CN111811920A - Method for detecting dispersion uniformity and stability of slurry - Google Patents
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- CN111811920A CN111811920A CN202010724664.8A CN202010724664A CN111811920A CN 111811920 A CN111811920 A CN 111811920A CN 202010724664 A CN202010724664 A CN 202010724664A CN 111811920 A CN111811920 A CN 111811920A
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- 239000002002 slurry Substances 0.000 title claims abstract description 191
- 239000006185 dispersion Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000012360 testing method Methods 0.000 claims abstract description 12
- 238000005070 sampling Methods 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims description 43
- 238000009826 distribution Methods 0.000 claims description 42
- 239000007788 liquid Substances 0.000 claims description 13
- 239000004094 surface-active agent Substances 0.000 claims description 13
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 12
- 238000007789 sealing Methods 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 6
- 238000010790 dilution Methods 0.000 claims description 5
- 239000012895 dilution Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 4
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical group CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 claims description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 2
- 238000013112 stability test Methods 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 4
- 238000011156 evaluation Methods 0.000 abstract description 4
- 230000000007 visual effect Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 239000011149 active material Substances 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004062 sedimentation Methods 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
- 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
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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
- G01N15/02—Investigating particle size or size distribution
- G01N15/0205—Investigating particle size or size distribution by optical means
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- General Health & Medical Sciences (AREA)
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Abstract
The invention provides a method for detecting the dispersion uniformity and stability of slurry, which comprises the following steps: the method comprises the following steps: preparing slurry; step two: sampling slurry; step three: preparing a sample; step four: testing the uniformity of the slurry; step five: and (5) testing the stability of the slurry. The detection method can realize the precise detection of the dispersion uniformity and stability of the slurry, quantify evaluation indexes, and avoid human errors caused by operation methods and visual observation.
Description
Technical Field
The invention belongs to the technical field of batteries, and particularly relates to a method for detecting dispersion uniformity and stability of slurry.
Background
The homogenizing is to uniformly disperse active substances, conductive agents, adhesives and the like in a solvent according to a certain mass ratio to form stable slurry with certain viscosity for coating the pole piece. The uniformity and stability of the slurry dispersion have a significant impact on the performance of lithium batteries. Therefore, a method is needed to effectively evaluate the dispersion effect of the slurry, and whether large particles which are not deagglomerated exist can be evaluated by detecting the particle size of the particles in the well-dispersed slurry, so as to reflect the dispersion effect of the whole slurry.
The traditional method for judging the stability of the slurry by adopting a rheometer to test a slurry shear rate-viscosity curve is simple and convenient, but can only reflect the integral stability of the slurry and cannot qualitatively judge the dispersion uniformity of the slurry; the fineness of the slurry can be detected by a scraper fineness gauge, but the fineness scraper is limited by sampling techniques and the influence of individual differences observed by eyes, and the requirement of accurate evaluation is difficult to achieve.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for detecting the uniformity and stability of slurry dispersion, so as to overcome the disadvantages of the existing evaluation method, such as single degree and low result stringency, and provide a method for quantitatively evaluating the uniformity and stability of slurry particle size, which is simple and convenient to operate and has strong practicability.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a method for detecting the dispersion uniformity and stability of slurry comprises the following steps:
the method comprises the following steps: slurry preparation
Mixing and stirring the slurry raw materials, dispersing the slurry raw materials into a homogeneous system, and measuring the stirred slurry as a slurry to be measured;
step two: slurry sampling
Extracting the slurry at different positions of the upper layer, the middle layer and the lower layer in the slurry to be detected, respectively placing the slurry in different subpackaging containers, respectively numbering the slurry, and simultaneously sealing, standing and storing the slurry to be detected;
step three: sample preparation
Adding a solvent into a proper amount of slurry to be detected in the subpackaging containers for dilution, adding a surfactant, and then putting the mixture into an ultrasonic dispersion machine for ultrasonic dispersion to obtain a colorless and transparent sample;
step four: slurry uniformity test
Detecting the particle size distribution of the three groups of samples in a laser particle size distribution instrument to obtain the particle size distribution of the slurry at different positions of the upper layer, the middle layer and the lower layer in the slurry to be detected, and judging whether the slurry is uniform according to a set standard;
step five: slurry stability test
And (5) standing the sealing slurry obtained in the step two, repeating the step two to the step four, and judging whether the slurry is stable according to a set standard.
