WO2015041612A1 - Procédé d'ajustement du coefficient de frottement du polyfluorure de vinylidène (pvdf) - Google Patents

Procédé d'ajustement du coefficient de frottement du polyfluorure de vinylidène (pvdf) Download PDF

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Publication number
WO2015041612A1
WO2015041612A1 PCT/SI2014/000052 SI2014000052W WO2015041612A1 WO 2015041612 A1 WO2015041612 A1 WO 2015041612A1 SI 2014000052 W SI2014000052 W SI 2014000052W WO 2015041612 A1 WO2015041612 A1 WO 2015041612A1
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mos
pvdf
friction
nanotube
nanotubes
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PCT/SI2014/000052
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English (en)
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Maja REMŠKAR
Janez JELENC
Andrej KRŽAN
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Institut "Jožef Stefan"
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/22—Expanded, porous or hollow particles
    • C08K7/24—Expanded, porous or hollow particles inorganic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/005—Reinforced macromolecular compounds with nanosized materials, e.g. nanoparticles, nanofibres, nanotubes, nanowires, nanorods or nanolayered materials
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08J2327/16—Homopolymers or copolymers of vinylidene fluoride
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
    • C08K2003/3009—Sulfides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/30—Sulfur-, selenium- or tellurium-containing compounds

Definitions

  • This disclosure provides three-dimensional and thin film morphologies of fluoro-polymer nanocomposites with adjusted friction properties, which contain inorganic nanomaterials as low-friction additives.
  • this disclosure provides Polyvinylidene fluoride (PVDF) based polymers, which contain MoS 2 -based nanomaterials and the method of adjusting friction properties of PVDF based polymers.
  • PVDF Polyvinylidene fluoride
  • the present invention relates generally to the field of polymer nanocomposites and more particularly to methods of adjusting the physical properties of thermoplastic high- performance fluoro-polymers, and especially friction properties of Polyvinylidene fluoride based polymers with use of MoS 2 -based nanotubes
  • Lovinger Macromoleculesl982, 15, 40- 44.
  • It has a relatively high PVDF-PVDF coefficient of friction in the range 0.25-0.45 that limits its application as friction-intensive or self-lubricative coatings or as protective barrier coatings.
  • Inorganic solid lubricant molybdenum disulfide (MoS 2 ) is a known lubricant, which has been applied extensively for decades. The easy mutual gliding of M0S2 layers along (001) basal planes and surface inertness of the MoS 2 (001) basal planes give it its low friction properties.
  • a dry lubricant or an oil or grease additive Unfortunately, the high-hardness edges of crystal layers are prone to oxidation, which reduces the efficiency of lubrication, especially in humid environment. Thin flakes with a high active surface and with a relatively low number of unsaturated bonds at edges are therefore preferable.
  • Standard use of MoS 2 platelets as additive for friction reduction and recent discoveries of new morphologies of MoS 2 have opened the route to prepare new PVDF-based nanocomposite films containing MoS 2 nanotubes or exfoliated MoS 2 nanotubes for self-lubricative and protective barrier coatings.
  • Curved, self-terminated shapes of MoS 2 as nanotubes and fullerene-like particles with a nano-onion morphology allow the"elimination" of edges. They are intensively investigated with regards to their particular appropriateness for a new generation of lubricants. Under mechanical stress the nanoparticles slowly deform and exfoliate transferring MoS 2 nano-sheets onto the underlying surfaces (third body effect), and continue to provide effective lubrication until they are totally exfoliated (Chhowalla M, Amaratunga GAJ: Ultra low friction and wear MoS 2 nanoparticle thin films. Nature 2000, 407: 164-167).
  • PVDF/M0S2 composites where MoS 2 are discribed as nanotubes are dislosed by: g) US 20080248201 and US20080249221 Al, where PVDF is listed indirectly as a member of polyvinylidene halides and MoS 2 as a posible nanofiller among a wide range of materials for low friction coatings, but with no data presented on this particular composition; h) US20060233692 Al, where a method is dislosed whereas a metal alloy substrate can be directly coated with nanotubes, among them also MoS2 nanotubes are listed, and applying a polymeric coating thereover. PVDF is dislosed as polymer binder of carbon nanotubes.
