Synthesis, Characterization and Applications of Nanoparticle-Polymer Based Green Composites

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研究生：	Mekuriaw assefa Kebede Mekuriaw assefa Kebede
論文名稱：	Synthesis, Characterization and Applications of Nanoparticle-Polymer Based Green Composites Synthesis, Characterization and Applications of Nanoparticle-Polymer Based Green Composites
指導教授：	今榮東洋子 Toyoko Imae
口試委員:	鄭國彬 Kuo-Bing Cheng 楊禎明 Jen-Ming Yang 呉昌諜 Chang-Mou Wu　　　　氏原真樹 Masaki Ujihara
學位類別：	博士 Doctor
系所名稱：	應用科技學院 - 應用科技研究所 Graduate Institute of Applied Science and Technology
論文出版年：	2018
畢業學年度：	106
語文別：	英文
論文頁數：	114
中文關鍵詞：	Cellulose fiber 、TEMPO-oxidation 、Metal nanoparticles 、Poly(amido amine) dendrimer 、Formaldehyde decomposition 、Antimicrobial activity 、Flexible electrode 、Carbon dot 、Dye sensitized solar cell 、Hydroxyapatite 、Agarose 、Poly(dimethyl acrylamide) 、Bone scafold 、Stereo lithography 、Mechanical strength
外文關鍵詞：	Cellulose fiber, TEMPO-oxidation, Metal nanoparticles, Poly(amido amine) dendrimer, Formaldehyde decomposition, Antimicrobial activity, Flexible electrode, Carbon dot, Dye sensitized solar cell, Hydroxyapatite, Agarose, Poly(dimethyl acrylamide), Bone scafold, Stereo lithography, Mechanical strength
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上一筆

本研究主要探討不同複合材料及其應用，首先利用黏膠人造纖維(viscose rayon cellulose fiber)為基底加載鉑(platinum)和銀(silver)奈米粒子其分別應用在分解甲醛氣體和抑菌材料上。其次是使用2,2,6,6-四甲基哌啶氧化纖維素奈米纖維(2,2,6,6-tetramethyl-1-piperidinyloxy radical -oxidized cellulose nanofiber, TOCNF) 為基底加載氧化鋅奈米粒子(zinc oxide nanoparticles)其應用在染料敏化太陽能電池(dye-sensitized solar cell)。最後使用丙烯酸酯(acrylate)為基底與瓊脂糖(agarose)合成一聚合物複合材料其應用在骨再生3D列印技術中。
首先黏膠人造纖維先被選擇性地氧化後引入羧酸官能基(carboxylate functional group)於其中，隨後在其表面個別分散奈米鉑和奈米銀粒子藉由第四層胺終端基的樹枝狀高分子(amine-terminated fourth generation poly(amido amine) dendrimer, PAMAM)與羧酸進行醯胺化反應(amidation reaction)。由實驗發現，含1 wt% PAMAM和2 wt% 奈米鉑粒子之黏膠人造纖維比未含有PAMAM和奈米鉑粒子的黏膠人造纖維高出84倍的吸附甲醛氣體能力且具65%分解甲醛氣體之催化效率(catalytic efficiency)。而加載0.2 wt% 奈米銀粒子之黏膠人造纖維由實驗結果顯示出對大腸桿菌(E. coli)具有優異的殺菌能力。因此，由上述結果可得知PAMAM可保護且將具功能性奈米金屬粒子有效固定於黏膠人造纖維上，並產生一具有功能性的黏膠人造纖維且有效應用在病態建築症候群(sick building syndrome) 之降解其病原體。
其次是在含有TOCNF下進行氧化鋅奈米棒(ZnO nanorod, ZnO-NR)的原位生長(in situ growth)，進而製備出一具軟性導電複合薄膜。我們利用該薄膜作為染料敏化太陽能電池之電極，在其表面加載氧化鋅奈米棒和碳點(carbon dots)。由實驗結果發現，最佳加載ZnO-NP@Cdot在TOCNF/ZnO-NR薄膜上是100 mg/(g TOCNF/ZnO-NR)為最佳優化比例。氧化鋅奈米棒和碳點之最佳優化比例為1:0.4，在藍光(波長479 nm, 強度為56.2 W / m2)照射下，染料敏化太陽能電池的功率轉換效率(power conversion efficiency)為0.15±0.08％。
最後將使用羥基磷灰石-聚（二甲基丙烯酰胺）(hydroxyapatite-poly(dimethyl acrylamide), HAp-PDMAAm)複合材料藉由光固化成形法(Stereolithography)之3D列印技術製備出一骨再生模擬物(bone mimicry)。除此之外，我們也使用另一種複合材料-HAp-瓊脂糖複合材料並藉由同一技術製備出另一骨再生模擬物，進一步將這兩種骨再生模擬物進行抗拉強度(tensile strength)和其形態(morphologies)比較。由實驗結果表示出HAp: PDMAAm的重量比在0.17之HAp-PDMAAm複合xerogel其抗拉強度具有30.2 MPa，而Hap含量重量比在0.5之瓊脂糖骨複合材料其抗拉強度有26.2 MPa。由此機械強度顯示出該複合材料可應用在骨再生醫學(bone-regenerative medicine)且對病患特定部位之再生在3D bioprinting技術具有無限潛力發展。
總括本實驗結果主要集中在生產出具低成本、高穩度且環保之綠色複合奈米材料以及評估其材料於醫學、環境及能源方面的應用。因此，由本研究結果將有助於目前奈米技術發展以利提高現代人類生活水準。

