CN113093029B - Test method for testing lithium precipitation amount of lithium ion battery cathode based on ICP method - Google Patents
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Abstract
The invention discloses a method for testing lithium precipitation amount of a lithium ion battery cathode based on an ICP method. The method comprises the following specific steps: firstly, disassembling a test battery after the test battery is fully charged under the test condition to be evaluated; taking a fresh battery at 0.1C or 0.2C, fully charging, then disassembling the fresh battery, and taking a negative plate with the same length as a sample to be tested as a reference sample; secondly, respectively carrying out powder scraping digestion constant volume treatment on the sample to be tested and the reference sample; measuring the content of lithium element in the treated sample; and thirdly, dividing the sample lithium element content obtained in the second step by the sample constant current charging capacity to obtain the lithium element content corresponding to the sample Ah constant current capacity, deducting the test sample by using a reference sample without lithium precipitation to obtain the relative lithium precipitation amount of the negative electrode of the test battery, and considering that the lithium precipitation occurs to the negative electrode of the battery to be tested when the relative lithium precipitation amount of the negative electrode is more than 0.05%.
Description
Technical Field
The invention relates to the field of lithium ion batteries, and relates to a method for testing lithium separation amount of a lithium ion battery cathode based on an ICP method.
Background
Based on market demand, the main direction of current lithium ion battery technology research and development is the improvement of energy density and quick charging capability. It is highly desirable for end users to combine the high energy density and fast charging capability of batteries, which is a key technical problem in battery development. However, one of the risks associated with rapid charging is lithium extraction.
It is well known that lithium ion batteries are designed based on lithium intercalation and deintercalation reactions, but when the negative electrode current is too large or the temperature is too low, the negative electrode potential is lower than Li/Li ＋ When the potential of the electrode is referenced, lithium metal is deposited on the surface of the negative electrode. The performance and safety of the lithium ion battery are seriously influenced by the lithium separation of the negative electrode. At present, for the observation of lithium precipitation of batteries, the conventional method is to disassemble the batteries and then observe whether metallic lithium exists on the surfaces of the batteries according to experience to judge. The method is direct and needs short time. However, this visual observation method cannot identify and quantify the sample in which lithium deposition occurs to a low degree.
Disclosure of Invention
In view of the above, the present invention provides a method for testing lithium deposition amount of a negative electrode of a lithium ion battery based on an ICP method, which includes the following steps:
the first step is as follows: obtaining a sample to be tested and a reference sample
The test battery is disassembled after being fully charged under the test condition to be evaluated, and a cathode piece with a certain length (2 cm-10 cm) is taken as a sample to be tested; taking a fresh battery (the same batch as a battery to be tested) and disassembling the fresh battery (the same charge state as the battery to be tested) after the fresh battery is fully charged (the charge state is the same as the charge state of the battery to be tested) at a small multiplying power (0.1C or 0.2C, and the normal-temperature charging at the current is considered that the battery does not generate lithium separation), and taking a negative plate with the same length as the sample to be tested as a reference sample; during the period, data such as time, voltage, current, capacity and the like in the battery charging process are collected.
The second step is that: processing a test sample and measuring the content of lithium element
Step 1) respectively scraping powder on the sample to be tested and the reference sample obtained in the first step, respectively placing the scraped active substances in different beakers for weighing and recording the mass of the active substances;
step 2) sample digestion constant volume treatment: adding a certain amount of hydrochloric acid, nitric acid and a certain amount of deionized water into the beaker obtained in the step 1) to carry out heating digestion treatment on the beaker, and carrying out filtration and volume fixing after cooling;
step 3) measuring the content of lithium element in the sample after the digestion treatment
Measuring the content of lithium element in the solution after constant volume by using an inductively coupled plasma emission spectrometer (ICP), and recording the test result as X1; finally, the content of lithium element contained in the sample is X2= X1N/m, wherein m is the mass of the active substance in the step 1) of the second step and is given in g; n is the final volume of constant volume;
the third step: data processing and determination
And because lithium separation occurs in the constant current stage, the lithium element content X2 of the sample obtained in the second step is divided by the constant current charging capacity of the sample to obtain the lithium element content X3 corresponding to the constant current capacity of the Ah unit of the sample, finally the test sample is deducted by a reference sample without lithium separation to obtain the relative lithium separation amount X of the negative electrode of the test battery, and when the relative lithium separation amount of the negative electrode is more than 0.05%, the negative electrode of the test battery is considered to have lithium separation.
The beneficial effects of the invention are: the method is more direct, the required time is shorter, and the method is easy to identify samples with lower lithium analysis degree.
Detailed Description
The present invention will be described in detail below with reference to the accompanying table, taking a commercial cylindrical lithium ion battery as an example, to further illustrate the substantial features and significant progress of the present invention.
Example 1
In this example, the test sample is a 21700 cylindrical lithium ion experimental battery, the 1C capacity is 4.8Ah, the condition to be evaluated is 0.5C =2.4A, and whether the sample is subjected to lithium deposition or not is observed by charging at the current.
The battery testing device is a conventional charging and discharging instrument, and the device adopted in the embodiment is an Arbin BT2000 charging and discharging testing system.
