of new MFDs requires a deep knowledge of the fluid- dynamic and heat transfer phenomena within microchannels in which a liquid or gas flows. For this reason, many experimental studies have been con- ducted in order to analyze the behavior of convection through microchannels, of which a review is given in [1–3] . In particular, the main goal of these studies was to determine the friction factors and the convective heat transfer coefficients through microchan- nels in which a pressure-driven flow was imposed. These experimental results have been used in order to verify if the laws governing transport phenomena within channels of mac-

Corresponding author. Tel.: +39 051 2093381; fax: +39 051 2093296. E-mail address: gianluca.morini3@unibo.it (G.L. Morini).

0894-1777/$ - see front matter 2011 Elsevier Inc. All rights reserved. doi: 10.1016/j.expthermflusci.2011.02.005

roscopic dimensions still hold at the microscale, and, if not, which new effects must be taken into account at the microscale. A large scatter in published experimental data and inconsisten- cies have been observed with respect to the classical theory but, from a chronological analysis of these results, it is possible to extrapolate how the deviations between the behavior of fluids through microchannels and through large-sized channels are decreasing. The last experimental works in Microfluidics seem to highlight that some of the observed discrepancies in the data were originated from the experimental methods used for the investiga- tion of convective microflows. In fact, in the last years a dramatic improvement of the tech- niques of microfabrication has enabled a more accurate control over the geometry of microchannels and innovative and more accurate measurement techniques for microflows have been pro- posed with a general improvement of the reliability/accuracy of the experimental data reported in the literature: these latest data seem to be in agreement with the classical theory. This highlights the need for the development of specific mea- surement techniques for the Microfluidics field or a refinement and adaption of the ones used at larger scales. In this work, we explore and categorize different approaches found in literature for measuring microflow characteristics – especially for gas flows – and the geometry of the microchannels

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Nomenclature

d

inner diameter of circular microtube (m)

Greek symbols

D h

hydraulic diameter of channel, 4 X / C (m)

a

coefficient defined in Table 3

f

friction factor

b

coefficient defined in Table 3

h

height of rectangular microchannel (m)

c

specific heat ratio

t

time (s)

C

wetted perimeter (m)

L

channel length (m)

k

gas mean free path (m)

K

pressure loss coefficient

l

dynamic viscosity (Pa s)

Kn

Knudsen number, k/ D h

q

gas density (kg/m 3 )

_

mass flow rate (kg/s)

coefficient related to channel geometry in Eq. (12)

m

r

Ma

Mach number

s

viscous stress (Pa)

p

pressure (Pa)

X

area of cross-section (m 2 )

R

specific gas constant (J/(kgK))

Re

Reynolds number

Subscripts

T

temperature (K)

cr

critical value

v

average axial velocity (m/s)

in

inlet value

V

volume (m 3 )

out

outlet value

w

width of rectangular microchannel (m)

w

pertains to the channel wall

W

mean flow velocity (m/s)

z

axial direction

by examining the advantages and disadvantages inherent to each of them. Starting from the operative definition of friction factor, the main parameters that must be checked in an experimental campaign in order to characterize the flow are highlighted. A discussion based on uncertainty analysis is presented in order to pinpoint the main operative parameters that must be measured accurately to determine the pressure drop in the microchannels with a low level of uncertainty.

2. Pressure drop and friction factor

The behavior of isothermal pressure-driven single phase fluid flows in microchannels can be studied by determining the velocity distribution in the fluid region with the help of the mass conserva- tion principle (continuity equation) and the equations of conserva- tion of fluid momentum (Navier–Stokes equation). Consider a flow through a straight microchannel having an axi- ally unchanging and uniform cross-section with an area equal to X and a wetted perimeter equal to C ; it is possible to define the hydraulic diameter of the microchannel as:

D h ¼ 4X

C

ð

1Þ

and the mean fluid velocity as the integrated average axial velocity over the flow area X :

W ¼

1

X Z X

v z dX ¼

_

m

qX ¼

RT m

_

X

p

ð

2Þ

In Eq. (2) the relationship between the average axial velocity

and the measurable quantities, like mass flow rate m , density q and cross-section area X or pressure p and temperature N for gases is highlighted ( R is the specific gas constant). It is important to highlight that Eq. (2) has been written for an ideal gas: this means that we have restricted our analysis to pressures below the critical one ( p cr ) and/or to temperature larger than two times the critical temperature ( T cr ) for the gas considered. This hypothesis holds in Microfluidics because the gas temperature is generally larger than the critical one. During experiments in microchannels it is difficult to directly derive the mean fluid velocity along the channel from the cross-sectional velocity profile, especially when the micro- channel is very small and without optical access which can enable the use of non-intrusive specific optical techniques developed with

_

this aim as the microParticle Image Velocimetry ( l PIV) [4] . The limitations of velocimetry techniques for gas flows in microchan- nels will be discussed in the next sections. Therefore, the mean velocity of flow is often calculated measuring the microchannel cross-sectional area, the fluid density and the mass flow rate, as per the RHS of Eq. (2) . The pressure drop D p along the channel and the viscous stresses at the channel walls can be related to the mean fluid velocity by means of the following expressions:

js w j ¼ f F qW 2 ! Dp ¼ f D

2

L

qW 2

D

h

2

¼

ð4f F Þ

L

qW 2

D

h

2

ð

3Þ

where L is the microchannel length. These equations are used as definition for the Fanning friction factor ( f F ) and the Darcy friction factor ( f D = 4f F ). Eq. (3) evidences that the pressure drop along a microchannel can be predicted if one knows the value of the friction factor. For an incompressible, isothermal flow the Darcy friction factor can be operatively defined as:

f D ¼ D h

L

2q

_

m

X

2

ð p in p out Þ

ð 4Þ

where p in and p out are the pressure at the channel inlet and outlet respectively. For isothermal compressible gas flows, using the state equation

of an ideal gas, the expression of friction factor can be re-written as

follows:

f D ¼ D h

L

p

2

in p out 2

RT

_

m

X

2

2 ln

p

in

p

out

!

ð 5Þ

where T is the gas temperature, and R the gas constant respectively. Since in microchannels the pressure drop along the tube length can be much larger than for conventional-size tubes, the effects of gas acceleration cannot be neglected in general, even for very low values of the Mach numbers as observed theoretically and experi- mentally by several authors [1,3,5]. The gas acceleration leads to the velocity profile change not only in magnitude but also in shape; the magnitude increment produces an additional pressure drop while the continuous variation in shape of the velocity profile means no fully or locally fully developed flow occurs. In heated microchannels, since the fluid radial temperature profile is

G.L. Morini et al. / Experimental Thermal and Fluid Science 35 (2011) 849–865

851

strongly dependent on the radial velocity profile no fully developed temperature profiles will occur as long as the flow is developing. In tubes having an inner diameter less than 500 l m and with a large length-to-diameter ratio (long tube) high pressure ratios be- tween inflow and outflow and high heat transfer ratios produce a significant increase of the Mach number along the tube and high Mach numbers yield higher friction factors and heat transfer rates. In adiabatic and in heated microchannels, the compressibility ef- fects can be monitored by using the diameter-to-lenght ratio ( d/ L ) of the microtube and the outlet Mach number defined as follows:

Ma out ¼

4

_

m

pd 2 p out

ffiffiffiffiffiffiffiffiffiffiffi

s

RT out

c

ð

6Þ

where c is the specific heat ratio of the gas considered and T out and p out are the gas bulk temperature and pressure at the outlet of microchannel. The conventional theory states that if the average value of the Mach number ( Ma avg ) along a channel is less than 0.3 the flow can be modeled locally as incompressible. In addition, when the pressure drop along the tube length is lower than 5% of the inlet pressure, the effect of the acceleration of the gas flow in the axial direction can be neglected (in other words, the variation of the gas density along the channel can be neglected):

(

Ma av g > 0: 3

p in p out

p in

> 0: 05

ð 7Þ

When the first inequality is satisfied, the gas flow is not locally incompressible and the momentum and energy equation have to

be solved as coupled. When the second inequality is satisfied, even

if the gas flow can be locally modeled as incompressible, the den-

sity variation along the tube cannot be ignored. In this case, the ef- fects due to the gas acceleration along the tube become important, even if the Mach number is low. The gas acceleration losses are ta- ken into account in the evaluation of the friction factor through the second term of the right-hand side of Eq. (5) . For microchannels, it has been demonstrated by Yang et al. [6] that the friction factor is influenced by the value of the Mach number at the outlet (Eq. (6) ); when Ma out is larger than 0.3 a deviation of the friction factor from the prediction of the conventional theory is evidenced. For this rea- son, the two constraints of Eq. (7) (with Ma out instead of Ma avg )

have always to be verified when an experimental determination of the friction factor in a microchannel for a gas flow is made in or- der to know whether compressibility effects can be considered negligible. In Fig. 1 the trend of the Darcy friction factor as a function of the Reynolds number for a nitrogen flow through a microtube having a circular cross-section, with an inner diameter equal to 172 l m and

a length of 10 cm is shown [6] . The error bars related to the exper-

imental friction factors are not shown in order to improve readabil- ity; the maximum relative uncertainty on the friction factor is equal to ±10% as indicated in [6] . It is possible to see that the agree-

ment between the experimental data and the Poiseuille law ( f D = 64/ Re ) is very good in the laminar regime, at least up to Re equal to 1200. For Re > 1200 it is evident a departure of the friction factors from the Poiseuille law; this behavior can be explained by observing the value taken by the outlet Mach number ( Ma out ) in this case, as it becomes larger than 0.3. This result is typical for microtubes having an inner diameter smaller than 500 l m. In the laminar regime, the deviation from the Poiseuille law can be theoretically explained by solving the Navier Stokes equation for compressible flows [5,7] . When the pressure ratio increases, the outlet Mach number increases, especially for short microtubes, and the friction factor increases with the Mach number. Asako

the friction factor increases with the Mach number. Asako Fig. 1. Darcy friction factors for nitrogen

