accurate mineralogical analysis for efficient lithium ore ......• measurement time per sample 8...

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Accurate mineralogical analysis for lithium ore processingAnalyse minéralogique pour le traitement du minerai de lithiumMarie-Ève Provencher & Dr. Uwe König


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October 21, 20202 Title of the presentation

TopicsMineralogical monitoring of lithium ores

Conclusions

Case study - Brines

Case study - Pegmatites

What is X-ray diffraction (XRD)

Lithium deposits and processing

Motivation & value


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Motivation & value


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Motivation and value

• Increased demand for lithium

• Efficiency of lithium ore processing depends on mineralogical properties (not only on chemistry)

• Increased complexity of mineralogy of new and existing deposits• Exact knowledge of ore domains needed for efficient ore sorting

and blending • Recovery rates and profitability of downstream processing requires

exact knowledge of mineralogical composition • Efficient use of reagents • Minimum downtime • …

Mineralogical monitoring of lithium ores


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Increased demand for lithium

October 21, 2020Title of the presentation5

How much lithium is in everyday item ?

Source: www.visiualcapitalist.com


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Increased demand for lithium


Forecast consumption


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Lithum deposits


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Lithium deposits


Overview

Sykes ‐MinExConsulting, 2019


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Lithium deposits


Brines versus pegmatites

• Formed by leaching of volcanic rocks in basin depositional environments

• Large low-grade deposits• Extraction of Li involving the pumping of brine,

concentration via evaporation, and purification through solvent extraction, end product mainly Li2CO3

• Lithium-bearing, aluminium silicate mineral which mostly occurs in lithium-rich pegmatites (granite-like igneous rock composed of quartz, feldspar and mica).

• Complex high-grade deposits • Spodumene usually recovered through open pit mining• Beneficiated via gravity techniques where the ore is

concentrated from 1-2% Li2O to a grade of ~6% Li2O


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Lithium deposits


Brines versus pegmatites


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Lithium deposits


Costs


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X-ray diffraction (XRD)


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Analytical techniques

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Elements and minerals

Wet chemistryWet chemistry

Neutron analysisNeutron analysis

XRFXRF

ElementsFe SiO2 Al2O3 MgO CaO S

1 26.5 22.2 0.4 17.9 2.1 4.02 57.9 6.1 0.8 3.9 1.9 4.93 34.5 23.1 2.0 12.5 4.4 2.1

Process parametersElectron microprobe

MLA, QEMSCAN0%

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Pyr

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Qua

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Alb

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Liz

XRD

MineralsNIR

Microscopy


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XRD in Geoscience

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Usage

Main fields of applications:

181803/06/2015Webinar: Modern XRD in Geosciences


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XRD in Geoscience

10/21/2020Solutions for automotive

What can we learn from XRD pattern?

width

Peak position

Phase composition

Amorphous content

Crystallite size/microstrain

Structural information

Process parameters


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X-ray diffraction

21 October 2020Title of the presentation20

How does it work ?

• Identification and quantification of crystalline phases and amorphous content • Monitoring of process parameters


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X-ray diffraction


Data evaluation

Position [°2Theta] (Copper (Cu))10 20 30 40 50 60

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40000 Barite 22.9 %Hematite, syn 21.8 %Quartz 5.9 %Goethite 29.7 %fluorapatite, syn 5.3 %Synchysite-(Ce) 2.7 %Duplicated_Barite 11.6 %

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Case study:Pegmatites


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Process


Pegmatite ores

Keliber BatterySupply Chain Europe /Düsseldorf, March13, 2018


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Process

Samples case study


Pegmatite ores

Keliber BatterySupply Chain Europe /Düsseldorf, March13, 2018


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Mineralogical monitoring…

• Samples from several parts during mining and processing of lithium ores were analyzed

• Lithium ore (raw material)• Concentrate (α – Spodumene)• Flotation tailings• Calcination product (β – Spodumene) • Residue (Analcime)

• Sample preparation• Automatic mill / press combination to ensure minimum sample preparation errors

• Measurement time per sample 8 min (Aeris Minerals, benchtop XRD)


Exploration, mine planning, process monitoring


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Cluster analysis

• Prior to phase identification and quantification a cluster analysis was performed using all available ore samples

• 2 cluster (groups of similar samples) are identified

• 2 outliers (not belonging to any cluster)

• fast check for different ore domains for greenfield or brownfield exploration


Lithium ores

High grade

Low grade


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Lithium containing minerals

• Spodumene theoretically contains 8.03% Li2OOctober 21, 2020Title of the presentation28

Pegmatites


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Lithium containing minerals

• Spodumene theoretically contains 8.03% Li2OOctober 21, 2020Title of the presentation29

Pegmatites


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Mineralogy

• Complex mineralogy

• 8 main and minor minerals identified in the lithium ores

• Additional mineral phases identifies in the processed ore

• XRD can distinguish between α- and β-spodumene !!!


