Course detail

Characterization Methods of Polymer Materials

FCH-MA_MCPMAcad. year: 2023/2024

The subject builds on basic knowledge obtained in previous terms regarding the field of macromolecular chemistry and structure of materials including polymers. It targets more thorough explanation and understanding of polymer structure from molecular to supramolecular one and the influence on final polymer properties. Since the structure of material controls properties, the measurement of the polymer properties serves as the feedback to its structure and understanding of the structure can lead to the “polymer tailoring”. Lectured are selected direct and indirect methods for imaging and deduction of supramolecular structure together with selected basic methods to determine the polymer composition and to identify polymers. Explained are principles of selected methods, suitable process of specimen preparation, proper choice of measuring conditions, and correct interpretation of the obtained data.
The sequence of particular themes is disordered a little in order to found theoretical basis for simultaneously running “Practices of Instrumental and Structure Analysis”.

Students are practically introduced with basic methods used for uncovering, observation and evaluation of supramolecular structure of polymer materials. Three quarters of practices serves for introduction with selected methods and the last one for self-measurement and characterization of one type of thermoplastic under suitable conditions. Selected are methods from microscopy, spectroscopy and thermal analysis. The stress is laid on the importance of proper preparation of the specimen, suitable setting of testing conditions, accurate evaluation and interpretation of the obtained data, but also on well-arranged report in right format.

Language of instruction

English

Number of ECTS credits

5

Mode of study

Not applicable.

Guarantor

Ing. Radka Bálková, Ph.D.

Department

Institute of Materials Science (ÚCHM)

Offered to foreign students

Of all faculties

Entry knowledge

Macromolecular chemistry, Structure of materials, Physical chemistry of macromolecules, Polymeric materials

Rules for evaluation and completion of the course

Lectures are finished by oral examination. The student can enter the exam only after handover of written report elaborated from submitted thermogravimetric curves of several specimens. The report must be handover at the latest one day before the exam date but ideally during the term. Classification of the report forms 30% of the final mark. On oral examination the students will get two questions chosen form the range of lectures.

The credit of practices will be given if the student passes all practicums and handovers all reports in required quality and in time.

To check if the students are able to use knowledge from lectures, thermogravimetric curves of a few materials are propound to evaluate required data and to write short report from measurements. Attendance in lectures is recommended.

The attendance in all practices is demanded. An unexcused absence is the reason for the loss of the credit. In case of the absence, the practice can be compensated with another group (according to the students number) or in the last week of the term. Theoretical knowledge of students regarding the particular practice is examined by the written tests with 10–13 questions at the beginning of the practice. The student cannot pass practice if the test fruitfulness is worse than 70%.
Each practice will be finished by written report handover till ten days after the practice date. The report will be one from each group and will be elaborated in a quality required for a scientific report including typographical rules. If the report is out of requirements, it will be pass back to rewrite. The credit will be given when all reports of required quality will be handover till the end of examination interval. It not, the whole group will repeat practices the next winter term.

Aims

The aim of the subject is to understand that the structure of polymer materials is responsible for their properties and that the change in properties reflects the change in structure. Basic knowledge of polymer material properties under various conditions/in different environment in which the materials are used is essential for their proper utilization. Therefore it is necessary both to qualify and to quantify properties of polymer materials. This is achieved by measurement. Numerous direct and indirect methods were developed to qualify and quantify various properties and to image/observe structure of materials. Theoretical part of this subject is dedicated to learn selected imaging techniques and methods to determine supramolecular structure and thermo-mechanical properties of polymer materials. It comprises both principal of methods including preparation of specimens and selection of suitable measurement conditions, and interpretation of obtained results on examples of many polymer materials and their additives.

The aim of practices is to prepare specimens from real polymer materials to image and evaluate supramolecular structure of semicrystalline polymers and copolymers, to prepare specimens for and to evaluate composition of selected polymer materials or their identification, to judge the influence of cooling rate on supramolecular structure, and finally to perform and interpret rheological measurements of polymer melts.
Knowldege of a student regarding preparation of specimens, selection of proper method including measurement conditions and interpretation of supramolecular structure of polymer materials including composition. Ability of a student to judge and prove (i) if the tested material was chemically degraded or physical or chemical degradation could occur during measurement, (ii) what is or could be a reason of unexpected mechanical properties of polymer materials, (iii) how it is changed or how it is possible to influence the structure and thus, final properties by high or low temperature, and (iv) visco-elastic properties of polymer materials.

From practices the ability of students (i) to prepare specimens of polymer materials for imaging on POM and CLSM, for measurement on DSC, FTIR-ATR and rheometer and (ii) to interpret correctly the observed images and the obtained data.

Study aids

Not applicable.

Prerequisites and corequisites

Not applicable.

