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Contents
Plastic
1.1 Influence of heat treatment on polyethyleneterephthalate (PET) -- 1 1.2 Heat history of polyethertherketone (PEEK) ----- 2
TMA Measurement
8.1 Thermal stress of polyethyleneterephthalate (PET) fiber -- 23 8.2 Shrink stress of magnetic tape --------------------- 24 8.3 Softening temperature of polymethylmethacrylate (PMMA) --- 25
Electronic Materials
9.1 Thermal expansion of a printed circuit board -- 26 9.2 Decomposition of a diode --------------------------- 27 9.3 Quantification of quartz in epoxy resin ----------- 28 9.4 Melting point of lead free solder ------------------- 29
Plastic
1.1 Influence of heat treatment on polyethyleneterephthalate (PET)
s Explanation PET bottle was measured by DSC. With the original sample, the peak by melting is mainly observed at 254.8 C. It shows that the structure before heating was crystalline. On the other hand, as for DSC (2nd-heating) of an original sample which is cooled rapidly after heating, glass transition is observed at 77.6 C. Because the glass transition occurs in a non-crystalline solid, it turns out that the PET becomes non-crystalline when it is cooled rapidly. The exothermic peak at 136.8C means that the non-crystalline PET changes to the crystalline PET at this temperature. s Analytical Conditions Instrument : DSC-60 Sample Sample Amount Flow Rate Heating Rate : PET : 6.72mg : 50mL/min : 10C/min
DSC mW
5.00
PET bottle(original)
136.81C -59.75J/g
0.00
77.60C 31.49J/g
254.84C
PET bottle(2nd-heating)
-5.00
-38.86J/g 254.00C
200.00
300.00
DSC mW/mg
181.42C
1.00
PEEK film
0.00
PEEK block
-1.00
-35.71J/g 339.22C
-2.00 0.00 100.00 200.00 Temp [C] 300.00 400.00
DSC mW
nylon A
2.00
108.25C
0.00
nylon B
-2.00
102.68C 199.25C
-4.00
200.17C
200.00
DSC mW
2.00
153.24C
0.00
nylon A
147.31C
-2.00
160.47C
-4.00
nylon B
100.00
Temp [C]
200.00
[Temperature Program]
DSC mW
2.00
PS
92.39C
0.00
High-impact PS
78.29C
103.90C
-2.00
87.20C
50.00
150.00
DSC mW
2.00
PS
97.82C
High-impact PS
0.00
85.31C
-2.00
50.00
150.00
[Temperature Program]
DSC mW 2.00
1.00
PVC(A)
81.68C
0.00
PVC(B)
-1.00
73.87C
-2.00
DSC mW
0.00
1st run
307.62C
371.40C
6.15J/g
-2.00
2nd run
314.82C
-4.00
200.00
400.00
[Temperature Program]
TGA % 100.20
100.10
-0.018mg -0.058%
100.00
99.90
99.80
TGA mg
0.00
-0.167%
-1.00
50.00
150.00
10
Atmospheric Gas : N2
[Temperature Program]
TGA %
100.00
-1.146%
99.00
98.00
0.00
200.00
11
TGA %
DTA uV
100.0
TG curve
-2.428% -94.878%
100.0
50.0
-1.771%
0.0
DTA curve
0.0
222.04C 601.85C
-50.0
447.31C
0.0 200.0 400.0 Temp [C] 600.0 800.0
12
TGA %
417.69C
100.00
-10.331mg -85.734%
50.00
0.00 0.00 100.00 200.00 300.00 Temp [C] 400.00 500.00 600.00
13
TGA % 105.00
Temp C
600.00
TG
100.00
60.00min -1.448%
90.00min -1.767%
120.00min -2.026%
400.00
95.00 200.00
Temperature
0.00
14
TGA %
424.05C
100.00
-99.076%
50.00
0.00
0.00
200.00
600.00
800.00
15
TGA %
Temp C
TG
100.00
60.00min -1.846%
90.00min -5.141%
120.00min -9.170%
600.00
90.00
400.00
Temperature
80.00 200.00
0.00 150.00
16
DSC mW
Temp C
Temperature
10.00
200.00
100.00
DSC
0.00
Change from N2 to O2
78.58min
17
DSC mW 20.00
Temp C
Temperature
200.00 10.00
0.00
DSC
20.46min Change from N2 to O2
100.00
-10.00
0.00 50.00
18
TGA %
569.16C
100.00
-99.988%
50.00
0.00
0.00
200.00
600.00
19
DSC mW
1.00
169.10C
70.90C
0.00
50.76J/g
81.30C
-1.00
200.00
20
TGA %
100.00
-7.369mg -65.853%
50.00
21
TGA mg
DTA uV
TG curve
0.0
2000
-68.405%
-10.0
-28.162%
1000
-20.0
-30.0
DTA curve
0 -40.0 0.0 10.0
497.01C
20.0 Time [min] 30.0 40.0
22
TMA Measurement
8.1 Thermal stress of polyethyleneterephthalate (PET) fiber
