Method for determining aluminum, zirconium in ternary material

Abstract

The present disclosure provides a method for determining aluminum and zirconium in ternary materials, and relates to the technical field of lithium batteries. The method for determining aluminum and zirconium in ternary materials comprises the following steps: adding fluoroboric acid solution and hydrochloric acid solution into the ternary material to be measured to obtain a sample to be measured; heating and digesting the sample to be measured on an electric hot plate to obtain a digested sample; and using an inductively coupled plasma emission spectrometer to determine the content of aluminum and zirconium in the digested sample. The method uses fluoroboric acid / hydrochloric acid as a digestion system and adopts an electric hot plate for digestion. The digestion method is easy to operate, and the obtained digestion product is clear and free of insoluble substances, so that accurate determination of aluminum and zirconium can be achieved.

Description

Technical Field

[0001] This disclosure relates to the field of lithium battery technology, and in particular to a method for determining aluminum and zirconium in ternary materials. Background Technology

[0002] With the increasing prominence of energy and environmental issues, lithium-ion batteries, due to their superior performance and environmental friendliness, are widely used in portable electronic products, electric vehicles, and energy storage. The cathode material is a key raw material in lithium-ion batteries, and its quality significantly impacts battery performance. Lithium-ion battery materials mainly include nickel-cobalt-manganese ternary materials, lithium iron phosphate, and lithium nickel oxide. In recent years, ternary materials have been widely used due to their high energy density. Currently, in the production process of nickel-cobalt-manganese ternary materials, aluminum and zirconium compounds are often used for coating and doping to improve the structural stability of the ternary material and enhance its electrochemical performance after being made into a battery cell. To accurately characterize the coating and doping effect of ternary materials, it is necessary to test the elemental content of aluminum and zirconium in the ternary material.

[0003] However, the current industry practice for testing the aluminum and zirconium content in nickel-cobalt-manganese ternary materials typically follows the People's Republic of China Nonferrous Metals Industry Standard YS / T 1006.2-2014. This involves weighing the sample into a beaker, adding hydrochloric acid, heating to dissolve, cooling, transferring to a volumetric flask, diluting with water to the mark, mixing thoroughly, and then using ICP-OES (Inductively Coupled Plasma Optical Emission Spectrometry) to determine the elemental content. This method cannot completely digest the sample, and the digestion products often contain insoluble substances, leading to inaccurate test results. Furthermore, the insoluble substances in the digestion products can easily clog the ICP-OES sample introduction system, affecting the instrument's lifespan.

[0004] It should be noted that the information disclosed in the background section above is only used to enhance the understanding of the background of this disclosure, and therefore may include information that does not constitute prior art known to those skilled in the art. Summary of the Invention

[0005] To address the aforementioned technical problems, this disclosure provides a method for determining aluminum and zirconium in ternary materials.

[0006] This disclosure provides a method for determining aluminum and zirconium in ternary materials, including:

[0007] Fluoroboric acid solution and hydrochloric acid solution were added to the ternary material to be tested to obtain the test sample;

[0008] The sample to be tested is heated and digested on a hot plate to obtain a digested sample;

[0009] The aluminum and zirconium content in the digested sample was determined using inductively coupled plasma atomic emission spectrometry.

[0010] In one exemplary embodiment of this disclosure, the mass concentration of the fluoroboric acid solution is 8-20%.

[0011] In one exemplary embodiment of this disclosure, the volume ratio of the fluoroboric acid solution to the hydrochloric acid solution is 1 to 6:10.

[0012] In an exemplary embodiment of this disclosure, the step of heating and digesting on a hot plate includes: placing the sample to be tested on the hot plate and digesting it at 200-240°C for 20-80 minutes.

[0013] In an exemplary embodiment of this disclosure, the ratio of the ternary material to the hydrochloric acid solution in the sample to be tested is 3-5 g: 100 mL.

[0014] In one exemplary embodiment of this disclosure, the step of determining the aluminum and zirconium content in the digested sample using an inductively coupled plasma atomic emission spectrometer includes:

[0015] Prepare a series of aluminum zirconium standard solutions with gradient concentrations, wherein the volume of the aluminum zirconium standard solution is V;

[0016] Add diluent to the digested sample and bring the volume to V.

[0017] The aluminum and zirconium standard solutions were measured using inductively coupled plasma atomic emission spectrometry to obtain standard curves for aluminum and zirconium.

[0018] The digested sample after volume adjustment was measured using inductively coupled plasma atomic emission spectrometry (ICP-AES) to obtain the test results.

