CN110031490A - The appraisal procedure of ternary cathode material of lithium ion battery thermal run away - Google Patents
The appraisal procedure of ternary cathode material of lithium ion battery thermal run away Download PDFInfo
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- 239000010406 cathode material Substances 0.000 title claims abstract description 152
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 133
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 132
- 238000000034 method Methods 0.000 title claims abstract description 45
- 238000001228 spectrum Methods 0.000 claims abstract description 44
- 238000000155 in situ X-ray diffraction Methods 0.000 claims abstract description 38
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 238000012545 processing Methods 0.000 claims abstract description 24
- 238000005516 engineering process Methods 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims description 9
- 229910000831 Steel Inorganic materials 0.000 claims description 7
- 239000010959 steel Substances 0.000 claims description 7
- 238000011156 evaluation Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- OXHNLMTVIGZXSG-UHFFFAOYSA-N 1-Methylpyrrole Chemical compound CN1C=CC=C1 OXHNLMTVIGZXSG-UHFFFAOYSA-N 0.000 claims description 4
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 4
- 238000005096 rolling process Methods 0.000 claims description 4
- 239000002390 adhesive tape Substances 0.000 claims description 3
- 238000002224 dissection Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 125000006850 spacer group Chemical group 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims 1
- 239000012071 phase Substances 0.000 description 29
- 230000007704 transition Effects 0.000 description 18
- 239000013078 crystal Substances 0.000 description 17
- 238000006243 chemical reaction Methods 0.000 description 14
- 238000012360 testing method Methods 0.000 description 11
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 10
- 239000000203 mixture Substances 0.000 description 10
- 239000011029 spinel Substances 0.000 description 9
- 229910052596 spinel Inorganic materials 0.000 description 9
- 230000009466 transformation Effects 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 239000002872 contrast media Substances 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 239000007774 positive electrode material Substances 0.000 description 3
- 238000009736 wetting Methods 0.000 description 3
- 229910017229 Ni0.8Co0.15Al0.05O2 Inorganic materials 0.000 description 2
- 102220494497 Ras-related protein Rab-5C_S85E_mutation Human genes 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011066 ex-situ storage Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 235000002639 sodium chloride Nutrition 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000002083 X-ray spectrum Methods 0.000 description 1
- 230000003281 allosteric effect Effects 0.000 description 1
- 210000000080 chela (arthropods) Anatomy 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
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- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
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- 239000000047 product Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
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- 239000012465 retentate Substances 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/20025—Sample holders or supports therefor
- G01N23/20033—Sample holders or supports therefor provided with temperature control or heating means
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Abstract
The present invention provides a kind of appraisal procedures of ternary cathode material of lithium ion battery thermal run away, ternary cathode material of lithium ion battery thermal run away is assessed using in situ X-ray diffraction diffractive technology, the following steps are included: providing the lithium ion battery of tertiary cathode material, the lithium ion battery is charged to different SOC states；By the lithium ion battery dismantling after charging, and collect the tertiary cathode material on anode pole piece；The tertiary cathode material is placed on the sample stage of in situ X-ray diffraction diffractometer, under vacuum conditions, sample is heated with the heating rate of 0.5 DEG C~1.5 DEG C/min, the scanning speed that in situ X-ray diffraction diffractometer is arranged is that 2.8~4.8 °/min, 2 θ of scanning angle are at least 15-72 °, full scan processing is carried out to the tertiary cathode material, obtains scanning spectra；The thermostabilization range of the tertiary cathode material is determined according to scanning spectra.
Description
Technical field
The invention belongs to technical field of lithium ion more particularly to a kind of ternary cathode material of lithium ion battery thermal run aways
Appraisal procedure.
Background technique
With the aggravation of energy crisis and the deterioration of environment, people's urgent need clean energy resource replaces traditional fossil energy
Source.Capacity is high, has extended cycle life and advantages of environment protection because having for lithium ion battery, is increasingly valued by people.
Lithium ion battery substitution internal combustion engine is used to have begun as the new-energy automobile of automobile power at present universal, but with universal
Popularization and the reason of pursue high-energy density, cause new-energy automobile some safety problems occur.Lithium-ion-power cell peace
The thermal runaway for being mainly shown as lithium ion battery of full sexual behavior event, is embodied in the phenomenon on fire of electric car.Analyze its original
Cause, predominantly lithium ion battery are outside normal discharge and recharge reaction, and there is also many potential exothermic auxiliary reactions, such as Charging state anode
Thermal decomposition, SEI film decomposes causes electrolyte in the reduction decomposition of exposed high-activity carbon negative terminal surface and the heat point of electrolyte
The generation of the exothermic auxiliary reactions such as solution, is likely to lead to the thermal runaway of lithium ion battery.Particularly, Charging state lithium ion battery three
First positive electrode can undergo phase transition a large amount of heat of generation and oxygen, the heat and oxygen of generation at high temperature can aggravate lithium ion
The generation of battery exothermic auxiliary reaction, therefore tertiary cathode material phase pole-changing is unfavorable for the security performance of lithium ion battery.
