Kajian Komparatif Metode Sintesis Satu Tahap dan Dua Tahap Karbon Berpori dari Polifenilen Sulfida Terdoping Heteroatom Nitrogen, Fosfor, dan Sulfur (N, P, dan S)

Wibowo, Chiara Geralda Dahayu (2026) Kajian Komparatif Metode Sintesis Satu Tahap dan Dua Tahap Karbon Berpori dari Polifenilen Sulfida Terdoping Heteroatom Nitrogen, Fosfor, dan Sulfur (N, P, dan S). Other thesis, Institut Teknologi Sepuluh Nopember.

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Abstract

Karbon berpori terdoping heteroatom merupakan material yang banyak dikembangkan karena memiliki luas permukaan tinggi, struktur pori yang dapat dikontrol, serta sifat permukaan yang dapat dimodifikasi melalui doping heteroatom. Metode sintesis berpengaruh terhadap perkembangan porositas, struktur karbon, dan retensi heteroatom yang terbentuk. Namun, kajian komparatif mengenai pengaruh metode sintesis satu tahap dan dua tahap pada karbon berpori berbasis Polifenilen sulfida (PPS) terdoping heteroatom nitrogen, fosfor dan sulfur masih terbatas. Oleh karena itu, penelitian ini bertujuan untuk mengkaji pengaruh metode sintesis satu tahap dan dua tahap terhadap karakteristik morfologi dan retensi heteroatom, menentukan rasio dopan optimum, serta mengevaluasi hubungan antara luas permukaan spesifik, distribusi ukuran pori, dan keberadaan heteroatom terhadap perkembangan struktur karbon berpori. Material hasil sintesis diberi notasi NPSC-x-y, di mana x menunjukkan variasi rasio massa dopan dan y menunjukkan suhu karbonisasi (650-850 ℃). Sampel dengan akhiran TS menandakan sampel metode dua tahap. Karakterisasi dilakukan menggunakan FESEM EDX, XRD, Raman, adsorpsi-desorpsi N2 , C; H; N; S; dan O, serta XPS. Hasil XRD menunjukkan terbentuknya karbon amorf yang ditandai dengan puncak lebar pada bidang (002) dan (100). Analisis Raman menunjukkan bahwa metode dua tahap menghasilkan tingkat cacat struktural lebih tinggi dengan rasio ID/IG maksimum sebesar 2,47 pada sampel NPSC-1-650 TS. Hasil FESEM dan adsorpsi-desorpsi N₂ menunjukkan bahwa metode dua tahap menghasilkan porositas yang lebih berkembang, sedangkan seluruh sampel didominasi oleh struktur mikro-mesopori. Luas permukaan spesifik tertinggi sebesar 282,850 m²/g dengan volume pori 0,183 cm³/g dicapai oleh NPSC-1-850 dengan rasio massa PPS:K₂CO₃:(NH₄)₂HPO₄ sebesar 1:1:1. Analisis C; H ; N; S; dan O membuktikan keberhasilan inkorporasi heteroatom, di mana NPSC-1-850 secara signifikan lebih efektif dalam mempertahankan kandungan karbon dan sulfur hingga 15,578%b dibandingkan NPSC-850TS. Analisis XPS juga menunjukkan bahwa NPSC-1-850 menghasilkan retensi heteroatom tertinggi dengan kandungan doping nitrogen, fosfor, dan sulfur berturut-turut sebesar 1,3, 3,9, dan 2,1%. Selain itu, XPS mengidentifikasi berbagai gugus fungsi permukaan, yaitu N hadir sebagai ikatan sianida/piridin, C-N/NH3, dan garam ammonium, sementara P didominasi oleh ikatan pirofosfat dan metafosfat, serta S hadir sebagai sulfida organik dan sulfur teroksidasi (sulfat/sulfon). Secara keseluruhan, metode dua tahap unggul dalam stabilitas porositas, sementara metode satu tahap lebih efektif dalam retensi heteroatom pada suhu tinggi.
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Heteroatom-doped porous carbon has attracted considerable attention due to its high specific surface area, tunable pore structure, and surface properties that can be modified through heteroatom doping. The synthesis method influences the development of porosity, carbon structure, and retention of the formed heteroatoms. However, comparative studies on the effects of one-step and two-step synthesis methods on porous carbon derived polyphenylene sulfide (PPS) doped with nitrogen, phosphorus, and sulfur heteroatoms are still limited. Therefore, this study aims to compare the effects of synthesis method, the morphological characteristics and heteroatom retention of porous carbon, determine the optimum dopant ratio, and evaluate the relationship between specific surface area, pore size distribution, and heteroatom incorporation in the development of porous carbon structures. The synthesized materials were denoted as NPSC-x-y, where x represents the dopant mass ratio and y represents the carbonization temperature (650–850 °C). Samples with the suffix TS indicate those prepared via the two-step synthesis method. The materials were characterized using FESEM-EDX, X-ray diffraction (XRD), Raman spectroscopy, N₂ adsorption-desorption analysis, C; H; N; S; and O elemental analysis, and X-ray photoelectron spectroscopy (XPS). X-ray diffraction (XRD) analysis confirmed the formation of amorphous carbon, as evidenced by the broad diffraction peaks corresponding to the (002) and (100) planes. Raman characterization revealed that the two-step synthesis method produced a higher degree of structural defects, with the highest ID/IG ratio of 2,47 observed for the NPSC-1-650-TS sample. FESEM observations and N₂ adsorption desorption analysis demonstrated that the two-step method promoted more developed porosity, while all samples exhibited predominantly micro-mesoporous structures. The highest specific surface area of 282,850 m²/g and total pore volume of 0,183 cm³/g were achieved by NPSC-1 850 with a PPS: K2CO₃ :(NH₄)₂HPO₄ mass ratio of 1:1:1. C; H; N; S; and O elemental analysis confirmed the successful incorporation of heteroatoms, with NPSC-1-850 exhibiting significantly better carbon and sulfur retention, maintaining a sulfur content of 15.578 wt% compared with NPSC-850TS. X-ray photoelectron spectroscopy (XPS) further demonstrated that NPSC-1-850 exhibited the highest heteroatom retention, containing 1,3% nitrogen, 3,9% phosphorus, and 2,1% sulfur. In addition, XPS identified various surface functional groups, where nitrogen detected as pyridinic/cyanide nitrogen, C–N/NH₃, and ammonium species, phosphorus was dominantly present as pyrophosphate and metaphosphate species, while sulfur was detected as organic sulfide and oxidized sulfur species (sulfate/sulfone). Overall, the two-step synthesis method exhibited superior performance in developing a more stable porous structure, whereas the one-step synthesis method was more effective in retaining heteroatoms at elevated carbonization temperatures.

Item Type:	Thesis (Other)
Uncontrolled Keywords:	Karbon Berpori, Polifenilen Sulfida, Doping Heteroatom, Nitrogen, Fosfor, Sulfur, Sintesis Satu Tahap, Sintesis Dua Tahap. Porous Carbon, Polyphenylene Sulfide, Heteroatom Doping, Nitrogen, Phosphorus, Sulfur, One step synthesis, Two step synthesis.
Subjects:	Q Science > QD Chemistry > QD281 Pyrolysis
Divisions:	Faculty of Science and Data Analytics (SCIENTICS) > Chemistry > 47201-(S1) Undergraduate Thesis
Depositing User:	Chiara Geralda Dahayu Wibowo
Date Deposited:	04 Aug 2026 01:26
Last Modified:	04 Aug 2026 01:26
URI:	http://repository.its.ac.id/id/eprint/142618

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