WO2007146703A2 - Émulsification de dispersions concentrées de particules colloïdales et de nanoparticules - Google Patents

Émulsification de dispersions concentrées de particules colloïdales et de nanoparticules Download PDF

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Publication number
WO2007146703A2
WO2007146703A2 PCT/US2007/070493 US2007070493W WO2007146703A2 WO 2007146703 A2 WO2007146703 A2 WO 2007146703A2 US 2007070493 W US2007070493 W US 2007070493W WO 2007146703 A2 WO2007146703 A2 WO 2007146703A2
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WIPO (PCT)
Prior art keywords
emulsion
shear thickening
fluid
stf
thickening fluid
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Ceased
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PCT/US2007/070493
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English (en)
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WO2007146703A3 (fr
Inventor
Norman J. Wagner
Caroline H. Nam
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UD Technology Corp
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UD Technology Corp
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Publication of WO2007146703A2 publication Critical patent/WO2007146703A2/fr
Publication of WO2007146703A3 publication Critical patent/WO2007146703A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
    • D06M23/08—Processes in which the treating agent is applied in powder or granular form
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F41—WEAPONS
    • F41H—ARMOUR; ARMOURED TURRETS; ARMOURED OR ARMED VEHICLES; MEANS OF ATTACK OR DEFENCE, e.g. CAMOUFLAGE, IN GENERAL
    • F41H1/00—Personal protection gear
    • F41H1/02—Armoured or projectile- or missile-resistant garments; Composite protection fabrics

