GB/T 24533-2019 PDF English
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Graphite negative electrode materials for lithium ion battery
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[Replaced by GB/T 24533-2019] Graphite negative electrode materials for lithium ion battery
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GB/T 24533-2019: Graphite negative electrode materials for lithium ion battery---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT24533-2019
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 29.050
Q 51
Replacing GB/T 24533-2009
Graphite negative electrode materials for lithium ion
battery
Issued on: MARCH 25, 2019
Implemented on: FEBRUARY 01, 2020
Issued by. State Administration for Market Regulation;
Standardization Administration of PRC.
Table of Contents
Foreword... 4
1 Scope... 8
2 Normative references... 8
3 Terms and definitions... 9
4 Classification and code... 9
5 Technical requirements... 11
6 Test methods... 11
7 Inspection rules... 13
8 Packaging, marking... 14
9 Storage and transportation... 15
Appendix A (Normative) Method for determination of particle size distribution
... 21
Appendix B (Normative) Method for determination of moisture content... 25
Appendix C (Normative) Method for determination of pH... 28
Appendix D (Normative) Method for determination of true density... 30
Appendix E (Normative) Method for determination of interlayer spacing d002
... 33
Appendix F (Normative) Method for determination of graphite orientation... 35
Appendix G (Normative) Method for determination of first coulomb efficiency
and first discharge specific capacity... 38
Appendix H (Normative) Method for determination of trace metal elements.. 42
Appendix I (Normative) Method for determination of anions... 45
Appendix J (Normative) Method for determination of sulfur content... 49
Appendix K (Normative) Method for determination of magnetic substances.. 52
Appendix L (Normative) Method for determination of powder compaction
density... 56
Appendix M (Normative) Method for determination of tap density... 58
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard replaces GB/T 24533-2009 “Graphite negative electrode
materials for lithium ion battery”. As compared with GB/T 24533-2009, the main
technical contents of this standard are as follows.
- MODIFY the normative references (see Chapter 2);
- MODIFY the definition of graphite negative electrode material for lithium ion
battery; MODIFY the “carbon anode” in the definition into “graphite anode”
(see 3.1);
- MODIFY the "mesophase carbon microsphere artificial graphite" into
"carbon micro bead"; MODIFY the "petroleum coke type artificial graphite"
into "common petroleum coke artificial graphite"; ADD the explanation of
composite graphite (see 4.1.1);
- MODIFY the grade of graphite anode materials for some lithium-ion
batteries; ADD the graphitization index (see 4.1.2);
- DELETE the "AG-PAG-I-18-340" from the example of product code (see
4.2 of 2009 edition);
- MODIFY the content of typical product technical indicators; MODIFY the
“Table 3 ~ Table 11” to “Table 3, Table 4, Table 5” (see 5.2);
- MODIFY the moisture determination into making determination according
to Appendix B or GB/T 3521 (see 6.3);
- MODIFY the determination of specific surface area into making
determination according to GB/T 19587 (see 6.6);
- ADD the determination method of the graphite orientation (reference index),
to make determination according to the provisions of Appendix F (see 6.9);
- DELETE the determination of NO2- and PO43- (see 6.12 of the 2009 edition);
- MODIFY the method for determination of organic content (see 6.17);
- MODIFY the method for determination of the content of restricted
substances (see 6.18);
- MODIFY the sampling and sample preparation into complying with the
provisions of GB/T 1427 (see 7.1.1);
- DELETE that "samples that are used for inspection and retention shall be
retained for at least 500 g" (see version 7.1.4 of 2009);
- In the exit-factory inspection, ADD the first discharge specific capacity, the
first coulombic efficiency; DELETE the pH value (see 7.2.1);
- DELETE the “raw material batch number” in the type test (see 7.2.2 of the