Preferably, the surfactant is a nonylphenol polyoxyethylene ether surfactant, and the addition amount of the surfactant is 5-25% of the mass of the powder in the slurry.
More preferably, the surfactant is NP-10, NP-20, NP-30, or NP-40.
Preferably, the ultrasonic dispersion time in the third step is 20-60 min.
Preferably, the determination criteria of the slurry uniformity are:
d50 of the sample is not more than 1.5 times of D50 of the powder, and the three groups of samples have good particle size distribution coincidence, so that the slurry is uniformly dispersed, otherwise, the slurry is not uniformly dispersed.
Preferably, the criterion for determining the stability of the slurry is as follows:
the slurry stability is good if the D50 variation of the sample is less than 2 μm, and poor if the D50 variation of the sampled slurry is greater than 2 μm.
Preferably, the standing time of the slurry in the step five is 12h, 24h or 48 h.
Preferably, the sampling position in the second step is a position which is 50 mm, 150 mm and 250 mm away from the liquid level of the slurry.
Compared with the prior art, the method for detecting the dispersion uniformity and stability of the slurry has the following advantages:
the detection method can realize the precise detection of the dispersion uniformity and stability of the slurry, quantify evaluation indexes, and avoid human errors caused by operation methods and visual observation.
Drawings
FIG. 1 is a particle size distribution of the active material of the slurry of example 1;
fig. 2 is a particle size distribution of a slurry of 50 mm from the liquid level of the slurry in an initial state of the slurry of example 1;
fig. 3 is a particle size distribution of a slurry of example 1, after standing for 12 hours, of 50 mm from the upper surface of the slurry;
fig. 4 is a particle size distribution of a slurry of 50 mm from the liquid level of the slurry after the slurry of example 2 is left to stand for 24 hours;
fig. 5 is a particle size distribution of the slurry of example 2 after being left to stand for 24 hours, which is 150 mm from the liquid level of the slurry;
fig. 6 is a particle size distribution of 250 mm slurry from the upper surface of the slurry after the slurry of example 2 is left to stand for 24 hours;
fig. 7 is a particle size distribution of a slurry of 250 mm from the slurry surface in an initial state of the slurry of example 3;
fig. 8 is a particle size distribution of 250 mm slurry from the upper surface of the slurry after the slurry of example 3 is left to stand for 48 hours.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meanings as commonly understood by one of ordinary skill in the art to which the present invention belongs. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
The present invention will be described in detail with reference to the following examples and accompanying drawings.
Example 1
A method for detecting the dispersion uniformity and stability of slurry comprises the following steps:
preparation of slurry: the components of the battery slurry are placed in a measuring cylinder according to the specified mass ratio and are uniformly dispersed into a homogeneous system through stirring and mixing.
Secondly, slurry sampling: preparing a plurality of small beakers, respectively transferring 10ml of slurry from positions 50 mm, 150 mm and 250 mm away from the liquid level of the slurry in a measuring cylinder by using a transfer pipette, numbering the slurry in the 3 small beakers by 1-3, and sealing and standing the slurry in the measuring cylinder for storage.
Preparing a sample: taking a proper amount of No. 1-3 slurry, adding a corresponding solvent for dilution, adding a surfactant NP-10, and performing ultrasonic dispersion in an ultrasonic dispersion machine (the dispersion time is about 30min, and a sample is colorless and transparent after dispersion)
Testing the uniformity of the slurry: detecting the particle size distribution of No. 1-3 samples by a laser particle size distribution instrument to obtain the particle size distribution of slurry at different positions of the upper part, the middle part and the lower part in the measuring cylinder (comparing 3 sample particle size distributions, the slurry D50 is less than or equal to 1.5 times of powder D50, and the good coincidence of the sample particle size distributions indicates that the slurry is uniformly dispersed);
testing the stability of the slurry: and (4) standing the sealing slurry in the step (II) for 12 hours, repeating the step (II) and the step (III) (the standing time can be selected from 12 hours, 24 hours and 48 hours), and if the particle size distribution change of the sampled slurry is small (D50 change is less than 2 mu m), indicating that the slurry stability is good, and if the particle size distribution change of the sampled slurry is large (D50 change is more than 2 mu m), indicating that the slurry stability is poor.
