GB/T 30836-2014 PDF English
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Lithium titanium oxide and its carbon composite anode materials for lithium ion battery
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GB/T 30836-2014: PDF in English (GBT 30836-2014) GB/T 30836-2014
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 29.050
Q 53
Lithium titanium oxide and its carbon composite anode
materials for lithium ion battery
ISSUED ON: JUNE 24, 2014
IMPLEMENTED ON: APRIL 01, 2015
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine;
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 ... 5
4 Classification and code ... 5
5 Technical requirements ... 6
6 Test methods ... 7
7 Inspection rules ... 10
8 Packaging, marking ... 12
9 Storage and transportation ... 12
Appendix A (Normative) Determination method of lithium content ... 14
Appendix B (Normative) Determination method of material crystal structure and
residual TiO2 ... 18
Lithium titanium oxide and its carbon composite anode
materials for lithium ion battery
1 Scope
This Standard specifies the terms and definitions, classification and code, technical
requirements, test methods, inspection rules, as well as packaging, marking, storage and
transportation of lithium titanium oxide and its carbon composite anode materials for
lithium ion battery.
This Standard applies to lithium titanium oxide and its carbon composite anode
materials for lithium ion battery (hereinafter referred to as lithium titanate oxide anode
materials). Lithium titanate oxide for electrochemical capacitors can also be used with
reference to this Standard.
2 Normative references
The following referenced documents are indispensable for the application of this
document. For dated references, only the edition cited applies. For undated references,
the latest edition of the referenced document (including any amendments) applies.
GB/T 191, Packaging - Pictorial marking for handling of goods
GB/T 5162, Metallic powders - Determination of tap density
GB/T 6283, Chemical products - Determination of water - Karl Fischer method
(general method)
GB/T 6388, Transport package shipping mark
GB/T 6682, Water for analytical laboratory use - Specification and test methods
GB/T 9724, Chemical reagent - General rule for the determination of pH
GB/T 13732, General rules for sampling inspection of bulk materials with uniform
size
GB/T 19077.1, Particle size analysis - Laser diffraction methods - Part 1: General
principles
GB/T 19587, Determination of the specific surface area of solids by gas adsorption
using the BET method
GB/T 20123, Steel and iron - Determination of total carbon and sulfur content
Infrared absorption method after combustion in an induction furnace (routine
method)
GB/T 24533-2009, Graphite negative electrode materials for lithium ion battery
DZ/T 0064.49, Methods for analysis of groundwater quality - Part 49: Determination
of carbonate, bicarbonate ions, hydroxy - Titrimetric method
JCPDS (00-049-0207), Lithium titanate X-ray powder diffraction standard pattern
IEC 62321, Electrotechnical products - Determination of levels of six regulated
substances (lead, mercury, cadmium, hexavalent chromium, polybrominated
biphenyls, polybrominated diphenyl ethers)
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
lithium titanium oxide and its carbon composite anode materials
Lithium titanate oxide, or carbon composite lithium titanate oxide materials which
realize the charging and discharging of lithium ion batteries when working together
with the cathode material in a certain system. During the charging process, the lithium
titanate oxide anode material accepts the insertion of lithium ions, and during the
discharging process, the lithium ions are released.
4 Classification and code
4.1 Product classification
The carbon-free lithium titanate oxide anode material is represented by LTO, and the
carbon composite lithium titanate oxide anode material is represented by LTO@C,
where LTO represents lithium titanate oxide, @ represents the composite of the two
materials, and C represents carbon:
-- Carbon-free lithium titanate oxide anode materials (LTO) are divided into three
categories, respectively represented as LTO-I, LTO-II, and LTO-III. Their specific
performance requirements are detailed in Table 2;
-- Carbon composite lithium titanate oxide anode materials (LTO@C) are divided
into three categories, respectively represented as LTO@C-I, LTO@C-II, and
LTO@C-III. Their specific performance requirements are detailed in Table 2.
Perform visual observation under natural light conditions.
6.2 Particle size D50
Carry out the measurement in accordance with the measurement method specified in
GB/T 19077.1.
6.3 Moisture content
Determine the moisture content according to the direct potentiometric titration method
specified in GB/T 6283.
6.4 pH
Successively weigh 1.000 g ± 0.001 g (accurate to 0.000 1 g) of sample and 50.00 g ±
0.01 g (accurate to 0.000 1 g) of water into a 100 mL beaker. After stirring, sonicate for
10 minutes and let stand to obtain the solution to be tested. Measure the solution to be
tested with reference to the measurement method specified in GB/T 9724, and the
measurement result is the pH value of the sample.
6.5 Tap density
Carry out the measurement in accordance with the measurement method specified in
GB/T 5162.
6.6 Powder compaction density
Carry out the measurement according to the measurement method specified in
Appendix L of GB/T 24533-2009.
6.7 True density
Carry out the measurement according to the measurement method specified in
Appendix E of GB/T 24533-2009.
6.8 BET specific surface area
Carry out the determination according to the volumetric method for measuring powder
BET specific surface area specified in GB/T 19587.
