CN119290768A - Method and system for determining lithium content in lithium-containing mixed materials - Google Patents
Method and system for determining lithium content in lithium-containing mixed materials Download PDFInfo
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Abstract
一种含锂混合物料中锂含量的测定方法和测定系统，测定方法包括对含锂混合物料进行抽样，得到多个测试样；将测试样的颜色特征转换为颜色模型中的变量数据，颜色特征包括色调、亮度和色饱和度中的一种或多种，变量数据用于反映多个测试样中的锂含量。上述测定方法可进一步包括：分析多个测试样的变量数据是否存在差异，并根据分析结果判断含锂混合物料的均一性是否合格。上述测定方法无需测定锂的具体含量，即可获得含锂混合物料内部锂含量的分布信息，并可以快速、准确评价含锂混合物料的均一性。A method and system for determining the lithium content in a lithium-containing mixed material, the determination method comprising sampling the lithium-containing mixed material to obtain a plurality of test samples; converting the color characteristics of the test samples into variable data in a color model, the color characteristics comprising one or more of hue, brightness and color saturation, the variable data being used to reflect the lithium content in the plurality of test samples. The above determination method may further comprise: analyzing whether there are differences in the variable data of the plurality of test samples, and judging whether the uniformity of the lithium-containing mixed material is qualified based on the analysis results. The above determination method can obtain the distribution information of the lithium content inside the lithium-containing mixed material without determining the specific content of lithium, and can quickly and accurately evaluate the uniformity of the lithium-containing mixed material.
Description
Technical Field
The application relates to the field of lithium ion battery material detection, in particular to a method and a system for measuring lithium content in a lithium-containing mixed material.
Background
As an energy storage medium widely used at present, the lithium ion battery has huge market demand, and the performance pursuit of the lithium ion battery in the market is also higher and higher. Each improvement of the performance of the lithium ion battery is derived from the performance improvement of the key material, and in the nickel cobalt lithium manganate compound positive electrode material, the local proportion of lithium, nickel, cobalt and manganese, such as the proportion of Li to Me (Me=Ni+Co+Mn), is different, so that the electrochemical performance of the positive electrode material is greatly influenced, and therefore, whether the mixing of ingredients is uniform becomes one of the keys influencing the performance of the positive electrode material.
The process of mixing a lithium raw material and a precursor (metal hydroxide or oxide) in a certain ratio is called dry mixing, and chemical titration or potentiometric titration is mainly adopted in the industry at present to obtain a measured value of lithium, wherein the measured value is uniform by default within an index range for uniformity of dry mixing. However, the method has the defects of long test time, high cost, complex pretreatment process and the like, has small test quantity of one-time sampling, is not representative enough, is unfavorable for evaluating the uniformity of the mixed materials, and can be evaluated through multiple tests, but the multiple tests take too long to be favorable for rapid detection.
Disclosure of Invention
In view of the above, the present application provides a method and a system for determining lithium content in a lithium-containing mixture, so as to solve at least one of the above problems.
In order to achieve the above object, according to a first aspect of the present application, there is provided a method for measuring lithium content in a lithium-containing mixture, the method comprising sampling the lithium-containing mixture to obtain a plurality of test samples, and converting color characteristics of the test samples into variable data in a color model, wherein the color characteristics include one or more of hue, brightness and saturation, and the variable data is used for reflecting the lithium content in the plurality of test samples.
In some possible implementations, the determination method further comprises analyzing whether the variable data of the plurality of test samples are different, and judging whether the uniformity of the lithium-containing mixture is qualified according to the analysis result.
In some possible implementations, the color features include brightness, and converting the brightness of the lithium-containing mixture into variable data in the color model includes providing an illumination source, obtaining tristimulus values of the lithium-containing mixture under the illumination source, and converting the tristimulus values into brightness variables in the color model.
In some possible implementations, obtaining the tristimulus values of the lithium-containing mixture under the illumination source includes collecting, by the sensor, spectra reflected by the lithium-containing mixture under the illumination source at a preset viewing angle, obtaining the tristimulus values of the lithium-containing mixture under the illumination source according to a color matching function, and converting the tristimulus values into brightness variations in the color model.
In some possible implementations, the preset viewing angle includes one or both of 1 ° to 4 ° and greater than 4 °.
In some possible implementations, the illumination source includes a standard light source and a fluorescent light source, the standard light source having a correlated color temperature of 2856K to 6504K.
In some possible implementations, the standard light source includes one of standard light source D65, standard light source C, and standard light source a.
In some possible implementations, the lithium-containing mixture includes a dry-mixed material of a lithium source and a metal hydroxide, or a dry-mixed material of a lithium source and a metal oxide.
