CN113155811A - Method for measuring content of zirconium element in lithium ion battery anode material - Google Patents
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Abstract
The invention discloses a method for measuring the zirconium content in the anode material of a lithium ion battery, which comprises the steps of firstly placing an anode material sample in hydrochloric acid, adding a certain amount of hydrochloric acid, placing the anode material sample on a resistance wire heating furnace capable of adjusting the temperature, heating and dissolving the sample, taking down the sample, cooling, adding a certain amount of concentrated sulfuric acid, continuing placing the sample on the resistance wire heating furnace for heating after ammonium sulfate is dissolved, cooling to room temperature to obtain a liquid to be tested when white smoke is emitted, selecting the optimal analysis spectral line of each element, preparing a set of standard solution with the concentration from low to high, introducing the standard solution into an ICP-OES spectrometer to draw a working curve under the optimized instrument working parameters, introducing the sample solution into the ICP-OES spectrometer to measure the intensity of the element to be tested, and determining the content of the element to be tested in the sample solution according to the working curve. The invention has less reagent consumption, reduces the pollution of chemical reagents to the environment and effectively meets the actual requirements of scientific research and production.
Description
Technical Field
The invention belongs to the technical field of chemical analysis and test, and particularly relates to a method for measuring the content of a zirconium element in a lithium ion battery anode material.
Background
In the actual use process of the lithium ion battery, many extremely severe working environments such as high and low temperature, high voltage, large current and the like need to be faced, the traditional anode material cannot meet the actual working conditions, and the anode material needs to be modified. The common modification method comprises surface coating and element doping, wherein atoms are introduced into crystal lattices to support the framework structure of the anode material, or an oxide layer is coated on the surface to isolate the corrosion of electrolyte, so that the stability of the material is improved.
With the continuous improvement of materials, single coating or single doping cannot achieve a good effect, at present, multiple elements are adopted to carry out coating and doping to improve the material performance, at the moment, the amount of the coated and doped elements is particularly critical, and accurate quantification of the doped elements is a prerequisite for preparing good materials.
Zirconium, strontium, yttrium, titanium and magnesium (Zr, Sr, Y, Ti and Mg) are the most commonly used coating doping elements in the current anode material. However, in the prior art, the test of Sr and Y under Zr and Zr-containing systems is always difficult. The reason is that Zr exists in the battery material in the form of zirconium dioxide and is difficult to dissolve in a conventional acid solution, and according to published data (hundred-degree encyclopedia), the zirconium dioxide burned at high temperature is difficult to dissolve in water, hydrochloric acid and dilute sulfuric acid and only can dissolve in hot concentrated hydrofluoric acid and concentrated sulfuric acid, but the concentrated sulfuric acid has too high viscosity and is not beneficial to ICP sample injection, and the hydrofluoric acid can corrode a glass container.
In the prior art, the test of the Zr-containing material is very complicated. Literature' ICP-OES method for rapidly determining LiFePO4The three elements of lithium, iron and phosphorus (Tan Zi Lizhi and the like) are used for independently testing the Zr element content, a sample is roasted first and then can be analyzed, the simultaneous analysis of multiple elements cannot be realized by adopting a traditional inductively coupled plasma emission spectrometer (ICP) method, and the operation process is complicated, so that the problems of long analysis period, large workload, high cost, poor precision and the like are caused.
Furthermore, the test is more complicated when both Y and Sr are present in the sample. During the preparation of the material, Y and Sr can form ZrSrO together with ZrxOr ZrYOxCompounds, pose further difficulties for analysis. And are currently availableThe coated or doped elements are all trace elements, the compound state is basically amorphous, and quantitative analysis of the compound state by XRD, EDS and the like is difficult. Therefore, it is a technical problem in the art how to simultaneously perform simple and accurate quantitative analysis on elements such as Zr, Y, Sr, etc. in the Zr-containing positive electrode material.