X-ray diffraction technical principle is to generate on its back side egative film when X-ray is with specific direction entrance crystal structure
The diffracting spectrum of regular distribution.The composition and element phase of sample can be analyzed according to ex-situ X-ray diffraction map
To content, but these information are far from being enough for the thermal stability for assessing lithium ion battery.
Summary of the invention
The purpose of the present invention is to provide a kind of appraisal procedures of ternary cathode material of lithium ion battery thermal run away, it is intended to solve
Certainly the prior art cannot effectively assess the problem of thermal stability of lithium-ion batteries.
For achieving the above object, The technical solution adopted by the invention is as follows:
The present invention provides a kind of appraisal procedure of ternary cathode material of lithium ion battery thermal run away, is spread out using in situ X-ray diffraction
Penetrate technology evaluation ternary cathode material of lithium ion battery thermal run away, comprising the following steps:
The lithium ion battery of tertiary cathode material is provided, the lithium ion battery is charged to different SOC states；
By the lithium ion battery dismantling after charging, and collect the tertiary cathode material on anode pole piece；
The tertiary cathode material is placed on the sample stage of in situ X-ray diffraction diffractometer, under vacuum conditions, with 0.5 DEG C
The heating rate of~1.5 DEG C/min heats sample, and the scanning speed of setting in situ X-ray diffraction diffractometer is 2.8~4.8 °/min, sweeps
It retouches 2 θ of angle and is at least 15-72 °, full scan processing is carried out to the tertiary cathode material, obtains scanning spectra；
Thermostabilization range of the tertiary cathode material under corresponding SOC state is determined according to scanning spectra.
Preferably, in the step of being scanned processing to the tertiary cathode material, obtaining scanning spectra, scanning temperature is preset
Spending range is 25 DEG C~500 DEG C, and actual scanning temperature range at least crosses over 300 DEG C.
Preferably, in the step of being scanned processing to the tertiary cathode material, obtaining scanning spectra, actual scanning temperature
Spending range is 25 DEG C~500 DEG C.
Preferably, in the step of lithium ion battery being charged to different SOC states, the lithium ion battery is being filled
Electric multiplying power be 0.5C, blanking voltage be respectively 3.90V, 3.95V, 4.00V, 4.05V, 4.10V, 4.15V, 4.20V, 4.25V and
Charging process is carried out under conditions of 4.30V, obtains the different SOC states of lithium ion battery.
Preferably, the lithium ion battery after charging is disassembled, and the step of collecting the tertiary cathode material on anode pole piece
In, after the anode pole piece is carried out soaking and washing processing, drying with dimethyl carbonate, just using the wetting of N- methyl pyrrole alkanone
After the pole piece of pole, the tertiary cathode material on anode pole piece is collected.
Preferably, the lithium ion battery after charging is disassembled, and the step of collecting the tertiary cathode material on anode pole piece
In, tertiary cathode material is scraped along a direction on the anode pole piece using scraper.
It preferably, further include by the tertiary cathode material after the step of collecting the tertiary cathode material on anode pole piece
Material is ground.
Preferably, the lithium ion battery be cylindrical battery, and by after charging lithium ion battery disassemble the step of, packet
It includes: in the environment of relative humidity is lower than 10%RH, thermal shrinkable sleeve is removed since negative electrode of lithium ion battery end；Along slot rolling notch
It cuts battery core and tab is straightened in cap pull-up, positive pole ear is wiped out along upper insulation spacer surface with pliers in parallel cells direction；
Steel shell is splitted along faucal edge coils solution, avoids the housing parts dismantled to puncture pole group short circuit in anatomic course, dissects under
When section part, steel shell is pulled out into tab along pole group axial direction negative pole end, negative lug is cut, takes out pole group；With blade along pole
Group diaphragm terminated line cuts terminal adhesive tape, and core, anode pole piece of tearing is unfolded.
Preferably, in the step of carrying out full scan processing to the tertiary cathode material, obtaining scanning spectra, setting is in situ
The scanning speed of X-ray diffractometer is 3.8 °/min, 2 θ of scanning angle is 15-72 °, with the heating rate of 1.2 DEG C/min by sample
Product temperature degree rises to 500 DEG C from 25 DEG C, collects scanning spectra.
The appraisal procedure of ternary cathode material of lithium ion battery thermal run away provided by the invention, has the advantage that
Firstly, carrying out procedural in situ X-ray diffraction Diffraction scans in sample heating process to sample, learning lithium-ion electric
All diffracting spectrums of the tertiary cathode material in Range of measuring temp in pond.And then it (can be by JADE software point by analysis
Analysis) diffracting spectrum of ternary cathode material of lithium ion battery, the variation of contrast material composition and crystal structure, energy under different temperatures
The information such as the phase transition temperature of ternary cathode material of lithium ion battery are accessed, so as to effectively assess lithium ion battery in high temperature
Thermal run away situation under environment finally determines thermostabilization range of the tertiary cathode material under corresponding SOC state.
