Analisis Pengaruh Variasi Holding Time dan Temperatur Kalsinasi Pasca-Proses Electrospinning Terhadap Pembentukan Fiber Mullite

Izzan, Zidniy AT (2024) Analisis Pengaruh Variasi Holding Time dan Temperatur Kalsinasi Pasca-Proses Electrospinning Terhadap Pembentukan Fiber Mullite. Other thesis, Institut Teknologi Sepuluh Nopember.

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Abstract

Fiber keramik memiliki peran penting dalam berbagai aplikasi suhu tinggi seperti industri logam, kiln refractory, dan lainnya. Salah satu bahan pembuatannya adalah mullite, yang merupakan material berstruktur serat berbahan dasar keramik. Mullite sering digunakan dalam pembuatan bahan refraktori. Salah satu cara untuk menyusun serat mullite adalah dengan menggunakan metode sol-gel electrospinning. Dalam penelitian ini, pengaruh dari variasi holding time dan temperatur kalsinasi dalam proses electrospinning terhadap sifat fisik, mekanik, dan termal dari serat mullite akan dianalisis. Polimer yang digunakan adalah PVP dengan grade K-60 dan tegangan listrik sebesar 500 kV. Langkah penelitian dimulai dari pembuatan alat electrospinning terlebih dahulu kemudian dilanjutkan mempersiapan larutan electrospinning yang berisi sol prekursor mullite dan larutan polimer dengan rasio konsentrasi 20%:80%. Larutan electrospinning diuji menggunakan FTIR untuk mencegah reaksi polimerisasi. Selanjutnya, larutan dimasukkan ke dalam spinneret, perangkat electrospinning disambungkan ke sumber tenaga listrik, dan laju injeksi diatur menjadi 0,2 ml/menit. Setelah larutan habis, sumber listrik diputus. Serat kemudian dikalsinasi pada variasi suhu 700 °C, 900 °C, dan 1000 °C dengan laju pemanasan 10 °C/menit dan ditahan selama 45 menit, 60 menit, dan 90 menit. Pengujian SEM didapatkan hasil bahwa serat-serat yang dihasilkan memiliki morfologi acak dan banyak pengotor yang disebabkan oleh kandungan air dan volatil yang belum sepenuhnya hilang sebelum proses furnace. Pada suhu kalsinasi 700°C, serat tidak mengalami penyusutan yang optimal, dengan diameter rata-rata serat menurun dari 28,708 µm (45 menit) menjadi 20,321 µm (60 menit) dan 21,167 µm (90 menit). Pada suhu 900°C, diameter serat berkurang dari 21,501 µm (45 menit) menjadi 12,926 µm (60 menit) dan 34,712 µm (90 menit). Pada suhu 1000°C, diameter serat lebih kecil yaitu 15,514 µm (45 menit), 13,371 µm (60 menit), dan 16,450 µm (90 menit). Hasil ini menunjukkan bahwa suhu dan waktu kalsinasi berpengaruh signifikan terhadap diameter serat mullite. Pengujian EDX menunjukkan variasi kecil dalam kandungan aluminium dan silikon serta perbedaan yang lebih besar dalam kandungan karbon antara sampel serat. Uji XRD mengindikasikan bahwa kalsinasi pada 700°C, 900°C, dan 1000°C belum cukup untuk membentuk mullite secara optimal, masih terdapat banyak sisa fasa SiO2, sedangkan pada suhu 1000°C memungkinkan dekomposisi bahan mentah menjadi Al2O3. Pada suhu ini, fase Al2O3 terbentuk sebagai bagian dari proses transformasi sebelum akhirnya menjadi mullite pada suhu yang lebih tinggi atau setelah waktu kalsinasi yang lebih lama.
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Ceramic fibers play an important role in various high-temperature applications such as the metal industry, refractory kilns, and others. One of the materials used to make it is mullite, which is a ceramic-based fiber-structured material. Mullite is often used in the manufacture of refractory materials. One way to form mullite fibers is by using the sol-gel electrospinning method. In this study, the effect of variations in holding time and calcination temperature in the electrospinning process on the physical, mechanical, and thermal properties of mullite fibers will be analyzed. The polymer used is PVP with a grade of K-60 and an electric voltage of 500 kV. The research steps start from making the electrospinning tool first and then continuing to prepare the electrospinning solution containing mullite precursor sol and polymer solution with a concentration ratio of 20%:80%. The electrospinning solution was tested using FTIR to prevent polymerization reactions. Furthermore, the solution was inserted into the spinneret, the electrospinning device was connected to a power source, and the injection rate was set to 0.2 ml/min. After the solution was exhausted, the power source was disconnected. The fibers were then calcined at various temperatures of 700 °C, 900 °C, and 1000 °C with a heating rate of 10 °C/min and held for 45 minutes, 60 minutes, and 90 minutes. SEM testing showed that the resulting fibers had random morphology and many impurities caused by water and volatile content that had not been completely removed before the furnace process. At a calcination temperature of 700 °C, the fibers did not experience optimal shrinkage, with the average fiber diameter decreasing from 28.708 µm (45 minutes) to 20.321 µm (60 minutes) and 21.167 µm (90 minutes). At 900°C, the fiber diameter decreased from 21.501 µm (45 min) to 12.926 µm (60 min) and 34.712 µm (90 min). At 1000°C, the fiber diameter was smaller, namely 15.514 µm (45 min), 13.371 µm (60 min), and 16.450 µm (90 min). These results indicate that calcination temperature and time have a significant effect on the diameter of mullite fibers. EDX testing showed small variations in aluminum and silicon content and larger differences in carbon content between fiber samples. XRD test indicates that calcination at 700°C, 900°C, and 1000°C is not enough to form mullite optimally, there are still many remaining SiO2 phases, while at 1000°C the decomposition of the raw material into Al2O3 is possible. At this temperature, the Al2O3 phase is formed as part of the transformation process before finally becoming mullite at higher temperatures or after longer calcination times.

Item Type: Thesis (Other)
Uncontrolled Keywords: Alumina, Elektrospinning, Mullite, PVP, Kalsinasi
Subjects: T Technology > TA Engineering (General). Civil engineering (General) > TA418.9.F5 Electrospinning. Nanofibers
T Technology > TP Chemical technology > TP1140 Polymers
Divisions: Faculty of Industrial Technology and Systems Engineering (INDSYS) > Material & Metallurgical Engineering > 28201-(S1) Undergraduate Thesis
Depositing User: Izzan Zidniy AT
Date Deposited: 10 Sep 2024 07:20
Last Modified: 10 Sep 2024 07:22
URI: http://repository.its.ac.id/id/eprint/112379

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