Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
  • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
  • B05B5/00—Electrostatic spraying apparatus; Spraying apparatus with means for charging the spray electrically; Apparatus for spraying liquids or other fluent materials by other electric means
  • B05B5/025—Discharge apparatus, e.g. electrostatic spray guns
  • B05B5/053—Arrangements for supplying power, e.g. charging power
  • B05B5/0533—Electrodes specially adapted therefor; Arrangements of electrodes
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
  • B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
  • B01J2/04—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a gaseous medium
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
  • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
  • B05B1/00—Nozzles, spray heads or other outlets, with or without auxiliary devices such as valves, heating means
  • B05B1/02—Nozzles, spray heads or other outlets, with or without auxiliary devices such as valves, heating means designed to produce a jet, spray, or other discharge of particular shape or nature, e.g. in single drops, or having an outlet of particular shape
  • B05B1/04—Nozzles, spray heads or other outlets, with or without auxiliary devices such as valves, heating means designed to produce a jet, spray, or other discharge of particular shape or nature, e.g. in single drops, or having an outlet of particular shape in flat form, e.g. fan-like, sheet-like
  • B05B1/044—Slits, e.g. narrow openings defined by two straight and parallel lips; Elongated outlets for producing very wide discharges, e.g. fluid curtains
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
  • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
  • B05B1/00—Nozzles, spray heads or other outlets, with or without auxiliary devices such as valves, heating means
  • B05B1/02—Nozzles, spray heads or other outlets, with or without auxiliary devices such as valves, heating means designed to produce a jet, spray, or other discharge of particular shape or nature, e.g. in single drops, or having an outlet of particular shape
  • B05B1/06—Nozzles, spray heads or other outlets, with or without auxiliary devices such as valves, heating means designed to produce a jet, spray, or other discharge of particular shape or nature, e.g. in single drops, or having an outlet of particular shape in annular, tubular or hollow conical form
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
  • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
  • B05B5/00—Electrostatic spraying apparatus; Spraying apparatus with means for charging the spray electrically; Apparatus for spraying liquids or other fluent materials by other electric means
  • B05B5/025—Discharge apparatus, e.g. electrostatic spray guns
  • B05B5/0255—Discharge apparatus, e.g. electrostatic spray guns spraying and depositing by electrostatic forces only
• • 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
  • B05B7/06—Spray pistols; Apparatus for discharge with at least one outlet orifice surrounding another approximately in the same plane
  • B05B7/061—Spray pistols; Apparatus for discharge with at least one outlet orifice surrounding another approximately in the same plane with several liquid outlets discharging one or several liquids
• • 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
  • B05B7/06—Spray pistols; Apparatus for discharge with at least one outlet orifice surrounding another approximately in the same plane
  • B05B7/062—Spray pistols; Apparatus for discharge with at least one outlet orifice surrounding another approximately in the same plane with only one liquid outlet and at least one gas outlet
  • B05B7/065—Spray pistols; Apparatus for discharge with at least one outlet orifice surrounding another approximately in the same plane with only one liquid outlet and at least one gas outlet an inner gas outlet being surrounded by an annular adjacent liquid outlet

Definitions

• Electrohydrodynamic atomization often called electrospray (ES)
• ES electrospray
• the technique enables the production of un-agglomerated, monodisperse particles of various materials with sizes ranging from micro-meter to nano-meter.
• a liquid meniscus at the exit of a capillary nozzle is subjected to an electrical stress, resulting from a divergent electrical field established between a spray head and a reference electrode. Due to the geometry of capillary nozzles, however, known ES systems have low mass throughput, which makes the feasibility of large scale implementation difficult.
• a nozzle for electrohydrodynamic atomization includes an inner rod, an outer tube concentrically aligned with the inner rod, an annular channel defined between the inner rod and the outer tube, the annular channel forming a circular slit at a spray end of the nozzle, and at least one electrically chargeable notch located on at least one of the inner rod and the outer tube proximate the circular slit.
• a system for electrohydrodynamic atomization includes a nozzle including a source end, a spray end, a first component including a first surface, a second component including a second surface, a fluid channel defined between the first surface and the second surface, the fluid channel forming an exit slit at the spray end of the nozzle (e.g., a circular exit slit, a planar or linear exit slit, etc.), and at least one electrically chargeable notch located on at least one of the first component and the second component proximate the exit slit.
• an exit slit e.g., a circular exit slit, a planar or linear exit slit, etc.
• the system may further include a voltage source electrically coupled to the nozzle and configured to supply a voltage to the at least one electrically chargeable notch, and a syringe pump in flow communication with the source end of the nozzle, the syringe pump configured to propel a spray liquid through the nozzle.
