Material Science and Engineering

Laboratory II - Physics
 Experiments
Exp. 1. Impact Test
Exp. 2. Creep Test
Exp. 3. Abbe Refractometer
Exp. 4. Limiting viscosity
Exp. 5.Polarizing Microscope
 Laboratory II - Physics
Physics

Abbe Polarizing
Impact Test Creep Test Limiting viscosity Microscope
Refractometer

PEG PVA PTT

PP PE
.
EXP 1-Impct Test
To learn:

1.What is the main purposes of impact testing?

2.What are the two types of impact testing?

3. What are the factors affecting the impact energy?

4.How is impact test calculated?

EXP 1-Impct Test
• The momentum converted from the potential energy of the pendulum itself is
applied to knock the test piece. The energy absorbed by the test piece is
obtained and is divided by the cross-sectional area in order to get the impact
strength of the material taking advantage of the law of conservation of energy.

Figure-1
EXP 1-Impct Test

E = Intact momentum,
E1= Energy by wind resistance,
E2 = Potential energy by inertia
E、= Energy absorbed by the test piece;
W = Weight of pendulum; R= Swinging radius; I= Impact strength

 E = (COS β – COS α)WR

 E1 = [(COS β、 – COS β) + (COS α、 – COS α)]WR/2

 E2 = (COS α、 – COS Θ)WR

 E、= E – (E1 + E2)

 I = E、/A
Comparison Table of Impact Angles and Energies
Swing angle β
Energy E
(Kg-cm)
EXP 1-Impact test

1.Sample 1-ASTM PP IZOD impact testing machine

2.Sample 2
 EXP 1-Impct Test
Experiments
• Production of test piece: Cut at one-half of the test piece to make a notch as instructed in Figure 1.
Beware of the fact that the shape at the bottom of the notch shall be smooth and there shall not
be any mark that will hurt the test.
ASTM Standard Test Piece

• The depth of notch of test piece d, the thickness near notch t, and the width b need to be precise
up to 0.01 mm. Hold the test piece (trim it to an adequate thickness of 12.7±0.1 mm X length of 64±2
mm) in the test piece support.

• Fixate the pendulum head in the upright position and lock it and have the pendulum also in the
upright position. Record the upright angle α. Open and place the pendulum head. Record the rising
angle β.

Impact
orientation Notch

Post-impact pendulum position Original

pendulum Impact strength
position Graduatio calculated with
n a base thickness
of one inch
Index
plate
Pointer

Support Impact A At notch: r=0.25±0.025mm

holder position B At notch: r=1.0±0.05mm
Symmetrical plane of the
Sample thickness notch
Notch sample (random)

Figure 1
EXP 1-Impct Test
Introduce the impact tester, the
Experiments pendulum, the sample support,
and the pointer, etc.

Prepare the sample test piece Impact orientation

Test piece 1 as shown in the Notch

figure to the right (cut and

prepared)
Test piece 2-ASTM Standard
Symmetrical
plane of the notch A At notch: r=0.25±0.025mm
B At notch: r=1.0±0.05mm

Figure 1
Fixate the test piece onto the
support

Fixate the pendulum with α=150

degrees
The pendulum falls to get Angle β

α =150 degrees. Test the Check the table and introduce

unloaded pendulum to get α’ Angles α α’and β β’ obtained
The pendulum is at Angle β. The into the formula to render the
pendulum falls to get Angle β’. impact strength of the test piece.
 EXP 1-Impct Test
Records and results

Table 1. Table 2.

Sample1 Sample1
Sample2 Sample2
P.P ASTM sheet P.P ASTM sheet

Energy value(E)
Starting angle( α)

Wind resistance Impact angle (β)

loss ( E1)
Unloaded swing
angle (α’)
Inertial loss (E2)
Impact angle
unloaded swing (β’)
Impact value (I) θ of four unloaded
swings

Calculation:
EXP 2-Creep Test
To learn:

1.What is a creep test?