Disclosure of Invention
The invention aims to provide a method for measuring the content of zirconium in a lithium ion battery anode material, aiming at the defects that the existing detection method for the lithium ion battery anode material is complex in Zr element test, various miscellaneous elements in the Zr-containing anode material are difficult to test simultaneously, the operation steps are complicated, errors are easy to cause and the like. The method has the advantages of simple operation, high analysis efficiency, reliable result and convenient implementation.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for measuring the content of zirconium element in a lithium ion battery anode material comprises the following steps:
mixing and heating the positive electrode material, hydrochloric acid, concentrated sulfuric acid and ammonium sulfate to carry out digestion reaction to obtain a positive electrode material solution to be detected; the mass volume ratio of the positive electrode material to the hydrochloric acid to the concentrated sulfuric acid to the ammonium sulfate is 0.1g: 5-10 mL: 1-5 mL: 1.0-3.0 g, wherein the element to be detected in the anode material comprises Zr, and the mass fraction of the hydrochloric acid is 5-10%;
selecting the optimal sensitive analysis spectral line of the element to be detected according to the type of the element to be detected, configuring a set of standard solution to be introduced into an inductively coupled plasma emission (ICP-OES) spectrometer, and drawing a standard working curve in the spectrometer; and introducing the to-be-detected liquid of the anode material into an ICP-OES spectrometer, measuring the spectral line intensity of each element to be detected in the to-be-detected liquid, and determining the content of the trace element to be detected in the to-be-detected liquid of the anode material according to the standard working curve of the trace element to be detected.
Preferably, the digestion reaction comprises the following specific steps: weighing a certain amount of the anode material in a conical flask, adding hydrochloric acid, heating and dissolving the anode material on a temperature-adjustable resistance wire heating furnace at the heating temperature of 300-700 ℃, taking down and cooling the conical flask after the anode material to be detected is dissolved, adding a certain amount of concentrated sulfuric acid and ammonium sulfate, continuing heating the conical flask on the resistance wire heating furnace, cooling the conical flask to room temperature after white smoke is exhausted, transferring the liquid in the conical flask to a volumetric flask, and fixing the volume to the constant volume to obtain the liquid to be detected of the anode material after shaking up uniformly.
Preferably, the mass-to-volume ratio of the cathode material, hydrochloric acid, concentrated sulfuric acid and ammonium sulfate is 0.1g:5mL:1mL:1.0 g.
Preferably, the cathode material is a ternary cathode material.
Preferably, the elements to be detected comprise Zr, Sr, Y, Ti and Mg.
Furthermore, in the detection by an ICP-OES spectrometer, Zr 339.198nm, Sr 346.446nm, Y371.030 nm, Ti 336.121nm and Mg 285.213nm are used as the optimal detection wavelengths of each element.
Preferably, the operating parameters of the ICP-OES spectrometer are: high-purity argon (volume fraction 99.99%) is used as cooling gas, auxiliary gas and carrier gas; the RF power is 1145 and 1155W; the atomization pressure is 1.8-2.2Mpa, and the flow rate of the atomizer is 0.5-0.8L/min; the sample washing time is 30-45s, and the exposure is repeated for 3-5 times; the auxiliary gas flow is 0.5-0.9L/min, the rinsing pump speed is 70-80rpm, the analyzing pump speed is 45-55rpm, and the pump stabilization time is 5 s.
The invention has the beneficial effects that: aiming at the actual characteristics of the anode material and the doping elements of the lithium ion battery, the invention innovatively adopts the digestion mode of hydrochloric acid, sulfuric acid and ammonium sulfate to pretreat the sample, and the addition of the ammonium sulfate can effectively promote the digestion of zirconium dioxide, improve the analysis precision of Zr element, reduce the consumption of concentrated sulfuric acid and greatly reduce the pollution of chemical reagents to the environment.
The digestion mode provided by the invention can completely digest the doped coating elements in the anode material at one time, the reagent dosage is less, the pollution of chemical reagents to the environment is greatly reduced, the ICP-OES spectrometer is adopted, the purpose of simultaneously measuring the contents of Zr and other miscellaneous elements in the ternary anode material can be achieved, and compared with the prior art, the method is simple, convenient, rapid and efficient, and effectively meets the actual requirements of scientific research and production.