Secondly, being risen with the heating rate of 0.5 DEG C~1.5 DEG C/min to the tertiary cathode material of test in the present invention
Temperature processing, meanwhile, in situ X-ray diffraction is carried out with ternary positive electrode active material of the scanning speed of 2.8~4.8 °/min to test and is spread out
Penetrate scanning.With this condition, since heating rate is slower, be conducive to tertiary cathode material and sufficiently undergo phase transition under high temperature environment
Reaction；Scanning speed is fast simultaneously, and the temperature difference of the high angle of diffraction of X-ray diffraction spectrum and low angle of diffraction is just smaller, is easily obtained
More fine diffracting spectrum finally obtains more accurate assessment result.Further, since 2 θ of scanning angle is arranged the present invention
It is 15-72 °, thus, it is possible to obtain ternary positive electrode active material whole diffraction situation in range, and then according to different temperatures item
The diffraction peak intensity of ternary positive electrode active material and diffraction maximum situation under part preferably determine phase transformation situation.
Detailed description of the invention
Fig. 1 is 4.20V provided in an embodiment of the present invention, is carried out to the tertiary cathode material NCM tertiary cathode material complete
Scan process, obtained in situ X-ray diffraction diffraction pattern；
Fig. 2 is that the appraisal procedure for the ternary cathode material of lithium ion battery thermal run away that the embodiment of the present invention 1 provides obtains
4.20V thermal run away situation map；
Fig. 3 is the appraisal procedure crystal knot for the ternary cathode material of lithium ion battery thermal run away that the embodiment of the present invention 1 provides
Structure and phase transition temperature situation map；
Fig. 4 is that the appraisal procedure for the ternary cathode material of lithium ion battery thermal run away that the embodiment of the present invention 2 provides obtains
4.20V thermal run away situation map；
Fig. 5 is that the appraisal procedure for the ternary cathode material of lithium ion battery thermal run away that the embodiment of the present invention 3 provides obtains
4.20V thermal run away situation map；
Fig. 6 is that the appraisal procedure for the ternary cathode material of lithium ion battery thermal run away that the embodiment of the present invention 4 provides obtains
4.20V thermal run away situation map.
Specific embodiment
In order to which technical problems, technical solutions and advantageous effects to be solved by the present invention are more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain
The present invention is not intended to limit the present invention.
In the description of the present invention, it is to be understood that, term " first ", " second " are used for description purposes only, and cannot
It is interpreted as indication or suggestion relative importance or implicitly indicates the quantity of indicated technical characteristic.Define as a result, " the
One ", the feature of " second " can explicitly or implicitly include one or more of the features.In the description of the present invention,
The meaning of " plurality " is two or more, unless otherwise specifically defined.
The embodiment of the present invention provides a kind of appraisal procedure of ternary cathode material of lithium ion battery thermal run away, using X in situ
Ray diffraction techniques assess ternary cathode material of lithium ion battery thermal run away, comprising the following steps:
S01., the lithium ion battery of tertiary cathode material is provided, the lithium ion battery is charged to different SOC states；
S02. the lithium ion battery after charging is disassembled, and collects the tertiary cathode material on anode pole piece；
S03. the tertiary cathode material is placed on the sample stage of in situ X-ray diffraction diffractometer, under vacuum conditions, with
The heating rate of 0.5 DEG C~1.5 DEG C/min heats sample, and the scanning speed of setting in situ X-ray diffraction diffractometer is 2.8~4.8 °/
Min, 2 θ of scanning angle are at least 15-72 °, carry out full scan processing to the tertiary cathode material, obtain scanning spectra；S04.
Thermostabilization range of the tertiary cathode material under corresponding SOC state is determined according to scanning spectra.
The appraisal procedure of ternary cathode material of lithium ion battery thermal run away provided in an embodiment of the present invention has following excellent
Point:
Firstly, carrying out procedural in situ X-ray diffraction Diffraction scans in sample heating process to sample, learning lithium-ion electric
All diffracting spectrums of the tertiary cathode material in Range of measuring temp in pond.And then it (can be by JADE software point by analysis
Analysis) diffracting spectrum of ternary cathode material of lithium ion battery, the variation of contrast material composition and crystal structure, energy under different temperatures
The information such as the phase transition temperature of ternary cathode material of lithium ion battery are accessed, so as to effectively assess lithium ion battery in high temperature
Thermal run away situation under environment finally determines thermostabilization range of the tertiary cathode material under corresponding SOC state.