2. Creep test of solid materials

 EXP 2- Creep test
At a fixed temperature, materials experience deformation with time when certain external stress is applied.
Lineal polymers
When loaded, first, transient deformation
ε1 (from Point A to Point B) occurs. Then, as
time goes by, minimal high-molecular chains
start to glide and viscous flows occur. As such,
creep that begins with Point B includes rubber
elastic and plastic deformations. By Point C,
rubber elasticity is completely developed.
Thereafter, deformation shows lineal changes
and such changes are unique of purely
viscous flows. If the load is removed at Point D,
elastic deformation e1 recovers immediately
(from Point D rubber elasticity ε 2 gradually
recovers (from Point E to Point F) and plastic
deformation ε 3 cannot be recovered; it
becomes permanent deformation.
to Point E) and
Lineal polymers
Cross-linking polymers
When loaded, transient deformation occurs
(from Point A to Point B). Deformation rises along
the line with time and towards the maximum
value.
If the load is removed at Point C, it bounces
back to Point D in an instant. The amount of
recovery from deformation equals ε 1,
indicating that ε 1 is elastic deformation.
Residual deformation gradually bounces back
to zero. The residual deformation at Point D Cross-linking polymers
equals the elongation ε 2 from Point B to Point
C. This segment of deformation carries the
properties of rubber elasticity and is entropy
elasticity.
 EXP 2-Creep test
TIME-TEMPERATURE EQUIVALENT PRINCIPLE
The time–temperature superposition principle is a concept in
polymer physics and in the physics of glass-forming liquids. This
superposition principle is used to determine temperature-
dependent mechanical properties of linear viscoelastic
materials from known properties at a reference temperature.
WLF( Williams-Landel-Ferry)Equivalent :
It depends on the reference temperature Ts selected and the
product is a constant (C1·C2 ≈ 900); it has to do with the
coefficient of thermal expansion of free volume αf.

With the corresponding relationship of time versus temperature,

the mechanical properties obtained of polymers under different 3 Illustration of the superimposed curve
of plotting stress relaxation among
temperatures or different frequencies can be compared or polymer relaxation moduli obtained at
converted in order to forecast some of the results that can hardly different temperatures (T1 < T2 < T3)
be obtained directly through experiments.
−𝐶1 (𝑇−𝑇𝑆 ) 𝜏(Relaxation time at Temperature T)
𝑙𝑜𝑔𝛼 𝑇 = 𝛼T =
𝜏𝑆 (Relaxation time at Designated Temperature T𝑆 )
𝐶2 +(𝑇−𝑇𝑆 )

Where t and ts are the time needed to a certain extent of

relaxation at Temperature T and Reference Temperature Ts: C1
and C2 are the constants relevant to Reference Temperature Ts.
EXP 2-Creep Test
Material deformation

• ORDINARY ELASTIC DEFORMATION

General elastic
deformation
• THE TRANSIENT CHANGES TO THE LENGTH AND ANGLE OF THE CHAIN
WHEN POLYMERS BEAR FORCE MEET THE HOOKE’S LAW.

𝑇𝑔

High elastic • HIGH ELASTIC DEFORMATION

deformation

• THE POLYMER CHAIN EXPERIENCES CONFORMATIONAL CHANGES

THROUGH SEGMENTAL MOTION UNDER FORCE; THE MOLECULAR
CHAIN GRADUALLY SPREADS OUT.

• VISCOUS FLOW
Viscous flow 𝑇𝑓
• MOLECULES EXPERIENCE RELATIVE GLIDE MOTION AND
CANNOT RETURN TO THEIR ORIGINAL STATE.
EXP 2- Creep test
Experiments
Materials
Size of PE plastic wrap: (Sheet thickness 0.02 mm X width 20 mm X length 70 mm)
Adhesive tape, steel ruler (ruler), utility knife, standard weights 200 g & 250 g, thermostatic
oven, clip

Hang the thin pieces of the PE film

Experimental inside the thermostatic oven
Loading conditions: 200 g & 250 g
Prepare materials Test piece 1 - Hang standard weight of
Cut four pieces of PE film 200 g
Dimension Test piece 2 - Hang standard weight of
(Thickness 0.02 mm X width 20 mm X length 70 mm) 250 g

Hang the thin pieces of the PE film inside the
thermostatic oven
Test piece 1 - Hang clamping standard weight of
200 g (load)
Test piece 2 - Hang clamping standard weight of
250 g (load)
Then, set the oven temperature to 50
degrees (T2)
Observe creep of the pieces of material
Record the length of the material once
every three minutes

For the experiment, record 25 degrees

Set the oven temperature to 25 degrees first (T1) and 50 degrees
Observe creep of the pieces of material Record the length of the material (cm)
Record the length of the material once every once every three minutes
three minutes Draw the curve of deformation length
versus time
EXP 2-Creep test
Records and results

Time (mins)
Temp.(℃) 0min 3min 6min 9min 12 min 15min

200g 250g 200g 250g 200g 250g 200g 250g 200g 250g 200g 250g
25℃

200g 250g 200g 250g 200g 250g 200g 250g 200g 250g 200g 250g
50℃

18min 21min 24min 27min 30min 33min

200g 250g 200g 250g 200g 250g 200g 250g 200g 250g 200g 250g
25℃

200g 250g 200g 250g 200g 250g 200g 250g 200g 250g 200g 250g
50℃
EXP. 3 Abbe Refractometer
To learn:

1. The principle of refractive index and the application principle of Abbe

refractometer.