Definitions

  • Shear thickening fluids are fluids whose viscosity increases with shear rate.
  • discontinuous STFs which at high shear rates transform into a material with solid-like properties.
  • a typical example of a discontinuous STF is a stabilized suspension of rigid colloidal particles with a high loading fraction of particles.
  • Such systems have been studied for many different combinations of fluid matrix and particle size and compositions (Egres, R.G., Lee, Y. S., Kirkwood, J.E., Kirkwood, K.M., Wetzel, E.D., and Wagner, NJ., "Novel flexible body armor utilizing shear thickening fluid composites.” Proceedings of 14 th International Conference on Composite Materials. San Diego, CA.
  • the shear thickening in the colloidal suspension is due to the formation of jamming clusters, or hydroclusters, (Lee, Y.S., Wagner, N.J., "Dynamic properties of shear thickening colloidal suspensions," Rheol Acta 42,199-208 (2003)) bound together by hydrodynamic lubrication forces.
  • the hydrocluster growth and collision eventually result in a percolated arrangement of the rigid particles across macroscopic dimension. This microstructural transformation leads to the bulk solid-like behavior.
  • the rigidized material Upon relaxation of the applied stresses, the rigidized material typically relaxes to the low strain rate, fluid-like behavior (Eric D. Wetzel, Y. S, Lee, R. G. Egres, K. M.
  • Shear-thickening fluids have been shown to have utility in the fabrication of energy dissipative devices, such as shock absorbers (Hesse, H., US Pat. No. 4,503,952), (Rosenberg, B.L., US Pat. No. 3,833,952), (Sheshimo, K., US Pat. No. 4,759,428) and more recently in the fabrication of ballistic fabric composites (Egres, R.G., Lee, Y.S., Kirkwood, J.E., Kirkwood, K.M., Wetzel, E.D., and Wagner, N. J., "Novel flexible body a ⁇ nor utilizing shear thickening fluid composites.” Proceedings of 14 th International Conference on Composite Materials. San Diego, CA.
  • shear thickening fluid is defined as any fluid that exhibits an increase in viscosity with increasing shear rate or applied stress.
  • Shear thickening is not shear dilatancy, which is a material property whereby the material's volume changes upon an applied stress or deformation. Shear thickening fluids, however, may exhibit dilatancy under specific conditions.
  • Emulsions of two immiscible or partially miscible fluids have been extensively explored in several areas of research.
  • Shear thickening "suspoemulsions” have been developed in a previous patent application (Wagner, Egres, Kirkwood, 2004 (U.S. Serial Number 11/260,742 which is incorporated by reference in its entirety for all useful).
  • STFs shear thickening fluids
  • Novel methods to emulsify dispersions into an immiscible or partially miscible carrier fluid are described in this patent application.
  • Typical processing of STF-fabric composites involves the use of copious amounts of a volatile solvent that can solubilize the STF, i.e., a co-solvent, such as ethanol (see prior art) to dilute the STF (approximate 50% by vol. silica particles dispersed in a polymeric matrix such as silicone oil).
  • a co-solvent such as ethanol (see prior art) to dilute the STF (approximate 50% by vol. silica particles dispersed in a polymeric matrix such as silicone oil).
  • ethanol not only poses potentially serious health and safety risks but also introduces process design challenges due to fire safety and VOC regulations.
  • the use of a co-solvent poses problems in that the particles can sediment out of the diluted solution, or the co-solvent may induce particle aggregation or precipitation.
  • ethanol is currently used in its present technology due to its benefits in STF-fabric processing: STF easily dissolves in ethanol and thus allows for ease in coating and manufacturing; ethanol can easily be removed to leave behind only STF in fabrics.
  • the use of water instead of ethanol would eliminate any safety or health hazards.
  • STFs are formulated with water insoluble or sparingly water soluble carrier fluids, water cannot be directly used as a co-solvent to dilute the STF.
  • the challenge is to develop a method whereby a STF can be emulsified as a dispersed phase in an aqueous solution.
  • An emulsion refers to a state of matter whereby a fluid phase, which may contain multiple components including particles, polymer, and or surfactants, is dispersed as droplets in an insoluble or sparingly soluble fluid. Further, the subsequent challenge is to maintain the stability of the emulsion as well as the integrity of the STF phase upon drying or separation of the aqueous carrier fluid. Neither of these specific challenges has been addressed in the literature.
  • This invention is a new process that was inspired by the need to improve coating conditions of shear thickening fluids to materials such as conventional body armor or ballistic material or commercial materials such as polyolefms, nylons and polyesters.
  • Conventional body armor materials are typically comprised of many layers of polyaramid poly(phenylene diamine terephthalamide) fabric, sold by DuPont under the registered name of KEVLAR®, with optional ceramic tile inserts.
  • An object of this invention enables coating of STFs into fabrics, such as required in continuous manufacturing of materials.
  • the most significant limitation is the stability of the emulsions. Coalescence and sedimentation can occur on the timescale of the use of the emulsion. However, stability can be improved by the use of various surface active agents, such as surfactants, polymers, particles or by changing the blending conditions or composition.
  • This invention has immediate applications in improving the manufacture of body armor composites as described above.
  • the invention also has implications in the fields of dispersion science, colloid science, emulsion science, and food science.
  • the most significant current limitation is the stability of the emulsions.
  • stability can be improved by conducting more experiments with various surfactants and other stabilizing agents, different formulations, and variations in processing conditions.
  • the methods can also entail the use of a co-solvent for the STF such as, but not limited to heptane, toluene, or alcohols to lower the viscosity of the particle dispersion and a surfactant dissolved in an immiscible carrier fluid, such as water.