[0019] The digestion sample was obtained based on the test results and the aluminum and zirconium standard curves.

[0020] In one exemplary embodiment of this disclosure, both the aluminum zirconium standard solution and the digestion sample contain an internal standard solution.

[0021] In one exemplary embodiment of this disclosure, the internal standard solution is selected from one or more of scandium standard solution, germanium standard solution, yttrium standard solution, indium standard solution and bismuth standard solution.

[0022] In one exemplary embodiment of this disclosure, the aluminum zirconium standard solution contains the fluoroboric acid solution and the hydrochloric acid solution.

[0023] In an exemplary embodiment of this disclosure, the ternary material to be tested includes lithium nickel cobalt manganese oxide doped with metal element M1 and / or lithium nickel cobalt aluminum oxide doped with metal element M2, wherein M1 includes at least one of Al and Zr; and M2 includes at least Zr.

[0024] The beneficial effects of the method for determining aluminum and zirconium in ternary materials according to the embodiments of this disclosure are:

[0025] The method disclosed herein employs plate digestion using a hot plate. The digestion process is simple, convenient, and suitable for high-volume testing scenarios, offering high detection efficiency. During plate digestion, fluoroboric acid / hydrochloric acid is used as the digestion system, resulting in a clear digestion product free of insoluble matter and demonstrating good digestion efficiency. This method can accurately determine aluminum and zirconium in ternary materials, and the method is stable and reliable, with a recovery rate of 90–110% and a repeatability RSD within 0.5%.

[0026] It should be understood that the above general description and the following detailed description are exemplary and explanatory only, and are not intended to limit this disclosure. Attached Figure Description

[0027] To more clearly illustrate the technical solutions of the embodiments of this disclosure, the accompanying drawings used in the embodiments will be briefly described below. It should be understood that the following drawings only show some embodiments of this disclosure and should not be regarded as a limitation of the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.

[0028] Figure 1 This is a flowchart of a method for determining aluminum and zirconium in ternary materials according to an embodiment of this disclosure.

[0029] Figure 2 This is the standard curve of Al element obtained in Example 1.

[0030] Figure 3 This is the standard curve of Zr element obtained in Example 1.

[0031] Figure 4 This is a photograph of the digestion sample obtained in Experiment 3, number 7, under laser irradiation.

[0032] Figure 5 This is a photograph of the digestion sample obtained in Experiment 3, number 12, under laser irradiation.

[0033] Figure 6 This is a photograph of the digestion sample obtained in Experiment 3, number 10. Detailed Implementation

[0034] To make the objectives, technical solutions, and advantages of the embodiments of this disclosure clearer, the technical solutions in the embodiments of this disclosure will be clearly and completely described below. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall apply. Reagents or instruments whose manufacturers are not specified are all conventional products that can be purchased commercially.

[0035] The method for determining aluminum and zirconium in ternary materials according to embodiments of this disclosure will be described in detail below.

[0036] This disclosure provides a method for determining aluminum and zirconium in ternary materials, comprising:

[0037] Step S1: Add fluoroboric acid solution and hydrochloric acid solution to the ternary material to be tested to obtain the test sample;

[0038] Step S2: The sample to be tested is heated and digested on a hot plate to obtain a digested sample;

[0039] Step S3: Use inductively coupled plasma atomic emission spectrometry to determine the content of aluminum and zirconium in the digested sample.

[0040] Existing technologies typically employ microwave digestion for sample pretreatment. Because microwave digestion is performed in a high-temperature, high-pressure environment, the requirements for digestion reagents are relatively low. However, microwave digestion demands sophisticated equipment and is complex and cumbersome to operate, making it unsuitable for large-scale operations. The method for determining aluminum and zirconium in ternary materials disclosed in this disclosure uses hot plate digestion, which has lower equipment requirements, is simple and convenient to operate, and is more suitable for large-scale detection scenarios, enabling efficient detection of large batches of samples. Using fluoroboric acid / hydrochloric acid as the digestion system, the digestion products of the clarified and insoluble substances can be obtained through plate digestion, thereby achieving accurate determination of aluminum and zirconium in ternary materials.

[0041] Specifically, in the embodiments of this disclosure, the ternary material to be tested includes lithium nickel cobalt manganese oxide doped with metal element M1 and / or lithium nickel cobalt aluminum oxide doped with metal element M2, wherein M1 includes at least one of Al and Zr; and M2 includes at least Zr.