2. Measure the refractive index of polymer solutions

 EXP. 3 Abbe Refractometer

Snell‘s Law
𝑛1 𝑠𝑖𝑛 𝜃1 = 𝑛2 𝑠𝑖𝑛 𝜃2

𝜃1
refractive index : 𝑛1
interface
refractive index : 𝑛2

𝜃2

normal
EXP. 3 Abbe Refractometer

Total Reflection

Critical angle of
reflection 𝜃𝑐

Total reflection area

𝑛1
interface
Reflection area 𝑛2

normal
𝑛1 sin 𝜃𝑐 = 𝑛2 sin 90
𝑛1 sin 𝜃𝑐 = 𝑛2
 EXP. 3 Abbe Refractometer

 chemical medicine: Poly(ethylene glycol) (PEG) Mw 20,000,

D.I water, dropper, cylinder

 Equipments： Abbe Refractometer

 EXP. 3 Abbe Refractometer
Experiments

Insert the 589 nm light fiter. Turn on power and adjust the source of
light and align the source of light with the secondary prism glass
window.

Press the LAMP button on the lighting device and the indicator
“LAMP” on the screen of the lighting device turns to “ON”.
Through the eyepiece, one can see the image to the right. If the
orange portion is too dark, the lighting intensity and the lighting
angle may be adjusted to make it brighter.

Calibration instrument ：
Use deionized water as the standard sample. Check the table to
obtain the refractive index of the water at the current
temperature. Adjust the instrument to make it conform to the
finding obtained from checking the table.
 EXP. 3 Abbe Refractometer
Experiments

Preparation of Sample:
Dilute 10 wt% PEG solution (to be prepared by the TA) to 2.5/5/7.5 wt%.

Measure the refractive index of the deionized water and 2.5/5/7.5/10

wt% PEG solutions;
obtain three measurements for each concentration and get the
mean value.

Data analysis:
Produce the trend line with the averaged data and extrapolate it
to a concentration of 0 wt%. Compare the refractive index of
deionized water obtained.
EXP. 3 Abbe Refractometer
Records and results
Test First Second Third
Sample sol’n measurement measurement measurement Average value

D.I Water

2.5 wt%

5 wt%

7.5 wt%

10 wt%
EXP. 3 Abbe Refractometer
Records and results
1. Results plotting

2. The trend line (Excel graph), print it out, and attach it to

this page.
 EXP 4-Limiting viscosity
To learn:

1. Principle of measuring the viscosity of dilute polymer solutions.

2. Characterize the molecular weight of the polymer by measuring the viscosity of

the polymer solution.
EXP 4-Limiting viscosity - 𝜂(𝑐)

Sh e ar s t ress , τ
𝐹
 τ=𝐴

∆𝑋 Shear rate, 𝛾ሶ
∆𝑋 𝑣
 𝛾ሶ = =
𝐿𝑡 𝐿

Viscosity,𝜂
𝜏
 𝜂= (F = A𝜂𝛾,ሶ 𝑁𝑒𝑤𝑡𝑜𝑛𝑖𝑎𝑛 𝑓𝑙𝑢𝑖𝑑)
𝛾ሶ

26
EXP 4-Limiting viscosity - 𝜂(𝑐)

𝜂 𝑆 𝜂 = 𝜂 𝑆 (1 + 𝐴𝑐 + 𝐵𝑐 2 +
⋯)
27
EXP 4-Limiting viscosity - 𝜂&C

Huggins’ Equation Kraemer’s Equation

𝜂 = 𝜂 𝑠 ( 1 + 𝜂 𝑐 + 𝑘𝐻 𝜂 2 𝑐 2 + … 𝜂 = 𝜂 𝑠 ( 1 + 𝜂 𝑐 + 𝑘𝐻 𝜂 2 𝑐 2 + …
↑ ↑ ↑
理想項 溶劑 – 溶質 溶質 – 溶質

