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研究生: 李其蔚
Lee, Chi-Wei
論文名稱: 金屬氧化物披覆合成雲母以製備珠光顏料之研究
A Study on the Preparation of Pearlescent Pigment from Metal Oxide Coated Synthetic Mica
指導教授: 雷大同
Ray, Dah-tong
學位類別: 碩士
Master
系所名稱: 工學院 - 資源工程學系
Department of Resources Engineering
論文出版年: 2016
畢業學年度: 104
語文別: 中文
論文頁數: 122
中文關鍵詞: 合成雲母珠光顏料化學液相沉積法色彩屬性
外文關鍵詞: synthetic mica, pearlescent pigment, liquid chemical deposition method, color attributes
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  • 高級珠光顏料一般是指在雲母薄片上披覆一層或多層高折射率的金屬氧化物薄膜,例如TiO2、Fe2O3等,而製成的一種顏料,在光線的照射下會產生珍珠般質感的光澤效果。人工合成雲母具透明度佳、表面光滑裂紋少、反射強、光澤佳等性質,故而取代天然雲母作為珠光顏料之基底材料。
    本研究使用人工合成氟金雲母作為基底,分別使用硫酸氧鈦與無水氯化鐵作為原料,以化學液相沉積法披覆TiO2及Fe2O3製成珠光顏料。藉由分光光度儀探討水解條及原料劑量之改變,對色彩飽和度及色相的影響,並以掃描式電子顯微鏡(SEM)照片觀察表面披覆狀態,配合X-Ray螢光成分分析(XRF)、X-Ray繞射分析(XRD)對披覆成份的晶相及含量進行分析。根據實驗結果可得以下結論:
    1. 合成雲母披覆TiO2之條件,以pH=0,95℃,煅燒750℃,2 hrs之條件披覆,能得到最佳彩度。
    2. 合成雲母披覆Fe2O3之條件,以pH=3,85℃能得到緻密平滑的披覆層。

    Pearlescent pigments generally refers to mica flakes coated with one or more layers of high refractive index metal oxide films, such as TiO2 and Fe2O3, so that’s presenting a pearl luster effect under the irradiation of light. Synthetic mica has the characteristics of good transparency, smooth surface, less cracks, reflecting strong, good gloss, which replace the natural mica pearlescent pigment used as the base material.
    In this study, pearlescent pigments were prepared by the liquid chemical deposition method in the presence of titanyl sulfate and ferric chloride as the titanium source and iron source and fluorphlogopite as the substrate to be coated with TiO2 and Fe2O3. The influence of hydrolysis condition and dosage on the chroma and hue were measured using sphere spectrophotometer. The coating state on the surface as examined by SEM. The chemical composition and crystal phase of coated components were analyzed by XRF and XRD. According to the results of experiments, the following conclusions are obtained:
    1. The optimum pH value and temperature for TiO2 coating on mica are: pH=0, 95℃, calcined at 750℃ for 2hrs. The best chroma of the products obtained is the best.
    2. For Fe2O3, at pH=3, it is able to obtain a dense and smooth coated layer.

    摘 要 I Extended Abstract II 致 謝 IX 目 錄 XI 表目錄 XIV 圖目錄 XV 第一章 緒論 1 1.1研究背景 1 1.2研究目的 3 第二章 理論基礎與前人研究 4 2.1 珠光顏料的概述 4 2.1.1簡介珠光顏料 4 2.1.2一般顏料與珠光顏料之比較 6 2.1.3珠光顏料的發展 7 2.2 色彩學理論 8 2.2.1 色彩屬性 8 2.2.2 CIE表色系統 10 2.3合成氟金雲母 14 2.3.1合成氟金雲母的組成與結構 14 2.3.2天然雲母與合成氟金雲母之比較 15 2.4珠光顏料的顯色及光學原理 16 2.4.1干涉原理 16 2.4.2雲母鈦珠光顏料的干涉現象 18 2.4.3珠光顏料的光學效應 23 2.4.4雲母鈦珠光顏料的分類 25 2.5珠光顏料的製備 26 2.5.1 雲母表面的帶電機制 26 2.5.2 金屬鹽類的水解反應 26 2.5.3 雲母披覆二氧化鈦與赤鐵礦珠光顏料的製備 27 2.6披覆對光學的影響 31 2.6.1晶核的生長模式 31 2.6.2反應條件的影響 31 2.6.3 雲母基材及氧化物薄膜對光學效果的影響 35 2.6.4 煅燒的影響 35 第三章 實驗 37 3.1材料及設備 37 3.1.1合成雲母原礦 37 3.1.2其他藥劑 39 3.1.3實驗設備 40 3.2 實驗步驟 41 3.2.1披覆二氧化鈦 41 3.2.2披覆赤鐵礦 41 3.3 性質分析 44 3.3.1高解析場發式掃描式電子顯微鏡(UHRFE-SEM)分析 44 3.3.2 X-Ray螢光成分分析(XRF) 44 3.3.3色度測定分析 44 3.3.4 X-Ray繞射分析儀(XRD) 45 第四章 結果與討論 46 4.1 氟金雲母之性質 46 4.2 偏鈦酸(H2TiO3)與二氧化鈦(TiO2)披覆量之計算 47 4.3 披覆偏鈦酸 49 4.3.1披覆偏鈦酸之水解條件 49 4.3.2 相同水解條件下改變偏鈦酸披覆量 64 4.4 煅燒結果 68 4.4.1 不同水解條件煅燒結果 68 4.4.2 相同水解條件下改變二氧化鈦披覆量 85 4.5 披覆赤鐵礦 89 4.5.1 赤鐵礦之性質 89 4.5.2 披覆四方纖鐵礦(β-FeOOH)與赤鐵礦(Fe2O3)用量之計算 91 4.5.3 緩慢加氨水方式披覆 92 4.5.4 以緩衝劑維持pH=3再調整pH值至8之修改 98 4.5.5 固定pH=3之結果 102 第五章 結論 106 參考文獻 108 附錄 色彩屬性資料 113

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