References of "Dubois, Philippe"
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See detailDual living free radical and ring opening polymerizations from a double-headed initiator
Hawker, Craig J; Hedrick, James L; Malmström, Eva E et al

in Macromolecules (1998), 31(2), 213-219

The concept of performing dual living polymerizations from a single initiating molecule with no intermediate activation, or transformation, steps is presented. The compatibility of “living”, or controlled ... [more ▼]

The concept of performing dual living polymerizations from a single initiating molecule with no intermediate activation, or transformation, steps is presented. The compatibility of “living”, or controlled free radical procedures, either nitroxide mediated or atom transfer radical polymerization (ATRP), with the living ring opening polymerization of ε-caprolactone, and vice versa, is demonstrated by the synthesis of a variety of well-defined block copolymers. For example, from a hydroxy-functionalized alkoxyamine, either the living ring opening polymerization of ε-caprolactone, or the “living” free radical polymerization of styrene can be performed leading to narrow polydispersity polymeric initiators. These polymeric initiators can then be used to initiate the living polymerization of the other monomer system without the need for intermediate steps. In a similar way, hydroxy-functionalized ATRP initiators can be used as bifunctional initiators for the polymerization of both ε-caprolactone and a variety of other vinyl monomers. The novel block copolymers that are obtained were shown to have low polydispersities and controllable molecular weights for both of the blocks. [less ▲]

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See detailControlled radical polymerization of methyl methacrylate initiated by an alkyl halide in the presence of the Wilkinson catalyst
Moineau, Georges; Granel, Claude; Dubois, Philippe ULg et al

in Macromolecules (1998), 31(2), 542-544

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See detailBonding electropolymerization: a new electron-transfer strategy for the tailoring of performant polymer-based composites
Baute, Noëlle; Calberg, Cédric ULg; Dubois, Philippe ULg et al

in Macromolecular Symposia (1998), 134

Careful control of experimental conditions in the cathodic electropolymerization of acrylonitrile allows the grafting of thin polymer films, on conducting surfaces offering electrons easily mobilized at a ... [more ▼]

Careful control of experimental conditions in the cathodic electropolymerization of acrylonitrile allows the grafting of thin polymer films, on conducting surfaces offering electrons easily mobilized at a relatively low potential. Matching relative polarity and donicity of solvent and monomer expands the applicability of this methodology to the whole class of (meth)acrylic monomers, paving the way to many new and useful multiphase materials. [less ▲]

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See detailPolyolefin-based composites by polymerization-filling technique
Dubois, Philippe ULg; Alexandre, Michaël ULg; Hindryckx, François et al

in Journal of Macromolecular Science - Reviews in Macromolecular Chemistry and Physics (1998), 38(3), 511-565

Dispersions of inorganic fillers within polymers are commonly designated as polymer-based composites. The properties of these materials are isotropic or anisotropic, depending on the geometry of the ... [more ▼]

Dispersions of inorganic fillers within polymers are commonly designated as polymer-based composites. The properties of these materials are isotropic or anisotropic, depending on the geometry of the filler particles and the effect of the processing conditions on their orientation. Fillers are used to improve some physicomechanical properties of the polymer, the material processability, or decrease the final cost. As a typical example, highly filled composites in which the filler concentration approaches the maximum packing fraction are known for their use in the shaping of ceramic articles. [less ▲]

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See detailSynthesis of poly(norbornene-g-ε-caprolactone) copolymers by sequential controlled ring opening polymerization
Lecomte, Philippe ULg; Mecerreyes, David; Dubois, Philippe ULg et al

in Polymer Bulletin (1998), 40(6), 631-638

Poly(norbornene-g-ε-caprolactone) copolymers have been prepared by the "grafting from" technique. Well controlled polynorbornene containing 5% acetate pendant groups has been firstly synthesized by ... [more ▼]

