FR3015682B1 - METHOD FOR DETERMINING THE KINETICS OF CRYSTALLIZATION OF A POLYMER BY DIFFERENTIAL CALORIMETRIC ANALYSIS OF A NANO-SAMPLE - Google Patents

METHOD FOR DETERMINING THE KINETICS OF CRYSTALLIZATION OF A POLYMER BY DIFFERENTIAL CALORIMETRIC ANALYSIS OF A NANO-SAMPLE Download PDF

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Publication number
FR3015682B1
FR3015682B1 FR1363574A FR1363574A FR3015682B1 FR 3015682 B1 FR3015682 B1 FR 3015682B1 FR 1363574 A FR1363574 A FR 1363574A FR 1363574 A FR1363574 A FR 1363574A FR 3015682 B1 FR3015682 B1 FR 3015682B1
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France
Prior art keywords
nano
sample
polymer
temperature
crystallization
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FR1363574A
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French (fr)
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FR3015682A1 (en
Inventor
Xavier Tardif
Nicolas Boyard
Vincent Sobotka
Didier Delaunay
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Centre National de la Recherche Scientifique CNRS
Universite de Nantes
Institut de Recherche Technologique Jules Verne
Original Assignee
Centre National de la Recherche Scientifique CNRS
Universite de Nantes
Institut de Recherche Technologique Jules Verne
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Priority to FR1363574A priority Critical patent/FR3015682B1/en
Priority to PCT/EP2014/079286 priority patent/WO2015097273A1/en
Publication of FR3015682A1 publication Critical patent/FR3015682A1/en
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00—Investigating or analyzing materials by the use of thermal means
    • G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
    • G01N25/48—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation
    • G01N25/4846—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation for a motionless, e.g. solid sample
    • G01N25/4866—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation for a motionless, e.g. solid sample by using a differential method

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Combustion & Propulsion (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Materials Using Thermal Means (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

L'invention concerne un procédé pour mesurer l'avancement de la cristallisation isotherme d'un polymère thermoplastique semicristallin au moyen d'un dispositif de nano-DSC, caractérisé en ce qu'il comporte les étapes consistant à : a. prélever un nano-échantillon dudit polymère et le placer, pour analyse, dans un dispositif de nano-DSC ; b. porter (110) ledit nano-échantillon à une température supérieure à la température (103) de fusion dudit polymère de sorte à effacer son histoire thermique ; c. refroidir (120) le nano-échantillon à une vitesse de refroidissement supérieure à 500 K.s jusqu'à une température palier correspondant à la température d'étude de la cristallisation isotherme ; d. maintenir (130) durant un temps t, défini l'échantillon au palier de température ; e. réchauffer (150) le nano-échantillon jusqu'à la température (103) de fusion du polymère à une vitesse de chauffage supérieure à 500 K.s ; f. mesurer chaleur latente de fusion et en déduire le taux de cristallinité obtenu par le maintien isotherme pendant le temps t .The invention relates to a method for measuring the progress of the isothermal crystallization of a semicrystalline thermoplastic polymer by means of a nano-DSC device, characterized in that it comprises the steps of: a. taking a nano-sample of said polymer and placing it, for analysis, in a nano-DSC device; b. bringing (110) said nanosample to a temperature above the melting temperature (103) of said polymer so as to erase its thermal history; vs. cooling (120) the nano-sample at a cooling rate greater than 500 K.s to a plateau temperature corresponding to the study temperature of isothermal crystallization; d. maintaining (130) for a time t, defined the sample at the temperature level; e. heating (150) the nano-sample to the polymer melting temperature (103) at a heating rate greater than 500 K.s; f. measure the latent heat of fusion and deduce therefrom the degree of crystallinity obtained by maintaining isothermal during the time t.

FR1363574A 2013-12-24 2013-12-24 METHOD FOR DETERMINING THE KINETICS OF CRYSTALLIZATION OF A POLYMER BY DIFFERENTIAL CALORIMETRIC ANALYSIS OF A NANO-SAMPLE Active FR3015682B1 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
FR1363574A FR3015682B1 (en) 2013-12-24 2013-12-24 METHOD FOR DETERMINING THE KINETICS OF CRYSTALLIZATION OF A POLYMER BY DIFFERENTIAL CALORIMETRIC ANALYSIS OF A NANO-SAMPLE
PCT/EP2014/079286 WO2015097273A1 (en) 2013-12-24 2014-12-23 Method for monitoring the crystallinity of a polymer during the manufacture of a part

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR1363574A FR3015682B1 (en) 2013-12-24 2013-12-24 METHOD FOR DETERMINING THE KINETICS OF CRYSTALLIZATION OF A POLYMER BY DIFFERENTIAL CALORIMETRIC ANALYSIS OF A NANO-SAMPLE

Publications (2)

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FR3015682A1 FR3015682A1 (en) 2015-06-26
FR3015682B1 true FR3015682B1 (en) 2021-01-15

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FR1363574A Active FR3015682B1 (en) 2013-12-24 2013-12-24 METHOD FOR DETERMINING THE KINETICS OF CRYSTALLIZATION OF A POLYMER BY DIFFERENTIAL CALORIMETRIC ANALYSIS OF A NANO-SAMPLE

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FR (1) FR3015682B1 (en)
WO (1) WO2015097273A1 (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111024749A (en) * 2019-12-31 2020-04-17 常州欣战江特种纤维有限公司 Method for evaluating spinning post-processing performance based on differential scanning calorimetry
EP3871804A1 (en) 2020-02-25 2021-09-01 Heraeus Amloy Technologies GmbH Method for adapting a component description of a workpiece to be manufactured with amorphous properties
CN114428077B (en) * 2020-09-30 2024-04-19 中国石油化工股份有限公司 Method for analyzing rubber particles in polymer material

Family Cites Families (1)

* Cited by examiner, † Cited by third party
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JP5461536B2 (en) * 2008-06-06 2014-04-02 パーキンエルマー・ヘルス・サイエンシーズ・インコーポレイテッド Calorimeter, method using the same, and control system therefor

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FR3015682A1 (en) 2015-06-26
WO2015097273A1 (en) 2015-07-02

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