EP3385413A1 - Traitement microfluidique de fibres polymères - Google Patents

Traitement microfluidique de fibres polymères Download PDF

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Publication number
EP3385413A1
EP3385413A1 EP17165605.1A EP17165605A EP3385413A1 EP 3385413 A1 EP3385413 A1 EP 3385413A1 EP 17165605 A EP17165605 A EP 17165605A EP 3385413 A1 EP3385413 A1 EP 3385413A1
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EP
European Patent Office
Prior art keywords
inlet
core
fibre
microfluidic device
flow
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Ceased
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EP17165605.1A
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German (de)
English (en)
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Eidgenoessische Materialprufungs und Forschungsanstalt EMPA
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Eidgenoessische Materialprufungs und Forschungsanstalt EMPA
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Priority to EP17165605.1A priority Critical patent/EP3385413A1/fr
Priority to PCT/EP2018/059066 priority patent/WO2018185349A1/fr
Publication of EP3385413A1 publication Critical patent/EP3385413A1/fr
Ceased legal-status Critical Current

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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
    • D01D5/28—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
    • D01D5/34—Core-skin structure; Spinnerette packs therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
    • B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
    • B01L3/502769—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by multiphase flow arrangements
    • B01L3/502776—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by multiphase flow arrangements specially adapted for focusing or laminating flows

