EP3412801B1 - Procédé de production d'un agencement régulier de gouttelettes d'un premier liquide en jet continu d'un second liquide - Google Patents
Procédé de production d'un agencement régulier de gouttelettes d'un premier liquide en jet continu d'un second liquide Download PDFInfo
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- EP3412801B1 EP3412801B1 EP17175132.4A EP17175132A EP3412801B1 EP 3412801 B1 EP3412801 B1 EP 3412801B1 EP 17175132 A EP17175132 A EP 17175132A EP 3412801 B1 EP3412801 B1 EP 3412801B1
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- Prior art keywords
- liquid
- droplets
- continuous jet
- regular
- stream
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- 239000007788 liquid Substances 0.000 title claims description 159
- 238000004519 manufacturing process Methods 0.000 title claims description 26
- 238000000034 method Methods 0.000 claims description 30
- 239000000835 fiber Substances 0.000 claims description 24
- 238000007711 solidification Methods 0.000 claims description 9
- 230000008023 solidification Effects 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- KEUKAQNPUBYCIC-UHFFFAOYSA-N ethaneperoxoic acid;hydrogen peroxide Chemical compound OO.CC(=O)OO KEUKAQNPUBYCIC-UHFFFAOYSA-N 0.000 description 20
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 12
- 238000005538 encapsulation Methods 0.000 description 7
- 239000007787 solid Substances 0.000 description 6
- 239000012071 phase Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000011258 core-shell material Substances 0.000 description 4
- 238000001523 electrospinning Methods 0.000 description 4
- 239000000839 emulsion Substances 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 230000000737 periodic effect Effects 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000011162 core material Substances 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 230000001225 therapeutic effect Effects 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 239000013598 vector Substances 0.000 description 2
- HIQIXEFWDLTDED-UHFFFAOYSA-N 4-hydroxy-1-piperidin-4-ylpyrrolidin-2-one Chemical compound O=C1CC(O)CN1C1CCNCC1 HIQIXEFWDLTDED-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- XRWMGCFJVKDVMD-UHFFFAOYSA-M didodecyl(dimethyl)azanium;bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCC XRWMGCFJVKDVMD-UHFFFAOYSA-M 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229960005486 vaccine Drugs 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
- B05B7/00—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
- B05B7/02—Spray pistols; Apparatus for discharge
- B05B7/08—Spray pistols; Apparatus for discharge with separate outlet orifices, e.g. to form parallel jets, i.e. the axis of the jets being parallel, to form intersecting jets, i.e. the axis of the jets converging but not necessarily intersecting at a point
- B05B7/0807—Spray pistols; Apparatus for discharge with separate outlet orifices, e.g. to form parallel jets, i.e. the axis of the jets being parallel, to form intersecting jets, i.e. the axis of the jets converging but not necessarily intersecting at a point to form intersecting jets
- B05B7/0846—Spray pistols; Apparatus for discharge with separate outlet orifices, e.g. to form parallel jets, i.e. the axis of the jets being parallel, to form intersecting jets, i.e. the axis of the jets converging but not necessarily intersecting at a point to form intersecting jets with jets being only jets constituted by a liquid or a mixture containing a liquid
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/36—Matrix structure; Spinnerette packs therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
- B05B12/00—Arrangements for controlling delivery; Arrangements for controlling the spray area
- B05B12/004—Arrangements for controlling delivery; Arrangements for controlling the spray area comprising sensors for monitoring the delivery, e.g. by displaying the sensed value or generating an alarm
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
- B05B17/00—Apparatus for spraying or atomising liquids or other fluent materials, not covered by the preceding groups
- B05B17/04—Apparatus for spraying or atomising liquids or other fluent materials, not covered by the preceding groups operating with special methods
- B05B17/06—Apparatus for spraying or atomising liquids or other fluent materials, not covered by the preceding groups operating with special methods using ultrasonic or other kinds of vibrations
Definitions
- the present invention relates to a method for producing a regular arrangement of droplets of at least one first liquid in a continuous jet of a second liquid, which can be further used for producing a fibre.