Composite materials were prepared by loading platinum, silver, and zinc oxide nanoparticles on cellulose-based substrates, independently. Additionally, agarose and acrylate-based synthetic polymer were also used to prepare different composites. Hence, synthesis, characterization and respective applications of the obtained composites are the major objectives of the study.
In the first work, viscose rayon cellulose fiber was selectively oxidized so that carboxylate functional group was introduced into the fiber. Enough dispersed platinum and silver nanoparticles having an average size of around 5 nm with narrow size distribution were prepared with a capping of amine-terminated fourth generation poly(amido amine) dendrimer and they were immobilized on oxidized fibers through amidation between terminal amine groups of dendrimer and carboxylic acids on oxidized fibers. The fiber-containing dendrimer (1 wt%) and platinum (2 wt%) exhibited 84 times higher adsorption capacity for formaldehyde gas on dendrimer site than on fiber site and the catalytic efficiency (65 %) towards decomposition of formaldehyde gas adsorbed on the dendrimer site, and the silver (0.2 wt%)-loaded fiber revealed excellent biocidal activity against E. coli. Thus, it can be noted that the immobilization of functional metal nanoparticles protected by dendrimer on cellulose fibers is effective to produce efficient textile products with smart functions like the degradation of causative agents for sick building syndromes.
In the second work, an in situ growth of ZnO nanorod (ZnO-NR) was performed in the presence of 2,2,6,6-tetramethyl-1-piperidinyloxy radical (TEMPO)-oxidized cellulose nanofiber (TOCNF), and then a stable, flexible and conductive composite film was prepared. This composite film was used as a substrate for loading zinc oxide nanoparticles (ZnO-NP) and carbon dots (Cdot). The ratio of loaded ZnO-NP@Cdot on TOCNF/ZnO-NR film was optimized at 100 mg/(g TOCNF/ZnO-NR). The optimized weight ratio of ZnO-NP to Cdot ratio was 1:0.4 that provided a power conversion efficiency of 0.15±0.08 % on the dye-sensitized solar cell under the illumination of blue light (479 nm wave length) with an intensity of 56.2 W/m2.
Lastly, a bone mimicry was fabricated from hydroxyapatite-poly(dimethyl acrylamide) (HAp-PDMAAm) composite through stereolithographic 3D printing technique, and additionally, the similar material was also obtained from HAp-agarose composite by using a mold preparation technique. The two bone-regenerative products were compared each other based on their tensile strength and morphologies: The HAp-PDMAAm composite xerogel from 0.17 weight ratio of HAp content against PDMAAm can possess a tensile stress of 30.2 MPa, whereas 26.2 MPa was observed in a case of agarose bone composite of 0.5 weight ratio of HAp content. The achieved mechanical strengths indicate that the products can be applied to bone-regenerative medicine and the utilized fabrication techniques will play a significant role towards patient-specific bioprinting technologies.
In general, all the above studies were focused on the development of facile procedures for the production of cheap, stable and environmentally friendly nanomaterials based green composites and on the evaluation of their performances on desired applications for the health, environment and energy production. Thus, the as-reported research will contribute to the current nanotechnologies towards the improvement of modern human life standard.