In some possible implementations, before converting the color characteristics of the lithium-containing mixture to the variable data in the color model, further comprising placing the lithium-containing mixture in a container with a ratio of height of the lithium-containing mixture to height of the container of 2/3-3/4, and compacting the lithium-containing mixture.
According to the method, the distribution of lithium in the lithium-containing mixed material has obvious influence on the color characteristics inside the lithium-containing mixed material, so that the color characteristics of a plurality of test samples in the lithium-containing mixed material are converted into variable data, and the variable data of the color characteristics can better reflect the lithium content in the test samples, so that the distribution information of the lithium content in different test samples is reflected according to the variable data of different test samples. In this way, the distribution information of the lithium content in the lithium-containing mixed material can be obtained without measuring the specific lithium content. Furthermore, the uniformity of the lithium-containing mixed material can be rapidly and accurately evaluated through whether the variable data among a plurality of test positions in the lithium-containing mixed material are different or not without measuring the specific content of lithium. The application also discovers that the distribution of lithium in the lithium-containing mixed material has more obvious influence on the brightness inside the lithium-containing mixed material, and the brightness of the test sample obtained by a specific light source condition, a tristimulus value and a color model with brightness variable can be used for more accurately mapping the lithium content in the test sample, so that the uniformity of the lithium-containing mixed material can be more accurately evaluated.
In a second aspect, the present application provides a system for determining the lithium content of a lithium-containing mixture, the system comprising a testing device for converting a color characteristic of the lithium-containing mixture into variable data in a color model, the color characteristic comprising one or more of hue, brightness and saturation, the variable data being for reflecting the lithium content of a plurality of test samples.
In some possible implementations, the measurement system further includes a processor, where the processor is configured to analyze whether there is a difference in variable data of the plurality of test samples, and determine whether the homogeneity of the lithium-containing mixture is acceptable according to the analysis result.
Detailed Description
Embodiments of the present application are described in detail below. The examples described below are illustrative only and are not intended to be limiting of the application, and it is to be understood that all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs unless otherwise defined, that embodiments of the application and features of the embodiments may be combined with one another without conflict, and that many specific details are set forth in the following description to provide a thorough understanding of the application, the described embodiments being merely some, but not all, embodiments of the application.
The uniformity evaluation of the existing positive electrode material mixture is usually carried out by dissolving out lithium and then carrying out chemical titration or potentiometric titration on the lithium, and the prior art relates to a pretreatment step and complex titration operation. The application notices that before the materials of the positive electrode materials are mixed, the lithium salt is white, the precursor is gray black or green, and the mixed materials are subjected to color change after the materials are mixed. Based on the theory of three primary colors, the perception of color is due to the combined result of light stimuli of three primary colors of red, green and blue, namely, the color can be described by tristimulus values, and the tristimulus values can be further converted into data variables in various color models to characterize the color characteristics of the substance.
In view of this, an embodiment of the present application provides a method for determining lithium content in a lithium-containing mixture, the method comprising:
And step one, sampling the lithium-containing mixture to obtain a plurality of test samples.
In some embodiments, the lithium-containing mixture comprises a dry blend of a lithium source and a metal hydroxide, or a dry blend of a lithium source and a metal oxide.
And step two, converting the color characteristics of the test samples into variable data in a color model, wherein the color characteristics comprise one or more of hue, brightness and color saturation, and the variable data are used for reflecting lithium content in a plurality of test samples.
In some embodiments, the color model includes one or more of CIEXYZ, CIEYxy, CIELab, CIELCh, CIELuv, hunter Lab, munsell color system, HSV, YUV, HSB, HIS, CMY, CMYK, and RGB.
In some embodiments, prior to converting the color characteristics of the lithium-containing mixture to the variable data in the color model, further comprising placing the lithium-containing mixture in a container with a ratio of height of the lithium-containing mixture to height of the container of 2/3-3/4, and compacting the lithium-containing mixture.
According to the method, the distribution of lithium in the lithium-containing mixed material has obvious influence on the color characteristics inside the lithium-containing mixed material, so that the color characteristics of a plurality of test samples in the lithium-containing mixed material are converted into variable data, and the variable data of the color characteristics can better reflect the lithium content in the test samples, so that the distribution information of the lithium content in different test samples is reflected according to the variable data of different test samples. In this way, the distribution information of the lithium content in the lithium-containing mixed material can be obtained without measuring the specific lithium content.
In some embodiments, the above-mentioned measuring method further comprises analyzing whether there is a difference in the variable data of the plurality of test samples, and judging whether the uniformity of the lithium-containing mixture is acceptable according to the analysis result. The uniformity of the lithium-containing mixed material can be rapidly and accurately evaluated by judging whether the variable data among a plurality of test positions in the lithium-containing mixed material are different or not without measuring the specific content of lithium.