Secondly, in the embodiment of the present invention, with the heating rate of 0.5 DEG C~1.5 DEG C/min to the tertiary cathode material of test
Heating treatment is carried out, meanwhile, in situ X-ray diffraction is carried out with tertiary cathode material of the scanning speed of 2.8~4.8 °/min to test
Diffraction scans.With this condition, since heating rate is slower, be conducive to tertiary cathode material and phase sufficiently occurs under high temperature environment
Become reaction；Scanning speed is fast simultaneously, and the temperature difference of the high angle of diffraction of X-ray diffraction spectrum and low angle of diffraction is just smaller, is easy to obtain
More fine diffracting spectrum is obtained, more accurate assessment result is finally obtained.Further, since the embodiment of the present invention is by scan angle
It spends 2 θ and is set as 15-72 °, thus, it is possible to obtain tertiary cathode material whole diffraction situation in range, and then according to not equality of temperature
The diffraction peak intensity of tertiary cathode material and diffraction maximum situation under the conditions of degree preferably determine phase transformation situation.
Specifically, the lithium ion battery is charged to different SOC states in above-mentioned steps S01, SOC (the charged shape
State) state according to the working condition of the lithium ion battery of specific tertiary cathode material determine.Such as the lithium-ion electric of tertiary cathode material A
Pond is usually A in rate of charge1C, blanking voltage is A2It works under conditions of V, then, in order to assess the lithium under the working condition
The lithium ion battery can be A in rate of charge by the thermal stability of ion battery1C, blanking voltage is A2Under conditions of V into
Row charging process.Certainly, in order to obtain the thermal stability under the unified a variety of difference SOC states of battery, a variety of difference SOC can be set
The evaluated in parallel of state detects.
In some embodiments, in the step of lithium ion battery being charged to different SOC states, by the lithium ion
Battery rate of charge be 0.5C, blanking voltage be respectively 3.90V, 3.95V, 4.00V, 4.05V, 4.10V, 4.15V, 4.20V,
Charging process is carried out under conditions of 4.25V and 4.30V, obtains the different SOC states of lithium ion battery.Under the charge condition, lithium from
A possibility that SOC higher of sub- battery, generation thermal run away, is bigger, and occurs to react more violent, the value of assessment when thermal run away
It is bigger.
In certain embodiments, after before charging, first lithium ion battery is placed on charge-discharge test instrument and is stood
Processing, time of repose are preferably greater than or equal to 30 minutes, so that lithium ion battery charges under stable condition, and positive electrode is in
Stable SOC state provides state to tertiary cathode material progress thermal stability evaluation using in situ X-ray diffraction diffractive technology to be subsequent
Basis.
In above-mentioned steps S02, the lithium ion battery after charging is disassembled, to obtain the anode pole piece of lithium ion battery.
Specifically, the method for dismantling lithium ion battery, can have different disassembling methods according to specific lithium ion battery type.
In some embodiments, when the lithium ion battery is cylindrical lithium ion battery, by the lithium ion after charging
The step of battery is disassembled, comprising: in the environment of relative humidity is lower than 10%RH, heat is removed since negative electrode of lithium ion battery end
Contracting set；Tab, parallel cells direction, with pliers along upper insulation spacer is straightened in cap pull-up along slot rolling notches cut battery core
Wipe out positive pole ear in surface；Steel shell is splitted along faucal edge coils solution, avoids the housing parts dismantled from puncturing in anatomic course
Steel shell when dissection to the lower section, is pulled out tab along pole group axial direction negative pole end, cuts negative lug, take out by the short circuit of pole group
Pole group；Terminal adhesive tape is cut along pole group diaphragm terminated line with blade, core, anode pole piece of tearing is unfolded.Specifically, relatively wet
Degree lower than 10%RH environment be preferably be provided with dehumidifier profession dissection room, can prevent steam to lithium ion battery ternary just
The influence of pole material.It can be handled using nozzle pincers along slot rolling notches cut battery core；It is dissected along faucal edge coils
Opening steel shell can be handled using diagonal cutting pliers.In this way, during being disassembled to avoid lithium ion battery, the anode
Pole piece is destroyed, and guarantees its integrality, and then the pattern of the tertiary cathode material on guarantee anode pole piece is complete, and then ensures
The accuracy of tertiary cathode material phase transition temperature is determined using in situ X-ray diffraction diffraction.
Collecting obtained anode pole piece need to seal up for safekeeping in closed environment, avoid contact steam and oxygen.
Preferably, the lithium ion battery after charging is disassembled, and the step of collecting the tertiary cathode material on anode pole piece
In, after the anode pole piece is carried out soaking and washing processing, drying with dimethyl carbonate, just using the wetting of N- methyl pyrrole alkanone
After the pole piece of pole, the tertiary cathode material on anode pole piece is collected.The anode pole piece is carried out at immersion using dimethyl carbonate
Reason, can remove lithium ion battery side reaction retentate and electrolyte component；It is preferred that impregnate 30 minutes or more.Soaking processing
Afterwards, the anode pole piece is spontaneously dried.Positive pole is scraped after further carrying out wetting anode pole piece using N- methyl pyrrole alkanone
Piece is detached from, to collect the tertiary cathode material on anode pole piece from collection liquid surface convenient for tertiary cathode material.