Poly(norbornene-g-ε-caprolactone) copolymers have been prepared by the "grafting from" technique. Well controlled polynorbornene containing 5% acetate pendant groups has been firstly synthesized by ruthenium complex-mediated ring opening metathesis polymerization. The acetate groups have been derivatized into aluminum alkoxides by hydrolysis into alcohol followed by reaction of the alcohol with triethylaluminum. The two polymerization steps are under complete control, so that graft copolymers have been synthesized with a narrow molecular weight distribution and are free from any detectable traces of the parent homopolymers as stated by selective fractionation experiments. These original copolymers have been characterized by SEC, FTIR, 1H NMR, DSC, TGA. [less ▲]

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See detailPorous silica obtained from biodegradable and biocompatible inorganic-organic hybrid materials
Tian, Dong; Blacher, Silvia ULg; Dubois, Philippe ULg et al

in Journal of Sol-Gel Science and Technology (1998), 13(1-3), 415-419

Porous silicas have been successfully prepared from poly(ε -caprolactone) (PCL)-silica hybrid materials based on the template approach. The final texture of the porous silica can be tailored by the PCL ... [more ▼]

Porous silicas have been successfully prepared from poly(ε -caprolactone) (PCL)-silica hybrid materials based on the template approach. The final texture of the porous silica can be tailored by the PCL template, i.e., molecular weight and molecular weight distribution, content, type and number of reactive end-groups per chain. Porosity has been investigated by nitrogen adsorption-desorption technique and small angle X-ray scattering (SAXS). [less ▲]

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See detailVersatile and controlled synthesis of star and branched macromolecules by dentritic initiation
Trollsas, Michaël; Hedrick, James L.; Mecerreyes, David et al

in Macromolecules (1997), 30(26), 8508-8511

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See detailDifunctional anionic initiator based on 1.3-diisopropenylbenzene. 5. Effect of polar additives and initiator seeding on the synthesis of poly(styrene-b-butadiene-b-styrene) copolymer
Yu, Y. S.; Dubois, Philippe ULg; Teyssié, Philippe et al

in Macromolecules (1997), 30(24), 7356-7362

The initiation of butadiene and styrene polymerization by a pure hydrocarbon soluble difunctional organolithium, 1,3-bis(1-lithio-1,3,3‘-trimethylbutyl)benzene, has been studied in a hydrocarbon solvent ... [more ▼]

The initiation of butadiene and styrene polymerization by a pure hydrocarbon soluble difunctional organolithium, 1,3-bis(1-lithio-1,3,3‘-trimethylbutyl)benzene, has been studied in a hydrocarbon solvent. The initiation occurs in such a way that part of the diadduct remains unreacted. When a second monomer feed along with tetrahydrofuran (THF) is added to the living chains, the residual diadduct is activated to the point where novel chains are formed. Weakly polar additives such as lithium alkoxides and aromatic ether can prevent part of the initiator from being inactive, although these additives are not effective enough to initiate the controlled synthesis of poly(styrene-b-butadiene-b-styrene) (SBS) triblock copolymers. The seeding of the initiator which consists of butadiene oligomerization in the presence of anisole and tBuOLi in cyclohexane, has proved to be very efficient in providing SBS containing 85% 1,4-microstructure polybutadiene (PBD) and with high mechanical properties, e.g., ultimate tensile strength higher than 30 MPa and elongation at a break of 1000%. [less ▲]

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See detailPoly [glycidyl methacrylate (GMA) / methylmethacrylate (MMA)-b-butadiene (B)-b-GMA/MMA] reactive thermoplastic elastomers: synthesis and characterization
Yu, Jian Ming; Dubois, Philippe ULg; Jérôme, Robert ULg

in Journal of Polymer Science. Part A, Polymer Chemistry (1997), 35(16), 3507-3515

New block copolymers of the ABA type, where B stands for polybutadiene (PBD) and A for polyglycidylmethacrylate(PGMA), poly(methylmethacrylate(MMA)-co-GMA) and PMMA-b-PGMA, respectively, have been ... [more ▼]

