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博碩士論文 etd-0701113-211213 詳細資訊
Title page for etd-0701113-211213
論文名稱
Title
雷射脈衝於水或四乙基矽酸鹽中合成鋯鈦氧化物與碳化物及其微觀組織與光譜分析
Synthesis and microstructure/optical property analyses of Zr/Ti oxide and carbide by laser pulses in water or tetraethyl orthosilicate
系所名稱
Department
畢業學年期
Year, semester
語文別
Language
學位類別
Degree
頁數
Number of pages
168
研究生
Author
指導教授
Advisor
召集委員
Convenor
口試委員
Advisory Committee
口試日期
Date of Exam
2013-07-17
繳交日期
Date of Submission
2013-08-01
關鍵字
Keywords
二氧化鋯、脈衝雷射剝蝕、核殼結構、晶向關係、銳鈦礦、聚炔烴、石墨烯
ZrO2, crystallographic relationship, polyyne, graphene-based lamellae, anatase, core-shell, pulsed laser ablation
統計
Statistics
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The thesis/dissertation has been browsed 5717 times, has been downloaded 53 times.
中文摘要
本實驗利用不同能量的脈衝雷射剝蝕金屬鋯靶、碳靶以及鈦靶,分別在水中及四乙氧基矽烷溶液中(TEOS)合成鋯鈦氧化物及碳化物。本實驗利用掃描及穿透式電子顯微鏡觀察奈米凝聚物的成分、形狀、晶體結構以及相變化等行為,並以吸收光譜、拉曼光譜、霍式紅外光譜儀和X-ray光電子能譜儀為輔,研究其在動態環境下合成時的能隙、鍵結、價數改變等情形。

首先是利用高能量雷射在水中剝蝕鋯靶合成氫化的c-, t-, m-ZrO2奈米凝聚物。在受到H+,Zr2+,Zr3+的影響下,藉由電子顯微鏡觀察到這些奈米凝聚物,表面富含{111}和{100}的階檻,並且在晶體內部沒有雙晶或疊差出現。此外,二氧化鋯進行麻田散鐵相變化的臨界粒徑大小約為20 nm,而吸收光譜並顯示其能隙值略微縮小至5.2-5.3 eV。

其次,將鋯靶置於TEOS溶液中並以長脈衝雷射剝蝕之,可得到c-, t-, m-ZrO2奈米凝聚物及以C-Si-H為主要成分的亂層層狀結構(turbostratic lamellae)。其中粒徑大小3-10nm,形狀為立方八面體的c-ZrO2比起常溫壓下的更為緻密(~10%)。粒徑更大的c-ZrO2與亂層層狀結構可進一步形成核殼結構,因而使內部受到一定大小的壓應力。另外,在穿透式電鏡觀察下亦可看到少數萊氏石(reidite)。

接著,若把碳靶置於TEOS溶液中進行雷射剝蝕會產生以碳的單、參鍵交替連結所形成的聚炔烴(polyyne)和參雜Si、H的石墨烯為基底的層狀結構。由UV-vis吸收光譜的多重吸收峰,我們可得知聚炔烴所形成的碳鏈可長達C16H2。石墨烯為基底的層狀結構會藉由皺紋至褶層(wrinkle to fold)的轉變以及不完美的接合生長而產生階級式的褶層(hierarchical folds)和差排。此外,層狀結構會組裝成為奈米緞帶碳(nanoribbons),在拉曼光譜的佐證下,可知道其含有高比例的sp3鍵結,我們可將其歸因於毛細現象(capillarity effect)和Si-H溶質陷入效應(solute trapping)所造成的。

再者,在TEOS溶液中剝蝕金屬鈦靶,從穿透式電鏡觀察顯示其主要分為大小兩種粒徑的奈米顆粒。其中,小粒徑主要為TiCxOy外面包裹著亂層石墨烯;而較大粒徑的顆粒則是富含缺陷的銳鈦礦結構TiO2,是藉由TiCxOy和β-Ti去穩定其結構並且形成特定的晶向關係。另外,銳鈦礦受到溶質陷入的影響也會在特定面上產生有序結構。

進一步以高分辨電鏡影像去觀察銳鈦礦顆粒間的特殊晶界,可發現其會有以[100]為軸的對稱傾斜晶界,且可分別以(001)和(01-1)面當成其界面。事實上,傾斜晶界亦可視為基面雙晶且擁有整合(001)和半整合(01-1)的界面,而此基面雙晶可藉由向量 = 1/2[0-10]+1/4[00-1]形成或消失。再者,銳鈦礦亦存在著以[1-10]為軸的非對稱傾斜晶界,其以(11-2)/(001)當成異質界面。

最後,同樣利用高分辨電鏡觀察到金紅石(Rt)和板鈦礦(Brk)所組成的核殼結構,其依循著[001]Brk//[111]Rt; (0-20)Brk//(2-1-1)Rt特定的晶向關係,跟本文藉由過去文獻所提到銳鈦礦/金紅石和銳鈦礦/板鈦礦的晶向關係所推論出來的結果不同。藉由計算晶格面的匹配程度,本文所觀察到的晶向關係是可以合理的存在,並且這樣的球面界面可使得表面能和應變能降到最低。
Abstract
This thesis is divided into seven chapters dealing with the synthesis and phase/microstructure characterizations of the condensates fabricated by pulsed laser ablation (PLA) of some bulk targets in liquid. In chapter 2 and 3, PLA of bulk Zr in water and a specific organic solvent (i.e. tetraethyl orthosilicate, TEOS) were comparatively studied, which triggered further researches on PLA of bulk graphite (chapter 4) versus Ti (chapter 5 to 7) in TEOS, for novel synthesis of organic/inorganic composites with special structures, compositions and optical properties as addressed in turn.