Basic literature

Ehrenstein G.W.: Polymeric Materials : Structure – Properties – Applications. Munich : Carl Hanser Verlag, 2001. 279 p. ISBN 3-446-21461-5. (EN)
Ehrenstein G.W., Riedel G., Trawiel P.: Thermal Analysis of Plastics: Theory and Practice. Hanser Gardner Publications, Cincinnati 2004. (EN)
Characterization and analysis of polymers. 1. Edition. Canada, New Jersey : Wiley, John & Sons, Incorporated, 2008. 977 p. ISBN: 978-0-470-23300-9. (EN)
Lednický František: Mikroskopie a morfologie polymerů : Díl 1. Mikroskopie polymerů a preparační techniky. 1. vyd. Liberec : Fastr typo-tisk, 2009. 71 s. ISBN 978-80-7372-486-3. (CS)
Lednický František: Mikroskopie a morfologie polymerů : Díl 2. Morfologie polymerů. 1. vyd. Liberec : Fastr typo-tisk, 2009. 97 s. ISBN 978-80-7372-486-3.3. (CS)
Menard K.P.: Dynamic Mechanical Analysis: A Practical Introduction to Techniques and Applications. CRC Press, Boca Raton 1999. (EN)
Woodward A.E.: Atlas of Polymer Morphology. USA : Oxford University Press, 1989. 544 p. ISBN 978-0195207583. (EN)
Woodward A.E.: Understanding Polymer Morphology. USA, New York : Hanser Gardner Publications, 1995. 130 p. ISBN 978-1569901410. (EN)

Recommended reading

Not applicable.

Elearning

eLearning: currently opened course

Classification of course in study plans

  • Programme NKCP_CHTM Master's 1 year of study, winter semester, compulsory
  • Programme NPCP_CHTM Master's 1 year of study, winter semester, compulsory
  • Programme NPAP_ENVI Master's 1 year of study, winter semester, compulsory

Type of course unit

 

Lecture

26 hod., optionally

Teacher / Lecturer

Ing. Radka Bálková, Ph.D.

Syllabus

Lecture topics:
1. Morphology of polymers – the separate discipline; supramolecular structure of polymers and basic structural figures of semcrystalline polymers; supramolecular structure of polypropylen
2. Microscopic techniques; Polarizing optical microscopy (POM), birefringent materials; nucleating agents
3. Methods for uncovering supramolecular structure of polymer materials; Confocal Laser Scanning Microscopy (CLSM)
4. Differential Scanning Calorimetry (DSC) and its importance for polymer materials
5. Modulated Differential Scanning Calorimetry (MDSC); Oxidative Induction Time and Temperature of polyolepines; study of semicrystalline polymers by DSC
6. Thermogravimetry (TGA) and its importance for polymer materials
7. Fourier-transformed Infrared Spectroscopy (FTIR) and its importance for polymer materials
8. Raman spectroscopy and its importance for polymer materials; bimodal polymers
9. Viscoelastic properties of polymer materials; rheology of melts
10. Dynamic-mechanical Analysis (DMA) of solid polymer materials
11. Tests of polymer materials softening used in industry; master curves from DMA
12. Morphology of liquid crystals, polymer blends, copolymers and polymer composites
13. Morphology of fractured polymer surfaces, morphology of defects in real products of polymer materials

Practice topics:
1. Introduction: Methods of direct and indirect imaging/evaluation of supramolecular structure of polymer materials and their identification; the reasons for selected methods for practicing; the practice running; the report form 2.–3. Practice: Isothermal and nonisothermal crystallization of selected thermoplastics (homopolymer and copolymer or nucleated material) performed and observed on POM
Checking the practice preparation: the entrance written test on polymer materials morphology and POM
Outcome: One report from measurement for a group (comparison of both types of crystallization for both specimens)
4.–5. Practice: Chemical etching of selected thermoplastics and imaging of etched surfaces on confocal laser scanning microscope
Checking the practice preparation: the entrance written test on methods used for uncovering of supramolecular structure and CLSM
Outcome: One report from etching and imaging for a group
6.–7. Practice: DSC of polyethylene terephthalate (PET) – the change of structure caused by cooling rate of the melt; identification of selected polymer materials, description of the change of morphology among the first and the second heating and cooling runs
Checking the practice preparation: the entrance written test on DSC and its application for polymer materials
Outcome: One report from measurement of PET and identification of polymeric materials for a group
8. Practice: FTIR-ATR of selected polymer materials, additives and reinforcements; determination/conformation of the structure; identification of selected polymer material commonly used in life
Checking the practice preparation: the entrance written test on FTIR and its application for polymer materials
Outcome: One report from measurement for a group
9.–10. Practice: Rheology of polymer melts of two selected thermoplastics; oscillation and flow measurements; the influence of branching, copolymer component and measurement conditions
Checking the practice preparation: the entrance written test on rheology of polymer melts (measurement modes and types of geometries, measuring conditions)
Outcome: One report from all measurements for a group
11.–12. Practice: Self-measurement of selected polymer material/s from industry in order to identify and/or determine the reason “good-bad” using POM, CLSM, DSC, and FTIR-ATR
Outcome: Compact and intelligible report from measurements written for “submitter” (one for a group).
13. Practice: reparative terms of practice; credit test

Guided consultation in combined form of studies

26 hod., optionally

Teacher / Lecturer

Ing. Radka Bálková, Ph.D.

Laboratory exercise

52 hod., compulsory

Teacher / Lecturer

Ing. Radka Bálková, Ph.D.
Ing. Šárka Jelínková

Elearning

eLearning: currently opened course