CN113237816A - Method for preliminarily detecting morphology of ternary cathode material precursor particles - Google Patents
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- CN113237816A CN113237816A CN202110433518.4A CN202110433518A CN113237816A CN 113237816 A CN113237816 A CN 113237816A CN 202110433518 A CN202110433518 A CN 202110433518A CN 113237816 A CN113237816 A CN 113237816A
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- 239000002245 particle Substances 0.000 title claims abstract description 91
- 239000002243 precursor Substances 0.000 title claims abstract description 61
- 239000010406 cathode material Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000002002 slurry Substances 0.000 claims abstract description 94
- 239000011521 glass Substances 0.000 claims abstract description 31
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000007865 diluting Methods 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000003085 diluting agent Substances 0.000 claims abstract description 5
- 239000006059 cover glass Substances 0.000 claims abstract description 3
- 238000002360 preparation method Methods 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 14
- 239000006228 supernatant Substances 0.000 claims description 13
- 238000010790 dilution Methods 0.000 claims description 6
- 239000012895 dilution Substances 0.000 claims description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 2
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 claims 1
- 230000003287 optical effect Effects 0.000 abstract description 21
- 239000010405 anode material Substances 0.000 abstract description 18
- 238000005054 agglomeration Methods 0.000 abstract description 5
- 230000002776 aggregation Effects 0.000 abstract description 5
- 238000001514 detection method Methods 0.000 abstract description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 2
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 13
- 238000012546 transfer Methods 0.000 description 12
- 238000012360 testing method Methods 0.000 description 6
- 238000001035 drying Methods 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000007774 positive electrode material Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/10—Investigating individual particles
- G01N15/1023—Microstructural devices for non-optical measurement
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/2813—Producing thin layers of samples on a substrate, e.g. smearing, spinning-on
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/10—Investigating individual particles
- G01N2015/1029—Particle size
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/10—Investigating individual particles
- G01N2015/103—Particle shape
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
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Abstract
The invention belongs to the technical field of lithium ion battery anode materials, and particularly relates to a method for preliminarily detecting the morphology of a ternary anode material precursor particle, which comprises the following steps: diluting the slurry: diluting the ternary cathode material precursor slurry taken out of the reaction kettle by using a diluent; preparation of observation samples: dripping the slurry diluted in the step (1) into a glass slide by using a pipette or a dropper, then dripping triethanolamine and covering a cover glass; and (3) observing a sample: and adjusting the corresponding objective lens and focal length, observing the sample, and observing whether the particles are agglomerated or not and whether the appearance is similar to a sphere or not. The method can effectively prevent the agglomeration of precursor particles in the slurry, so that the accurate morphology of the precursor of the ternary cathode material can be detected through an optical microscope, and the detection speed is improved.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery anode materials, and particularly relates to a method for preliminarily detecting the morphology of a precursor particle of a ternary anode material.
Background
In the production process of the ternary cathode material precursor, the particle morphology of the ternary cathode material precursor needs to be monitored discontinuously to ensure that the ternary cathode material precursor is in a sphere-like shape, and in order to improve the production efficiency, the time for detecting the particle morphology of the ternary cathode material precursor needs to be shortened as much as possible. At present, the morphology of the ternary cathode material precursor particles is generally detected by an optical microscope firstly, and then the morphology of the ternary cathode material precursor particles is accurately detected by a scanning electron microscope.
Although the method for preliminarily detecting the morphology of the precursor particles of the ternary cathode material by using the optical microscope has the characteristics of rapidness and low equipment cost, the method for preliminarily detecting the morphology of the precursor particles of the ternary cathode material by using the optical microscope still has important defects at present. The current common method is to take out the slurry from the reaction kettle, directly put the slurry into a glass slide and then directly observe the slurry from an ocular lens, or to take out the slurry from the reaction kettle, directly put the slurry into the glass slide, then directly observe the slurry from the ocular lens after drying the slurry on an electric furnace. By processing the sample in the two modes, particles in the slurry are easy to agglomerate together, and particularly when the particle size of the particles is smaller than 3 micrometers, the agglomeration is more serious, so that the accuracy of primarily detecting the morphology of the precursor particles of the ternary cathode material based on an optical microscope is seriously influenced.
Disclosure of Invention
Aiming at the problem that the accuracy of detecting the morphology of the ternary cathode material precursor particles based on an optical microscope is not high at present, the invention provides a method for primarily detecting the morphology of the ternary cathode material precursor particles, which can effectively prevent the agglomeration of the precursor particles in the slurry, so that the accurate morphology of the ternary cathode material precursor can be detected through the optical microscope.
