CN117629974A

CN117629974A - Method for measuring aluminum and zirconium in ternary material

Info

Publication number: CN117629974A
Application number: CN202311429147.8A
Authority: CN
Inventors: 林月明; 庄启钊; 陈焘; 胡珍
Original assignee: Xiamen Xiaw New Energy Materials Co ltd
Current assignee: Xiamen Xiaw New Energy Materials Co ltd
Priority date: 2023-10-31
Filing date: 2023-10-31
Publication date: 2024-03-01

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 measuring aluminum and zirconium in the ternary material comprises the following steps: and adding a fluoboric acid solution and a hydrochloric acid solution into the ternary material to be tested to obtain a sample to be tested. Heating and digesting the sample to be tested on an electric heating plate to obtain a digested sample; and determining the content of aluminum element and zirconium element in the digestion sample by using an inductively coupled plasma emission spectrometer. According to the method, fluoboric acid/hydrochloric acid is used as a digestion system, an electric heating plate is used for digestion, the digestion mode is easy to operate, and the obtained digestion product is clear and free of insoluble matters, so that accurate determination of aluminum and zirconium can be realized.

Description

Method for measuring aluminum and zirconium in ternary material

Technical Field

The disclosure relates to the technical field of lithium batteries, and in particular relates to a method for measuring aluminum and zirconium in ternary materials.

Background

Along with the increasing prominence of energy problems and environmental protection problems, the lithium ion battery is widely applied to the fields of portable electronic products, electric vehicles, energy storage and the like due to the excellent performances of high voltage, high power density, long service life and the like and the environmental protection. The positive electrode material is a key raw material in the lithium ion battery, and the quality of the positive electrode material can have an important influence on the performance of the lithium ion battery. The lithium ion battery material mainly comprises a nickel-cobalt-manganese ternary material, lithium iron phosphate, lithium nickel oxide and the like. In recent years, ternary materials have been widely used due to their high energy density. At present, in the production process of the nickel-cobalt-manganese ternary material, aluminum and zirconium compounds are often used for cladding doping so as to improve the stability of the structure of the ternary material and improve the electrochemical performance of the ternary material after being manufactured into a battery cell. In order to accurately characterize the product cladding doping effect of the ternary material, the elemental content of aluminum and zirconium in the ternary material needs to be tested.

However, the current industry tests for the content of aluminum and zirconium in nickel-cobalt-manganese ternary materials are generally performed with reference to the non-ferrous metal industry standard YS/T1006.2-2014 of the people's republic of China, namely, a sample is put into a beaker, hydrochloric acid is added, heating and dissolving are carried out, cooling is carried out, the sample is transferred into a volumetric flask, water is used for dilution to a scale, mixing is carried out, and then ICP-OES (inductively coupled plasma emission spectrometer) is adopted for element content testing. The method can not completely digest the test sample, and insoluble matters often exist in the digested product, so that the test result is inaccurate. Meanwhile, insoluble substances in the digestion products are easy to cause blockage to an ICP-OES sampling system, and the service life of the instrument is influenced.

It should be noted that the information disclosed in the above background section is only for enhancing understanding of the background of the present disclosure and thus may include information that does not constitute prior art known to those of ordinary skill in the art.

Disclosure of Invention

In order to solve the technical problems, the disclosure provides a method for measuring aluminum and zirconium in ternary materials.

The present disclosure provides a method for determining aluminum, zirconium in ternary materials, comprising:

adding a fluoboric acid solution and a hydrochloric acid solution into the ternary material to be detected to obtain a sample to be detected;

heating and digesting the sample to be tested on an electric heating plate to obtain a digested sample;

and determining the content of aluminum element and zirconium element in the digestion sample by using an inductively coupled plasma emission spectrometer.

In one exemplary embodiment of the present disclosure, the fluoroboric acid solution has a mass concentration of 8-20%.

In one exemplary embodiment of the present disclosure, the volumetric usage ratio of the fluoroboric acid solution and the hydrochloric acid solution is 1-6:10.

In one exemplary embodiment of the present disclosure, the heating digestion on the electric plate includes: and placing the sample to be tested on an electric heating plate, and digesting for 20-80 min at the temperature of 200-240 ℃.

In an exemplary embodiment of the disclosure, in the sample to be tested, the feed liquid ratio of the ternary material to the hydrochloric acid solution is 3 to 5g:100mL.