- Drops can be encapsulated in a liquid continuous phase in the form of emulsions, which is well-known.
- a regular arrangement of drops, particularly a regular spatial arrangement of monodisperse drops, is, however, hardly obtainable.
- Existing approaches try to achieve that goal by means of guiding the continuous phase through pipes or channels, which prevents, however, the formation of fibres.
- core-shell nanofibres can be produced using electrospinning, it is not possible to produce a regular arrangement of inclusion and encapsulated objects, respectively, see e.g. Md. Fazley Elahi et al., "Core-shell Fibers for Biomedical Applications-A Review", Journal of Bioengineering & Biomedical Sciences 2013, Volume 3, Issue 1, 1000121 .
- fibres with encapsulated objects are usually not cylindrical, but exhibit constrictions between the encapsulated objects, which can be disadvantageous for some applications.
- US20017/054119 discloses a microfluidic flow-focusing device for forming monodisperse particles.
- a first liquid comes from a central channel and a second liquid flows as a continuous phase from side channels such that the continuous liquid phase surrounds the inner liquid stream.
- the resulting inner liquid stream has an unstable cylindrical morphology and breaks up within the orifice in a periodic manner to release fluidic droplets contained within the continuous liquid phase into the outlet channel.
- WO 2014/120321 discloses an electrospinning fiber manufacturing device for producing ultra-thin continuous core-shell and hollow fibres where the device includes two closely spaced parallel thin conductive wires as a spinneret (a dual-wire spinneret) for delivery of two-polymer emulsions (two immiscible polymers dissolved in an organic solvent or similar aqueous two-compound emulsion) along the dual-wire spinneret.
- a spinneret a dual-wire spinneret
- two-polymer emulsions two immiscible polymers dissolved in an organic solvent or similar aqueous two-compound emulsion
- the method should allow for the subsequent production of fibres, more particularly of cylindrical fibres, with regularly arranged encapsulated objects.
- a method for producing a regular arrangement of droplets of at least one first liquid in a continuous jet of a second liquid wherein the first liquid and the second liquid are immiscible and chosen such that a surface tension ( ⁇ d ) of the first liquid is greater than the sum of a surface tension ( ⁇ j ) of the second liquid and an interfacial tension ( ⁇ dj ) between the first liquid and the second liquid, wherein at least one regular stream of the droplets is produced using at least one first nozzle and the continuous jet is produced using a second nozzle, wherein the nozzles are adjusted such that the continuous jet and the at least one regular stream of droplets are in a common plane, collide and the continuous jet of the second liquid encapsulates the regular arrangement of the droplets of the at least one first liquid after the collision.
- both liquids have densities in the range from 700 kg/m 3 to 2000 kg/m 3 and viscosities in the range from 0,5 mPa s to 5 Pa s.
- the choice of the surface tensions and interfacial tension ensures the thermodynamic stability of the full encapsulation of the drops by the jet. In other words, due to surface tensions of the two liquids and the interfacial tension between them the first liquid can be totally wetted by the second liquid, ensuring full encapsulation of the droplets in the jet.
- the above condition can be met employing silicon oils as second liquid, i.e. for the jet, and aqueous glycerol solutions for the first liquid, i.e. for the stream of droplets.
- silicon oils as second liquid
- aqueous glycerol solutions for the first liquid
- suitable couples of liquids can be easily found.
- adding surfactants in the aqueous phase e.g. didodecyldimethylammonium bromide with an appropriate oil like isopropyl myristate, enables the exploration of cases where the encapsulating jet is aqueous. This means, however, that in practice the surface and interfacial tensions of the liquids can be routinely adjusted by means of surfactants, in order to fulfil the above-mentioned relation, making possible an almost arbitrary choice of the liquids.
- Regular stream of droplets means in particular that the spatial arrangement of the droplets within the stream is regular, e.g. due to a periodic spatial arrangement.
- the liquids are supplied to the nozzles by well-known means and liquid supplying system, respectively, e.g. by means of pressurised tanks, with each liquid being stored in an own pressurised tank.
