Aluminium electrolytic bath analysis CubiX 3 Potflux The production of aluminium from purified alumina by electrolysis (Hall- Héroult-process) is a very energy-consuming process. The concentration of main components in the electrolyte must be rigidly controlled in order to maintain optimum conditions during the production process. X-ray diffraction (XRD) is the optimal technique for fast and accurate monitoring of the bath parameters and the phase composition. It can be applied on different types of electrolytic baths (addition of Ca, Mg, Li, K). Innovative methods provide true phase concentrations in addition to common bath parameters such as bath ratio (BR), excess AlF 3 (exAlF 3 ), calcium content (CaF 2 ) and free alumina content (α-Al 2 O 3 ). In addition to the monitoring of electrolytic baths, XRD can also be used to inspect incoming goods such as, refined alumina, carbon anodes, cryolites and bauxites. Benefits • Maintain optimal bath conditions by frequent monitoring of bath parameters • Simultaneous analysis of true bath parameters and real phase composition • One method for a wide range of bath ratios • No consumables for sample taking and analysis • Fully automatable (from sample preparation to result reporting) • Fast ROI due to multiple applications (raw materials, alumina, electrolytic baths, carbon anodes) • Effective use of energy
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Aluminium electrolytic bath analysis
CubiX3 Potflux
The production of aluminium from purified alumina by electrolysis (Hall-
Héroult-process) is a very energy-consuming process. The concentration
of main components in the electrolyte must be rigidly controlled in
order to maintain optimum conditions during the production process.
Modern Rietveld analysis of electrolytic bathsThe powerful and fast full pattern Rietveld method is the state-of-art technique for the determination of the phase composition and the relevant bath parameters (e.g. bath ratio, excess AlF3, CaF2, MgF2, α-Al2O3, etc.) in electrolytic bath samples. Typical measurement times are ca. 1-2 minutes. No standards, intensity monitors and recalibrations are required. Different Ca-cryolite phases in standard electrolytic baths samples can easily be quantified using the Rietveld method which is not possible with traditional calibration line based analysis.
Traditional calibration line based bath analysisCalibration based analysis of aluminium baths can be done with a linear detector such as the X’Celerator or with a point detector. For the simultaneous monitoring of the total calcium content (CaF2) the CubiX3 Potflux diffractometer features a high intensity XRF channel. Benefits are very short measurement times that allow frequently bath monitoring.
6.0
Co
nce
ntr
atio
n
Intensity [kcps]
CaF25.5
5.0
4.5
4.0
3.5
3.0
2.5
2.0
60 80 100 120 140 160 180
Calibration curve for fluorite
Global and near PANalytical B.V.Lelyweg 1, 7602 EA AlmeloP.O. Box 13, 7600 AA AlmeloThe NetherlandsT +31 (0) 546 534 444F +31 (0) 546 534 598 [email protected]
Analysis of carbon anodesCubiX3 Potflux can also be used to monitor the quality of the carbon anodes. The efficiency and lifetime of an anode is mainly controlled by the average crystallite size (Lc) of the graphite platelets. XRD allows the analysis of the crystallite size and respectively the efficiency of the anodes.The ASTM standard test method (ASTM D5187) is included in PANalytical’s solution for electrolytic bath analysis.
Example of the analysis of the crystallite size Lc of a graphite anodeReferencesScarlett, N.V.Y. & Madsen, I.C. (2006) Quantification of phases with partial or no known crystal structure. Powder Diffraction, 21(4), 278-284
Rietveld analysis of a standard electrolytic bath showing phase concentrations, including two different Ca-Cryolite phases from a minute scan