In one exemplary embodiment of the present disclosure, the step of determining the content of elemental aluminum and elemental zirconium in the digestion sample using an inductively coupled plasma emission spectrometer comprises:

preparing a series of aluminum-zirconium standard solutions with gradient concentration, wherein the volume of the aluminum-zirconium standard solution is V;

adding diluent into the digestion sample, and fixing the volume until the volume is V;

measuring the aluminum element zirconium standard solution by using an inductively coupled plasma emission spectrometer to obtain an aluminum element standard curve and a zirconium element standard curve;

measuring the digestion sample after volume fixing by using an inductively coupled plasma emission spectrometer to obtain a test result;

and obtaining the digestion sample according to the test result, the aluminum element standard curve and the zirconium element standard curve.

In one exemplary embodiment of the present disclosure, an internal standard solution is added to both the aluminum zirconium standard solution and the digestion sample.

In one exemplary embodiment of the present 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.

In one exemplary embodiment of the present disclosure, the aluminum zirconium standard solution has the fluoroboric acid solution and the hydrochloric acid solution added thereto.

In one exemplary embodiment of the present disclosure, the ternary material to be tested includes a metal element M ₁ Doped lithium nickel cobalt manganate and/or metallic element M ₂ Doped lithium nickel cobalt aluminate, wherein the M ₁ Comprises at least one of Al and Zr; the M is ₂ At least includes Zr.

The method for measuring aluminum and zirconium in the ternary material has the beneficial effects that:

the determination method adopts the electric heating plate to carry out the flat plate digestion, the digestion process is simple, the operation is convenient, the method can be suitable for detecting scenes in a large batch, and the detection efficiency is high. In the process of plate digestion, fluoboric acid/hydrochloric acid is used as a digestion system, and the obtained digestion product is clear and has no insoluble matters and good digestion effect. The method for measuring the aluminum and zirconium elements in the ternary material can realize the accurate measurement of the aluminum and zirconium, is stable and reliable, has the recovery rate of 90-110%, and has the repeatability level RSD of less than 0.5%.

It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the disclosure.

Drawings

In order to more clearly illustrate the technical solutions of the embodiments of the present disclosure, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present disclosure and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person of ordinary skill in the art.

FIG. 1 is a flow chart of a method for determining aluminum and zirconium in ternary materials according to an embodiment of the present disclosure.

Fig. 2 is a standard graph of Al element plotted in example 1.

FIG. 3 is a standard chart of Zr element obtained by drawing in example 1.

FIG. 4 is a physical view of the digested sample obtained in test example 3 under laser irradiation, wherein the sample is subjected to No. 7.

FIG. 5 is a physical view of the digested sample obtained in test example 3 under laser irradiation, wherein the sample is subjected to No. 12.

FIG. 6 is a physical view of the digested sample obtained in Experimental example 3, number 10.

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present disclosure more apparent, the technical solutions in the embodiments of the present disclosure will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.

The method for measuring aluminum and zirconium in ternary materials in the embodiment of the disclosure is specifically described below.

The embodiment of the disclosure provides a method for determining aluminum and zirconium in ternary materials, which comprises the following steps:

step S1, adding a fluoboric acid solution and a hydrochloric acid solution into a ternary material to be tested to obtain a sample to be tested;

s2, heating and digestion are carried out on the sample to be tested on an electric heating plate, so that a digested sample is obtained;

and S3, measuring the content of aluminum element and zirconium element in the digestion sample by using an inductively coupled plasma emission spectrometer.

In the prior art, a microwave digestion mode is generally adopted to pretreat a sample to be tested, and the requirement on a digestion reagent is relatively low because the microwave digestion is carried out in a high-temperature and high-pressure environment. However, microwave digestion has high requirements on equipment, is complex and cumbersome to operate, and is not suitable for a large-batch operating environment. The method for determining the aluminum and the zirconium in the ternary material provided by the disclosure is characterized in that the electric heating plate is used for digestion, the equipment requirement is low, the operation is simple and convenient, the method is more suitable for large-scale detection scenes, and the efficient detection of a large number of samples is realized. The fluoboric acid/hydrochloric acid is used as a digestion system, and a digestion product of the insoluble matters of the clarified matters can be obtained in a flat plate digestion mode, so that the accurate determination of aluminum and zirconium in the ternary material is realized.

