CN109030389A - The measuring method of total sulfur in a kind of anode material for lithium-ion batteries - Google Patents
The measuring method of total sulfur in a kind of anode material for lithium-ion batteries Download PDFInfo
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- CN109030389A CN109030389A CN201810812805.4A CN201810812805A CN109030389A CN 109030389 A CN109030389 A CN 109030389A CN 201810812805 A CN201810812805 A CN 201810812805A CN 109030389 A CN109030389 A CN 109030389A
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- total sulfur
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- ion batteries
- anode material
- measuring method
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
Abstract
The present invention relates to a kind of measuring methods of total sulfur in anode material for lithium-ion batteries.The measuring method includes: to calcine after 1) mixing positive electrode, alkali carbonate, magnesia, washes with water calcined product, collecting cleaning solution is solution to be measured；2) sulfur content in solution to be measured is detected, conversion obtains the total sulfur content of positive electrode.The measuring method of total sulfur in anode material for lithium-ion batteries provided by the invention, to be calcined after positive electrode, alkali carbonate, magnesia mixing, it is transferred to the total sulfur in positive electrode in cleaning solution, and then detection simple, quickly, economic, environmentally friendly obtains the total sulfur content in positive electrode.Testing result shows that this method is consistent with the testing result of total sulfur content obtained by IC method of testing, ICP method of testing, can be very good total sulfur content in reflection positive electrode.
Description
Technical field
The invention belongs to the detection and analysis fields of lithium ion battery electrode material, and in particular to a kind of lithium ion cell positive
The measuring method of total sulfur in material.
Background technique
Lithium ion battery is due to having many advantages, such as that high-energy density, high power density, long-life, memory-less effect become
The first choice of portable electronic product battery and power battery.Positive electrode is the important component of lithium ion battery.Positive material
The catalytic action of excess of sulfur will lead to electrolyte in material and the electrochemical window of battery mismatches, so that the self discharge of battery increases
Greatly, it is therefore desirable to which the total sulfur in positive electrode is controlled.
Currently, total sulfur is mostly used ICP test in positive electrode, sample treatment is acid resolution, and sour digestion process can generate largely
Acid mist generates harm to human body；In addition, the speciality based on sulphur, ICP detection sulphur need to increase argon gas purging, and testing expense is high, and
ICP-OES regular maintenance cost is also higher.
Summary of the invention
The purpose of the present invention is to provide a kind of measuring methods of total sulfur in anode material for lithium-ion batteries, to solve existing
The problem that methodical continuous mode is complicated, cost of determination is high.
To achieve the above object, the technical scheme adopted by the invention is that:
The measuring method of total sulfur in a kind of anode material for lithium-ion batteries, comprising the following steps:
1) it is calcined after mixing positive electrode, alkali carbonate, magnesia, washes with water calcined product, collect cleaning
Liquid is solution to be measured；
2) sulfur content in solution to be measured is detected, conversion obtains the total sulfur content of positive electrode.
The measuring method of total sulfur in anode material for lithium-ion batteries provided by the invention, with positive electrode, alkali metal carbonic acid
It is calcined after salt, magnesia mixing, is transferred to the total sulfur in positive electrode in cleaning solution, and then simple, quick, economic, environmental protection
Detection obtain the total sulfur content in positive electrode.Testing result shows total obtained by this method and IC method of testing, ICP method of testing
The testing result of sulfur content is consistent, can be very good total sulfur content in reflection positive electrode.
In step 1), positive electrode is the positive active material that LiFePO4, ternary material etc. need to detect total sulfur.It is preferred that
, the positive electrode is by drying pretreatment.The temperature of the drying is 120 DEG C, and the time is no less than 2h.By drying pre- place
Reason can remove moisture in materials, improve test sample and weigh accuracy.
Alkali carbonate, the dosage of magnesia are mainly determining according to the sulfur content in positive electrode, it is however generally that, anode
Material, alkali carbonate, magnesia mass ratio be (0.5-1): (0.5-1.5): (1.5-2.5).Preferably, alkali metal carbon
Hydrochlorate selects sodium carbonate and/or potassium carbonate.Alkali carbonate, magnesia can convert completely element sulphur in positive electrode, together
When avoid element sulphur from overflowing, improve the accuracy of testing result.
For the conversion for preferably promoting sulphur, the test accuracy of element sulphur is improved, it is preferred that the temperature of the calcining is
900-1000 DEG C, the time of calcining is 1-3h.