s Explanation Thermal stress measurement is the method which measures the strength of stress to the change of temperature after giving a constant strain to a sample and maintaining the rate of strain, and can know size stability, form stability, etc. Here, PET fiber was measured. 1% of strain was given to the sample and heated. The increase in stress is observed from 97.6C. This was caused by the shrinkage of strained fiber. In case of the sample that was made by being strained and oriented, if it exceeds the processing temperature at the time of drawing, the orientation is canceled and the shrinkage is observed. After that, the stress decreases gradually, and the sample melts near 255C,then the stress becomes 0. s Analytical Conditions Instrument : TMA-60 Sample : PET fiber Sample Length : 15.25mm [Temperature Program] Heating Rate : 10C/min
LOAD g 20.00
141.05C
97.64C
10.00
254.76C
23
LOAD g 40.00
30.00
194.17C 27.23g
20.00
10.00
0.00
100.71C
-10.00 100.00 Temp [C] 200.00 300.00
24
TMA Measurement
8.3 Softening temperature of polymethylmethacrylate (PMMA)
s Explanation Penetration measurement can be used as an index that mainly estimates the softening temperature and the heat modification temperature of plastic material. Here, the softening temperature of PMMA was measured. It turns out that softening of a sample has occurred from near 111.6C. s Analytical Conditions Instrument : TMA-60 Sample : PMMA Sample Length : 10.03mm [Temperature Program] Heating Rate : 5C/min
TMA um 100.00
111.56C
50.00
0.00
100.00
25
Electronic Materials
9.1 Thermal expansion of a printed circuit board
s Explanation With the parts with which an epoxy resin is joined to metal like a printed circuit board or IC, a coefficient of thermal expansion becomes important. Here, the expansion curve of a printed circuit board is shown. The inflection point of glass transition is observed near 90C, and it turns out that the coefficient of thermal expansion is changing remarkably before and behind it. s Analytical Conditions Instrument : TMA-60 Sample : Printed circuit board Sample Length : 10.01mm [Temperature Program] Heating Rate : 5C/min
TMA % 3.00
2.00
1.00
0.00
26
Electronic Materials
9.2 Decomposition of a diode
s Explanation The diode of semiconductor parts was measured. A part of component which constitutes the diode is melting near 225C, and decomposition has started from near 300C. s Analytical Conditions Instrument : DTG-60 Sample Sample Amount : Diode : 10.1mg
TGA %
DTA uV 400.00
TG curve
100.00
-58.752% 489.84C
300.00
50.00
-13.178%
200.00
435.37C
100.00 0.00
DTA curve
225.85C
0.00 100.00 200.00
361.31C
0.00
-50.00
400.00
500.00
600.00
27
TGA %
DTA uV 150.0
TG curve
100.0
489.9C
-33.83%
100.0
50.0 50.0
DTA curve
84.9C
0.0
358.3C
0.0 200.0 400.0 Temp [C]
425.1C
579.9C
600.0
28
Electronic Materials
9.4 Melting point of lead free solder
s Explanation Development of the lead free solder that does not contain a lead from the problem of the environmental pollution is performed. Here, melting point of the lead free solder with which the conventional Sn-Pb solder differs from composition ratio of components was measured. Although, as for the solder containing a lead, melting was observed at 182.3C, with lead free solder, melting was observed at 209.2C and 217.5C. s Analytical Conditions Instrument : DSC-60 Sample (Fig.9.4.1) : Solder Sample Amount Sample Amount Sample Amount : 11.26mg : 10.38mg : 10.71mg Sample (Fig.9.4.2) : Lead free solder Sample (Fig.9.4.3) : Lead free solder Atmospheric Gas : N2 [Temperature Program] Heating Rate : 10C/min
182.25C
4.00
3.00
2.00
1.00
29
209.23C
-2.00
-4.00
217.54C
-2.00
-4.00
30
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