6.9 Carbon content
Carry out the measurement in accordance with the measurement method specified in
GB/T 20123.
6.10 Lithium content
Carry out the measurement according to the measurement method specified in
Appendix A.
6.11 Iron content
Carry out the measurement according to the measurement method specified in
Appendix H of GB/T 24533-2009.
6.12 Crystal structure
Carry out the measurement according to the measurement method specified in
Appendix B.
6.13 Anatase TiO2 peak intensity ratio I101/I111
Carry out the measurement according to the measurement method specified in
Appendix B.
6.14 Rutile TiO2 peak intensity ratio I110/I111
Carry out the measurement according to the measurement method specified in
Appendix B.
6.15 First reversible specific capacity
Carry out the measurement according to the measurement method specified in
Appendix G of GB/T 24533-2009. Some of the measurement parameters are as follows:
the mass fractions of the sample, conductive electrode, and binder are 80% ~ 90%, 2%
~ 10%, and 2% ~ 10% respectively; the experimental battery is measured at 20 °C ~
25 °C; the limited charging voltage is 2.5 V; the end of discharge voltage is 1.0 V; the
charge and discharge current rate is 1 C.
6.16 First coulombic efficiency
Measure according to the measurement method specified in Appendix G of GB/T
24533-2009, and the test parameters are the same as 6.15.
6.17 Magnetic substance content
Carry out the measurement according to the measurement method specified in
Appendix K of GB/T 24533-2009.
6.18 Residual alkali content
Weigh 5.000 g ± 0.005 g (accurate to 0.000 1 g) of the sample into a 100 mL beaker;
add 50 mL of water, sonicate for 5 minutes; filter and add water to fix the volume in a
100 mL volumetric flask; shake well; let stand until tested. Measure the solution to be
tested according to the measurement method specified in DZ/T 0064.49, and the
measurement result is the residual alkali content of the sample.
6.19 Anion content (Cl-, SO42-)
7.1.3.2 The effective storage period of spare samples is 12 months.
7.2 Inspection
7.2.1 Ex-factory inspection
Inspect the physical and chemical properties, electrochemical properties, magnetic
substance content, total sulfur content, restricted substance content, residual alkali
content, etc. of each batch of samples, and deliver them only after the inspection is
qualified.
7.2.2 Type inspection
Inspect all technical requirements specified in this Standard. Carry out the type
inspection when one of the following situations occurs:
a) when there are changes in raw material models, suppliers, etc.;
b) when there are changes in the production process;
c) when the production equipment which has been stopped for more than half a year
is put into production again for the first time;
d) when customers have special requirements.
7.3 Acceptance rules
7.3.1 A product that meets all the technical indicators required by a certain category in
Table 2 is a qualified product. If an indicator fails to meet the requirements of this
category, double samples shall be taken from the sampling bags of the same batch of
products for re-inspection of the unqualified items, and the re-inspection results will be
used as the final result. Products that do not fall into the product categories in Table 2
or have special requirements shall be determined through negotiation between the
supply and demand parties.
7.3.2 The inspection department of the manufacturer shall ensure that the products
delivered meet the requirements specified in this Standard, and send a product quality
inspection report to the receiving party at the same time as each batch of products leaves
the factory.
7.3.3 The receiving party has the right to accept products in accordance with this
Standard and the right to reject products that do not meet the requirements of this
Standard.
7.3.4 The receiving party shall conduct acceptance inspection of the product within one
month after receiving the product. If there is any objection, a spare sample shall be used
for re-inspection. If there is still a dispute, it shall be arbitrated by the superior quality
supervision department.
8 Packaging, marking
8.1 Pack according to the net weight of 25 kg per package. Special packaging
requirements shall be agreed upon by both parties.
8.2 Pack in a dry environment, and first put the product into waterproof packaging.
Special packaging requirements shall be agreed upon by both parties.
8.3 The packaged products are then packaged in composite bags, plastic barrels, paper
barrels, etc.
8.4 The marking of lithium titanate oxide anode material shall comply with the
requirements in GB/T 191. There shall be an eye-catching marking on the front of each
product packaging bag. The marking shall include the following:
a) product name;
b) model and specifications;
c) number of the standard implemented;
d) net weight;
e) manufacturer name;
f) manufacturing date, production batch number or production date and serial
number;
g) warning instructions;
h) other identifications.
It can also be marked according to customer needs.
9 Storage and transportation
9.1 Product transportation markings shall comply with the regulations on transportation
packaging receipt and delivery markings in GB/T 6388.
9.2 Products shall be stored in a ventilated and dry warehouse.
9.3 Products shall be stacked neatly and cleanly, and markings such as registered
trademark, production batch number, and production date shall be clear and easy to
identify.
9.4 Avoid mixing storage and transportation with items that may cause product
deterioration or damage packaging bags.
Appendix A
(Normative)
Determination method of lithium content
A.1 Scope of application
This Appendix is applicable to the determination of lithium content in samples by
inductively coupled plasma-atomic emission spectrometry.