- pressurised tank e.g. a peristaltic pump, a syringe pump, etc.
- the adjustment of the nozzles is done not only with respect to the orientation and position of the nozzles, but in general with respect to collision parameters, like velocities and (spatial) periodicities of the continuous jet and the stream of droplets, respectively.
- collision parameters like velocities and (spatial) periodicities of the continuous jet and the stream of droplets, respectively.
- the typical distance between nozzle orifices is in the range from 1 mm to 20 cm, particularly from 5 mm to 10 cm
- the typical distances between a point or region of collision and the nozzle orifices is in the range from 1 mm to 20 cm, particularly from 1 cm to 10 cm.
- That the continuous jet and the stream of droplets are in the same (common) plane particularly means that a trajectory of the continuous jet and a trajectory of the droplets and the stream of droplets, respectively, are in said plane.
- each of these streams are of a different first liquid (instead of the same first liquid), with each first liquid being immiscible with the second liquid and fulfilling the above-mentioned condition ( ⁇ d > ⁇ j + ⁇ dj ).
- Each stream of droplets can be provided by a corresponding first nozzle.
- Each first liquid can be supplied to each first nozzle by means of, e.g. an own pressurised tank or an own pump.
- the different streams of droplets - of the same first liquid or of several first liquids - collide with the continuous jet at different positions or in different regions.
- the continuous jet and the at least one stream of droplets enclose an angle in the common plane, which angle is in the range from 1° to 170°, preferably from 5° to 90°.
- a diameter of an orifice of the at least one first nozzle and a diameter of an orifice of the second nozzle are adjusted in the range from 10 ⁇ m to 1500 ⁇ m.
- the nozzles can have variable orifices, wherein such nozzles are known in the art.
- the given range of orifice diameters guarantee a particularly reliable production of the continuous jet of the second liquid encapsulating the regular arrangement of the droplets of the first liquid in the course of the collision of the continuous jet and the stream of droplets.
- the droplet diameter can be precisely tuned by choosing the nozzle diameter, but typically is not equal to the latter.
- a nozzle diameter from 30 to 1300 ⁇ m can cause droplet diameters from 50 ⁇ m to 2700 ⁇ m.
- the nozzle diameter directly corresponds to the jet diameter, i.e. a nozzle diameter from 30 ⁇ m to 1500 ⁇ m causes identical jet diameters from 30 ⁇ m to 1500 ⁇ m.
- the jet diameter is chosen larger than the droplet diameter.
- the droplet diameter can be precisely tuned, as already mentioned above, it is possible to control the diameter of the droplets in the stream of droplets and consequently also the diameter of the droplets encapsulated in the continuous jet of the second liquid, i.e. of those droplets that form the encapsulated regular arrangement in the continuous jet.
- regular does not exclusively relate to the spatial arrangement of the droplets, but also to their size.
- the regular stream of droplets with the droplets being monodisperse.
- the at least one regular stream of the droplets is produced with the size of the droplets being deliberately adjusted, preferably with the droplets being monodisperse, in order to achieve the regular arrangement of the droplets of the at least one first liquid encapsulated by the continuous jet of the second liquid with the size of the droplets being deliberately adjusted, preferably with the droplets being monodisperse.
- micro stages are used for adjusting orientations and positions of the nozzles.
- Micro stages as such are well-known.
- each nozzle can be precisely translated in all three directions in space in the range from -5 mm to +5 mm and can be precisely rotated in the common plane in the range from 0° to 170° by means of the micro stages.
- the at least one regular stream of droplets is produced with a droplet production frequency in the range from 1 Hz to 100 kHz, preferably from 5 kHz to 50 kHz. Accordingly, the regular arrangement of the droplets is an easily produced periodic spatial arrangement as a function of to the production frequency.
- the at least one first nozzle can be equipped with a piezo actuator, for example, which is known in the art.
- the resulting regularity of the droplet stream provides perfectly reproducible collisions.