Drawings
FIG. 1 is a graph fitted to the magnesium element in example 1;
FIG. 2 is a curve fitted to the titanium element in example 1;
FIG. 3 is a curve fitted to the zirconium element in example 1;
FIG. 4 is a curve fitted to the strontium element in example 1;
FIG. 5 is a curve fitted to the yttrium element of example 1.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments and examples, and the advantages and various effects of the present invention will be more clearly apparent therefrom. It will be understood by those skilled in the art that these specific embodiments and examples are for the purpose of illustrating the invention and are not to be construed as limiting the invention.
A method for measuring the content of zirconium element in a lithium ion battery anode material comprises the following steps:
mixing and heating the positive electrode material, hydrochloric acid, concentrated sulfuric acid and ammonium sulfate to carry out digestion reaction to obtain a positive electrode material solution to be detected; wherein the mass fraction of the hydrochloric acid is 5-10%, and the mass volume ratio of the positive electrode material, the hydrochloric acid, the concentrated sulfuric acid and the ammonium sulfate is 0.1g: 5-10 mL: 1-5 mL:1.0 to 3.0g (most preferably, 0.1g:5mL:1mL:1.0 g); the element to be measured in the positive electrode material comprises Zr.
Selecting an optimal sensitive analysis spectral line of the element to be detected according to the type of the element to be detected, and configuring a set of standard solution to be introduced into an inductively coupled plasma emission spectrometer (ICP-OES) spectrometer to draw a standard working curve;
and introducing the to-be-detected liquid of the anode material into an ICP-OES spectrometer, measuring the spectral line intensity of each element to be detected in the to-be-detected liquid, and determining the content of the trace element to be detected in the to-be-detected liquid of the anode material according to the standard working curve of the trace element to be detected.
The inventor is through a large amount of experiments, discovers and adds the ammonium sulfate at the in-process of digesting, can effectual reduction improve Zr and digest efficiency at the bumping phenomenon of digesting the in-process production of Zr, gets rid of the influence of other elements to the test result to can the effectual quantity that reduces concentrated sulfuric acid, reduce the solution viscosity, its principle as follows: in the digestion process of a sample to be detected containing Zr element, the following reactions can occur:
ZrO2+H2SO4→ZrOSO4/Zr(SO4)2+H2O
however, the reaction rate of the present reaction is relatively slow and therefore the reaction is often incomplete, ZrO2Zr in the test sample cannot be completely digested, and the test result is often inaccurate.
And the reaction temperature is too high, concentrated sulfuric acid is unstable at high temperature and is easy to splash, so a small amount of ammonium sulfate needs to be added in the reaction process, the concentration of sulfate ions is increased, the reaction activity is increased, and the reaction speed is improved. The mass volume ratio of the positive electrode material to the hydrochloric acid to the concentrated sulfuric acid to the ammonium sulfate is 0.1g: 5-10 mL: 1-5 mL:1.0 to 3.0g (most preferably, 0.1g:5mL:1mL:1.0 g). Through a large number of experiments, the inventor finds that the proper acidity can be generated at the ratio, so that ions can be dissolved to the maximum extent, and less impurities and interfering elements are introduced.
When 0.1g of sample is dissolved, the lower limit of concentrated sulfuric acid is 1mL, the ion digestion cannot be completed when too little concentrated sulfuric acid is added, the concentrated sulfuric acid is too much, the viscosity of the digestion solution is too high, the sample introduction of an ICP instrument is influenced, and the instrument is damaged; the lower limit of the corresponding ammonium sulfate is 1.0g, the upper limit is 3.0g, the solution splashing can be caused by too little ammonium sulfate, the adding of too much ammonium sulfate can not accelerate the speed of the zirconium oxide being dissolved completely, and the analysis signals of other elements can be inhibited due to the increase of the dosage of the ammonium sulfate, so that the aim of accurate analysis and determination can not be achieved.
Preferably, in the invention, the optimal weight ratio of each digestion of 0.1g of the cathode material, hydrochloric acid, concentrated sulfuric acid and ammonium sulfate is 5ml: 1.0 ml:1.0 g.
