Accurate Analysis of NMC Cathodes and Precursors Using Revontium XRF Spectrometer

07 September 2026

Accurate XRF Analysis of NMC Battery Cathodes and Precursors

Lithium nickel manganese cobalt oxide, commonly known as Li-NMC or NMC, is an important cathode material used in lithium-ion batteries for electric vehicles, portable electronics, and energy-storage applications. The concentrations of nickel, manganese, and cobalt influence critical aspects of cathode performance, including energy density, stability, safety, and operating lifetime. Reliable elemental analysis is therefore essential throughout battery-material development and production.

This application note examines how energy-dispersive X-ray fluorescence, or EDXRF, can support quantitative analysis of NMC cathodes and precursor materials. XRF offers a rapid and straightforward alternative to techniques such as inductively coupled plasma analysis. Its combination of precision, accuracy, and limited analytical complexity makes it particularly relevant to routine quality assurance, raw-material qualification, research and development, and process control.

Why Calibration Materials Matter for NMC Analysis

Standardless XRF can provide rapid elemental screening and semi-quantitative results. Accurate production and quality-control measurements, however, require calibration using appropriate reference materials. Battery materials present a practical calibration challenge because suitable standards have historically been limited.

The method described in the application note uses a set of 12 synthetic NMC certified reference materials developed specifically for XRF calibration with fused beads. These CRMs cover nickel, manganese, cobalt, and selected minor elements across concentration ranges relevant to NMC materials. They may also support the analysis of NCA, LCO, LMO, and associated precursor materials.

The reference materials are prepared gravimetrically from high-purity chemicals and provide metrological traceability and compliance with ISO 17034. A fusion recipe and XRF method template are also included. These resources help laboratories establish a controlled and repeatable calibration workflow rather than relying only on standardless estimates.

Fused-Bead Preparation and Revontium EDXRF Measurement

Calibration standards and a validation CRM were prepared as 32-mm fused beads using lithium-borate fusion. The preparation used a 1:10 sample-to-flux ratio and a fusion temperature of 1100 °C. Fusion is recommended when high accuracy and repeatability are required because it can provide homogeneous specimens for XRF measurement. The CRMs can also be used to prepare secondary pressed-pellet standards.

Measurements were performed using a Revontium EDXRF spectrometer equipped with an Ag-anode X-ray tube, primary and secondary filters, four simultaneous high-resolution silicon drift detectors, a spinner, and an automatic sample changer. The measurements were conducted under vacuum with an oil-free dry pump and did not require helium.

Each specimen was measured for 4.5 minutes, corresponding to a throughput of approximately 13 samples per hour. Laboratories can adjust measurement time according to their required precision and analytical scope. Calibration curves were established for NiO, CoO, MnO, and SO₃, linking measured XRF intensities with certified concentrations.

What the Full Application Note Covers

The concentration ranges covered by the NMC certified reference materials
The Revontium EDXRF instrument configuration and measurement conditions
The lithium-borate fused-bead preparation procedure
Calibration results for major and minor components
Same-day repeatability results from ten replicate fused beads
Method stability and precision results collected across three days
Comparison of measured averages with certified concentrations and ISO Guide 35-based allowable differences

The complete method was validated using BAM-S014, a certified Li-NMC 111 cathode material. The evaluation considered both the bead-making process and XRF measurement, providing a practical view of whole-method performance rather than instrument precision alone.

Register for full access to review the complete calibration, precision, and validation data and learn how Revontium EDXRF with NMC-specific CRMs can support efficient routine elemental analysis of battery cathodes and precursors.

Introduction

Lithium nickel manganese cobalt oxide (Li-NMC) cathodes are widely used in lithium-ion batteries for electric vehicles, portable electronics, and energy storage. The concentrations of Ni, Mn, and Co strongly influence cathode performance, including energy density, stability, safety, and lifetime. Accurate elemental analysis is therefore essential for raw-material qualification, process control, R&D, and quality assurance.

XRF provides a rapid and simple alternative to techniques such as ICP, offering high precision and accuracy with minimal analytical complexity. This makes it well suited to routine analysis of cathode and precursor materials. This application note demonstrates quantitative NMC analysis using a Revontium EDXRF spectrometer, NMC-specific certified reference materials (CRMs), and lithium-borate fused-bead preparation.

NMC Certified Reference Materials

Standardless XRF provides rapid elemental screening and semi-quantitative results. For accurate production and quality-control measurements, calibration with appropriate reference materials is required. To address the limited availability of battery-material standards, Malvern Panalytical has developed 12 synthetic NMC CRMs specifically for XRF calibration using fused beads.

[AN260907-image1.png] AN260907-image1.png

Table 1: Minimum and maximum concentrations of NCM CRMs
	Li (wt%)*	Mn (wt%)	Co (wt%)	Ni (wt%)	Al (wt%)	Ca (wt%)	Zr (wt%)	Na (wt%)	S wt(%)
Lowest cal. point **	5.70	3.00	3.00	10.00	0	0	0	0	0
Highest cal. Point	9.00	27.00	27.00	55.00	2.00	0.10	2.00	1.00	0.40

* Lithium or Lithium oxide cannot be measured directly by XRF instruments, but they are added to the composition to simulate battery cathode mixes.

** The lowest calibration point should not be considered as the minimum concentration that can be reported. Instead, the Limit of Quantification (LOQ) is used for this purpose. LOQ depends on sample preparation, XRF instrument, measurement conditions, and measurement time.

The CRMs are prepared gravimetrically from high-purity chemicals, providing metrological traceability and compliance with ISO 17034. The package also includes a fusion recipe and XRF method template.