  • PVDF/MoS 2 nanocomposites where MoS 2 is in cylindrical geometry of nanotubes or as exfoliated MoS 2 nanotubes and mixed into disolved PVDF before a coating preparation and tested for their friction properties have not been disclosed yet.
  • the MoS 2 nanotubes introduced into an isotactic polypropylene (iPP)decreased coefficient of friction for 15 % and wear for more than 50 % (M. Naffakh, M. Remskar, et al., J. Mater.Chem. 22, 17002-17010 (2012).). This is the only polymer-MoS 2 nanotube composite reported to date.
  • iPP isotactic polypropylene
  • This disclosure provides three-dimensional and thin film morphologies of fluoro-polymer nanocomposites with adjusted friction properties, which contain inorganic nanotube-based nanomaterials as low-friction additives.
  • nanotube-based nanomaterials means nanomaterials which occur in cylindrical geometry, or are derived from cylindrical geometry by using mechanical or chemical methods.
  • this disclosure provides a method of adjusting friction properties of PVDF based polymers with MoS 2 -nanotube- based as inorganic low-friction additives. Friction of the PVDF/MoS 2 nanotube-based nanomaterials is substantionaly reduced with respect to PVDF coatings without the said additives.
  • the MoS 2 nanotube-based nanomaterials are added to PVDF in form of a solution in an appropriate solvent or PVDF in melt form, and further homogenized by means of mechanical stirring.
  • Nanocomposite films may be prepared by various techniques applied to a polymer- nanoparticle mixture in liquid or plasticized state. Two of them are: a) solution casting on a suitable substrate by means of doctor blade applicator; b) spin-coating on a suitable substrate. The films are cured at different heating regimes with or without application of an atmosphere with a controlled composition.
  • the PVDF/MoS 2 nanotube-based nanomaterials in shape of films and coatings with thicknesses in the range between 10 ⁇ and 500 ⁇ were prepared.
  • Controlled crystal structure and morhology of the nanocomposites may be prepared using different co-additives in a role of inhibitors of agglomeration and sedimentation of MoS 2 nanotube-based nanomaterials and by varying of application and curring conditions.
  • the so-prepared nanocomposites were tested for their physical and chemical properties, particularly for their crystal structure, surface morphology, distribution of MoS 2 -nanotube- based nanomaterials inside the PVDF-based polymers, and thickness of the nanocomposite films.
  • FIG1 shows X-ray diffraction patterns of PVDF/MoS 2 films with 0 wt. % (label-0), 1 wt. % (label- 1), and 2 wt.% (label-2) of M0S 2 nanotubes.
  • the diffraction peaks corresponding to MoS 2 are labelled with *. Other peaks correspond to PVDF.
  • FIG2 is an optical micrograph taken in transmision mode showing homogeneous distribution of MoS 2 nanotubes inside the PVDF film containing 0.5 wt. % of MoS 2 nanotubes.
  • FIG3 is scanning electron microscopy image of the upper surface of a PVDF/MoS 2 nanotube film containing 2 wt.% of MoS 2 nanotubes showing porous structure.
  • FIG4 is a scanning electron microscopy image of the lower surface (at the interface with glass substrate) of a PVDF/MoS 2 nanotube film containing 1 wt.% of MoS 2 nanotubes.
  • FIG5 shows results of friction tests in a flat-on-flat geometry for PVDF/MoS 2 nanocomposite films with (a) 0 wt. %; (b) 1 wt.%, and (c) 2 wt.% of MoS 2 nanotubes, with polished stainlessteel AISI 316. as counterpart.
  • FIG6 shows results of friction tests in ball-on-disk geometry for PVDF/MoS 2 nanocomposite films with (a) 0 wt. %, (b) 2 wt. %, and (c) 16.7 wt.% of MoS 2 nanotubes, and stainless steel AISI 316 ball.
  • PVDF dimethylformamide
  • DMF dimethylformamide
  • MoS 2 nanotubes in 0.5 wt. %, 1 wt. %, and 2 wt. % with respect to wt. of PVDF were added into the PVDF/DMF solution and mixed using a magnetic stirrer for additional 30 minutes. Then the so-produced dispersion was sonicated for 30 minutes in an ultrasonic bath at 40 kHz and 200 W. A homogeneous dispersion of nanotubes in the polymer solution was obtained.
  • the dispersion was cast on a glass plate and drawn by a doctor blade with solution film thickness of 300 ⁇ , moved by means of a film applicator (Erichsen).