- the latter can be imaged using stroboscopic illumination (e.g. by means of LEDs) at the droplet production frequency, allowing for an elegant way of in-situ controlling the production of the continuous jet of the second liquid encapsulating the regular arrangement of the droplets of the first liquid.
- the at least one regular stream of droplets has a velocity u d
- the continuous jet has a velocity u j
- the droplets in the regular stream are spaced at a spatial period l d
- the continuous jet has a diameter D j
- the following relation holds l d / D j * u j / u d ⁇ 2 , preferably l d / D j * u j / u d ⁇ 1,8 .
- velocities u j and u d are defined in the laboratory frame of reference. Absolute values of these velocities are typically in the range from 1 m/s to 20 m/s.
- the above-described method also allows for an easy production of fibres with encapsulated objects that are regularly arranged within the fibres. Therefore, the continuous jet of the second liquid encapsulating the regular arrangement of the droplets of the first liquid (also referred to as “continuous jet with droplets” in the following) only needs to be hardened.
- a method for producing a fibre wherein it is provided according to the present invention that a regular arrangement of droplets of at least one first liquid in a continuous jet of a second liquid is produced using a method according to the present invention and that the continuous jet of the second liquid encapsulating the regular arrangement of the droplets of the at least one first liquid is hardened.
- the encapsulated objects and inclusions, respectively in the so-produced fibre, which objects are built by the droplets not only can be spatially regularly arranged in the fibre, but also their sizes can be deliberately adjusted, since the size of the droplets can be deliberately adjusted, as described above.
- fibres with encapsulated monodisperse objects can thus be produced.
- the resulting fibres can be of particular interest for materials sciences, for example, since the inclusions can provide specific properties to the fibres. Moreover, the contrast between the properties of the hardened continuous jet of the second liquid and of the inclusions as well as the regularity of their spatial distribution in the fibre can be of interest in optics, since the inclusions can act as an array of lenses, for example. Furthermore the resulting fibres can be of interest for biological and pharmaceutical applications where encapsulation is a very active field. Encapsulating active biological elements such as cells or micro-organisms opens the routes to several therapeutic and non-therapeutic applications including, for example, tissue engineering, regenerative medicine, oral delivery of vaccines, etc.
- the difficulties lie in keeping the encapsulated cells or microorganisms (referred to as "reservoirs" in the following) alive during the encapsulation process but also after the encapsulation process for a longer period which depends on the specific application. Particularly, it should be able that nutriments diffuse through the encapsulating phase and it is therefore essential to achieve a spatial distribution of the encapsulated reservoirs which allows equal supply to all of them. Encapsulating each reservoir individually is unsatisfactory because of tremendous difficulties in manipulating and "dosing" the reservoirs, particularly in case of medical applications.
- the production method according to the invention does offer the possibility to control and tune the distribution of the encapsulated objects via the formation of regular structures, i.e. via the formation of a regular arrangement of the droplets of at least one first liquid in the continuous jet of the second liquid, leading to regularly arranged objects in the fibres.
- regular structures i.e. via the formation of a regular arrangement of the droplets of at least one first liquid in the continuous jet of the second liquid, leading to regularly arranged objects in the fibres.
- hardening can be achieved by exploiting a sol-gel transition.
- hardening can also be achieved by cooling down the continuous jet with droplets at least below the solidification temperature of the second liquid.
- This can be done utilising the naturally occurring cooling down of the continuous jet with droplets along its trajectory in air (or in another chosen ambient gas in a certain production set-up).
- the continuous jet with droplets has e.g. an initial temperature of 60°C (which is above the solidification temperature of the second liquid in this example) and cools down along its trajectory downstream the region of the collision to a temperature of 30° (which is at least below the solidification temperature of the second liquid, preferably also below the solidification temperature of the first liquid in this example).
- the hardening is achieved by cooling down the continuous jet of the second liquid encapsulating the regular arrangement of the droplets of the at least one first liquid below a solidification temperature of the second liquid. If the temperature is reduced below the temperature of the at least one first liquid too, a fibre is obtained with encapsulated regularly arranged objects that are solid.