Preferably, the digestion reaction comprises the following specific steps: weighing a certain amount of the anode material in a conical flask, adding hydrochloric acid, heating and dissolving the anode material on a temperature-adjustable resistance wire heating furnace at the heating temperature of 300-700 ℃, taking down and cooling the conical flask after the anode material is dissolved, adding a certain amount of concentrated sulfuric acid and ammonium sulfate, continuing heating the conical flask on the resistance wire heating furnace, cooling the conical flask to room temperature after white smoke is emitted, transferring the liquid in the conical flask to a volumetric flask, and fixing the volume to the constant volume to obtain the liquid to be measured of the anode material.
The lower limit of the digestion temperature is 300 ℃, the digestion temperature is too low, the reaction rate is slow, the upper limit of the digestion temperature is 700 ℃, the digestion temperature is obtained according to thermodynamic calculation in a reaction equation, the reaction is carried out spontaneously below 700 ℃, and the reaction is non-spontaneous reaction above 700 ℃.
Preferably, the cathode material is a ternary cathode material.
Preferably, the elements to be detected comprise Zr, Sr, Y, Ti and Mg.
Furthermore, in the detection by an ICP-OES spectrometer, Zr 339.198nm, Sr 346.446nm, Y371.030 nm, Ti 336.121nm and Mg 285.213nm are used as the optimal detection wavelengths of each element.
The selection process of the optimal detection wavelength is as follows: selecting several sensitive spectral lines of Ti, Mg, Zr, Sr and Y from a spectral line chart and a spectral line chart provided by an instrument, respectively scanning analysis spectral lines of 5Mg/L of Ti, Mg, Zr, Sr and Y by using 5Mg/L of Ti, Mg, Zr, Sr and Y mixed standard liquid, superposing and contrasting the spectral lines of the elements in different solutions, recording spectral line signals and background intensity, and selecting the sensitive spectral line with less interference and high signal-to-noise ratio as an analytical line, finally adopting Ti 336.121nm, Mg 285.213nm, Zr 339.198nm, Sr 346.446nm and Y371.030 nm as the analytical line of each element. The spectral lines corresponding to different wavelengths have different intensities and different anti-interference capacities, and the inventor finds that the selective response intensity of the analysis spectral lines of zirconium, strontium, yttrium, titanium and magnesium is high, the peak type is good and the detection limit is low through a large number of experiments.
Preferably, the operating parameters of the ICP-OES spectrometer are: high-purity argon (volume fraction 99.99%) is used as cooling gas, auxiliary gas and carrier gas; the RF power is 1145 and 1155W; the atomization pressure is 1.8-2.2Mpa, and the flow rate of the atomizer is 0.5-0.8L/min; the sample washing time is 30-45s, and the exposure is repeated for 3-5 times; the auxiliary gas flow is 0.5-0.9L/min, the rinsing pump speed is 70-80rpm, the analyzing pump speed is 45-55rpm, and the pump stabilization time is 5 s. Under the detection conditions, the peak pattern is good, and the test result is stable.
The invention provides a measuring method capable of simultaneously testing Zr and other elements in the anode material, and the measuring method is accurate in result, simple and feasible.
The present invention will be described in detail below with reference to specific examples and experimental data.
The invention has no special description, and all the reagents are analytically pure.
Example 1
(1) And (2) sample treatment, namely accurately weighing 0.1 +/-0.002 g of sample, placing the sample in a 100mL triangular flask, adding 5mL of hydrochloric acid, placing the sample on a temperature-adjustable resistance wire heating furnace for heating and dissolving, setting the temperature at 400 ℃, sequentially adding 1mL of concentrated sulfuric acid and 1g of ammonium sulfate, continuing placing the sample on the resistance wire heating furnace for heating, cooling the sample to room temperature after white smoke is emitted, transferring the sample to a 100mL volumetric flask for constant volume to reach a scale, and shaking up uniformly.
(2) Preparing standard working solution, respectively transferring 10mL of 1000ug/mL single-standard national standard solution of Ti, Mg, Zr, Sr and Y into a volumetric flask, and preparing mixed standard containing Ti, Mg, Zr, Sr and Y with the concentration of 100Mg/L as standard stock solution.