[0042] Specifically, in one embodiment, the ternary material to be tested is lithium nickel cobalt manganese oxide doped with metal element M1, wherein M1 includes at least one of Al and Zr. The ternary material to be tested may also be doped with other elements besides M1, which is not specifically limited in this disclosure.

[0043] Specifically, in another embodiment, the ternary material to be tested is nickel-cobalt doped with the metal element M2; lithium aluminate, wherein M2 includes at least one of Zr. The ternary material to be tested may also be doped with other elements besides M2, which is not specifically limited in this disclosure.

[0044] It should be noted that the ternary material to be tested can be coated or doped to introduce metal elements M1 or M2, and this disclosure does not impose specific restrictions.

[0045] In the embodiments of this disclosure, in step S1, fluoroboric acid solution and hydrochloric acid solution are added to the ternary material to be tested to obtain the test sample.

[0046] Specifically, in this step, the mass concentration of the fluoroboric acid solution is 8-20%. More preferably, the mass concentration of the fluoroboric acid solution is 10-15%. Specifically, a commercially available 50wt% fluoroboric acid aqueous solution can be purchased and diluted with ultrapure water to obtain a fluoroboric acid solution of the predetermined concentration.

[0047] Specifically, in this step, the hydrochloric acid solution has a mass concentration of 20%–40%, for example, concentrated hydrochloric acid with a mass concentration of 36%–38% can be used as the hydrochloric acid solution. Using a fluoroboric acid-hydrochloric acid digestion system can achieve better digestion results, resulting in more thorough digestion of aluminum and zirconium, and more accurate detection results.

[0048] Furthermore, in one embodiment of this disclosure, the volume ratio of the fluoroboric acid solution to the hydrochloric acid solution is 1–6:10. More preferably, the volume ratio of the fluoroboric acid solution to the hydrochloric acid solution is 4–6:10. At this ratio, the mixed acid system formed by the fluoroboric acid solution and the hydrochloric acid solution can completely digest the ternary material, thereby ensuring the accuracy of the test results.

[0049] Specifically, in this step, the fluoroboric acid solution and hydrochloric acid solution can be added in batches, or the fluoroboric acid solution and hydrochloric acid solution can be mixed first and then added to the ternary material to be tested. More preferably, in this embodiment, the fluoroboric acid solution is added to the ternary material first, followed by the hydrochloric acid solution, to obtain the sample to be tested.

[0050] Specifically, in this step, the ratio of ternary material to hydrochloric acid solution in the sample to be tested is 3-5 g: 100 mL, and the ratio of ternary material to fluoroboric acid solution is 3-5 g: 50 mL. That is, 3-5 g of ternary material is added to 100 mL of hydrochloric acid solution and 50 mL of fluoroboric acid solution. The ratio of sample volume to digestion reagent volume will affect the digestion effect. If the amount of digestion reagent is too small, the sample cannot be completely digested; if the amount of digestion reagent is too large, it will be wasteful. In addition, the higher the sample volume, the higher the element concentration in the sample to be tested, and the better the test stability; secondly, the larger the sample volume, the better the representativeness of the sample.

[0051] In step S2, the sample to be tested is heated and digested on a hot plate to obtain a digested sample.

[0052] Furthermore, this step specifically includes: placing the sample to be tested on a hot plate and digesting it at 200–240°C for 20–80 minutes. For example, an electrically heated constant temperature platform device can be used for safe digestion. During operation, it is only necessary to place the sample to be tested on the heated plate and adjust the temperature and time, making the operation convenient.

[0053] More preferably, the digestion time is 30–40 minutes. When the digestion time reaches 30 minutes or more, complete digestion of Al and Zr can be achieved.

[0054] In step S3, the aluminum and zirconium content in the digested sample is determined using inductively coupled plasma optical emission spectrometry (ICP-OES). In one embodiment, step S3 specifically includes:

[0055] S31, Prepare a series of aluminum zirconium standard solutions with gradient concentrations, wherein the volume of the aluminum zirconium standard solution is V;

[0056] S32, add diluent to the digested sample and bring the volume to V;

[0057] S33, ICP-OES was used to determine the aluminum-zirconium standard solutions to obtain aluminum and zirconium standard curves respectively;

[0058] S34, The digested sample after volume adjustment is measured using ICP-OES to obtain the test results;

[0059] S35. Based on the test results and the aluminum and zirconium standard curves, the digestion sample is obtained.