The first step is as follows: obtaining a test sample and a reference sample
Disassembling the test battery after the test battery is fully charged with 2.4A current, and taking a negative plate with the length of 10cm +/-2 cm as a test sample to be tested; taking a fresh battery (the same batch as the battery to be tested) and disassembling the fresh battery (the same charge state as the battery to be tested) after the fresh battery is fully charged (the charge state is the same as the charge state of the battery to be tested) at 0.1C =0.480A (the lithium cannot be separated out due to normal-temperature charging at the current), and taking a negative plate with the same length as the sample to be tested as a reference sample; during the period, data such as time, voltage, current, capacity and the like in the battery charging process are collected. Wherein the constant current capacity of the test sample: q (sample) =3.181Ah
Q (reference) =3.934 Ah.
The second step: processing a test sample and measuring the content of lithium element
1) Respectively scraping the powder of the sample to be detected and the reference sample obtained in the first step, respectively placing the scraped active substances into different beakers for weighing, and recording the mass of the active substances, wherein the mass is 0.9400g and 0.9010 g.
2) Sample digestion constant volume treatment: adding 4.5ml of hydrochloric acid, 1.5ml of nitric acid and 25ml of deionized water into the beaker in the step 1) to carry out heating digestion treatment on the mixture, and carrying out filtration and constant volume dilution treatment after cooling; the final volume was 10000 ml.
3) Measuring the content of lithium element in the digested sample
Respectively measuring the content of lithium element in the to-be-measured solution and the reference solution after constant volume by using an inductively coupled plasma emission spectrometer (ICP), wherein the test results X1 (to be measured) = 8.2040ppm and X1 (reference) =7.9470 ppm; the final sample contained elemental lithium content X2= X1 × N/m, where m is the mass of the active substance in the second step 1), in g; n is the final volume of constant volume; by calculation, X2 (to be measured) =87276.6 ppm, X2 (reference) = 88202.2 ppm.
The third step: data processing and determination
Because the lithium analysis occurs in the constant current stage, the lithium element content data X2 is divided by the constant current capacity of the corresponding sample to obtain the lithium content X3 corresponding to the constant current capacity of the sample unit Ah, namely
X3 (test) =87276.6/3.181 × 0.000001=2.744%,
x3 (reference) =88202.0/3.934 × 0.000001=2.242%
Finally, the test sample is deducted by a reference sample without lithium precipitation to obtain the relative lithium precipitation amount of the negative electrode of the test battery
X = X3 (test) -X3 (reference) =2.744% -2.242% =0.502%
And X is more than 0.05 percent, so that the lithium precipitation of the negative electrode of the battery to be detected is carried out, and the lithium precipitation amount is 0.502 percent.
Claims (2)
1. A test method for testing lithium analysis amount of a lithium ion battery cathode based on an ICP method is characterized in that the method judges whether the battery generates lithium analysis under the test condition to be evaluated, and the test method comprises the following steps:
the first step is as follows: obtaining a sample to be tested and a reference sample
The test battery is disassembled after being fully charged under the test condition to be evaluated, and a negative plate with the length of 2cm-10cm is taken as a sample to be tested; taking a fresh battery with the same batch as the battery to be tested, fully charging the fresh battery at 0.1C or 0.2C, disassembling the fresh battery, and taking a negative plate with the same length as the sample to be tested as a reference sample;
the second step is that: processing a sample to be tested and determining the content of lithium element
Step 1) respectively scraping powder on the sample to be tested and the reference sample obtained in the first step, respectively placing the scraped active substances in different beakers for weighing and recording the mass of the active substances;
step 2), sample digestion and volume fixing treatment: adding 3ml-6ml of hydrochloric acid, 1ml-3ml of nitric acid and 20ml-30ml of deionized water into the beaker in the step 1) to perform heating digestion treatment, cooling, filtering and fixing the volume;
step 3) measuring the content of lithium element in the sample after the digestion treatment
Measuring the content of lithium element in the solution after constant volume by using an inductively coupled plasma emission spectrometer, and recording the test result as X1; the final sample contained elemental lithium content X2= X1 × N/m, where m is the mass of the active substance in step 1) of the second step in g; n is the final volume of constant volume;
the third step: data processing and determination
Because lithium is separated in a constant current stage, the sample lithium element content X2 obtained in the second step is divided by the sample constant current charging capacity to obtain the lithium element content X3 corresponding to the constant current capacity of the Ah unit of the sample, finally the test sample is deducted by a reference sample without lithium separation to obtain the relative lithium separation amount of the negative electrode of the test battery, and when the relative lithium separation amount of the negative electrode is more than 0.05%, the lithium separation of the negative electrode of the battery to be tested is considered.
2. The ICP method-based test method for testing lithium evolution quantity of the negative electrode of the lithium ion battery according to claim 1, wherein the test conditions to be evaluated in the first step further comprise large-current charging, low-temperature charging and cycle testing.
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| CN113740404B (en) * | 2021-09-03 | 2023-10-27 | 厦门厦钨新能源材料股份有限公司 | Method for nondestructively evaluating lithium cobalt molar ratio in lithium battery electrode |
| CN115840020A (en) * | 2021-09-18 | 2023-03-24 | 北京昇科能源科技有限责任公司 | Method for detecting lithium analysis content of lithium ion battery |
| CN114184964B (en) * | 2021-12-08 | 2023-08-29 | 蜂巢能源科技(无锡)有限公司 | Method and device for evaluating internal temperature distribution of battery cell |
| CN114426312B (en) * | 2022-01-13 | 2024-06-25 | 南京同宁新材料研究院有限公司 | Method for preparing high-pressure lithium cobaltate by utilizing waste lithium cobaltate |
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