Fig. 1. Darcy friction factors for nitrogen flow through a microtube in adiabatic conditions as a function of the Reynolds number (from Yang et al. [6] ).

et al. [7] have calculated numerically how the friction factor de- pends on the Mach number in the laminar regime and proposed the following correlation:

2

f D ¼ 64 þ 2:703 Ma þ 93: 89 Ma Re

Re

Re

ð 8Þ

As can be noticed from Eq. (4), for incompressible flows the knowl- edge of the differential pressure between the microchannel inlet and outlet is required only in order to determine the friction factor. On the contrary, Eq. (5) shows that for a compressible flow even the absolute value of the gas pressure at the inlet or at the outlet is needed. This aspect underlines that the experimental strategies for the determination of the friction factor must be different whether compressibility effects are negligible or not. The local measurement of pressure is problematic for micro- channels: drilling pressure taps along the channel can be challeng- ing due to the small dimensions involved. For this reason, in the most accurate experimental works, special microchannels are de- signed with customized pressure taps along their length (Bavière et al. [8] ). On the other hand, when commercial microtubes or standard microdevices are used in the tests, the measurement of the pressure along the microchannel becomes impossible. In these cases, pressure measurements are usually performed by connect- ing with appropriate fittings both sides of the microchannel to a larger reservoir, where the pressure taps can be drilled without difficulties. However, in this way the pressure measured is not that at the inlet and outlet, which is associated with the change of section. These non-negligible minor losses ( D p in , D p out ) are due to the abrupt change in flow area between the manifolds and the channel. The total pressure drop, which is the measured pressure difference between the reservoirs, can be expressed as follows:

Dp total ¼ Dp in þ ðp in p out Þ þ Dp out

ð 9Þ

For perfect gas flows, the minor losses at the inlet and outlet can be determined as follows:

Dp in ¼

K in

2

_

m

X

2

RT

p in

;

Dp out ¼

K out

2

_

m

2

RT

p

X

out

ð

10Þ

For conventional-sized tubes the values of K in and K out have been established for a number of simple entrance and exit geometries and are quoted in many textbooks (e.g. Idelchik [9]). These coeffi- cients have been evaluated under the assumption of essentially uni- form velocity at the inlet but considering a fully established velocity

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G.L. Morini et al. / Experimental Thermal and Fluid Science 35 (2011) 849–865

profile in the channels (that means L D h ). These assumptions can be considered verified for microchannels, where L > 100 D h as a rule. In applying the data related to the values of K in and K out it should be remembered that these coefficients already include the pressure change associated with the change in the velocity profile and depend on the geometry of the ends and of the channels. In addition, for the estimation of the minor losses it is mandatory to know the absolute value taken by the pressure at the inlet or at the outlet, as evidenced by Eq. (10) . In Fig. 2 the minor losses at the inlet ( D p in ) and at the outlet ( D p out ) are compared with the value of the net pressure drop ( D p n = p in p out ) for two microtubes (5 cm and 50 cm long) with an internal diameter equal to 100 l m [10] when a nitrogen flow is imposed through the microtubes. From Fig. 2 it is evident that the minor losses at the outlet of the microtubes are one order of magnitude lower than the net pressure drop while those at the in- let are two order of magnitude less. The relative weight of the min- or losses increases for large values of the Reynolds number and the contribution at the inlet becomes more important for short micro- tubes. On the contrary, the value of the minor losses at the outlet is independent of the length of the microtube because in the experi- mental tests of Morini et al. [10] the gas at the exit vented directly into the atmosphere and hence the pressure at the exit was always equal to the atmospheric value. Fig. 2 underlines that the role of the minor losses on the evaluation of the friction factor in laminar regime has to be considered of importance for short microtubes ( d/ L > 0.01) having a low value of the inner diameter. The correct evaluation of these losses is a crucial point for the accurate calculation of the friction factors for gas flows in micro- channels. For example, to the best of the Authors’ knowledge, the effect of the rarefaction of gases on the K in and K out have not been systematically investigated up to now and this fact can be an important source of error for the experimental investigation of the pressure drop for rarefied flows through microchannels. When the effects related to rarefaction become significant the friction factor is influenced by the value of the Knudsen number, the ratio of the gas mean free path ( k ) and the characteristic dimension (usually D h ) of the channel:

Kn ¼ k

D

h

¼ l

D h p

r

ffiffiffiffiffiffiffiffiffi

pRT

2

ð11Þ

where l is the dynamic viscosity of the gas, p is the local value of the pressure and the gas mean free path is evaluated with the

pressure and the gas mean free path is evaluated with the Fig. 2. Minor losses and

Fig. 2. Minor losses and net pressure drop ( D p n = p in p out ) for nitrogen flow through microtubes 5 cm long (empty symbols) and 50 cm long (full symbols) with an internal diameter equal to 100 l m (from Morini et al. [10] ).

formula k M ¼

1879 [11] . The analysis of gas rarefaction effects in internal flows is a spe- cific feature of the analysis of convective flows through microchan- nels. When the Knudsen number is less than 0.001, rarefaction effects can be considered negligible; for 0.001 < Kn < 0.1 the slip flow regime occurs. From a theoretical perspective, the friction fac- tor tends to be reduced when the Knudsen number increases be- cause of the slip existing between the gas and the channel walls. It has been demonstrated that in laminar regime the friction factor depends on the Knudsen number and on the cross-section geome- try of the microchannel as follows:

RT proposed originally by Maxwell in

ffiffiffiffiffiffiffiffiffi

p

p

= 2

l = q

p

ffiffiffiffiffiffi

f D ð Kn Þ ¼ f D ð Kn ¼ 0 Þ

1

1 þ rKn

ð

12Þ

where f D (Kn = 0) indicates the value of the Darcy friction factor in the laminar regime for the channel geometry considered when the rarefaction is negligible ( Kn = 0); the friction factor reduction is related to the channel geometry through the coefficient r and to the Knudsen number. The value of r for channels with different geometries, typical of microfluidic applications (i.e. circular, rectan- gular, trapezoidal and double-trapezoidal) and different aspect ra- tios was reported by Morini et al. [12] . Observing Eqs. (4)–(12) it is evident that, in order to character- ize and analyze a microchannel flow in terms of friction factor, the following quantities should be determined:

(a) microchannel geometry, including the roughness of the channel wall, the hydraulic diameter: this means to know the geometrical characteristics of the cross-section, the geometry of the connections between the microchannels and the reservoirs (if any) and the microchannel length; (b) operating conditions including quantities such as fluid tem- perature, differential pressure between inlet and outlet, absolute pressure at one end of the channel and mass flow rate.

The above observations can be summarized by stating that the friction factor for a microchannel can be considered in general a function of the following quantities:

f D ¼ f D ð Dp; p ; m; T ; C; X; L ; K in ; K out Þ

_

ð

13Þ

Among the other variables appearing in Eq. (13) the friction factor can depend in turbulent regime also on the wall relative roughness (e /D h ) of the microchannel; it has been demonstrated that, even in laminar regime, very large values of the relative roughness ( e / D h > 5%) can influence the value of the friction factor [13] . Using the physical variables recalled in Eq. (13) one can calcu- late also the Mach number by means of Eq. (6) and the Knudsen number by means of the Eq. (11) ; through these values one can check the effect of compressibility and of rarefaction on the friction factor and compare the results with the theoretical predictions for compressible and rarefied gases. With these parameters in mind, special consideration must be paid both to the design of the experimental setup and to measure- ments during a specific test round at such a small scale to ensure a certain accuracy for reasonable results. Focussing on the experi- mental determination of the friction factor in microchannels for gas flows, with the aim to discuss the role played by each param- eter on its determination, a detailed analysis of the most interest- ing experimental techniques for the measurement of the channel dimensions, gas pressure, temperature, velocity and mass flow rate, together with the analysis of the typical values of their uncer- tainty, is presented in the coming sections.

G.L. Morini et al. / Experimental Thermal and Fluid Science 35 (2011) 849–865

853

3. Measurement techniques for microchannels

In this section the most interesting measurement techniques proposed for the determination of the physical quantities useful for the determination of the friction factor in microchannels are summarized.

3.1. Measurement of microchannel dimension and of its roughness

In the experimental tests devoted to the pressure drop analysis in microchannels some methods have been used in order to esti- mate the inner diameter of microtubes. Poiseuille [14] in 1840 used mercury to fill glass capillary tubes (down to 15 l m of diam- eter) of a fixed length in order to determine the average diameter by weighing the tube before and after filling. This technique is very simple and enables an accurate determination of the average flow- ing area of a microchannel along its whole length. One limitation is that, in order to obtain a good accuracy of the measurement for very small tubes, one has to use very long microtubes. An advan- tage of this method is that only a precision balance is required to estimate the flowing area. One interesting development of this technique is based on the accumulation of a heavy liquid (water, mercury, etc.) flowing through a microtube under a constant pressure drop, which gener- ates a constant mass flow rate through the channel [7] . If one knows the length of the microchannel, the fluid density and the viscosity, the cross-sectional area of the microchannel can be determined by a careful measurement of the liquid weight passing through the microtube over a certain time interval: this implies that the Poiseuille law is assumed to hold at the microscale too. This technique can be very useful to reduce the uncertainty on the determination of the inner diameter of a microtube as demon-

strated by Asako et al. [7] , who reported an uncertainty of the order of ±0.2 l m on average inner diameter measurement for a tube with

a nominal diameter of 150 l m (±0.13%). For very small mass flow rates this measurement technique requires very long time for li-