Further, the lithium ion battery after charging is disassembled, and collects the step of the tertiary cathode material on anode pole piece
In rapid, scraped on the anode pole piece along a direction using scraper and collect tertiary cathode material.(edge by this way
A direction), can be to avoid the pattern damage of tertiary cathode material, and then guarantee the standard of in situ X-ray diffraction diffraction patterns
True property.
Further, collect anode pole piece on tertiary cathode material the step of after, further include by the ternary just
Pole material is ground, and tertiary cathode material is made to be uniformly dispersed.The milled processed carries out preferably in mortar, in order to
Tertiary cathode material material dispersion is uniform, and does not allow destructible material morphology.
In above-mentioned steps S03, the tertiary cathode material is placed on the sample stage of in situ X-ray diffraction diffractometer, to sample
Environmental chamber locating for platform vacuumizes, and is in test sample in vacuum environment, prevents sample under hot environment from oxidation reaction occurs.
In the embodiment of the present invention, sample is heated with the heating rate of 0.5 DEG C~1.5 DEG C/min, using in situ X-ray diffraction diffraction
Technology scans the sample diffraction map in heating temperature range, by comparing diffraction peak intensity and position in sample diffraction map
Variation obtains the variation of Matter Composition and crystal structure, obtains the information such as the phase transition temperature of ternary cathode material of lithium ion battery,
Effectively pass through the information evaluation lithium ion battery collected thermal run away situation in a high temperauture environment.Wherein, it will heat up rate control
In 0.5 DEG C~1.5 DEG C/min, heating rate is slower, and reaction time of the tertiary cathode material in pyroreaction region is more sufficient, instead
Should be more abundant, tertiary cathode material could sufficiently undergo phase transition reaction under high temperature environment.And when heating rate is too fast, it may
So that the reaction in this pyroreaction region is skipped over due to busy reaction, reaction can not be undergone phase transition.It is furthermore preferred that with 1.2
DEG C/heating rate of min heats sample, it slowly heats up, tertiary cathode material is made sufficiently to undergo phase transition reaction under high temperature environment,
The smaller diffracting spectrum of the temperature difference is obtained simultaneously, and then obtains the change information of more accurately Matter Composition and crystal structure, effectively
Lithium ion battery thermal run away situation in a high temperauture environment is assessed, finally determines the tertiary cathode material under corresponding SOC state
Thermostabilization range.
In the embodiment of the present invention, in the step of being scanned processing to the tertiary cathode material, obtain scanning spectra, in advance
If scanning temperature range is 25 DEG C~500 DEG C, i.e. scanning temperature range can specifically scan model within the scope of 25 DEG C~500 DEG C
The temperature starting point enclosed can be with flexible setting, but actual scanning temperature range at least crosses over 300 DEG C, so as to obtain more temperature
The scanning spectra of point is spent, to obtain finer scanning spectra, and then guarantees the accuracy and reliability of pattern analysis results.
In particular preferred embodiment, the step of being scanned processing to the tertiary cathode material, obtain scanning spectra
In, actual scanning temperature range is 25 DEG C~500 DEG C.I.e. with the heating rate of 0.5 DEG C~1.5 DEG C/min, by the three of test
First positive electrode is warming up to 500 DEG C from 25 DEG C, and the diffracting spectrum collected in the temperature range compares and analyzes, contrast material at
The variation of part and crystal structure, obtains the information such as the phase transition temperature of ternary cathode material of lithium ion battery, so as to effectively comment
Estimate lithium ion battery thermal run away situation in a high temperauture environment.
In the embodiment of the present invention, the scanning speed of the in situ X-ray diffraction diffractometer is 2.8~4.8 °/min, scanning angle 2
θ is at least 15-72 °.Under the condition of scanning, scanning speed is fast, the high angle of diffraction of the faster X-ray diffraction spectrum of scanning speed and low spreads out
The temperature difference of firing angle degree is just smaller, and assessment is accurate；Simultaneously as 2 θ of scanning angle covers 15-72 ° of range, it is available to be somebody's turn to do
The whole diffraction situation of tertiary cathode material in range, so can with tertiary cathode material in range whole diffraction situation.It keeps away
When exempting to be scanned by single scanning speed and single scanning angle, diffraction maximum substance shifts or imperfect, causes
Accurately derivative profile information can not be obtained, and then the variation of Matter Composition and crystal structure can not be obtained.Certainly, it should manage
Solution, X-ray spectrum angle of diffraction may range from 0-90 °, but since tertiary cathode material does not have in lower or higher angle of diffraction
Diffractive features peak, therefore, preferred 2 θ of scanning angle of the embodiment of the present invention are 15-72 °.