Definitions

  • the present invention generally relates to microfluidic processing of polymeric fibres. More particularly, the invention relates to a microfluidic device for creating sheathed flow, to a system for producing a polymeric fibre comprising such a device and to a method of forming a polymeric fibre.
  • An essential feature required for the controlled formation of layered micro and nanofibres is the establishment of a sheath flow, i.e. of a flow pattern comprising at least two concentrically disposed layers of flowing medium.
  • a sheath flow i.e. of a flow pattern comprising at least two concentrically disposed layers of flowing medium.
  • US 2011/0193259 A1 which relates to a method of creating a sheathed flow comprising a first and second fluid.
  • the method relies on a device with a flow channel having opposed facing top and bottom surfaces each provided with a so-called fluid transporting structure serving to divert the flow direction of one of the fluids in a transversal direction.
  • fluid transporting structure can be realized e.g. as a comparatively simple arrangement of oblique grooves, formation of a very regular layered structure appears difficult and variability of the process to yield differently dimensioned layered structures is limited.
  • US 8834780 B2 discloses a process of forming a polymer fibre by hydrodynamic spinning wherein a plurality of fluids is forced to flow through a conduit and to form a laminar flow comprising three or more layers of generally coaxial fluid flows.
  • the conduit is selected to define a cross-section of a tubular middle layer comprising a cross-linkable polymer precursor while another layer comprises a cross-linking agent.
  • Substantial diffusion of the polymer precursor away from the middle layer is prevented but a portion of cross-linking agent is allowed to diffuse into the middle layer to facilitate cross linking of the polymer precursor in the middle layer.
  • This approach requires formation of at least three layers, and variation of layered structures is essentially limited to changing the input flow rates of the respective layers of fluid flows.
  • a microfluidic device for creating sheathed flow comprising
  • a system for producing a polymeric fibre comprising a microfluidic device according to the invention, wherein each inlet channel is connected to an individual supply device providing a controllable inlet flow rate and wherein the outlet section is connected to fibre processing device selected from a dry and melt spinning system, a wet spinning system, an electrospinning system and a 3D-printing system.
  • fibre processing device selected from a dry and melt spinning system, a wet spinning system, an electrospinning system and a 3D-printing system.
  • a method of forming a polymeric fibre by means of a microfluidic device comprising pumping a polymerizable liquid into one of said core inlet and sheath inlet, and pumping an additional liquid into the other one of said core inlet and sheath inlet, in such manner as to form a sheathed laminar flow region comprising a core region of one of said liquids surrounded by a sheath layer of the other one of said liquids, the method further comprising inducing polymerization of the polymerizable liquid in the sheathed laminar flow region.
  • microfluidic shall be understood as known in the field of microfluidics, which field deals with the behaviour, control and manipulation of fluids that are geometrically constrained to a small, typically sub-millimetre, scale. Accordingly, the relevant regions of the tubular flow chamber and of the inlet channels, and also the terminal opening of the core inlet tube have a cross sectional size not exceeding 10 mm. There will also be some lower bound to the dimensions of the above mentioned features, which will be determined by the limitations of machining, but also by the practical requirement of achieving certain minimal flow rates.
  • “relevant regions” means regions of a component which have an impact on the sheath flow pattern generally pursued by the invention. A non-relevant region of an inlet channel could be, e.g. a liquid supply tube located clearly upstream of the microfluidic device.
  • a key feature of the present invention is the ability to vary the longitudinal position of the terminal opening of the core inlet tube in relation to the inlet openings of the one or optionally several sheath inlets, thereby allowing to modify and control the reaction time for the various components introduced into the flow chamber.
  • the range of longitudinal positions may reach from a position upstream of the most upstream inlet openings to a position downstream of the most downstream inlet openings.
  • the microfluidic device of the present invention is intended to provide sheathed flow of certain liquids that are useful for forming polymeric fibres.
  • these liquids comprise but are not limited to liquids containing polymerizable species, liquids containing polymerization agents, liquids containing inert species serving e.g. to assist an intended layering structure and liquids containing effective species such as dyes, chemical agents or biological agents.
  • the liquids may be in the form of aqueous or nonaqueous solutions.
  • the tubular flow chamber is substantially cylindrical.
  • substantially cylindrical is meant that the elongated channel formed in the chamber body has a cylindrical shape. Such a shape is convenient for the manufacturing process and is favourable for establishing the desired laminar flow. Nevertheless, according to another embodiment, a cylindrically symmetric shape with variable cross section along the longitudinal axis, for example a slowly converging circular cross section could be used.
  • the chamber body may have outer shapes substantially deviating from cylindrical.
  • the outer shape of the chamber body has a cylindrical or nearly cylindrical main part and a frusto-conically shaped distal part near the outlet.
  • the sheath inlet comprises a first group of at least two first inlet channels with inlet openings at a first axial position Z s1 and it further comprises a second group of at least two second inlet channels with inlet openings at a second axial position Z s2 axially displaced therefrom in a downstream direction.
  • this arrangement allows for additional flexibility in forming a layered laminar flow.
  • variation of the longitudinal position of the terminal opening of the core inlet tube in relation to the one or optionally several sheath inlets represents an important control parameter for the laminar flow and the process occurring therein.
