Crystallite Size and Microstrain Measurement of Cathode Material after Mechanical Milling using Neutron Diffraction Technique

Fajar, Andika; Gunawan, Gunawan; Kartini, Evvy; Mugirahardjo, Herry; Ihsan, Mohammad

doi:10.17146/aij.2010.27

Cited by 12 publications

(6 citation statements)

References 8 publications

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“…However, larger changes are observed with respect to the c-axis, in agreement with other works. 9,[59][60][61][62] The Rietveld refinement also confirmed the presence of a minority second phase of the spinel Co 3 O 4 in the blank test, gelatin and starch samples. This observation is related to the crystallite energy formation.…”

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confidence: 59%

“…A small amount of spinel Co 3 O 4 was found as secondary phase in the diffraction patterns of the blank test and of the starch and gelatin precursors, although HT-LiCoO 2 can be described as a major constituent. 6,9,[57][58][59][60][61][62] The XRD analyses of the HT-LiCoO 2 compounds synthesized with the precursors and the blank test were compared to evaluate the influence of the gelling agent in the product structural formation. The analysis of Figure 4 shows that the precursors' XRD has narrower peaks than the blank test.…”

Section: Resultsmentioning

confidence: 99%

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Synthesis and Characterization of LiCoO2 from Different Precursors by Sol‑Gel Method

Freitas

Siqueira

Costa

et al. 2017

J. Braz. Chem. Soc.

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Lithium cobalt oxide, LiCoO 2 , widely used as cathode in lithium ion batteries was synthesized and their structural and electronic properties investigated. The crystalline powders were prepared by the sol-gel method with four complexing agents: citric acid, glycine, starch and gelatin. These syntheses were compared with the blank test (without complexing agent). The X-ray diffraction and vibrational spectroscopy allowed the identification of the rhombohedral phase LiCoO 2 ( ) as the only or principal crystalline component in all samples. A small fraction of a second phase of cubic spinel Co 3 O 4 was observed in the samples of starch, gelatin and the blank test. The Rietveld refinements showed small structural variations, indicating reduced influence of the complexing agents on the synthesis. The theoretical HOMO-LUMO (highest occupied molecular orbital-lowest unoccupied molecular orbital) gap values are in agreement to those estimated by diffuse reflectance spectroscopy (DRS). The scanning electron microscopy (SEM) showed morphological pattern regardless of the complexing agent used, showing an alternative method.Keywords: LiCoO 2 , sol-gel method, XRD, Rietveld refinement, lithium ion batteries, DFT IntroductionLithium cobalt oxide, LiCoO 2 , has been the focus of many studies regarding their structural and electronic properties. [1][2][3][4][5][6][7][8] This system has interesting electrochemical features that allows a wide use as cathodes of lithium ion batteries. 2,4 The investigation of the structural aspects of the material is a crucial issue to better understand the electrochemical properties of the LiCoO 2 compound. [1][2][3][4][5][6][7][8][9][10][11][12][13][14][15][16][17] For example, the nature of the crystal, its size and shape, are directly related with its electrochemical characteristics. 2 The LiCoO 2 synthesized at low temperatures (LT), below 500 °C, presents a cubic spinel structure ( ), while the synthesis at high temperatures (HT) (above 500 °C), generates the rhombohedral structure with stratified layers ( ). Therefore, several authors usually classify these structures as LT-LiCoO 2 and HT-LiCoO 2 , respectively . 1,2,7,8,[18][19][20][21][22][23][24] The rhombohedral phase is characterized by a structure with alternating layers of cobalt and lithium cations intercalated with oxygen anions. 22 The lithium and cobalt(III) ions are arranged in intercalated layers (Figure 1a). The cobalt(III) ion is located at the octahedral sites, forming a strong bond with the neighboring oxygen anion to constitute the Co−O layers (Figure 1b). Finally, the lithium layers are intercalated between the CoO 2 plans. 1,3,4 The octahedral sites of these layers are occupied by lithium and cobalt(III) ions alternately that forms a sequential stacking with oxygen ion layers in a close packing of the ABCABC type ( Figure 1c). 4,5 This specific stacking arrangement leads to an environment equivalent for all ions, allowing the maximum charge delocalization and the minimal system energy. 1,3,4 The degree of crystal orde...

