Production of Biofuel via Catalytic Hydrocracking of Kapuk (Ceiba pentandra) Seed Oil with NiMo/HZSM-5 Catalyst

Biofuel is one of alternative energy that is being developed today to solve the problem of limited fossil fuel as an energy source. The goal of this study is to produce biofuel from kapuk (Ceiba pentandra) seed oil (KSO) through catalytic hydrocracking process using NiMo/HZSM-5 catalyst. NiMo/HZSM-5 catalyst was obtained by impregnation of nickel and molybdenum as metallic precursors on HZSM-5 catalyst as support using incipient wetness impregnation method. It was found that the surface area of the catalyst was 222.1350 m2/g, the pore diameter was 3.0148 nm and the pore volume was 0.1674 cm3/g. The diffraction peaks of nickel oxide phase and the metallic phase of nickel were observed at 2θ of 62.5102° and 51.7283°. Molybdenum oxide phases were observed at 2θ of 53.5674° and 60.4682°. The catalytic hydrocracking process was performed using slurry pressure batch reactor at the temperature of 350°C for 2 h. The obtained liquid product was analyzed using GC-MS in order to determine the organic content. It has been found that the highest compounds were the palmitic acid with 23.14 area%. Besides, the hydrocarbon composition consisted of 33.93 area% (i.e. 4.34 area% cycloparaffins, 16.02 area% n-paraffins, 12.26 area% olefins, and 1.30 area% of aromatics) and 58.73 area% of carboxylic acid. Thus, it can be concluded that NiMo/HZSM-5 catalyst can convert KSO into biofuel through catalytic hydrocracking process at the temperature of 350°C for 2 h.

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Synthesis of Nickel-loaded Sulfated Zirconia Catalyst and Its Application for Converting Used Palm Cooking Oil to Gasoline via Hydrocracking Process

Periodica Polytechnica Chemical Engineering ◽

10.3311/ppch.18209 ◽

2021 ◽

Author(s):

Ilyas Taufik Abdul Aziz ◽

Wahyu Dita Saputri ◽

Wega Trisunaryanti ◽

Sri Sudiono ◽

Akhmad Syoufian ◽

...

Keyword(s):

Sulfated Zirconia ◽

Liquid Product ◽

Gasoline Fraction ◽

Incipient Wetness Impregnation ◽

Impregnation Method ◽

Cooking Oil ◽

Hydrocracking Process ◽

Ni Content ◽

Zirconia Catalyst ◽

Sulfated Zirconia Catalyst

The synthesis of the nickel-loaded sulfated zirconia catalyst (Ni-SZ) and its application for the hydrocracking process have been carried out. This work has been conducted to determine the activity and selectivity from various Ni concentrations loaded on sulfated zirconia (SZ) in the hydrocracking of used palm cooking oil. The synthesis technique was preceded by sulfation of ZrO2 through incipient wetness impregnation method using H2SO4 solution and then continued with the impregnation of Ni via hydrothermal method employing NiSO4 · 6H2O precursor salt. The hydrocracking process was performed in a fix-bed microreactor at the optimum temperature (350 °C). The SZ loaded with 3 wt% of Ni (Ni-SZ 3) successfully produced the highest liquid product (44.25 wt%) and selectivity on gasoline (100 %). Besides, the gasoline fraction in the liquid product was dominated by unwanted aromatics compounds. The excellent performance of Ni-SZ 3 due to it has high acidity value, specific surface area, and Ni content.

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Biofuel from hydrocracking of Cerbera manghas oil over Ni-Zn/HZSM-5 catalyst

Eclética Química Journal ◽

10.26850/1678-4618eqj.v47.1.2022.p17-39 ◽

2022 ◽

Vol 47 (1) ◽

pp. 17-39

Author(s):

Lenny Marlinda ◽

Danawati Hari Prajitno ◽

Achmad Roesyadi ◽

Ignatius Gunardi ◽

Yustia Wulandari Mirzayanti ◽

...