New block copolymers of the ABA type, where B stands for polybutadiene (PBD) and A for polyglycidylmethacrylate(PGMA), poly(methylmethacrylate(MMA)-co-GMA) and PMMA-b-PGMA, respectively, have been successfully synthesized by using the diadduct of tert-butyllithium (tert-BuLi) to meta-diisopropenylbenzene (m-DIB) as a difunctional initiator. The PBD midblock has been synthesized in a cyclohexane/diethylether (100/6, v/v) mixture at room temperature, whereas the methacrylate outer blocks have been synthesized in a cyclohexane/diethylether/THF (100/6/150, v/v/v) mixture at -78°C. Block copolymers of a very narrow molecular weight distribution (1.10) have been analyzed by differential scanning calorimetry (DSC), transmission electron microscopy (TEM), and tensile testing. These materials are phase separated and can exhibit tensile strength up to 22 MPa together with very high elongation at break (1500%). [less ▲]

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See detailNew polybutadiene-based thermoplastic elastomers: synthesis, morphology and mechanical properties
Dubois, Philippe ULg; Yu, Y. S.; Teyssié, Philippe et al

in Rubber Chemistry and Technology (1997, November), 70(5), 714-726

Well defined poly[styrene-b-butadiene-b-styrene] block copolymers (SBS) end-capped with poly(t-butyl methacrylate) (PtBMA) and poly(methacrylic acid) (PMA) outer blocks, respectively, have been ... [more ▼]

Well defined poly[styrene-b-butadiene-b-styrene] block copolymers (SBS) end-capped with poly(t-butyl methacrylate) (PtBMA) and poly(methacrylic acid) (PMA) outer blocks, respectively, have been synthesized by the sequential anionic polymerization of butadiene, styrene and tBMA, followed by the selective hydrolysis of the PtBMA blocks into the corresponding PMA blocks. The structure-property relationships of these new thermoplastic elastomers have been investigated, with a special emphasis on the effect of the ester or acid outer blocks on the bulk properties. As a rule, tensile strength is improved by increasing the length of the ester or acid outer blocks from 0 to 140 methacrylic units. Dipole-dipole intermolecular interaction of the PtBMA blocks and hydrogen bonding of the PMA blocks may account for enhanced mechanical properties. However, too high a degree of strong intermolecular interactions can constitute a deterrent to good phase separation. This is supported by morphological observations and loss in tensile properties when the relative content of the ester or acid outer blocks exceeds some critical value. In the case of a high acid content, DSC analysis shows two thermal transitions at -70 ??C and 230 ??C for PBD and PMA blocks, respectively. [less ▲]

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See detailDifunctional initiator based on 1,3-diisopropenylbenzene. 7. Mechanical and thermal properties of new butadiene-based thermoplastic elastomers
Yu, Y. S.; Dubois, Philippe ULg; Jérôme, Robert ULg et al

in Rubber Chemistry and Technology (1997, November), 70(5), 820-838

Mechanical and thermal properties of SBS thermoplastic elastomers, in which S stands for polystyrene and B for polybutadiene, can be remarkably improved through end-capping by syndiotactic poly(methyl ... [more ▼]

Mechanical and thermal properties of SBS thermoplastic elastomers, in which S stands for polystyrene and B for polybutadiene, can be remarkably improved through end-capping by syndiotactic poly(methyl methacrylate) sequences. Furthermore, the upper service temperature of these sPMMA teleblock copolymers can also be enhanced by blending with isotactic PMMA so that the rubbery PBD soft segments are connected to high-melting stereocomplexed hard segments. The factors which affect the mechanical and thermal properties of these novel thermoplastic elastomers have been extensively investigated. [less ▲]

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See detailPoly[poly(isobornyl methacrylate-co-methyl methacrylate) (poly(IBMA-co-MMA))-b-polybutadiene-b-poly(IBMA-co-MMA)] Copolymers: synthesis, morphology, and properties
Yu, J. M.; Dubois, Philippe ULg; Jérôme, Robert ULg

in Macromolecules (1997), 30(21), 6536-6543

Anionic random and block copolymerization of isobornyl methacrylate (IBMA) and methyl methacrylate (MMA) has been studied in THF at −78 °C by using (1,1-diphenyl-3,3-dimethylbutyl)lithium (DDBLi) as ... [more ▼]