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confidence: 59%

Section: Resultsmentioning

confidence: 99%

Synthesis and Characterization of LiCoO2 from Different Precursors by Sol‑Gel Method

Freitas

Siqueira

Costa

et al. 2017

J. Braz. Chem. Soc.

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“…The broadening of the magnetic peaks also suggests a short magnetic coherence length estimated to B1/5 of the crystalline coherence length from the Scherrer equation, which likely explains the low value of the refined magnetic moment. 17 In comparison with similar A-site manganites, DPv_Mn 2 LiReO 6 presents exclusive factors that may explain the unprecedented giant coercivity values observed. The other four existent DPv_Mn 2 BReO 6 (B = Mn 2+ , Fe 3+ , Co 2+ , Ni 2+ ) [8][9][10][11][12][13] contain Re in either 5+ (5d 2 ) or 6+ (5d 1 ) oxidation states with not-quenched SOC.…”

Section: Resultsmentioning

confidence: 94%

Giant coercivity and spin clusters in high pressure polymorphs of Mn₂LiReO₆.

et al. 2022

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“…The microstrain, ε, in %, was calculated from the full width half maximum (FWHM) Lorentzian component, X, from each sample, assuming [62]: 1The neutron induced defects were imaged using a transmission electron microscope, TEM (Tecnai TF30-FEG STwin STEM, FEI Company, Hillsboro, OR, USA) equipped with an electron energy loss spectroscope, EELS (GIF System, Gatan, Inc., Pleasanton, CA, USA), and an energy dispersive X-ray spectroscope, EDX (EDAX Inc., Mahwah, NJ, USA). TEM lamellas were prepared using a Ga + focused ion beam, FIB, (Quanta 3D FEG, FEI, Hillsboro, OR, USA) by milling out ~ 25×2×15 µm 3 sections from the irradiated resistivity bars, which were then lifted onto TEM Cu grids.…”

Section: Introductionmentioning

confidence: 99%

Effects of neutron irradiation of Ti3SiC2 and Ti3AlC2 in the 121–1085 °C temperature range

Tallman

Gan

et al. 2017

Journal of Nuclear Materials

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Herein we report on the formation of defects in response to neutron irradiation of polycrystalline Ti 3 SiC 2 and Ti 3 AlC 2 samples exposed to total fluences of ≈ 6×10 20 n/m 2 , 5×10 21 n/m 2 and 1.7×10 22 n/m 2 at irradiation temperatures of 121(12), 735(6) and 1085(68) °C. These fluences correspond to 0.14, 1.6 and 3.4 dpa, respectively. After irradiation to 0.14 dpa at 121 °C and 735 °C, black spots are observed via transmission electron microscopy in both Ti 3 SiC 2 and Ti 3 AlC 2. After irradiation to 1.6 and 3.4 dpa at 735 °C, basal dislocation loops, with a Burgers vector of b = ½ [0001] are observed in Ti 3 SiC 2 , with loop diameters of 21(6) and 30(8) nm after 1.6 dpa and 3.4 dpa, respectively. In Ti 3 AlC 2 , larger dislocation loops, 75(34) nm in diameter are observed after 3.4 dpa at 735 °C, in addition to stacking faults. Impurity particles of TiC, as well as stacking fault TiC platelets in the MAX phases, are seen to form extensive dislocation loops under all conditions. Cavities were observed at grain boundaries and within stacking faults after 3.4 dpa irradiation, with extensive cavity formation in the TiC regions at 1085 °C. Remarkably, denuded zones on the order of 1 μm are observed in Ti 3 SiC 2 after irradiation to 3.4 dpa at 735 °C. Small grains, 3-5 μm in diameter, are damage free after irradiation at 1085 °C at this dose. The results shown herein confirm once again that the presence of the A-layers in the MAX phases considerably enhance their irradiation tolerance. Based on these results, and up to 3.4 dpa, Ti 3 SiC 2 remains a promising candidate for high temperature nuclear applications as long as the temperature remains > 700 °C.

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Crystallite Size and Microstrain Measurement of Cathode Material after Mechanical Milling using Neutron Diffraction Technique

Cited by 12 publications

References 8 publications

Synthesis and Characterization of LiCoO2 from Different Precursors by Sol‑Gel Method

Synthesis and Characterization of LiCoO2 from Different Precursors by Sol‑Gel Method

Giant coercivity and spin clusters in high pressure polymorphs of Mn₂LiReO₆.

Effects of neutron irradiation of Ti3SiC2 and Ti3AlC2 in the 121–1085 °C temperature range

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Crystallite Size and Microstrain Measurement of Cathode Material after Mechanical Milling using Neutron Diffraction Technique

Cited by 12 publications

References 8 publications

Synthesis and Characterization of LiCoO2 from Different Precursors by Sol‑Gel Method

Synthesis and Characterization of LiCoO2 from Different Precursors by Sol‑Gel Method

Giant coercivity and spin clusters in high pressure polymorphs of Mn2LiReO6.

Effects of neutron irradiation of Ti3SiC2 and Ti3AlC2 in the 121–1085 °C temperature range

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Giant coercivity and spin clusters in high pressure polymorphs of Mn₂LiReO₆.