Keyword(s):

Batch Reactor ◽

Hydrocarbon Composition ◽

Absorption Spectrometry ◽

Gas Chromatography Mass Spectrometry ◽

Incipient Wetness Impregnation ◽

Impregnation Method ◽

X Ray Diffraction ◽

Transportation Fuel ◽

X Ray ◽

Cerbera Manghas

The effects of reaction temperature on the hydrocarbon composition of biofuel produced in hydrocracking of Cerbera manghas oil with Ni-Zn/HZSM-5 catalyst were investigated. The incipient wetness impregnation method was applied to prepare the Ni-Zn/HZSM-5 catalysts. Furthermore, the properties of catalysts were measured by X-ray diffraction, atomic absorption spectrometry, and nitrogen physisorption. Hydrocracking process was carried out in Parr USA pressure batch reactor at pressure of 20 � 5 bar after flowing H2 for 1 h. The reaction with a catalyst/oil ratio of 1 g/150 mL proceeded at various temperatures of 350, 375 and 400 �C for 2 h. Gas chromatography-mass spectrometry was�used to analyze biofuel. The most abundant hydrocarbon compounds in biofuel were identified as pentadecane and heptadecane (a major diesel fuel compound) with a different amount at different reaction temperatures. It can be said that the hydrodecarboxylation/decarbonylation routes were the predominant reaction pathways and oxygen removal occurred during hydrocracking. The Cerbera manghas oil can be recommended as a promising biofeed to produce the gasoil as an alternative transportation fuel.

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Triglycerides Hydrocracking Reaction of Nyamplung Oil with Non-sulfided CoMo/γ-Al2O3 Catalysts

BULLETIN OF CHEMICAL REACTION ENGINEERING AND CATALYSIS ◽

10.9767/bcrec.13.2.734.196-203 ◽

2018 ◽

Vol 13 (2) ◽

pp. 196

Author(s):

Rismawati Rasyid ◽

Rahmaniah Malik ◽

Heri Septya Kusuma ◽

Achmad Roesyadi ◽

Mahfud Mahfud

Keyword(s):

Kinetic Model ◽

Operating Temperature ◽

Batch Reactor ◽

Liquid Product ◽

Reaction Engineering ◽

Impregnation Method ◽

Hydrocracking Process ◽

Reaction Conversion ◽

Simple Kinetic Model ◽

Al2o3 Catalyst

The purpose of this research are to study the temperature influence in hydrocracking process of the nyamplung oil (Calophyllum inophyllum) using a non-sulfided CoMo/γ-Al2O3 catalyst and to develop a simple kinetic model in interpreting the data of hydrocracking products. The experiment was carried out in a pressurized batch reactor operated pressure up 30 bar. The CoMo catalyst supported with γ-Al2O3 was prepared through impregnation method without sulfidation process. The operating temperature varied from 200 to 350 oC. The results show that the non-sulfided CoMo/γ-Al2O3 catalysts, nyamplung oil triglycerides can converted into gasoil and gasoline-like hydrocarbons. The triglyceride hydrocracking reaction of nyamplung oil followed a several stages, i.e., hydrogenation, dehydrogenation, and cracking. Based on the compounds contained in liquid product, hydrocracking reaction was dominated by decarboxylation. The products obtained in hydrocracking process of nyamplung oil are classified to gasoil (C11-C18) and gasoline (C5-C10). The triglycerides hydrocracking reaction of nyamplung oil was assumed by following a series reaction mechanism and a simple kinetic model used for determined the kinetics constants. The highest reaction conversion is 99.10% obtained at temperature of 350 °C for 160 minutes reaction time. Copyright © 2018 BCREC Group. All rights reservedReceived: 20th October 2017; Revised: 8th September 2017; Accepted: 17th September 2017; Available online: 11st June 2018; Published regularly: 1st August 2018How to Cite: Rasyid, R., Malik, R., Kusuma, H.S., Roesyadi, A., Mahfud, M. (2018). Triglycerides Hydrocracking Reaction of Nyamplung Oil with Non-sulfided CoMo/γ-Al2O3 Catalysts. Bulletin of Chemical Reaction Engineering & Catalysis, 13 (2): 196-203 (doi:10.9767/bcrec.13.2.734.196-203)

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Zn-Mo/HZSM-5 Catalyst for Gasoil Range Hydrocarbon Production by Catalytic Hydrocracking of Ceiba pentandra oil

BULLETIN OF CHEMICAL REACTION ENGINEERING AND CATALYSIS ◽

10.9767/bcrec.13.1.1508.136-143 ◽

2018 ◽

Vol 13 (1) ◽

pp. 136 ◽

Cited By ~ 2

Author(s):

