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GB/T 24533-2019 English PDF (GBT24533-2019)

GB/T 24533-2019 English PDF (GBT24533-2019)

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GB/T 24533-2019: Graphite negative electrode materials for lithium ion battery

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.
GB/T 24533-2019
GB
NATIONAL STANDARD OF THE
PEOPLE 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
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 and expression and
judgement of limiting values
GB/T 9724 Chemical reagent - General rule for the determination of pH
- 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:
- Product name;
- Product code and specifications;
- This standard number;
- Net weight;
Appendix B
(Normative)
Method for determination of moisture content
B.1 Scope
This Appendix applies to the Karl Fischer Coulometric titrator to measure the moisture content of the specimen.
B.2 Principle
The following reactions occur in the presence of water, iodine and sulfur dioxide in the presence of organic bases and methanol:
H2O + I2 + SO2 + CH3OH + 3RN ??? [RHN]SO4CH3 + 2[RHN]I
The iodine therein is produced by electrochemically oxidizing the electrolytic cell.
2I- ??? I2 + 2e-
The amount of iodine produced is proportional to the electric quantity passing through the electrolytic cell, so the electric quantity consumed by electrolysis is recorded, and according to Faraday's law, the moisture content of the specimen (10.72 mC ??? 1 ??g H2O) can be obtained. Moisture content is expressed as a percentage:
Water [%] = {(consumption [mC] ?? 10.72 [mC/??g] - (drift [??g/min] ?? duration [min]) - blank value [??g]) ?? 100 [%]} / {mass [g] ?? 106[mg/g]}
In order to obtain the moisture content expressed in ppm, it may be multiplied by 10000. In order to obtain the moisture content expressed in grams/kilograms (g/kg), it may be multiplied by 10.
B.3 Reagents and materials
B.3.1 Desiccant: 3A molecular sieve.
B.3.2 Electrolyte: Diaphragm-free electrolyte (commodity: shelf life, 5 years; storage conditions: moisture-proof sealed).
B.4 Instruments and equipment
B.4.1 Karl Fischer coulometric titrator: The measurement range is 0.0001% ~ 1%.
Appendix C
(Normative)
Method for determination of pH
C.1 Scope
This Appendix applies to the use of pH meter to test the pH value of the graphite negative electrode materials.
C.2 Principle
Mix the specimen and the distilled water. Use pH meter to determine the pH value of the specimen.
C.3 Reagents and materials
C.3.1 Pure water (GB/T 6682), grade-III.
Before use, put it in a chemically resistant glass container and boil for 5 min ~ 10 min. Cover it to cool to room temperature. Let it be standing for not more than 30 min.
C.3.2 In the analysis, unless otherwise specified, analytically pure or superior grade reagents are used. The bagged pH standard substance with certificate may be used according to the instruction manual. It may also be prepared according to the provisions of GB/T 9724.
C.4 Instruments and equipment
C.4.1 Analytical balance: Sensitivity 0.0001 g.
C.4.2 pH meter: measuring range, 0 ~ 14, accuracy 0.02.
C.4.3 Glass beaker: 100 mL.
C.4.4 Ultrasonic cleaning instrument: Ultrasonic power 240 W.
C.4.5 Measuring cylinder: Capacity 50 mL.
C.4.6 The test environment is free of pollution by chemical gas such as acid and alkali. During determination, the temperature of the specimen shall be consistent with that of the buffer solution.
C.5 Preparation of specimens
C.5.1 Weigh 5.00 g of specimen, accurate to 0.01 g. Place it in a 100 mL glass Appendix D
(Normative)
Method for determination of true density
D.1 Scope
This Appendix applies to the use of a true density tester to test the true density of the specimens.
D.2 Principle
True density refers to the density as obtained through dividing the powder mass (W) by the volume (true volume Vt) that does not include the voids inside and outside the particle. Place the sample material into the true density tester. Use helium as a medium. Gradually increase the pressure in the measurement
chamber to a specified value. Then the helium expands and enters the
expansion chamber. Use instrument to automatically record the equilibrium pressure of the two processes. According to the law of conservation of mass, after using the standard ball to calibrate the volume of the measurement chamber and the expansion chamber, determine the true volume of the sample material. Calculate the true density.
D.3 Reagents and materials
Helium, the purity of which is not less than 99.9%.
D.4 Instruments and equipment
D.4.1 True density tester.
D.4.2 Standard balls, the volume of which is about 7.0699 cm3, 70.699 cm3 respectively.
D.4.3 Series sample cells, the volume of which is about 10 cm3, 50 cm3, 135 cm3.
D.4.4 Electronic balance: The sensitivity is 0.0001 g.
D.5 Analytical procedures
D.5.1 Turn on the true density tester. Lead in the helium gas. Warm it up for 30 min. Check the air tightness of the gas path.
D.5.2 Before each test, use the standard ball to calibrate the instrument. Appendix E
(Normative)
Method for determination of interlayer spacing d002
E.1 Scope
This Appendix applies to the use of X-ray diffractometer to test the interplanar spacing d002 of the specimen.