Anionic random and block copolymerization of isobornyl methacrylate (IBMA) and methyl methacrylate (MMA) has been studied in THF at −78 °C by using (1,1-diphenyl-3,3-dimethylbutyl)lithium (DDBLi) as initiator in the presence of LiCl. The random copolymerization of MMA and IBMA has also been carried out at 0 °C, all the other conditions being kept unchanged. Poly[poly(IBMA)-b-poly(BD)-b-poly(IBMA)] (IBI), poly[poly(IBMA-co-MMA)-b-poly(BD)-b-poly(MMA-co-IBMA)] (I/MBM/I), and poly[poly(IBMA)-b-poly(MMA)-b-poly(BD)-b-poly(MMA)-b-poly(IBMA)] (IMBMI) block copolymers have been synthesized by sequential anionic polymerization of butadiene, MMA, and IBMA initiated by the m-diisopropenylbenzene (m-DIB)/tert-butyllithium (t-BuLi) diadduct. These block copolymers of a monomodal and narrow molecular weight distribution (M̄w/M̄n = 1.1) have been analyzed by size exclusion chromatography (SEC), NMR, differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), and transmission electron microscopy (TEM). Stereocomplexation of IMBMA and I/MBM/I with iPMMA has also been studied by DSC. Although IBI triblock copolymers show a lamellar morphology even for relatively low hard block content (33 wt %), cylindrical and lamellar morphologies have been observed for the other block copolymers under consideration. These new block copolymers exhibit high ultimate tensile strength (30 MPa), elongation at break (1000%), and upper service temperature (140−200 °C). [less ▲]

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See detailMacromolecular engineering of lactones and lactides. 24. Controlled synthesis of (R,S)-β-butyrolactone-b-ε-caprolactone block copolymers by anionic and coordination polymerization
Kurcok, Piotr; Dubois, Philippe ULg; Sikorska, Wanda et al

in Macromolecules (1997), 30(19), 5591-5595

Block copolymers of (R,S)-β-butyrolactone and ε-caprolactone have been synthesized by combining the anionic polymerization of the first monomer with the coordinative ring-opening polymerization of the ... [more ▼]

Block copolymers of (R,S)-β-butyrolactone and ε-caprolactone have been synthesized by combining the anionic polymerization of the first monomer with the coordinative ring-opening polymerization of the second one. The copolymerization yield is close to 100% and the final molecular weight of each sequence can be predicted from the initial monomer-to-initiator molar ratio. The molecular weight distribution of copolymers obtained is quite narrow (Mw/Mn ≤ 1.3). According to NMR and DSC analysis, the polybutyrolactone block is atactic and totally amorphous, in contrast to the polycaprolactone block which is semicrystalline. A partial miscibility of the two blocks in the amorphous phase has however been detected. Thermal and enzymatic degradations of the block copolymers have been investigated. The enzymatic degradation rate promoted by the lipase form Rhizopus arrhizus strongly depends on the copolyester composition and increases with the β-butyrolactone content. [less ▲]

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See detailBulk polymerization of lactides initiated by aluminum isopropoxide. 1. Mechanism and kinetics
Degée, Philippe; Dubois, Philippe ULg; Jérôme, Robert ULg

in Macromolecular Symposia (1997), 123

Commercially available Al isopiopoxide (Al(OiPr)3) has proved to be an efficient initiator for the bulk polymerization of lactide. The ring-opening polymerization proceeds through a "coordination ... [more ▼]

Commercially available Al isopiopoxide (Al(OiPr)3) has proved to be an efficient initiator for the bulk polymerization of lactide. The ring-opening polymerization proceeds through a "coordination-insertion" mechanism and the selective rupture of the acyl-oxygen bond of the monomer Polyester chains are selectively end-capped with an aluminum alkoxide and an isopropoxy group. Therefore, substitution of Al tris(4-penten-1-olate) for Al(OiPr)3 leads to the formation of macromonomers In the temperature range from 110 to 150°C, polymerization is "living", i.e. the molecular weight can be predicted by the initial monomer-to-Al molar ratio and the monomer conversion. The narrower polydispetsity of poly(L,L-lactide) compared to the amorphous poly(D,L-lactide) ( 1.3 compared to 1.9, respectively), both prepared in the bulk, is thought to result from the restricted mobility of the crystallized isotactic polyester chains. When the temperature is increased up to 180°C, inter- and intramolecular transesterification reactions interfere with chain propagation. [less ▲]