quid accumulation. As underlined by Asako et al. [7] , when water

is used as test fluid, care must be used in order to estimate the lost

weight of the accumulated liquid due to evaporation during the experimental tests, which strongly depends on the environmental condition. This aspect can be very critical when lower mass flow rates are generated in the smaller microchannels. Currently, one of the most common methods to measure micro- channel dimensions is the scanning electron microscopy (SEM), which images the profile of the channel cross-section with a high resolution. When the tested microchannels are closed (e.g. com- mercial microtubes), this technique is applicable to the inlet and outlet sections only; no information can be derived on the axial variation of the channel geometry and on the roughness distribu- tion along the channel. This can represent a strong limitation for the correct evaluation of the average channel roughness because the inlet and the outlet sections may be non-representative of the dominant cross-section along the length due to the cutting which may deform the ends. In this case, only with destructive tests after the experimental investigation can one try to recon- struct the axial variation of the roughness and of the cross-section by grinding the channel open. Multiple cuts along the channel may prove useless because the action can change the channel’s cross- section permanently. On the contrary, for open or optically acces- sible microchannels (like silicon rectangular microchannels bonded with a silicon/glass cover) this technique can be applied before the specimens are sealed. With magnification and image processing, the dimensions of the channel cross-section and the topology of the roughness can be determined with a good accuracy. Since this technique is convenient and exhibits satisfying accuracy,

it has been employed by many investigators (Tang et al. [15] , Celata et al. [16] , Zohar et al. [17] , Morini et al. [10,18] ). It is inter- esting to note that the Poiseuille [14] and Asako et al. [7] methods allow to measure directly the average flowing area along the whole length of the microchannel, which is a significant parameter for the evaluation of the friction factor as compared to the algebraic aver- age of the inlet and outlet area obtained by SEM imaging. Still concerning the roughness, in non-circular microchannels made by chemical or ion etching on silicon wafers and sealed with different materials (glass, Pyrex, silicon) the distribution of the wall roughness along the wetted perimeter of the channel can ex- hibit a strong non-uniformity. However, in this case the measure- ment of the wall roughness is generally possible by using scanning electron microscope or profilometers along the channel before sealing it. Another characteristic dimension of the microchannels which must be evaluated for the determination of the pressure drop is the channel length L . For long microchannels, the length L is in gen- eral larger than the inner diameter; typical values of the D h /L ratio fall within the range 0.1–0.001. In this case, the measurement of L is easier than the measurement of the inner diameter. On the con- trary, when the behavior of rarefied gases through microchannel is studied in order to verify the predictions of the mathematical mod- els based on the Boltzmann equation for transitional and free molecular regimes, very short microchannels must be tested which are characterized by D h /L ratios near unity (Marino [19] ). In this case, the measurement of L can become problematic and, as gen- eral rule, characterization of the microchannel must take also the tube length into account, rather than just the hydraulic diameter, as is otherwise customary.

3.2. Measurement of pressure

In the experimental works devoted to pressure drop analysis through microchannels, pressure measurement has been carried out: (i) only at the inlet and at the outlet of the channel (Kandlikar et al. [20] , Asako et al. [7] , Morini et al. [18] , Celata et al. [16] , Tang et al. [15] , Demsis et al. [21] ); (ii) and/or along the channel in order to reconstruct the axial distribution (Zohar et al. [17] , Hsieh et al. [22] , Jang and Wereley [23] , Turner et al. [24] , Kohl et al. [25] ). In the latter case, the knowledge of the axial pressure trend enables to identify special effects, as those related to compressibility and rarefaction, which can play an important role in the determination of the pressure drop; however, the microchannel must be specifi- cally provided with pressure taps along its length. If traditional pressure transducers are used, these are generally placed in the reservoirs connected to the microchannel inlet and outlet. Their presence introduces pressure losses at the inlet and the outlet of the channel which can be determined with Eq. (10) . In order to eliminate the effects of these minor losses the tube cutting method has been proposed by Du et al. [26] and other authors (Asako et al. [7] , Celata et al. [16] ). This technique consists of repeating the same mass flow rate conditions of a long tube in a short one with the same inner diameter. Since the effect of the minor losses is approx- imately identical for both tubes, one can eliminate it by subtracting the total pressure drop determined for the two. The short and the long tube can be selected from a set of identical tubes or one can obtain the short one by cutting the long tube. In the latter case, care must be exerted in minimizing the effect of the cut on the geometry of the microchannel. When the selection of the short tube and the long one is made among commercial tubes with the same nominal diameter, Asako et al. [7] demonstrated that the real inner diameter may actually vary markedly: in their work in order to obtain a diameter difference in each pair chosen less than 0.1 l m only three pairs of tubes were selected from precise inner diameter measurement among more than 30 specimens, which

854

G.L. Morini et al. / Experimental Thermal and Fluid Science 35 (2011) 849–865

have a nominal diameter of 150 l m but actually vary from 148 l m to 154 l m. This kind of difference in diameter is stochastic and uncontrollable, which means that with the tube cutting method, the smaller the difference in tube pairs one desires, the larger the number of the sample one has to provide. With this method, the value of the friction factor for a microtube can be calculated as follows (as indicated in Morini et al. [18] ):

f ¼ 2q

l

2

Dp

total

ð L Þ Dp

1

total

ð L Þ

2

L

1

L

2

D

3

h

Re

2

ð14Þ

where L 1 and L 2 are the lengths of the longer and shorter tube respectively. It has been demonstrated that this method can only be applied correctly when the pressure drop in the tube is linear, as for incom-

pressible flows (liquids or gases under low pressure ratio p in / p out ). When the pressure distribution along the channel is not linear, as

in the case of compressible and/or rarefied flows, this method can-

not be applied. In fact, in this case the effect of the minor losses

cannot be eliminated completely, as demonstrated by Morini

et al. [18] . This means that for gas flows this method holds only

for low Reynolds numbers which corresponds to low Mach num- bers at the outlet. When the goal is to determine the axial distribution of the pres- sure along a microchannel other techniques can be employed. A

non-intrusive one for the pressure determination along a micro- channel is based on Pressure-Sensitive Paints (PSP). PSPs are optical ‘‘molecular-sensors’’ which enable the measure of the pressure over a surface. When excited by an outer light source of a certain wavelength, the luminescent molecules with which the surface of the channel cover is coated will emit lumines- cence of a longer wavelength. By appropriate filtering, the emitted luminescence can be detected. The luminescent intensity is sensi- tive to oxygen molecules near the cover surface and for this reason this technique has been proposed for the analysis of gas flows. Spe- cifically, an increase in the oxygen concentration causes a decrease

in the intensity of the luminescence, which is known as oxygen

quenching (Huang et al. [27] and Liu et al. [28] ). After calibration,

a relation between pressure and luminescent intensity can be

established. This non-intrusive measurement technique can pro- vide pressure data with high spatial resolution both along the

channel and at the channel entrance and exit. On the other hand,

as this technique is based on oxygen quenching, it cannot be ap-

plied to test of other pure gases, such as N 2 and He. Moreover, the pressure sensitive paint is coated on a transparent cover of

the microchannel to ensure the direct contact with oxygen and excitation of luminescent molecules from an external light source.

It is evident that the main disadvantage of this technique is tied to

the shape of the microchannel tested: circular or elliptical micro- tubes make it impossible to coat the pressure sensitive paint onto the inner wall, and passages which do not have a transparent side cannot benefit from this optical technique.

The pressure sensitive paint (PSP) technique has been applied to the measurement of the pressure distributions in high Knudsen

number regimes by Liu et al. [29] and Bell et al. [30]. Because the PSP works as a so-called ‘‘molecular sensor’’, it is considered suit- able for the analyses of high Knudsen number flows, which require diagnostic tools at the molecular level. However, an application of PSPs to microdevices is very difficult, because conventional PSPs are very thick compared to the dimension of microdevices owing

to the use of polymer binders. Moreover, they do not have suffi-

cient spatial resolution for the pressure measurement of micro- flows due to the aggregation of luminescent molecules in polymer binders as indicated by Mori et al. [31] . More recently, for localmeasurement of pressure in high Knudsen numbers Matsuda et al. [32,33] developed a pressure-sensitive

molecular film method (PSMF) by using the Langmuir–Blodgett (LB) technique. Before applying PSMF to micro gas flows, the authors have tested the dependence of temperature on pressure sensitivity, which is the main factor of the measurement error for this kind of pressure sensor. Matsuda et al. [33] have demon- strated that their paint composed of Pt(II) Mesoporphyrin IX and arachidic acid showed a small dependence of pressure sensitivity on temperature, while that of luminescent intensity is significant.

In addition, the authors have demonstrated how, compared with the classical PSP method, the PSMF method can offer more uniform pressure sensitivity and an enhanced intensity of luminescence emission. By applying their technique to the determination of the pressure field for gaseous flow through a 2-D nozzle [32] , they con- cluded that the spatial resolution of PSMF is high enough for microscale flow measurements whose characteristic length is over 50 l m. In order to measure the local pressure along a microchannel Kohl et al. [25] explored and proposed the optical lever method for pressure measurement. The microchannel presents a number of micrometric pressure taps connected to silicon membranes which deform according to the local pressure. The deformation was measured recording the change in deflection angle of a fixed incident laser targeting the membrane surface. The change in deflection angle was measured by a photodiode sensor which can be precisely moved and positioned. Based on this principle, an inte- grated pressure sensor can be produced. The sensitivity of this integrated pressure sensor can be easily adjusted by changing the spatial resolution (the distance between the membrane and the photodiode sensor). The uncertainty on the measured pressure ranged from ±2.4% to ±13.3%. Since a very precise optical system to test quantitatively the slight slope of the pressurized membrane is involved, it requires great labor to adjust this system. Also such optical system, which includes a laser, a lens and several adjustable stands for precise positioning, is expensive. In addition, the range of the measurable pressure is limited by the mechanical strength of the membrane material and the channel must be customized for use with this technique. Even microstrain gauges membranes can be employed to sense the pressure induced at the tap from the microchannel. The defor- mation of the membrane results in the variation of the electrical resistance of the material making up the membrane, therefore information on pressure can be transformed into an electrical sig- nal, which is usually magnified for better accuracy via a Wheat- stone bridge on the membrane, as in the work by Zohar et al. [17] and Bavière and Ayela [8] . After careful calibration, a correla- tion between pressure and voltage in the circuit can be given. This pressure sensor can be used to test local pressure along the micro- channel and has very low temperature sensitivity (±0.011% C 1 ), as reported by Bavière and Ayela [8] , who found no effects which might actually be the result of inaccurate measurements at the small scale. The constant coefficient which links pressure and elec- trical voltage varies from one membrane to another, and each strain gauge needs to be calibrated over a certain pressure range before measurement. Even in this case, the microchannel and the membranes must be specifically designed in order to use this tech- nique. For liquids through very small microchannel, Celata et al. [16] demonstrated that the measurement of the differential pres- sure along the channel can be linked to the fluid temperature rise between the inlet and the outlet of the channel due to the viscous dissipation. This effect is more evident for fluids having a low spe- cific heat and a large viscosity (i.e. iso-propanol). For gases, the temperature rise due to the viscous dissipation is compensated by the cooling due to the gas acceleration along the channel. For this reason, this effect is not useful for the determination of the dif- ferential pressure along a microchannel for gas flows.