E.2 Principle
The X-ray diffractometer automatically records the 002, 004, 110, 112 diffraction line patterns of carbon; simultaneously reads the diffraction angle (2??obs)c; uses the internal standard method to obtain the corrected diffraction angle (2??cor)c; uses the formula (E.1) to calculate the interlayer spacing d002 of the specimen. It is calculated according to the Bragg equation (E.1):
E.3 Reagents and materials
Single-crystal silicon powder: purity ??? 99.99%.
Use an agate mortar to pulverize it. Use the silica powder which all passes the 45 ??m (325 mesh) standard sieve as an internal standard substance for X-rays. E.4 Instruments and equipment
E.4.1 Automatic recording X-ray diffractometer, with copper target K?? X-ray. E.4.2 Electronic balance: The sensitivity is 0.0001 g.
E.4.3 Agate mortar.
E.5 Preparation of specimen
E.5.1 Weigh 1.5 g of silicon powder and 3.5 g of specimen (accurate to 0.0001 g). Place them in a mortar to grind it.
E.5.2 Add the ground and uniformly mixed sample to the groove of the sample holder. Use the slide to press it tightly and flatten it.
E.6 Analytical procedures
E.6.1 Place the sample holder on the test bench of the X-ray diffractometer. Appendix F
(Normative)
Method for determination of graphite orientation
F.1 Scope
This Appendix applies to the use of X-ray diffractometer to test the orientation of specimen.
F.2 Principle
Add the binder and thickener into the specimen. Stir to uniformly distribute it. Spread it on an aluminum foil. Dry it. After drying, scrape off the sample. Use an agate mortar to grind it finely. Make it pass through a 74 ??m (200 mesh) standard sieve. Use a compaction densitometer to compact the sample powder into the tablet of a predetermined size. After the tablet is rebounded for a certain period of time, measure the compaction density. Use the X-ray diffractometer to test the orientation.
The X-ray diffractometer automatically record the 002, 004, 110, 112 diffraction line patterns of the graphite samples. Read the heights of the 002, 004, 110 crystal plane diffraction peaks. Calculate the graphite orientations I002/I110 and I004/I110.
F.3 Reagents and materials
F.3.1 Binder: Styrene-butadiene rubber (SBR) powder, superior grade, model SN-307R, prepared with pure water to make 50% slurry.
F.3.2 Thickener: Sodium carboxymethylcellulose (CMC), analytically pure, model BVH8, prepared with pure water to make 1.2% solution.
F.3.3 Pure water: It meets the requirements of the grade-III water or above in the standard GB/T 6682.
F.3.4 Aluminum foil: The purity is more than 99.9%.
F.4 Instruments and equipment
F.4.1 Automatic recording type X-ray diffractometer, with copper target K?? X- ray.
F.4.2 Electronic balance: The sensitivity is 0.0001 g.
F.4.3 Agate mortar.
F.4.4 High-speed disperser, or other mixing-dispersing equipment.
F.4.5 Constant temperature drying oven, with a working temperature above 95 ??C.
F.4.6 Compaction densitometer, with a maximum pressure of more than 25 kN. F.4.7 Standard screen, 74 ??m (200 mesh).
F.4.8 Thickness gauge.
F.4.9 Dryer.
F.5 Preparation of specimen
F.5.1 Weigh 19.3 g of specimen, 25.0 g of thickener (see F.3.2), 0.8 g of binder (see F.3.1) in a clean plastic container, accurate to 0.0001 g.
F.5.2 Use a high-speed disperser or other stirring-dispersing equipment to disperse the above mixed sample fully and uniformly. Then uniformly spread it on aluminum foil (see F.3.4). Place it in a constant temperature drying oven. Dry it at 95 ??C for more than 6 h.
F.5.3 Scrape off the dried sample into agate mortar. Fully grind it finely. Make it pass through a standard sieve of 74 ??m (200 mesh).
F.5.4 Weigh 4 parts of the ground and sieved sample 0.50 g ?? 0.001 g, accurate to 0.0001 g. Respectively, place them in the mold of the compaction
densitometer. Respectively at the pressure of 2.5 kN, 5.0 kN, 14.5 kN, 24.5 kN, prepare it into tablet. The pressure is held for 30 s.
F.5.5 The prepared 4 tablets are separately packed in a clean sample bag and placed in a desiccator. Avoid the tablet from bearing pressure. Let it be standing for 16 h. Then take out the tablet. Use the thickness gauge to test the thickness of the tablet. Calculate the compaction density of each tablet. Take records. After finishing the test of compaction density of tablet, test the orientation within 8 h. Otherwise, it shall re-prepare the tablet.
F.6 Analytical procedures
F.6.1 Place the tablet that has been allowed to stand, tested, recorded of compaction density into the X-ray diffractometer-specific sample holder, to make the upper surface of the tablet be in the same plane as the upper surface of the sample holder. Fix the sample holder onto the sample bench of X-ray diffractometer. Align the position of the sample holder, to make the tablet be in the center of the sample bench.