- a cylindrical fibre which according to the present invention is obtainable by a method according to the present invention.
- the size of the inclusions can be deliberately adjusted, as already mentioned above.
- monodisperse inclusions can be achieved.
- this includes that also a regular arrangement of droplets of a first liquid in a continuous jet of a second liquid is provided, which is obtainable by a method according to the present invention.
- the size of the droplets of the regular arrangement in the continuous jet can be deliberately adjusted, as described above.
- the droplets of the regular arrangement in the continuous jet can be monodisperse.
- Fig. 1 shows a schematic view of a set-up for carrying out a method for producing a regular arrangement of droplets 3 of a first liquid 1 in a continuous jet 5 of a second liquid 2 according to the present invention.
- the first liquid 1 and the second liquid 2 are immiscible and chosen such that a surface tension ⁇ d of the first liquid 1 is greater than the sum of a surface tension ⁇ j of the second liquid 2 and an interfacial tension ⁇ dj between the first liquid 1 and the second liquid 2, i.e. the following relation holds: ⁇ d > ⁇ j + ⁇ dj .
- the first liquid 1 can be totally wetted by the second liquid 2.
- a regular stream 4 of the droplets 3 is produced using at a first nozzle 6 and the continuous jet 5 is produced using a second nozzle 7.
- the first nozzle is equipped with a piezo actuator (not shown), which is known in the art.
- the droplets can be produced with a droplet production frequency in the range from 1 Hz to 100 kHz, e.g. with a droplet production frequency of 10 kHz.
- the resulting regularity of the droplets 3 in the stream 4 provides perfectly reproducible collisions.
- the latter can be imaged using stroboscopic illumination by means of an LED (light-emitting diode) 10 at the droplet production frequency, allowing for an elegant way of in-situ controlling the production of the continuous jet 5 of the second liquid 2 encapsulating the regular arrangement of the droplets 3 of the first liquid 1.
- the LED 10 is arranged downstream the point or region where the collision takes place.
- the LED 10 is positioned at one side of the continuous jet 5 with the encapsulated droplets 3 and a camera 9 is positioned on the other side, opposite the LED 10 for taking the corresponding images, preferably with an integer multiple of the droplet production frequency.
- the nozzles 6, 7 are adjusted such that the continuous jet 5 and the regular stream 4 of droplets 3 are in a common plane 8, collide and the continuous jet 5 of the second liquid 2 encapsulates the regular arrangement of the droplets 3 of the at least one first liquid 1 after the collision. Thereby, the above-mentioned relation ensures full encapsulation of the droplets 3 in the jet 5.
- the common plane 8 is parallel to spatial directions x, y that are standing perpendicular to each other as well as to spatial direction z, cf. Fig. 2 .
- the distance between nozzle orifices is in the range from 5 mm to 5 cm and the distances between a point or region of collision and the nozzle orifices is in the range from 1 cm to 10 cm, typically.
- micro stages are used for adjusting the orientation (+/- 90°) and position (+/- 5 mm) of the nozzles 6, 7 very precisely.
- the orifices have diameters that can be varied and are preferably adjusted in the range from 10 ⁇ m to 1500 ⁇ m.
- both liquids 1, 2 have densities in the range from 700 kg/m 3 to 2000 kg/m 3 and viscosities in the range from 0,5 mPa s to 5 Pa s.
- the first liquid 1 is an aqueous solution of glycerol with 50 wt.% glycerol and 50 wt.% water and the second liquid 2 is a silicon oil.
- the orifices of the nozzles 6, 7 are adjusted such that a Diameter D j of the continuous jet 5 (of the silicon oil) is 300 ⁇ m and a diameter D d of the droplets 3 (of the aqueous solution of glycerol) is 192 ⁇ m. In the shown example, this leads to a flow rate of 348 ⁇ l/s for the continuous jet 5 of the second liquid 2 and to a flow rate of 44 ⁇ l/s for the regular stream 4 of droplets 3.