  • the axial separation between the inlet channel groups constitutes a further design parameter providing even more flexibility in adjusting the polymerization processes occurring in the flow chamber.
  • the sheath inlet comprises a third group or even further groups of inlet channels.
  • the inlet section and the outlet section are provided with coupling elements for forming a medium-tight connection with a supply device and with a fibre processing device, respectively.
  • the coupling elements are configured according to some established laboratory standard for fluid connectors.
  • the polymeric material forming the chamber body is made of polycarbonate or PMMA. These materials are convenient to handle during assembly and use of the system, and they are suitable for contact with many media used in the field of polymeric fibre processing technology.
  • PMMA is sufficiently transparent to allow implementation of photolytic polymerization through the chamber body, i.e. without the need of additional window elements. This does not exclude further embodiments in which only specific regions of the device are made of such transparent material.
  • the core inlet tube is made of stainless steel.
  • the core inlet tube is formed as a simple, substantially cylindrical tube.
  • the core inlet tube comprises at least two substantially parallel core inlet channels, which allows forming multiple core fluids running in parallel.
  • the core inlet tube has a core-shell structure, i.e. it is formed of two concentric channels,
  • polymerization is induced photolytically, i.e. by irradiation with light of a suitable wavelength.
  • polymerization is induced by reaction of the polymerizable liquid and a polymerization agent contained in the additional liquid.
  • the method relies on a controlled exchange at the interface between the polymerizable liquid and the additional liquid.
  • a controlled exchange is provided according to the invention by establishing sheathed laminar flow having a flow pattern that can be appropriately controlled over a significant operational range.
  • reaction shall be understood broadly and shall include not only chemical reactions in the strict sense but also physical processes that lead to polymerization upon contacting two or more species.
  • the polymerizable liquid is pumped into the first inlet channels, a first additional liquid is pumped into the core inlet and a second additional liquid is pumped into the second inlet channels.
  • a laminar flow pattern of three concentric layers can be established, which allow implementation of a multitude of fibre forming processes.
  • the first and second additional liquids are identical.
  • the first and second additional liquids may be a polymerization agent which will form, respectively, a core region and an external region embedding therebetween a polymerizable liquid introduced via the first inlet channels.
  • the polymerizable liquid contains an admixture of a species of interest.
  • a species of interest can be any species selected from a whole variety of small molecules or nanoparticles that may serve a specific purpose when incorporated in a defined region of a polymeric fibre.
  • a first embodiment of a microfluidic device for creating sheathed flow as shown in Fig. 1 comprises a tubular flow chamber 2 with a longitudinal centre axis A.
  • the flow chamber has an inlet section 4 and an outlet section 6 axially displaced therefrom in a downstream direction.
  • the inlet section comprises a core inlet 8 and one sheath inlet 10.
  • the flow chamber is formed as an elongated channel 11 within a polymeric chamber body 12.
  • the core inlet comprises a core inlet tube 14 disposed coaxially within the flow chamber and having some entrance opening 15 and a terminal opening 16, wherein the latter is selectively positionable between a first core axial position (not shown in this figure) and a second core axial position shown in the figure.
  • the core inlet tube 14 is disposed in an axially slidable manner within the channel 11 by means of a schematically indicated element 17 forming a medium-tight sliding connection.
  • the sheath inlet comprises a group of two inlet channels 18a, 18b leading into the flow chamber at respective inlet openings 20a, 20b.
  • the inlet channels of this channel group are formed as substantially identical elongated channels within the chamber body and are disposed symmetrically at opposed sides of the longitudinal centre axis in a manner converging in downstream direction at an inclination angle ⁇ .
  • the inlet openings have substantially identical axial positions z s and the inclination angle shown for illustration purposes is approximately 30o.
  • a second embodiment of a microfluidic device for creating sheathed flow as shown in Figs. 2 and 3 comprises, in addition to the features of the first embodiment, a second group of two inlet channels 22a, 22b.
  • the first group of first inlet channels 18a, 18b has inlet openings at a first axial position z s1 and the second group of second inlet channels 22a, 22b has inlet openings 24a, 24b at a second axial position z s2 axially displaced therefrom in a downstream direction.
  • the terminal opening 16 of the core inlet tube 14 is selectively positionable between a first core axial position z c 1 and a second core axial position z c 2.
  • Figs. 4 to 7 show various embodiments of a system for producing a polymeric fibre, wherein each system comprises a microfluidic device of the above described kind.
  • the various inlet channels are connected to a respective supply device providing a controllable inlet flow rate.
  • the outlet section is connected to a basically known fibre processing device, which can be a dry and melt spinning system 26 ( Fig. 4 ), a wet spinning system 28 ( Fig. 5 ), an electrospinning system 30 ( Fig. 6 ) and a 3D-printing system 32 ( Fig. 7 ).
  • the stainless steel core inlet tube for forming a microjet is fabricated by using BD-syringe needle ( ⁇ 0.6 mm i.d.), which was bought from VWR.
  • the body's material of microjet is PTFE.
  • the connecting PTFE tubes ( ⁇ 1 mm i.d. & ⁇ 1.4 mm o.d.) were obtained from VWR International, Switzerland.
  • the 5 ml and 2.5 ml syringe (Discardit II) was purchased from VWR.
  • PEEK microfluidic tubing connectors from IDEX Europe GmbH, Germany
  • the neMESYS syringe pump system was purchased from Cetoni GmbH in Germany.
  • ZEISS Axio Observer A1 inverted microscope with 488 nm and 350 nm wavelength lasers (Zeiss, Germany) was applied.