In step 2), the method for sulphur in existing detection solution can be used to measure the sulfur content in solution, such as turbidimetry, again
Amount method etc..Preferably, barium chloride and emulsifier are added into solution to be measured, is detected using UV-VIS spectrophotometry to be measured
Sulfur content in solution.The basic principle of this method is that total sulfur is reacted with barium chloride after processing in positive electrode, generates sulfuric acid
Precipitated barium is dispersed in solution system in the form of emulsion, with lambert-in the presence of emulsifier in certain time
Beer law is theoretical basis, with calibration curve method, finds out total sulfur content.
The stabilizers such as gelatin, PVA may be selected in emulsifier, for preferably removal influence the accuracy of total sulfur element test because
Element is scattered in sample to be tested uniformly in solution system, it is preferred that the emulsifier is nonylphenol polyoxyethylene ether and dense salt
The mixed liquor of acid.Still more preferably, nonylphenol polyoxyethylene ether and the volume ratio of concentrated hydrochloric acid are (0.5-1.5): (0.05-
0.1).Nonylphenol polyoxyethylene ether is preferably NP-5；Concentrated hydrochloric acid is commercially available customary commercial, mass concentration 36%-38%.
Solution to be measured, barium chloride, emulsifier composition test system in, barium chloride should be excessive relative to sulphur, ordinary circumstance
Under, the additional amount that every gram of positive electrode sample corresponds to barium chloride is 1-2g.In test system, the volume fraction of concentrated hydrochloric acid is
0.05-0.1%, the mass fraction of nonylphenol polyoxyethylene ether are 0.5-1.5%.Under the concentration range, it can get preferable
Emulsifying effectiveness, uniformity, the stability of test system are good, and accuracy, the reliability of measurement result, which have, preferably to be guaranteed.
To obtain better test effect, it is preferred that emulsifier is first added into solution to be measured and is uniformly mixed, adds chlorine
Change barium mixing, stand, is then tested.The time of the standing is 5-10min.
The Detection wavelength of UV-VIS spectrophotometry is 460nm.Compared to other Detection wavelength conditions, 460nm into
Row test, can get the range of linearity wider (reaching 2 orders of magnitude) standard curve, linearly dependent coefficient up to 99.9% with
On, inspection range is 0.5-80 μ g/mL, and the range of linearity is 0.2-160 μ g/mL.
In the test process of UV-VIS spectrophotometry, the cuvette of quartz or glass material can be used, for matching
System test solution, can also facilitate the detection of sample using the ultraviolet-visible spectrophotometer with quantitative measurment function.
Detailed description of the invention
Fig. 1 is standard curve spectrogram of the total sulfur on ultraviolet-visible spectrophotometer in the method for embodiment 1；
Fig. 2 is the canonical plotting of the method for comparative example 2.
Specific embodiment
Embodiments of the present invention are described further combined with specific embodiments below.In following embodiment, nonyl phenol
Polyoxyethylene ether NP-5, concentrated hydrochloric acid are commercially available customary commercial, and the mass concentration of concentrated hydrochloric acid is 36-38%.Other reagents for example without
Specified otherwise is commercially available excellent pure grade.
Ultraviolet-visible spectrophotometer, a ten thousandth balance, magnetic stirring apparatus, baking oven, high-temperature cabinet are commercially available conventional dress
It sets.
Embodiment 1
The measuring method of total sulfur in the anode material for lithium-ion batteries of the present embodiment, using following steps:
1) it establishes standard curve: weighing anhydrous potassium sulfate (K2SO4) 0.5434 ± 0.001g dissolves in a small amount of distilled water,
And the constant volume in 200ml volumetric flask, it prepares and obtains the mother liquor that sulphur concentration is 500 μ g/mL；
Using mother liquor and water, compound concentration is respectively the series mark of 0,5,10,15,20,30 μ g/mL in 50mL colorimetric cylinder
Quasi- solution, addition 4mL emulsifier (by nonylphenol polyoxyethylene ether NP-5, concentrated hydrochloric acid, 10:1 is mixed emulsifier by volume,
The mass fraction that volume fraction of the concentrated hydrochloric acid in test system is 0.1%, NP-5 be 1%) after be uniformly mixed, add 0.3g
Chlorination crystal of barium, and timing immediately stir 120s ± 5s, stand 8min, are in wavelength on ultraviolet-visible spectrophotometer
Absorbance is tested under 460nm, draws standard curve.