The method for preliminarily detecting the morphology of the precursor particles of the ternary cathode material, provided by the invention, comprises the following steps of:
(1) diluting the slurry: diluting the ternary cathode material precursor slurry taken out of the reaction kettle by using a diluent;
(2) preparation of observation samples: dripping the slurry diluted in the step (1) into a glass slide by using a pipette or a dropper, then dripping triethanolamine and covering a cover glass;
(3) and (3) observing a sample: and adjusting the corresponding objective lens and focal length, observing the sample, and observing whether the particles are agglomerated or not and whether the appearance is similar to a sphere or not.
The viscosity of triethanolamine is 280mpa under the environment of 35 ℃, the surface tension is 54.9dyne/cm, the alkalinity of the triethanolamine is weaker than that of ammonia (pKa7.82), the triethanolamine has the properties of tertiary amine and alcohol, can generate chelate of 2-4 ligands with various metals, chelates heavy metal ions through various chelating groups, generates hydrophobic structures to precipitate, and therefore, the triethanolamine has the fixing effect under the state of slurry.
Further, in the step (1), the precursor slurry of the ternary cathode material is a solid-liquid mixture, and the solid volume of the precursor slurry of the ternary cathode material accounts for 10% -20% of the total volume of the ternary cathode material.
Further, in the step (1), the diluent is a supernatant of the ternary cathode material precursor slurry after the slurry in the overflow kettle is completely precipitated, and the supernatant comprises ammonium sulfate, sodium sulfate and the ternary cathode material.
Further, in the step (1), the dilution factor is 50-200.
Further, in the step (1), the dilution factor is 100 times. When the dilution multiple is too large, the sample is too dispersed and cannot be accurately observed, and when the dilution concentration multiple is too small, the sample is too compact, so that whether agglomeration is formed or not cannot be accurately judged.
Further, in the step (2), the concentration of triethanolamine is 98%.
Further, in the step (2), the adding amount of the triethanolamine is 0.5-1.0 time of the volume of the diluted slurry in the glass slide.
Further, in the step (3), when the particle size of the observed sample particles is 0.5-10 microns, a 40-time objective lens is adopted, and the focal length is adjusted according to the data of the laser particle analyzer D50, wherein the adjustment state is that the profile and the appearance of the observed sample can be clearly seen.
The invention has the beneficial effects that:
(1) the method for preliminarily detecting the morphology of the precursor particles of the ternary cathode material, provided by the invention, does not need to dry a sample, only needs to simply dilute the slurry, and can improve the detection speed.
(2) According to the method, after triethanolamine is used as a fixing agent, agglomeration of precursor particles in the slurry can be effectively prevented, so that the accurate morphology of the precursor of the ternary cathode material can be detected through an optical microscope, and the defects of the existing method for detecting the morphology of the precursor particles of the ternary cathode material based on the optical microscope are overcome.
Drawings
In order to more clearly illustrate the embodiments or technical solutions in the prior art of the present invention, the drawings used in the description of the embodiments or prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained based on these drawings without creative efforts.
FIG. 1 is a photograph of the morphology of particles obtained by testing 523 slurry with a particle size of 1 μm in example 1;
FIG. 2 is a photograph of the morphology of particles obtained by testing slurry with a particle size of 523 μm in example 2;
FIG. 3 is a photograph of the morphology of the particles obtained by testing slurry of 523 mm in size in example 3;
FIG. 4 is a photograph of the morphology of particles obtained by testing slurry of 523 mm in particle size in comparative example 1;
FIG. 5 is a photograph of the morphology of comparative example 2, in which slurry having a particle size of 523 μm was examined;
FIG. 6 is a photograph of the morphology of comparative example 3, in which slurry with a particle size of 523 μm was examined;
FIG. 7 is a photograph of the morphology of comparative example 4, in which slurry with a particle size of 523 mm was examined;
FIG. 8 is a photograph of the morphology of comparative example 5 particles obtained by detecting slurry with a particle size of 523 mm;
FIG. 9 is a photograph of the morphology of particles obtained by testing slurry of comparative example 6, which has a particle size of 523 μm.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution in the embodiment of the present invention will be clearly and completely described below with reference to the drawings in the embodiment of the present invention, and it is obvious that the described embodiment is only a part of the embodiment of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Taking 523 type ternary anode material slurry out of a reaction kettle, measuring the particle size D50 of the slurry to be about 1 micron by a laser particle size instrument, diluting the slurry by 100 times by adopting prepared slurry supernatant, transferring 20 microliters of diluted slurry into a glass slide by using a disposable liquid transfer gun, transferring 20 microliters of triethanolamine (produced by Tianjin Henxing reagent company and having a concentration of 98%) into the slurry on the glass slide by using the disposable liquid transfer gun, covering the glass slide, adjusting an optical microscope objective (40 times) and a focal length, observing, and observing the picture as shown in figure 1, wherein the shape of the observed precursor particles is well dispersed particles.
