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This standard is developed 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. The following main technical changes have been made with respect to GB/T 24533-2009:
——The “Normative references” is modified (see clause 2);
——The definition of graphite negative electrode materials for lithium ion battery is modified, changing the "carbon negative electrode" in the definition to "graphite negative electrode" (see 3.1);
——The "MCMB type artificial graphite" is changed to "CMB artificial graphite", the "needle coke type artificial graphite" is changed to "needle coke artificial graphite", and the "petroleum coke type artificial graphite" is changed to "common petroleum coke artificial graphite", and the explanation of composite graphite is added (see 4.1.1);
——The grades of some of the graphite negative electrode materials for lithium ion batteries are modified and the indexes of graphitization degree are added (see 4.1.2);
——The “AG-PAG-I-18-340” in the product code example is deleted (see 4.2 of Edition 2009);
——The content on technical index of typical products is modified, and the content "Tables 3 to 11 is modified to "Tables 3, 4 and 5" (see 5.2);
——The moisture determination is modified as: it shall be determined in accordance with Annex B or the requirements of GB/T 3521 (see 6.3);
——The specific surface area determination is modified as: it shall be determined in accordance with GB/T 19587 (see 6.6);
——The determination method of graphite orientation (reference index) is added, and the graphite orientation shall be determined according to those specified in Annex F (see 6.9);
——The determination of NO2- and PO43- is deleted (see 6.12 of Edition 2009);
——The determination method of organic matter content is modified (see 6.17);
——The determination method of restricted substance content is modified (see 6.18);
——The sampling and sample preparation are modified to be carried out in accordance with GB/T 1427 (see 7.1.1);
——The requirement “The samples for inspection and retention shall be reserved for at least 500g” is deleted (see 7.1.4 of Edition 2009);
——The first discharge specific capacity and initial Coulombic efficiency are added in and the pH value is deleted from end-of-manufacturing inspection (see 7.2.1);
——The “raw material batch number” is deleted from the type inspection (see 7.2.2 of Edition 2009);
——The provision "The consignee is entitled to carry out acceptance inspection on the products in accordance with this standard and reject the products that do not meet the requirements of this standard” is deleted from the acceptance rules (see 7.3.3 of Edition 2009);
——The requirements of packaging and marking are modified as: The packaging and marking of products shall meet those specified in GB/T 191 and GB/T 6388, and the net weight shall be negotiated by the supplier and the demander (see 8.1);
——The provision "Suggestion: in an environment with a temperature ≤45℃ and a humidity ≤ 75%” is deleted (see 8.2 of Edition 2009);
——The provision “There shall be conspicuous marking on the front surface of each pacing bag of the graphite negative electrode materials for lithium ion battery” is deleted (see 8.4.1 of Edition 2009);
——The provision "Suggestion: temperature ≤45℃ and humidity ≤ 75%” is deleted (see 9.1 of Edition 2009);
——The requirements for dispersing agents in Annex A are modified (see A.3.1);
——The test range of particle size is modified (see A.4.3);
——The instrument setting parameters in Annex A are modified as: Set the optimum parameters according to the instrument instruction (see A.4.4);
——The “Result calculation and data processing” in Annex A is modified, with the “Dmax” added (see A.7);
——The “Instruments and apparatus” in Annex B is modified, with the sensitivity of the balance modified to "0.0001 g", and the capacity of microinjector increased by "5μL" (see B.4.2 and B.4.3);
——The “Reagents and materials” in Annex C is modified (see C.3);
——The “Instruments and apparatus” in Annex C is modified, with the watch glasses and electric hot plate deleted, and the ultrasonic cleaner added (see C.4);
——The “Specimen preparation” in Annex C is modified (see C.5);
——The “Instruments and apparatus” in Annex D is modified, with the sensitivity of the balance modified to "0.0001 g” (see D.4.4);
——The rounding-off requirements for result calculation and data processing in Annex D are added (see D.6.3);
——The Annex F “Method for determining orientation of graphite” is added (see Annex F);
——The binder in Annex G is modified (see G.3.2);