The CRMs cover Ni, Mn, Co and selected minor elements across the concentration ranges relevant to NMC materials. They can also be used for NCA, LCO, LMO and their precursor materials. Fusion preparation is recommended for high accuracy and repeatability, while the CRMs can also be used to prepare secondary pressed-pellet standards.

Instrumentation and Sample Preparation

Measurements were performed on a Revontium EDXRF spectrometer equipped with a 50 W, 5 mA, 60 kV Ag-anode X-ray tube, primary and secondary filters, four simultaneous high-resolution silicon drift detectors, a spinner, and an automatic sample changer. Measurements were performed under vacuum using an oil-free dry pump, without the need for helium.

Calibration standards and the validation CRM were prepared as 32-mm fused beads via lithium-borate fusion. A sample-to-flux ratio of 1:10 was used, with fusion performed at 1100 °C using an Eagon 2 automatic fusion machine. The complete cold-to-cold cycle required approximately 30 minutes.

Measurement and Calibration

Each specimen was measured for 4.5 minutes, providing a throughput of approximately 13 samples per hour. Measurement time can be adjusted according to the required precision and analytical scope.

Calibration curves for NiO, CoO, MnO, and SO₃ showed excellent correlation between measured XRF intensities and certified concentrations, demonstrating the suitability of the calibration materials and analytical method.

[AN260907-figure1.png] AN260907-figure1.png — Figure 1: Calibration plot of NiO in NCM CRM standards prepared as fused beads.

[AN260907-figure2.png] AN260907-figure2.png — Figure 2: Calibration plot of CoO in NCM CRM standards prepared as fused beads.

[AN260907-figure3.png] AN260907-figure3.png — Figure 3: Calibration plot of MnO in NCM CRM standards prepared as fused beads.

[AN260907-figure4.png] AN260907-figure4.png — Figure 4: Calibration plot of SO₃ in NCM CRM standards prepared as fused beads.

Precision and Validation

The complete method was validated using BAM-S014, a certified Li-NMC 111 cathode material. Ten replicate fused beads measured on the same day showed close agreement with the certified concentrations, as shown in Table 2.

Table 2: Precision and validation results of the whole method including the bead-making process on the same day. The smaller the RMS value, the better the precision.
Sample ID	NiO (wt%)	CoO (wt%)	MnO (wt%)	SO₃ (wt%)
BAM-S014_repeat_bead_01	19.505	19.625	17.974	0.1450
BAM-S014_repeat_bead_02	19.634	19.777	18.079	0.1498
BAM-S014_repeat_bead_03	19.778	19.867	18.175	0.1482
BAM-S014_repeat_bead_04	19.738	19.836	18.145	0.1490
BAM-S014_repeat_bead_05	19.672	19.774	18.104	0.1474
BAM-S014_repeat_bead_06	19.694	19.810	18.117	0.1490
BAM-S014_repeat_bead_07	19.782	19.902	18.185	0.1482
BAM-S014_repeat_bead_08	19.699	19.788	18.103	0.1502
BAM-S014_repeat_bead_09	19.690	19.820	18.122	0.1486
BAM-S014_repeat_bead_10	19.659	19.787	18.116	0.1558
Measured average conc.	19.685	19.799	18.112	0.149
RMS of average conc.	0.079	0.074	0.059	0.003
Certified conc.	19.760	19.800	18.220	0.142
RMS of certified conc.	0.130	0.120	0.140	0.007
RMS between labs	0.210	0.200	0.250	0.012

The method was also evaluated over three days. As shown in Table 3, the measured averages remain close to the certified values, with differences well within the allowable limits calculated according to ISO Guide 35.

Table 3: Precision and validation results of the whole method including bead making process, spread over 3 days. The smaller the RMS value, the better the precision.
Sample ID	NiO (wt%)	CoO (wt%)	MnO (wt%)	SO₃ (wt%)
BAM-S014_day 1_bead 1	19.671	19.773	18.087	0.1422
BAM-S014_day 1_bead 2	19.749	19.873	18.157	0.1438
BAM-S014_day 2_bead 1	19.801	19.921	18.208	0.1454
BAM-S014_day 2_bead 2	19.648	19.783	18.093	0.1426
BAM-S014_day 2_bead 3	19.608	19.732	18.056	0.1494
BAM-S014_day 3_bead 1	19.724	19.857	18.134	0.1438
BAM-S014_day 3_bead 2	19.846	19.966	18.234	0.1490
Measured average conc.	19.721	19.843	18.138	0.145
RMS of average conc.	0.085	0.085	0.066	0.003
Certified conc.	19.760	19.800	18.220	0.142
RMS of certified conc.	0.130	0.120	0.140	0.007
RMS between labs	0.210	0.200	0.250	0.012
Absolute difference	0.039	0.043	0.082	0.003
Allowed difference*	0.155	0.147	0.155	0.007

*Allowed differences between average concentration and certified concentration, calculated according to the ISO Guide 35 requirements.

This demonstrates good repeatability and stability of the complete sample-preparation and measurement procedure.

Conclusion

Revontium EDXRF provides accurate, precise, and repeatable quantitative analysis of NMC cathode and precursor materials prepared as fused beads. The combination of NMC-specific CRMs, reproducible fusion preparation, and rapid XRF measurement provides a robust solution for battery-materials R&D, process control, and quality assurance. With a 4.5-minute measurement time and throughput of approximately 13 samples per hour, Revontium enables efficient routine elemental analysis of NMC materials.