2009 edition);
- In the acceptance rules, DELETE that “the receiving party has the right to
accept the product according to this standard and has the right to reject
products that do not meet the requirements of this standard” (see 7.3.3 of
the 2009 edition);
- MODIFY the requirements for packaging and marking. the packaging and
marking of the product conform to the provisions of GB/T 191 and GB/T
6388; the net weight is negotiated between the supplier and the purchaser
(see 8.1);
- DELETE "Recommendation. in an environment with temperature ≤ 45 °C
and humidity ≤ 75%" (see 8.2 of 2009 edition);
- DELETE that "At the front side of each package of the graphite negative
electrode material for lithium-ion battery, it shall have a prominent mark”
(see 8.4.1 of 2009 edition);
- DELETE the "Recommendations. temperature ≤ 45 °C and humidity ≤ 75%"
(see 9.1 of 2009 edition);
- MODIFY the requirements for dispersant in Appendix A (see A.3.1);
- MODIFY the scope of the particle test (see A.4.3);
- MODIFY the instrument setting parameters in Appendix A to. Set the
optimal parameters according to the instrument manual (see A.4.4);
- MODIFY the results calculation and data processing in Appendix A, adding
"Dmax" (see A.7);
- MODIFY the instrument and equipment in Appendix B; MODIFY the
balance sensitivity to “0.0001 g”; INCREASE the micro-injector by “5 μL”
(see B.4.2 and B.4.3);
- MODIFY the reagents and materials in Appendix C (see C.3);
- MODIFY the instruments and equipment in Appendix C; DELETE the watch
glass and the hot plate; ADD the ultrasonic cleaner (see C.4);
- MODIFY the preparation of specimen in Appendix C (see C.5);
- MODIFY the instruments and equipment in Appendix D; MODIFY the
balance sensitivity to “0.0001 g” (see D.4.4);
- ADD the requirements for rounding off of the result calculation and data
processing in Appendix D (see D.6.3);
- ADD the Appendix F, Determination of graphite orientation (see Appendix
F);
- MODIFY the binder in Appendix G (see G.3.2);
- MODIFY the analysis procedure in Appendix G; MODIFY it into “charge-
discharge rate of 0.1C” (see G.6);
- MODIFY the scope of Appendix H and ADD the “cobalt, zinc” (see H.1);
- MODIFY the reagents and materials in Appendix H; ADD the standard
solutions of cobalt and zinc (see H.3);
- MODIFY the instruments and equipment in Appendix H; MODIFY the
balance sensitivity to “0.0001 g” (see H.4);
- MODIFY the determination requirements in Appendix H; ADD the reference
wavelengths of cobalt and zinc (see H.7);
- DELETE the "NO2-" and "PO43-" from the scope of Appendix I (see I.1 of the
2009 edition);
- DELETE the preparation of the standard solution of "NO2-" and "PO43-" from
the reagents and materials in Appendix I (see I.3 of 2009 edition);
- MODIFY the determination range in Appendix K; ADD the cobalt content
(see K.1);
- MODIFY the reagents and materials in Appendix K; ADD the cobalt
standard solution (see K.3.5);
- MODIFY the instruments and equipment in Appendix K (see K.4);
- MODIFY the specimen preparation in Appendix K (see K.5);
- MODIFY the preparation of a series of mixed standard solutions in
Appendix K (see K.6);
- MODIFY the analytical procedures in Appendix K (see K.7);
- MODIFY the reagents and materials in Appendix L; ADD the absolute
ethanol (see L.3.2);
- MODIFY the instruments and equipment in Appendix L; USE the digital
thickness gauge to replace the Vernier caliper (see L.4.3);
- MODIFY the analytical procedures in Appendix L (see L.5);
- MODIFY the results calculation and data processing in Appendix L (see L.6);
- MODIFY the sensitivity of the electronic balance in instruments and
equipment in Appendix M to “0.0001 g” (see M.3.1);
- In Appendix M, DELETE that the “25 cm3 measuring cylinder is mainly used
to measure powders with a bulk density of more than 4 g/cm3” (see M.3.2.2
of the 2009 edition);
- MODIFY the Table of bulk density and powder amount in the analytical
procedures of Appendix M (see M.4.2);
- DELETE the original Appendix D, Appendix N, Appendix O (see 2009
edition).
This standard was proposed by the China Iron and Steel Association.
This standard shall be under the jurisdiction of the National Steel
Standardization Technical Committee (SAC/TC 183).