  • a co-solvent for the STF such as, but not limited to heptane, toluene, or alcohols to lower the viscosity of the particle dispersion and a surfactant dissolved in an immiscible carrier fluid, such as water.
  • a co-solvent for the STF such as, but not limited to heptane, toluene, or alcohols to lower the viscosity of the particle dispersion and a surfactant dissolved in an immiscible carrier fluid, such as water.
  • Different techniques can be used to achieve an emulsion: sonication and/or mechanical mixing, or the use of microfluidic devices or 3 -way
  • Figure 1 Images of the A) Heptane STF mixture, B) Water-surfactant mixture, C)
  • the emulsification process of water and STF was found to require a pre-treatment of the highly viscous fluid and certain amount of energy that can be achieved from an ultrasonic bath, horn sonication, or heavy duty blending.
  • the preferred surfactants are those that have a suitable hydophilic/lyophilic balance (HLB), preferably from 8 to 18 and more preferably typically around 15.
  • HLB hydophilic/lyophilic balance
  • Other nonionic, anionic, cationic or zwitterionic surfactant suitable for forming aqueous emulsions of insoluble oils may be used depending upon the specific STF carrier fluid composition.
  • nonionic, anionic, or cationic polymers may also be employed, again depending on the specific STF carrier fluid composition.
  • Stability can also be achieved through the use of particles, commonly known as a picker ing emulsion. These particles may be the same as those comprising the STF, or may be specifically chosen to stabilize the oil-water interface.
  • Other "Surfactants can be chosen from among those recommended by standard industrial practice handbooks, such as Flick "Industrial Surfactants”.
  • the surfactant In the case of a water like system, the surfactant would have an HLB of about 8 to about 20, preferably around 15. In the case of an oil like system, the surfactant would have an HLB of about 3 to about 8, (See Kirk-Othmer Encyclopedia of Chemical Technology, "Emulsions” by Edward Kostartsek, Rohm and Haas Co.,Copyright ⁇ 2003 by John Wiley & Sons, ⁇ ncDOI:
  • Water like would include water and aqueous soluble solvents such as alcohols.
  • the materials that can be used are conventional body armor or ballistic material.
  • Conventional body armor materials are typically comprised of many layers of polyaramid poly(phenylene diamine terephthalamide) fabric, sold by DuPont under the registered name of KEVLAR®, with optional ceramic tile inserts.
  • Reactive polymers include polyurethanes that cure through the chemical reaction of components (polyols and isocyanates), epoxies that cure through the addition of a catalyst, and UV curable resins.
  • a preferred second material of this type would be from the class of elastomeric or elastomeric gel materials, such as silicone rubber (cross-linked PDMS) or silicone gels and the like, which can be relatively low viscosity liquids prior to cross-linking, whereafter they form resilient materials with good rebound characteristics.
  • elastomers exist to provide a wide range of properties such as chemical and solvent resistance, temperature resistance, and hardness (durometer).
  • the liquid-like second material could subsequently be cured, or the curing could be accelerated through heating or the addition of additional components that catalyze the reaction and transform the second material into a solid. Curing could be accomplished by UV. Further, the liquid could be gelled by physical and or chemical crosslinking of polymers or by the addition of structure forming agents, such as fumed silica.
  • melt processable polymers include but are not limited to polyolefins such as polyethylene and polypropylene, nylon, polymethylmethacrylate, polyvinylchloride, polyethylene, polyesters such as but not limited to terephthalate (PET), polycarbonate and the like.
  • Thermoplastic elastomers would include such as materials as those sold under the trade names SantopreneTM (Exxon Mobil Chemical), Hytrel® (DuPont Company), and Engage TM from DuPont-Dow Elastomers. In this instance, increased temperature is used to liquefy a polymeric material.
  • the shear thickening fluid would be compounded with the polymer meJt to achieve the desired level of mixing and microstructure. The temperature would subsequently be reduced to generate the solid polymer-shear thickening fluid composite.
  • the pre-treatment of the STF involved dissolving the STF in a co-solvent such as but not limited to alcohol, alkanes, such as heptane and hexane, or toluene. Any soluble or partially material that does not adversely affect the STF properties can be employed.
  • a co-solvent such as but not limited to alcohol, alkanes, such as heptane and hexane, or toluene. Any soluble or partially material that does not adversely affect the STF properties can be employed.
  • This boiling point of this co-solvent needs to be lower than the boiling point of the solvent component of the STF, which in this case, is a silicone oil.
  • the amount of co- solvent should also be minimized, but sufficient to enable the STF to be emulsified.
  • a preferred amount of co-solvent is around 10% by volume in order to avoid any significant processing issues and to ease the evaporation of the co-solvent.
  • 150 niL of STF (50% 450nm silica particles (Shokubai, KEP- 50, Nissan Chemical) dispersed in polytrimethicone(PTM-20, ISP, Inc.) and 15 mL of heptane (reagent grade, Fischer Scientific) were mixed by hand-shaking the container for 1 minute and subsequently, placing the container on a roll-mixer for 10 minutes.
  • a surfactant Pluronic L64, BASF
  • the stock solution was placed in the ultrasonic bath for 1 hour under heating to 35 0 C.
  • the emulsion as prepared was placed in a dip coating pan for STF-fabric manufacturing.
  • a standard procedure, previously published was followed.
  • the fabric used was a 15"xl5" sheet of Twaron (1011-123.0-1002, provided by Barrday, Inc.). The fabric was submerged in the emulsion for 1 minute and then drawn through a set of 2 rubber nip-rollers to remove excess fluid.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