Phase identification pegmatites

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Residue + Peak List

Accepted Patterns


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Mineralogy


Phase identification

Mineral FormulaSpodumene LiAl(SiO3)2Quartz SiO2Albite NaAlSi3O8Anorthite CaAl2Si2O8Lepidolite K(Li,Al) 3(Al,Si,Rb)4O10(F,OH) 2Orthoclase KAlSi3O8Tourmaline (Elbaite) Na(Li1.5Al1.5)Al6Si6O18 (BO3) 3(OH)4 Beryl Be3Al2(SiO3)6

• Complex mineralogy

• 8 main and minor minerals identified in the lithium ores

• Additional mineral phases identifies in the processed ore

• XRD can distinguish between α- and β-spodumene !!!


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Mineralogy (quantification)


Lithium ores

Position [°2θ] (Copper (Cu))10 20 30 40 50 60 70 80

Counts

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Spodumene-alpha 26.5 %Spodumene-beta 0.0 %Quartz 23.2 %Albite 40.4 %Anorthite 6.7 %Orthoclase 0.4 %Lepidolite 2.0 %Beryl 0.7 %Elbaite 0.0 %Analcime 0.0 %

Rwp = 10.126902000-20004000

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Spodumene‐alpha [%] Spodumene‐beta [%] Quartz [%]

Albite [%] Anorthite [%] Orthoclase [%]

Lepidolite [%] Beryl [%] Elbaite [%]

Measurement time 8 min

Example of a full-pattern Rietveld quantification of a hard-rock lithium ore


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Position [°2θ] (Copper (Cu))10 20 30 40 50 60 70 80

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40000Spodumene-alpha 89.6 %Spodumene-beta 0.4 %Quartz 1.3 %Albite 1.4 %Anorthite 3.7 %Orthoclase 0.6 %Lepidolite 0.8 %Beryl 0.3 %Elbaite 0.6 %Analcime 1.5 %

Rwp = 9.4128

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Processed lithium ore

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Analcime [%]

Example of a full-pattern Rietveld quantification of a spodumene concentrate


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Results


Mineralogical monitoring pegmatite processing

Clustering


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Results



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Mineral composition Clustering


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Results



Low grade

Waste

Low grade

Low grade

High grade

Grade blocks

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Mineral composition Clustering


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Case study:Brines


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ProcessBrines

Haber, LSM Conference, Las Vegas, 26-28thJanuary 2010


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Cluster analysis


Brine samples

Lithium salts

Halite >> Sylvine

Carnaliite

Bischofite

Halite > Sylvine

Gypsum

Sylvine >> Halite


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22 24 26 28 30 32 342Theta (°)

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Inte

nsity

(cou

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Bis

BisBis

Bis

Bis

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LiCar Li

CarLiCar

LiCar

LiCar

LiSul

Mineralogy


Phase identification brines

Mineral FormulaHalite NaClSylvine KClCarnallite KMgCl3 ꞏ 6H2OBischofite MgCl2 ꞏ 6H2O

Anhydrite CaSO4Gypsum CaSO4 ꞏ 2H2O Kainite KMg(Cl,SO4) ꞏ 2.75H2O

Li-sulfate monohydrate

Li2SO4 ꞏ H2O

Li-Carnallite LiMgCl3 ꞏ 7H2O


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Lithium brines

Position [°2Theta] (Copper (Cu))20 30 40 50 60

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11C-C1 HXHalite 27.3 %Sylvine 11.0 %Carnallite, syn 45.8 %Chloromagnesite 0.5 %Anhydrite 1.6 %Picromerite, syn 1.0 %Polyhalite 10.1 %Lithium Sulfate Monohydrate 1.1 %Lithium Chloride Magnesium Dichloride Heptahydrate 1.6 %


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Conclusions


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Conclusions

• Fast tool to monitoring qualitative and quantitative mineral composition of lithium ore

• Fast detection of impurities or off-spec ore mineralogy

• BT XRD in laboratories or containers or an automated environment


Mineralogical monitoring of lithium ores and brines

Fast decision making and counteractions on changing conditions, reduced operational costs

Additional information for mine planning and downstream processing

Higher degree of process automation with less manual testing, improved safety, lowest energy costs


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www.malvernpanalytical.com

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Dr. Uwe Kö[email protected]

Marie-Ève [email protected]

Questions ?

accurate mineralogical analysis for efficient lithium ore ......• measurement time per sample 8...

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