• a method for electrohydrodynamic atomization may use one or more of the nozzle configurations described herein.
• the method may include providing a nozzle including an inner rod, an outer tube concentrically aligned with the inner rod, an annular channel defined between the inner rod and the outer tube, the annular channel forming a circular slit at a spray end of the nozzle, and a plurality of notches located on at least one of the inner rod and the outer tube proximate the circular slit.
• the method further may include supplying a voltage to the plurality of notches, and pumping a spray liquid through the annular channel of the nozzle.
• Figure 1 is a schematic diagram of an exemplary electrospray system.
• Figure 2 is a cross-sectional view of an exemplary nozzle that may be used with the system of Figure 1.
• Figures 3 A and 3B are perspective views of exemplary nozzles that may be used with the system of Figure 1.
• Figures 4A and 4B are plan views of the exemplary nozzles of Figures 3B and 3B.
• Figures 5A-5C are images of exemplary nozzles that may be used with the system of Figure 1.
• Figures 6A-6L are cross-sectional views of exemplary nozzles that may be used with the system of Figure 1.
• Figure 7 is a graph that illustrates the applied voltage for establishing stable multi- jet operation for nozzles of various numbers of notches.
• Figures 8A-8C are graphs illustrating spray current as a function of applied voltage for nozzles with six, twelve, and twenty notches.
• Figure 9 is a graph that illustrates maximum liquid flowrate as a function of electrical conductivity of a spray liquid.
• Figure 10 is a graph illustrating a ratio of maximum liquid flowrate of a liquid sheet nozzle to the maximum liquid flowrate of a single-capillary nozzle.
• Figure 1 1 is a plan view of an exemplary nozzle that may be used with the system of Figure 1.
• Figure 12 is a perspective view of the exemplary nozzle shown in Figure 11.
• Embodiments provide electrohydrodynamic atomization using a liquid sheet to produce un-agglomerated, monodisperse droplets.
• nozzles with exit slit openings shape a spray liquid into a thin liquid sheet as the spray liquid exits from the slit opening.
• Stable multi-jet operation is achieved by including notches along the edge of the slit. The notches separate the liquid sheet into multiple jets to provide anchoring and stable multi-jet operation. That is, each notch anchors a corresponding jet by preventing the corresponding jet from migrating around the nozzle, substantially fixing the position of the corresponding jet.
• the liquid sheet electrospray techniques and nozzles described herein provide high mass throughput and versatile multiplexing spray systems while reducing the engineering effort and high
• System 100 includes a syringe pump 102, a nozzle 104, and a high-voltage source 106.
• syringe pump 102 is a Harvard Apparatus PHD2000 series pump.
• syringe pump 102 is any pump that enables system 100 to function as described herein.
• High-voltage source 106 is coupled to nozzle 104 such that high-voltage source 106 enables a voltage to be applied to a spray end 108 of nozzle 104.
• high-voltage source 106 provides a voltage ranging from 13kV to 16 kV to spray end 108.
• high- voltage source may apply any voltage to nozzle 104 that enables system 100 to function as described herein.
• System 100 also includes a monitoring system 1 10.
• Monitoring system 110 includes a microscopic lens 112, a digital camera 114, a monitor 1 16, and a computer 1 18, which enable monitoring system 110 to monitor the spray produced by nozzle 104.
• System 100 also includes a current system 120.
• Current system 120 includes a multimeter 122 electrically coupled to a ground 124 and electrically coupled to ring 126 across a resistor 128. By measuring the voltage across resistor 128, current system 120 can measure the current of the spray produced by nozzle 104. Through multimeter 122, ring 126 is also electrically coupled to ground 124.
• FIG. 2 is a cross-sectional view of an exemplary nozzle 200 that may be used with system 100.
• Nozzle 200 includes a source end 202 and a spray end 204.
• Nozzle 200 includes an inner rod 206 coaxially aligned with an outer tube 208 along a longitudinal axis 210 of nozzle 200.
• An annular flow channel 212 is defined between an inner surface 214 of outer tube 208 and an outer surface 216 of inner rod 206.
• annular flow channel 212 becomes a circular slit 218.
• an inner diameter 220 of circular slit 218 is 2,950 ⁇
• an outer diameter 222 of circular slit 218 is 3,250 ⁇ , such that a width 224 of circular slit 218 is 150 ⁇ .
• circular slit 218 may have any dimensions that enable nozzle 200 to function as described herein.
• syringe pump 102 applies a pressure to a spray liquid, such that the spray liquid is pushed towards nozzle 200 and received at source end 202 of nozzle 200.
