Analisis Pengaruh Suhu dan Waktu Hidrotermal Terhadap Struktur Kristal, Morfologi, dan Performa Elektrokimia N-Doped Ti₃C₂Tₓ Mxene

Sianipar, Gherald Rheinart (2026) Analisis Pengaruh Suhu dan Waktu Hidrotermal Terhadap Struktur Kristal, Morfologi, dan Performa Elektrokimia N-Doped Ti₃C₂Tₓ Mxene. Other thesis, Institut Teknologi Sepuluh Nopember.

Text 5011221005-Undergraduate_Thesis.pdf - Accepted Version Restricted to Repository staff only Download (11MB) | Request a copy

Abstract

MXene Ti₃C₂Tₓ merupakan material dua dimensi yang banyak diteliti sebagai elektroda superkapasitor karena memiliki konduktivitas listrik tinggi, struktur berlapis, serta kemampuan transport ion yang baik. Modifikasi melalui doping nitrogen secara hidrotermal diketahui dapat menambah situs aktif redoks dan memengaruhi jarak antar lapisan, namun suhu dan waktu reaksi sangat menentukan stabilitas struktur serta efektivitas doping yang dihasilkan. Penelitian ini mensintesis Ti₃C₂Tₓ melalui etsa in situ HF berbasis LiF/HCl, dilanjutkan delaminasi menggunakan DMSO, kemudian doping nitrogen secara hidrotermal menggunakan urea pada variasi suhu 160 °C dan 180 °C serta waktu 6, 9, dan 12 jam. Karakterisasi XRD menunjukkan bahwa peningkatan suhu doping dari 160 °C ke 180 °C secara konsisten mempersempit jarak antarlapisan pada seluruh durasi akibat percepatan restacking, sedangkan penambahan waktu dari 6 ke 9 jam cenderung memperlebar jarak antarlapisan. Hasil SEM-EDX menunjukkan morfologi accordion dan kandungan nitrogen tertinggi (4,03 wt%) diperoleh pada suhu 160 °C selama 6 jam, sementara durasi 12 jam pada kedua suhu serta suhu 180 °C secara umum menyebabkan degradasi struktur berlapis dan penurunan kandungan nitrogen. Pengujian elektrokimia (CV, GCD, EIS) dalam sistem tiga elektroda mengonfirmasi bahwa doping nitrogen menambahkan kontribusi pseudokapasitif berupa gelombang redoks dibandingkan elektroda delaminated MXene tanpa doping yang bersifat murni kapasitif. Sampel N-doped MXene 160 °C/6 jam menunjukkan performa paling optimal, dengan gelombang redoks paling tegas, resistansi seri dan transfer muatan yang rendah, sudut fase paling mendekati kapasitor ideal, serta rapat energi tertinggi pada Ragone plot di antara seluruh variasi. Dengan demikian, kondisi hidrotermal suhu 160 °C selama 6 jam teridentifikasi sebagai kondisi optimum untuk menghasilkan elektroda N-doped Ti₃C₂Tₓ MXene dengan struktur berlapis terjaga dan performa elektrokimia terbaik untuk aplikasi superkapasitor.
================================================================================================================================
Ti3C2Tx MXene is a two-dimensional material widely studied as a supercapacitor electrode due to its high electrical conductivity, layered structure, and excellent ion transport capabilities. Modification through hydrothermal nitrogen doping is known to increase redox active sites and affect interlayer spacing; however, the reaction temperature and duration significantly dictate the structural stability and doping effectiveness. In this study, Ti3C2Tx was synthesized via in situ HF etching using a LiF/HCl system, followed by delamination using DMSO, and subsequent hydrothermal nitrogen doping using urea at temperatures of 160 °C and 180 °C for 6, 9, and 12 hours. XRD characterization revealed that increasing the doping temperature from 160 °C to 180 °C consistently narrowed the interlayer spacing across all durations due to accelerated restacking, whereas extending the reaction time from 6 to 9 hours tended to widen the interlayer spacing. SEM-EDX results indicated that an accordion-like morphology and the highest nitrogen content (4.03 wt%) were obtained at 160 °C for 6 hours. Conversely, the 12-hour duration at both temperatures, as well as the 180 °C condition generally, caused the degradation of the layered structure and a reduction in nitrogen content. Electrochemical evaluations (CV, GCD, EIS) in a three-electrode system confirmed that nitrogen doping introduced a pseudocapacitive contribution, evidenced by redox peaks, compared to the undoped delaminated MXene electrode which exhibited purely capacitive behavior. The N-doped MXene sample synthesized at 160 °C for 6 hours demonstrated optimal performance, featuring the most distinct redox peaks, low equivalent series and charge transfer resistances, a phase angle closest to that of an ideal capacitor, and the highest energy density on the Ragone plot among all variations. Therefore, the hydrothermal condition of 160 °C for 6 hours was identified as the optimum parameter to produce N-doped Ti3C2Tx MXene electrodes with a well-preserved layered structure and superior electrochemical performance for supercapacitor applications.

Item Type:	Thesis (Other)
Uncontrolled Keywords:	In situ HF, MXene, Superkapasitor, In situ HF, MXene, Supercapacitor
Subjects:	Q Science Q Science > QD Chemistry Q Science > QD Chemistry > QD115 Electrochemical analysis
Divisions:	Faculty of Industrial Technology and Systems Engineering (INDSYS) > Material & Metallurgical Engineering > 28201-(S1) Undergraduate Thesis
Depositing User:	Gherald Rheinart Sianipar
Date Deposited:	28 Jul 2026 04:22
Last Modified:	28 Jul 2026 04:22
URI:	http://repository.its.ac.id/id/eprint/138647

Actions (login required)

View Item