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博碩士論文 etd-0616115-022254 詳細資訊
Title page for etd-0616115-022254
論文名稱
Title
鎳分別於四乙基正矽酸鹽和氨水中經脈衝雷射剝蝕後之相變化行為及缺陷微觀組織
Phase transformation and resultant defect microstructures by pulsed laser ablation of nickel in TEOS versus aqueous ammonia
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
109
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
2015-06-11
繳交日期
Date of Submission
2015-07-21
關鍵字
Keywords
氧化鎳、岩鹽結構、四乙基正矽酸鹽及氨水、電子顯微鏡、振動/吸收光譜、X光光電子能譜、形狀、奈米凝聚物、脈衝雷射剝熔蝕
NH4OH, aqueous ammonia, nanocondensates, shape and superstructure, x-ray/electron diffraction, nickel oxide, vibration and absorption spectroscopy, rocksalt structure, pulsed laser ablation in TEOS
統計
Statistics
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中文摘要
本實驗第一部分,以高能量Nd-YAG脈衝雷射(波長1064nm-FR模式1000mJ /pulse) 於四乙基正矽酸鹽中剝溶蝕純鎳靶,產生佈植碳、矽、氫元素,因而具有由岩鹽結構序化為特殊超晶格的Ni1-xO次微米凝固顆粒與石墨烯奈米凝聚物,散佈於非晶質Si-C-O-H物質之中。這些特殊超晶格,包括沿著岩鹽母結構的 主軸<100>形成3x3x3的超晶結構與一維6×(010)混摻,以及另一岩鹽母結構2x2x2的尖晶石態超晶格(Ni2SiO4)。這些物質與Ni1-xO在脈衝雷射製程高溫高壓環境之Si-C-H共摻和壓縮內應力作用有關。
  在第二部分,則以同樣脈衝雷射於氨水(0.25 M NH4OH)中剝溶蝕FCC結構之純鎳靶,產生佈植氮、氫元素具有岩鹽結構的NiO次微米球狀凝固顆粒,以及佈植氮、氫元素具有六方晶格結構的三氧化二鎳(Ni2O3)介穩奈米凝聚物。穿透式電子顯微鏡觀察發現其中岩鹽結構的球狀NiO顆粒有微小{100}表面,而且因氮原子在格隙位置造成較大的晶格參數; 而Ni2O3介穩奈米凝聚顆粒有非等軸外形,而且因奈米效應或因壓縮內應力造成較小的晶格參數。此外偏光與掃瞄電子顯微鏡觀察發現額外具有雙折射光性的帶狀物,是氫氧化鎳(Ni-雙層氫氧化物)聚簇的結果,而且在0.25M氨水環境中進行脈衝雷射剝熔蝕的氧化過程,並未形成硝酸鎳。上述物質具有特徵平面缺陷,以及X-光光電子能譜與紫外吸收光譜。
Abstract
In the first part, pulsed laser ablation (PLA) of Ni in TEOS resulted in the formation of Si-C-H-codoped Ni1-xO particulates and nanocondensates with rocksalt-type derived superstructures, i.e. 2x2x2 (Ni2SiO4 spinel) and 3x3x3 mixed with 1-D 6x(010), graphene and amorphous Ni-O-Si-H phase. The superstructure phases can be attributed to Si-C-H codopant in Ni1-xO at high temperature and high pressure by the PLA process in TEOS.
In the second part, PLA of Ni in aqueous solution of ammonium hydroxide (0.25 M NH4OH) enabled the co-synthesis of N-H doped spherical NiO particulates with rocksalt-type structure and N-H doped nanocondensates Ni2O3 with hexagonal structure.  Transmission electron microscopic observations indicated that the spherical N-H doped NiO particulates are slightly {100} and {110} facetted and have a larger lattice parameter due to N dopant in the intersititial site of the rocksalt-type structure; whereas the N-H doped Ni2O3 nanocondensates vulnerable to electron dosage are nonequiaxed and have a smaller lattice parameters due to smaller sized N dopant in substitution for oxygen atoms and/or internal compressive stress. Optical polarized microscopy further revealed the birefringent Ni-double layered hydroxide as elongate assembly. The 0.25 M NH4OH environment was oxidizing enough to exclude the formation of nickel nitrate during the PLA process. The overall particulates and nanocondensates have modified optoelectronic properties as indicated by X-ray photo spectroscopy and UV absorbance.
目次 Table of Contents
第一部分………..…………………………………………..……………….….1
壹、前言………..…………………………………………..……………….….1
貳、實驗流程……………………………………………….………….…...….4
四乙基正矽酸鹽中脈衝雷射剝熔蝕..……….…………………………...4
參、實驗步驟及方法…………………………………….………………...…..5
一.脈衝雷射剝熔蝕….……………………………….…..…………..…...5
二. X光繞射分析………………………………………….………….....…5
三.測量UV-Vis吸收光譜……………………………………………....…5
四.穿透式電子顯微鏡(TEM)…………………………………..…………5
  五.掃描式電子顯微鏡(SEM)…………………………………..…………5
  六.偏光顯微鏡(POM) …………………………………………………….6
肆、實驗結果………………………………………….………….…….….….7
一.X光繞射分析……………………………………………………..……7
二.UV-Vis吸收光譜分析………………………………….…………..….7
  三.掃描式電子顯微鏡(SEM)觀察…………………………….……….……….7
四.穿透式電子顯微鏡(TEM)觀察…………………………….……….…7
伍、討論…………………………..…………..…………….……………..…...9
陸、結論………………………………………..………….………………...…12
柒、參考文獻………………………………….………………………….....…13

第二部分………………………………….……………………………....…….45
壹、前言………………………………….……………………………....…….45
貳、實驗流程………………………………….……………………...……..…48
氨水中脈衝雷射剝熔蝕………………………………….……...………...48
參、實驗步驟及方法………………………………….……………...………..49
一.脈衝雷射剝熔蝕….……………………………….…..…………..…....49
二.穿透式電子顯微鏡(TEM).…………………………………...………...49
三.掃描式電子顯微鏡(SEM)…….……………………………...………...49
四.偏光顯微鏡(POM) ………………………………….……..…………...49
五.X光光電子能譜分析(XPS) …………………………….…………..….49
六.測量UV-Vis吸收光譜……………………………….……..…………………..50
肆、實驗結果………………………………….…………………………….….51
  一.UV-Vis吸收光譜分析………………….………………………….……51
  二.掃描式電子顯微鏡(SEM)觀察………………………..………...……...51
三.X光光電子能譜(XPS)分析…………………………….……...………..51
四.穿透式電子顯微鏡(TEM)觀察…………………………………………52
伍、討論………………………………….………………………..……………55
陸、結論……………………………………….………………..………………59
柒、參考文獻………………………………….……………..…………………60
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第二部分
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