Specifically, in embodiments of the present disclosure, the ternary material to be tested includes a metal element M ₁ Doped lithium nickel cobalt manganate and/or metallic element M ₂ Doped lithium nickel cobalt aluminate, wherein the M ₁ Comprises at least one of Al and Zr; the M is ₂ At least includes Zr.

Specifically, in one embodiment, the ternary material to be tested is a metal element M ₁ Doped lithium nickel cobalt manganate, said M ₁ Comprises at least one of Al and Zr. The ternary material to be tested can also be doped with a material other than M ₁ Other elements than those described above are not particularly limited in this disclosure.

Specifically, in another embodiment, the ternary material to be tested is a metal element M ₂ Doped nickel cobalt; lithium aluminate, the M ₂ At least one of Zr. The ternary material to be tested can also be doped with a material other than M ₂ Other elements than those described above are not particularly limited in this disclosure.

It should be noted that the ternary material to be tested can be doped with the metal element M ₁ Or M ₂ The present disclosure is not particularly limited.

In the embodiment of the present disclosure, in step S1, a solution of fluoroboric acid and a solution of hydrochloric acid are added to a ternary material to be measured, to obtain a sample to be measured.

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

Specifically, in the step, the hydrochloric acid solution is 20-40% by mass, for example, concentrated hydrochloric acid with a mass concentration of 36% -38% is selected as the hydrochloric acid solution. The fluoboric acid-hydrochloric acid digestion system can obtain a better digestion effect, so that aluminum and zirconium are digested more thoroughly, and the detection result is more accurate.

Further, in one embodiment of the present disclosure, the volumetric usage ratio of the fluoroboric acid solution and the hydrochloric acid solution is 1-6:10. More preferably, the volume usage ratio of the fluoboric acid solution to the hydrochloric acid solution is 4-6:10. Under the proportion, the mixed acid system formed by the fluoboric acid solution and the hydrochloric acid solution can realize complete digestion of the ternary material so as to ensure the accuracy of a test result.

Specifically, in this step, the fluoroboric acid solution and the hydrochloric acid solution may be added in batches, or the fluoroboric acid solution and the hydrochloric acid solution may be mixed and then added to the ternary material to be measured. Further preferably, in this embodiment, the solution of fluoroboric acid is added to the ternary material first, and then the solution of hydrochloric acid is added to obtain the sample to be tested.

Specifically, in the step, in the sample to be detected, the feed liquid ratio of the ternary material to the hydrochloric acid solution is 3-5 g:100mL, the feed liquid ratio of the ternary material to the fluoboric acid solution is 3-5 g:50mL. Namely, 100mL of hydrochloric acid solution and 50mL of fluoroboric acid solution are added to 3-5 g of ternary material. The ratio of the amount of sample to the amount of digestion reagent will have an effect on the digestion. The sample cannot be completely digested if the consumption of the digestion reagent is too small; excessive consumption of digestion reagent can result in waste. In addition, the higher the sample amount is, the higher the element concentration in the sample to be tested is, and the better the test stability is; second, the larger the sample size, the better the sample representativeness.

In step S2, the sample to be tested is heated and digested on an electric heating plate, so as to obtain a digested sample.

Further, the method specifically comprises the following steps: and placing the sample to be tested on an electric heating plate, and digesting for 20-80 min at the temperature of 200-240 ℃. For example, an electric heating constant temperature platform device can be selected for safe digestion. During operation, only need to be measured sample place on the heating flat board, temperature and time are adjusted can, convenient operation.

Further preferably, the digestion time is 30 to 40 minutes. When the digestion time reaches more than 30min, complete digestion of Al and Zr can be realized.

In step S3, the aluminum element and zirconium element contents in the digestion sample are determined using an inductively coupled plasma emission spectrometer (ICP-OES). In one embodiment, the step S3 specifically includes:

s31, preparing a series of aluminum-zirconium standard solutions with gradient concentration, wherein the volume of the aluminum-zirconium standard solution is V;

s32, adding diluent into the digestion sample, and fixing the volume until the volume is V;

s33, measuring the aluminum zirconium standard solution by using ICP-OES to obtain an aluminum element standard curve and a zirconium element standard curve;

s34, measuring the digestion sample after volume fixing by using ICP-OES to obtain a test result;

s35, obtaining the digestion sample according to the test result, the aluminum element standard curve and the zirconium element standard curve.

