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Author: 洪梅星
Stella Patricia Angdiarto
Thesis Title: 以煅燒牡蠣殼灰、奈米二氧化矽、脫硫石膏及β-半水石膏增進單劑型鹼激發爐石粉漿體工程性質之研究
Study on the Enhancement of Engineering Properties of One-part Alkali-activated Slag Paste Using Calcined Oyster Shell Ash, Nano-silica, FGD Gypsum, and β-hemihydrate
Advisor: 陳君弢
Chun-Tao Chen
Ta-Peng Chang
Committee: 黃然
Huang Ran
Wen-Zheng Liao
Yu-Chen Ou
Chong-Zhan Hong
Li-Hsien Chen
Jian-Guo Qiu
Chun-Tao Chen
Ta-Peng Chang
Degree: 博士
Department: 工程學院 - 營建工程系
Department of Civil and Construction Engineering
Thesis Publication Year: 2023
Graduation Academic Year: 112
Language: 英文
Pages: 147
Keywords (in Chinese): 單劑型鹼激發爐石粉β-半水石膏FGD煅燒牡蠣殼灰β-半水石膏奈米二氧化矽
Keywords (in other languages): One-part alkali-activated slag, calcined oyster shell ash, FGD, nano-silica, β-hemihydrate
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  • 經研究發現,以爐石粉、煅燒牡蠣殼灰(COSA)、奈米二氧化矽粉、煙氣脫硫(FGD)石膏和β-半水石膏(HH)等組合之粉末混合物可改善單劑型鹼激發爐石基漿體之工程性質,隨著COSA質量從10%增加至20%,漿體初凝時間和終凝時間分別從298分鐘和365分鐘減少到157分鐘和275分鐘,添加納米矽粉發現有類似降低工作性及加速凝結時間之效果,此外,以3%質量奈米矽粉和20% 質量COSA混合物製成之試體,相較於僅添加20%質量 COSA之試體,分別顯著提高抗壓強度31.55%,熱導率從0.434 W/(m.K)增加到0.715 W/(m.K),吸水率從10.43%降低到3.02%,
    以10% 質量FGD石膏與10% 質量COSA混合物為最佳組合,將試體抗壓強度提高到46.53 MPa。這種強度的改善歸因於存在之氫氧化鈣被CaSO₄·2H₂O有效消耗,導致水化熱從32°C降至21.5°C。相比之下,在混合物添加10%質量β-半水石膏導致氫氧化鈣未能被成功消耗,使水化熱從32°C增加到39°C。因此,卜作嵐反應受到抑制,導致28天抗壓強度降至39.6 MPa。
    此外,10% 質量FGD石膏與10%質量 COSA組合之試體在水中養護後之抗壓強度從46.53 MPa降至41.12 MPa,這種減少歸因於由COSA和FGD之鹼離子(例如Ca2+)濾滲到水中所致。相反地,所有含有FGD和HH之試體顯示出更高的抗壓強度,因為試體中的硫酸根離子(SO₄²⁻)阻止鹼性物質之滲出。因此,在混合物中觀察到如鈣礬石和C-S-H/C-A-S-H膠體之水化物,其中鈣礬石擔任填充試體孔隙之作用。

    The engineering properties of a one-part alkali-activated slag-based paste were investigated to be improved by applying the powder blends of slag, calcined oyster shell ash (COSA), nano-silica, flue gas desulphurization (FGD) gypsum, and β-hemihydrate (HH). The paste, with an increase of COSA from 10% to 20% by mass, had its initial and final setting times reduced from 298 minutes and 365 minutes to 157 minutes and 275 minutes, respectively. Similar results of reducing workability and accelerating setting times by adding nano-silica were found. In addition, the mixture of 3 mass% nano-silica and 20 mass% COSA, significantly increased compressive strength by 31.55%, enhanced thermal conductivity from 0.434 W/(m.K) to 0.715 W/(m.K), and decreased the water absorption value from 10.43% to 3.02% when compared with the specimens incorporating 20 mass% COSA without nano-silica, respectively.
    The combination of 10 mass% FGD gypsum with 10 mass% COSA was the optimum mixture with an increased the compressive strength of 46.53 MPa. This strength improvement was attributed to the presence of portlandite, which was effectively consumed by CaSO₄·2H₂O, resulting in a decrease in hydration heat from 32°C to 21.5°C. In contrast, the addition of 10 mass% of β-hemihydrate to the mix resulted in the unsuccessful consumption of the portlandite (Ca(OH)2), leading to an increase in hydration heat from 32˚C to 39˚C. Consequently, the pozzolanic reaction was inhibited, causing a decreased in compressive strength of 39.6 MPa at 28 days.
    Moreover, the combination of 10 mass% FGD gypsum with 10 mass% COSA resulted in a decrease in the compressive strength from 46.53 MPa to 41.12 MPa after water curing. This reduction was attributed to the alkalis, such as calcium ion (Ca2+) from COSA and FGD, leaching out into the water. In contrast, all samples incorporating FGD and HH exhibited higher compressive strength, as sulfate ions (SO₄²⁻) within the samples prevented the alkalis from leaching. Consequently, the hydration products such as ettringite and C-S-H/C-A-S-H gel were observed in the mixture, with ettringite playing a role in filling the pores of the specimens.