• the spray liquid is then evenly distributed into annular flow channel 212 and emitted from circular slit 218 as a thin liquid sheet.
• the emitted liquid sheet is substantially cylindrical.
• Nozzle 200 further includes one or more notches 230 proximate to circular slit 218.
• a "notch" refers to a protruding element that extends from a spray end of a nozzle, such as notches 230 extending from spray end 204 of nozzle 200.
• such notches may extend or protrude further in the direction of the spray jet than other regions of the spray end separating such notches.
• notches 230 are located on both inner rod 206 and outer tube 208.
• notches 230 may be located only on inner rod 206 or outer tube 208.
• the shape and configuration of notches 230 facilitate local enhancement of an electric field at notches 230.
• the spray liquid reaches the circular slit 218, it exits nozzle 200 as a thin liquid sheet due to the shape of annular flow channel 212.
• the thin liquid sheet is separated into multiple jets. Each jet is located at one of notches 230 due to the locally intensified electric field at each notch 230.
• stable multi-jet operation means that a jet of spray liquid is emitted from each notch 230 on nozzle 200.
• Figures 3 A and 3B are perspective views of exemplary nozzles 200 that may be used with the system of Figure 1.
• Figures 4A and 4B are plan views of the nozzles 200 shown in Figures 3A and 3B.
• the embodiment shown in Figures 3A and 4A includes six notches 230, and the embodiment shown in Figures 3B and 4B includes twenty notches 230.
• Notches 230 are circumferentially spaced apart from one another by a circumferential distance, 240.
• circumferential distance 240 is no less than a size of a notch 230.
• Circumferential distance 240 is chosen such that the number of notches 230 is maximized while maintaining regions of intensified electric field. That is, if circumferential distance 240 between notches 230 is too small, the electric field generated at one notch 230 will interfere with the electric field generated at an adjacent notch 230. However, as the circumferential distance 240 between notches 230 increases, fewer notches 230 can be located on nozzle 200. With fewer notches 230, fewer jets are created, and the overall mass throughput of nozzle 200 is decreased.
• Figures 5A-5C are images of nozzles 200 producing multiple jets 250 of a spray liquid.
• the nozzles 200 in Figures 5A, 5B, and 5C include six, twelve, and twenty notches 230, respectively.
• Figures 6A-6L are cross-sectional views of exemplary nozzles 300 that may be used with the system of Figure 1. As demonstrated by the embodiments shown in Figures 6A- 6L, several different configurations of nozzle 300 enable nozzle 300 to function as described herein. Moreover, configurations of nozzle 300 are not limited to those specifically described herein.
• Each nozzle 300 in Figures 6A-6L includes a source end 302 and a spray end 304. Further, each nozzle 300 includes an inner rod 306 coaxially aligned with an outer tube 308 along a longitudinal axis 310 of nozzle 300. An annular flow channel 312 is defined between an inner surface 314 of outer tube 308 and an outer surface 316 of inner rod 306. At spray end 304, annular flow channel 312 becomes a circular slit 318. Further, at spray end 304, inner rod 306 includes a center piece 320, and outer tube 308 includes an end portion 322. Each nozzle 300 also includes a plurality of notches 330 which function substantially similar to notches 230 shown in Figure 2. The embodiments of Figures 6A-6L are each discussed in detail below.
• both inner rod 306 and outer tube 308 includes notches 330 thereon. Further, center piece 320 is not retracted or extended with respect to end portion 322. During operation of the embodiment shown in Figure 6A, a spray liquid is emitted from circular slit 318.
• outer tube 308 includes notches 330 thereon. That is, inner rod 306 does not include notches 330. Further, center piece 320 is retracted with respect to end portion 322. During operation of the embodiment shown in Figure 6B, the spray liquid is emitted from circular slit 318.
• the embodiment of nozzle 300 shown in Figure 6C is substantially similar to the embodiment shown in Figure 6A, except that the embodiment shown in Figure 6C includes a central flow channel 340 defined through inner rod 306.
• the embodiment of nozzle 300 shown in Figure 6D is substantially similar to the embodiment shown in Figure 6B, except that the embodiment shown in Figure 6D includes central flow channel 340 defined through inner rod 306.
• a stabilizing gas is emitted from central flow channel 340. The emitted gas facilitates maintaining the thin liquid sheet shape of the spray liquid when the spray liquid is emitted from circular slit 318.
• nozzle 300 shown in Figures 6E and 6F are substantially similar to the embodiments shown in Figures 6C and 6D respectively, except that instead of a stabilizing gas, a stabilizing liquid is emitted from central flow channel 340. Similar to the stabilizing gas, the stabilizing liquid facilitates maintaining the thin liquid sheet shape of the spray liquid when the spray liquid is emitted from circular slit 318.