Yustia Wulandari Mirzayanti ◽

Firman Kurniawansyah ◽

Danawati Hari Prayitno ◽

Achmad Roesyadi

Keyword(s):

Vegetable Oil ◽

Batch Reactor ◽

Liquid Hydrocarbon ◽

Incipient Wetness Impregnation ◽

Impregnation Method ◽

Gas Oil ◽

Transportation Fuel ◽

Hydrocarbon Production ◽

Ceiba Pentandra ◽

Metal Ratio

Biofuel from vegetable oil becomes one of the most suitable and logical alternatives to replace fossil fuel. The research focused on various metal ratio Zinc/Molybdenum/HZSM-5 (Zn-Mo/HZSM-5) catalyst to produce liquid hydrocarbon via catalytic hydrocracking of Ceiba penandra oil. The catalytic hydrocracking process has been applied in this study to crack Ceiba pentandra oil into a gasoil range hydrocarbon using Zn-Mo/HZSM-5 as a catalyst. The effect of various reaction temperature on the catalytic hydrocracking of Ceiba pentandra oil were studied. The Zn-Mo/HZSM-5 catalyst with metal ratio was prepared by incipient wetness impregnation method. This process used slurry pressure batch reactor with a mechanical stirrer. A series of experiments were carried out in the temperature range from 300-400 oC for 2 h at pressure between 10-15 bar. The conversion and selectivity were estimated. The liquid hydrocarbon product were identified to gasoline, kerosene, and gas oil. The results show that the use of Zn-Mo/HZSM-5 can produce gas oil as the most component in the product. Overall, the highest conversion and selectivity of gas oil range hydrocarbon was obtained when the ZnMo/HZSM-5 metal ratio was Zn(2.86 wt.%)-Mo(5.32 wt.%)/HZSM-5 and the name is Zn-Mo/HZSM-5_102. The highest conversion was obtained at 63.31 % and n-paraffin (gas oil range) selectivity was obtained at 90.75 % at a temperature of 400 oC. Ceiba pentandra oil can be recommended as the source of inedible vegetable oil to produce gasoil as an environmentally friendly transportation fuel. Copyright © 2018 BCREC Group. All rights reservedReceived: 8th September 2017; Revised: 9th September 2017; Accepted: 17th September 2017; Available online: 22nd January 2018; Published regularly: 2nd April 2018How to Cite: Mirzayanti, Y.W., Kurniawansyah, F., Prajitno, D.H., Roesyadi, A. (2018). Zn-Mo/HZSM-5 Catalyst for Gasoil Range Hydrocarbon Production by Catalytic Hydrocracking of Ceiba pentandra oil. Bulletin of Chemical Reaction Engineering & Catalysis, 13 (1): 136-143 (doi:10.9767/bcrec.13.1.1354.136-143)

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The Characterization of Synthetic Zeolite for Hydrocracking of Waste Cooking Oil into Fuel

REAKTOR ◽

10.14710/reaktor.20.2.89-95 ◽

2020 ◽

Vol 20 (2) ◽

pp. 89-95

Author(s):

Siti Salamah ◽

Agus Aktawan ◽

Ilham Mufandi

Keyword(s):

Batch Reactor ◽

Liquid Product ◽

Waste Cooking Oil ◽

Synthetic Zeolite ◽

Zeolite A ◽

Hydrogen Flow ◽

Cooking Oil ◽

Hydrocracking Process ◽

Hydrocracking Catalyst ◽

Pore Properties

Zeolite A was used as hydrocracking catalyst to convert cooking oil into potential renewable fuels. The experiment was performed by characterize the diffraction, and pore properties the synthetic zeolite and it was confirmed the synthetic zeolite was zeolite A. The hydrocracking process of waste cooking oil was carried out in semi-fixed batch reactor system at 450° C for 2 hours, under the hydrogen flow of 20 ml/minute. The diffractogram and Si/Al ratio, 1.6, were matched to zeolite A properties, with the surface area, pore diameter, and pore volume were, 1.163 m2/g, 3.93 nm, and 0.001 cc/g, respectively. Liquid product from hydrocracking process of cooking oil consisted of 28.99% alkane and alkene 26.59% that are potential as renewable fuels.Keywords: waste cooking oil; zeolite A; hydrocracking

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Catalytic and Thermal Cracking of Bio-Oil from Oil-Palm Empty Fruit Bunches, in Batch Reactor