In chapter 2, PLA of Zr plate in water under Q-switch mode and a fluence of 700 and 800 mJ/pulse for a rather high power density of 1.5×1011 and 1.7 × 1011 W/cm2, respectively was employed to fabricate ZrO2 nanocondensates. X-ray diffraction and transmission electron microscopic observations indicated such nanocondensates are full of {111} and {100} facets and predominantly in monoclinic (m-) rather than cubic- (c) and/or tetragonal (t-) crystal symmetry in particular when fabricated at 700 mJ/pulse. The hydrogenated ZrO2 nanocondensates underwent martensitic t→m transformation at a rather small critical size (ca. 20 nm) due to H+ signature and hence oxygen vacancy deficiency in the lattice. The resultant m-phase was free of twin and fault due to site saturation and rather limited growth of the nanosized particles. Spectroscopic characterizations indicated that the nanocondensates have a significant internal compressive stress, (H+, Zr2+, Zr3+) co-signature and hence a smaller band gap of 5.2-5.3 eV for potential applications in UV region.

By comparison, a turbostratic C-Si-H lamellar phase with 0.35~0.39 nm interspacing and ZrO2 condensates having c-, t- and m- structure stabilized by increasing particle size were synthesized by PLA of Zr plate in TEOS and characterized by X-ray/electron diffraction and optical spectroscopy in chapter 3. The c-ZrO2 phase ca. 10% denser than the ambient lattice was stabilized as 3-10 nm sized cubo-octahedral nanoparticles but as abnormal large-sized (up to 30 nm) ones when encapsulated by the C1-xSix:H multiple shell with defective graphite-like structure units to exert an effective compressive stress. The potential application of such core-shell nanostructure with enhanced binding of Zr and O ions and implication for natural dynamic occurrence of the C1-xSix:H phase are addressed. The reidite-type ZrSiO4 occasionally occurred as nanoparticle with (010) and (11-2) facets shedding light on the dense compound formation in natural dynamic settings.

In chapter 4, polyynes and graphene-based lamellae doped with both Si and H were synthesized simultaneously by PLA of bulk graphite in TEOS for optical spectroscopy and X-ray/electron diffraction characterizations. The polyyne molecules have long carbon chains (up to C16H2) to give multiple ultraviolet absorptions. The graphene-based lamellae were assembled as nanoribbons having hierarchical folds and dislocations due to wrinkle-to-fold transitions and imperfect attachment growth of the lamellae. A rather high fraction of sp3 bonds in the nanoribbons, as manifested by Raman shift, can be ascribed to capillarity force and Si-H solute trapping under the influence of particle size and lattice imperfections. The implications of the present composite phases on the natural dynamic occurrence and potential engineering applications are discussed.

By comparison as endeavored in chapter 5, titanium oxides doped with C and H were fabricated by pulsed laser ablation of Ti in tetraethyl orthosilicate and characterized by transmission electron microscopy. The doped titanium oxides showed bimodal size distribution, the finer faceted ones being TiCxOy of rock salt-type structure encapulated with turbostratic graphene lamellae, and the larger spherical ones, anatase with (hkl)-specific ordering and faulting/twinning due to solute (Ti2+, C and H) trapping, phase transformation and/or deformation. The defective anatase was stabilized and nucleated from paracrystalline β-Ti and TiCxOy nuclei following specific crystallographic relationships. The colloidal suspension containing such composite condensates showed visible absorbance for potential photocatalytic applications.

The anatase nanocondensates with commensurate superstructure as prepared by pulsed laser ablation of Ti in tetraethyl orthosilicate were identified by transmission electron microscopy to have special grain boundaries, i.e. symmetrical [100] tilt boundaries with (001) or (01-1) interface and asymmetrical [1-10] tilt boundary with (11-2)/(001) heterointerface. The [100] tilt boundaries are in fact about basal twinning with a coherent (001) and a semi-coherent (01-1) interface, respectively, both following the Burgers vector =1/2[0-10]+1/4[00-1]. The (11-2)/(001) heterointerface is decorated with {101} ledges, both having a primitive coincidence site lattice for fair lattice coherency. These special grain boundaries can be rationalized by the (hkl)-specific rotation/coalescence of the crystalline nanocondensates.