In one embodiment, by taking 4.20VNCM tertiary cathode material as an example, the step to the tertiary cathode material into
The processing of row full scan, obtained three-dimensional in situ X-ray diffraction diffraction pattern are shown in Fig. 1.
In particular preferred embodiment, full scan processing is carried out to the tertiary cathode material, obtains the step of scanning spectra
In rapid, the scanning speed of setting in situ X-ray diffraction diffractometer is 3.8 °/min, 2 θ of scanning angle is 15-72 °, with 1.2 DEG C/min's
Sample temperature is risen to 500 DEG C from 25 DEG C by heating rate, collects scanning spectra, to help to obtain more accurate assessment knot
Fruit.
In above-mentioned steps S04, according to the diffracting spectrum that step S03 is scanned in scanning temperature range, substance is analyzed
The variation of composition and crystal structure, and then the information such as phase transition temperature for determining ternary cathode material of lithium ion battery, are effectively assessed
Lithium ion battery thermal run away situation in a high temperauture environment finally determines heat of the tertiary cathode material under corresponding SOC state
Stability range, i.e. safety.
With ex-situ X-ray diffraction Technical comparing, in situ X-ray diffraction diffractive technology can effectively analyze vary with temperature lithium from
The variation of sub- battery tertiary cathode material Matter Composition and crystal structure.Pass through the object of tertiary cathode material under analysis different temperatures
The variation of matter composition and crystal structure can obtain the phase transition temperature of ternary cathode material of lithium ion battery, the letter such as oxygen release temperature
Breath, so as to effectively assess lithium ion battery thermal run away situation in a high temperauture environment.Such as tertiary cathode material
Li0.33Ni0.8Co0.15Al0.05O2Blanking voltage is 4.12VvsLi/Li+, phase transformation reaction equation is With
Tertiary cathode material Li0.33Ni0.8Co0.15Al0.05O2Can generate a large amount of heat and oxygen when undergoing phase transition, a large amount of heat and
Oxygen aggravates the generation of lithium ion battery exothermic auxiliary reaction, and lithium ion battery exothermic auxiliary reaction will lead to thermal runaway, pole
It is unfavorable for the security performance of lithium ion battery.
By using the method, we have evaluated the tertiary cathode material of four sections of different Ni contents, find four sections of difference nickel
The phase transition temperature that content tertiary cathode material layer structure mutually changes to spinel structure mutually changes to rock salt with spinel structure and mutually ties
The phase transition temperature of structure is all different.By analyzing phase transition temperature, we obtain the thermal safety of four sections of tertiary cathode materials are as follows: N1L
> S85E > S800 > EO211.It is illustrated combined with specific embodiments below.
Embodiment 1
A kind of appraisal procedure of ternary cathode material of lithium ion battery thermal run away is assessed using in situ X-ray diffraction diffractive technology
Ternary cathode material of lithium ion battery thermal run away, comprising the following steps:
Lithium ion battery S800 is provided, by the lithium ion battery rate of charge is 0.5C, blanking voltage is 4.20V's
Under the conditions of carry out charging process, charging front and back battery stands 30min on charge-discharge test instrument；
By the lithium ion battery dismantling after charging, and collect the tertiary cathode material on anode pole piece；
The tertiary cathode material is placed on the sample stage of in situ X-ray diffraction diffractometer, under vacuum conditions, with 0.5 DEG C
Sample is heated to 500 DEG C from 25 DEG C by the heating rate of~1.5 DEG C/min, and the scanning speed of setting in situ X-ray diffraction diffractometer is
3.8 °/min, 2 θ of scanning angle be 15-72 °, to the tertiary cathode material carry out full scan processing, obtain scanning spectra；
Thermostabilization range of the tertiary cathode material under corresponding SOC state is determined according to scanning spectra.
The appraisal procedure for the ternary cathode material of lithium ion battery thermal run away that embodiment 1 provides, obtained 4.20V thermal run away
Situation map is as shown in Fig. 2, as seen from the figure, and (108) and the division of (110) peak are obvious at 30 DEG C, shows that crystal is layer structure；84℃
When (108) and the fusion of (110) peak, (003) peak intensity is substantially reduced, shows that layer structure has been destroyed, start to spinelle knot
Allosteric transformation；Occur (021) (202) (111) diffraction maximum of rock salt structure NiO at 156 DEG C, shows that rock salt structure initially forms.Three
Crystal structure and the phase transition temperature of first positive electrode stratiform phase, Spinel and rock salt phase are as shown in figure 3, the corresponding X-ray of Fig. 2
The corresponding Matter Composition of diffraction crystal face is as shown in table 1 below.
