GB/T 39861-2021 PDF English
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Electrochemical Performance Test of Lithium Manganese Oxide - Test Method for Discharge Plateau Capacity Ratio and Cycle Life
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GB/T 39861-2021: Electrochemical Performance Test of Lithium Manganese Oxide - Test Method for Discharge Plateau Capacity Ratio and Cycle Life
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GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.160
CCS H 21
Electrochemical Performance Test of Lithium
Manganese Oxide - Test Method for Discharge Plateau
Capacity Ratio and Cycle Life
ISSUED ON: MARCH 9, 2021
IMPLEMENTED ON: OCTOBER 1, 2021
Issued by: State Administration for Market Regulation;
Standardization Administration of the People’s Republic of
China.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative References ... 4
3 Terms and Definitions ... 4
4 Test Conditions ... 4
5 Reagents or Materials ... 5
6 Instruments and Equipment ... 6
7 Test Procedures ... 7
8 Test Data Processing ... 15
9 Test Report ... 16
Electrochemical Performance Test of Lithium
Manganese Oxide - Test Method for Discharge Plateau
Capacity Ratio and Cycle Life
1 Scope
This Standard specifies the test method for discharge plateau capacity ratio and cycle
life of lithium manganese oxide as the cathode material of lithium ion batteries.
This Standard is applicable to the test of discharge plateau capacity ratio and cycle life
of lithium manganese oxide as the cathode material of lithium ion batteries.
2 Normative References
The content in the following document constitutes indispensable clauses of this
document through normative references in the text. In terms of references with a
specified date, only versions with a specified date are applicable to this document. In
terms of references without a specified date, the latest version (including all the
modifications) is applicable to this document.
GB/T 18287 General Specification of Lithium-ion Cells and Batteries for Mobile Phone
3 Terms and Definitions
The following terms and definitions are applicable to this document.
3.1 Solid Content
Solid content refers to the mass fraction (of the total amount) of the remaining part of
emulsion or paint after drying under the specified conditions.
4 Test Conditions
When there are no special instructions, the various test procedures specified in this
document should be carried out in a drying room (the environmental dew-point
temperature is ≤ -20 °C). For the situation where there is no drying room, the various
test procedures shall be carried out under the following environmental conditions: the
relative humidity is ≤ 20.0% and the temperature is 20 °C ~ 30 °C.
160 μm; the thickness of the aluminum foil coated on the surface of the aluminum-
plastic film is: 30 μm ~ 40 μm.
5.17 Insulating glue: with a length of 53.0 mm ± 1.0 mm.
5.18 Nitrogen: purity (volume fraction) ≥ 99.9%.
5.19 Electrolyte for lithium ion batteries: composed of a solution (with a concentration
of 1 mol/L) of lithium hexafluorophosphate (LiPF6) dissolved in an organic solvent (the
volume ratio of ethylene carbonate EC, dimethyl carbonate DMC, ethyl methyl
carbonate EMC is 1 : 1 : 1); moisture content ≤ 0.0015%; free acid (HF) ≤ 0.003%;
density: 1.23 g/cm3 ± 0.02 g/cm3; chroma ≤ 50 Hazen.
6 Instruments and Equipment
6.1 Electronic balance: with a measuring range of 3,000 g and a division value of 0.01
g.
6.2 Electronic balance: with a measuring range of 100 g and a division value of 0.0001
g.
6.3 Drying oven.
6.4 Desiccator.
6.5 Sanding machine.
6.6 Planetary stirrer.
6.7 Coating machine: the length of drying tunnel is > 2.0 m.
6.8 Vacuum oven.
6.9 Cutting machine.
6.10 Banister brush.
6.11 Adjustable slitting machine.
6.12 Sheet-punching machine: the mold is a square with a side length of 10 cm or a
circle with a diameter of 10 cm.