The granularity distribution of the active substances of the slurry is shown in figure 1, the granularity distribution of the slurry at a distance of 50 mm from the upper surface of the slurry in an initial state is shown in figure 2, and the granularity distribution of the slurry at a distance of 250 mm from the liquid level of the slurry after standing for 12 hours is shown in figure 3.
The active material D50 used in the slurry in fig. 1 was 13.33 μm, the slurry D50 at 50 mm from the liquid level of the slurry in the initial state in fig. 2 was 16.32 μm, and the slurry D50 at 50 mm from the lower surface of the slurry after standing for 12 hours in fig. 3 was 17.06 μm, indicating that the slurry dispersion effect was good.
Example 2
A method for detecting the dispersion uniformity and stability of slurry comprises the following steps:
preparation of slurry: the components of the battery slurry are placed in a measuring cylinder according to the specified mass ratio and are uniformly dispersed into a homogeneous system through stirring and mixing.
Secondly, slurry sampling: preparing a plurality of small beakers, respectively transferring 10ml of slurry from positions 50 mm, 150 mm and 250 mm away from the liquid level of the slurry in a measuring cylinder by using a transfer pipette, numbering the slurry in the 3 small beakers by 1-3, and sealing and standing the slurry in the measuring cylinder for storage.
Preparing a sample: taking a proper amount of No. 1-3 slurry, adding a corresponding solvent for dilution, adding a surfactant NP-10, and performing ultrasonic dispersion in an ultrasonic dispersion machine (the dispersion time is about 30min, and a sample is colorless and transparent after dispersion)
Testing the uniformity of the slurry: detecting the particle size distribution of No. 1-3 samples by a laser particle size distribution instrument to obtain the particle size distribution of slurry at different positions of the upper part, the middle part and the lower part in the measuring cylinder (comparing 3 sample particle size distributions, the slurry D50 is less than or equal to 1.5 times of powder D50, and the good coincidence of the sample particle size distributions indicates that the slurry is uniformly dispersed);
testing the stability of the slurry: and (4) standing the sealing slurry in the step (II) for 24 hours, repeating the step (II) and the step (III), wherein the change of the particle size distribution of the sampled slurry is small (the change of D50 is less than 2 mu m), so that the stability of the slurry is good, and if the change of the particle size distribution of the sampled slurry is large (the change of D50 is more than 2 mu m), the stability of the slurry is poor.
The slurry D50 of the slurry of 50 mm from the slurry liquid level in fig. 4 was 15.04 μm, the slurry D50 of 150 mm from the slurry upper liquid level in fig. 5 was 14.76 μm, and the slurry D50 of the slurry of 250 mm from the slurry liquid level in fig. 6 was 15.60 μm, and the change in the particle size distribution was small, indicating that the slurry was uniformly dispersed throughout without sedimentation.
Example 3
A method for detecting the dispersion uniformity and stability of slurry comprises the following steps:
preparation of slurry: the components of the battery slurry are placed in a measuring cylinder according to the specified mass ratio and are uniformly dispersed into a homogeneous system through stirring and mixing.
Secondly, slurry sampling: preparing a plurality of small beakers, respectively transferring 10ml of slurry from positions 50 mm, 150 mm and 250 mm away from the liquid level of the slurry in a measuring cylinder by using a transfer pipette, numbering the slurry in the 3 small beakers by 1-3, and sealing and standing the slurry in the measuring cylinder for storage.
Preparing a sample: taking a proper amount of No. 1-3 slurry, adding a corresponding solvent for dilution, adding a surfactant NP-10, and performing ultrasonic dispersion in an ultrasonic dispersion machine (the dispersion time is about 30min, and a sample is colorless and transparent after dispersion)
Testing the uniformity of the slurry: detecting the particle size distribution of No. 1-3 samples by using a laser particle size distribution instrument to obtain the particle size distribution of the slurry at different positions of the upper part, the middle part and the lower part in the measuring cylinder (comparing the particle size distribution of 3 samples, the slurry D50 is less than or equal to 1.5 times of powder D50, and the good coincidence of the particle size distribution of the samples indicates that the slurry is uniformly dispersed);
testing the stability of the slurry: and (4) standing the sealing slurry in the step (II) for 48h, repeating the step (II) and the step (III), wherein the stability of the slurry is proved to be good if the particle size distribution change of the sampled slurry is small (D50 change is less than 2 mu m), and the stability of the slurry is proved to be poor if the particle size distribution change of the sampled slurry is large (D50 change is more than 2 mu m).