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See detailPoly[methyl methacrylate (M)-b-styrene (S)-b-butadiene (B)-b-S-b-M] pentablock copolymers: synthesis, morphology, and properties.
Yu, Jian Ming; Dubois, Philippe ULg; Jérôme, Robert ULg

in Macromolecules (1997), 30(17), 4984-4994

A series of poly[methyl methacrylate (M)-b-styrene (S)-b-butadiene (B)-b-S-b-M], or MSBSM, pentablock copolymers have been successfully synthesized by sequential living anionic polymerization initiated ... [more ▼]

A series of poly[methyl methacrylate (M)-b-styrene (S)-b-butadiene (B)-b-S-b-M], or MSBSM, pentablock copolymers have been successfully synthesized by sequential living anionic polymerization initiated with the diadduct of tert-butyllithium (t-BuLi) onto m-diisopropenylbenzene (m-DIB) in a cyclohexane/diethyl ether mixture for the butadiene and styrene polymerization at room temperature and in a cyclohexane/THF mixture for the MMA polymerization at −78 °C. All the pentablock copolymers have a monomodal and narrow molecular weight distribution (Mw/Mn < 1.20), and their weight composition varies from 11 to 55% M, 18 to 55% S, and 15 to 64% B. Toluene-cast films of these copolymers have been analyzed by differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), and transmission electron microscopy (TEM). All these materials show a phase separation of the soft B component from the hard S and M blocks, which cannot, however, be distinguished one from each other by DSC or DMA. Indeed, a single transition is observed for the binary hard phase at a temperature intermediate between the glass transition temperature of polystyrene (PS) and poly(methyl methacrylate) (PMMA). In addition to classical phase morphologies, such as cylindrical and lamellar phase organization, two nonclassical morphologies, i.e., catenoid−lamellar and strut phase structures have been observed by TEM. The phase morphology strongly depends on the pentablock composition and any chemical modification of blocks. For instance, the cylindrical morphology, characteristic of an MSBSM copolymer containing equal amounts of hard and soft phases, is changed into a lamellar morphology upon hydrogenation of the B midblock. Copolymers of a relatively low hard phase content typically behave as thermoplastic elastomers of high ultimate tensile strength (ca. 30 MPa) and elongation at break (ca. 900%). These mechanical properties, however, depend on the casting solvent. [less ▲]

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See detailBiodegradable and biocompatible inorganic-organic hybrid materials. 1. Synthesis and characterization
Tian, Dong; Dubois, Philippe ULg; Jérôme, Robert ULg

in Journal of Polymer Science. Part A, Polymer Chemistry (1997), 35(11), 2295-2309

The hydroxyl or vinyl end-groups of linear or three-arm star-shaped poly(-caprolactone) (PCL) chains have been derivatized into triethoxysilane groups reactive in the sol-gel process. New transparent ... [more ▼]

The hydroxyl or vinyl end-groups of linear or three-arm star-shaped poly(-caprolactone) (PCL) chains have been derivatized into triethoxysilane groups reactive in the sol-gel process. New transparent hybrid materials that combine tetraethylorthosilicate (TEOS) and PCL known for biodegradability and biocompatibility have accordingly been prepared. The sol-gel process is, however, limited by the early vitrification of the reactive system. However, thermal posttreatment can overcome these diffusional and/or kinetic limitations as assessed by a set of analytical methods. The thermal stability of PCL is improved by incorporation into the silica network. Conversely, the thermal stability of the ceramer depends on the effective PCL content. The extent of PCL incorporation into the silica network depends on PCL molecular weight, number, and reactivity of the PCL functional groups. IR spectroscopy has shown that hydrogen bonding occurs between the ester groups of PCL and residual OH groups of the silicate component. © 1997 John Wiley [less ▲]