6.13 Desktop digital thickness gauge: with a resolution of 1 μm.
6.14 Roller machine: exclusive to lithium batteries.
6.15 Ruler: stainless-steel; with a measuring range of 100 cm, accurate to 0.5 mm.
Add the weighed NMP (5.4) into the stirring tank in the sanding machine (6.5);
gradually add the weighed polyvinylidene fluoride (5.3) and perform dispersive stirring,
until it is completely dissolved. Afterwards, add the weighed conductive agent (5.2) and
perform dispersive stirring. After the dispersion is uniform, add the weighed lithium
manganese oxide (5.1) and perform dispersive stirring, until the dispersion is uniform.
7.2.3 Coating
Use the coating machine (6.7) to evenly coat the stirred cathode paste on both sides
of the aluminum foil (5.5). The coating speed parameter of the coating machine (6.7)
is set to 800 mm/min; the blast baking temperature is set to 130 °C. Control the single
surface areal density within the range of 200 g/m2 ~ 230 g/m2, the thickness difference
≤ 3 μm and the areal density deviation of the front and back surfaces < 5.0 g/m2. After
the coating is completed, transfer the preliminarily dried and winded cathode sheet to
the vacuum oven (6.8) for secondary drying. The baking temperature is controlled at
110 °C ~ 120 °C; bake for 12 h; cool down under nitrogen (5.18) atmosphere.
7.2.4 Preparation
Take the cathode sheet in 7.2.3, which is dried and reaches the requirements of being
processed; use the sheet-punching machine (6.12) to punch out a circular or square
cathode sheet with an area of Sc. Use the electronic balance (6.2) and the desktop
digital thickness gauge (6.13) to perform mass measurement mc and thickness
measurement dc on the punched cathode sheet.
Use the sheet-punching machine (6.12) to punch out an aluminum foil substrate with
an area of Sc. Use the electronic balance (6.2) and the desktop digital thickness gauge
(6.13) to perform mass measurement mAl and thickness measurement dAl on the
punched aluminum foil substrate.
The compaction density c of the cathode sheet shall be calculated in accordance with
Formula (1):
Where,
c---the compaction density of the cathode sheet, expressed in (g/cm3);
mc---the mass of the cathode sheet, expressed in (g);
mAl---the mass of the aluminum foil substrate, expressed in (g);
Sc---the area of the cathode sheet, expressed in (cm2);
dc---the thickness of the cathode sheet, expressed in (μm);
graphite anode (5.9), conductive agent (5.2), sodium carboxymethyl cellulose (5.10)
and styrene butadiene rubber emulsion (5.11); use the electronic balance (6.1) for
weighing. In accordance with the solid content of 50.0% ~ 60.0%, calculate deionized
water (5.12); use the electronic balance (6.1) for weighing.
7.3.2 Pulping
Add the weighed deionized water (5.12) into the stirring tank in the planetary stirrer
(6.6); gradually add the weighed sodium carboxymethyl cellulose (5.10) and perform
dispersive stirring for over 2 h, until it is uniform. Add the weighed conductive agent
(5.2) and perform dispersive stirring, until the dispersion is uniform. Add the weighed
artificial graphite anode (5.9) and perform dispersive stirring. Finally, add the weighed
styrene butadiene rubber emulsion (5.11) and perform dispersive stirring, until the
dispersion is uniform.
7.3.3 Coating
In accordance with the areal capacity of the anode sheet: when the areal capacity of
the cathode sheet is ≥ 1.1, calculate the single surface areal density of the anode sheet;
control the areal density deviation of the front and back surfaces < 5.0 g/cm2.
Use the coating machine (6.7) to evenly coat the 7.3.2 stirred anode paste on both
sides of the copper foil (5.13). The coating speed parameter of the coating machine
(6.7) is set to 800 mm/min; the blast baking temperature is set to 90 °C.
After the coating is completed, transfer the preliminarily dried and winded anode sheet
to the vacuum oven (6.8) for secondary drying. The baking temperature is controlled
at 100 °C ~ 110 °C; bake for 12 h; cool down under nitrogen (5.18) atmosphere.