A.2 Method summary
Dissolve the sample with a mixed acid of concentrated sulfuric acid and concentrated
hydrochloric acid (volume ratio 1:3), and measure the lithium content using an
inductively coupled plasma-atomic emission spectrometer under selected optimal
conditions.
A.3 Reagents and materials
Unless otherwise specified, the water used in the tests in this Standard refers to grade-
3 water meeting the requirements in GB/T 6682, and the reagents used in the tests are
all analytical reagents.
A.3.1 Concentrated sulfuric acid
ρ1.84 g/mL.
A.3.2 Concentrated hydrochloric acid
ρ1.19 g/mL.
A.3.3 Argon gas
Volume fraction not less than 99.999%.
A.3.4 Lithium standard solution
Concentration 1 000 μg/mL, national certified reference material which can be stored
for 1 year.
A.3.5 Preparation of stock standard solution
Take 5.00 mL of lithium standard solution (see A.3.4) in a 100 mL volumetric flask;
add 2 mL of concentrated hydrochloric acid (see A.3.2); adjust the volume to the mark;
shake well; prepare it a stock standard solution with a lithium ion concentration of 50
μg/mL.
A.3.6 Preparation of series standard solutions
Accurately measure 0 mL, 1.00 mL, 2.00 mL, 5.00 mL, and 10.00 mL of lithium ion
stock standard solutions (see A.3.5) into five 100 mL volumetric flasks; add 2 mL of
concentrated hydrochloric acid (see A.3.2) to each; dilute to the mark; shake well;
prepare it standard blank and series standard solutions with lithium ion concentrations
of 0 μg/mL, 0.50 μg/mL, 1.00 μg/mL, 2.50 μg/mL, and 5.00 μg/mL. The ion content in
the solution to be tested shall be within the range of the standard curve.
A.4 Instruments and apparatuses
A.4.1 Inductively coupled plasma-atomic emission spectrometer.
A.4.2 Heating plate or digestion device of equivalent performance (working
temperature range: 50 °C ~ 400 °C).
A.4.3 Analytical balance (sensitivity: 0.000 1 g).
A.5 Analysis steps
A.5.1 Number of determinations
Take two samples for parallel sample testing and take their arithmetic average.
A.5.2 Blank test
Do a blank test with the sample.
A.5.3 Standard curve
Linear correlation coefficient ≥0.999 5.
A.5.4 Preparation of sample solution to be tested
Weigh 0.10 g ± 0.02 g (accurate to 0.000 1 g) of sample into a 50 mL beaker; add 9 mL
of concentrated hydrochloric acid (see A.3.2) and 3 mL of concentrated sulfuric acid
(see A.3.1); place it on the heating plate (see A.4.2); digest completely; cool to room
temperature; filter and dilute to volume. Properly dilute the sample solution to a
constant volume (referring to the preparation method of the stock standard solution for
dilution) to ensure that the lithium ion concentration in the sample solution to be tested
is within the standard curve.
A.5.5 Determination
After the instrument is running stably, according to the conditions in Table A.1, inject
the blank and the series standard solutions (see A.3.6) of the standard sample
sequentially for measurement; draw a standard curve; then measure the sample blank
and the sample solution to be tested (see A.5.4) in the same method, and correct the
results by subtracting the blank.
Appendix B
(Normative)
Determination method of material crystal structure and residual TiO2
B.1 Scope of application
This Appendix is applicable to the crystal structure of the sample tested by the X-ray
diffractometer, as well as the qualitative content of the anatase TiO2 and rutile TiO2
residues.
B.2 Method summary
Take the crystal as a stack of many parallel atomic planes. When X-rays are irradiated
onto the atomic plane, the scattered waves of all atoms have the same phase in the
reflection direction of the atomic plane, which is the direction of enhanced interference.
Since X-rays can penetrate into the interior, to make the internal atoms become the
source of scattering waves, the diffracted ray is regarded as the result of the
superposition of the amplitudes of the reflected waves reflected by many parallel atomic
planes. The condition for interference enhancement is that the phase difference of the
scattered waves of atoms on any adjacent atomic plane in the crystal in the reflection
direction of the atomic plane is an integer multiple of 2π, or the optical path difference
is equal to an integer multiple of the wavelength. It can be seen from Figure B.1 that
the conditions for interference enhancement are: 2d sinθ = nλ, where n is an integer,
which is called the reflection series, θ is the angle between the incident ray and the
reflecting surface, which is called the grazing angle, 2θ is called the diffraction angle,
and the above equation is called the Bragg equation. X-rays diffract on different atomic
planes, and appear as diffraction lines at different diffraction angle positions in the
diffraction pattern. The X-ray diffractometer automatically records the diffraction line
pattern of the lithium titanate oxide anode material in the range of 10° ~ 90°, and
compares the obtained diffraction pattern with the standard X-ray powder diffraction
patterns of lithium titanate oxide, anatase TiO2 and rutile TiO2, to analyze the crystal
structure of the lithium titanate oxide material, and calculate the anatase TiO2 and rutile
TiO2 residues, which are represented by the "peak intensity ratio" of the designated
diffraction peaks of lithium titanate oxide and anatase TiO2 and rutile TiO2.
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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