Indonesian Journal of Chemistry ◽

10.22146/ijc.44076 ◽

2020 ◽

Vol 20 (5) ◽

pp. 1000

Author(s):

Santiyo Wibowo ◽

Lisna Efiyanti ◽

Gustan Pari

Keyword(s):

Specific Gravity ◽

Oil Palm ◽

Batch Reactor ◽

Liquid Product ◽

Calorific Value ◽

Product Yield ◽

Catalyst Characterization ◽

Impregnation Method ◽

Empty Fruit Bunches ◽

Bio Oil

The world’s potency of fossil-derived petroleum fuels has declined steadily, while its consumption continues to rise ominously. Therefore, several countries have started to develop renewable fuels like bio-oil from biomass. Relevantly, the aim of this research was to explore the technical feasibility of upgrading the qualities of crude bio-oil (CBO) produced from the pyrolysis on oil-palm empty fruit bunches (OPEFB) using Ni/NZA catalyst in a batch reactor. The natural zeolite (NZ) was activated by HCL 6 N and NH4Cl (obtained sample NZA). Supporting Ni onto NZA was conducted with an impregnation method using a salt precursor of Ni(NO3)2·6H2O followed by calcination with a temperature of 500 °C. Catalyst characterization includes determining the site of TO4 (T = Si or Al) in zeolites, acidity, crystallinity, and catalyst morphology. Cracking reaction of CBO was carried out in batch reactor in varied temperatures of 250 and 300 °C with the variation of catalyst weight of 0, 4, 6, and 8% toward CBO. Several analyses of the liquid product such as product yield, specific gravity, pH, viscosity, calorific value, and chemical compound were conducted. The results showed that acidification and Ni loading on zeolite samples increased their acidity. The optimum CBO’s cracking condition was judged to be the temperature of 300 °C with 6% Ni/NZA catalyst use, whereby the fuel yield reached 26.42% and dominated by particular compounds comprising phenol, octanoic acid, and alkane hydrocarbons. Under such conditions, the characteristics of fuel were pH 3.54, specific gravity 0.995, viscosity 14.3 cSt, and calorific value 30.85 MJ/kg.

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Hydrocracking of Cerbera manghas Oil with Co-Ni/HZSM-5 as Double Promoted Catalyst

BULLETIN OF CHEMICAL REACTION ENGINEERING AND CATALYSIS ◽

10.9767/bcrec.12.2.496.167-184 ◽

2017 ◽

Vol 12 (2) ◽

pp. 167 ◽

Cited By ~ 5

Author(s):

Danawati Hari Prajitno ◽

Lenny Marlinda ◽

Muhammad Al-Muttaqii ◽

Ignatius Gunardi ◽

Achmad Roesyadi

Keyword(s):

Batch Reactor ◽

Initial Pressure ◽

Hydrocarbon Composition ◽

Operating Conditions ◽

Gas Chromatography Mass Spectrometry ◽

Incipient Wetness Impregnation ◽

Transportation Fuel ◽

Rich Mixture ◽

Metals Loading ◽

Cerbera Manghas

The effect of various reaction temperature on the hydrocracking of Cerbera manghas oil to produce a paraffin-rich mixture of hydrocarbons with Co-Ni/HZSM-5 as doubled promoted catalyst were studied. The Co-Ni/HZSM-5 catalyst with various metal loading and metal ratio was prepared by incipient wetness impregnation. The catalysts were characterized by XRD, AAS, and N2 adsorption-desorption. Surface area, pore diameter, and pore volume of catalysts decreased with the increasing of metals loading. The hydrocracking process was conducted under hydrogen initial pressure in batch reactor equipped with a mechanical stirrer. The reaction was carried out at a temperature of 300-375 oC for 2 h. Depending on the experimental condition, the reaction pressure changed between 10 bar and 15 bar. Several parameters were used to evaluate biofuel produced, including oxygen removal, hydrocarbon composition and gasoline/kerosene/diesel yields. Biofuel was analyzed by Fourier Transform Infrared Spectroscopic (FTIR) and gas chromatography-mass spectrometry (GC-MS). The composition of hydrocarbon compounds in liquid products was similar to the compounds in the gasoil sold in unit of Pertamina Gas Stations, namely pentadecane, hexadecane, heptadecane, octadecane, and nonadecane with different amounts for each biofuel produced at different reaction temperatures. However, isoparaffin compounds were not formed at all operating conditions. Pentadecane (n-C15) and heptadecane (n-C17) were the most abundant composition in gasoil when Co-Ni/HZSM-5 catalyst was used. Cerbera Manghas oil can be recommended as the source of non-edible vegetable oil to produce gasoil as an environmentally friendly transportation fuel. Copyright © 2017 BCREC Group. All rights reservedReceived: 20th May 2016; Revised: 30th January 2017; Accepted: 10th February 2017How to Cite: Prajitno, D.H., Roesyadi, A., Al-Muttaqii, M., Marlinda, L., Gunardi, I. (2017). Hydrocracking of Cerbera manghas Oil with Co-Ni/HZSM-5 as Double Promoted Catalyst. Bulletin of Chemical Reaction Engineering & Catalysis, 12 (2): 167-184 (doi:10.9767/bcrec.12.2.496.167-184)Permalink/DOI: http://dx.doi.org/10.9767/bcrec.12.2.496.167-184