[0060] In one embodiment of this disclosure, both the aluminum zirconium standard solution and the digestion sample contain an internal standard solution.

[0061] Furthermore, the internal standard solution is selected from one or more of scandium standard solution, germanium standard solution, yttrium standard solution, indium standard solution, and bismuth standard solution. Preferably, in this embodiment, the internal standard solution is a Sc standard solution. Using Sc as the internal standard allows for the calibration of the analyte content, compensating for non-spectral interference caused by the matrix solution. This corrects for the influence of factors such as solvent, operational error, and instrument drift on the test results, improving the accuracy of the detection results.

[0062] Furthermore, fluoroboric acid solution and hydrochloric acid solution are added to the aluminum zirconium standard solution. By adding fluoroboric acid solution and hydrochloric acid solution to the standard solution, the solvent composition of the standard solution and the test sample is kept consistent, reducing interference. Specifically, fluoroboric acid solution and hydrochloric acid solution are added to the standard solution in a volume ratio of 1–2:8–10. The amount of hydrochloric acid solution added is approximately equal to that of the test sample.

[0063] Specifically, in step S31, the preparation process of the aluminum-zirconium standard solution is as follows: A certain amount of fluoroboric acid solution and hydrochloric acid solution (volume ratio 1-2:8-10) are added to a volumetric flask; a certain volume of scandium standard solution (concentration 100 μg / mL) is added; and a certain volume of aluminum standard solution (concentration 1000 μg / mL) and zirconium standard solution (concentration 1000 μg / mL) are added. The solution is then diluted to volume V with ultrapure water to obtain a gradient series of standard solutions. Specifically, the volume V can be 50 mL, 100 mL, 500 mL, etc.

[0064] Furthermore, in one specific embodiment, the concentration of scandium in the aluminum-zirconium standard solution is 0.2–1 μg / mL. The concentration gradients of aluminum in the aluminum-zirconium standard solution are 0, 2 μg / mL, 8 μg / mL, and 14 μg / mL; the concentration gradients of zirconium are 0, 4 μg / mL, 10 μg / mL, and 16 μg / mL.

[0065] Specifically, in step S32, the volume adjustment process for the digested sample is as follows: the digested sample is transferred to a volumetric flask, washed several times with ultrapure water during the transfer, a certain volume of scandium standard solution (concentration 100 μg / mL) is added, and the volume is adjusted to volume V with ultrapure water. That is, the adjusted volume of the digested sample is consistent with that of the aluminum zirconium standard solution. Furthermore, the concentration of scandium in the digested sample after volume adjustment is consistent with that of the aluminum zirconium standard solution.

[0066] Specifically, in steps S33 and S34, the operating conditions of ICP-OES are as follows: the analysis wavelength for aluminum is 396.153 nm, the analysis wavelength for zirconium is 343.823 nm, and the analysis wavelength for scandium is 361.384 nm.

[0067] Specifically, the instrument operating conditions of ICP-OES can be set as follows: argon plasma source, power 1150W, nebulizer flow rate 0.70L / min, auxiliary gas flow rate 0.5L / min, and observation height 12mm.

[0068] The features and performance of this disclosure will be further described in detail below with reference to embodiments.

[0069] Example 1

[0070] This embodiment provides a method for determining Al and Zr in ternary materials, comprising the following steps:

[0071] (1) Prepare the sample to be tested: Weigh 0.4 ± 0.0004 g of the sample to be tested into a 150 mL polytetrafluoroethylene beaker. The sample to be tested is an Al and Zr doped nickel-cobalt-manganese ternary material.

[0072] (2) Preparation of fluoroboric acid solution: Add 1L of 50% fluoroboric acid and 4L of ultrapure water to a 5L solution bottle, mix well, and prepare a 10wt% fluoroboric acid solution.

[0073] (3) Sample digestion: Add 5 mL of 10 wt% fluoroboric acid solution and 10 mL of 37 wt% hydrochloric acid solution to the sample to be tested in step (1); place it on a hot plate and digest at 220℃ for 30 min to obtain a digested sample. The digested sample is clear and has no insoluble precipitate.

[0074] (4) Prepare sample solution: Transfer the digested sample obtained in step (3) to a 100 mL plastic volumetric flask, washing it at least 3 times during the transfer. Add 0.5 mL of scandium standard stock solution (concentration 100 μg / mL), and make up to 100 mL. Shake well and set aside.

