Unravelling Ultraslow Lithium-Ion Diffusion in γ-LiAlO2: Experiments with Tracers, Neutrons, and Charge Carriers
Wiedemann, Dennis; Nakhal, Suliman; Rahn, Johanna; Witt, Elena; Islam, Mazharul M.; Zander, Stefan; Heitjans, Paul; Schmidt, Harald; Bredow, Thomas; Wilkening, Martin; Lerch, Martin; Chemistry of Materials 28 (2016) 915–; doi:10.1021/acs.chemmater.5b04608

data_4002658
_publ_section_title
;
 Unravelling Ultraslow Lithium-Ion Diffusion in \g-LiAlO2: Experiments
 with Tracers, Neutrons, and Charge Carriers
;
_journal_issue                   3
_journal_name_full               'Chemistry of Materials'
_journal_page_first              915
_journal_paper_doi               10.1021/acs.chemmater.5b04608
_journal_volume                  28
_journal_year                    2016
_chemical_absolute_configuration unk
_chemical_formula_sum            'Al Li O2'
_chemical_formula_weight         65.9
_chemical_name_common            '\g-lithium aluminate'
_chemical_name_structure_type    \g-LiAlO~2~
_chemical_name_systematic        '\g-lithium aluminium dioxide'
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      92
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   notdet
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   notdet
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.1965(2)
_cell_length_b                   5.1965(2)
_cell_length_c                   6.3464(3)
_cell_measurement_temperature    1023
_cell_volume                     171.376(12)
_computing_cell_refinement       'JANA2006 (Pet\<r\'i\<cek, 2014)'
_computing_data_collection       'CARESS 6.6 (Busse et al., 2013)'
_computing_data_reduction        'BEAN 9.2 (Fromme et al., 2000)'
_computing_molecular_graphics    'Diamond 3.2 (Brandenburg, 2013)'
_computing_publication_material  'JANA2006 (Pet\<r\'i\<cek, 2014)'
_computing_structure_refinement  'JANA2006 (Pet\<r\'i\<cek, 2014)'
_computing_structure_solution    'ICSD (Bergerhoff, 1987)'
_diffrn_ambient_environment      vacuum
_diffrn_ambient_temperature      1023
_diffrn_detector                 '^3^He counter'
_diffrn_detector_details
; array of eight DENEX area detectors (active area: 300 \\times 300 mm^2^) with
oscillating radial collimator for background reduction
;
_diffrn_measurement_device       'one-circle powder diffractometer'
_diffrn_measurement_device_details
; D. M. T\"obbens, N. St\"u\&ser, K. Knorr, H. M. Mayer, G. Lampert,
Mater. Sci. Forum 2001, 378-381, 288-293
;
_diffrn_measurement_device_type  FIREPOD
_diffrn_measurement_method       'profile data from area detector'
_diffrn_radiation_monochromator  'Sapphire filter, Ge (511)'
_diffrn_radiation_probe          neutron
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     1.7982(1)
_diffrn_source                   'nuclear reactor'
_diffrn_source_type              'BER II beamline T5'
_exptl_absorpt_coefficient_mu    0.165
_exptl_absorpt_correction_type   cylinder
_exptl_absorpt_process_details
; correction for a cylindrical sample with \mR = 0.487 as
implemented in JANA2006
;
_exptl_crystal_density_diffrn    2.5549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             52.62
_pd_char_atten_coef_mu_calc      0.100
_pd_char_colour                  colourless
_pd_instr_2theta_monochr_pre     111.7
_pd_instr_beam_size_ax           90
_pd_instr_dist_mono/spec         2500
_pd_instr_dist_spec/detc         980
_pd_instr_dist_src/mono          11000
_pd_instr_geometry               Debye-Scherrer
_pd_instr_location
; Fine Resolution Powder Diffractometer (FIREPOD, E9), Helmholtz-Zentrum,
Berlin (Germany)
;
_pd_instr_monochr_pre_spec       'Sapphire filter, Ge (511)'
_pd_instr_soller_eq_mono/spec    0.66667
_pd_instr_soller_eq_spec/detc    0.16667
_pd_instr_soller_eq_src/mono     0.30000
_pd_meas_2theta_range_inc        0.075
_pd_meas_2theta_range_max        141.755
_pd_meas_2theta_range_min        0.005
_pd_meas_number_of_points        1891
_pd_meas_scan_method             step
_pd_proc_2theta_range_inc        0.075
_pd_proc_2theta_range_max        138.23
_pd_proc_2theta_range_min        15.005
_pd_proc_info_data_reduction
; integration of measured 2D intensities along Debye--Scherrer rings to give
1D data
;
_pd_proc_ls_background_function
; manual background (visual estimation, unrefined) interpolated by ten
Legendre polynomials
;
_pd_proc_ls_pref_orient_corr     none
_pd_proc_ls_profile_function
; pseudo-Voigt profile with Thompson-Cox-Hastings approach:
G~U~ = 586(7), G~V~ = -1004.3, G~W~ = 661(7), L~X~ = 6.9(5), L~Y~ = 0,
B\'erar-Baldinozzi asymmetry correction:
A~0~ = 0.434(7), A~1~ = -0.9253
;
_pd_proc_ls_prof_R_factor        0.0249
_pd_proc_ls_prof_wR_expected     0.0278
_pd_proc_ls_prof_wR_factor       0.0321
_pd_spec_mounting                'compacted powder in tantalum can'
_pd_spec_mount_mode              transmission
_pd_spec_orientation             vertical
_pd_spec_shape                   cylinder
_pd_spec_size_axial              55
_pd_spec_size_equat              9.7
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.27
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.15
_refine_ls_matrix_type           fullcycle
_refine_ls_number_constraints    0
_refine_ls_number_parameters     40
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0136
_refine_ls_R_I_factor            0.0196
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Inet
_refine_ls_weighting_details     w=1/[\s^2^(F~o~)+(0.01F~o~)^2^]
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0191
_refine_ls_wR_factor_gt          0.0132
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            cm5b04608_si_003.cif
_cod_data_source_block           lialo2-pow-750C
_cod_depositor_comments
'Adding full bibliography for 4002658--4002660.cif.'
_cod_original_cell_volume        171.376(15)
_cod_original_formula_sum        'Al1 Li1 O2'
_cod_database_code               4002658