7.3.4 Preparation
Take the anode sheet in 7.3.3, which is dried and reaches the requirements of being
processed; use the sheet-punching machine (6.12) to punch out a circular or square
anode sheet with an area of Sa. Use the electronic balance (6.2) and the desktop digital
thickness gauge (6.13) to perform mass measurement ma and thickness measurement
da on the punched anode sheet.
Use the sheet-punching machine (6.12) to punch out a copper foil substrate with an
area of Sa. Use the electronic balance (6.2) and the desktop digital thickness gauge
(6.13) to perform mass measurement mCu and thickness measurement dCu on the
punched copper foil substrate.
The compaction density a of the anode sheet shall be calculated in accordance with
Formula (2):
c) Take the cathode sheet in 7.2.4 and place it on the above-mentioned half-
folded separator; align the cathode sheet, the separator and the anode sheet
in the center; make the active substance coverage area of the cathode sheet
completely aligned with the active substance coverage area of the anode
sheet, and then, perform winding;
d) Take out the winding core, which is winded in a certain shape, from the
winding needle. Use the insulating glue (5.17) to paste the tail of the winding
core and the battery body together;
e) Place the winding core flatwise on the battery flat press (6.17) to press and
level it;
f) Number and record the leveled winding cores one by one; place them in the
vacuum oven (6.8); set the oven temperature to 80 °C; vacuumize and dry for
24 h. During the baking process, in every 4 h, vacuumize and supplement
nitrogen once;
g) Use the aluminum-plastic film heat sealing machine (6.18) to seal the pack
the winding core in the aluminum-plastic film (5.16), with an air bag and liquid
injection tube (6.21) on one side;
h) Place the plastic-sealed battery in the drying oven (6.3) and bake it for 10 h.
Set the oven temperature to 80 °C. After baking, transfer it to the inert
atmosphere (argon) glove box (6.20). At the air bag of the battery, use the
liquid injector (6.22) to inject the electrolyte for lithium ion batteries (5.19) into
the liquid injection tube (6.21); use the insulating glue (5.17) to seal it;
i) Place the test battery (with the air bag facing upwards) with the injected
electrolyte for lithium ion batteries (5.19) aside for 24 h ~ 36 h.
7.6 Battery Formation
Take the test battery, which is placed aside in 7.5; place it in insulating splints; use an
appropriate mode to fix it. Afterwards, place the test battery with the insulating splints
into the thermostat (6.23). Set the thermostat temperature to 45 °C ± 1 °C; preserve
the heat for 2 h ~ 3 h.
Use the lithium-ion battery electrochemical performance testing machine (6.24) for
charging and discharging. The charging and discharging system is as follows:
a) Charging cut-off voltage: 4.20 V;
b) Discharging cut-off voltage: 3.00 V;
In the first cycle, charge in accordance with the requirements: 0.02 C for 4 h, 0.05 C
for 4 h, 0.1 C for 2 h, and 0.2 C, until it reaches the cut-off voltage; perform constant-
voltage in the nth cycle is recorded as Qn.
8 Test Data Processing
8.1 Calculation of Discharge Plateau Capacity Ratio
The discharge plateau capacity ratio in the nth cycle of lithium manganese oxide is
calculated in accordance with Formula (4):
Where,
Pn---the discharge plateau capacity ratio in the nth cycle;
Qn.U---the discharge capacity when discharged to the voltage U (3.60 V) requested by
the test in the nth cycle, expressed in (mA h);
Qn---the discharge capacity when discharged to the cut-off voltage in the nth cycle,
expressed in (mA h).
The calculation result shall retain one decimal place.
8.2 Calculation of Cycle Life
The ratio of the discharge capacity of lithium manganese oxide in the nth cycle to the
discharge capacity in the first cycle is calculated in accordance with Formula (5):
Where,
n---the ratio of the discharge capacity in the nth cycle to the discharge capacity in the
first cycle;
Qn---the discharge capacity in the nth cycle, expressed in (mA h);
Q1---the discharge capacity in the first cycle, expressed in (mA h).
The cycle life of lithium manganese oxide shall be determined in accordance with the
following method: when n ≥ 80%, n+1 < 80%, the number of cycles (n) is the cycle life
of the test sample.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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