𝜂 𝜂
− 1 = 𝜂 𝑐 + 𝑘𝐻 𝜂 2𝑐 2
+ … 𝑙𝑛 = 𝑙𝑛(1 + 𝜂 𝑐 + 𝑘𝐻 𝜂 2 𝑐 2 + …
𝜂𝑠 𝜂𝑠
↑
𝜂𝑠𝑝
𝜼𝒔𝒑 𝒍𝒏 𝜼𝒓
= 𝜼 + 𝒌𝑯 𝜼 𝟐𝒄 + … = 𝜼 − 𝜷 𝜼 𝟐𝒄 + …
𝒄 𝒄

28
EXP 4-Limiting viscosity

 Materials : Polyvinyl alcohol (PVA) (Mw =10,000-22,000), Pure water

 Equipment : Cannon-Ubbelohde Viscometer
Pipet safety bulbs
Soft plug
Timer
Water bath
 EXP 4-Limiting viscosity
Experiments
Add water to a suitable level of the water
bath and set the temperature at 50 °C
Sequentially test four types of concentration
from low to high, respectively, to get the time of
the liquid to flow through two graduates and
record it.

How to operate the Ubbelohde viscometer Record the number of seconds and introduce
them into the formula. Produce the graphic and
obtain the limiting viscosity and the molecular
weight of the sample

When the temperature of the water bath reaches 50℃, add

pure water into the capillary tube and place it inside the
thermostatic tank. Test the time for it to flow through the
graduates of the capillary tube and record it.
 EXP 4-Limiting viscosity

Records and results

𝜂
relative viscosity : 𝜂𝑟 =
𝜂𝑠
Time 𝜂𝒔𝒑 𝒍𝒏𝜂𝒓
Sample 𝜂𝒓 𝜂𝒔𝒑
(sec) 𝒄 𝒄
𝜂−𝜂𝑠
specific viscosity ：𝜂𝑠𝑝 = 𝜂𝑟 − 1 =
𝜂𝑠
water

𝑙𝑛 𝜂𝑟 𝜂𝑠𝑝 0.25 wt%

Limiting viscosity: 𝜂 = 𝑙𝑖𝑚 = 𝑙𝑖𝑚
𝑐→0 𝑐 𝑐→0 𝑐
( 𝑢𝑛𝑖𝑡 𝑜𝑓 𝑐: 𝑔
Τ𝑑𝑙 ~ % ) 0.5 wt%

0.75 wt%
Mark-Houwink Eq : 𝜼 = 𝑲𝑴𝜶
for ideal solution, 𝛼 =0.5 1 wt%
for PVA solution at 30℃ , =5.9 × 10−4 , 𝛼 =0.67
31
EXP 5-Polarizing Microscope
To learn:

1.The principle and use method of polarizing microscope.

2. The crystalline state of polymers under different crystallization conditions.

3. The optical effect of the birefringent body in the polarized field and the extinction
pattern of the spheroidal black cross
 EXP 5-Polarizing Microscope

Optical depolarization : Crystalline birefringence leads to changes in strength of transmitted light

Eyepiece

Detector
Basic configuration Analyzer
of the polarizing
microscope

Objective lens
Polarizer Crystallization Analyzer

Sample
table

Polarizer
Thermoregulator

Reflector
Polarizer

Analyzer
EXP 5-Polarizing Microscope

Forming conditions of spherulite - Growth of spherulite –

extracted from thick solutions - no reduced surface energy
external force during crystallization
EXP 5-Polarizing Microscope
Materials

Poly Trimethylene
Terephthalate

Temperature

𝑇𝑔 (45𝑜𝐶) 𝑇𝑐 (55𝑜𝐶) 𝑇𝑚0 (252𝑜𝐶)

EXP 5-Polarizing Microscope
Experiments

Turn on power and adjust brightness for the polarizing Obseravation and operational steps for
microscope melting and crystallization
Operate respective functions and understand them
of the polarizing microscope

Prepare PTT sample

First clamp the round slide and then the sample
and place them on the carrier
Confirm brightness of light
Slowly turn for rough or fine adjustment. Adjust the
focus and observe the spherulite; it may be
observed on the screen or through the eyepiece
Learn to adjust the focus and observe the pattern Set Temperatures Ｔｍ＆Ｔc through two
of the spherulite on the screen heating tables, respectively, to be ready for
Record and Take Pictures temperature control

Use different spherulite test pieces and place them

on the carrier to facilitate observation Observe the spherulite of the material
Upon completion of observation, restore the
microscope to the initial instrument settings
EXP 5-Polarizing Microscope
Records and results

Attach the pictures of spherulites of different samples

observed in the figure below as the experiment results

Sample 1 Sample 2 Sample 3