In fig. 7, the slurry D50 which is 250 mm from the upper surface of the slurry is 15.60 microns, and in fig. 8, the slurry D50 which is standing for 48 hours and 250 mm from the upper surface of the slurry is 15.10 microns, so that the particle size distribution basically has no obvious change, which indicates that the overall stability of the slurry is better, and the slurry does not settle after standing for 48 hours.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. A method for detecting the dispersion uniformity and stability of slurry is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: slurry preparation
Mixing and stirring the slurry raw materials, dispersing the slurry raw materials into a homogeneous system, and measuring the stirred slurry as a slurry to be measured;
step two: slurry sampling
Extracting the slurry at different positions of the upper layer, the middle layer and the lower layer in the slurry to be detected, respectively placing the slurry in different subpackaging containers, respectively numbering the slurry, and simultaneously sealing, standing and storing the slurry to be detected;
step three: sample preparation
Adding a solvent into a proper amount of slurry to be detected in the subpackaging containers for dilution, adding a surfactant, and then putting the mixture into an ultrasonic dispersion machine for ultrasonic dispersion to obtain a colorless and transparent sample;
step four: slurry uniformity test
Detecting the particle size distribution of the three groups of samples in a laser particle size distribution instrument to obtain the particle size distribution of the slurry at different positions of the upper layer, the middle layer and the lower layer in the slurry to be detected, and judging whether the slurry is uniform according to a set standard;
step five: slurry stability test
And (5) standing the sealing slurry obtained in the step two, repeating the step two to the step four, and judging whether the slurry is stable according to a set standard.
2. The method for detecting the dispersion uniformity and stability of the slurry according to claim 1, wherein: the surfactant is nonylphenol polyoxyethylene ether surfactant, and the addition amount of the surfactant is 5-25% of the mass of the powder in the slurry.
3. The method for detecting the dispersion uniformity and stability of the slurry according to claim 2, wherein: the surfactant is NP-10, NP-20, NP-30 or NP-40.
4. The method for detecting the dispersion uniformity and stability of the slurry according to claim 1, wherein: the ultrasonic dispersion time in the third step is 20-60 min.
5. The method for detecting the dispersion uniformity and stability of the slurry according to claim 1, wherein: the judging standard of the slurry uniformity is as follows:
d50 of the sample is not more than 1.5 times of D50 of the powder, and the three groups of samples have good particle size distribution coincidence, so that the slurry is uniformly dispersed, otherwise, the slurry is not uniformly dispersed.
6. The method for detecting the dispersion uniformity and stability of the slurry according to claim 1, wherein: the judgment standard of the slurry stability is as follows:
the slurry stability is good if the D50 variation of the sample is less than 2 μm, and poor if the D50 variation of the sampled slurry is greater than 2 μm.
7. The method for detecting the dispersion uniformity and stability of the slurry according to claim 1, wherein: and the standing time of the slurry in the step five is 12 hours, 24 hours or 48 hours.
8. The method for detecting the dispersion uniformity and stability of the slurry according to claim 1, wherein: and the sampling position in the second step is a position which is 50 mm, 150 mm and 250 mm away from the liquid level of the slurry.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112414883A (en) * | 2020-11-22 | 2021-02-26 | 同济大学 | Method for testing stability of catalyst slurry of proton exchange membrane fuel cell |
| CN114544442A (en) * | 2020-11-24 | 2022-05-27 | 立邦涂料（中国）有限公司 | Detection method for rapidly evaluating fineness of 700-mesh heavy calcium carbonate |
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| CN112414883A (en) * | 2020-11-22 | 2021-02-26 | 同济大学 | Method for testing stability of catalyst slurry of proton exchange membrane fuel cell |
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| CN114544442A (en) * | 2020-11-24 | 2022-05-27 | 立邦涂料（中国）有限公司 | Detection method for rapidly evaluating fineness of 700-mesh heavy calcium carbonate |
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Application publication date: 20201023 |