Drafting organizations of this standard. Shenzhen Beiterui New Energy
Materials Co., Ltd., Guangdong Dongdao New Energy Co., Ltd., Beiterui
(Jiangsu) New Materials Technology Co., Ltd., Huizhou Beiterui New Material
Technology Co., Ltd., Shanxi Beiterui New Energy Technology Co., Ltd., Tianjin
Beiterui New Energy Materials Co., Ltd., Metallurgical Industry Information
Standards Institute.
The main drafters of this standard. He Xueqin, Chen Nanmin, Zhou Haihui, Yue
Min, Huang Youyuan, Ren Jianguo, Zheng Jingxu, Wu Qixiu, Yan Huiqing,
Wang Hongjing, Xiao Wei, Zhou Chengkun, Zhang Qinglai, Mao Aiping, Zhou
Huijian, Zheng Haichi, Zhang Jinying, Miao Yanli, Li Shoubin, Wang Peichu,
Geng Linhua, Zhou Haomao.
This standard replaces the standard previously issued as follows.
- GB/T 24533-2009.
Graphite negative electrode materials for lithium ion
battery
1 Scope
This standard specifies the terms and definitions, classification and code,
technical requirements, test methods and inspection rules for graphite negative
electrode materials for lithium ion battery.
This standard applies to graphite-based negative electrode materials used as
negative electrodes for lithium ion batteries.
2 Normative references
The following documents are essential to the application of this document. For
the dated documents, only the versions with the dates indicated are applicable
to this document; for the undated documents, only the latest version (including
all the amendments) are applicable to this standard.
GB/T 191 Packaging - Pictorial marking for handling of goods
GB/T 1427 Sampling method for carbon material
GB/T 3120 Nickel wire
GB/T 3521 Method for chemical analysis of graphite
GB/T 3782 Acetylene black
GB/T 4369 Lithium
GB/T 5187 Foil of copper and copper alloy
GB/T 6388 Sign for transport packaging receipt and delivery
GB/T 6682 Water for analytical laboratory use - Specification and test
methods
GB/T 8170 Rules of rounding off for numerical values & expression and
judgement of limiting values
GB/T 9724 Chemical reagent - General rule for the determination of pH
GB/T 19587 Determination of the specific surface area of solids by gas
adsorption using the BET method
GB/T 26125 Electrical and electronic products - Determination of six
regulated substances (lead, mercury, cadmium, hexavalent chromium,
polybrominated biphenyls, polybrominated diphenyl ethers)
EPA 8260C.2006 Volatile organic compounds by gas chromatography/mass
spectrometry (GC/MS)
EPA 5021.1996 Volatile organic compounds, oils and other solid matrices
using equilibrium headspace analysis
3 Terms and definitions
The following terms and definitions apply to this document.
3.1
Graphite negative electrode materials for lithium ion battery
The graphite negative electrode material for lithium ion battery adopts a
carbon material with a graphite crystalline layer structure, which synergizes
with the positive electrode material in a certain system to realize multiple
charging and discharging of the lithium ion battery. In the charging process,
the graphite negative electrode receives the insertion of lithium ion; whilst in
the discharging process, it realizes the release of the lithium ion.
Note. The theoretical capacity of graphite negative electrode materials is 372
(mA • h)/g, the color is gray black or steel ash, with a metallic luster.
4 Classification and code
4.1 Classification of products
4.1.1 Categories of graphite negative electrode material for lithium ion battery.
a) Natural graphite, expressed by NG.
b) Artificial graphite, represented by AG, which is divided into the following
three types.
1) Carbon micro bead, expressed by CMB;
2) Needle coke artificial graphite, expressed by NAG;
3) Common petroleum coke artificial graphite, expressed by CPAG.
c) Composite graphite, a graphite material containing at least two
components of natural graphite and artificial graphite, expressed by CG.
4.1.2 The grades of the graphite negative electrode materials for lithium ion
battery are as shown in Table 1.
5 Technical requirements
5.1 Appearance
The powder which has a grayish black or steel ash, with a metallic luster.
5.2 Physical and chemical indicators
The physical and chemical indicators of graphite negative electrode materials
for lithium ion batteries shall comply with the requirements of Table 1.If there
are special requirements, the supplier and the purchaser shall determine it by
negotiation. Tables 3, 4, 5 are typical product specifications.
6 Test methods
6.1 Appearance
Visual observation under natural light conditions.