In one embodiment of the disclosure, an internal standard solution is added to both the aluminum zirconium standard solution and the digestion sample.

Further, 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 Sc standard solution. Sc is selected as an internal standard, and the content of the element to be detected can be calibrated to compensate the non-spectral interference caused by the matrix solution. Thereby correcting the influence of factors such as solvent, operation error, instrument drift and the like on the test result and improving the accuracy of the detection result.

Further, the standard solution of aluminum zirconium is added with fluoboric acid solution and hydrochloric acid solution. And the fluoboric acid solution and the hydrochloric acid solution are added into the standard solution, so that the consistency of the standard solution and the solvent components of the sample to be detected is ensured, and the interference is reduced. Specifically, the standard solution is added with fluoboric acid solution and hydrochloric acid solution with the volume ratio of 1-2:8-10. The addition amount of the hydrochloric acid solution is approximately equal to that of the sample to be tested.

Specifically, in step S31, the preparation process of the aluminum zirconium standard solution is as follows: adding a certain amount of fluoroboric acid solution and hydrochloric acid solution (volume ratio is 1-2:8-10) into a volumetric flask, adding a certain volume of scandium standard solution (concentration is 100 mug/mL), adding a certain volume of aluminum standard solution (concentration is 1000 mug/mL) and zirconium standard solution (concentration is 1000 mug/mL), and using ultrapure water to fix volume to volume V to obtain a gradient series standard solution. Specifically, the constant volume V may be 50mL, 100mL, 500mL, etc.

Further, in a specific embodiment, the concentration of scandium element in the aluminum zirconium standard solution is 0.2-1 μg/mL. In the aluminum zirconium standard solution, the concentration gradient of aluminum element is 0, 2 mug/mL, 8 mug/mL and 14 mug/mL respectively; the concentration gradient of zirconium element was 0, 4. Mu.g/mL, 10. Mu.g/mL and 16. Mu.g/mL, respectively.

Specifically, in step S32, the constant volume process of sample elimination is as follows: the digested sample was transferred to a volumetric flask, washed several times with ultrapure water during the transfer, and a certain volume of scandium standard solution (concentration 100. Mu.g/mL) was added, and the volume was set to volume V with ultrapure water. Namely, the constant volume of the sample to be digested is consistent with that of the standard solution of aluminum and zirconium. And the concentration of scandium element in the digestion sample after constant volume is consistent with that of the aluminum zirconium standard solution.

Specifically, in steps S33 and S34, the ICP-OES operating conditions are: the analysis wavelength of the aluminum element is 396.153nm, the analysis wavelength of the zirconium element is 343.823nm, and the analysis wavelength of the scandium element is 361.384nm.

Specifically, the instrument operating conditions for ICP-OES may be set as: argon plasma light source, power 1150W, atomizer flow 0.70L/min, auxiliary air flow 0.5L/min, and observation height 12mm.

The features and capabilities of the present disclosure are described in further detail below in connection with the examples.

Example 1

The method for determining Al and Zr in the ternary material provided by the embodiment comprises the following steps:

(1) Preparing a sample to be measured: the sample to be measured was weighed 0.4.+ -. 0.0004g in a 150mL polytetrafluoroethylene beaker. The sample to be measured is an Al-Zr doped nickel-cobalt-manganese ternary material.

(2) Preparing a fluoboric acid solution: 1L of fluoroboric acid with the mass concentration of 50% and 4L of ultrapure water are added into a 5L solution bottle, and uniformly mixed to prepare a 10wt% fluoroboric acid solution.

(3) Sample digestion: adding 5mL of 10wt% fluoboric acid solution and 10mL of 37wt% hydrochloric acid solution into the sample to be tested in the step (1); placing on an electric heating plate, and digesting for 30min at 220 ℃ to obtain a digestion sample. The digested sample is clear and has no insoluble precipitate.

(4) Preparing a sample solution: transferring the digestion sample obtained in the step (3) into a 100mL plastic volumetric flask, and cleaning at least 3 times during transfer. And 0.5mL scandium standard stock solution (concentration 100. Mu.g/mL) was added, the volume was fixed to 100mL, and the mixture was shaken for use.