Example 2
Taking 523 type ternary anode material slurry out of a reaction kettle, measuring the particle size D50 of the slurry to be about 2 microns by a laser particle size instrument, diluting the slurry by 100 times by adopting prepared slurry supernatant, transferring 20 microliters of diluted slurry into a glass slide by using a disposable liquid transfer gun, transferring 10 microliters of triethanolamine (produced by Tianjin Henxing reagent company and having a concentration of 98%) into the slurry on the glass slide by using the disposable liquid transfer gun, covering the glass slide, adjusting an optical microscope objective (40 times) and a focal length, observing, and observing the picture as shown in figure 2, wherein the shape of the observed precursor particles is well dispersed particles.
Example 3
Taking 523 type ternary positive electrode material slurry out of a reaction kettle, measuring the particle size D50 of the slurry to be about 5 microns by a laser particle size instrument, diluting the slurry by 50 times by adopting the supernatant of the prepared ternary positive electrode material precursor slurry, transferring 20 microliters of the diluted slurry into a glass slide by using a disposable liquid transfer gun, transferring 10 microliters of triethanolamine (produced by Tianjin Hengxing reagent company and having a concentration of 98%) into the slurry on the glass slide by using the disposable liquid transfer gun, covering the glass slide, adjusting the objective lens (40 times) and the focal length of an optical microscope, and observing, wherein an observation picture is shown in figure 3, and the appearance of the observed precursor particles is well dispersed particles.
Comparative example 1
Taking 523 type ternary anode material slurry out of a reaction kettle, measuring the particle size D50 of the slurry to be about 1 micron by a laser particle size instrument, diluting the slurry by 100 times by adopting the prepared supernatant of the ternary anode material precursor slurry, transferring 20 microliters of the diluted slurry into a glass slide by using a disposable liquid transfer gun, covering the glass slide, adjusting an optical microscope objective lens (40 times) and the focal length, observing, and observing the picture as shown in figure 4, wherein the morphology of the observed precursor particles is seriously agglomerated particles.
Comparative example 2
Taking 523 type ternary anode material slurry out of a reaction kettle, measuring the particle size D50 of the slurry to be about 2 microns by a laser particle size instrument, diluting the slurry by 100 times by adopting the prepared supernatant of the ternary anode material precursor slurry, transferring 20 microliters of the diluted slurry into a glass slide by using a disposable liquid transfer gun, covering the glass slide, adjusting an optical microscope objective lens (40 times) and the focal length, observing, and observing the picture as shown in figure 5, wherein the morphology of the observed precursor particles is seriously agglomerated particles.
Comparative example 3
Taking 523 type ternary anode material slurry out of the reaction kettle, measuring the particle size D50 of the slurry to be about 5 microns by a laser particle size instrument, diluting the slurry by 50 times by adopting the prepared supernatant of the ternary anode material precursor slurry, transferring 20 microliters of the diluted slurry into a glass slide by using a disposable liquid transfer gun, covering the glass slide, adjusting an optical microscope objective lens (40 times) and the focal length, observing, and observing the picture as shown in figure 6, wherein the morphology of the observed precursor particles is seriously agglomerated particles.
Comparative example 4
Taking 523 type ternary anode material slurry out of a reaction kettle, measuring the particle size D50 of the slurry to be about 1 micron by a laser particle size instrument, diluting the slurry by 100 times by adopting the prepared supernatant of the ternary anode material precursor slurry, transferring 20 microliters of the diluted slurry into a glass slide by using a disposable liquid transfer gun, drying the glass slide attached with the dried slurry on an electric furnace, putting the glass slide into an optical microscope sample measuring platform, adjusting an optical microscope objective lens (40 times) and the focal length, observing, and observing the picture as shown in figure 7, wherein the shape of the observed precursor particles is seriously agglomerated particles.