[0075] (5) Preparation of standard solutions: Prepare four 100mL plastic volumetric flasks. Add 10mL of 37wt% hydrochloric acid solution and 2mL of 10wt% fluoroboric acid to each flask, and add 0.5mL of scandium standard stock solution (concentration 100μg / mL). Add 0, 0.2, 0.8, and 1.4mL of aluminum standard stock solution (concentration 1000μg / mL) and 0, 0.4, 1.0, and 1.6mL of zirconium standard stock solution (concentration 1000μg / mL) to each volumetric flask, respectively. Dilute to 100mL with ultrapure water and mix well.

[0076] (6) Using the instrument operating conditions described above, ICP-OES was used to test the standard solution prepared in step (5). Based on the ratio of the emission intensity of Al, Zr and the internal standard Sc and their concentration ratio, standard curves for Al and Zr were plotted. Figure 2 The image shows the standard curve of the Al element. Figure 3 The figure shown is the standard curve of Zr element obtained by plotting.

[0077] (7) The sample solution prepared in step (4) was tested using ICP-OES to obtain the test results. The test results were then substituted into the standard curves of Al and Zr elements to calculate the Al and Zr content of the sample to be tested.

[0078] Experimental Example 1: Spiked Recovery and Repeatability Test

[0079] Following the determination procedure in Example 1, a spiked recovery experiment was performed on one of the test samples. The experimental results are shown in Table 1 below:

[0080] Table 1

[0081]

[0082]

[0083] Following the steps in Example 1, another sample was tested repeatedly, and the test results are shown in Table 2 below:

[0084] Table 2

[0085]

[0086]

[0087] As can be seen from Tables 1 and 2, the methods for determining Al and Zr provided in this embodiment have recovery rates between 90% and 110%, and the repeatability level RSD can reach below 0.5%. The scheme is reliable and the measurement results are highly accurate.

[0088] Test Example 2: Digestion Equipment Test

[0089] The same test samples were selected and digested using different heating devices. The experimental group used a hot plate heating device, while the control group used a voltage-regulating electric furnace heating device. The digestion conditions for the voltage-regulating electric furnace were 150V for 30 minutes, and for the hot plate, the conditions were 200℃ for 30 minutes. After digestion, the digested samples after standing for 18 hours and after shaking were tested, respectively. The testing process was carried out in accordance with the steps in Example 1. The experimental results are shown in Table 3 below:

[0090] Table 3

[0091]

[0092]

[0093] During the experiment, it was found that in the control group, when using a voltage-regulating electric furnace for digestion, the measurement results of multiple parallel digestion samples differed significantly. This may be due to the large temperature difference at different locations of the voltage-regulating electric furnace, with some samples having higher temperatures, causing the digestion reagent to evaporate too quickly, resulting in a short time and poor effect on the sample, thus leading to incomplete digestion and lower test results.

[0094] Furthermore, as shown in Table 3, there is a significant difference between the test results of the digested sample after standing and the test results after shaking. This indicates that there are Al-containing insoluble substances in the digested sample, and these insoluble substances settle over time, leading to the large differences in the test results.

[0095] In the experimental group, digestion was performed using a hot plate. The measurement results among the parallel digested samples showed almost no difference, indicating precise temperature control during hot plate digestion and that the digestion process for each parallel sample was kept under identical conditions. Furthermore, as shown in Table 3, the test results of the digested samples after standing were very similar to those after shaking, demonstrating that hot plate digestion is extremely effective and produces no insoluble precipitates.

[0096] Experimental Example 3: Digestion Reagent Test

[0097] A 0.4g sample of ternary material doped with aluminum and zirconium was weighed and digested using different digestion reagents. The digestion conditions were: using a hot plate at 200℃ for 30 minutes. After digestion, the state of the digested sample was observed. The experimental results are shown in Table 4.

[0098] Table 4

[0099]

[0100]

[0101] As can be seen from Table 4, increasing the amount of hydrochloric acid added has little effect on the digestion effect; using hydrochloric acid-hydrogen peroxide system, nitric acid, nitric acid-fluoroboric acid, nitric acid-hydrogen peroxide system, aqua regia, phosphoric acid and phosphoric acid-fluoroboric acid, hydrochloric acid-phosphoric acid mixture, none of these materials can be completely digested under plate digestion conditions.

