3212 XXXI International Mineral Processing Congress 2024 Proceedings/Washington, DC/Sep 29–Oct 3
SAMPLE CHARACATERIZATION
Three black mass (BM) samples were received from two
commercial lithium-ion battery (LIB) recyclers. Each
sample was oven dried at 80°C overnight, homogenized,
and riffled into either 150g, 200g, or 250g charges. Sub-
samples were collected and submitted for chemical analy-
sis, particle size analysis, thermal gravimetric analysis, and
scanning electron microscopy.
Chemical Analysis
Each BM sample was analyzed for total carbon using
Elementar vario EL Cube and Co, Li, Mn, and Ni using
an Agilent 5900 inductive coupled plasma optical emis-
sion spectrometer (ICP-OES). Results are presented in
Table 1. The total carbon found in Sample A (37.1%) and
C (36.5%) were similar but differed significantly to Sample
B (24.8%). It should be noted that the total carbon mea-
sured will includes not only the graphite present but any
other carbon species in the sample such as the binder but
should be insignificant. The four combined major cathodic
metals, Co, Li, Mn, and Ni also varied significantly with the
lowest found in Sample B (26.9%) and highest in Sample
C (38.2%). The highest Ni, Co, and Mn content were
found in Sample A (15.3% Ni), Sample B (10.1% Co),
and Sample C (18.5% Mn), respectively. Typical NMC or
NCA chemistries were not found an indication that vari-
ous battery chemistry or type were processed.
Particle Size Analysis
Particle size analysis was conducted on the as-received
Sample A and B using a Horiba LA905v2 laser scatter-
ing size analyzer. Samples were measured in water using a
refractive index value of 1.97. Sample A was found to be
80% passing 45µm but particles as large as 390µm were
found. In Sample B, the particle distribution curve shifted
to the right with 80% passing 175µm. Graphite used in
LIB is fine as typical spheridized graphite is ~10–40µm.
The coarse particles are likely poorly liberated particles or
agglomerated from the mechanical separation process. The
overly coarse or fine particles present a challenge as they
are beyond the typical range of 100–200µm for flotation
which may hinder flotation kinetics, recovery, or selectivity.
Thermogravimetric Analysis Coupled with Fourier-
Transform Infrared Spectroscopy (TGA-FTIR)
The thermogravimetric analyzer used was a TA Instruments
model Q5000 IR while the FTIR spectrometer was a
Nicolet 6700 equipped with a TGA accessory. In conven-
tional TGA, approximately 50 mg of black mass in a plati-
num pan was inserted in the furnace at room temperature
Table 1. Elemental analysis—head sample
Element Sample A Sample B Sample C
C (Total), %37.1 24.8 36.5
Co, %6.52 10.1 5.94
Li, %3.33 2.74 3.19
Mn, %7.06 2.91 18.5
Ni, %15.3 11.1 10.6
Total Co+Li+Mn+Ni, %32.2 26.9 38.2
0
10
20
30
40
50
60
70
80
90
100
0
2
4
6
8
10
12
Diameter, μm
Sample A Sample B Sample A Sample B
Figure 1. Particle size analysis of as-received black mass (Sample A and Sample B)
0.051 0.076 0.115 0.172 0.259 0.389 0.584 0.877 1.318 1.981 2.976 4.472 6.72 10.097 15.172 22.797 34.255 51.471 77.34 116.21 174.616 262.376 394.244 592.387 890.116 1337.481
Cumulative
Passing
(%)
Fraction
(%)
SAMPLE CHARACATERIZATION
Three black mass (BM) samples were received from two
commercial lithium-ion battery (LIB) recyclers. Each
sample was oven dried at 80°C overnight, homogenized,
and riffled into either 150g, 200g, or 250g charges. Sub-
samples were collected and submitted for chemical analy-
sis, particle size analysis, thermal gravimetric analysis, and
scanning electron microscopy.
Chemical Analysis
Each BM sample was analyzed for total carbon using
Elementar vario EL Cube and Co, Li, Mn, and Ni using
an Agilent 5900 inductive coupled plasma optical emis-
sion spectrometer (ICP-OES). Results are presented in
Table 1. The total carbon found in Sample A (37.1%) and
C (36.5%) were similar but differed significantly to Sample
B (24.8%). It should be noted that the total carbon mea-
sured will includes not only the graphite present but any
other carbon species in the sample such as the binder but
should be insignificant. The four combined major cathodic
metals, Co, Li, Mn, and Ni also varied significantly with the
lowest found in Sample B (26.9%) and highest in Sample
C (38.2%). The highest Ni, Co, and Mn content were
found in Sample A (15.3% Ni), Sample B (10.1% Co),
and Sample C (18.5% Mn), respectively. Typical NMC or
NCA chemistries were not found an indication that vari-
ous battery chemistry or type were processed.
Particle Size Analysis
Particle size analysis was conducted on the as-received
Sample A and B using a Horiba LA905v2 laser scatter-
ing size analyzer. Samples were measured in water using a
refractive index value of 1.97. Sample A was found to be
80% passing 45µm but particles as large as 390µm were
found. In Sample B, the particle distribution curve shifted
to the right with 80% passing 175µm. Graphite used in
LIB is fine as typical spheridized graphite is ~10–40µm.
The coarse particles are likely poorly liberated particles or
agglomerated from the mechanical separation process. The
overly coarse or fine particles present a challenge as they
are beyond the typical range of 100–200µm for flotation
which may hinder flotation kinetics, recovery, or selectivity.
Thermogravimetric Analysis Coupled with Fourier-
Transform Infrared Spectroscopy (TGA-FTIR)
The thermogravimetric analyzer used was a TA Instruments
model Q5000 IR while the FTIR spectrometer was a
Nicolet 6700 equipped with a TGA accessory. In conven-
tional TGA, approximately 50 mg of black mass in a plati-
num pan was inserted in the furnace at room temperature
Table 1. Elemental analysis—head sample
Element Sample A Sample B Sample C
C (Total), %37.1 24.8 36.5
Co, %6.52 10.1 5.94
Li, %3.33 2.74 3.19
Mn, %7.06 2.91 18.5
Ni, %15.3 11.1 10.6
Total Co+Li+Mn+Ni, %32.2 26.9 38.2
0
10
20
30
40
50
60
70
80
90
100
0
2
4
6
8
10
12
Diameter, μm
Sample A Sample B Sample A Sample B
Figure 1. Particle size analysis of as-received black mass (Sample A and Sample B)
0.051 0.076 0.115 0.172 0.259 0.389 0.584 0.877 1.318 1.981 2.976 4.472 6.72 10.097 15.172 22.797 34.255 51.471 77.34 116.21 174.616 262.376 394.244 592.387 890.116 1337.481
Cumulative
Passing
(%)
Fraction
(%)