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3.3. Measurement of temperature

The measurement of the bulk fluid temperature along a micro- channel cannot be made directly without large disturbance on the fluid flow. Suspended micro temperature sensors within micro- channels have been proposed in the past, as reported in an inter- esting review paper of Nguyen [34] . The first prototypes of suspended sensors made by Petersen et al. [35] and Lammerink et al. [36] demonstrated that full integration between this kind of temperature sensors and the microchannels was possible but their impact on fluid flow was not negligible at all. Nowadays microfabrication offers a large variety of devices to achieve local temperature measurements. Among the existing devices it is pos- sible to distinguish three groups: (i) thin film resistance tempera- ture detector ( l RTD), (ii) thin film thermocouple ( l TFTC) and (iii) semiconducting sensors (SC). In microchannels, to avoid disturbances of the fluid flow, in many cases only the wall temperature along the channel is deter- mined by means of integrated temperature sensors and the direct determination of the fluid bulk temperature can only be obtained at the inlet and outlet sections of the channel by using specific ple- nums. Sometimes, the thermal inertia of the temperature sensors placed at the walls of the microchannel is larger or comparable to that of the channel walls. In this case, the presence of the sen- sors can modify the wall temperature distribution. The problem is how to calculate the fluid temperature when the wall tempera- ture is known. In adiabatic flows this is simple if one can assume that thermal equilibrium exists between the walls and the fluid. This is not the case when the flow is heated. In the following a summary of the most interesting temperature microsensors developed in the last years is given with the indica- tion of the main advantages and drawbacks of each one. In Fig. 3 a schematic representation of these three different kind of temper- ature microsensors together with their characteristic calibration curves is given in order to highlight the main differences among l RTD, l TFTC and SC due to their different working principle. The first kind of temperature microsensors which can be inte- grated in microchannels are the Microresistance Temperature Detectors ( l RTDs). This type of temperature sensors is widely used

in microtechnology devices firstly because it is easy to make and secondly because it generally is characterized by a linear response. The functioning principle of a l RTD is the same as that of the clas- sical RTD in which the temperature-dependent electrical resistivity of a material is used in order to estimate the temperature ( Fig. 3 a). Among the several materials used for the realization of the l RTDs the most common are Pt, poly-Si, Al, Ni, W, Au or yet Ag [37–43]. The fabrication of the sensitive metal elements for l RTDs is well controlled by using sputtering or evaporation CVD pro- cesses. Platinum is commonly used for different applications in microtechnology for its catalytic property in combination with some gases or, at other times, for its inert properties in combina- tion with a large variety of fluids. However, platinum films can present some drawbacks: the first one is the need of an adhesion layer on almost all the substrates. In many cases the deposition of the platinum film generates an alloy with different thermal properties than the pure material and the characteristic curve of the electrical resistance vs temperature of the l RTD can change completely. Moreover, platinum films can be damaged if the tem- perature becomes larger than 550 C. Other drawbacks of the plat- inum films is their cost and their CMOS incompatibility [39] . For these reasons, some microfluidics technical applications of l RTD use polysilicon (poly-Si) [40] . Thin Film Thermocouples ( l TFTCs) are active elements which use the Seebeck effect to measure the temperature of a two-metal junction ( Fig. 3 b). Microfabrication of l TFTCs can be more or less complex depending on the existing material constraints for the specific microdevice needed. Zhang et al. [44] proposed a chromel thin film thermocouple embedded on a Ni substrate and demon- strated that their behavior is similar to the standard K-Type ther- mocouples. In fact, the embedded TFTCs of Zhang et al. [44] on Ni substrates have shown that their thermal sensitivity is not af- fected by the junction size between 25 l m and 80 l m. This ther- mal sensitivity has been precisely measured for a chromel film of 100 nm and a junction of (60 l m 60 l m) up to 900 C; the See- beck coefficient of this l TFTCs was 40.6 l V C 1 in agreement with the standard value of this coefficient for the classical K-Type ther- mocouples. The results obtained by Zhang et al. [44] were con- firmed by Choi and Li [45] who showed as a K- l TFTCs with a

(a) µRTD (b) µTFTC (c) SC Tmeas PN Junction Metal b Typical sensors Metal a
(a) µRTD
(b) µTFTC
(c) SC
Tmeas
PN Junction
Metal b
Typical sensors
Metal a
layout
Metal a
I
R
V
dV
Tref
I
Characteristic
Curve
T: Temperature
R: Resistance
V: Voltage
I: Current
V

Fig. 3. Schematic representation of the most common temperature micro-sensors with the indication of their characteristic curve; (a) thin film resistance t emperature detector ( l RTD); (b) thin film thermocouple ( l TFTC) and (c) semiconducting sensors (SC).

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junction of 25 l m 25 l m and a film thickness of 150 nm were able to provide a good sensitivity (40.4 l V C 1 ) up to 800 C and a fast response time (28 ns). However, the authors underline that a microfabrication trouble for this kind of microcomponents is linked to the surface quality (especially roughness) of the thin film layers used in these l TFTCs which can strongly influence the stability of these temperature microsensors. With the aim to take advantage of the CMOS compatibility pro- cess (integration, low cost) an alternative for the temperature mic- rosensors are the Semiconducting sensors (SCs) which use Polysilicon active elements ( Fig. 3 c). Bianchi et al. [46] present a state of the art of integrated smart temperature SCs sensors like MOS transistors, bipolar transistors and diodes. The use of MOS transistors as temperature sensors needs the use of the transistors in weak inversion in order to obtain a linear relation between tem- perature and their electrical parameters even if some limitations due to leakage currents at high temperature can exist [47,48] . Bipolar transistors and diodes present directly a junction voltage proportional to the absolute temperature. Generally, at room tem- perature, silicon p n junctions have a forward voltage drop of 0.7 V, and this voltage decrease by 2 mV for every degree of in- crease [49] . Typical temperature range of these sensors could be 55 to 175 C with a typical accuracy between ±0.1 and ±3 C [46] . Transistors with CMOS or bipolar IC technologies enable the realization of all the needed circuits in order to integrate directly the temperature compensation or calibration functions to the sen- sors. Filanovsky and Lee [48] realized two temperature sensors with signal-conditioning amplifiers to extract directly from a MOS transistor the linear temperature dependence of V T . Using BiCMOS technology, the first solution chosen was a threshold extractor circuit which gave a linear temperature characteristic be- tween 40 and 150 C but showed some disparities linked to fab- rication. The second one was a resistive Wheatstone bridge which gave a non-linear temperature response but with a good repeat- ability in the same range of temperature. Finally, planar diffused silicon diodes seem to be a simpler way to measure temperature when employing SCs sensors. Guha et al. [39] showed a high temperature gas sensor consisting of an embedded diode able to give a linear response up to 260 C accord- ing to the calibration with a sensitivity of 1.2 ± 0.005 mV/ C. In a pH sensitive ISFET chip, Chin et al. [50] have integrated a p-n diode which presented good linearity with a sensitivity of 1.51 mV/ C (in the range 0–50 C) and which also have been used with a spe- cific compensation circuit dedicated to the application. Even if, up to now, CMOS technologies are not so frequently used in Microfluidics applications, in the future SC sensors could have a wide range of applications in this field due to their flexibil- ity and to their high scale of integration that enables to expand the single sensor to an array of sensors. For example, Han and Kim [51]

have developed a 32 32 diodes (1024 diodes) array for measur- ing the temperature distribution on a small surface (8 mm 8 mm). This kind of sensor reduce the 2048 interconnections pads needed for 32x32 RTD or TFTC sensor array to only 64 interconnec- tions pads that involve a tiny chip and the simplest design. In Han and Kim’s work [49] , calibration experiments evidenced the linear output temperature signal of this array in the range 0–100 C with an accuracy of ± 0.5 C. In compensation of this flexibility at the fabrication level, array sensors need a multiplexer to read the measurements. In Table 1 a selected list of microsensors for temperature mea- surement is shown with the indication of the main technical char- acteristics (when available) of these sensors (thermal sensitivity, accuracy and range of application). In many of the published scientifical works temperature mea- surements are still obtained using traditional sensors like thermo- couples or Platinum RTD. Bavière et al. [52] measured the temperature along a rectangular channel by arranging four ther- mocouples uniformly in line with the channel axis. The thermo- couples were planted in blind holes 500 l m from the channel wall surface. To predict the temperature of the wall surface a cor- relation was presented based on calibration experiments and the temperature measured by thermocouples a constant distance away from the wall surface. This approach provides an indirect way to obtain the local wall surface temperature along the whole channel, which makes it possible to analyze the local heat transfer charac- teristics. However, the existence of these holes near the channel walls may alter the temperature distribution inside because they introduce a heterogeneous thermal conductivity. Demsis et al. [21] investigated the convective heat transfer coefficient in a coun- ter flow, tube-in-tube heat exchanger. Two ports perpendicular to the axis of the microchannel were machined and connected to the inlet section of the inner tube 35 mm before the heated section, one for the measurement of temperature and the other for pres- sure. The measurement of the outlet pressure and temperature was proposed in the same way through two ports 35 mm after the heated section. The risk of this technique is linked to the erro- neous evaluation of the fluid outlet temperature: if the part of tube between the end of the heated section and the outlet side port is not thermally insulated with care, the fluid temperature decreases along this stretch and the temperature recorded at the exit side port differs from the fluid temperature at the end of the heating section. Also, the side ports may disturb the main stream inside the tube. This kind of side ports can be readily applied to non- circular microchannels or circular microtubes with relatively large inner diameter; however, if the inner diameter is very small, below 0.3 mm, it becomes difficult to manufacture them. Besides thermocouples or diode arrays which can provide single or multipoint measurement of temperature, some specific optical techniques have been used for the measurement of a

Table 1 Characteristics of the micro-sensors for temperature measurement.