Table of contents
Contents                                                                                                                                                        Page
Abstract  .......................................................................................................................................................................i
Acknowledgments................................................................................................................................................... v
Table of contents......................................................................................................................................................viii
List of figures, schemes, and tables.................................................................................................................. xi
CHAPTER ONE: Introduction............................................................................................................................... 1
1.    Background..................................................................................................................................................... 1
2.    Cellulose and its composites.................................................................................................................... 7
2.1.    Structure of cellulose................................................................................................................................ 7
2.2.    Cellulose nanoparticles............................................................................................................................ 9
2.3.    Cellulose-based composites.................................................................................................................10
3.    Dendrimer molecules and their composites.......................................................................................14
3.1.    Definition and structure of dendrimer molecules..........................................................................14
3.2.    Dendrimer-based composites...............................................................................................................16
4.    Dye-sensitized Solar cell..............................................................................................................................18
5.    Objectives..........................................................................................................................................................24
CHAPTER TWO: Preparation of Platinum and Silver-loaded Viscose Rayon Fibers for Formaldehyde Decomposition and Antimicrobial Functionality............................................................27
1    Motivation..........................................................................................................................................................27
2    Experimental......................................................................................................................................................29
2.1    Materials and methods..............................................................................................................................29
2.2    TEMPO-oxidation of viscose rayon (VR) fiber...................................................................................30
2.3    Synthesis of nanoparticles........................................................................................................................31
2.4    Chemical attachment of nanoparticles on TOVR.............................................................................31
2.5    Detection of formaldehyde on TOVR-DenPtNPs.............................................................................32
2.6    Antibacterial activity test on TOVR-DenAgNPs................................................................................32
3    Results and Discussion...................................................................................................................................33
3.1    Chemical immobilization of nanoparticles on TEMPO-oxidized rayon fiber........................33
3.2    Formaldehyde removal/decomposition effect of TOVR-DenPtNPs........................................40
3.3    Antibacterial effect of TOVR-DenAgNPs............................................................................................43
4    Conclusions.......................................................................................................................................................44
CHAPTER THREE: Flexible film Electrode Consisting of ZnO/Cellulose Composite for Dye-Sensitized Solar Cell Application.........................................................................................................................46
1.    Motivation.........................................................................................................................................................46
2.    Experimental.....................................................................................................................................................47
2.1.    Materials and methods.............................................................................................................................47
2.2.    Synthesis of Tempo-Oxidized Cellulose Nanofiber (TOCNF)....................................................48
2.3.    Preparation TOCNF/ZnO-NR Composite film electrode.............................................................49
2.4.    Preparation of TOVR/ZnO-NR/ZnO-NP@Cdot composite film electrode..........................49
2.5.    Conductivity measurement.....................................................................................................................50
2.6.    Fabrication of dye-sensitized solar cell (DSSC)...............................................................................50
2.7.    Photocurrent (J-V) measurement of DSSC........................................................................................51
3.    Results and Discussion.................................................................................................................................51
3.1.    Characterization of TOCNF/ZnO-NR and TOCNF/ZnO-NR/ZnO-NP@Cdot composite films.................................................................................................................................................................................51
3.2.    Electrochemical measurement..............................................................................................................55
3.3.    Photo-electrochemical measurement of fabricated DSSC solar cell......................................56
3.4.    Effect of ZnO-NP@ Cdot coating on photo-electrochemical property of TOCNF/ZnO-NR electrode................................................................................................................................................................57
5.    Conclusions......................................................................................................................................................60
CHAPTER FOUR: Stereolithographic and Molding Fabrications of Hydroxyapatite - Polymer Gels Applicable to Bone Regeneration Materials....................................................................................................62
1.    Motivation.........................................................................................................................................................62
2.    Experimental.....................................................................................................................................................64
2.1.    Materials and Characterization..............................................................................................................64
2.2.    Preparation of HAp − PDMAAm composite hydrogels/xerogels............................................64
2.3.    Preparation of HAp - Agarose composite hydrogels/xerogels.................................................65
3.    Results and discussion..................................................................................................................................66
3.1.    HAp  -  PDMAAm composites................................................................................................................66
3.2.    HAp - Agarose composites and their comparison with HAp - PDMAAm composites....71
4.    Conclusions.......................................................................................................................................................72
CHAPTER FIVE: General Conclusions and Future Perspectives................................................................74
References.....................................................................................................................................................................77
List of Publications.....................................................................................................................................................98


                                

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