(3) Respectively and accurately weighing 5 parts of 0.1 +/-0.0001 g of ternary positive electrode material which does not contain Ti, Mg, Zr, Sr and Y elements and is used as a testing substrate to be placed in a triangular flask, sequentially adding 5mL of hydrochloric acid into the triangular flask, placing the triangular flask on a resistance wire heating furnace, heating at the temperature of 300 ℃ and 700 ℃, dissolving the sample, taking down the sample, adding 1mL of concentrated sulfuric acid and 1g of ammonium sulfate in sequence, continuously placing the sample on a resistance wire heating furnace for heating until white smoke is emitted, cooling to room temperature, transferring the sample to a 100mL volumetric flask, then accurately transferring 0, 1, 2, 5 and 10mL of standard solution stock solution into a volumetric flask, and (5) using ultra-high purity water to fix the volume to a scale mark, and obtaining a standard working solution containing Ti, Mg, Zr, Sr and Y with the mixed standard concentration of 0Mg/L, 1Mg/L, 2Mg/L, 5Mg/L and 10 Mg/L.
(4) And (3) introducing the obtained standard working solution into an ICP-OES instrument, mixing the standard working solution before entering an atomizer, measuring the standard working solution according to a pre-selected analysis line of Ti, Mg, Zr, Sr and Y to ensure that all correlation coefficients can reach more than 0.999, wherein a fitting graph of a curve can be shown in figures 1-5, and the curve graph shows that the test requirement can be met under the condition.
(5) The working parameters of the inductively coupled plasma lithium ion spectrometer are as follows: RF power is 1150W; the atomization pressure is 1.8-2.2Mpa, and the flow rate of the atomizer is 0.5L/min; the sample washing time was 30s and the exposure was repeated 3 times; the auxiliary gas flow is 0.5L/min; integration time long wave 5s, short wave 15s, washing pump speed 75rpm, analysis pump speed 50rpm, pump stability time 5 s.
The analysis line of each element in the step 5 is as follows: ti 336.121nm, Mg 285.213nm, Zr 339.198nm, Sr 346.446nm and Y371.030 nm
(6) And (3) introducing the sample solution to be tested obtained in the step (1) into ICP-OES for repeated measurement for 10 times, and calculating the standard deviation and the recovery rate of each element, wherein the experimental results are shown in Table 1.
Different amounts of Ti, Mg, Zr, Sr, Y standard solutions were added to known weighed samples, respectively, and the sample analysis method was operated, and the recovery rate of the measurement method was determined, and the results are shown in Table 2.
TABLE 1 recovery and standard deviation of repeated measurements of samples
TABLE 2 recovery of the samples with the addition of standard
The experimental result shows that the RSD of the method is less than 5%, the recovery rate of the method is between 98% and 103%, the requirements of analysis and test are completely met, and the method is accurate and reliable.
The above experimental steps are repeated, under the premise that the sample quality is not changed, the addition amount of concentrated sulfuric acid and the addition amount of ammonium sulfate are changed, parallel experiments of the embodiments 2 to 5 are carried out, and the amount of the dissolving reagent required for completely digesting the sample, the dissolving condition and the time required for the recovery rate are shown in a table 3.
TABLE 3 Experimental results for different reagent additions
As can be seen from the above table: when 0.1g of sample is completely dissolved by adopting the method, the optimal consumption of pure ammonium sulfate is 1g, and the optimal consumption of concentrated sulfuric acid dissolving reagent is 1-5 mL.
From the experimental data in the table, it can be seen that the lower limit of concentrated sulfuric acid is 1mL for dissolving 0.1g of sample, the ion digestion cannot be completed if the concentrated sulfuric acid is added too little, but if the concentrated sulfuric acid is too much, the solution viscosity is high in the digestion process, and the ICP equipment is damaged.
The lower limit of the corresponding ammonium sulfate is 1.0g, the upper limit is 3.0g, the solution splashing can be caused by too little ammonium sulfate, the adding of too much ammonium sulfate can not accelerate the speed of the zirconium oxide being dissolved completely, and the analysis signals of other elements can be inhibited due to the increase of the dosage of the ammonium sulfate, so that the aim of accurate analysis and determination can not be achieved.