    Tables of contents 摘要 i Abstract iii Personal Acknowledgements v Tables of contents vii List of symbols and abbreviations xi List of Tables xiii List of Figures xv Chapter 1 Introduction 1 1.1 Research background 1 1.2 Research Significance 6 1.3 Research aim 6 1.4 Research outline 7 Chapter 2 Literature Review 13 2.1 Ground granulated blast furnace slag (GGBFS) 13 2.1.1 Physical and chemical of ground granulated blast furnace slag (GGBFS) 13 2.1.2 Development of ground granulated blast furnace slag (GGBFS) 14 2.2 Calcined oyster shell ash (COSA) 15 2.2.1 Physical and chemical properties of calcined oyster shell ash (COSA) 15 2.2.2 Development of Calcined Oyster Shell Ash (COSA) 16 2.3 Nano-silica 17 2.3.1 Physical and chemical properties of nano-silica 17 2.3.2 Development of nano-silica 17 2.4 Flue gas desulphurization (FGD) gypsum and β-hemihydrate 18 2.4.1 Physical and chemical properties of flue gas desulfurization (FGD) gypsum 18 2.4.2 Development of flue gas desulfurization (FGD) gypsum 20 2.5 Development of curing method on alkali-activated binders 20 Chapter 3 Materials and Experimental Methods 33 3.1 Materials 33 3.2 Design of mixed proportion 36 3.3 Test methods 37 3.3.1 Methods of fresh properties analyses 37 Workability test 37 Setting time test 38 Isothermal calorimetry of paste specimen 39 3.3.2 Methods of hardened properties analyses 39 Compressive strength test 39 Splitting tensile strength test 40 Thermal conductivity test 40 Ultrasonic pulse velocity test 41 Drying shrinkage test 41 3.3.3 Microstructural analyses 42 Water absorption 42 Mercury Intrusion Porosimetry (MIP) 43 X-ray diffraction (XRD) test 43 Scanning electron microscopy (SEM) and Energy Dispersive X-Ray Spectroscopy (EDS) test 43 Chapter 4 Results and discussions of one-part alkali activator cured in room temperature 59 4.1 Fresh properties 59 4.1.1 Slump flow test 59 4.1.2 Setting times test 60 4.1.3 Isothermal calorimetry of paste 61 4.2 Hardened properties 63 4.2.1 Compressive strength and splitting tensile strength test 63 4.2.2 Thermal conductivity 65 4.2.3 Ultrasonic pulse velocity 67 4.2.4 Drying shrinkage 69 4.3 Microstructural analysis 69 4.3.1 Water absorption 69 4.3.2 Mercury intrusion porosity test 71 4.3.3 X-ray diffraction test (XRD) 72 4.3.4 Scanning Electron Microscopy (SEM) 73 4.3.5 The Energy Dispersive Spectroscopy (EDS) 74 Chapter 5 Results and discussions of one-part alkali activator cured in water and soaked in sulfate environment 115 5.1 Hardened properties 115 5.1.1 Compressive strength test 115 5.1.2 Thermal conductivity test 116 5.1.3 Soundness loss test 117 5.2 Microstructural analysis 117 5.2.1 Mercury intrusion porosity (MIP) 117 5.2.2 X-ray diffraction (XRD) 118 5.2.3 Scanning electron microscopy (SEM) 118 Chapter 6 Conclusion and suggestions 129 6.1 Conclusion 129 6.2 Suggestions 130 Acknowledgement 133 References 135

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