Measurement of contact angles The contact of 4 He crystals with walls: hysteresis of the contact...

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measurement of contact measurement of contact angles angles The contact of The contact of 4 4 He crystals with walls: He crystals with walls: hysteresis of the contact angle hysteresis of the contact angle S. Sasaki S. Sasaki a a , F. Caupin and S. Balibar , F. Caupin and S. Balibar Laboratoire de Physique Statistique de l'ENS (Paris, France) Laboratoire de Physique Statistique de l'ENS (Paris, France) a - now at North Western Univ. (USA) a - now at North Western Univ. (USA) Abstract Abstract : : We have measured the contact angle of the liquid-solid interface of helium 4 with different walls. It was known to be about 45° but we have found that is rather hysteretic with advancing angles of about 25° and receding angles of about 55 ° . Although these angles are similar for copper, glass, and graphite substrates, the hysteresis seems to increase with roughness, as expected from the work of Rolley and Guthmann (Phys. Rev. Lett. 98, 166105, 2007). This angle is an important parameter for the existence of liquid channels where grain boundaries meet walls. The hysteresis of the contact angle is known to increase with The hysteresis of the contact angle is known to increase with the substrate roughness (see, for example, the work of E. the substrate roughness (see, for example, the work of E. Rolley and C. Guthmann, PRL 98, 166105, 2007). We see Rolley and C. Guthmann, PRL 98, 166105, 2007). We see perhaps such a tendancy. perhaps such a tendancy. The surface of our HOPG graphite was difficult to clean but, The surface of our HOPG graphite was difficult to clean but, after 3 days pumping of the cell at 100°C, we could observe after 3 days pumping of the cell at 100°C, we could observe frequent nucleation of oriented crystals on either one or the frequent nucleation of oriented crystals on either one or the other graphite piece (see photograph on the right). The other graphite piece (see photograph on the right). The contact angle on graphite is similar to that on glass or copper contact angle on graphite is similar to that on glass or copper because the helium crystals are not oriented parallel to the because the helium crystals are not oriented parallel to the graphite lattice. graphite lattice. The value of the contact angle The value of the contact angle c c is important for the is important for the existence of liquid channels where grain boundaries meet existence of liquid channels where grain boundaries meet walls. Indeed, these channels exist only if the contact angle walls. Indeed, these channels exist only if the contact angle c c < < , where , where is half the dihedral angle of grooves is half the dihedral angle of grooves appearing where GBs emerge at the liquid-solid interface. appearing where GBs emerge at the liquid-solid interface. a square hole (11 x 11 mm a square hole (11 x 11 mm 2 2 ) in a gold- ) in a gold- plated copper plate (either 10 mm or 3 plated copper plate (either 10 mm or 3 mm thick) mm thick) 2 glass windows sealed with indium O- 2 glass windows sealed with indium O- rings. rings. the cell stands pressures up to at least 64 the cell stands pressures up to at least 64 bar and can be cooled down to 35 mK. bar and can be cooled down to 35 mK. see Sasaki, Caupin and Balibar, see Sasaki, Caupin and Balibar, submitted to J. Low Temp. Phys., July submitted to J. Low Temp. Phys., July 2008. 2008. the experimental cells the experimental cells the shape of the liquid-solid interface depends on gravity and surface tension, as the shape of the liquid-solid interface depends on gravity and surface tension, as for an ordinary liquid surface. for an ordinary liquid surface. The contact angle si measured thanks to a fit with the Laplace equation near the The contact angle si measured thanks to a fit with the Laplace equation near the wall: wall: where x is the horizontal distance to the reference x where x is the horizontal distance to the reference x 0 0 , l , l c c ~ 1 mm ~ 1 mm is the capillary is the capillary length and z is the vertical height. length and z is the vertical height. Results: Results: substrate substrate advancing angle advancing angle receding angle receding angle copper copper 7 < 7 < adv adv < 30° < 30° 42 < 42 < rec rec < 63° < 63° glass glass 13 < 13 < adv adv < 38° < 38° 40 < 40 < rec rec < 66° < 66° graphite graphite 31 < 31 < adv adv < 43° < 43° 44 < 44 < rec rec < 62° < 62° During growth, the « advancing angle » is smaller than during melting (« receding During growth, the « advancing angle » is smaller than during melting (« receding angle »). angle »). We used either HOPG graphite which was difficult to clean properly since we coudl We used either HOPG graphite which was difficult to clean properly since we coudl only warm it at 100°C under moderate vacuum (3 days pumping through the fill only warm it at 100°C under moderate vacuum (3 days pumping through the fill line) line) Discussion Discussion contact with a glass plate contact with a glass plate contact with a copper wall contact with a copper wall growing (16 growing (16 m/s) m/s) melting (10 melting (10 m/s) m/s) fits with Laplace eq. fits with Laplace eq. growing (60 growing (60 m/s) m/s) melting (5 melting (5 m/s) m/s) nucleation of an oriented nucleation of an oriented helium crystal on HOPG helium crystal on HOPG graphite graphite the contact line of a grain boundary the contact line of a grain boundary (GB) with a wall is in reality a liquid (GB) with a wall is in reality a liquid channel with triangular cross section channel with triangular cross section if the wall is sufficiently favorable to if the wall is sufficiently favorable to the liquid phase (if the liquid phase (if c < < crystal grain 1 crystal grain 1 crystal grain 2 crystal grain 2 liquid liquid wall wall mixing chamber mixing chamber pressure gauge pressure gauge fill line (0.6 mm ID) fill line (0.6 mm ID)

Transcript of Measurement of contact angles The contact of 4 He crystals with walls: hysteresis of the contact...