• the embodiment of nozzle 300 shown in Figure 6G is substantially similar to the embodiment shown in Figure 6F, except that center piece 320 is extended with respect to end potion 322.
• FIG. 6H and 61 The embodiments of nozzle 300 shown in Figures 6H and 61 are substantially similar to the embodiments shown in Figures 6C and 6D respectively, except that the embodiments of Figures 6H and 61 further include a second outer tube 350.
• Second outer tube 350 is concentrically aligned with outer tube 308 such that a second annular flow channel 352 is defined between an outer surface 354 of outer tube 308 and an inner surface 356 of second outer tube 350.
• Second annular flow channel 352 becomes a second circular slit 360 at spray end 304.
• second outer tube 350 includes notches 330 thereon.
• a sheath liquid is emitted from second circular slit 360 in a thin liquid sheet shape.
• particle encapsulation is facilitated, such that the particles produced by nozzle 300 include particles of spray liquid encapsulated by particles of sheath liquid and/or particles of sheath liquid encapsulated by particles of spray liquid.
• a stabilizing gas emitted from central flow channel 340 facilitates maintaining the thin liquid sheet shape of the spray liquid and the sheath liquid.
• a stabilizing liquid may be emitted from central flow channel 340.
• the embodiment shown in Figure 6J is substantially similar to the embodiment shown in Figure 61, except that the center piece 320 is extended with respect to end portion 322.
• the embodiment of nozzle 300 shown in Figure 6K is substantially similar to the embodiment shown in Figure 6H, except that the embodiment of Figure 6K further includes a third outer tube 370.
• Third outer tube 370 is concentrically aligned with second outer tube 350 such that a third annular flow channel 372 is defined between an outer surface 374 of second outer tube 350 and an inner surface 376 of third outer tube 370.
• Third annular flow channel 372 becomes a third circular slit 380 at spray end 304.
• third outer tube 370 includes notches 330 thereon.
• an outer liquid is emitted from third circular slit 380 in a thin liquid sheet shape.
• the emission of liquids from first circular slit 318, second circular slit 360, and third circular slit 380 facilitates particle encapsulation and the production of multi- layered particles.
• a stabilizing gas emitted from central flow channel 340 facilitates maintaining the thin liquid sheet shape of the emitted liquids.
• a stabilizing liquid may be emitted from central flow channel 340.
• the embodiment shown in Figure 6L is substantially similar to the embodiment shown in Figure 6K, except that the circular slits 318, 360, and 380 are arranged in a stepped configuration, such that outer tube 308 is extended with respect to second outer tube 350, and second outer tube 350 is extended with respect to third outer tube 370. Due to the stepped configuration, less voltage may be applied to the embodiment shown in Figure 6L than the embodiment shown in Figure 6K to achieve stable multi-jet operation.
• the outer liquid emitted from third circular slit 380 may be the same liquid as at least one of the spray liquid emitted from first circular slit 318 and the sheath liquid emitted from second circular slit 360.
• the spray liquid, the sheath liquid, and the outer liquid may all be different liquids.
• certain flow channels are denoted as containing a gas or a liquid, alternatively, any suitable fluid (i.e., gas, liquid) may be provided in any flow channel that enables nozzle 300 to function as described herein.
• Figure 7 is a graph that illustrates the applied voltage for establishing stable multi- jet operation for nozzles having various numbers of notches. The graph demonstrates that the applied voltage increases with the number of notches. It was also determined that the applied voltage for establishing stable multi-jet operation is also slightly proportional to the feed flowrate of the spray liquid.
• FIGS. 8A-8C are graphs illustrating the spray current as a function of the applied voltage for nozzles with six, twelve, and twenty notches, respectively.
• the spray current and the number of jets increased with the increase of applied voltage.
• the stable multi-jet operation in which the number of jets is the same as the number of notches, was achieved at a sufficiently high applied voltage.
• the applied voltage was reduced, the number of jets correspondingly decreased. Further, as shown in the graphs, a hysteresis phenomenon was observed.
• FIG. 9 is a graph that illustrates the maximum liquid flowrate as a function of the electrical conductivity of the spray liquid.
• the graph demonstrates that the value of Qmax significantly decreases as the electrical conductivity of the spraying liquid increases, due to the fact that spray liquids with higher electrical conductivity generally use a stronger electric field to establish stable multi-jet operation.
• the graph also demonstrates that Qmax increases as the number of notches increases. This is because a greater number of notches allow more jets to be established, thus increasing the spray liquid flowrate and the overall mass throughput.
