CN102455341B - Method for detecting and determining batch consistency of lithium iron phosphate material - Google Patents
Method for detecting and determining batch consistency of lithium iron phosphate material Download PDFInfo
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- CN102455341B CN102455341B CN201110052794.2A CN201110052794A CN102455341B CN 102455341 B CN102455341 B CN 102455341B CN 201110052794 A CN201110052794 A CN 201110052794A CN 102455341 B CN102455341 B CN 102455341B
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Abstract
The invention relates to the field of lithium ion batteries, and discloses a method for detecting and determining batch consistency of a lithium iron phosphate material. The method comprises the following steps: randomly sampling a lithium iron phosphate material of a batch; detecting main elements, doped elements, and impurity elements in the sampled lithium iron phosphate material, determining the contents of the main elements, doped elements, and impurity elements; determining a particle size distribution curve of the lithium iron phosphate material, determining the numbers, positions, heights, and full widths at half maximum of the peaks in the curve; determining that the consistency of the lithium iron phosphate material of the batch is qualified if the batch fluctuation ranges of the weight percent content parameters of the main elements and the doped elements are equal to or less than 0.5%, and the batch fluctuation range of the content parameter of the impurity elements is less than 50%, and the number of the peaks in the particle size distribution curve does not change, and the fluctuation ranges of the peak positions, heights, and full widths at half maximum are equal to or less than 5%; otherwise, determining that the lithium iron phosphate material of the batch is unqualified. The invention can determine the batch consistency of the lithium iron phosphate material with high efficiency and accuracy.
Description
Technical field
The present invention relates to lithium ion battery field, relate in particular to the method that a kind of LiFePO 4 material batch consistency detection is judged.
Background technology
Operating voltage is high owing to having for lithium ion battery, specific energy density is large, have extended cycle life, self-discharge rate is low, memory-less effect and the advantage such as environmental pollution is little, has first obtained huge success in the field such as mobile communication equipment, mobile electronic device.At present to large-scale energy storage device, the expansion of electric automobile field.
In recent years, due to energy crisis, the climate warming problem that especially greenhouse gas emission causes, is used the eco-friendly power source of low emission to become an urgent demand.Therefore, in recent years, the development and utilization of the clean energy resourcies such as sun power, wind energy has obtained significant progress.But sun power, wind power generation etc. is all the unsettled energy, realizing the prerequisite of generating electricity by way of merging two or more grid systems is the problem that solves energy storage; The advantages such as electric automobile low because discharging (or zero-emission), higher energy conversion efficiency, its research and application have obtained huge progress.The development that new forms of energy strategy in global range is power lithium-ion battery provides a unprecedented platform.
LiFePO4 has long circulation life, high security and becomes the desirable positive electrode of lithium ion battery used for electric vehicle, energy-storage battery compared with high theoretical electrochemistry capacity.
But, because the synthesis condition of LiFePO4 is harsher, if process regulation is bad, very easily there is the situation of the product inconsistency of batch production, thereby the problem that the consistance that causes the ferric phosphate lithium ion battery of being made up of these materials is poor, cause the poor problem of consistance of ferric phosphate lithium ion battery group, thereby cause the harmony of the cell in power battery pack poor, and above-mentioned problem becomes one of Main Bottleneck of the LiFePO4 marketization.
For lithium-ion-power cell manufacturing enterprise, the consistance in power battery pack is problem anxious to be resolved, and the consistance of LiFePO 4 material itself is the conforming basis of electrokinetic cell.Therefore, the conforming reliable method of inspection LiFePO 4 material is all expected to set up by lithium-ion-power cell enterprise.
At present, the conforming common way of inspection LiFePO 4 material is that LiFePO 4 material is in batches sampled, make half cell or full battery, then the electrochemistry capacitance to battery, high rate performance, cycle performance etc. are tested, thereby determine the consistance of LiFePO 4 material by the ferric phosphate lithium ion battery of system.
But, adopt above-mentioned detection mode consuming time longer, and have the inaccurate hidden danger of test.Particularly the inventor finds in research process of the present invention carrying out, and adopts the potential danger that prior art is brought the variation of micro impurity element in material to lack assessment effectively.
Summary of the invention
The invention process the first object is to provide a kind of LiFePO 4 material method that batch consistency detection is judged, whether its consistance that can determine efficiently and accurately LiFePO 4 material batch is qualified, is conducive to ensure the electrical property consistency of the ferric phosphate lithium ion power battery pack of being made up of this batch of material.