Page 1: Measurement of contact angles The contact of 4 He crystals with walls: hysteresis of the contact angle S. Sasaki a, F. Caupin and S. Balibar Laboratoire.

measurement of contact anglesmeasurement of contact angles

The contact of The contact of 44He crystals with walls:He crystals with walls:hysteresis of the contact anglehysteresis of the contact angle

S. Sasaki S. Sasaki aa, F. Caupin and S. Balibar , F. Caupin and S. Balibar Laboratoire de Physique Statistique de l'ENS (Paris, France)Laboratoire de Physique Statistique de l'ENS (Paris, France)

a - now at North Western Univ. (USA)a - now at North Western Univ. (USA)

AbstractAbstract:: We have measured the contact angle of the liquid-solid interface of helium 4 with different walls.It was known to be about 45° but we have found that is rather hysteretic with advancing angles of about 25° and receding angles of about 55 ° . Although these angles are similar for copper, glass, and graphite substrates, the hysteresis seems to increase with roughness, as expected from the work of Rolley and Guthmann (Phys. Rev. Lett. 98, 166105, 2007). This angle is an important parameter for the existence of liquid channels where grain boundaries meet walls.

The hysteresis of the contact angle is known to increase with the The hysteresis of the contact angle is known to increase with the substrate roughness (see, for example, the work of E. Rolley and C. substrate roughness (see, for example, the work of E. Rolley and C. Guthmann, PRL 98, 166105, 2007). We see perhaps such a tendancy.Guthmann, PRL 98, 166105, 2007). We see perhaps such a tendancy.The surface of our HOPG graphite was difficult to clean but, after 3 The surface of our HOPG graphite was difficult to clean but, after 3 days pumping of the cell at 100°C, we could observe frequent days pumping of the cell at 100°C, we could observe frequent nucleation of oriented crystals on either one or the other graphite nucleation of oriented crystals on either one or the other graphite piece (see photograph on the right). The contact angle on graphite is piece (see photograph on the right). The contact angle on graphite is similar to that on glass or copper because the helium crystals are not similar to that on glass or copper because the helium crystals are not oriented parallel to the graphite lattice.oriented parallel to the graphite lattice.The value of the contact angle The value of the contact angle cc is important for the existence of is important for the existence of

liquid channels where grain boundaries meet walls. Indeed, these liquid channels where grain boundaries meet walls. Indeed, these channels exist only if the contact angle channels exist only if the contact angle cc < < , where , where is half is half

the dihedral angle of grooves appearing where GBs emerge at the the dihedral angle of grooves appearing where GBs emerge at the liquid-solid interface.liquid-solid interface.

a square hole (11 x 11 mma square hole (11 x 11 mm22) in a gold-plated ) in a gold-plated copper plate (either 10 mm or 3 mm thick)copper plate (either 10 mm or 3 mm thick)2 glass windows sealed with indium O-rings.2 glass windows sealed with indium O-rings.the cell stands pressures up to at least 64 bar the cell stands pressures up to at least 64 bar and can be cooled down to 35 mK.and can be cooled down to 35 mK.

see Sasaki, Caupin and Balibar, submitted to J. see Sasaki, Caupin and Balibar, submitted to J. Low Temp. Phys., July 2008.Low Temp. Phys., July 2008.

the experimental cells the experimental cells

the shape of the liquid-solid interface depends on gravity and surface tension, as for an ordinary the shape of the liquid-solid interface depends on gravity and surface tension, as for an ordinary liquid surface.liquid surface.The contact angle si measured thanks to a fit with the Laplace equation near the wall:The contact angle si measured thanks to a fit with the Laplace equation near the wall:

where x is the horizontal distance to the reference xwhere x is the horizontal distance to the reference x00, l, lcc ~ 1 mm~ 1 mm is the capillary length and z is is the capillary length and z is

the vertical height.the vertical height.Results:Results:

substratesubstrate advancing angleadvancing angle receding anglereceding anglecoppercopper 7 < 7 < advadv < 30° < 30° 42 < 42 < recrec < 63° < 63°

glassglass 13 < 13 < advadv < 38° < 38° 40 < 40 < recrec < 66° < 66°

graphitegraphite 31 < 31 < advadv < 43° < 43° 44 < 44 < recrec < 62° < 62°

During growth, the « advancing angle » is smaller than during melting (« receding angle »).During growth, the « advancing angle » is smaller than during melting (« receding angle »).We used either HOPG graphite which was difficult to clean properly since we coudl only warm We used either HOPG graphite which was difficult to clean properly since we coudl only warm it at 100°C under moderate vacuum (3 days pumping through the fill line)it at 100°C under moderate vacuum (3 days pumping through the fill line)

DiscussionDiscussion

contact with a glass platecontact with a glass plate

contact with a copper wallcontact with a copper wall

growing (16 growing (16 m/s)m/s) melting (10 melting (10 m/s)m/s)

fits with Laplace eq.fits with Laplace eq.

growing (60 growing (60 m/s)m/s) melting (5 melting (5 m/s)m/s)

nucleation of an oriented helium nucleation of an oriented helium crystal on HOPG graphitecrystal on HOPG graphite

the contact line of a grain boundary (GB) the contact line of a grain boundary (GB) with a wall is in reality a liquid channel with a wall is in reality a liquid channel with triangular cross section if the wall is with triangular cross section if the wall is sufficiently favorable to the liquid phase sufficiently favorable to the liquid phase

(if (if cc < <

crystal grain 1crystal grain 1

crystal grain 2crystal grain 2

liquidliquidwal

lw

all

mixing chambermixing chamber

pressure gaugepressure gauge

fill line (0.6 mm ID)fill line (0.6 mm ID)