- the liquids 1, 2 are supplied to the nozzles 6, 7 by means of pressurised tanks 11, 12 that are independent from each other. Thereby, the first liquid 1 is stored in the pressurised tank 11 and the second liquid 2 is stored in the pressurised tank 12.
- Supply tubes 13 connect each of the pressurised tanks 11, 12 with the respective nozzle 6, 7.
- the continuous jet 5 of the second liquid 5 encapsulating the regular arrangement of the droplets 3 of the first liquid 1 remains after the collision, i.e. downstream of the point or region where the collision takes place.
- the continuous jet 5 and the stream 4 of droplets 3 enclose an angle ⁇ in the common plane 8, which is in the range from 1° to 170°, preferably from 5° to 90°, more preferably from 10° to 90°.
- the angle ⁇ can be seen in the detailed view of Fig. 2 . Moreover, it is illustrated that the regular stream 4 of droplets 3 has a velocity u d (note that bold letters indicate vectors) and the continuous jet 5 has a velocity u j in the laboratory frame. Absolute values
- are typically in the range from 1 m/s to 20 m/s.
- the resulting relative velocity U (indicated by the vectors for U /2 in Fig. 2 ) is given by u d - u j .
- the Cartesian coordinate system spanned by spatial directions x, y, z is rotated such that the spatial direction y is parallel to U .
- Fig. 3 further illustrates how perfectly regular the achieved arrangement of the droplets 3 in the continuous jet 5 after the collision is.
- the continuous jet 5 contains regularly embedded droplets 3, with the regular arrangement of the droplets 3 encapsulated in the continuous jet 5 being determined by the regular arrangement of the droplets 3 in the stream 4 just before the collision.
- Said regular arrangement of the droplets 3 encapsulated in the continuous jet 5 manifests in a spatial period l i .
- the resulting continuous jet 5 encapsulating the regular arrangement of the droplets 3 can be hardened, e.g. by cooling, in order to produce a (solid) fibre 14 containing a regular arrangement of inclusions.
- said regular arrangement of the inclusions can (but in general does not have to) manifest in the spatial period l i of the droplets 3 encapsulated in the continuous jet 5.
- the fibre 14 contains liquid inclusions, i.e. the regularly arranged inclusions are the regularly arranged droplets 3 of the first liquid 1.
- Fig. 4 shows such a fibre 14, wherein a solidified second liquid 15 forms a body of the fibre 14. Within the solidified second liquid 15 and the body of the fibre 14, respectively, the droplets 3 of the first liquid 1 are regularly arranged along the fibre 14, i.e. the droplets 3 of the first liquid 1 form the regularly arranged inclusions.
- the body of the fibre 14 is perfectly cylindrical, i.e. a diameter of the body is essentially constant along the fibre 14, which is advantageous for many applications.
- the perfectly cylindrical shape can be achieved for solid inclusions as well - for example, when cooling down is done also below the solidification temperature of the first liquid 1.
Claims (11)
- Procédé de production d'un agencement régulier de gouttelettes (3) d'au moins un premier liquide (1) dans un jet continu (5) d'un second liquide (2), dans lequel le premier liquide (1) et le second liquide (2) sont immiscibles et choisis de sorte qu'une tension de surface (σd) du premier liquide (1) est supérieur à la somme d'une tension de surface (σj) du second liquide (2) et d'une tension interfaciale (σdj) entre le premier liquide (1) et le second liquide (2),
dans lequel au moins un courant régulier (4) des gouttelettes (3) est produit à l'aide d'au moins une première buse (6) et le jet continu (5) est produit à l'aide d'une seconde buse (7), dans lequel les buses (6, 7) sont ajustées de sorte que le jet continu (5) et l'au moins un courant régulier (4) de gouttelettes (3) soient dans un plan commun (8), qu'ils entrent en collision et que le jet continu (5) du second liquide (2) encapsule l'agencement régulier des gouttelettes (3) de l'au moins un premier liquide (1) après la collision. - Procédé selon la revendication 1, caractérisé en ce que l'au moins un courant régulier (4) des gouttelettes (3) est produit avec la taille des gouttelettes (3) délibérément ajustée, de préférence avec les gouttelettes (3) monodispersées, afin d'obtenir l'agencement régulier des gouttelettes (3) de l'au moins un premier liquide (1) encapsulé par le jet continu (5) du second liquide (2) avec la taille des gouttelettes (3) délibérément ajustée, de préférence avec les gouttelettes (3) monodispersées.