(5) Preparing a standard solution: 4 plastic volumetric flasks of 100mL were prepared, 10mL of 37wt% hydrochloric acid solution and 2mL of 10wt% fluoroboric acid were added to the flasks, and 0.5mL of scandium standard stock solution (concentration 100. Mu.g/mL) was added; to each volumetric flask were added 0, 0.2, 0.8, 1.4mL of standard stock solution of aluminum (concentration 1000. Mu.g/mL) and 0, 0.4, 1.0, 1.6mL of standard stock solution of zirconium (concentration 1000. Mu.g/mL), respectively. The volume is fixed to 100mL by ultrapure water, and the mixture is shaken for standby.

(6) And (3) testing the standard solution prepared in the step (5) by using ICP-OES under the instrument working conditions with the parameters, and drawing an Al element standard curve and a Zr element standard curve according to the response intensity ratio of Al element, zr element and internal standard Sc emission and the concentration ratio of the Al element, zr element and internal standard Sc emission. The standard graph of the Al element is drawn as shown in fig. 2, and the standard graph of the Zr element is drawn as shown in fig. 3.

(7) And (3) testing the sample solution prepared in the step (4) by using ICP-OES to obtain a test result. Substituting the test result into a standard curve of the Al element and the Zr element for calculation to obtain the Al and Zr contents of the sample to be tested.

Test example 1 labeled recovery and repeatability test

According to the measurement procedure in example 1, a standard recovery test was performed on one of the samples to be tested, and the test results are shown in table 1 below:

TABLE 1

According to the procedure of example 1, another sample to be tested was subjected to repeated tests, the test results are shown in Table 2 below:

TABLE 2

From tables 1 and 2, it can be seen that the method for measuring Al and Zr provided in this example has recovery rate of 90% -110%, repeatability level RSD of less than 0.5%, reliable scheme and high accuracy of measurement result.

Test example 2 digestion device test

And selecting the same sample to be tested, and carrying out digestion by using different heating devices, wherein the experimental group is an electric heating plate heating device, and the comparison group is a voltage-regulating electric furnace heating device, wherein the digestion condition of the voltage-regulating electric furnace is 150V, the digestion time is 30min, and the digestion condition of the electric heating plate is 200 ℃ and the digestion time is 30min. After digestion is completed, the digestion sample after standing for 18 hours and the digestion sample after shaking are used for testing, and the testing process is performed in the dark in the step of the embodiment 1. The test results are shown in table 3 below:

TABLE 3 Table 3

In the test process, the fact that the difference of measurement results between a plurality of parallel digestion samples is larger when the voltage-regulating electric furnace is used for digestion in the comparison group is found, and the fact that the difference of measurement results between the plurality of parallel digestion samples is larger is probably due to the fact that the temperature difference of different positions of the voltage-regulating electric furnace is larger, the temperature of some samples is higher, so that digestion reagents volatilize too fast, the time for acting on the samples is short, the effect is poor, digestion is incomplete, and the test result is lower.

Further, as can be seen from table 3, and the difference between the test result after standing of the digested sample and the test result after shaking was extremely large. Indicating that the digested sample contains insoluble matters containing Al, and the insoluble matters are settled along with the time, so that the test results have larger difference.

In the experimental group, the electric heating plates are used for digestion, the measurement results among the parallel digestion samples are almost not different, the temperature control of the electric heating plates for digestion is accurate, and the digestion process of the parallel samples can be controlled under the same condition. In addition, as can be seen from table 3, the difference between the test result after standing and the test result after shaking up of the digested sample is very small, and it can be seen that the digestion effect is very good without insoluble precipitate.

Test example 3 digestion reagent test

Weighing 0.4g of ternary material sample doped with aluminum and zirconium, and carrying out digestion by using different digestion reagents under the following conditions: adopting an electric heating plate, and carrying out digestion for 30min at the temperature of 200 ℃. After completion of digestion, the state of the digested sample was observed. The test results are shown in Table 4.

TABLE 4 Table 4

As can be seen from table 4, increasing the addition amount of hydrochloric acid had little effect on the digestion effect; the hydrochloric acid-hydrogen peroxide system, nitric acid-fluoboric acid, nitric acid-hydrogen peroxide system, aqua regia, phosphoric acid-fluoboric acid, hydrochloric acid-phosphoric acid mixed acid are used, and the materials cannot be completely digested under the condition of plate digestion.