La présente invention concerne un procédé d'application d'un fluide épaississant par cisaillement sur un matériau, ledit procédé comprenant l'émulsification de dispersions d'un fluide épaississant par cisaillement (STF, shear thickening fluid) dissous dans un fluide vecteur miscible ou un fluide vecteur partiellement miscible pour former une émulsion, et l'application de ladite émulsion sur le matériau. L'invention concerne en outre une émulsion-suspension contenant un fluide épaississant par cisaillement émulsifié dans un solvant volatil. L'invention concerne également une méthode de revêtement d'un matériau. L'invention concerne en outre une méthode de revêtement d'un matériau à l'aide de l'émulsion-suspension.
PCT/US2007/070493 2006-06-06 2007-06-06 Émulsification de dispersions concentrées de particules colloïdales et de nanoparticules Ceased WO2007146703A2 (fr)

Applications Claiming Priority (2)

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US81133906P 2006-06-06 2006-06-06
US60/811,339 2006-06-06

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WO2007146703A2 true WO2007146703A2 (fr) 2007-12-21
WO2007146703A3 WO2007146703A3 (fr) 2008-06-26

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010093632A1 (fr) * 2009-02-10 2010-08-19 Orthoaccel Technologies, Inc. Plaque dentaire vibrante et accessoires
CN103359740A (zh) * 2012-03-27 2013-10-23 浩华科技实业有限公司 一种二氧化硅剪切增稠液的制备方法
US8636506B2 (en) 2008-06-23 2014-01-28 OrthAccel Technologies, Inc. Differential vibration of dental plate
US9028250B2 (en) 2007-03-14 2015-05-12 Orthoaccel Technologies, Inc. Vibrating dental devices
JP2019500060A (ja) * 2015-12-21 2019-01-10 モンサント テクノロジー エルエルシー 導入遺伝子の効率的な標的指向化のための構成物及び方法
US10188159B2 (en) 2013-10-25 2019-01-29 Armour Technologies, Inc. Apparatus, system, and method for reducing head or neck trauma
US10347934B2 (en) 2014-09-26 2019-07-09 Ut-Battelle, Llc Shear activated impact resistant electrolyte
US10347945B2 (en) 2017-12-08 2019-07-09 Ut-Battelle, Llc Stabilized shear thickening electrolyte
US10500019B2 (en) 2007-03-14 2019-12-10 Orthoaccel Technologies, Inc. System and method for correcting malocclusion
US10637100B2 (en) 2018-04-20 2020-04-28 Ut-Battelle, Llc Fabrication of films and coatings used to activate shear thickening, impact resistant electrolytes
US12567600B2 (en) 2023-12-14 2026-03-03 Safire Technology Group, Inc. Systems and methods for enhancing safety of electrochemical cells via electrolyte thickening