Therefore, in the method of the present invention, the proportions of the positive electrode material, hydrochloric acid, concentrated sulfuric acid and ammonium sulfate are very important, and the inventors found through extensive studies that the optimal weight proportion of the positive electrode material, hydrochloric acid, concentrated sulfuric acid and ammonium sulfate per 0.1g of digestion is 5ml: 1.0 ml:1.0 g.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. A method for measuring the content of zirconium element in a lithium ion battery anode material is characterized by comprising the following steps:
1) mixing and heating the positive electrode material, hydrochloric acid, concentrated sulfuric acid and ammonium sulfate to carry out digestion reaction to obtain a positive electrode material solution to be detected; the mass volume ratio of the positive electrode material to the hydrochloric acid to the concentrated sulfuric acid to the ammonium sulfate is 0.1g: 5-10 mL: 1-5 mL: 1.0-3.0 g, wherein the element to be detected in the positive electrode material comprises zirconium, and the mass fraction of the hydrochloric acid is 5-10%;
2) selecting the optimal sensitive analysis spectral line of the element to be detected according to the type of the element to be detected, configuring a set of standard solution to be introduced into an inductively coupled plasma emission (ICP-OES) spectrometer, and drawing a standard working curve in the spectrometer; and introducing the to-be-detected liquid of the anode material into an ICP-OES spectrometer, measuring the spectral line intensity of each element to be detected in the to-be-detected liquid, and determining the content of the trace element to be detected in the to-be-detected liquid of the anode material according to the standard working curve of the trace element to be detected.
2. The measurement method according to claim 1, characterized in that: the digestion reaction in the step 1) comprises the following specific steps: weighing a certain amount of the anode material in a conical flask, adding hydrochloric acid, heating and dissolving the anode material on a temperature-adjustable resistance wire heating furnace at the heating temperature of 300-700 ℃, taking down and cooling the conical flask after the anode material to be detected is dissolved, adding a certain amount of concentrated sulfuric acid and ammonium sulfate, continuing heating the conical flask on the resistance wire heating furnace, cooling the conical flask to room temperature after white smoke is exhausted, transferring the liquid in the conical flask to a volumetric flask, and fixing the volume to the scale and shaking the volume uniformly to obtain the liquid to be detected of the anode material.
3. The measurement method according to claim 1, characterized in that: the mass-to-volume ratio of the positive electrode material, the hydrochloric acid, the concentrated sulfuric acid and the ammonium sulfate in the step 1) is 0.1g to 5mL to 1mL to 1.0 g.
4. The measurement method according to claim 1, characterized in that: the anode material in the step 1) is a ternary anode material.
5. The measurement method according to claim 1, characterized in that: the elements to be detected in the anode material in the step 1) comprise Zr, Sr, Y, Ti and Mg.
6. The measurement method according to claim 5, characterized in that: the optimal detection wavelength of the element to be detected in the anode material in the step 4) is as follows: zr: 339.198nm, Sr: 346.446nm, Y: 371.030nm, Ti: 336.121nm, Mg: 285.213 nm.
7. The measurement method according to claim 1, characterized in that: the working parameters of the inductively coupled plasma emission spectrometer are as follows: high-purity argon (volume fraction 99.99%) is used as cooling gas, auxiliary gas and carrier gas; the RF power is 1145 and 1155W; the atomization pressure is 1.8-2.2Mpa, and the flow rate of the atomizer is 0.5-0.8L/min; the sample washing time is 30-45s, and the exposure is repeated for 3-5 times; the auxiliary gas flow is 0.5-0.9L/min, the rinsing pump speed is 70-80rpm, the analyzing pump speed is 45-55rpm, and the pump stabilization time is 5 s.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116754349A (en) * | 2023-08-16 | 2023-09-15 | 四川赛科检测技术有限公司 | ICP-OES-based digestion method for lithium sulfide impurity elements and content determination method thereof |
| CN116754349B (en) * | 2023-08-16 | 2023-11-21 | 四川赛科检测技术有限公司 | ICP-OES-based digestion method for lithium sulfide impurity elements and content determination method thereof |
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