Evaluation of NCM layered structure; analysis of Li/Ni mixing; detection of trace impurity phases in lithium iron phosphate feedstock; in-situ battery cycling.
X-ray diffraction was used to identify the phase and analyze the crystal structure of lithium nickel cobalt manganese oxide cathode material, and the degree of Li/Ni cation mixing in the sample was evaluated by Rietveld structure refinement.
Instrument Name: Ariston N8 DiffraX Diffractometer
● Optical system: DiffraX Vertex One™
● Test mode: High energy resolution mode
● X-ray source: Cu-Kα
● Scan range: 10°–140°（2θ）
● Step size:0.02°
● Time per step: 0.5 s
Phase analysis results indicate that the main phase of the sample is:
● Phase name: Lithium nickel cobalt manganese oxide
● Chemical formula: LiMn₀.₄Co₀.₂Ni₀.₄O₂
● Crystal system: Hexagonal crystal system
● Space Group: R-3m（No. 166）
● Unit cell parameters: a = 2.87045 Å，c = 14.25071 Å
The measured diffraction peaks matched well with the standard structure data, and no obvious independent impurity phase peaks were observed, indicating that the sample phase purity was high and the layered crystal structure remained intact.
The Rietveld structural finishing results show that:
● The occupancy of Li at site 3a in the lithium layer is 0.962;
● The occupancy of Ni at site 3a in the lithium layer is 0.038.
● The occupancy rate of Li at the 3b site of the transition metal layer is 0.037.
Therefore, the proportion of Ni occupying Li sites in the sample is approximately 3.8%, which means the Li/Ni cation mixing rate is approximately 3.8%.
The results indicate that the sample exhibits good overall layered cation ordering, but still contains a small number of Li/Ni antisite defects. Ni entering the lithium layer may occupy some lithium-ion diffusion channels, potentially affecting the material's rate performance and cycle stability.
The main phase of the sample is a layered LiMn₀.₄Co₀.₂Ni₀.₄O₂ in space group R-3m, with good crystallinity and no obvious impurity phases detected. Structural refinement yielded a Li/Ni mixing ratio of approximately 3.8%, indicating a relatively intact layered structure and good cation order.
The ÅdoNano N8 DiffraX diffractometer can simultaneously perform phase identification, crystal structure analysis, and quantitative analysis of Li/Ni mixing in ternary cathode materials, providing reliable data support for material development, process optimization, and quality control.
Lithium iron phosphate is an important cathode material for power batteries and energy storage batteries. Its phase composition and impurity phase content directly affect the material performance and batch consistency. Therefore, it is necessary to accurately analyze the purity of the main phase and trace impurity phases using X-ray diffraction.
Instrument Name: Ariston N8 DiffraX Diffractometer
● Optical system: DiffraX Vertex One™
● Test mode: High energy resolution mode
● X-ray source: Cu-Kα
● Scan range: 10°–90°（2θ）
● Step size: 0.02°
● Time per step: 0.8 s
● Data processing method: Rietveld full-spectrum refined quantitative analysis
Based on the XRD patterns and Rietveld refinement results, the main phase composition of the sample is as follows:
Phase of matter | Content |
LiFePO₄ (lithium iron phosphate) | 94.2% |
Li₃PO₄ (Lithium phosphate) | 3.2% |
FeP (Iron Phosphate) | 1.3% |
LiPO₃ (Lithium metaphosphate) | 1.1% |
Fe (metallic iron) | 0.2% |
The sample was dominated by lithium iron phosphate, with a content of 94.2%. Small amounts of lithium phosphate, iron phosphide, lithium metaphosphate, and metallic iron were also detected, indicating that the overall reaction degree of the sample was high. However, there is still room for further optimization in terms of raw material ratio, sintering atmosphere, and reaction uniformity.
Lithium iron phosphate (LFP) samples exhibit high fluorescence background, requiring instruments with strong background suppression and weak peak recognition capabilities. In this test, the N8 DiffraX demonstrated the following characteristics:
● The peak-to-back ratio reaches over 110 times;
● High signal-to-noise ratio, clear weak peaks;
● It can effectively identify low-content impurity phases;
● Even 0.2% metallic iron can still be detected and quantified;
● The measured spectrum and the refined spectrum are in good agreement, which meets the analysis requirements of complex multiphase systems.
The N8 DiffraX diffractometer from Aidu Nano obtained high-quality diffraction data in the testing of high-fluorescence lithium iron phosphate raw materials and achieved reliable quantitative analysis of the main phase and low-content impurity phases.
Test results show that the sample contains 94.2% lithium iron phosphate, along with trace amounts of Li₃PO₄, FeP, LiPO₃, and Fe. The instrument's excellent peak-to-background ratio, signal-to-noise ratio, and trace phase detection capabilities provide reliable data support for lithium iron phosphate material research and development, production process optimization, and quality control.
A multi-functional desktop X-ray diffraction solution, offering performance and functionality comparable to traditional large-scale diffractometers...
The N3 PhniX Plus diffractometer system, employing an external sample introduction system, boasts strong automation compatibility and ensures stability and consistency...
An X-ray diffraction platform designed for the characterization of advanced materials and complex samples, equipped with different innovative optical systems...