 

Authors

 

Material

Thermal sensitivity

Accuracy

Temperature range

RTDs

Schöler et al. [38] Wu et al. [42]

Platinum

20–80 C 45–105 C

Silver paint

Wu

et

al.

[40]

Silicon

0.05 C

Choi et al. [43]

Gold

TFTCs

Zhang et

al. [44]

Chromel

40.6 l V C 1 40.4 l V C 1

 

20–900 C 20–800 C

Choi and

Li [45]

Chromel

Kim and Kim [61]

Chromel

SCs

Guha et al. [39] Bianchi et al. [46] Chin et al. [50] Han and Kim [51]

Silicon

1.20 mV C 1

0.005 mV C 1 ±0.1–3 C

20–260 C 55–175 C 10–50 C 0–100 C

Silicon

Silicon

1.51 mV C 1

Silicon

±0.5 C

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two-dimensional temperature field on a solid surface at micromet- ric scales, such as liquid crystal thermography (Muwanga and Hassan [53] ), infrared thermography (Mosyak et al. [54] ) and temperature sensitive paints (Liu and Sullivan [28] ). The most important constrain of these optical techniques is that these methods can be successfully applied only in the cases in which the external surface of the test section is not thermally insulated.

3.4. Measurement of local velocity data

There is a crucial need of local experimental gas velocity data through microdevices but all the velocimetry techniques proposed for liquid flows in microchannels present strong limitations if ap- plied to the analysis of gas flows through microchannels. For the determination of the local velocity of a gas in a microchannel three optical velocimetry techniques have been proposed in the open lit- erature up to now: (i) the Laser-Doppler Anemometry (LDA); (ii) the microParticle Image Velocimetry ( l PIV) and (iii) the Molecu- lar-Tagging Velocimetry (MTV). The Laser-Doppler Anemometry (LDA) has been preliminary used by Ladewig et al. (cited in [55] ) in order to measure gas-phase data in an operational U-shaped mini-fuel cell with channels of 2 mm 2 mm rectangular cross-section. The flow was seeded with water droplets, but the velocity data obtained were not yet com- plete enough to fully characterize the flow inside the minichannels. Furthermore, LDA is a point-measurement technique; in order to obtain a more representative visualization of the whole velocity field in a microdevice a field-measurement technique as the micro- Particle Image Velocimetry can be more useful. For the problems related to the systematic use of the LDA technique for the recon- struction of the velocity profiles in microchannels the LDA tech- nique can be considered useless in measuring the velocity within channels having an inner hydraulic diameter below 1 mm. On the contrary, for the investigation of the velocity field in micro- channels having inner diameters below 1 mm the microParticle Image Velocimetry is nowadays a consolidated technique but only for liquid flows. An interesting and complete review of the progress of this technique in the recent years is due to Lindken et al. [4] . Up to now, few works have described the application of this technique for the analysis of gas flows through microchannels. One reference paper in this field is due to Yoon et al. [55] ; in this paper the micro PIV technique has been used to directly measure gas-phase velocities in situ in an operational fuel cell with chan- nels having characteristic dimensions of 1–2 mm. For PIV measure- ments, in macro-scale gas flows, the gas is often seeded with olive oil particles generated by an atomizer. To this aim, high pressures and a high flow rates are needed for the generation of the oil seed particles. On the contrary for microscale gas flow applications, as microfuel cell, the gas flow rate is relatively small (Reynolds num- bers of the order of hundreds to a few thousands) and this can cre- ate problems in the generation of appropriate tracer particles. Since PIV is based on imaging of particulates introduced into the flow, the accuracy of the gas-phase flow velocity measurement is strongly dependent on the ability of the tracer particles to follow the stream. In the work of Yoon et al. [55] , water droplets have been used as seed particles for measuring the flow in a straight minichannel. This choice was motivated for fuel cells with the opportunity to introduce the water particles in the gas flow using the humidifier section without contaminating the system. The re- sults of Yoon et al. have demonstrated that certain limitations are encountered when trying to use such tracer in flows with sig- nificant decelerations, such as in a 180 switchback turn. In partic- ular, the experimental results of Yoon et al. have evidenced that tracer particles smaller than 1 l m are required to accurately follow the flow in such regions. This aspect is one of the most important constraints in the application of the l PIV technique for the analysis

of gas flows in microchannels. Sugii and Okamoto [56] have ap- plied the PIV technique in order to investigate the velocity distri- bution in a fuel cell with 1 mm 0.5 mm rectangular polymer microchannels. Even in this paper, it is stressed how the main problem for the application of this technique to the investigation of micro gas flow is the generation of proper seeding. In this work fluorescent oil particles having a diameter between 0.5 and 2 l m were used as tracer particles in a nitrogen flow for low Reynolds numbers between 26 and 130. Molecular-Tagging Velocimetry (MTV) is a whole-field optical technique that relies on molecules that can be turned into long life- time tracers upon excitation by photons of appropriate wavelength [57] . These molecules can be either premixed or naturally present in the flowing medium (unseeded applications). Typically, a pulsed laser is used to ‘‘tag’’ the regions of interest, and those tagged re- gions are interrogated at two successive times within the lifetime of the tracer. Lagrangian displacement vector provides the estimate of the velocity vectors. This technique can be thought of as essentially a molecular counterpart of Particle Image Velocimetry (PIV), and it can offer advantages compared to particle-based techniques where the use of seed particles is difficult, or may lead to complications as for gas flows in microdevices. However, this technique has been only used for the analysis of liquid flows in microchannels [58,59]. On the contrary, up to now the application of this technique for the analysis of gas flows in microchannels is not completely consolidated. A specific European research project (GASMEMS project) devoted to the development of velocimetry techniques for gas flows in microchannels has been launched in order, among others, to demonstrate the possibility of using l PIV and MTV for the analysis of the gas flows in channels having inner dimensions below 1 mm [60]. It is possible to conclude that for the measurement of the local velocity data in microchannels much work is still needed in order to adapt the velocimetry techniques proposed for liquid flows through microdevices to the analysis of gas flows; this field is of strategic importance especially for the optimization of microfluidic components as, for example, the micro- and mini-fuel cells.

3.5. Measurement of flow rate

The flow rate through a microchannel can be measured directly by means of appropriate instruments (mass or volumetric flow me- ters) or in an indirect way by checking the value taken by other measurable quantities, like pressure, forces, weight, volume, tem- perature or a combination thereof. As a rule of thumb, it is possible to use a commercial mass or volumetric flow meter for gas flows only if the gas mass flow rate through a microchannel is larger than 10 8 kg/s (0.1 Nml/min). On the contrary, for very low mass flow rates (<10 8 kg/s) indirect methods can be considered more reli- able in order to determine the flow rate with low values of uncertainty. The commercial flow meters for gas flows can be divided in two groups: the volumetric flow meters and the mass flow meters. The volumetric flow meters give an indication of the flow rate regard- less of the fluid tested; the mass flow meters, on the contrary, can be used only with the fluid for which they have been calibrated. The sensors of the commercial gas flow meters can be divided in non-thermal flow sensors and thermal flow sensors. The first kind is classified according to the mechanical working principle by means of which the flow rate can be measured indirectly:

(1) by the drag force (i.e. using silicon cantilevers); (2) by pressure measurements (i.e. using capacitive and/or piezoresistive pressure sensors); (3) by using the Coriolis principle.

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The main disadvantage of the non-thermal flow sensors is linked to the dependence of the force, pressure difference and Cori- olis force on the density of the working fluid. Since the gas density depends on the gas temperature, a temperature compensation is a compelling need for this kind of sensors. As indicated by Nguyen [34] , the thermal flow sensors em- ployed in the commercial flow meters can be classified as follows:

(1) thermal mass flow sensors which measure the effect of the flowing fluid on a hot body (micro hot-wire and micro hot- film sensors); (2) thermal mass flow sensors which measure the asymmetry of temperature profile around a micro heater which is modu- lated by the fluid flow (calorimetric sensors); (3) thermal mass flow sensors which measure the delay of a heat pulse over a known distance (time-of-flight sensors).