Finally, in chapter 7, titania nanocondensates as fabricated by pulsed laser ablation of Ti in tetraethyl orthosilicate were occasionally characterized by transmission electron microscopy to have a rutile-brookite (Rt-Brk) core-shell structure. Lattice imaging of the core-shell showed a definite crystallographic relationship [001]Brk//[111]Rt; (0-20)Brk//(2-1-1)Rt, which is different from that inferred from the reported anatase/rutile and anatase/brookite relationships. The real relation has fair +/- mixed match for multiple lattice plane pairs across a spherical interface to minimize strain energy and interfacial energy. The nucleation and growth of rutile single crystal, with 2x(10-1) and 2x(1-21) superstructure, from the core of brookite nanoparticle can be rationalized by the capillarity effect under the influence of radiant heating upon laser pulses in liquid.
目次 Table of Contents
Contents
中文摘要 i
Abstract iii
Contents vi
List of Figures x
List of Appendixes and Tables xx
List of Supplements xxiii


Chapter 1
Research outline and background

Chapter 2
Surface modification, martensitic transformation, and optical properties of hydrogenated ZrO2 nanocondensates via pulsed laser ablation in water

2-1. Introduction 3
2-2. Experimental 4
2-3. Results 5
2-3.1. Phases and composition of the condensates identified by XRD and SEM 5
2-3.2. Microstructures of the condensates revealed by TEM 6
2-3.3. Spectroscopic analysis of the condensates 7
2-4. Discussion 9
2-4.1. Effect of OH- group on the phase selection of ZrO2 nanocondensates 9
2-4.2. Site saturation and twin free t→m- transformation of ZrO2 nanocondensate 10
2-4.3. Narrower band gap of hydrogenated ZrO2 nanocondensates 11
2-5. Conclusions 12

Chapter 3
On the densification of cubic ZrO2 nanocondensates by capillarity force and turbostratic C–Si–H multiple shell

3-1. Introduction 29
3-2. Experimental 30
3-3. Results 31
3-3.1. Phase, Structure and composition of the condensates 31
3-3.2. Spectroscopic characteristics of the condensates 33
3-4. Discussion 34
3-4.1. phase selection and structure units of turbostratic C1-xSix:H shell around ZrO2 condensates 34
3-4.2. Shape of the c-ZrO2 nanocondensates 36
3-4.3. Effect of capillarity force and turbostratic shell on the densification of c-ZrO2 36
3-4.4. Implications 37
3-5. Conclusions 38

Chapter 4
Polyynes and flexible Si-H doped carbon nanoribbons by pulsed laser ablation of graphite in tetraethyl orthosilicate

4-1. Introduction 52
4-2. Experimental 53
4-3. Results 54
4-3.1. XRD 54
4-3.2. UV-visible absorbance 54
4-3.3. Raman probe 55
4-3.4. XPS 56
4-3.5. TEM-EDX 56
4-4. Discussion 58
4-4.1. Co-genesis of polyynes and Si-H doped graphene-based lamellae 58
4-4.2. Defects due to attachment growth and bending of the lamellar condensates 59
4-4.3. sp3 bonds due to solutes and lattice imperfections in the turbostratic lamellae 59
4-4.4. Implications 60
4-5. Conclusions 61

Chapter 5
TiCxOy stabilized anatase by pulsed laser ablation of Ti in tetraethyl orthosilicate

5-1. Introduction 74
5-2. Experimental 75
5-3. Results 76
5-3.1. XRD 76
5-3.2. Optical spectroscopy 76
5-3.2.1. Raman probe 76
5-3.2.2. UV-visible absorbance 77
5-3.3. Microstructures and crystallographic relationships of phases revealed by TEM 77
5-3.3.1. TiCxOy nanoparticles with C1-xSix:H shell and paracrystalline defect clusters 77
5-3.3.2. Anatase particles with defects and epitaxial phases 78
5-4. Discussion 79
5-4.1. Phase transformation path in the PLA process 79
5-4.2. Lattice mismatch-controlled interphase interface of titanium suboxides and anatase 81
5-4.3. Type and cause of defects in β-Ti, TiCxOy and anatase with dopants 81
5-4.4 Implications 83
5-5. Concluding remarks 84

Chapter 6
Special grain boundaries of ordered anatase nanocondensates by oriented attachment

6-1. Introduction 98
6-2. Experimental 98
6-3. Results and discussion 99
6-3.1. Transmission electron microscopic observations 99
6-3.2. Octahedra configuration for the coherent and semicoherent twin boundaries 99
6-3.3. Coincidence site lattice of special interfaces 101
6-3.4. Brownian motion and (hkl)-specific coalescence of anatase nanocondensates to form special interfaces 101
6-4. Conclusions 103

Chapter 7
On the crystallographic relationships between rutile and brookite

7-1. Introduction 116
7-2. Experimental 117
7-3. Results and Discussion 117
7-3.1. Crystallographic relationship revealed by TEM 117
7-3.2. Crystallographic relation selection by fair lattice match 118
7-3.3. Surface energy dependent shape and phase of titania 118
7-3.4. Expanding spherical interface for rutile core growth 119
7-4. Concluding remarks 120

References 128
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