Solvent-Induced Crack and Crack Healing in Poly(Methyl Methacrylate)

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研究生：	吳憲俊 Wu, Hsien-Chun
論文名稱：	Solvent-Induced Crack and Crack Healing in Poly(Methyl Methacrylate) 有機溶劑在聚甲基丙基酸甲酯裡引發裂紋與裂紋癒合之行為研究
指導教授：	李三保 Lee, Sanboh
口試委員:
學位類別：	碩士 Master
系所名稱：	工學院 - 材料科學工程學系 Materials Science and Engineering
論文出版年：	2009
畢業學年度：	97
語文別：	英文
論文頁數：	53
中文關鍵詞：	裂縫、2-乙基己醇、甲醇、溶劑引發應力、聚甲基丙基酸甲酯
外文關鍵詞：	crack, 2-ethylhexyl alcohol, methanol, solvent-induced stress, PMMA
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在過去的文獻裡，高分子擴散行為和溶劑在高分子內引發的硬力已經被深入研究。在這個實驗裡，我們利用重量、厚度與傅立葉紅外光轉換光譜（PMMA）發現2-己基乙醇可以快速的將甲醇從聚甲基丙基酸甲酯（PMMA）抽出，同時在PMMA表面產生裂紋。我們利用光學顯微鏡（OM）觀察在不同的實驗參數條件下對於裂紋的影響（如：溶劑的浸泡時間與浸泡溫度），不同的浸泡時間與浸泡溫度會造成不同的裂紋密度與深度。我們藉由拉伸試驗將裂紋對PMMA的破壞程度量化並且利用電腦軟體ImageJ計算裂紋密度與量測裂紋深度。
溶劑引發高分子裂縫癒合在過去也已經被廣泛的研究，在這個實驗當中我們也用甲醇使裂縫癒合並用拉伸試驗量化癒合的程度。我們發現PMMA可以癒合到近乎原始的強度。在本實驗最後的部份，我們會在甲醇癒合的部份加入染劑使裂縫癒合完後裂縫會有顏色。這個過程未來也許可以被應用於微顆粒在PMMA表面的嵌鑲。

Diffusion in polymer and solvent-induced stresses has been well
investigated in the past. In this experiment, we found that 2-ethylhexyl alcohol
could rapidly extract methanol from PMMA by mass measurement, thickness
measurement and FTIR spectrum. Crack formed during methanol desorption.
We observed the crack growth with optical microscope (OM) and studied
different parameters affected crack growth like immersion tempersture and
immersion time. Different immersion times and immertion temperatures
carried out different crack densities and crack depths. We utilized tensile test
to quantify the extent of crack destruction on specimens and the software
ImageJ to calculate the crack density and crack depth.
Crack healing in PMMA with solvent has been proposed. We heals the
cracked specimen with methanl at different temperatures and utilized tensile
test to quantify the extent of crack healing. The healing rate increases with
increasing temperature. Finally. we used mixture of methanol with dye to heal
the cracked specimen which is possiblely applied for embedding particles in
polymer.