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Bio-kerosene and Bio-gasoil from Coconut Oils via Hydrocracking Process over Ni-Fe/HZSM-5 Catalyst

BULLETIN OF CHEMICAL REACTION ENGINEERING AND CATALYSIS ◽

10.9767/bcrec.14.2.2669.309-319 ◽

2019 ◽

Vol 14 (2) ◽

pp. 309 ◽

Cited By ~ 1

Author(s):

Muhammad Al-Muttaqii ◽

Firman Kurniawansyah ◽

Danawati Hari Prajitno ◽

Achmad Roesyadi

Keyword(s):

Reaction Temperature ◽

Batch Reactor ◽

Coconut Oil ◽

Liquid Hydrocarbon ◽

Biofuel Production ◽

Gas Chromatography Mass Spectrometry ◽

Incipient Wetness Impregnation ◽

Impregnation Method ◽

X Ray Diffraction ◽

X Ray

In this study, hydrocracking of coconut oil over Ni-Fe/HZSM-5 catalyst was carried out in a batch reactor under different reaction temperature. Coconut oil is proposed as one of the potential feedstock for biofuel production. The Ni-Fe/HZSM-5 catalyst was prepared by incipient wetness impregnation method. The characterization of Ni-Fe/HZSM-5 catalyst by X-Ray Diffraction (XRD), Scanning Electron Microscopy-Energy Dispersive X-ray (SEM-EDAX), and Brunauer-Emmett-Teller (BET). The chemical composition of biofuel was analyzed by Gas-Chromatography-Mass Spectrometry (GC-MS). The results from the GC-MS analysis showed that the hydrocracking reaction over 10 % (Ni-Fe)/HZSM-5 catalyst at temperature of 375 oC obtained the highest hydrocarbon content (contained 49.4% n-paraffin, 26.93 % isoparaffin, 3.58 % olefin) and the highest yield of bio-gasoil 38.6 % in the biofuel liquid hydrocarbon. Pentadecane (n-C15) and heptadecane (n-C17) were the most abundant hydrocarbon compounds in biofuel liquid hydrocarbon. Decarboxylation and/or decarbonylation was the dominant reaction pathways in this process. Based on the result, the reaction temperature had a significant effect on the distribution of biofuel composition and yield of biofuel from coconut oil. Copyright © 2019 BCREC Group. All rights reserved

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Catalytic Conversion of Residual Palm Oil in Spent Bleaching Earth (SBE) By HZSM-5 Zeolite based-Catalysts

BULLETIN OF CHEMICAL REACTION ENGINEERING AND CATALYSIS ◽

10.9767/bcrec.13.3.1929.456-465 ◽

2018 ◽

Vol 13 (3) ◽

pp. 456 ◽

Cited By ~ 3

Author(s):

Mohd Lukman Musa ◽

Ramli Mat ◽

Tuan Amran Tuan Abdullah

Keyword(s):

