abcit characterization of polyammides. abcit 3 methods p infrared spectroscopy p differential...

Characterization of PolyammidesCharacterization of Polyammides

3 methods3 methods

Infrared SpectroscopyInfrared Spectroscopy Differential Scanning CalorimetryDifferential Scanning Calorimetry Dynamic Mechanic AnalysisDynamic Mechanic Analysis

Infrared SpectroscopyInfrared Spectroscopy

We send an infrared beam We send an infrared beam on the sampleon the sample

The radiation will be The radiation will be attenuated only at specific attenuated only at specific wavelenghtswavelenghts

The graph is called The graph is called Spectrum and is a Spectrum and is a “fingerprint” of every “fingerprint” of every moleculemolecule

PA 6PA 6

4000.0 3000 2000 1500 1000 630.0

2.8

20

40

60

80

99.7

cm-1

%T

3296.45

3082.50

2933.19

2861.77

1637.50

1541.33

1460.951437.50

1370.83

1261.301200.94

1170.09

1118.56

1074.34

974.46

929.67

830.80

685.91

PA 6,6PA 6,6

4000.0 3000 2000 1500 1000 630.0

3.110

20

30

40

50

60

70

80

90

101.8

cm-1

%T

3298.45

3071.87

2933.19

2861.04

1635.18

1538.06

1465.04

1418.371370.551274.35

1200.08

1065.05935.20

872.23

829.63

797.44

689.97

Overlay of PA 6 and 6,6Overlay of PA 6 and 6,6

1786.7 1700 1600 1500 1400 1300 1200 1100 1000 912.6cm-1

%T

PA 6

PA 6 61635.18 1538.06

1465.04 1418.371370.55 1274.35

1200.08

1065.05935.20

1637.50 1541.33

1460.95

1437.501370.83

1261.30

1200.94

1170.09

1118.56

1074.34974.46

929.67

Differential Scanning CalorimetryDifferential Scanning Calorimetry

DSC of PA 6DSC of PA 6

DDSC of Nylon:Heat Flow and Storage Cp

Figure 2

Temperature (°C)

Heat Flo

w (m

W)

Specifi

c H

eat (J

/g°C

)

Storage Cp

Heat Flow

Onset 78.43°C

Peak 56.41°C

H 69.17 J/g

Tg 90.01°C

Cp 0.153 J/g°C

0.0 25.0 50.0 75.0 100.0 125.0 150.0

0.0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1.0

1.6

1.8

2.0

2.2

2.4

2.6

2.8

Tue Apr 4 10:14:20 1995

Heat F

low

(m

W)

S2 std.pans Applications LabTemperature ( C)

Curve 1: DDSC in DDSC ModeFile info: nylon003 Mon Mar 20 11:09:31 1995Sample Weight: 6.171 mg

nylon floss, 1st heat

PERKIN-ELMER7 Series Thermal Analysis System

Temp 1:-30.0 C Time 1: 30.0 s Rate 1: 4.00 C/min Temp 2:-28.0 C

Segment: Iso-Scan Repeated 100 times

End:170.0 C Time: 100.0 min

nylon floss, 1st heat

Specific

Heat

(J/g

C)

StepScan DSC of NylonStepScan DSC of Nylon

Nylon 6 polymers yield simultaneous moisture evolution peak Nylon 6 polymers yield simultaneous moisture evolution peak and plasticized Tgand plasticized Tg

Standard DSC has difficulty detecting plasticized Tg because Standard DSC has difficulty detecting plasticized Tg because of moisture peakof moisture peak

StepScan DSC can separate out the moisture evolution peak StepScan DSC can separate out the moisture evolution peak (‘slow’ process) from the Tg (‘fast’)(‘slow’ process) from the Tg (‘fast’)

StepScan DSC of Ambient Humidity Nylon 6 FibersStepScan DSC of Ambient Humidity Nylon 6 Fibers

StepScan DSC of Saturated Nylon 6 FibersStepScan DSC of Saturated Nylon 6 Fibers

StepScan DSC of Dry Nylon 6 FibersStepScan DSC of Dry Nylon 6 Fibers

Dynamic Mechanic AnalysisDynamic Mechanic Analysis

A typical DMA curve...A typical DMA curve...

PA 6PA 6

RH20%

RH0%

RH40%

RH60%

RH80%

Ｔ

RH80%

RH20%RH0%

RH40%RH60%

Ｔ

PA 12PA 12

Moisture effect on DMA of PA 6 and 12Moisture effect on DMA of PA 6 and 12

Frequency effect on ModulusFrequency effect on Modulus

ＰＭＭＡ　（ 0.01 ～ 100Hz ）