The method that a kind of LiFePO 4 material that the present embodiment provides batch consistency detection is judged, comprising:
Get arbitrarily sample batch LiFePO 4 material;
Detect essential element, doped chemical, impurity element in the LiFePO 4 material of each sampling, determine the content of essential element, doped chemical, impurity element;
Determine the grain-size distribution curve of the LiFePO 4 material of each sampling, determine position, the height at peak, the halfwidth at the number at peak in each described curve, each peak;
If a weight percent content parameter batch fluctuation range for the principal element in described LiFePO4 and doped chemical is equal to or less than 0.5%,
And a weight percent content parameter batch fluctuation range for impurity element is less than 50%,
And the number at peak does not change in the grain-size distribution curve of the LiFePO 4 material of each sampling,
And the position at the size-grade distribution peak of the LiFePO 4 material of each sampling, the height at peak, the halfwidth fluctuation range at peak are equal to or less than 5%, judge: the consistance of this batch of LiFePO 4 material is qualified;
Otherwise, judge that this batch of LiFePO 4 material is defective.
Alternatively, described in, mix element and be and improve the element that the chemical property of described LiFePO 4 material adds:
Kation: Mg, Ti, Cr, Cu, Al;
Negative ion: F, Cl.
Alternatively, described impurity element is: Na, Si, Mg, Ti, Cu, Pb, Cd, Cl, K, Ca, Co, Mn, Ni, Cl.
Alternatively, described essential element is: Li, Fe, P, C and O.
Alternatively, using inductive coupling plasma emission spectrograph to detect determines: the content of the metallic element in described essential element, doped chemical, impurity element;
Using carbon and sulfur analytical instrument to detect determines: the mass percentage content of described carbon;
Adopting ion chromatograph to detect determines: the mass percentage content of other nonmetalloids in described essential element, doped chemical, impurity element outside de-carbon.
Therefore, the technical scheme of the application embodiment of the present invention, in research process of the present invention, find carrying out according to the inventor: the physical and chemical index that forms LiFePO 4 material Conformance Assessment is numerous, for batch LiFePO4 of same manufacturer production, the fluctuation of process conditions, can have influence on its all or part of physical and chemical index.And the inventor finds in research process of the present invention:
First: the size-grade distribution of LiFePO 4 material has high susceptibility to the variation of synthetic technological condition, the quality of synthetic technological condition control, will inevitably be reflected in the variation of size-grade distribution of LiFePO 4 material.Therefore, the size-grade distribution situation of material is analyzed, just can be learnt the control status of whole synthesis and production process condition.
Second: in LiFePO 4 material except essential element can impact the chemical property of battery, security performance, trace doped element in material and the unusual fluctuations of micro impurity element also can cause potential threat to the chemical property of battery, security performance, its index has also reflected the situation of the process conditions such as raw-material purity, the cleaning of LiFePO 4 material of synthesizing iron lithium phosphate, therefore, also using the content of each element in material as judging LiFePO 4 material batch conforming steps necessary.
To sum up, use the inventive method to judge fast and accurately a LiFePO 4 material batch consistance fast.
In prior art: by LiFePO4 sampling, make half cell or full battery, the technical scheme that then electrochemistry capacitance to battery, high rate performance, cycle performance etc. are tested.Adopt technical solution of the present invention not only consuming time longer, and the potential danger that the variation of micro impurity element in material is brought lacks assessment effectively, the conforming method of inspection LiFePO 4 material provided by the present invention, for consistance quick, comprehensive assessment LiFePO 4 material, open up new way.
Brief description of the drawings
Accompanying drawing described herein is used to provide a further understanding of the present invention, forms the application's a part, does not form inappropriate limitation of the present invention, in the accompanying drawings:
The one that Fig. 1 provides for the embodiment of the present invention 1
Embodiment
Describe the present invention in detail below in conjunction with accompanying drawing and specific embodiment, be used for explaining the present invention in this illustrative examples of the present invention and explanation, but not as a limitation of the invention.
Embodiment 1:
Shown in Figure 1, the method flow that a kind of LiFePO 4 material that the present embodiment provides batch consistency detection is judged mainly comprises the following steps:
Step 101: get arbitrarily sample batch LiFePO 4 material.
In the LiFePO 4 material of judgement to be detected, sample arbitrarily certain LiFePO 4 material, to sampling is carried out to the detection analysis of step below.
Wherein sampling method can be, but not limited to carry out according to the regulation of GB/T 13732.
Step 102: respectively the essential element in the LiFePO 4 material of each sub-sampling, doped chemical, impurity element are detected, determine the mass percentage content of essential element, doped chemical, impurity element.
Wherein, essential element is the effect positive and negative pole material Constitution Elements in LiFePO4: phosphorus (P), iron (Fe), lithium (Li), oxygen (O).
Doped chemical is to improve the chemical property of LiFePO 4 material and the element that initiatively adds, and this doped chemical pre-determines in material manufacture process.In the time detecting, can test specific doped chemical mass percentage content according to this predetermined situation.