2) preparation of blank sample: taking ultrapure water in color-comparison tube, after 4mL emulsifier (identical as step 1)) is added
It is uniformly mixed, adds 0.3g chlorination crystal of barium, stir 120s ± 5s, stand 8min, blank sample is made.
The preparation of solution to be measured: using a kind of nickle cobalt lithium manganate as product to be tested, drying is no less than cooled to room temperature after 2 hours,
The sample of 2g (being accurate to 0.0001g) is weighed in 100mL beaker, 1g sodium carbonate and 2g magnesia is added, in high temperature furnace in
950 DEG C of calcining 2h, are cooled to room temperature, add ultrapure water 100mL, clean 3 times, each 10min repeatedly, collect cleaning solution in volumetric flask
In, it is settled to 500mL, solution as to be measured；
It takes 50mL solution to be measured in color-comparison tube, emulsifier and barium chloride is added by the identical mode of step 1).
3) using behind blank sample school zero, the absorbance value of solution to be measured is tested, brings standard curve into, is calculated to be measured
Sulfur content in solution obtains the total sulfur content in positive electrode after converting.
It, can be by C in the embodimentTotal sulfur=(CIt surveys×500)/mSampleIt is calculated total sulfur content, in formula, CTotal sulfurFor sample to be tested
Total sulfur content, unit are μ g/g；CIt surveysFor the sample to be tested concentration directly measured on instrument, unit is μ g/mL；mSampleFor to test sample
Product sample weighting amount, unit g.Finally measuring total sulfur result is 1145.8 μ g/g.
Standard curve obtained by step 1) reaches 2 quantity as shown in Figure 1, the standard curve range of linearity of this method is wider
Grade, related coefficient reach 99.99%.
Embodiment 2
The measuring method of total sulfur, substantially the same manner as Example 1 in the anode material for lithium-ion batteries of the present embodiment, and difference is only
It is, in step 1), emulsifier being added and makes in test system, the volume fraction of concentrated hydrochloric acid is the quality point of 0.05%, NP-5
Number is 0.5%；The additional amount of chlorination crystal of barium is 0.2g.In step 2), the quality difference of positive electrode, sodium carbonate, magnesia
For 3g, 1.5g, 2.5g.
Embodiment 3
The measuring method of total sulfur, substantially the same manner as Example 1 in the anode material for lithium-ion batteries of the present embodiment, and difference is only
It is, in step 1), emulsifier being added and makes in test system, the volume fraction of concentrated hydrochloric acid is the quality point of 0.08%, NP-5
Number is 1.5%；The additional amount of chlorination crystal of barium is 0.4g.In step 2), the quality difference of positive electrode, sodium carbonate, magnesia
For 0.5g, 0.5g, 1.5g.
Comparative example 1
The measuring method of total sulfur, substantially the same manner as Example 1 in the anode material for lithium-ion batteries of comparative example 1, and difference is only
It is, in solution to be measured preparation, is added without sodium carbonate and magnesia, but directly calcine positive electrode sample, so
Gained solution to be measured is tested afterwards.
Comparative example 2
The measuring method of total sulfur, substantially the same manner as Example 1 in the anode material for lithium-ion batteries of comparative example 1, and difference is only
Be, emulsifier is different, equivalent replacement is carried out to the nonylphenol polyoxyethylene ether NP-5 in embodiment 1 using gelatin, then into
Row subsequent detection.
Test example 1
This test example evaluates the precision of the measuring method of embodiment 1, accuracy.
1.1 precision test
11 parts of cell positive material samples are taken in parallel, are tested in parallel, as a result in terms of total sulfur content, the results are shown in Table 1.
The Precision test result of 1 embodiment method of table
By the testing result of table 1 it is found that the method using the present embodiment carries out Duplicate Samples test, relative standard deviation RSD
It is 0.9%, relative standard deviation meets elemental analysis requirement.
1.2 accuracy test
6 parts of the solution to be measured of Example 1 does the test of sample mark-on reclaims, and the results are shown in Table 2.
The mark-on reclaims testing inspection result of 2 embodiment method of table
By the mark-on reclaims test result of table 2 it is found that the obtained standard items rate of recovery is between 90%-110%, recycling
Rate meets Element detection requirement.
To same positive electrode sample, tested respectively with ion chromatography, ICP-OES, the results are shown in Table 3.
The test result comparison of the different test methods of table 3
As shown in Table 3, the result basic one of embodiment method testing result and IC test, ICP test method
It causes, can be very good the total sulfur content in reflection positive electrode sample.