Table 1
Embodiment 2
A kind of appraisal procedure of ternary cathode material of lithium ion battery thermal run away is assessed using in situ X-ray diffraction diffractive technology
Ternary cathode material of lithium ion battery thermal run away, comprising the following steps:
Lithium ion battery N1L is provided, by the lithium ion battery rate of charge is 0.5C, blanking voltage is 4.20V's
Under the conditions of carry out charging process, charging front and back battery stands 30min on charge-discharge test instrument；
By the lithium ion battery dismantling after charging, and collect the tertiary cathode material on anode pole piece；
The tertiary cathode material is placed on the sample stage of in situ X-ray diffraction diffractometer, under vacuum conditions, with 0.5 DEG C
Sample is heated to 500 DEG C from 25 DEG C by the heating rate of~1.5 DEG C/min, and the scanning speed of setting in situ X-ray diffraction diffractometer is
3.8 °/min, 2 θ of scanning angle be 15-72 °, to the tertiary cathode material carry out full scan processing, obtain scanning spectra；
Thermostabilization range of the tertiary cathode material under corresponding SOC state is determined according to scanning spectra.
The appraisal procedure for the ternary cathode material of lithium ion battery thermal run away that embodiment 2 provides, obtained 4.20V thermal run away
Situation map is as shown in figure 4, as seen from the figure, and (108) and the division of (110) peak are obvious at 30 DEG C, shows that crystal is layer structure；156
DEG C when (108) and (110) peak permeate peak, show that layer structure has been destroyed, be at this time spinel structure；At 372 DEG C
There is (021) (202) (220) diffraction maximum of rock salt structure NiO, shows that spinel structure is to rock salt structure phase transformation at this time.
Embodiment 3
A kind of appraisal procedure of ternary cathode material of lithium ion battery thermal run away is assessed using in situ X-ray diffraction diffractive technology
Ternary cathode material of lithium ion battery thermal run away, comprising the following steps:
There is provided lithium ion battery EO211, by the lithium ion battery rate of charge be 0.5C, blanking voltage 4.20V
Under conditions of carry out charging process, charging front and back battery stands 30min on charge-discharge test instrument；
By the lithium ion battery dismantling after charging, and collect the tertiary cathode material on anode pole piece；
The tertiary cathode material is placed on the sample stage of in situ X-ray diffraction diffractometer, under vacuum conditions, with 0.5 DEG C
Sample is heated to 500 DEG C from 25 DEG C by the heating rate of~1.5 DEG C/min, and the scanning speed of setting in situ X-ray diffraction diffractometer is
3.8 °/min, 2 θ of scanning angle be 15-72 °, to the tertiary cathode material carry out full scan processing, obtain scanning spectra；
Thermostabilization range of the tertiary cathode material under corresponding SOC state is determined according to scanning spectra.
The appraisal procedure for the ternary cathode material of lithium ion battery thermal run away that embodiment 3 provides, obtained 4.20V thermal run away
Situation map is as shown in figure 5, as seen from the figure, and (108) and the division of (110) peak are obvious at 30 DEG C, and crystal is layer structure；At 120 DEG C
Layer structure has been destroyed, and starts to be changed into spinel structure；Occurs (202) (104) diffraction of rock salt structure NiO at 138 DEG C
Peak shows that spinel structure is to rock salt structure phase transformation at this time.
Embodiment 4
A kind of appraisal procedure of ternary cathode material of lithium ion battery thermal run away is assessed using in situ X-ray diffraction diffractive technology
Ternary cathode material of lithium ion battery thermal run away, comprising the following steps:
Lithium ion battery S85E is provided, in rate of charge is that 0.5C, blanking voltage are respectively by the lithium ion battery
Charging process is carried out under conditions of 4.20V, charging front and back battery stands 30min on charge-discharge test instrument；
By the lithium ion battery dismantling after charging, and collect the tertiary cathode material on anode pole piece；
The tertiary cathode material is placed on the sample stage of in situ X-ray diffraction diffractometer, under vacuum conditions, with 0.5 DEG C
Sample is heated to 500 DEG C from 25 DEG C by the heating rate of~1.5 DEG C/min, and the scanning speed of setting in situ X-ray diffraction diffractometer is
3.8 °/min, 2 θ of scanning angle be 15-72 °, to the tertiary cathode material carry out full scan processing, obtain scanning spectra；
Thermostabilization range of the tertiary cathode material under corresponding SOC state is determined according to scanning spectra.
The appraisal procedure for the ternary cathode material of lithium ion battery thermal run away that embodiment 4 provides, obtained 4.20V thermal run away
Situation map is as shown in fig. 6, as seen from the figure, and (108) and the division of (110) peak are obvious at 30 DEG C, shows that crystal is layer structure；138
DEG C when layer structure have begun destruction, to spinel structure change；Occurs rock salt structure Ni at 210 DEG C6MnO8(111) spread out
Peak is penetrated, shows that spinel structure is to rock salt structure phase transformation at this time；The main peak of 318 DEG C~500 DEG C of diffracting spectrums always exists lithiumation
Object shows non-complete deactivation.