Palm Oil ◽

Batch Reactor ◽

Bleaching Earth ◽

Fixed Bed ◽

Nitrogen Adsorption ◽

Catalytic Conversion ◽

Fixed Bed Reactor ◽

Incipient Wetness Impregnation ◽

Impregnation Method ◽

Liquid Biofuel

Bleaching earth is used to remove colour, phospholipids, oxidized products, metals and residual gums in the palm oil process refinery. Once adsorption process end, the spent bleaching earth (SBE) which contains approximately 20-40 wt. % of the adsorbed oil was usually disposed to landfills. The oil content in SBE was recovered by catalytic cracking using transition metal (Cu, Zn, Cr, and Ni) doped HZSM-5 zeolite in a batch reactor (pyrolysis zone) and fixed bed reactor (catalyst bed). The 5 wt. % of each metallic was introduced in HZSM-5 zeolite using incipient wetness impregnation method. The main objective of this study was to investigate the performance of modified HZSM-5 zeolite for cracking of residual oil in SBE. The physicochemical properties of the catalysts were characterized using XRD, FTIR, Nitrogen adsorption, and TPD-NH3. Liquid biofuel obtained from cracking was analyzed by GC-MS. The incorporation of metallic loaded on HZSM-5 zeolite has reduced the surface area of the catalyst that gives a significant impact to the catalytic behavior. The Ni/HZSM-5 zeolite exhibited the highest yields of alkenes as compared to others but slightly decreases the yield of alkanes whereas in contrast with the Cr/HZSM-5, the obtained alkanes were found higher than that of alkenes. In addition, the Cr/HZSM-5 and Ni/HZSM-5 favored the conversion of polycyclic aromatics to mono-aromatics, whereas parent HZSM-5 catalyst favored the formation of poly-aromatics. These results indicated that the metal loaded on HZSM-5 can promote the cracking of heavy fractions to lighter hydrocarbon thus can be used for cracking oil in SBE. Copyright © 2018 BCREC Group. All rights reservedReceived: 10th December 2017; Revised: 31st May 2018; Accepted: 10th June 2018How to Cite: Musa, M.L., Mat, R., Abdullah, T.A.T. (2018). Catalytic Conversion of Residual Palm Oil in Spent Bleaching Earth (SBE) By HZSM-5 Zeolite based-Catalysts. Bulletin of Chemical Reaction Engineering & Catalysis, 13 (3): 456-465 (doi:10.9767/bcrec.13.3.1929.456-465)Permalink/DOI: https://doi.org/10.9767/bcrec.13.3.1929.456-465

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Tungsten Oxide-Modified SSZ-13 Zeolite as an Efficient Catalyst for Ethylene-To-Propylene Reaction

Catalysts ◽

10.3390/catal11050553 ◽

2021 ◽

Vol 11 (5) ◽

pp. 553

Author(s):

Mansurbek Urol ugli Abdullaev ◽

Sungjune Lee ◽

Tae-Wan Kim ◽

Chul-Ung Kim

Keyword(s):

Tungsten Oxide ◽

Fixed Bed ◽

Acid Sites ◽

Fixed Bed Reactor ◽

Incipient Wetness Impregnation ◽

Impregnation Method ◽

Efficient Catalyst ◽

X Ray ◽

Propylene Selectivity ◽

Temperature Programmed

Among the zeolitic catalysts for the ethylene-to-propylene (ETP) reaction, the SSZ-13 zeolite shows the highest catalytic activity based on both its suitable pore architecture and tunable acidity. In this study, in order to improve the propylene selectivity further, the surface of the SSZ-13 zeolite was modified with various amounts of tungsten oxide ranging from 1 wt% to 15 wt% via a simple incipient wetness impregnation method. The prepared catalysts were characterized with several analysis techniques, specifically, powder X-ray diffraction (PXRD), Raman spectroscopy, temperature-programmed reduction of hydrogen (H2-TPR), temperature-programmed desorption of ammonia (NH3-TPD), inductively coupled plasma-atomic emission spectroscopy (ICP-AES), and N2 sorption, and their catalytic activities were investigated in a fixed-bed reactor system. The tungsten oxide-modified SSZ-13 catalysts demonstrated significantly improved propylene selectivity and yield compared to the parent H-SSZ-13 catalyst. For the tungsten oxide loading, 10 wt% loading showed the highest propylene yield of 64.9 wt%, which was 6.5 wt% higher than the pristine H-SSZ-13 catalyst. This can be related to not only the milder and decreased strong acid sites but also the diffusion restriction of bulky byproducts, as supported by scanning transmission electron microscopy-energy dispersive X-ray spectroscopy (STEM-EDS) observation.

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