In some embodiments, the uniformity of the lithium-containing mixture material can be judged whether to be qualified or not according to the result of the significance difference analysis by carrying out the significance difference analysis on the variable data obtained by the plurality of conversion.
In some embodiments, the significance differential analysis comprises a single factor analysis of variance. Further, a one-factor analysis of variance may be performed in mintab.
In some embodiments, the color feature comprises brightness. According to the application, the distribution of lithium in the lithium-containing mixed material has a more obvious effect on the brightness inside the lithium-containing mixed material, and the brightness of the test sample obtained through specific light source conditions, tristimulus values and a color model with brightness variable can be used for more accurately mapping the lithium content in the test sample, so that the uniformity of the lithium-containing mixed material can be more accurately evaluated.
When the color characteristic is brightness, converting the brightness of the lithium-containing mixture into variable data in the color model includes:
s10, providing an illumination light source.
And S20, obtaining the tristimulus value of the lithium-containing mixed material under the illumination light source.
And S30, converting the tristimulus values into brightness variables in the color model.
In some embodiments, the color model includes one or more of CIELab, CIELCh, CIELuv, hunter Lab, munsell color system, HSV, YUV, HSB, and HIS. It will be appreciated that when the color characteristic is brightness, a color model with brightness parameters is selected to convert the brightness of the material to variable data.
In order to convert the brightness of a test sample into a brightness variable, a tristimulus value of a material needs to be obtained, in the field of color science, the tristimulus value of a material can be measured by a sensor (such as a spectrum sensor, more specifically, such as a color difference meter) to obtain a spectrum of a specific wavelength (red, green and blue) reflected by the material under a specific illumination light source, and then the spectrum is converted into the tristimulus value according to a color matching function, and the conversion process can be completed by calculating the color matching function and related formulas in a processor. Thus, S20 may comprise the following more specific steps:
S21, collecting the spectrum reflected by the lithium-containing mixture under the illumination light source at a preset visual angle through a sensor.
In some embodiments, the preset viewing angle comprises one or both of 1 ° to 4 ° and greater than 4 °. It should be noted that, the viewing angle is also called a standard observer, and refers to an included angle of projection of the standard sample in eyes of the observer, the size of the object can cause the human eyes to affect the identification of colors, the distance between the standard observer and the eyes is a certain object, if the area of the object is large, the opening angle formed by the eyes is also large, the image of the object on the retina is large, and otherwise, the image is small. The object is observed under the visual angle of 1-4 degrees, mainly the central concave cone cells of human eyes act, and the object is observed under the visual angle of more than 4 degrees, mainly the central concave cone cells and the rod body cells around the central concave act, the visual angle is increased, and the perception of human eyes on the color can be changed. Different color matching functions are obtained for different viewing angles. It will be appreciated that when a preset viewing angle of 1 ° to 4 ° is employed, tristimulus values are obtained by conversion of the 2 ° standard observer color matching function, whereas when a preset viewing angle of greater than 4 ° is employed, tristimulus values are obtained by conversion of the 10 ° supplemental standard observer color matching function.
In some embodiments, the illumination source comprises a standard light source and a fluorescent light source, the standard light source having a correlated color temperature of 2856K to 6504K. In some embodiments, the standard light source comprises one of standard light source D65, standard light source C, and standard light source a.
S22, obtaining the tristimulus values of the lithium-containing mixed material under the illumination light source according to the color matching function.
S23, converting the tristimulus values into brightness variables in the color model.
In some embodiments, the color model includes one or more of CIELab, CIELCh, CIELuv, hunter Lab, and munsell color systems. It will be appreciated that in the relevant art, the above color model is selected to be compatible with the test methods of S21, S22 and S23.
The application also provides a measuring system capable of implementing the method for measuring the lithium content in the lithium-containing mixed material, and the measuring system comprises a testing device.
The testing device is used for converting color characteristics of the lithium-containing mixture into variable data in a color model, wherein the color characteristics comprise one or more of hue, brightness and color saturation, and the variable data are used for reflecting lithium content in a plurality of test samples.
In some embodiments, when the color feature is brightness, the testing device includes a light source emitter and a color measuring instrument.
As the light source emitter, a standard light source and a fluorescent light source are configured, and the correlated color temperature of the standard light source is 2856K to 6504K. In some embodiments, the standard light source comprises one of standard light source D65, standard light source C, and standard light source a.
As a color measuring instrument, a spectrum sensor is arranged. In some embodiments, the color measuring instrument is further configured with a first data processor for converting the data of the spectral sensor into tristimulus values according to a color matching function comprising a2 ° standard observer color matching function and a 10 ° supplemental standard observer color matching function. In some embodiments, the color measuring instrument is further configured with a second data processor for converting tristimulus values into luminance variables in a color model comprising one or more of CIELab, CIELCh, CIELuv, hunter Lab, and munsell color systems.