——The “Analytical procedure” in Annex G is modified, with the corresponding content modified to "charge/discharge rate: 0.1C" (see G.6);
——The “Scope” in Annex H is modified, with "cobalt and zinc” added in it (see H.1);
——The “Reagents and materials” in Annex H is modified, with the standard solutions of cobalt and zinc added (see H.3);
——The “Instruments and apparatus” in Annex H is modified, with the sensitivity of the balance modified to "0.000 1 g” (see H.4);
——The determination requirements in Annex H are modified, with the reference wavelengths of cobalt and zinc added (see H.7);
——The "NO2-"and "PO43-" in the scope of Annex I are deleted (see I.1 of Edition 2009);
——The preparations of standard solutions of "NO2-"and "PO43-"in “Reagents and materials” in Annex I are deleted (see I.3 of Edition 2009);
——The determination scope in Annex K is modified, with the content of cobalt added (see K.1);
——The “Reagents and materials” in Annex K is modified, with the cobalt standard solution added (see K.3.5);
——The “Instruments and apparatus” in Annex K is modified (see K.4);
——The “Specimen preparation” in Annex K is modified (see K.5);
——The “Preparation of series mixed standard solutions” in Annex K is modified (see K.6);
——The “Analytical procedure” in Annex K is modified (see K.7);
——The “Reagents and materials” in Annex L is modified, with the anhydrous ethanol added (see L.3.2);
——The “Instruments and apparatus” in Annex L is modified, with the vernier caliper replaced by digital thickness gauge (see L.4.3);
——The “Analytical procedure” in Annex L is modified (see L.5);
——The “Result calculation and data processing” in Annex L is modified (see L.6);
——The sensitivity of the balance in “Instruments and apparatus” in Annex M is modified to "0.0001 g” (see M.3.1);
——The provision "The 25 cm3 measuring cylinder is mainly used for measuring powders with an apparent density greater than 4 g/cm3" (see M.3.2.2 of Edition 2009);
——The table of correspondence between apparent density and powder amount in the “Analytical procedure” in Annex M is modified (see M.4.2);
——The original Annexes D, N and O are deleted (see Edition 2009).
This standard was proposed by China Iron and Steel Industry Association.
This standard is under the jurisdiction of SAC/TC 183 National Technical Committee on Iron and Steel of Standardization Administration of China.
The previous edition of this standard is as follows:
——GB/T 24533-2009.
Graphite negative electrode materials for lithium ion battery
1 Scope
This standard specifies terms and definitions, classification and code, technical requirements, test methods, inspection rules, etc. of graphite negative electrode materials for lithium ion battery.
This standard is applicable to graphite negative electrode materials with lithium ion battery as the negative electrode.
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 1427 Sample method of carbon material
GB/T 3120 Nickel wires
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 Transport package shipping mark
GB/T 6682 Water for analytical laboratory use - Specification and test methods
GB/T 8170 Rules of rounding off for numerical values & expression and judgment 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 in soils and other solid matrices using equilibrium headspace analysis
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
graphite negative electrode materials for lithium ion battery
graphite carbon material with crystalline layered structure, which cooperates with positive electrode material in a certain system to realize multiple charging and discharging of lithium ion battery, graphite negative electrode accepting lithium ion insertion in the charging process while lithium ion leaving the graphite negative electrode in the discharging process
Note: The theoretical capacity of graphite negative electrode material is 372 (mA·h)/g, and the color is gray black or steel gray with metallic luster.
4 Classification and code
4.1 Product classification
4.1.1 Types of graphite negative electrode materials for lithium ion battery:
a) natural graphite, expressed by NG.
b) artificial graphite, expressed by AG, which is divided into the following 3 types:
1) mesophase carbon micro bead artificial graphite, expressed by CMB (Carbon Micro Bead);
2) needle coke artificial graphite, expressed by NAG;
3) common petroleum coke artificial graphite, expressed by CPAG.
c) composite graphite, graphite material containing at least natural graphite and artificial graphite, expressed by CG.
