Lecture 4:Characterizing Hybrids

First step in characterizing a hybrid:

• Use your senses (take pictures to document)– What color? Does it fluoresce – Transparent or opaque?– Homogeneous in appearance?– Solid or liquid– Tacky or sticky or brittle or tough

• Mass – compare with theoretical yield

Describe the material below

Describe the material below

Second, try and dissolve the hybrid in different solvents

• Water, ethanol, benzene, methylene chloride, tetrahydrofuran, acetonitrile, hexane, acetone, diethyl ether, dimethyl sulfoxide, N-methyl pyrrolidone (NMP)

• Leave it at room temp overnight. Look for swelling if not dissolved.

• Boil solvent for 4 hours.• If it doesn’t dissolve its probably cross-linked or

really crystalline

Types of Polymers & solubility

Won’t dissolveWill dissolve

Third, Structural Characterization of soluble polymers

• 1H & 13C & 29Si Nuclear Magnetic Resonance and infrared spectroscopy

• Molecular weight by gel permeation chromatography

• Composition by combustion analyses• X-ray diffraction on film or powder• Viscosity of dilute solutions- shape of polymer

X-ray diffraction

Semi-crystalline polymer shows diffraction rings

amorphous materials shows diffuse band

Or third, Structural Characterization of insoluble polymers

• Harder to characterize• Does it burn (many inorganics do not)• Solid state 1H & 13C & 29Si Nuclear Magnetic

Resonance and infrared spectroscopy• Composition by combustion analyses• X-ray diffraction on film or powder• X-ray fluorescence if inorganic

Literature procedure:

See how experimentals are written in good papers. Use them as model

Template for lab notebook:

Template for research labnotebook:

Morphological Characterization of polymers

• If opaque or transluscent, SEM and optical microscopy (bifringence)-crystalline or amorphous & more.

• Fracture polymer and look at fracture surfaces• Look for phase separation (like immiscible block

copolymers)• Look for long range order• Look for pores

Thermal characterization of polymers

• Thermal gravimetric analyses (TGA) – determines decomposition temperature

• Differential scanning calorimetry (DSC)– detects phase changes (melting or glass transition temperatures) or chemical reactions

DSC analysis

Thermal gravimetric analysis

Mechanical characterization of polymers

• Stress-strain curves:– Young’s modulus (brittleness)– Tensile strength-pull sample appart – Flexural strength- bend until it breaks– Compressive strength-crush sample

• Dynamic mechanical analyses (same info as above but with cyclic application of stress or strain.– Generate modulus temperature curves– Fatigue studies to predict failure under cyclic stress

Stress-Strain Analysis

Not every polymer needs all of these analyses, but structure is the most

basic and important• Known (described in literature) polymers

need less structural characterization. Often just IR and Mw from GPC.

• New polymers need complete structural characterization: NMR, IR, Combustion analysis, GPC, solubility, glass transition temp and/or melting point.

Morphological and Mechanical studies are dependent on research interests.

• If you are interested in strong polymers, then morphological, mechanical & thermal studies are important

• Other applications requiring morphological, mechanical & thermal studies would include preparation and testing of 1) membranes, 2) coatings, 3) paint, 4) polymer foams, 5) organic photovoltaics, 6) OLED’s, 7) adhesives and 8) low friction coatings

Other polymer properties that are important for specialty polymers

• Coatings, packaging, membranes, Photovoltaics & OLED’s; gas and water permeability should be measured.

• Battery and fuel cell membranes: gas & water permeability and ion conductivity

• Dielectrics, wiring insulation: dielectric and electrical conductivity

• Fabrics & building materials: fire resistance• Any polymer used in sunlight or radiation or in the

presence of chemicals: resistance to oxidative degradation.