Test example 2
Using the total sulfur content of the method detection same sample of comparative example 1, the results are shown in Table 4.
The measurement result of the method for 4 comparative example 1 of table
As shown in Table 4, the detection mean value of total sulfur content is 961.8 μ in the same sample that the method for comparative example 1 detects
G/g, it can be seen that it differs greatly with ICP test method.Compared with the method for comparative example 1, the inspection of the method for embodiment 1
Surveying result more can really reflect the total sulfur content in positive electrode sample.
Test example 3
The stability of detection architecture obtained by the method for this test example comparing embodiment 1 and comparative example 2, two kinds of measuring methods
Standard curve difference is as depicted in figs. 1 and 2.
By the above test result it is found that the present invention uses the emulsifier system of concentrated hydrochloric acid and nonylphenol polyoxyethylene ether NP-5
More stable solution system can be obtained, the linear result of standard curve is more preferable, corresponding test result it is reproducible, credible
Degree is high, and the measurement analysis for total sulfur in positive electrode provides more convenient practical testing scheme.
Carbon in anode material for lithium-ion batteries of the invention in the other embodiments of the measuring method of total sulfur, in emulsifier
Sour sodium can be replaced for potassium carbonate, and the relative amount of sodium carbonate or potassium carbonate and positive electrode sample, magnesia can be in this hair
In the range of bright restriction, it is adjusted according to conditions such as positive electrode amount of samples, calcination temperatures；In emulsifier, nonyl phenol is poly-
The ratio of ethylene oxide ether NP-5 and concentrated hydrochloric acid and content in test system can be in the framework of the present definition, according to sample
The factors such as the substantially content of the sulphur of product, emulsifying effectiveness are adaptively adjusted, and can get and the comparable effect of embodiment 1.
Claims (10)
1. the measuring method of total sulfur in a kind of anode material for lithium-ion batteries, which comprises the following steps:
1) it is calcined after mixing positive electrode, alkali carbonate, magnesia, washes with water calcined product, collecting cleaning solution is
For solution to be measured；
2) sulfur content in solution to be measured is detected, conversion obtains the total sulfur content of positive electrode.
2. the measuring method of total sulfur in anode material for lithium-ion batteries as described in claim 1, which is characterized in that step 1)
In, positive electrode, alkali carbonate, magnesia mass ratio be (0.5-1): (0.5-1.5): (1.5-2.5).
3. the measuring method of total sulfur in anode material for lithium-ion batteries as claimed in claim 2, which is characterized in that the alkali gold
Belonging to carbonate is sodium carbonate and/or potassium carbonate.
4. the measuring method of total sulfur in anode material for lithium-ion batteries as described in claim 1, which is characterized in that the calcining
Temperature be 900-1000 DEG C, time of calcining is 1-3h.
5. such as the measuring method of total sulfur in anode material for lithium-ion batteries of any of claims 1-4, feature exists
In, in step 2), barium chloride and emulsifier are added into solution to be measured, it is to be measured molten using UV-VIS spectrophotometry detection
Sulfur content in liquid.
6. the measuring method of total sulfur in anode material for lithium-ion batteries as claimed in claim 5, which is characterized in that the emulsification
Agent is the mixed liquor of nonylphenol polyoxyethylene ether and concentrated hydrochloric acid.
7. the measuring method of total sulfur in anode material for lithium-ion batteries as claimed in claim 6, which is characterized in that nonyl phenol is poly-
The volume ratio of ethylene oxide ether and concentrated hydrochloric acid is (0.5-1.5): (0.05-0.1).
8. the measuring method of total sulfur in anode material for lithium-ion batteries as claimed in claim 6, which is characterized in that test system
In, the volume fraction of concentrated hydrochloric acid is 0.05-0.1%, and the mass fraction of nonylphenol polyoxyethylene ether is 0.5-1.5%.
9. the measuring method of total sulfur in anode material for lithium-ion batteries as claimed in claim 5, which is characterized in that every gram of anode
The additional amount that material sample corresponds to barium chloride is 1-2g.
10. the measuring method of total sulfur in anode material for lithium-ion batteries as claimed in claim 5, which is characterized in that ultraviolet-can
The Detection wavelength for seeing spectrophotometry is 460nm.
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| CN110865142A (en) * | 2019-11-20 | 2020-03-06 | 镇江海关综合技术中心 | Detection method for measuring total sulfur content in food by ion chromatography |
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