4.1.2 The grades of graphite negative electrode materials for lithium ion battery are shown in Table 1.
Table 1 Grades of graphite negative electrode materials for lithium ion battery
Type Grade First discharge specific capacity (mA·h)/g Initial Coulombic efficiency
% Powder compaction density
g/cm3 Graphitization degree
% Fixed carbon content
% Magnetic substance content
ppm Iron content
ppm ROHS certification
Natural graphite (NG) I ≥360.0 ≥95.0 ≥1.65 ≥96 ≥99.97 ≤0.1 ≤10 Passed
II ≥360.0 ≥93.0 ≥1.55 ≥94 ≥99.95 ≤0.1 ≤30 Passed
III ≥345.0 ≥91.0 ≥1.45 ≥92 ≥99.90 ≤0.5 ≤50 Passed
Artificial graphite
(AG) Carbon micro bead
(CMB) I ≥350.0 ≥95.0 ≥1.50 ≥94 ≥99.97 ≤0.1 ≤20 Passed
II ≥340.0 ≥94.0 ≥1.40 ≥90 ≥99.95 ≤0.5 ≤50 Passed
III ≥330.0 ≥90.0 ≥1.20 ≥90 ≥99.70 ≤1.5 ≤100 Passed
Needle coke
(NAG) I ≥355.0 ≥94.0 ≥1.25 ≥94 ≥99.97 ≤0.1 ≤20 Passed
II ≥340.0 ≥93.0 ≥1.20 ≥90 ≥99.95 ≤0.1 ≤50 Passed
III ≥320.0 ≥90.0 ≥1.10 ≥85 ≥99.70 ≤1.5 ≤100 Passed
Common petroleum coke
(CPAG) I ≥350.0 ≥95.0 ≥1.40 ≥94 ≥99.97 ≤0.1 ≤20 Passed
II ≥330.0 ≥93.0 ≥1.20 ≥90 ≥99.95 ≤0.1 ≤50 Passed
III ≥300.0 ≥90.0 ≥1.00 ≥85 ≥99.70 ≤1.5 ≤100 Passed
Composite graphite
(CG) I ≥355.0 ≥94.0 ≥1.60 ≥94 ≥99.97 ≤0.1 ≤20 Passed
II ≥345.0 ≥92.0 ≥1.50 ≥92 ≥99.95 ≤0.1 ≤30 Passed
III ≥330.0 ≥91.0 ≥1.40 ≥90 ≥99.70 ≤0.5 ≤50 Passed
Notes:
1 The product shall be of certain grade only if its indexes meet the requirements of all indexes of such grade.
2 RoHS certification refers to passing the restricted substance content detection certification.
4.2 Product code
The product code consists of type code, grade code, D50 and first discharge specific capacity, which are arranged in sequence, namely:
Type code-grade code-D50-first discharge specific capacity; see Table 2 for specific examples.
Table 2 Examples of product codes and their meanings
Example Meaning
NG-I-18-360 Grade I natural graphite negative electrode materials for lithium ion battery, with D50 = (18.0±2.0) μm, and first discharge specific capacity ≥ 360 (mA·h)/g
AG-CMB-I-22-350 Grade I artificial graphite mesophase graphite negative electrode materials for lithium ion battery, with D50 = (22.0±2.0) μm and first discharge specific capacity ≥ 350 (mA·h)/g
AG-NAG-I-18-355 Grade I needle coke artificial graphite negative electrode materials for lithium ion battery, with D50 = (18.0±2.0) μm and first discharge specific capacity ≥ 355 (mA·h)/g
CG-I-17-355 Grade I composite graphite negative electrode materials for lithium ion battery, with D50 = (17.0±2.0) μm and first discharge specific capacity ≥ 355 (mA·h)/g
5 Technical requirements
5.1 Appearance
Gray black or steel gray powder with metallic luster.
5.2 Physical and chemical indexes
The physical and chemical indexes of graphite negative electrode materials for lithium ion battery shall meet those specified in Table 1, and the special requirements, if any, shall be determined through negotiation between the supplier and the demander. The technical indexes of typical products are listed in Tables 3, 4 and 5.
Foreword i
1 Scope
2 Normative references
3 Terms and definitions
4 Classification and code
5 Technical requirements
6 Test methods
7 Inspection rules
8 Packaging and marking
9 Storage and transport
Annex A (Normative) Method for measuring particle size distribution
Annex B (Normative) Method for determining moisture content
Annex C (Normative) Method for determining pH value
Annex D (Normative) Method for determining true density
Annex E (Normative) Method for determining of interplanar spacing d
Annex F (Normative) Method for determining orientation of graphite
Annex G (Normative) Method for determining initial Coulombic efficiency and first discharge specific capacity
Annex H (Normative) Method for determining trace metal elements
Annex I (Normative) Method for determining anions
Annex J (Normative) Method for determining sulfur content
Annex K (Normative) Method for determining magnetic substances
Annex L (Normative) Method for determining powder compaction density
Annex M (Normative) Method for determining tap density