Comparative example 5
Taking 523 type ternary anode material slurry out of a reaction kettle, measuring the particle size D50 of the slurry to be about 2 microns through a laser particle size instrument, diluting the slurry by 100 times by adopting the prepared supernatant of the ternary anode material precursor slurry, transferring 20 microliters of the diluted slurry into a glass slide by using a disposable liquid transfer gun, drying the glass slide on which the dried slurry is attached on an electric furnace, putting the glass slide on which the dried slurry is attached into an optical microscope sample measuring table, adjusting an optical microscope objective lens (40 times) and the focal length, observing, and observing the observation picture as shown in figure 8, wherein the morphology of the observed precursor particles is seriously agglomerated particles.
Comparative example 6
Taking 523 type ternary anode material slurry out of a reaction kettle, measuring the particle size D50 of the slurry to be about 5 microns through a laser particle size instrument, diluting the slurry by 50 times by adopting the prepared supernatant of the ternary anode material precursor slurry, transferring 20 microliters of the diluted slurry into a glass slide by using a disposable liquid transfer gun, drying the glass slide attached with the dried slurry on an electric furnace, putting the glass slide into an optical microscope sample measuring platform, adjusting an optical microscope objective lens (40 times) and the focal length, observing, and observing the picture as shown in figure 9, wherein the shape of the observed precursor particles is seriously agglomerated particles.
From the test results of examples 1 to 3 and comparative examples 1 to 6, it can be seen that: the technology can effectively prevent the precursor particles of the ternary cathode material from agglomerating in the detection process, thereby accurately detecting the real morphology of the precursor particles of the ternary cathode material.
Although the present invention has been described in detail by referring to the drawings in connection with the preferred embodiments, the present invention is not limited thereto. Various equivalent modifications or substitutions can be made on the embodiments of the present invention by those skilled in the art without departing from the spirit and scope of the present invention, and these modifications or substitutions are within the scope of the present invention/any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (8)
1. A method for preliminarily detecting the morphology of particles of a precursor of a ternary cathode material is characterized by comprising the following steps of:
(1) diluting the slurry: diluting the ternary cathode material precursor slurry taken out of the reaction kettle by using a diluent;
(2) preparation of observation samples: dripping the slurry diluted in the step (1) into a glass slide, then dripping triethanolamine and covering a cover glass;
(3) and (3) observing a sample: and adjusting the corresponding objective lens and focal length, observing the sample, and observing whether the particles are agglomerated or not and whether the appearance is similar to a sphere or not.
2. The method for preliminarily detecting the morphology of the precursor particles of the ternary cathode material as claimed in claim 1, wherein in the step (1), the precursor slurry of the ternary cathode material is a solid-liquid mixture, and the solid volume of the precursor slurry of the ternary cathode material accounts for 10% -20% of the total volume of the precursor slurry of the ternary cathode material.
3. The method for preliminarily detecting the morphology of the precursor particles of the ternary cathode material as claimed in claim 1, wherein in the step (1), the diluent is a supernatant of the slurry of the precursor of the ternary cathode material after the slurry in the overflow tank is completely precipitated, and the supernatant comprises ammonium sulfate, sodium sulfate and the ternary cathode precursor material.
4. The method for preliminarily detecting the morphology of the precursor particles of the ternary cathode material according to claim 1, wherein in the step (1), the dilution factor is 50-200 times.
5. The method for preliminarily detecting the morphology of the precursor particles of the ternary cathode material as claimed in claim 4, wherein in the step (1), the dilution factor is 100 times.
6. The method for preliminarily detecting the morphology of the precursor particles of the ternary cathode material as claimed in claim 1, wherein in the step (2), the concentration of triethanolamine is 98%.
7. The method for preliminarily detecting the morphology of the precursor particles of the ternary cathode material as claimed in claim 1, wherein in the step (2), the addition amount of triethanolamine is 0.5-1.0 times of the volume of the diluted slurry in the glass slide.
8. The method for preliminarily detecting the morphology of particles of the precursor of the ternary cathode material according to claim 1, wherein in the step (3), when the particle size of the observed sample particles is 0.5 to 10 micrometers, a 40-fold objective lens is adopted, and the focal length is adjusted according to data of a laser particle sizer D50, so that the profile and the morphology of the observed sample can be clearly seen.
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| CN116493251A (en) * | 2023-06-29 | 2023-07-28 | 宁德时代新能源科技股份有限公司 | Screening apparatus |
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