課題番号                ：S-19- NI-0041

利用形態                ：共同研究

利用課題名（日本語）    ：廃棄物からのナノ複合材料の合成と評価

Program Title (English) ：Green synthesis and characterization of nanocomposite materials

Username (English)     ：Mohd Hafiz Bin Mohd Zaid ¹⁾

所属名（日本語）        ：1) マレーシアプトラ大学

Affiliation (English)  ：1) University Putra Malaysia

１．概要（Summary ）

This study was conducted to synthesize the carbon based and glass-ceramic nanocomposite materials using waste materials as precursors.  For the former synthesis, utilization of cooking waste (waste cooking oil; palm oil and animal lipid) and laboratory waste (waste latex glove) as carbon precursor during manufacturing of carbon nanomaterials (CNMs) helps in reducing the pollution impact from the waste to the environment and stimulating the mass production of nanomaterials by reducing the cost of carbon precursor during the manufacturing. For the latter synthesis, foam glass-ceramic using glass bottle waste as a precursor and eggshell as a foaming agent was tackled and investigated the effect of sintering temperature on the crystal growth, microstructure, and mechanical properties of the final product. The invention of foam glass-ceramics from waste materials can be applied as a potential building insulation material that gives benefit to the environment and energy usage.

２．実験（Experimental）

For the synthesis of the carbon-based nanocomposites, high purity Copper foil (99.9% purity) with low carbon solubility were employed as metal catalyst for the growth of CNMs in dual-furnace chemical vapor deposition process (DF-CVD) provided by Nagoya Institute of Technology (NITech) nanotechnology platform. Low temperature region (450°C) of DF-CVD responsible in supplying energy in bond breaking within the carbon precursor while high temperature region (700°C-1000°C) applied for the metal catalyst-carbon precursor reaction. CNMs have been characterized by MALDI-TOFMS, Raman Spectroscopy, Scanning Electron Microscopy and Transmission Electron Microscopy (ARM-200F) at NITech.

For the synthesis of foam glass-ceramics, the glass powder was filtered to obtain the powder with 45 μm particle size using stainless steel sieve while the ES ground using mortar and pestle and sieve into 45 μm size. Then, the powder was pressed using a hydraulic pressing machine with a diameter of 13 mm and 2 mm thickness with an applied load of 5 MPa transformed into pellet form. The samples undergo the sintering process at different temperatures such as 700, 800 and 900 °C for 60 min with the heating rate of 10 °C/min. The structural properties were studied by XRD, FTIR and SEM measurement.

３．結果と考察（Results and Discussion）

Identification of hydrocarbon bonding in the carbon precursor was done with MALDI-TOFMS and GC-MS at the first stage. Long chain hydrocarbon Pentadecane (C₁₅H₃₂) contributed from heavy cooked animal lipid while Methyl (3S)-3-methylnonadecanoate (C₂₁H₄₂O₂) from laboratory rubber glove provided sufficient carbon atoms with minimum enthalpy energy during the formation of CNMs. Synthesized CNMs from this DF-CVD process showed the nano-graphite formed on the copper foil with heavy cooked palm oil as carbon precursor. It showed the possibility in having low cost and green carbon precursor in synthesizing CNMs.

Figure 1 Raman Spectrum and TEM image of DF-CVD product using used cooking oil as carbon precursor.

SEM is a test used to visualize the topographic/microstructure details on the bulk or surface crystallization of the materials. SEM revealed the microstructure in parallel cross-section of foam glass-ceramics at 700, 800 and 900 ºC of temperature as shown in Fig. 2. As can be seen from Fig. 2, there were homogenous pores distributed with small size in diameter. Increasing the sintering temperature to 800 ºC, the pores became larger and well foamed with the size in the range of 250-350 µm. From this work, foam glass-ceramics with closed porosity can be fabricated from waste materials and would give a great benefit to the economy and solve the environmental pollution issues.

Fig. 2  Microstructure of foam glass–ceramics (SEM image).

４．その他・特記事項（Others）

The researchers thank to Sakura Science Exchange Program by Japan Science and Technology, Japan and Malaysia Ministry of Education (Fundamental Research Grant Scheme, Grant No.5540132 and Grant No. 5540268).

５．論文・学会発表（Publication/Presentation）

1. Saparuddin, DI, Hisham, NAN, Ab Aziz, S., Matori, KA, Honda, S, Iwamoto, Y, & Zaid, MHM. Effect of sintering temperature on the crystal growth, microstructure and mechanical strength of foam glass-ceramic from waste materials. Journal of Materials Research and Technology. (2020), in press (https://doi.org/10.1016/j.jmrt.2020.03.089).
2. K.F. Chan, A. K. Ranude, P. Desai, M. Tanemura, G. Kalita, M. S. Mamat and Y. Yaakob, American Institute of Physics (AIP) Conference Proceedings, (2020) (submitted)
3. K. F. Chan and Y. Yaakob, Malaysia-Japan International Conference on Nanoscience, Nanotechnology and Nanoengineering 2020 (MJIC 2020), 28 February 2020

６．関連特許（Patent）

None