In some embodiments, the assay system described above further comprises a processor. The processor is used for analyzing whether the variable data of a plurality of test samples are different or not and judging whether the uniformity of the lithium-containing mixed material is qualified or not according to the analysis result.
The processor is used for carrying out significance difference analysis on the variable data obtained through the conversion.
In some embodiments, the processor determines whether the homogeneity of the lithium-containing mixture is acceptable based on the results of the significance differential analysis by performing a significance differential analysis on the plurality of transformed variable data.
In some embodiments, the significance differential analysis comprises a single factor analysis of variance. Further, a one-factor analysis of variance may be performed in mintab.
The scheme of the present application will be explained below with reference to examples. It will be appreciated by those skilled in the art that the following examples are for illustrative purposes only and are not to be construed as limiting the application. Unless otherwise indicated, the reagents, software and instrumentation involved in the examples below are all conventional commercial products or open source.
Example 1:
In the first step, 3 batches of NCM dry-mixed samples are selected, all indexes (electrical properties, granularity and element composition) of finished products corresponding to the 3 batches of samples are qualified, and the samples are paved, wherein 2 samples on the left side, 2 samples on the middle side and 2 samples on the right side are taken in each batch, and 6 test samples are taken in total.
In the second step, using a D65 light source (S (lambda) relative to the spectral energy distribution), the colorimeter was at a 10 degree viewing angle and the sample port size was 30 mm (i.e., the measurement area was a circle of 30 mm diameter).
And thirdly, pouring the test sample into a culture dish, pouring the sample into the culture dish with the height 2/3 higher than that of the culture dish, paving uniformly, compacting the sample, and testing each test sample for 2 times by using a color meter under the condition set in the second step to obtain the spectral reflectance R (lambda) of the material.
Fourth, obtaining the color matching function of the observer according to the 10 DEG supplement standardThe tristimulus value Y is calculated by the following equation (1) and equation (2):
(1);
(2)。
A fifth step of calculating a brightness variable L from the following formula (3) when Y/Yn is not less than 0.008856 and from the formula (4) when Y/Yn <0.008856 according to the CIELab color model, wherein Yn is a value corresponding to a green primary color among tristimulus values obtained when the total reflection diffuse reflector is irradiated with the same light source S:
(3);
(4)。
Step six, the measured L value is imported mintab to carry out single-factor analysis of variance, and the result is shown in Table 1.
TABLE 1 mean and standard deviation of the L values of the test samples in 3 NCM dry-blended samples in example 1 of the present application
In Table 1, the P value >0.05, indicates that the samples were uniformly mixed. 3 batches of NCM dry-mixed samples can be used as standard samples, so that the uniformity index meeting qualified production can be set to be 29.02+/-0.48 according to X+3Σ.
Example 2:
Firstly, selecting NCA dry-mixed samples (the samples are new product small test materials and do not correspond to finished products meeting various indexes), paving, taking 2 left, 2 middle and 2 right test samples, and carrying out sample uniformity evaluation on the total of 6 test samples.
In the second step, using a D65 light source (S (lambda) relative to the spectral energy distribution), the colorimeter was at a 10 degree viewing angle and the sample port size was 30 mm (i.e., the measurement area was a circle of 30 mm diameter).
And thirdly, pouring the test sample into a culture dish, pouring the sample into the culture dish with the height 2/3 higher than that of the culture dish, paving uniformly, compacting the sample, and testing each test sample for 3 times by using a color meter under the condition set in the second step to obtain the spectral reflectance R (lambda) of the material.
Fourth, obtaining the color matching function of the observer according to the 10 DEG supplement standardThe tristimulus value Y is calculated by the following equation (1) and equation (2):
(1);
(2)。
A fifth step of calculating a brightness variable L from the following formula (3) when Y/Yn is not less than 0.008856 and from the formula (4) when Y/Yn <0.008856 according to the CIELab color model, wherein Yn is a value corresponding to a green primary color among tristimulus values obtained when the total reflection diffuse reflector is irradiated with the same light source S:
(3);
(4)。
step six, the measured L value is imported mintab to carry out single-factor analysis of variance, and the result is shown in Table 2.
TABLE 2 evaluation of homogeneity of NCA Dry mix samples (small samples) according to example 2 of the application
For a new product of the small test material, namely, a finished product which does not meet each index correspondingly, an L value can be obtained through the embodiment 2, single-factor variance analysis is carried out on the L value, and whether the average value of the sample has no significant difference is checked to represent the uniformity of mixing of the small test material. In Table 2, the P value >0.05, indicates that the batch was uniformly mixed.
The above embodiments are only for illustrating the technical solution of the present application and not for limiting the same, and although the present application has been described in detail with reference to the above preferred embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the technical solution of the present application.
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