The most popular sensors among the commercial flow meters are the calorimetric sensors: this kind of flow meters are able to predict the mass flow rate through the sensor by means of the fol- lowing balance equation:

_

m ¼

Q th

c p ð T b; out T b;in Þ

ð15Þ

which puts in evidence how the gas mass flow rate can be deter- mined by means of two local measures of temperature (T b,out and T b,in ) and the knowledge of the heat power (Q th ) transferred to the gas by the heater. By using microfabrication, this kind of thermal mass flow sensor can be directly integrated into a microchannel. Schöler et al. [38] have shown as two classic Pt RTDs and a microheater made on a glass substrate can be directly integrated on a SU-8 epoxy resist microchannel (50 l m 15 l m 8000 l m). As demonstrated by Kim and Kim [61] by using a capacitive mass flow sensor using two K-Type TFTC (150 l m 150 l m) associated to a PDMS micro- channel (800 l m 800 l m 4 cm), the accuracy of this kind of mass flow meters can be strongly influenced by the position and the thermal insulation of the microsensor. When the gas mass flow rates that one wants to measure through microchannels are very low (<10 8 kg/s) the use of com- mercial devices becomes unsuitable because of the high level of uncertainty afflicting the measurements. In addition, accurate measurements of mass flow rate in microchannels are challenging for gas flows, which have a density very sensitive to the room pres- sure and temperature fluctuations. Low gas flow rates can be determined using the general expres- sion of the mass flow rate as the change of mass over time:

_

m

¼ dm

dt

ð16Þ

If the gas can be considered as an ideal gas, the mass flow rate can always be expressed as follows:

m ¼ p

_

dV

V

dp pV dT

RT 2

dt

RT dt þ RT dt

ð17Þ

It can be noted from Eq. (17) that if two of the three variables (vol- ume, pressure and temperature of the gas) are kept constant while the third one is monitored during the experiment, the mass flow rate of the gas can be determined. This provides the basic insights into gas mass flow rate measurements. In practice, it is impossible to keep two of the three variables strictly unchanged, so great ef- forts are made to minimize the fluctuations of the nominally un- changed variables to determine the mass flow rate as accurately as possible. These fluctuations are usually the main source of errors in low mass flow rate measurements for gas microflows.

Based on Eq. (17) several techniques have been proposed for the determination of the mass flow rate below 10 8 kg/s. In the droplet tracking technique the gas volumetric flow rate is measured by introducing the outflow gas into a pipette, in which the gas pushes a droplet forward. By recording the position of the droplet versus time under the assumption of constant pressure and temperature, the velocity of the droplet can be determined and knowing the diameter of the pipette the mass flow rate of gas can be calculated. In this case, Eq. (17) can be re-written as:

m ¼ p

_

dV

¼ p

RT

2

pip

pd

Dl

4

Dt

RT dt

ð 18Þ

where d pip is the diameter of the pipette and D l is the distance the droplet moves during a certain time interval (D t ). This technique does not require expensive meters and can be performed by using multiple microchannels. The lowest mass flow rate that can be mea- sured with this technique depends on the specific setups and on the maximum number of microchannels tested in parallel. As rule of thumb, the lowest value of the mass flow rate that can be measured by using the droplet tracking technique is of the order of 10 10 kg/s. However, it is possible to obtain lower mass flow rates if the mea- surement is made using hundreds of identical microchannels in parallel in a single test section. This is the case of Shih et al. [62] who measured the mass flow rate of helium through microchannels in the order of 10 12 kg/s, which is the same order measured by Ewart et al. [63] with nitrogen. Colin et al. [64] obtained the mass flow rate down to the order of 10 13 kg/s for helium, while Celata et al. [16] reached flow rates of the order of 10 8 kg/s for the same type of gas with this technique. However, it is technically difficult to maintain a constant moving speed for the droplet. Another problem is the accurate measurement of the pipette inner diameter, which weighs most in determining the mass flow rate, as shown in Eq. (18), and, in the case of parallel channels, their dimensions may vary significantly and thus the value obtained is only an average. If gas flow is accumulated in a tank for a certain time interval, there will be a pressure rise in the tank during the flow. If the pres- sure in the tank is under reasonable control and not very high, the expansion of the tank or the increase in its volume can be safely neglected. In this case Eq. (17) becomes:

_

m

¼ V

dp pV dT

RT dt

RT 2

dt

ð

19Þ

If the second term in the right-hand side of Eq. (19) is very small compared to the first one (i.e. <1%) it can also be dropped and by careful measurement and recording of pressure rise inside the tank versus time the mass flow rate can be determined. This is usually referred to as constant volume technique. Based on this principle, Ewart et al. [65] built an experimental setup in which the outlet of the microchannel is connected to a large tank. By recording the pressure versus time inside the tank, the mass flow rate can be determined. The lowest mass flow rate measured with this tech- nique was of the order of 10 13 kg/s. The volume of the tank should be carefully chosen so that the pressure change is detectable by a pressure sensor for mass flow rate calculation and at the same time negligible to remain a nearly constant outlet pressure. Great care should also be paid to the temperature fluctuation of the gas as it is compressed into the tank, so that the temperature change can be neglected, which greatly simplifies the calculation of the mass flow rate. Arkilic et al. [66] used a two-tank, modified constant-volume accumulation technique to measure the mass flow rate of gas, as the single-tank procedure would not ensure the thermal stability needed for their experiment. In this case, Eq. (19) is not sufficient to calculate the mass flow rate, as both upstream and downstream pressures vary during the experiment. Instead, the pressure

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859

difference between the two tanks (both located downstream of the microchannel) is measured. During the test one tank is used to accumulate the gas flowing out of the microchannel and the other one remains in steady state which provides a pressure reference. The pressure difference between the two tanks is measured instead of the absolute pressure for the determination of mass flow rate, as given by:

m ¼ V

_

RT

dð DpÞ DpV dT

dt

RT 2

dt ð

20Þ

where Dp is the pressure difference between the reference tank and the flow tank. As the two tanks are connected before the flow starts, this quantity is 0 at the beginning. Due to the relatively small mass flow rate of gas through the microchannels, when the flow finishes the pressure difference can be very small, quite several orders of magnitude smaller than the absolute pressure in Eq. (19). Therefore, the sensitivity of mass flow rate to the tank temperature fluctuation is reduced by several orders, and the tank for gas accumulation can be reasonably regarded as isothermal during the experiment. In addition, this technique requires that the two tanks have identical temperature and undergo the same thermal fluctuations, which can be realized by a good design, arrangement and thermal insula- tion of the tanks. For this reason, in the work by Pitakarnnop et al. [67] the whole setup was thermally regulated with Peltier modules to maintain a constant temperature. This method provided data for mass flow rates of an order of 10 11 kg/s and a sensitivity as low as 7 10 15 kg/s (Arkilic et al. [68] ) was reported; Pitakarnnop et al. [67] developed a new setup for gas microflows in which the constant volume method for mass flow rate measurement was implied to both the upstream and downstream flow. This offers a double-check providing the possi- bility to compare the measured results for the same flow. Their measured values of mass flow rates can be as small as to 7.1 10 14 kg/s.

To achieve a constant mass flow rate with this technique, the pressure difference between the two tanks should increase linearly with time during the experiment. As the outlet of the microchannel is directly connected to the tank, the outlet pressure keeps chang- ing and is uncontrolled. The inlet pressure should be very carefully adjusted with the passage of time to achieve a linear increase of pressure difference between the two tanks. This is very difficult to achieve in practice. Thus, the process of gas flow in the micro-

channel becomes time-dependent with this method. In order to complete this review, it is possible to highlight that the most sensitive technique for the gas detection and for the mea- surement of very low mass flow rates in leaks is based on mass spectrometry and it has been presented by Tison in 1993 [69] . Tison developed a specific setup to measure gaseous capillary leak rates ranging from 10 6 mol/s to 10 14 mol/s. A series of complex operation steps are involved in the test so that the final determina- tion of flow rate is dependent on the ratio of measured quantities instead of their absolute values, which reduces the sensitivity of possible fluctuations (temperature, pressure and so on) and ex- pands the measurement to very low range (pressures between 10 4 and 10 8 Pa). In this work, however, the focus is on the deter- mination of leak rates of a specific gas, helium, which, at such pres- sures, is actually part of a mixture, so that it is the partial pressure which has to be determined, and either ion gauges or mass spec- trometers are used to this aim. It can be highlighted that Tison’s technique is time-consuming (6–8 h for a single test) with respect the other techniques reviewed and its use in microfluidics can be considered useful only for specific tests in which the gas mass flow rates are very low (<10 15 kg/s). To summarize the main observations made in section for each technique, Table 2 shows the most important methods proposed for the fluid-dynamic investigation in microchannels. For each technique, the typical ranges of values for which they have been applied together with the typical values of uncertainty

Table 2 Summary of the experimental techniques proposed for the analysis of the gas flows in microfluidic applications.

Physical

Technique

Range

Typical uncertainty

References

quantity

Mass flow

Flow meters

50000–0.05 Nml/min

0.6%, 1%, 2%

Morini et al. [18] , Celata et al. [16] , Tang et al. [15] Celata et al. [16] Shih et al. [62] , Ewart et al. [63] , Colin et al. [64] Ewart et al. [65] , Pitakarnnop et al.

rate

 

Droplet tracking

10 8 kg/s 10 10 –10 13 kg/s (hundreds of parallel microchannels) 10 13 kg/s

9.64% (calculated)

 

3–4%

 

Single tank constant volume

4.5%

 

[67]

 

Two-tank constant volume 10 11 kg/s

Arkilic et al. [66,68] Tison [69]

Mass spectrometry method

4 10 17 kg/s–4 10 8 kg/s

1–8%

Diameter

Accumulation of heavy liquid SEM

150 l m 0.5–40 l m 133–730 l m 10–300 l m 30–254 l m

0.13%

Asako et al. [7] Zohar et al. [17] Morini et al. [18] Tang et al. [15] Celata et al. [16]

1.25–2%

 

2%

0.3–2.98%

2.48–3.67%

Temperature Thermocouples (directly, at inlet and outlet) Thermocouples (indirectly, along microchannel) Thermocouples (directly, after inlet and before outlet)

0–200 C

0.17%, 0.25%

Tang et al. [15], Morini et al. [18]

Systematic error reduced by around 0.8 K

Baviere et al. [52]

Inlet and outlet effects minimized

Demsis et al. [21]

Infrared thermography 50–130 C

Sensitivity: 0.1 C Mosyak et al. [54]

 

Liquid crystal thermography 43–50 C

1.1–1.5 C

Muwanga et al. [53]

Temperature sensitive paint

10–100 C

Sensitivity. 1% C 1 Liu et al. [28]

Pressure

Pressure transducer

0–1.5 MPa

0.25%, 0.5%

Tang et al. [15], Morini et al. [18] ,

Tube cutting Pressure-Sensitive Paints Pressure-sensitive molecular film

From near vacuum to 2 atm. 10 2 –10 4 Pa

Minor losses minimized 1 mbar –

Asako et al. [7] Asako et al. [7] , Celata et al. [16] Huang et al. [27] , Liu et al. [28] Matsuda et al. [32,33]

Microstrain gauge

membrane

0.1–0.4 MPa

1%

Zohar et al. [17] , Baviere et al. [8]

Optical lever

0–1.4 MPa

2.4–13.3%

Kohl et al. [25]

860

G.L. Morini et al. / Experimental Thermal and Fluid Science 35 (2011) 849–865

are shown. The data in Table 2 may be employed during the design of a new test rig in order to select the best measurement tech- niques with the goal to minimize the global uncertainty on the de- rived quantities, as shown in the next section.

