GB/T 30835-2014 PDF English

GB/T30835-2014 (GBT30835-2014): PDF in English

GB/T 30835-2014 GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 29.050 Q 53 Lithium iron phosphate-carbon composite cathode 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 of the People's Republic of China; 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 codes ... 5 5 Technical requirements ... 6 6 Test methods ... 7 7 Inspection rules ... 9 8 Packaging, marks ... 11 9 Storage and transportation ... 11 Annex A (normative) Method for determination of lithium content (excluding carbon content) ... 13 Annex B (normative) Method for determination of iron content (excluding carbon content) ... 17 Annex C (normative) Method for determination of phosphorus content (excluding carbon content) ... 21 Annex D (informative) Method for determination of crystal structure ... 26 Annex E (normative) Method for determination of iron ion dissolution rate ... 29 Annex F (normative) Method for determination of first coulombic efficiency, first reversible specific capacity, rate performance ... 33 Annex G (normative) Method for determination of conductivity ... 38 Lithium iron phosphate-carbon composite cathode materials for lithium ion battery 1 Scope This Standard specifies the terms and definitions, classification and codes, technical requirements, test methods, inspection rules and packaging, marking, storage and transportation for lithium iron phosphate-carbon composite cathode materials for lithium ion battery. This Standard applies to lithium iron phosphate-carbon composite cathode materials for lithium ion battery. 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 and storage marks 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 12805, Laboratory glassware -- Burettes 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 JCPDS (01-077-0179), Lithium iron phosphate 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 iron phosphate-carbon composite cathode materials Lithium-ion battery cathode material composed of lithium iron phosphate and carbon with an olivine structure. Lithium iron phosphate belongs to the orthorhombic crystal system. It has a one-dimensional lithium embedded channel. Lithium ions can be reversibly deintercalated within the crystal lattice. The theoretical specific capacity of the material is 170 mA·h/g. NOTE: LFP@C mentioned in this Standard all represents lithium iron phosphate-carbon composite cathode materials. 4 Classification and codes 4.1 Product classification Lithium iron phosphate-carbon composite cathode materials are divided into energy type and power type according to charge and discharge characteristics and usage requirements, represented by LFP@C-E and LFP@C-P respectively. LFP represents lithium iron phosphate, @ represents the composite of two materials, C represents carbon, E represents energy type, and P represents power type: - Energy type lithium iron phosphate-carbon composite cathode materials (LFP@C- E) are divided into three categories, represented by LFP@C-E-Ⅰ, LFP@CE-Ⅱ, and LFP@C-E-Ⅲ. The specific performance requirements are detailed in Table 2; - Power type lithium iron phosphate-carbon composite cathode materials (LFP@C- P) are divided into three categories, represented by LFP@C-P-Ⅰ, LFP@CP-Ⅱ, and LFP@C-P-Ⅲ. The specific performance requirements are detailed in Table 2. 6.17 Conductivity Measure according to the measurement method specified in Annex G. 6.18 Restricted substance content The measurement is carried out according to the measurement method specified in IEC 62321. 7 Inspection rules 7.1 Sampling method 7.1.1 Sampling 7.1.1.1 Lithium iron phosphate-carbon composite cathode materials for bagged lithium- ion batteries shall be sampled in accordance with GB/T 13732. Open the bag of lithium iron phosphate-carbon composite cathode material to be collected in a dry environment. Use a clean stainless steel sampling drill to insert into the bag along the axis. The insertion depth shall not be less than 4/5 of the depth of the sampling bag. Samples are taken within 20 mm around the central axis of the material in the bag. 7.1.1.2 In order to make the collected samples represent the quality of this batch of products, all collected samples are combined. Place on a square film of sufficient strength and appropriate size or firm, soft drying paper. Mix evenly by rolling repeatedly (turn more than 15 times). The mixed sample shall not be less than 500 g. Cut off two 250 g specimens, one for testing and one for backup. 7.1.2 Sample label After the sample is placed in the PVC sample jar, a label is immediately attached to the outer wall. The label includes the following: a) Sample type and number; b) Overall material batch number and quantity; c) Sample size; d) Sampling date; e) Name of sampler. 7.1.3 Storage of samples 7.1.3.1 Samples shall be sealed and stored in anti-breakage bags, rain-proof, moisture- proof and other environments. 7.1.3.2 The effective storage period of spare samples is 12 months. 7.2 Inspection 7.2.1 Exit-factory inspection Inspect the particle size, carbon content, moisture content, BET specific surface area, tap density, electrochemical performance, iron ion dissolution amount, conductivity and other indicators of each batch of samples. They can be shipped only after passing the inspection. 7.2.2 Type inspection All technical requirements specified in this Standard shall be inspected. Type inspection is carried out when one of the following situations occurs: a) When there are changes in raw material models, supplier manufacturers, etc.; b) When there are changes in the production process; c) When the production equipment has been shut down for more than half a year and then starts production for the first time; d) When customers have special requirements. 7.3 Acceptance rules 7.3.1 Products that meet all the technical indicators required by a certain category in Table 2 are qualified products. 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 to re-inspect the unqualified items. The re-inspection results shall be taken as the final result. Products that do not fall into the product categories in Table 2 or have special requirements must be determined through negotiation between the supplier and the purchaser to determine whether they are qualified. 7.3.2 The inspection department of the manufacturer shall ensure that the products shipped meet the requirements of this Standard. When each batch of products leaves the factory, a product quality inspection report is sent to the recipient. 7.3.3 The consignee 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 consignee 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 will be arbitrated by the superior quality supervision department. Annex A (normative) Method for determination of lithium content (excluding carbon content) A.1 Scope of application This appendix is applicable to the determination of lithium content (except carbon content) in specimens by inductively coupled plasma optical emission spectrometry. A.2 Method summary The specimen is dissolved in hydrochloric acid. In hydrochloric acid medium, according to the optimized working conditions of the instrument, use the working curve method and the inductively coupled plasma emission spectrometer to measure the lithium ion content. A.3 Reagents and materials Without special instructions, the water used in the tests in this Standard refers to water that meets the requirements in GB/T 6682 for the grade three water. All reagents used in the test are analytically pure. A.3.1 Concentrated hydrochloric acid ρ 1.19 g/mL. A.3.2 Argon gas The volume fraction is not less than 99.999%. A.3.3 Lithium standard solution The concentration is 1000 μg/mL. It is a national certified standard sample and can be stored for 1 year. A.3.4 Preparation of reserve standard solutions Take 5.00 mL of lithium standard solution (see A.3.3) in a 100 mL volumetric flask. Add .......
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