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See detailSynthesis and characterization of hydrogenated poly[alkylmethacrylate(-b-styrene)-b-butadiene-b-(styrene-b-) alkylmethacrylate] triblock and pentablock copolymers
Yu, Jian Ming; Yu, Yisong; Dubois, Philippe ULg et al

in Polymer (1997), 38(12), 3091-3101

Triblock and pentablock copolymers of the X(Y)B(Y)X type have been synthesized by the sequential living anionic polymerization of butadiene (B), styrene (Y) and alkylmethacrylate (X), respectively. The ... [more ▼]

Triblock and pentablock copolymers of the X(Y)B(Y)X type have been synthesized by the sequential living anionic polymerization of butadiene (B), styrene (Y) and alkylmethacrylate (X), respectively. The diadduct of t-BuLi onto m-diisopropenylbenzene (m-DIB) has been used as a difunctional initiator. Methylmethacrylate (MMA), t-butylmethacrylate (tBMA) and isobornylmethacrylate (IBMA) have been used as precursors of the outerblocks X. The polybutadiene (PBD) midblock that contains ca 42-45% 1,2-units has been selectively hydrogenated into a saturated poly(ethylene-co-1-butene) (PEB) block. The homogeneous hydrogenation catalysis has no deleterious effect on the copolymer integrity. These completely soluble thermoplastic elastomers have been characterized by FT i.r., n.m.r., d.s.c. and d.m.a. The PEB midblock has a low Tg (-50°C) and a small propensity to crystallize. The effect of hydrogenation on the morphology and mechanical properties depends on the outer block. Upon hydrogenation of the PBD midblock in polymethylmethacrylate (PMMA) and polyisobornylmethacrylate (PIBMA) containing triblock copolymers, the ultimate tensile strength is increased (except for a hard block content > 50%) due to a sharper phase separation, whereas the elongation at break is decreased. The extent of phase separation is reduced in polyt-butylmethacrylate(PtBMA) containing triblock copolymers upon hydrogenation and the ultimate tensile strength is slightly decreased. Stereocomplexation of the syndiotactic PMMA outerblocks is observed to occur upon blending with isotactic PMMA [less ▲]

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See detailDifunctional initiator based on 1,3-diisopropenylbenzene. 6. Synthesis of methyl methacrylate-butadiene-methyl methacrylate triblock copolymers
Yu, Y. S.; Dubois, Philippe ULg; Teyssié, Philippe et al

in Macromolecules (1997), 30(15), 4254-4261

Synthesis of PMMA−PBD−PMMA (MBM) triblock copolymers with a 1,3-diisopropenylbenzene- (DIB-) based initiator is studied. Diethyl ether, tert-butyl methyl ether, N,N,N‘,N‘-tetramethylethylenediamine (TMEDA ... [more ▼]

Synthesis of PMMA−PBD−PMMA (MBM) triblock copolymers with a 1,3-diisopropenylbenzene- (DIB-) based initiator is studied. Diethyl ether, tert-butyl methyl ether, N,N,N‘,N‘-tetramethylethylenediamine (TMEDA) and THF were found to be efficient polar additives for obtaining PMMA−PBD−PMMA triblock copolymers, but these triblock copolymers displayed a high 1,2-microstructure of the PBD block. A combination of the initiator seeding technique and weakly polar additives has allowed MBM triblock copolymers with high 1,4-microstructure of PBD to be obtained. These copolymers exhibited a definitely higher upper service temperature than conventional thermoplastic elastomers, i.e. SBS or SIS Kratons. The influence of chain microstructure, copolymer composition and block length on the mechanical properties has been studied. Short polystyrene blocks of ca. Mn 2000 have been incorporated in between the PBD central block and the PMMA outer sequences. A higher tensile strength was observed for these MBM-like triblock coplymers. Contamination by a diblock structure expectedly had a very depressive effect on the bulk properties, and the stress−strain behavior mainly depended on the PMMA content and secondarily on molecular weight. [less ▲]

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