4. Uncertainty analysis

Eq. (13) highlights that the friction factor is a function of

many parameters. Eqs. (4) and (5) link the friction factor and the measurable quantities. The friction factor is a general function

f

¼ f ð x 1 ; x 2 ;

;

x n Þ in which

the single measurable variable x i is

characterized by a known absolute uncertainty d x i which corre- sponds to the relative uncertainty d x i . Based on the theory of uncertainty propagation, the absolute uncertainty on the friction factor is given by [70] :

x

i

df ¼

s

ffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi

X

@ x j covð x i ; x j Þ

f

@

@

x i

2

n

i¼1

ð dx i Þ 2 þ 2 X

n

i¼1 X j¼iþ1

n

@ f @ f

@ x i

ð21Þ

where cov ð x i ; x j Þ is the covariance associated with x i and x j . If x i and x j are independent, their covariance is 0; if the two variables are correlated, their covariance will not be 0. However, in experiment the singly measured variables are independent of each other, which greatly reduces the complexity of calculation. Even with such sim- plification, the measurable variables might be correlated by the instrumentation used in the experimental setup (i.e. the use of the same pressure sensor or temperature sensor and so on) and/ or by the room conditions (via data acquisition system). However, this kind of correlation is relatively weak (i.e. Agilent 34420A digital multimeter for data acquisition presents a slight sensitivity of the magnitude of 0.0008% with regard to room temperature) and can be either negative or positive, which tends to balance out the total contribution to the overall uncertainty of the function f . For this rea- son, in the following discussion the measurable variables will be considered independent to each to other, and Eq. (21) can be simply expressed as follows for the total relative uncertainty of f :

df

f ¼

s

ffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi

2

@ f

x

1

2

d

x 1

2

þ

2

f

@

x

2

dx

2

@ x 2 f

x

2

2

þ

@ f

x

n

2

dx

n

@ x 1 f

x

1

@ x n f

x

n

ð22Þ

For flow in microtubes, by considering all the directly measurable quantities (inner diameter, channel length, temperature, pressure drop, outlet pressure and mass flow rate) in the determination of the value of friction factor, the relative uncertainty of friction factor is given by:

df

f ¼

s

ffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi

2

k

2

1

d

D

h

D

h

2 þ k 2

2

d

L

L

2

2

3

d

T

T

2

þ k

2

4

dD p

p

2 þ k 2

5

dp out

p

out

2 þ k 2

6

d

_

m

_

m

þ k

ð

23 Þ

where the sensitivity coefficients, k 1 , k 2 ,

uncertainty of each measurable parameter contributes quantita- tively to the uncertainty of friction factor, are listed in Table 3 for both incompressible and compressible flow. The analytical expres- sion of these coefficients, reported in Table 3 , can be calculated by Eqs. (22) and (23) for which:

, k 6 , which show how the

k i ¼ @ f

x

i

@ x i f

ð

24Þ

and depends on the flow conditions in the experimental test as well on the measurement strategies adopted (i.e. the use of two absolute pressure sensors at the inlet and at the outlet of the microchannel

or the use of one differential pressure sensor with one absolute

pressure sensor and so on). Eq. (23) highlights that the relative uncertainty of the friction factor is more sensitive to the measured variables which are asso-

ciated to larger sensitivity coefficients and the largest one domi- nates the total relative uncertainty. Specifically, the accuracy of microchannel diameter measurement has the greatest weight in the determination of the friction factor uncertainty, followed by mass flow rate and pressure (for compressible flows) measure- ment, while the accuracy of length and temperature measurement is comparatively less important. This analysis suggests that for accurate calculations of the friction factor the measurement of the channel diameter is of crucial importance: even a small error may induce a large error in the calculated quantity. When compressibility effects become important and for very low mass flow rates (<10 8 kg/s), uncertainty in flow rate measure- ments becomes large; as explained in the previous section, in these cases the flow rate is not directly measured but it is calculated with Eqs. (17)–(20) as a function of temperature, pressure and volume of the system: this increases the influence of such quantities mea- surement on the total uncertainty of the friction factor. It can also be noted from Table 3 that, for incompressible flows and compressible flows with low pressure drop, the uncertainty of friction factor can be directly calculated from the error of each measurement, without knowing the absolute values of the mea- sured parameters. On the contrary, for compressible flows with comparatively large pressure drops (which is usually the case in microchannels), the friction factor uncertainty depends on the absolute values of the following experimental parameters:

a ¼ Dp ;

p

out

b ¼ 2D h

fL

ð

25Þ

where D p is the pressure drop along the whole microchannel, p out is the outlet pressure, f is the friction factor and L in the total length of

the microchannel.

For compressible flows different strategies can be used in order

to determine the friction factor depending on the type of pressure

sensors involved in the measurement.

Table 3 Sensitivity coefficients of operative parameters in the calculation of friction factor.

Sensitivity

In-compressible

Compressible flow (negligible a a )

 

Compressible flow (non-negligible a a ) Strategy #1

Compressible flow (inlet and outlet pressure measured) Strategy #2

coefficients

flow

k 1 (diameter) k 2 (length) k 3 (temperature) k 4 (pressure drop)

5

5

5 + 4 b ln(1 + a )

 

5+4 b ln(1 + a )

 

1

1

1

1

0

1

1 + b ln(1 + a )

 

1+ b

ln(1 + a )

1

1

1 þ

a

2 þ a b

1 þ a þ b 1 þ

a

 

2

a

þ a

ln ð 1 þ a Þ

2 þ a 2 þ 2 a b þ 2 b 1 þ

of D p )

2

1

a 2 þ 2 a

ln ð 1 þ a Þ (for p in instead

k 5 (outlet pressure) k 6 (mass flow rate)

0

1

 

1

þ

 

h

 

2

þ

 

i

2

a 2 þ 2 a ½ 1 þ b ln ð 1 þ a Þ b

1

a

þ b

2

ln ð 1 þ a Þ þ

1

a

þ a

 

2

a

 

2

2

2+2 b ln (1 + a )

 

2+2 b ln (1 + a )

 

a a = D p / p out ; b = 2 D h /( fL ).

G.L. Morini et al. / Experimental Thermal and Fluid Science 35 (2011) 849–865

861

For example, one can measure:

the total pressure drop due to the microtube by using a differ- ential pressure sensor together with the determination of the absolute value of the outlet pressure (indicated as Strategy #1 in Table 3 ) or the absolute value of the pressure at the inlet and at the outlet of the microtube (indicated as Strategy #2 in Table 3 ).

Of course, other combinations of pressure sensors are possible. Each different strategy causes some difference in the expression of friction factor and thus changes the sensitivity coefficients of each measurement (Eq. (24)), as shown in Table 3 . In order to give some numerical examples, the influence of sensitivity coefficients of the six measurable quantities (inner diam- eter, microtube length, temperature, total pressure drop, outlet pressure, mass flow rate) on the uncertainty of the friction factor is investigated quantitatively with a set of error-free data generated from gas flow in a 100 l m microtube with a length of 30 mm. The flow is assumed to be compressible, isothermal and in the laminar regime, and the gas is discharged to the atmosphere. The typical value of uncertainty for each measurement can be chosen by using the data in Table 2 ; we have assumed an uncertainty of ±2% for inner diameter measurement, ±0.3% for length measurement, ±0.25% for temperature measurement, ±0.5% for pressure measurement and ±2% for mass flow rate measurement. Fig. 4 shows the influence of each measurement on the uncer- tainty of friction factor. It can be seen that the accuracy of friction factor is most sensitive to the measurement of inner diameter, which results in an uncertainty of more than 10% on the friction factor. This contribution grows gradually with the increase of Reynolds number. The importance of mass flow rate measurement takes the second place and a 2% deviation results in an error of 4–5.5% in friction factor. Compared with diameter and mass flow rate, the influence of other quantities (pressure drop, outlet pres- sure, length and temperature) on the accuracy of friction factor is small. In practice, the uncertainty evaluation is more complicated than the previous simulation, which based on assumption of constant values for the relative uncertainty of each measured quantity. Dur- ing a specific test round for isothermal flow, four out of the six quantities to be measured (inner diameter, microtube length, tem- perature, total pressure drop, outlet pressure, mass flow rate) al- most remain constant when the imposed Reynolds number is changed, namely inner diameter, length, temperature and outlet

pressure (here it is assumed that the gas is discharged directly into the atmosphere). On the other hand the value of the pressure drop and the mass flow rate increase greatly in microchannels when the Reynolds number increases. This causes a change in the relative uncertainty of these two quantities, which tends to be larger when the pressure drop and mass flow rates are farther from the full scale (FS) value of the instrument. To further explore this effect, we assume the relative uncer- tainty for pressure drop and mass flow rate is ±0.5% of the full scale (FS) reached when the Reynolds number is 2300. Fig. 5 shows the single contribution of the uncertainty of these two parameters to the uncertainty on friction factor. The total fric- tion factor uncertainty is calculated based on the changing uncer- tainty of pressure drop and mass flow rate, as well as the constant relative uncertainty of inner diameter (±2%), length (±0.3%), outlet pressure (±0.5%) and temperature (±0.25%). It can be seen that for low Reynolds number (<500), or more generally when the mea- sured values are far from the full scale, the uncertainty of friction factor becomes very large and sometimes this leads to unreason- able results in Microfluidics experiments. In order to control the uncertainty during experimental tests over a wide range of Reynolds numbers it becomes mandatory to use a series of devices with different full scale (FS) values. As shown in Fig. 6 , if two pressure meters and two flow rate me- ters are used having their FS at Re = 500 and at Re = 2300 when the

30 total uncertainty pressure drop, FS ±0.5% 25 mass flow rate, FS ±0.5% 20 15
30
total uncertainty
pressure drop, FS ±0.5%
25
mass flow rate, FS ±0.5%
20
15
10
5
0
0 500
1000
1500
2000
2500
uncertainty of friction factor (%)

Re

Fig. 5. Contribution of the differential pressure sensor and of the mass flow rate sensor having an uncertainty equal to ±0.5% of FS (Re = 2300) on friction factor uncertainty.