  • Adobe Photoshop and Image J were applied to process images. Scanning Electron Microscopy (SEM) and Energy Dispersive X-Ray Analysis (EDX) were used for visualization and characterization.
  • SEM Scanning Electron Microscopy
  • EDX Energy Dispersive X-Ray Analysis
  • the 0.099g Sodium Alginate was solved in 5 ml distilled water with stirring (approx. 2hrs).
  • the 0.099g Sodium Alginate was mixed with 0.691 g Phenylbis (2,4,6-trimethylbenzoyl) phosphine oxide in 5ml distilled water with stirring (approx. 2hrs.).
  • the 1.126 g Iron (II) tetrafluoroborate hexahydrate 97% was solved into 5ml 99.8% ethanol.
  • the 0.435g CaCl 2 powder was solved into 5ml distilled water.
  • the 0.01 g Rhodamine B (for fluorescence) was solved in 10 ml distilled water.
  • the 1ml 25% Glutaraldehyde solution was mixed into 9 ml 99.8% ethanol. All chemicals above were purchased from Sigma-Aldrich, Switzerland.
  • microjet device In this project work, we fabricated 2 types of microjet device : one is with 3 inlets, while another has 5 inlets.
  • the microjet device was used to form controllable laminar flows by adjusting injection pressure at inlets. It works for us to confine the central flow stream between the side flows (such as Figure 4 A-B ).
  • 150 ⁇ l/min was regarded as optimized flow rate for all inlets, depending on properties of selected materials.
  • functional fibre with different structure design or functional properties could be produced.
  • hydrodynamic flow focusing technique with producing fibre, we can successfully fabricate hollow fibre, solid fibre, functional fibre (such as surface functionalization or materials filling into fibre).
  • Figs. 8a and 8b are schematic drawing showing two types of ⁇ -Jet devices.
  • One stainless tube with adjustable length was fixed at middle inlet. The adjustable length will help to control different flow mixing point between core flow and shell flows inside the device. Finally, all inlets and 1 outlet were connected with PTFE tubes.
  • the two types of microjet devices (3 inlets and 5 inlets) were fabricated and used for different aims.
  • the middle inlet is formed by a stainless tube with adjustable length.
  • the adjustable length of stainless tube will allow defining, i.e. positioning, the mixing point between core flow and shell flows inside system of microjet device.
  • the microjet device can be connected to syringe pumps through PTFE tubing.
  • Core flow rate ( ⁇ l/min) Shell flow rate 1 ( ⁇ l/min) Shell flow rate 2 ( ⁇ l/min) Flow rate ratio (Core vs.2 Shells) Fibre diameter ( ⁇ m) 1 150 150 150 2 220 to 330 2 150 300 300 4 130 to 170 3 150 600 600 8 50 to 80 4 150 1200 1200 16 20 to 30 5 150 2250 2250 30 15 to 20 6 150 3000 3000 40 10 to 15 7 150 3750 3750 50 5 to 10
  • the other available ⁇ -Jet device with 5 inlets and 1 outlet is useful for producing fibres with structure control.
  • the cross-sections of fresh alginate fibres with Rhodamine B fluorescence dye are shown in Figure 9 .
  • the core size of the hollow centre alginate fibre was varied by controlling the laminar flow rate ratio inside the system of 5 inlets ⁇ -Jet device as shown in Figure 10 :
  • A-B) 5 inlets ⁇ -Jet device was used to fabricate hollow alginate fibre with changing 5 inlets flow rate ratio.
  • the inlets 1, 4 and 5 were supplied with injected ethanol solution with increasing flow rate (from 150 ⁇ l/ min to 300 ⁇ l/ min). Meanwhile, the inlets 2 and 3 were supplied with injected alginate solution with constant flow rate at 150 ⁇ l/ min.
  • C-D) SEM images show two fabricated alginate fibre with different core size.
  • the inlets 2 and 3 were supplied with injected Alginate solution, while the inlets (1, 4 and 5) were supplied with injected Ethanol solution. All flow rates in 5 inlets were 150 ⁇ l/ min. Then, the core size of produced alginate fibre was approx. 31 ⁇ m ( Figure 10 C) . In contrast, if inlets 2 and 3 were supplied with injected Alginate solution with 150 ⁇ l/ min as each flow rate, while the inlets (1, 4 and 5) were supplied with injected Ethanol solution with 300 ⁇ l/ min as each flow rate, the core size of produced alginate fibre could be increased to 250 ⁇ m ( Figure 10 D) .
  • Figure 12 shows the visible difference while the Trizo-Fe 2+ crystals were formed at inside or outside of alginate fibre under optic microscope.
  • the 3 inlets ⁇ -Jet device in Figure 12-A
  • inlet 1 was supplied with injected Alginate-Trizo solution
  • inlets 2 and 3 were supplied with injected Fe 2+ solution.
  • Trizo-Fe 2+ crystals are formed at different locations on the alginate fibre (inside or outside).
  • a combination of SEM and EDX was used.
  • Trizo-Fe 2+ crystals were covered onto the surface of Alginate fibre.
  • Figures 13C and 13D show that the Trizo-Fe 2+ crystals were coated in core layer inside alginate fibre. Based on SEM images (B and D), we could easily observe a difference between the alginate surface and Trizo-Fe 2+ crystals coating layer.
  • the selected region 1 (Trizo-Fe 2+ crystals coating region) clearly show Fe 2+ element with higher percentage (around 40% of all elements).
  • the selected region 2 (Only alginate layer) barely shows any Fe 2+ element. That means, we can control Trizo-Fe 2+ crystals to be formed at selected regions (inside or outside of fibre) during the production of alginate fibre. It will be helpful to compare their physical difference in following tests.
  • Trizo-Fe 2+ crystals were synthesized on alginate fibre, and we next focused on the size of induvial Trizo-Fe 2+ crystal particles.
  • the mean diameter of induvial Trizo-Fe 2+ crystal particles on the surface of alginate fibre was 0.123 ⁇ 0.022 ⁇ m ( Figure 14 A)
  • the mean diameter of individual Trizo-Fe 2+ crystal particles on core layer inside alginate fibre was 0.103 ⁇ 0.021 ⁇ m ( Figure 14 B) .
  • Trizo-Fe 2+ crystal surface coating an alginate fibre was shown on a glass coverslip with designed graph by applying 3 inlets ⁇ -Jet device.
  • inlet 1 was supplied with injected Alginate-Trizo solution, while inlets 2 and 3 were supplied with injected Fe 2+ solution.
  • a fresh Trizo-Fe 2+ crystal surface coating Alginate fibre with white colour was produced ( Figure 15 B ).
  • the colour of the fibre had changed into red colour ( Figure 15 C ), due to the beginning of formation and reaction of Trizo-Fe 2+ crystals.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Textile Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Hematology (AREA)
  • Clinical Laboratory Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Multicomponent Fibers (AREA)
EP17165605.1A 2017-04-07 2017-04-07 Traitement microfluidique de fibres polymères Ceased EP3385413A1 (fr)