F.6.2 Set the starting angle of scan to 10??, the end angle to 90??, the step size Appendix G
(Normative)
Method for determination of first coulomb efficiency and first discharge specific capacity
G.1 Scope
This Appendix applies to the use of the battery tester to test the first discharge specific capacity and the first charge specific capacity of the sample. G.2 Method and summary
G.2.1 First Coulomb efficiency: Use the metal lithium as the electrode. At 23 ??C ?? 2 ??C, carry out test according to the operating procedures of battery charge- discharge test instrument. The tested half-cell discharge specific capacity (delithiation) is divided by the charge specific capacity (lithium intercalation) to obtain the coulombic efficiency.
G.2.2 First discharge specific capacity (delithiation): Use the metal lithium as the electrode. At 23 ??C ?? 2 ??C, follow the operating procedures of battery charge-discharge test instrument to test the half-cell discharge specific capacity (delithiation).
G.3 Reagents and materials
G.3.1 Conductive agent: Acetylene black (according to GB/T 3782) or
conductive carbon black of the same performance.
G.3.2 Binder: SBR powder, superior grade, model SN-307R or binder of
equivalent performance.
G.3.3 Graphite current collector: Copper foil (according to GB/T 5187) or the current collector of same performance.
G.3.4 Lithium current collector: Nickel mesh (according to GB/T 3120) or the current collector of same performance.
G.3.5 Metal lithium strip or lithium tape (according to GB/T 4369).
G.4 Instruments and equipment
G.4.1 Battery tester: (Current accuracy: 0.1% RD + 0.1% FS; voltage accuracy: 0.1% RD + 0.1% FS) or the tester of same type.
G.4.2 Analog battery: Closed system, battery mold of PTFE or equivalent type of (such as button battery).
G.4.3 Glove box: 20 ??C constant temperature, one standard atmospheric
pressure, 99.999% inert gas, H2O ??? 1 ppm, O2 ??? 1 ppm or the glove box of same type.
G.4.4 Vacuum drying oven (accuracy: vacuum < 100 Pa, temperature range
50 ??C ~ 250 ??C) or the drying oven of same type.
G.4.5 Air drying oven: (10 ??C ~ 250 ??C) or the drying oven of same type. G.4.6 Drying vessel: Relative humidity < 25% or the drying vessel of same type. G.4.7 Balance: Sensitivity of 0.00001g or balance of the same type.
G.4.8 Paddle type agitator: 3000 r/min or the agitator of same type.
G.4.9 Coating applicator (specification 200 ??m): 3000 r/min or the applicator of same type.
G.5 Preparation of specimens
The specimen is prepared in a dry room at a temperature of 23 ??C ?? 2 ??C and dew point < -30 ??C.
G.5.1 Follow the sampling rule in the sampling method of (7.1) to take specimen and conductive agent. Place the specimen and the conductive agent into a vacuum oven. Bake it at 120 ??C for 4 h. Then transfer it in a drying vessel to cool it down. Then at the mass ratio of specimen : binder : conductive agent = 92:5:3, weigh 9.5 g of the mixed powder of the specimen and conductive agent (accurate to 0.00001 g).
G.5.2 Add the powder of the mixture of specimen and conductive agent to a 40 mL small beaker. Then add the N-methyl-2-pyrrolidone solution (H2O ??? 10 ppm) with a concentration of 5% binder. Use the paddle type stirrer to prepare it into a paste (stirring time 30 min, stirring speed 1500 r/min).
G.5.3 Spread the paste evenly on the copper foil. Use the 200 ??m applicator to scrape the paste onto the copper foil, until the surface is smooth. Then place it in a forced air oven to bake it at 100 ??C for 8 h.
G.5.4 The baked electrode pieces are cut and pressed into various shapes of electrodes (rectangular strips, strips or circles, etc.). Accurately weigh it. Place it in a vacuum drying oven. Under vacuum conditions, bake it at 100 ??C for 8 h, to obtain a working carbon electrode.
G.5.5 In a glove box under an argon atmosphere, cut the metal lithium into strip or belt. Then press the above-mentioned cut metal lithium to the end of the Appendix H
(Normative)
Method for determination of trace metal elements
H.1 Scope
This Appendix is applicable to the use of inductively coupled plasma emission spectrometer to test the content of trace metals such as iron, sodium, chromium, copper, nickel, aluminum, molybdenum, cobalt, zinc in the specimen.
H.2 Principle
After adding the sample to aqua regia (concentrated HNO3: concentrated HCl, volume ratio 1:3), use a microwave digestion instrument to dissolve it. After filtration and reaching to certain volume, in an acidic medium, under the selected optimal conditions, respectively determine the intensity of the emitted light on the inductively coupled plasma emission spectrometer.
H.3 Reagents and materials
The water used in this Appendix shall meet the requirements of grade-I water in GB/T 6682.
H.3.1 Nitric acid: Grade-GR.
H.3.2 Hydrochloric acid: Grade-GR.
H.3.3 Argon: Purity 99.999%.
H.3.4 Prepare the f...

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