14 12 10 diameter, ±2% length, ±0.3% temperature, ±0.25% 8 pressure drop, ±0.5% outlet pressure,
14
12
10
diameter, ±2%
length, ±0.3%
temperature, ±0.25%
8
pressure drop, ±0.5%
outlet pressure, ±0.5%
mass flow rate, ±2%
6
4
2
0
0
500
1000
1500
2000
2500
uncertainty of friction factor (%)

Re

Fig. 4. Influence of each measured parameter with typical uncertainty for a microtube having an inner diameter of 100 l m and a length of 30 mm.

14 12 10 total uncertainty 8 pressure drop, FS ±0.5% mass flow rate, FS ±0.5%
14
12
10
total uncertainty
8
pressure drop, FS ±0.5%
mass flow rate, FS ±0.5%
6
4
2
0
0 500
1000
1500
2000
2500
uncertainty of friction factor (%)

Re

Fig. 6. Effect of the use of two differential pressure sensors and mass flow rate sensors having different FS (Re = 500 and Re = 2300) on friction factor uncertainty.

862

G.L. Morini et al. / Experimental Thermal and Fluid Science 35 (2011) 849–865

Reynolds number becomes lower than 500 the measurement can be switched to the set of devices having their FS at Re = 500 and this can greatly reduce the overall uncertainty of friction factor at lower Reynolds number. By comparing the data of Fig. 6 with those of Fig. 5 it is evident that using more devices having different full scale values it is pos- sible to expand the range of the Reynolds number in which the fric- tion factor uncertainty stays below ±14%.

6 5 pressure drop outlet pressure (corresponds to pressure drop) 4 inlet pressure outlet pressure
6
5
pressure drop
outlet pressure (corresponds to pressure drop)
4
inlet pressure
outlet pressure (corresponds to inlet pressure)
3
2
1
0
-1
0
500
1000
1500
2000
2500
sensitivity coefficient

Re

Fig. 7. Comparison of the influence of different strategies for the pressure measurement on the sensitivity coefficients of the inlet, outlet and differential pressure (sensors with a fixed uncertainty (±0.5%)).

As shown in Table 3 , using pressure sensors of identical uncer- tainty but different strategies of pressure measurement may result in a different accuracy for friction factor too. In this sense, an ‘‘a priori’’ uncertainty analysis can become an important design tool for microfluidics experiences as underlined in [71] . Fig. 7 indicates that if the inlet and outlet pressure are mea- sured for the determination of the friction factor for a compressible gas microflow (Strategy #2), the sensitivity coefficients for friction factor will be very large at lower Reynolds number compared with the measurement of pressure drop and outlet pressure. It is evident that for Reynolds number larger than 500, it is more advisable to choose an absolute pressure sensor with a higher accuracy for the inlet section in order to reduce the total uncertainty on friction factor. On the contrary, if the pressure drop and outlet pressure are measured (Strategy #1), it is more beneficial to use a more accu- rate differential pressure transducer in order to obtain a low total uncertainty. Uncertainty analysis can also be used to check the validity of the results published in the literature: sometimes discrepancies from the predictions of the theory can be traced back to the use of inaccurate instrumentation for the measurements. A list of experimental papers has been examined in order to check the level of uncertainty associated to the measured values of the friction fac- tors for liquids and gases. In Table 4 the declared uncertainties on the friction factors re- ported by Ferguson et al. [72] for experiments with liquid flows are summarized in order to have a reference for a comparison with the values described in this paper for gas flows. It is interesting to

Table 4 Declared uncertainties of quantities measured in experiments with liquid flows in percentage (from Ferguson et al. [72] ).

Authors

Geometry

Pressure (%)

Mass flow rate (%)

Re (%)

Friction factor (%)

d (%) (circular)

h, w (%) (rectangular)

L (%)

Li et al. [73] Liu and Garimella [74] Wu and Cheng [75] Mala and Li [76] Judy et al. [77] Chen et al. [78] Celata et al. [16] Peng et al. [79,80]

2

0.1

1.5

2

3.9

0.25

1.01

10.5

11.8

1.83

0.37

0.68

1.69

2

0.2

2

2

3

9.2

2.5

2.5–5

0.25

2

5

10.5

5.4

––

7

5

7

1.5

2.5

8

10

Table 5 Declared uncertainties of quantities measured in experiment with gas flows in percentage.

Authors

Geometry

Pressure

Temperature

Mass flow rate (%)

Re

Friction factor (%)

d (%) (circular)

h, w (%) (rectangular)

L (%)

(%)

(%)

(%)

Ewart et al. [63]

1.39

1.5

0.02

4.5 (const. volume); 4.2 (drop tracking)

Ewart et al. [65] Celata et al. [16]

h : 2.13; w : 0.20 –

1.06

0.5

0.02

4.5

– 19 (flow meter);27 (pipette)

2.48–3.67

Asako et al. [7] Zohar et al. [17] Hsieh et al. [22] Maurer et al.

0.13

h : 2; w : 1.25 h : 1; w : 1

0.003

0.42

0.98

12.5

<1

<1

<8.5

0.7

0.04

4.0

1.46

1.82

h : 2; w :1

1

2

2

[81]

Morini et al. [18] Araki et al. [82]

2

0.3

0.5

0.25

0.5–0.6

3

10

triangle and trapezoid D h : 3.23 –

0.2

5.13

2.2

10.9

Turner et al. [83] Tang et al. [15] Colin et al. [64]

4.9

4.8

0.3–2.98

0.02–0.07

0.25

0.17

2

4.5

5.9

h : 2.23–18.5 w :

0.2

 

0.58–1.4

Pitakarnnop et al. [67]

h : 5.3 w : 1.4

0.2

0.5

0.2

4 (const. volume); 3.1 (drop tracking)

G.L. Morini et al. / Experimental Thermal and Fluid Science 35 (2011) 849–865

Table 6 Typical values of parameters in experiments with gas flows.

863

Authors

 

Geometry and size ( l m)

Length (mm) Pressure (kPa)

 

T (K)

Mass flow rate (kg/s)

Re

 

Inlet

Outlet

Ewart

et

al.

[63]

Circ. d : 25.2 l m Rect. h: 9.38; w: 492 Circ. d : 30–254 Circ. d : 150

53

1.22–12.11

0.25–2.47

296.5

0.02–2 10 10 0.0049–22.5 10 10 – 4 10 6 1.5–6 10 9

0.0018–2.5

Ewart et al. [65] Celata et al. [16] Asako et al. [7]

9.4

0.060–115.47 0.012–32.65 –

50–91

Up to 1000

100

0.8–500

30–50

300

190

300

1508–2188

Zohar et al. [17]

Rect. h: 0.5 and 1; w : 40

4

Up to 400

100

Hsieh

et al. [22]

Rect.

h:

50; w : 200

24

2.7–64.63

0.68–13.19

300

0.88 10 8 –40.9 10 8 2.6–89.4

Maurer et al. [81] Morini et al. [18]

Rect. h: 1.14; w : 200 Circ. d : 133–730

10

140–500

48–100

296

6 10 12 5 10 10

0.001–0.07

200–1000

– – – – Up to 300

– 0.2 10 10 1.0 10 10 – 4 10 13 2 10 9 8 10 14 2 10 11

100–5000

Araki et al. [82] Tang et al. [15] Colin et al. [64]

Triangular and trapezoidal D h : 3.92–10.3 15 and 25

100

295

0.042–4.19

Circular and rectangular D h : 10–300 Rect. h: 0.5–4.5; w : 20, 50

27.5–100

100

295

3–6200

5

65–200

294

Pitakarnnop et al. [67] Rect. h: 1.88; w : 21.2

5

2–50

298.5

note that the typical values of the friction factor uncertainties vary from ±5.4% to ±11.8% and, in many papers, the most important uncertainty, related to the inner diameter, was not declared. In these works the flow was adiabatic and in many cases the temper- ature of the test flow was not checked. Table 5 reports a collection of declared uncertainties for exper- iments with gases. Comparing the data of Table 4 with those of Ta- ble 5 it is seen that for gas flows the uncertainty on the friction factor can be larger than ±12% due to the smaller dimensions of the tested microchannels (less than 150 l m generally) and to the larger uncertainties on mass flow rate measurement. In fact, very low flow rates and low values of pressure are used in these exper- iments in order to obtain large values of the Knudsen number (large rarefaction effects). By observing the total uncertainties of the friction factor of Ta- ble 5 it is interesting to note that in many experimental works the data about the uncertainty analysis are incomplete and it is impos- sible to know the real value of the total uncertainty on the exper- imental friction factors. The typical values of temperature, pressure and mass flow rate for these works are given in Table 6 , together with the range of Reynolds numbers investigated. It is interesting to highlight that in the experimental works in which the tested Reynolds numbers were larger than 10 only com- pressibility effects were evidenced and analysed; on the contrary, in order to study the rarefaction effects on the gas microflows the Reynolds number must be less than 10 (very low mass flow rates). In fact, in order to study the gas rarefaction effects small channels (usually less than 20 l m) and low values of pressure (less than 0.1 bar) must be used. Under these conditions the values of the mass flow rate are very low (10 6 10 14 kg/s) and