  • the films were dried at 22 °C and at 50 % relative humidity for 24 hours. After the drying the films were removed from the glass plate.
  • the film surface, which was exposed to the air during the drying is designated as the upper surface.
  • the film surface, which formed at the film/glass interface is designated as the lower surface.
  • the angular range 2 ⁇ was chosen from 6° to 73° with a step size of 0.04° and a collection time of 4 s.
  • Crystal structure characterization of the PVDF/MoS 2 nanotube films by x-ray diffraction as represented on FIG1 confirmed the presence of MoS 2 in the film.
  • the MoS 2 peaks are marked with (*). Other peaks correspond to ⁇ phase of PVDF.
  • the peak at 16.8° corresponds to a doubled unit cell of ⁇ -phase of PVDF.
  • PVDF/MoS 2 nanocomopsites were studied by scanning electron microscope FE-SEM, Supra 35 VP, Carl Zeiss.
  • the upper surface of PVDF/MoS 2 nanotube films are porous and composed of sphelurites as it is represented by FIG3.
  • the MoS 2 nanotubes are not visible because they are covered by PVDF.
  • the lower surface of the PVDF/MoS 2 nanotube film contains MoS 2 nanotubes, which are covered with a thinner layer of PVDF than the upper surface. MoS 2 nanotubes in the lower surface become visible when higher accelerating voltages in scanning electron investigation are applied, as it is shown in FIG4.
  • the thickness of the PVDF and PVDF/MoS 2 films and surface roughness were measured by a profilometer (Form Talysurf Series,Taylor-Hobson Ltd.), with resolution: in x- direction 0.25 ⁇ , in y-direction 1 ⁇ , in z-direction 3 nm. Pure PVDF films were 18.7 ⁇ ⁇ 1 ⁇ in thickness. PVDF/MoS 2 films which contained 1 wt.% of MoS 2 nanotubes were 22.3 ⁇ ⁇ 1 ⁇ thick. PVDF/MoS 2 films which contained 2 wt.% of MoS 2 nanotubes were 30 ⁇ ⁇ 1 ⁇ thick.
  • Friction was tested at normal room conditions: relative humidity in the range: 43-52% and in the temperature range: 20-25 °C. Friction tests were performed in a flat-on-flat geometry for PVDF/MoS 2 nanocomposite films with 0 %, 1 wt.% and 2 wt.% of MoS 2 nanotubes. The results are represented in FIG5. The presence of MoS 2 nanotubes in the PVDF films eliminated running-in peaks which are typical for pure PVDF films. The presence of MoS 2 nanotubes decreased coefficient of friction.
  • PVDF dimethylformamide
  • DMF dimethylformamide
  • MoS 2 nanotubes in 2 wt. % and 16.7 wt.% with respect to wt. of PVDF were added into the PVDF/MoS 2 solution and mixed using a magnetic stirrer for additional 15 minutes.
  • so-produced dispersion was sonicated for lh 45' in ultrasonic bath at 40 kHz and 200 W.
  • the PVDF and PVDF/MoS 2 nanotube-based coatings were prepared by solution drop casting directly on AISI 316 disks polished to arithmetical mean surface rougness Ra of 2 micrometers. The coatings were dried at 22 °C and at 50 % relative humidity until constant mass were reached.
  • PVDF/MoS 2 coatings on the AISI 316 disks were 50 ⁇ in thickness.
  • PVDF/MoS 2 coatings on the AISI 316 disks which contained 2 wt.% of MoS 2 nanotubes were 50 ⁇ thick.
  • PVDF MoS 2 coatings which contained 16.7 wt.% of MoS 2 nanotubes were 60 ⁇ thick.
  • Friction tests were performed with a standard ball bearing, 6 mm in diameter, made of stainless steel AISI 316 as counterpart to PVDF and PVDF/MoS 2 nanotube coatings.
  • the arithmetic mean surface rougness Ra of the ball was 200 nm
  • load applied to the ball was 1 N
  • radius of the circular path was 5.2 mm
  • contact pressure was 0.2 MPa
  • velocity of the ball with respect to the disk was 1 cra/s.
  • results of friction tests in ball-on-disk geometry indicate that the MoS 2 nanotubes added to PVDF as decribed in the invention, reduce friction at the contact between PVDF/MoS 2 nanotube composite and AISI 316.
  • the PVDF/MoS 2 nanotube coating with 2 wt.% of MoS 2 nanotubes revealed reduced friction by 7 % with respect to pure PVDF coating.
  • the PVDF/MoS 2 nanotubes coating with 16.7 wt.% of MoS 2 nanotubes revealed reduced friction in the first 12 m of sliding by 73% with respect to pure PVDF coating. After the sliding length of 12 m the coefficient of friction gradually increased to 0.43 and slowly approached 0.47 at 77 m of sliding.
  • Friction test results obtained in ball-on-disk geometry indicate that the MoS 2 nanotubes added to PVDF as decribed in the invention strongly reduce friction at the contact between PVDF/M0S2 nanotube composite and AISI 316.