6.2 Particle size distribution
It is determined according to the provisions of Appendix A.
6.3 Moisture
It is determined according to the provisions of Appendix B or GB/T 3521.
6.4 pH
It is determined according to the provisions of Appendix C.
6.5 Fixed carbon content
It is determined according to the provisions of GB/T 3521.
6.6 Specific surface area
It is determined according to the provisions of GB/T 19587.
6.7 True density
It is determined according to the provisions of Appendix D.
6.8 Inter-layer spacing d002 and graphitization degree
It is determined according to the provisions of Appendix E.
6.9 Graphite orientation (reference indicator)
It is determined according to the provisions of Appendix F.
6.10 First Coulomb efficiency
It is determined according to the provisions of Appendix G.
6.11 First discharge specific capacity
It is determined according to the provisions of Appendix G.
6.12 Trace metal elements
It is determined according to the provisions of Appendix H.
6.13 F-, Cl-, SO42-, NO3-, Br- ion indicator
It is determined according to the provisions of Appendix I.
6.14 Sulfur content
It is determined according to the provisions of Appendix J.
7 Inspection rules
7.1 Sampling method
7.1.1 Sampling and sample preparation shall be carried out in accordance with
the provisions of GB/T 1427.The stainless-steel sampling braze is stainless
steel of grade 316 or equivalent, the diameter is not more than 30 mm, the
length is 500 mm ~ 700 mm.
7.1.2 After the sample is placed in the plastic sample can, it shall attach a sign
to its outer wall, which indicate the following contents.
a) Sample category and number;
b) Overall material lot number and quantity;
c) Amount of sample;
d) Date of sampling;
e) Name of sampler.
7.1.3 Samples shall be preserved in a sealed form and stored in an environment
that is resistant to breakage, rain exposure, moisture. The spare sample has a
storage period of 18 months.
7.2 Classification of inspections
7.2.1 Exit-factory inspection. After the particle size, carbon content, moisture,
tap density, powder compaction density, specific surface area, trace elements
(iron, sodium, chromium, copper, nickel, aluminum, molybdenum), magnetic
substances (iron + chromium + nickel + zinc + cobalt), first discharge specific
capacity, first coulombic efficiency of each batch pass the inspection, chop the
quality inspection seal.
7.2.2 Type inspection. All technical requirements as specified in this standard
shall be inspected. Type inspection is performed in one of the following cases.
- When the models of raw material, supplier, etc. are changed;
- When there is a change in the production process;
- When the production equipment is shut down for more than half a year and
production is started again;
- When the customer has special requirements.
7.3 Acceptance rules
7.3.1 The product complies with all the technical indicators in Table 1, Table 3,
Table 4 and Table 5 as qualified products. If one of the indicators does not meet
the requirements of this standard, it shall be doubled from the sampling bag of
the same batch of products for re-inspection of the unqualified items. If all the
re-inspections are qualified, it is qualified; if one item fails, it is unqualified.
7.3.2 The manufacturer shall ensure that the exit-factory products meet the
requirements as stipulated in this standard. Each batch of products shall be
accompanied by an inspection report when exit-factory.
7.3.3 The re-inspection period of the consignee shall be two months. If there is
any objection, it shall be double-sampled and re-inspected. If there is still
dispute, it shall be inspected by a qualified third-party testing agency.
8 Packaging, marking
8.1 The packaging and marking of the product shall comply with the provisions
of GB/T 191.The net weight shall be negotiated between the supplier and the
purchaser.
8.2 The packaging shall be carried out under dry conditions. The product is first
placed into a waterproof packaging bag (PE sealed bag, aluminum plastic
sealed bag is recommended). Special packaging requirements are agreed
upon by the supplier and the purchaser.
8.3 The packaged product is then packaged by the outer packaging material,
which is agreed by the supplier and the purchaser.
8.4 The marking shall comply with the provisions of GB/T 6388, and generally
shall include the following contents, or may be marked according to customer
needs.
9 Storage and transportation
9.1 The product shall be stored in a ventilated, dry warehouse.
9.2 The product stack shall be neat and clean; the production lot number and
other signs shall be clearly identifiable.
9.3 Avoid the product from being stored and transported together with other
articles which may deteriorate the product or damage the package.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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