MACROMOLECULES LABORATORY

Course objectives

The course is organized in such a way as to provide the master's degree students with in-depth information on some experimental techniques used for the characterization of polymeric materials. Through the analysis of the acquired results the correlations between the observed properties and the structure of the materials and their fields of application will be highlighted. In particular, the course describes topics relating to surface tension of polymer solids, dynamo-mechanical analysis, kinetics of crystallization, applications of Fourier transform infrared spectroscopy in the characterization of polymers and the electrical properties of insulating and conducting polymers. For each topic covered, the course is developed in three phases. In the first one, the physical and chemical quantities measured by the instrumental technique, the theories that describe the analyzed phenomena, the correlations between the chemical structure of the materials and their behaviour will be analysed in detail. In the second phase, the instrumentation and the experimental procedures to be used in relation to the information to be acquired will be described. The used procedures will be compared with those proposed, if existing, by international regulations. In the third phase, the experimental tests will be carried out and data will be acquired for the subsequent elaborations. The results obtained will be analyzed according to the theories described in the first phase. The student will be able to manage the used instrumentation. Moreover, he will acquire the appropriate awareness to analyze which experimental and instrumental parameters are important to carry out characterization tests, also by employing techniques not used in the course. The importance dedicated to the analysis and processing of experimental data is aimed at acquiring the ability to critically apply mathematical models able to describe and, therefore, predict the behavior of materials, even in conditions not directly examined. The achievement of this objective is obtained through group work, drafting of written technical reports, the presentation of the results achieved and numerical exercises on macromolecular problems.

Channel 1
ANDREA MARTINELLI Lecturers' profile

Program - Frequency - Exams

Course program
Polymer crystallization processes • Micro-kinetics model • Primary and secondary nucleation, crystal growth. (Hoffman-Lauritzen theory) • Spherulitic morphology and spherulitic growth rate determination by optical microscopy. • The optical microscope, birefringence, optical indicatrix. Macro-kinetics model, overall crystallization • Avrami theory, primary nd secondary crystallization • Crystallization rate determination: methods and instrumentations. • Differential scanning calorimetry. Visco-elastic behaviour and dynamic mechanical analysis • Definition of polymer visco-elastic behavior. • Primary and secondary relaxations. • Parameters affecting the polymer visco-elastic properties(crystallinity, crosslinks, filler, plasticizer) • WLF and VTF theories. • Dynamic mechanical measurements: instruments, measurements condition, pretension, data analysis and interpretation. Electrical polymer behavior • Electrical conductivity of insulating, filled and conducting polymers. • Instrumentations for conductivity measurements: multimeters, electrometers, source-meter apparatus. • Surface and bulk conductivity • Two and three electrodes and four probe measurements. Surface tension of solids and contact angle • Definition of surface tension, work of adhesion and cohesion, Young equation, contact angle. • Girifalco, Fowks and Young equation. • Thermodynamic and kinetic hysteresis, rough and heterogeneous surfaces. • Static and dynamic contact angle measurements. • polymer surfaces. FT-IR spectroscopy of polymer • Instrument description • Sampling techniques (transmission, internal or external reflection) • Attenuated total reflection (ATR) • Spectroscopic features-structure correlations • thermal transition studied by FT-IR Laboratory experiences (2 cfu) • Spherulitic radian growth rate determination by optical microscopy • Crystallization kinetics study by differential scanning calorimetry • Dynamic mechanical characterization of polymers • Conducting polymer synthesis, doping and electrical characterization. • Conductivity measurements on filled and insulating polymers. • Contact angle measurements on bare or modified polymer surfaces. • Surface tension determination. Numerical exercises (1 cfu) • Application of models through curve fitting of experimental results
Prerequisites
Basic knowledge of the chemical, chemical-physical and mechanical characteristics of macromolecules and polymeric materials
Books
-S. Bruckner, G. Allegra, M. Pegoraro, F. P. La Mantia, Scienza e Tecnologia dei Materiali Polimerici, Ed. EdiSES, Napoli; -Ciardelli F., Farina M., Giusti P., Cesca S., Macromolecole. Scienza e Tecnologia Vol. I e II, Centro Stampa “Nuova Cultura”,Roma -Mechanical Properties of Solid Polymers: Third Edition-Author(s):I. M. WardJ. Sweeney-DOI:10.1002/9781119967125-John Wiley & Sons, Ltd -Introduction to Polymers, Third Edition-Robert J. Young, Peter A. Lovell-CRC Press; All texts can be found in the library of the Department of Chemistry Teacher's notes at available with prior authorization.
Frequency
For frontal lessons, there is no obligation to attend. Participation in laboratory exercises is mandatory.
Exam mode
The verification of knowledge will take place through a final oral exam.
Lesson mode
The course is structured in lectures on the description of the instruments, the models that describe the physical quantities analyzed and the way in which the data are processed. At the end of each topic discussed, laboratory exercises will take place with the acquisition of data to be processed. The students will process the data in groups and present a report on the results obtained.
  • Lesson code1020324
  • Academic year2024/2025
  • CourseIndustrial Chemistry
  • CurriculumMateriali Polimerici (MP)
  • Year1st year
  • Semester2nd semester
  • SSDCHIM/04
  • CFU9
  • Subject areaDiscipline chimiche ambientali, biotecnologiche, industriali, tecniche ed economiche