Fig. 4 is a view showing a sample of the digested sample obtained by the number 7 under laser irradiation, and fig. 5 is a view showing a sample of the digested sample obtained by the number 12 under laser irradiation. The digested samples obtained with numbers 10 and 11 are shown in FIG. 6. As can be seen, the presence of insoluble particles in the sample of fig. 4 produces the tyndall effect when irradiated by a laser pen. The sample in fig. 5 is clear, without insolubles, and without the tyndall effect. The digested sample in fig. 6 was hardly dissolved. To the digested samples of Nos. 10 and 11, 10mL of 37wt% HCl was added, respectively, and then the digested samples were subjected to plate digestion (digestion at 200℃for 30 minutes using a hot plate) to become clear and transparent.

Test example 4

And respectively weighing 0.1g and 0.4g of ternary material samples doped with aluminum and zirconium, adding different digestion reagents, and digesting at 200 ℃ by using an electric hot plate. The digested solution was filtered using a filter membrane, and then the filter membrane was digested with a strong acid (10 mL of concentrated nitric acid+2 mL of concentrated sulfuric acid) on an electric furnace at high temperature, and the concentration of Al, zr in insoluble matters trapped on the filter membrane was tested according to the procedure in example 1. The test results are shown in Table 5.

TABLE 5

As can be seen from Table 5, when the sample amount is reduced to 0.1g, the content of Al in insoluble substances after digestion of hydrochloric acid and sulfuric acid-hydrochloric acid mixed acid is still higher, and little Al and Zr remain after digestion of the hydrochloric acid-fluoroboric acid system; under the hydrochloric acid-fluoboric acid system, the sample weighing amount is increased to 0.4g, and the digestion effect under different digestion time is tested, so that the result shows that when the digestion time is 30min and above, the complete digestion of Al and Zr in the sample can be realized.

The embodiments described above are some, but not all, embodiments of the present disclosure. The detailed description of the embodiments of the present disclosure is not intended to limit the scope of the disclosure, as claimed, but is merely representative of selected embodiments of the disclosure. All other embodiments, which can be made by one of ordinary skill in the art without inventive effort, based on the embodiments in this disclosure are intended to be within the scope of this disclosure.

Claims

1. A method for determining aluminum and zirconium in a ternary material, comprising:

2. The method for measuring aluminum and zirconium in ternary materials according to claim 1, wherein the mass concentration of the fluoboric acid solution is 8-20%.

3. The method for determining aluminum and zirconium in ternary materials according to claim 1, wherein the volume ratio of the fluoboric acid solution to the hydrochloric acid solution is 1-6:10.

4. The method for determining aluminum and zirconium in ternary materials according to claim 1, wherein the step of performing heating digestion on an electric hot plate comprises: and placing the sample to be tested on an electric heating plate, and digesting for 20-80 min at the temperature of 200-240 ℃.

5. The method for measuring aluminum and zirconium in ternary materials according to claim 1, wherein in the sample to be measured, the feed liquid ratio of the ternary materials to the hydrochloric acid solution is 3-5 g:100mL.

6. The method for determining aluminum and zirconium in ternary materials according to claim 1, wherein the step of determining the content of aluminum element and zirconium element in the digestion sample by using an inductively coupled plasma emission spectrometer comprises:

preparing a series of aluminum-zirconium standard solutions with gradient concentration, wherein the volume of the standard solution is V;

measuring the aluminum-zirconium standard solution by using an inductively coupled plasma emission spectrometer to obtain an aluminum element standard curve and a zirconium element standard curve;

7. The method for determining aluminum and zirconium in ternary materials according to claim 6, wherein an internal standard solution is added to both the aluminum zirconium standard solution and the digestion sample.

8. The method of determining aluminum and zirconium in ternary materials according to claim 7, wherein 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.

9. The method for measuring aluminum and zirconium in ternary materials according to claim 6, wherein the aluminum zirconium standard solution is added with the fluoboric acid solution and the hydrochloric acid solution.

10. The method for determining aluminum and zirconium in ternary materials according to claim 1, wherein the ternary materials to be determined comprise a metal element M ₁ Doped nickelLithium cobalt manganate and/or metal element M ₂ Doped lithium nickel cobalt aluminate, wherein the M ₁ Comprises at least one of Al and Zr; the M is ₂ At least includes Zr.