Such as, the inventor is the kation initiatively adulterating in the doped chemical of carrying out the LiFePO 4 material in research process of the present invention: Mg, Ti, Cr, Cu, Al etc. and the initiatively negative ion of doping: F, Cl etc.
Impurity element is due to the various trace elements that starting material are impure or bring in process of production, general according to the knowhow analysis of LiFePO 4 material.
The impurity element of monitoring in experiment such as the inventor generally includes but is not limited to following element: sodium (Na), silicon (Si), magnesium (Mg), titanium (Ti), copper (Cu), plumbous (Pb), cadmium (Cd), chlorine (Cl), potassium (K), calcium (Ca), cobalt (Co), manganese (Mn), nickel (Ni), zinc (Zn) etc.
In the mass percentage content testing process of carrying out various elements of the present invention, can be, but not limited to use the mass percentage content of current inductive coupling plasma emission spectrograph (being called for short ICP-AES) to the metallic element in above-mentioned various essential elements, doped chemical, impurity element in the LiFePO 4 material of sampling to carry out monitoring analysis determines; Use carbon and sulfur analytical instrument to measure the mass percentage content of the carbon in each sampling; Adopt ion chromatograph to measure the mass percentage content of other nonmetalloids in sampling.
Step 103: determine respectively the grain-size distribution curve of LiFePO 4 material of each sub-sampling, determine the following parameter in the corresponding grain-size distribution curve of LiFePO 4 material of every sub-sampling: the number at peak, the position at each peak, the height at peak, halfwidth.
Can be, but not limited in the present embodiment use laser particle size analyzer conventional in prior art (Saturn DigiSizer) to adopt optimum heterogeneity to intersect three-dimensional Fan-Shaped Detector array and without constrained fitting inversion method, measure exactly tested LiFePO 4 material distribution of particle sizes, and obtain grain-size distribution curve according to the result of measuring.
Determine the number of this curve medium wave peak, the position of each crest, height and the halfwidth of each crest according to grain-size distribution curve, to carry out material analysis according to these parameters in step 104.
Step 104: determine that according to step 102,103 testing result whether the consistance of current batch LiFePO 4 material is qualified.
The algorithm whether test material consistance is qualified is specific as follows:
According to the grain-size distribution curve characteristic of each sampling LiFePO 4 material of determining in the element testing result of each sampling LiFePO 4 material of determining in step 102 and step 103, carry out following judgement:
If in the sampling monitoring of each time, a weight percent content parameter batch fluctuation range for principal element in LiFePO4 and doped chemical is equal to or less than 0.5%, and a weight percent content parameter batch fluctuation range for impurity element is less than 50%, and in the grain-size distribution curve of the LiFePO 4 material of each sampling, the number at peak does not change, and the position at the size-grade distribution peak of the LiFePO 4 material of each sampling, the height at peak, the halfwidth fluctuation range at peak are equal to or are less than 5%, judge: the consistance of this batch of LiFePO 4 material is qualified; Otherwise, judge that this batch of LiFePO 4 material is defective.
In research process of the present invention, find carrying out according to the inventor: the physical and chemical index that forms LiFePO 4 material Conformance Assessment is numerous, and for batch LiFePO4 of same manufacturer production, the fluctuation of process conditions, can have influence on its all or part of physical and chemical index.And the inventor finds in research process of the present invention:
First: the size-grade distribution of LiFePO 4 material has high susceptibility to the variation of synthetic technological condition, the quality of synthetic technological condition control, will inevitably be reflected in the variation of size-grade distribution of LiFePO 4 material.Therefore, the size-grade distribution situation of material is analyzed, just can be learnt the control status of whole synthesis and production process condition.
Second: in LiFePO 4 material except essential element can impact the chemical property of battery, security performance, trace doped element in material and the unusual fluctuations of micro impurity element also can cause potential threat to the chemical property of battery, security performance, its index has also reflected the situation of the process conditions such as raw-material purity, the cleaning of LiFePO 4 material of synthesizing iron lithium phosphate, therefore, also using the content of each element in material as judging LiFePO 4 material batch conforming steps necessary.
To sum up, use the inventive method to judge fast and accurately a LiFePO 4 material batch consistance fast.
In prior art: by LiFePO4 sampling, make half cell or full battery, the technical scheme that then electrochemistry capacitance to battery, high rate performance, cycle performance etc. are tested.Adopt technical solution of the present invention not only consuming time longer, and the potential danger that the variation of micro impurity element in material is brought lacks assessment effectively, the conforming method of inspection LiFePO 4 material provided by the present invention, for consistance quick, comprehensive assessment LiFePO 4 material, open up new way.