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  • Chemical Kinetics & Catalysis (AREA)
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  • Polymers & Plastics (AREA)
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Abstract

Cette divulgation concerne des morphologies de films tridimensionnels et minces à base de nanocomposites polymères ayant des propriétés de frottement ajustées, qui contiennent des nanomatériaux inorganiques à base de nanotubes à titre d'additifs à faible coefficient de frottement. Le terme "nanomatériaux à base de nanotubes" désigne des nanomatériaux qui existent sous une géométrie cylindrique, ou sont dérivés d'une géométrie cylindrique à l'aide de procédés mécaniques ou chimiques. En particulier, cette divulgation concerne un procédé d'ajustement des propriétés de frottement de polymères à base de PVDF à l'aide de nanomatériaux à base de nanotubes MoS2 à titre d'additifs inorganiques à faible coefficient de frottement. Le coefficient de frottement des PVDF/nanomatériaux à base de nanotubes MoS2 est sensiblement réduit par rapport à celui des revêtements PVDF dépourvus desdits additifs.
PCT/SI2014/000052 2013-09-19 2014-09-19 Procédé d'ajustement du coefficient de frottement du polyfluorure de vinylidène (pvdf) WO2015041612A1 (fr)

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SI201300282A SI24472A (sl) 2013-09-19 2013-09-19 Fluoro-polimerni nanokompoziti s prilagojenimi tornimi lastnostmi
SIP-201300282 2013-09-19

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105185901A (zh) * 2015-08-06 2015-12-23 天津理工大学 一种基于二硫化钼的复合阻变存储器件及其制备方法
EP3346149A1 (fr) * 2017-01-09 2018-07-11 Hamilton Sundstrand Corporation Ensemble palier avec couche de surface

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105185901A (zh) * 2015-08-06 2015-12-23 天津理工大学 一种基于二硫化钼的复合阻变存储器件及其制备方法
EP3346149A1 (fr) * 2017-01-09 2018-07-11 Hamilton Sundstrand Corporation Ensemble palier avec couche de surface
US11221039B2 (en) 2017-01-09 2022-01-11 Hamilton Sundstrand Corporation Bearing assembly with surface layer

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