[0102] like Figure 4 The image shown is a photograph of the digestion sample obtained (sample number 7) under laser irradiation. Figure 5 The image shown is a photograph of the digestion sample obtained (number 12) under laser irradiation. Figure 6 The image shows digestion samples obtained from numbers 10 and 11. As can be seen from the figure, Figure 4 The sample contains insoluble particles that will produce the Tyndall effect when irradiated with a laser pointer. Figure 5 The sample was clear, contained no insoluble matter, and did not exhibit the Tyndall effect. Figure 6 The digested samples in the first sample were almost insoluble. In samples numbered 10 and 11, 10 mL of 37 wt% HCl was added to each sample, followed by plate digestion (using a hot plate at 200°C for 30 min). The digested samples became clear and transparent.

[0103] Test Example 4

[0104] 0.1 g and 0.4 g of ternary material samples doped with aluminum and zirconium were weighed respectively, and different digestion reagents were added. The samples were digested using a hot plate at 200 °C. The digested solutions were filtered through a filter membrane, and then the filter membrane was digested at high temperature on an electric furnace using a strong acid (10 mL concentrated nitric acid + 2 mL concentrated sulfuric acid). The concentrations of Al and Zr in the insoluble matter retained on the filter membrane were tested according to the steps in Example 1. The test results are shown in Table 5.

[0105] Table 5

[0106]

[0107]

[0108] As shown in Table 5, when the sample weight was reduced to 0.1 g, the Al content in the insoluble matter after digestion with hydrochloric acid and sulfuric acid-hydrochloric acid mixture was still relatively high, while there was almost no Al and Zr residue after digestion with hydrochloric acid-fluoroboric acid system. In hydrochloric acid-fluoroboric acid system, the sample weight was increased to 0.4 g, and the digestion effect at different digestion times was tested. The results showed that when the digestion time was 30 min or more, complete digestion of Al and Zr could be achieved.

[0109] The embodiments described above are some, but not all, of the embodiments of this disclosure. The detailed description of the embodiments of this disclosure is not intended to limit the scope of the claimed disclosure, but merely to illustrate selected embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of this disclosure without inventive effort are within the scope of protection of this disclosure.

Claims

1. A method for determining aluminum and zirconium in ternary materials, characterized in that, include: Fluoroboric acid solution and hydrochloric acid solution were added to the ternary material to be tested to obtain the test sample; The sample to be tested is heated and digested on a hot plate to obtain a digested sample; The aluminum and zirconium content in the digested sample was determined using inductively coupled plasma atomic emission spectrometry. The mass concentration of the fluoroboric acid solution is 8-20%; the volume ratio of the fluoroboric acid solution to the hydrochloric acid solution is 1-6:

10.

2. The method for determining aluminum and zirconium in ternary materials according to claim 1, characterized in that, The step of heating and digesting on a hot plate includes: placing the sample to be tested on the hot plate and digesting it at 200~240℃ for 20~80 minutes.

3. The method for determining aluminum and zirconium in ternary materials according to claim 1, characterized in that, In the sample to be tested, the ratio of the ternary material to the hydrochloric acid solution is 3~5g:100mL.

4. The method for determining aluminum and zirconium in ternary materials according to claim 1, characterized in that, The steps for determining the aluminum and zirconium content in the digested sample using inductively coupled plasma atomic emission spectrometry include: Prepare a series of aluminum zirconium standard solutions with gradient concentrations, wherein the volume of the standard solution is V; Add diluent to the digested sample and bring the volume to V. The aluminum-zirconium standard solutions were measured using inductively coupled plasma atomic emission spectrometry to obtain standard curves for aluminum and zirconium. The digested sample after volume adjustment was measured using inductively coupled plasma atomic emission spectrometry (ICP-AES) to obtain the test results. The digestion sample was obtained based on the test results and the aluminum and zirconium standard curves.

5. The method for determining aluminum and zirconium in ternary materials according to claim 4, characterized in that, Both the aluminum zirconium standard solution and the digestion sample contain an internal standard solution.

6. The method for determining aluminum and zirconium in ternary materials according to claim 5, characterized in that, The internal standard solution is selected from one or more of scandium standard solution, germanium standard solution, yttrium standard solution, indium standard solution and bismuth standard solution.

7. The method for determining aluminum and zirconium in ternary materials according to claim 4, characterized in that, The aluminum zirconium standard solution contains the fluoroboric acid solution and the hydrochloric acid solution.

8. The method for determining aluminum and zirconium in ternary materials according to claim 1, characterized in that, The ternary material to be tested includes lithium nickel cobalt manganese oxide doped with metal element M1 and / or lithium nickel cobalt aluminum oxide doped with metal element M2, wherein M1 includes at least one of Al and Zr; and M2 includes at least Zr.

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