YB/T 6139.1-2023 English PDF (YBT6139.1-2023)

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YB/T 6139.1-2023: Test methods for graphite-type negative electrode materials - Part 1: Determination of graphitization
YB/T 6139.1-2023
YB
FERROUS METALLURGICAL INDUSTRY STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
ICS 29.050
CCS Q 50
Test methods for graphite-type negative electrode materials -
Part 1: Determination of graphitization
ISSUED ON: DECEMBER 20, 2023
IMPLEMENTED ON: JULY 01, 2004
Issued by: Ministry of Industry and Information Technology 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 Principle ... 5
5 Reagents and materials ... 5
6 Instruments and equipment ... 5
7 Sample ... 5
8 Test steps ... 5
9 Test data processing ... 6
10 Precision ... 7
11 Test report ... 7
Foreword
This document was drafted in accordance with the rules given in GB/T 1.1-2020
"Directives for standardization - Part 1: Rules for the structure and drafting of
standardizing documents".
YB/T 6139 "Test methods for graphite-type negative electrode materials" is divided
into the following two parts:
- Part 1: Determination of graphitization;
- Part 2: Determination of oil absorption value.
This document is Part 1 of YB/T 6139.
Attention is drawn to the possibility that some of the elements of this document may be
the subject of patent rights. The issuing authority shall not be held responsible for
identifying any or all such patent rights.
This document was proposed by China Iron and Steel Association.
This document shall be under the jurisdiction of National Technical Committee on Steel
of Standardization Administration of China (SAC/TC 183).
The drafting organizations of this document: B and T New Materials Group Co., Ltd.,
Guangdong Brunp Recycling Technology Co., Ltd., Shanxi Coal Chemistry Research
Institute of the Chinese Academy of Sciences, Henan Yicheng Hanbo Energy
Technology Co., Ltd., and Metallurgical Industry Information Standards Research
Institute.
Main drafters of this document: Wang Yuhui, Sun Hua, Zhang Ruifang, Xie Yinghao,
Huang Xianhong, Cui Qiang, Zhang Nan, Wang Xiaoyuan, Tang Jianxiao, Yu Hongxing,
Li Zikun, Dai Haitao, Li Fei, Huang Youyuan, Zhang Qinglai.
This document is first issued.
Test methods for graphite-type negative electrode materials -
Part 1: Determination of graphitization
1 Scope
This document specifies terms and definitions, principles, test procedures, precision,
test reports for determination methods for graphitization of graphite-type negative
electrode materials.
This document is applicable to the determination of the graphitization degree of
graphite negative electrode materials using X-ray diffractometer (XRD).
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 8170, Rules of rounding off for numerical values and expression and
judgement of limiting values
GB/T 24533, Graphite negative electrode materials for lithium ion battery
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1 graphitization degree
Graphite has a layered structure. The carbon atoms in each layer form a three-
coordinated hexagonal mesh plane with an angle of 120° to each other in the shape of
sp2 hybrid orbitals. The mesh plane is parallel to the layer, forming a hexagonal graphite
crystal. The degree to which carbon atoms form a hexagonal graphite crystal structure
is called the graphitization degree. The graphitization degree is represented by the letter
G. The value of G is expressed as a percentage (%).
[Source: Carbon Terminology Dictionary]
4 Principle
When X-rays are projected into graphite crystals, they are scattered by atoms and
electrons in the crystals. Due to the periodic arrangement of atoms in the crystals, there
is a fixed phase difference between these scattered waves, which interfere in space,
causing the scattered waves to reinforce each other in some scattering directions and
cancel each other out in some directions, thus causing diffraction. The diffractometer
automatically records the diffraction pattern of the sample and analyzes the diffraction
pattern to obtain sample information.
Crystalline silicon (the diffraction angle of the 111 plane is 28.442°) is used as an
internal standard. By adding crystalline silicon to the sample to be tested, the diffraction
angle of the (002) plane in the graphite crystal can be accurately located (at around
26.5°). The graphite interlayer spacing (d002) is calculated using the Bragg equation.
The graphitization degree is then calculated using the Franklin equation.
5 Reagents and materials
5.1 Monocrystalline silicon powder: purity ≥99%; particle size ≤45 μm.
6 Instruments and equipment
6.1 X-ray diffractometer: Cu target, diffraction angle accuracy ≤ ± 0.02°; diffraction
angle repeatability ≤ 0.002°;
6.2 Agate mortar;
6.3 Electronic balance: sensitivity is 0.1 mg.
7 Sample
The samples shall comply with the requirements of GB/T 24533.
8 Test steps
8.1 Test conditions
Laboratory environment temperature: (23±5)℃; humidity: ≤60%RH. The equipment
and reagents used shall be kept under laboratory environment conditions for 24 h.
8.2 Sample preparation
According to the intensity ratio of the graphite (002) peak and the silicon powder (111)