Priority Applications (2)

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EP17165605.1A EP3385413A1 (fr) 2017-04-07 2017-04-07 Traitement microfluidique de fibres polymères
PCT/EP2018/059066 WO2018185349A1 (fr) 2017-04-07 2018-04-09 Traitement microfluidique de fibres polymères

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1818432A2 (fr) 2004-03-22 2007-08-15 Universidad de Sevilla Procede destine a generer des nanotubes et des nanofibres composees a partir de jets coaxiaux
WO2009060202A1 (fr) * 2007-11-09 2009-05-14 Q Chip Limited Dispositif microfluidique et procédé de production d'un fluide gainé
US20110193259A1 (en) 2005-06-09 2011-08-11 The Government Of The United States Of America, As Represented By The Secretary Of The Navy Sheath flow device and method
CN103911678A (zh) * 2014-04-17 2014-07-09 华中科技大学 一种用于电流体喷印的同轴喷嘴
US8834780B2 (en) 2008-02-29 2014-09-16 Agency For Science, Technology And Research Hydrodynamic spinning of polymer fiber in coaxial laminar flows

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1818432A2 (fr) 2004-03-22 2007-08-15 Universidad de Sevilla Procede destine a generer des nanotubes et des nanofibres composees a partir de jets coaxiaux
US20110193259A1 (en) 2005-06-09 2011-08-11 The Government Of The United States Of America, As Represented By The Secretary Of The Navy Sheath flow device and method
WO2009060202A1 (fr) * 2007-11-09 2009-05-14 Q Chip Limited Dispositif microfluidique et procédé de production d'un fluide gainé
US8834780B2 (en) 2008-02-29 2014-09-16 Agency For Science, Technology And Research Hydrodynamic spinning of polymer fiber in coaxial laminar flows
CN103911678A (zh) * 2014-04-17 2014-07-09 华中科技大学 一种用于电流体喷印的同轴喷嘴

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