• Figure 10 is a graph illustrating a ratio of the maximum liquid flowrate of the liquid sheet nozzles described herein to the maximum liquid flowrate of a known single- capillary nozzle as a function of the electrical conductivity of the spray liquid.
• the diameter of the single-capillary nozzle and the width of the circular slit in the liquid sheet nozzle were both 150 ⁇ .
• the maximum liquid flowrate, Qmax, of the liquid sheet nozzle with 20 notches was one hundred and sixty-six times greater than the maximum liquid flowrate for the single-capillary nozzle.
• the maximum liquid flowrate of the liquid sheet nozzle with twenty notches was seventy times greater than the maximum liquid flowrate for the single-capillary nozzle.
• the value of Qmax for a liquid sheet nozzle with twenty notches is much higher than the sum of the total liquid flowrates for twenty single-capillary nozzles.
• This same phenomenon was also observed using liquid sheet nozzles with six and twelve notches. This indicates that, as compared to existing one-dimensional and two-dimensional arrays of single- capillary nozzles, liquid sheet nozzles have potential to drastically increase the mass throughput for spray liquids having a wide range of electrical conductivity.
• FIG. 1 1 is a plan view of an alternative nozzle 500 that may be used with system 100.
• Figure 12 is a perspective view of nozzle 500 shown in Figure 11.
• nozzle 500 includes a first plate 502, a second plate 504, a source end 506, and a spray end 508.
• a planar flow channel 510 is defined between first plate 502 and second plate 504. Planar flow channel 510 becomes a linear slit 512 at spray end 508.
• a spray liquid is emitted from nozzle 500 from linear slit 512. While the thin liquid sheet emitted from nozzle 200 is substantially cylindrical, the thin liquid sheet emitted from nozzle 500 is substantially planar.
• a plurality of notches 514 are located on both first plate 502 and second plate 504, and staggered with respect to one another.
• notches 514 may only be located on one of first plate 502 and second plate 504. With a voltage applied to notches 514, notches 514 facilitate separating the thin liquid sheet into a plurality of jets, substantially similar to notches 230 of nozzle 200.
• the nozzles illustrated in Figures 1-6L, 11, and 12 constitute exemplary means for emitting a liquid sheet. Further, the notches illustrated in Figures 2-6L, 11, and 12 constitute exemplary means for separating a liquid sheet emitted by a nozzle into multiple jets. Moreover, nozzles illustrated in Figures 6C-6L constitute exemplary means for maintaining a shape of a liquid sheet emitted from a nozzle.
• Embodiments described herein enable electrohydrodynamic atomization, or electrospray (ES), using nozzles that produce a thin liquid sheet.
• the methods and systems described herein increase the mass throughput of ES systems while decreasing the design and manufacturing costs as compared to known ES systems utilizing multiple single-capillary nozzles.
• the nozzles described herein include annular and/or planar slits designed emit a thin liquid sheet of spray liquid. To separate the thin liquid sheet into multiple jets and to anchor the jets for stable operation, a plurality of notches are included at the annular and/or planar slits.
• each notch anchors a corresponding jet by preventing the corresponding jet from migrating around the nozzle, substantially fixing the position of the corresponding jet.
• these notches enable local enhancement of an electric field. Further, stable multi-jet operation of the nozzles described herein can be established for a wide range of spray liquids having various electrical conductivities.
• the maximum flowrate for liquid sheet nozzles with various numbers of notches was consistently greater than the total flowrate sum of an array of an equivalent number of single-capillary nozzles. Accordingly, the liquid sheet nozzles described herein enable superior ES techniques. Further, the liquid sheet shape of the spray liquid, as opposed to the cone jet emitted from known single-capillary nozzles, enables the nozzle design to have various geometries, including, but not limited to annular and/or planar slits.

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• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Electrostatic Spraying Apparatus (AREA)
• Nozzles (AREA)
• Glanulating (AREA)

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• 2012
  • 2012-01-18 EP EP12736538.5A patent/EP2665559B1/en not_active Not-in-force
  • 2012-01-18 US US13/979,260 patent/US10562048B2/en active Active
  • 2012-01-18 WO PCT/US2012/021723 patent/WO2012099961A2/en not_active Ceased
  • 2012-01-18 CA CA2824930A patent/CA2824930A1/en not_active Abandoned
  • 2012-01-18 JP JP2013550564A patent/JP5961630B2/ja not_active Expired - Fee Related
• 2020
  • 2020-02-13 US US16/789,865 patent/US20200179963A1/en not_active Abandoned
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