The technical scheme above embodiment of the present invention being provided is described in detail, applied principle and the embodiment of specific case to the embodiment of the present invention herein and set forth, the explanation of above embodiment is only applicable to help to understand the principle of the embodiment of the present invention; , for one of ordinary skill in the art, according to the embodiment of the present invention, in embodiment and range of application, all will change, in sum, this description should not be construed as limitation of the present invention meanwhile.
Claims (2)
1. the method that LiFePO 4 material batch consistency detection is judged, is characterized in that, comprising:
Get arbitrarily sample batch LiFePO 4 material;
Detect main essential element, doped chemical, impurity element in the LiFePO 4 material of each sampling, determine the content of essential element, doped chemical, impurity element;
Described essential element is: Li, Fe, P, C and O;
Described doped chemical is the element that the chemical property of the described LiFePO 4 material of improvement adds: kation: Mg, Ti, Cr, Cu, Al; Negative ion: F, Cl;
Described impurity element is: Na, Si, Mg, Ti, Cu, Pb, Cd, Cl, K, Ca, Co, Mn, Ni, Cl;
Determine the grain-size distribution curve of the LiFePO 4 material of each sampling, determine position, the height at peak, the halfwidth at the number at peak in each described curve, each peak;
If a weight percent content parameter batch fluctuation range for the principal element in described LiFePO4 and doped chemical is equal to or less than 0.5%,
And a weight percent content parameter batch fluctuation range for impurity element is less than 50%,
And the number at peak does not change in the grain-size distribution curve of the LiFePO 4 material of each sampling,
And the position at the size-grade distribution peak of the LiFePO 4 material of each sampling, the height at peak, the halfwidth fluctuation range at peak are equal to or less than 5%, judge: the consistance of this batch of LiFePO 4 material is qualified;
Otherwise, judge that this batch of LiFePO 4 material is defective.
2. the method that LiFePO 4 material according to claim 1 batch consistency detection is judged, is characterized in that,
Using inductive coupling plasma emission spectrograph to detect determines: the content of the metallic element in described essential element, doped chemical, impurity element;
Using carbon and sulfur analytical instrument to detect determines: the mass percentage content of described carbon;
Adopting ion chromatograph to detect determines: the mass percentage content of other nonmetalloids in described essential element, doped chemical, impurity element outside de-carbon.
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| CN103558208A (en) * | 2013-11-07 | 2014-02-05 | 天津力神电池股份有限公司 | Impurity testing method for nano conductive slurry of lithium ion battery |
| CN110296916A (en) * | 2019-05-29 | 2019-10-01 | 合肥国轩高科动力能源有限公司 | Method for detecting and judging batch compaction stability of high-compaction lithium iron phosphate material |
| CN112763447A (en) * | 2020-12-21 | 2021-05-07 | 中国电子产品可靠性与环境试验研究所（（工业和信息化部电子第五研究所）（中国赛宝实验室）） | Quality consistency improving method |
| CN114048422A (en) * | 2021-09-26 | 2022-02-15 | 东软睿驰汽车技术（沈阳）有限公司 | Battery foreign matter detection method, device and storage medium |
| CN114577884B (en) * | 2022-05-06 | 2022-08-19 | 四川富临新能源科技有限公司 | PH value detection equipment for removing lithium iron phosphate impurities and detection method thereof |
| CN115096983B (en) * | 2022-05-06 | 2024-05-31 | 乳源东阳光新能源材料有限公司 | Method for detecting content of metal impurities in lithium ion battery anode material |
| CN116008848B (en) * | 2023-02-03 | 2024-02-13 | 济南大学 | Application of color difference technology in detection of lithium ion battery electrode material and electrode plate |
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| CN101262053A (en) * | 2008-04-29 | 2008-09-10 | 张守文 | A method for making Fe lithium phosphate compound anode material |
| CN101276909A (en) * | 2007-02-28 | 2008-10-01 | 三洋电机株式会社 | Method of producing active material for lithium secondary battery, method of producing electrode for lithium secondary battery, method of producing lithium secondary battery, and method of monitoring |
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| TWI548589B (en) * | 2008-10-22 | 2016-09-11 | Ｌｇ化學股份有限公司 | Lithium iron phosphate having olivine structure and method for analyzing the same |
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| CN101276909A (en) * | 2007-02-28 | 2008-10-01 | 三洋电机株式会社 | Method of producing active material for lithium secondary battery, method of producing electrode for lithium secondary battery, method of producing lithium secondary battery, and method of monitoring |
| CN101262053A (en) * | 2008-04-29 | 2008-09-10 | 张守文 | A method for making Fe lithium phosphate compound anode material |
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