To sum up, the type and thermal stability evaluation result of four sections of tertiary cathode materials are as shown in table 2 below.
Table 2
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (9)
1. a kind of appraisal procedure of ternary cathode material of lithium ion battery thermal run away, which is characterized in that use in situ X-ray diffraction diffraction
Technology evaluation ternary cathode material of lithium ion battery thermal run away, comprising the following steps:
The lithium ion battery of tertiary cathode material is provided, the lithium ion battery is charged to different SOC states；
By the lithium ion battery dismantling after charging, and collect the tertiary cathode material on anode pole piece；
The tertiary cathode material is placed on the sample stage of in situ X-ray diffraction diffractometer, under vacuum conditions, with 0.5 DEG C~1.5
DEG C/heating rate of min heats sample, the scanning speed of setting in situ X-ray diffraction diffractometer is 2.8~4.8 °/min, scan angle
It spends 2 θ and is at least 15-72 °, full scan processing is carried out to the tertiary cathode material, obtains scanning spectra；
Thermostabilization range of the tertiary cathode material under corresponding SOC state is determined according to scanning spectra.
2. the appraisal procedure of ternary cathode material of lithium ion battery thermal run away as described in claim 1, which is characterized in that institute
It states in the step of tertiary cathode material is scanned processing, obtains scanning spectra, presetting scanning temperature range is 25 DEG C~500
DEG C, and actual scanning temperature range at least crosses over 300 DEG C.
3. the appraisal procedure of ternary cathode material of lithium ion battery thermal run away as claimed in claim 2, which is characterized in that institute
It states in the step of tertiary cathode material is scanned processing, obtains scanning spectra, actual scanning temperature range is 25 DEG C~500
℃。
4. the appraisal procedure of ternary cathode material of lithium ion battery thermal run away as claimed in any one of claims 1 to 3, feature
In the step of being, the lithium ion battery is charged to different SOC states, it is in rate of charge by the lithium ion battery
0.5C, blanking voltage are respectively the item of 3.90V, 3.95V, 4.00V, 4.05V, 4.10V, 4.15V, 4.20V, 4.25V and 4.30V
Charging process is carried out under part, obtains the different SOC states of lithium ion battery.
5. the appraisal procedure of ternary cathode material of lithium ion battery thermal run away as claimed in any one of claims 1 to 3, feature
Be, the lithium ion battery after charging disassembled, and in the step of collecting the tertiary cathode material on anode pole piece, by it is described just
After pole pole piece carries out soaking and washing processing, drying with dimethyl carbonate, after soaking anode pole piece using N- methyl pyrrole alkanone, receive
Collect the tertiary cathode material on anode pole piece.
6. the appraisal procedure of ternary cathode material of lithium ion battery thermal run away as claimed in claim 5, which is characterized in that will fill
Lithium ion battery dismantling after electricity, and in the step of collecting the tertiary cathode material on anode pole piece, using scraper it is described just
Tertiary cathode material is scraped along a direction on the pole piece of pole.
7. the appraisal procedure of ternary cathode material of lithium ion battery thermal run away as claimed in claim 6, which is characterized in that collect
It further include being ground the tertiary cathode material after the step of tertiary cathode material on anode pole piece.
8. the appraisal procedure of ternary cathode material of lithium ion battery thermal run away as claimed in any one of claims 1 to 3, feature
Be, the lithium ion battery be cylindrical battery, and by after charging lithium ion battery disassemble the step of, comprising: opposite
Humidity is lower than in the environment of 10%RH, and thermal shrinkable sleeve is removed since negative electrode of lithium ion battery end；Along slot rolling notches cut battery core,
By cap pull-up, tab is straightened, positive pole ear is wiped out along upper insulation spacer surface with pliers in parallel cells direction；Along faucal
Edge coils solution splits steel shell, and the housing parts dismantled is avoided to puncture the short circuit of pole group in anatomic course, when dissection to the lower section,
Steel shell is pulled out into tab along pole group axial direction negative pole end, negative lug is cut, takes out pole group；It is terminated with blade along pole group diaphragm
Line cuts terminal adhesive tape, and core, anode pole piece of tearing is unfolded.
9. the appraisal procedure of ternary cathode material of lithium ion battery thermal run away as claimed in any one of claims 1 to 3, feature
In the step of being, carrying out full scan processing to the tertiary cathode material, obtain scanning spectra, in situ X-ray diffraction diffraction is set
The scanning speed of instrument is 3.8 °/min, 2 θ of scanning angle is 15-72 °, with the heating rate of 1.2 DEG C/min by sample temperature from 25
500 DEG C DEG C are risen to, scanning spectra is collected.
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