Content
中文摘要： ...........................................................6
Abstract: .............................................................7
1.Introduction.
....................................................... 8
2.Experimental procedure:.
................................ 12
2.1.Material:.
............................................................................12
2.2.Sample Preparation:.
........................................................12
2.3.Methanol absorption：
.................................................... 13
2.4.Methanol desorption:.
......................................................14
2.5.Surface morphology by SPM (Scanning Probe
Microscope):.
.......................................................................... 14
2.6.Mass measurement:
.........................................................14
2.7.Thickness measurement:
................................................ 15
2.8.FTIR spectrum measurement:
.........................................15
2.9.Observation of Crack pattern and cross section view of
crack :.
..................................................................................... 16
2.10.Crack density and crack depth calculation:
................ 16
2.11.Tensile test:.
....................................................................17
2.12.DSC(Differential Scanning Calorimeter,) measurement
..................................................................................................17
2.13.Methanol induced crack healing.
..................................18
2.14.Healing with dye.
............................................................19
3.Result and discussion.
.................................... 20
3.1.Rapid desorption of methanol by 2-ethylhexyl alcohol
and crack formation:
..............................................................20
3.2.Mass measurement and thickness measurement during
methanol desorption:.
............................................................20
3.3.FTIR spectrum measurement:
.........................................21
3.4.Mechanism of Crack formation:
......................................21
3.5.Relationship between crack growth and immersion
parameter of 2-ethylhexyl alcohol:.
...................................... 22
3.6.Crack pattern varies with immersion time of 2-
ethylhexyl alcohol:.
................................................................ 22
3.7.Crack depth verus immersion time of 2-ethylhexyl
alcohol:.
...................................................................................23
3.8.Crack growth verus immersion temperature of 2-
ethylhexyl alcohol:.
................................................................ 24
3.9.Relationship between amount of methanol absorption
and crack growth.
...................................................................25
3.10.Crack pattern varies with immersion time of methanol:
..................................................................................................26
3.11.Crack growth verus immersion time of methanol:.
.....26
3.12.Crack healing and application.
..................................... 28
4.Figure.
............................................................... 30
Figure 1: Dimension of tensile specimen
............................................. 30
Figure 2: desorption of methanol in specimen versus time during
immersion in 2-ethylhexyl alcohol at different temperatures(m0≈ 2.3 g,
3
before immeres in 2- ethylhexyl alcohol, specimen was immersed in
methanol for 25min at 50°C)
................................................................ 31
Figure 3: thickness decrement of PMMA immersed in methanol during
immersion in 2-ethylhexyl alcohol at different temperatures (B0~3.0
mm, before immersion in tensile 2- ethylhexyl alcohol, specimen was
immersed in methanol for 25min at 50°C)
............................................32
Figure. 4: FTIR spectrum of PMMA for absorption and desorption of
methanol..
............................................................................................ 33
Figure 5: crack growth of PMMA varies with increasing immersion time
of in 2-ethylhexyl alcohol at 30°C.(PMMA was immersed in methanol
for 25 min at 50°C befroe immersed in 2-ethylhexyl alcohol)
.............. 34
Figure 6: crack densityh of PMMA varies with increasing immersion
time of in 2-ethylhexyl alcohol at 30°C.(PMMA was immersed in
methanol for 25 min at 50°C befroe immersed in 2-ethylhexyl alcohol)
.............................................................................................................35
Figure 7: crack growth with time of immersion in 2-ethylhexyl alcohol at
30°C(square specimen; PMMA was immersed in methanol for 25 min
at 50°C befroe immersed in 2-ethylhexyl alcohol) (cross-section view)
.............................................................................................................36
Figure 8: Crack pattern varies with immersion time in methanol and in
immersed in 2-ethylhexyl alcohl at different immersion temperature for
60 min..
................................................................................................ 37
Figure 9: crack density as a function of immersion times of methanol
and different immersion temperatures of 2- ethylhexyl alcohol.
...........38
Figure 10: SPM surface scanning of crack (tensile specimen; PMMA
was immersed in methanol for 1 min at 50°C and then immersed in
2EA for 60 min at 50°C).
...................................................................... 39
Figure 11: Tensile strength varies with time of immersion in methanol
and immersion temperature in 2-ethylhexyl alcohol.
............................40
Fig. 12: side view of crack at different immersion times in methanol and
different immersion temperatures in 2EA.
............................................41
Figure 13: Crack depth varies with immersion time in methanol and
immersion temperature in 2-ethylhexyl alcohol
....................................42
Figure. 14: DSC measurement of surface thin film of PMMA absorbed
methanol for 5 min
............................................................................... 43
Figure 15: Tensile stress versus immersion time in methanol healing at
different temperature..
..........................................................................44
4
Figure 16 Tensile stress versus immersion time in methanol at 60°C
under different cracking condition (5 min, 15 min, 40 min immersion in
methanol at 50°C then 60 min immersion in 2EA at 30°C)
...................45
Figure 17:.
..............Crack healing; (a) cracked specimen before healing
(Cracked specimen of PMMA was immersed in methanol for 3 min at
50°C and then immersed in 2-ethylhexyl alcohol for 60 min at 50°C), (b)
cracked specimen after healing.(healing with methanol for 20 min at
50°C)..
.................................................................................................. 46
Figure 18:.
.Crack healing with mixture of methanol with ink. (a) cracked
specimen before healing (Cracked specimen of PMMA was immersed
in methanol for 15 min at 50°C and then immersed in 2-ethylhexyl
alcohol for 60 min at 50°C), (b) cracked specimen after healing.(healing
with mixture of methanol and ink for 20 min at 50°C).
..........................47
5.References:
.......................................................48
6.Conclusions:.
....................................................52

                                

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