- Procédé selon l'une quelconque des revendications 1 à 2,
caractérisé en ce que le jet continu (5) et l'au moins un courant (4) de gouttelettes (3) englobent un angle (α) dans le plan commun (8), lequel angle (α) se trouve dans la plage de 1° à 170°, de préférence de 5° à 90°. - Procédé selon l'une quelconque des revendications 1 à 3,
caractérisé en ce qu'un diamètre d'un orifice de l'au moins une première buse (6) et un diamètre d'un orifice de la seconde buse (7) sont ajustés dans la plage de 10 µm à 1 500 µm. - Procédé selon l'une quelconque des revendications 1 à 4,
caractérisé en ce que des micro-étages sont utilisés pour ajuster des orientations et des positions des buses (6, 7). - Procédé selon l'une quelconque des revendications 1 à 5,
caractérisé en ce que l'au moins un courant régulier (4) de gouttelettes (3) est produit avec une fréquence de production de gouttelette dans la plage de 1 Hz à 100 kHz, de préférence de 5 kHz à 50 kHz. - Procédé selon l'une quelconque des revendications 1 à 6,
caractérisé en ce que l'au moins un courant régulier (4) de gouttelettes (3) a une vitesse ud , le jet continu (5) a une vitesse uj , les gouttelettes (3) dans le courant régulier (4) sont espacées à une période spatiale ld, le jet continu a un diamètre Dj, et la relation suivante s'applique - Procédé selon l'une quelconque des revendications 1 à 7,
caractérisé en ce que plusieurs courants réguliers (4) de gouttelettes (3), de préférence de plusieurs premiers liquides (1), sont fournis, dans lequel les plusieurs courants réguliers (4) des gouttelettes (3) sont produits à l'aide de plusieurs premières buses (6). - Procédé de production d'une fibre, caractérisé en ce qu'un agencement régulier de gouttelettes (3) d'au moins un premier liquide (1) dans un jet continu (5) d'un second liquide (2) est produit à l'aide du procédé selon l'une quelconque des revendications 1 à 8
et en ce que le jet continu (5) du second liquide (2) encapsulant l'agencement régulier des gouttelettes (3) de l'au moins un premier liquide (1) est durci. - Procédé selon la revendication 9, caractérisé en ce que le durcissement est obtenu par refroidissement du jet continu (5) du second liquide (2) encapsulant l'agencement régulier des gouttelettes (3) de l'au moins un premier liquide (1) sous une température de solidification du second liquide (2).
- Procédé selon l'une quelconque des revendications 9 et 10,
caractérisé en ce que seul le second liquide (2) est solidifié pendant le durcissement.
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EP17175132.4A EP3412801B1 (fr) | 2017-06-09 | 2017-06-09 | Procédé de production d'un agencement régulier de gouttelettes d'un premier liquide en jet continu d'un second liquide |
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EP17175132.4A EP3412801B1 (fr) | 2017-06-09 | 2017-06-09 | Procédé de production d'un agencement régulier de gouttelettes d'un premier liquide en jet continu d'un second liquide |
Publications (2)
Publication Number | Publication Date |
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EP3412801A1 EP3412801A1 (fr) | 2018-12-12 |
EP3412801B1 true EP3412801B1 (fr) | 2020-02-19 |
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US20070054119A1 (en) * | 2005-03-04 | 2007-03-08 | Piotr Garstecki | Systems and methods of forming particles |
WO2014120321A2 (fr) * | 2012-11-14 | 2014-08-07 | Ndsu Research Foundation | Nanofibres auto-cicatrisantes, composites et leurs procédés de production |
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