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1217446A (en) * 1968-06-07 1970-12-31 Sherwin Williams Co Dilatant latex
ES2346743T3 (es) * 2001-09-13 2010-10-20 Daniel James Plant Material flexible absorbente de energia y procedimientos de fabricacion del mismo.
US7226878B2 (en) * 2003-05-19 2007-06-05 The University Of Delaware Advanced body armor utilizing shear thickening fluids
US20060234572A1 (en) * 2004-10-27 2006-10-19 Ud Technology Corporation Shear thickening fluid containment in polymer composites

Cited By (24)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10500019B2 (en) 2007-03-14 2019-12-10 Orthoaccel Technologies, Inc. System and method for correcting malocclusion
US9028250B2 (en) 2007-03-14 2015-05-12 Orthoaccel Technologies, Inc. Vibrating dental devices
US11806206B2 (en) 2007-03-14 2023-11-07 Dentsply Sirona Inc. System and method for correcting malocclusion
US10806545B2 (en) 2007-03-14 2020-10-20 Advanced Orthodontics And Education Assiocation, Llc System and method for correcting malocclusion
US8636506B2 (en) 2008-06-23 2014-01-28 OrthAccel Technologies, Inc. Differential vibration of dental plate
US8708701B2 (en) 2009-02-10 2014-04-29 Orthoaccel Technologies, Inc. Vibrating dental plate and accessories
WO2010093632A1 (fr) * 2009-02-10 2010-08-19 Orthoaccel Technologies, Inc. Plaque dentaire vibrante et accessoires
CN103359740A (zh) * 2012-03-27 2013-10-23 浩华科技实业有限公司 一种二氧化硅剪切增稠液的制备方法
US10188159B2 (en) 2013-10-25 2019-01-29 Armour Technologies, Inc. Apparatus, system, and method for reducing head or neck trauma
US10827786B2 (en) 2013-10-25 2020-11-10 Armour Technologies, Inc. Apparatus, system, and method for reducing head or neck trauma
US12144387B2 (en) 2013-10-25 2024-11-19 Armour Technologies, Inc. Apparatus, system, and method for reducing head or neck trauma
US11596187B2 (en) 2013-10-25 2023-03-07 Armour Technologies, Inc. Apparatus, system, and method for reducing head or neck trauma
US10347934B2 (en) 2014-09-26 2019-07-09 Ut-Battelle, Llc Shear activated impact resistant electrolyte
JP2019500060A (ja) * 2015-12-21 2019-01-10 モンサント テクノロジー エルエルシー 導入遺伝子の効率的な標的指向化のための構成物及び方法
US10563220B2 (en) 2015-12-21 2020-02-18 Monsanto Technology Llc Compositions and methods for efficient targeting of transgenes
EP3394272A4 (fr) * 2015-12-21 2019-07-31 Monsanto Technology LLC Compositions et procédés permettant de cibler efficacement des transgènes
EP4219729A3 (fr) * 2015-12-21 2023-09-27 Monsanto Technology LLC Compositions et procédés pour le ciblage efficace de transgènes
US10347945B2 (en) 2017-12-08 2019-07-09 Ut-Battelle, Llc Stabilized shear thickening electrolyte
US10637100B2 (en) 2018-04-20 2020-04-28 Ut-Battelle, Llc Fabrication of films and coatings used to activate shear thickening, impact resistant electrolytes
US11824163B2 (en) 2018-04-20 2023-11-21 Ut-Battelle, Llc Method of making a passively impact resistant battery
US11824162B2 (en) 2018-04-20 2023-11-21 Ut-Battelle, Llc Battery with shear thickening, impact resistant electrolytes
US11233271B2 (en) 2018-04-20 2022-01-25 Ut-Battelle, Llc Fabrication of films and coatings used to activate shear thickening, impact resistant electrolytes
US12237469B2 (en) 2018-04-20 2025-02-25 Ut-Battelle, Llc Battery with shear thickening, impact resistant electrolytes
US12567600B2 (en) 2023-12-14 2026-03-03 Safire Technology Group, Inc. Systems and methods for enhancing safety of electrochemical cells via electrolyte thickening

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