CN116026731B - Method for judging whether dispersion of carbon nano tube slurry meets standard by in-situ identification of particle size - Google Patents
Method for judging whether dispersion of carbon nano tube slurry meets standard by in-situ identification of particle size Download PDFInfo
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- CN116026731B CN116026731B CN202211441590.2A CN202211441590A CN116026731B CN 116026731 B CN116026731 B CN 116026731B CN 202211441590 A CN202211441590 A CN 202211441590A CN 116026731 B CN116026731 B CN 116026731B
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- 239000002002 slurry Substances 0.000 title claims abstract description 62
- 239000006185 dispersion Substances 0.000 title claims abstract description 44
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000002245 particle Substances 0.000 title claims abstract description 32
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 31
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 15
- 238000000967 suction filtration Methods 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 16
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 239000011148 porous material Substances 0.000 claims abstract description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 9
- 239000010935 stainless steel Substances 0.000 claims description 9
- 230000000903 blocking effect Effects 0.000 claims description 5
- 238000012360 testing method Methods 0.000 abstract description 10
- 239000011324 bead Substances 0.000 abstract description 6
- 238000012216 screening Methods 0.000 abstract description 2
- 239000002071 nanotube Substances 0.000 abstract 1
- 238000000227 grinding Methods 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000006870 function Effects 0.000 description 2
- 238000007790 scraping Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000013178 mathematical model Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000009288 screen filtration Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Sampling And Sample Adjustment (AREA)
Abstract
The invention provides a method for judging whether the dispersion of carbon nano tube slurry reaches the standard by in-situ identification of particle size. According to the technical scheme, the cause of a limit friction dispersion blind area is firstly explored, and then the relation between the granularity D90 of the carbon nanotube slurry and the diameter of the spherical beads is obtained, so that the nanotube slurry is subjected to suction filtration by adopting a specific pore-size filter material, and whether the dispersion of the carbon nanotube slurry reaches the standard can be judged according to the residual condition of the slurry on the surface of the filter material after the suction filtration. Specifically, if the surface of the filter material has no residue, the dispersion is up to the standard, and if the slurry is remained on the filter material to block the net, the dispersion granularity is larger and the dispersion is not up to the standard; wherein, the following relation is satisfied between the filter pore diameter R and the ball diameter D of the slurry: r=0.07 d·a, where a=15/14. The invention samples without any pretreatment, thus maintaining the authenticity of the structure of the slurry; the accuracy of the test result is ensured through the filtering and screening of the slurry particles D90; meanwhile, the testing method is rapid and convenient, and the timeliness of testing and judging is guaranteed.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a method for judging whether carbon nano tube slurry dispersion reaches the standard by in-situ identification of particle size.
Background
At present, in the process of industrially producing carbon nanotube slurry, quality and technicians are often required to judge whether the carbon nanotube slurry is dispersed and qualified. The usual methods are: 1) Scraping slurry on a fineness plate by a scraping plate fineness method, and observing whether large granular sense exists or not by naked eyes, wherein the method has extremely large subjective factors and extremely large errors; 2) The viscosity of the slurry dispersed at different times is tested by a viscometer test method, and whether the viscosity values are consistent is observed. The slurry viscosity itself has a certain fluctuation, and it is also the fact that there is a dynamic balance of the dispersion of the slurry for a period of time, so the viscosity judgment has an error of too early or too late of the grinding dispersion. 3) The laser particle size test method comprises the steps of diluting part of slurry to a certain concentration, ultrasonically dispersing the slurry into a certain specific solvent, and testing the slurry by a particle size analyzer; the method cannot be implemented on a sampling site, and the steps of dilution, ultrasonic dispersion and the like in the method have destructive effects on the slurry, so that the test result is distorted.
Disclosure of Invention
Aiming at the technical defects of the prior art, the invention provides a method for judging whether the dispersion of carbon nano tube slurry meets the standard by in-situ identification of particle size, so as to solve the technical problems of large error, easiness in damaging the slurry, incapability of being implemented on site and the like of the conventional method.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
the method for judging whether the dispersion of the carbon nano tube slurry meets the standard by in-situ identification of the particle size comprises the following steps: carrying out suction filtration on the carbon nano tube slurry by using a negative pressure filter device, if the surface of the filter material has no residue after the suction filtration is finished, indicating that the dispersion reaches the standard, and if the slurry has a blocking net remained on the filter material, indicating that the dispersion granularity is larger and does not reach the standard; wherein, the following relation is satisfied between the filter pore diameter R and the ball diameter D of the slurry: r=0.07 d·a, where a=15/14.
Preferably, the carbon nanotube slurry is used in an amount of 20mL.
Preferably, the duration of the suction filtration is 3-5 min.
Preferably, the negative pressure filter device comprises a filter flask, a negative pressure suction filter port, a filter funnel and a filter material, wherein the negative pressure suction filter port is positioned at the side end of the filter flask, the filter funnel is arranged at the top end of the filter flask, the filter material is fixed in the filter funnel and intercepts at least one cross section of the filter funnel, and a vacuum pump is connected to the negative pressure suction filter port.
Preferably, the filter medium is a stainless steel filter screen.
Preferably, the stainless steel filter screen is closely attached to the surface of the filter bucket.
The invention provides a method for judging whether the dispersion of carbon nano tube slurry reaches the standard by in-situ identification of particle size. The method samples without any pretreatment, and keeps the authenticity of the structure of the slurry; the accuracy of the test result is ensured through the filtering and screening of the slurry particles D90; meanwhile, the testing method is rapid and convenient, and the timeliness of testing and judging is guaranteed.
Drawings
FIG. 1 is a schematic view of a negative pressure filter apparatus according to the present invention;
FIG. 2 is a schematic view of microscopic states of different numbers of beads rubbing against each other;
in the figure:
| 1. filter flask | 2. Negative pressure suction filtration port | 3. Filter bucket | 4. A filter material. |
Detailed Description
Hereinafter, embodiments of the present invention will be described in detail. In order to avoid unnecessary detail, well-known structures or functions will not be described in detail in the following embodiments. Approximating language, as used in the following examples, may be applied to create a quantitative representation that could permissibly vary without resulting in a change in the basic function. Unless defined otherwise, technical and scientific terms used in the following examples have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
Example 1
A method for judging whether the dispersion of carbon nano tube slurry meets the standard by in-situ particle size identification (namely, testing the filtration passing property of the particle size D90):
1) The core of the device is the determination of the number of the filter meshes in the middle of the filter funnel and the compact combination of the filter screen and the filter funnel.
2) And judging the granularity D90 of the carbon nano tube slurry. The dispersion of the carbon nanotube paste is based on continuous motion friction of the beads. The double-ball friction can realize seamless friction and achieve nano dispersion; however, when three balls are rubbed, a limit friction dispersion blind area is easy to appear, and an agglomeration range of dispersed particles, namely the size of D90 particles is formed. D90 is equal to 0.07 times the diameter of the beads.
3) 20ml of carbon tube slurry with the diameter of 1.0mm and the ball size of which are dispersed is selected, the slurry is filtered on a negative pressure filter device by a vacuum suction filtration method (a filter screen is selected to be 200 meshes and has the aperture of 75 um), the suction filtration is carried out for 3 to 5 minutes, the surface of the filter screen has no residue, the dispersion is qualified, the residue is blocked, the dispersion granularity is larger, and the dispersion is unqualified.
The core technical links are as follows:
1. simple negative pressure filter device
As shown in figure 1, the device consists of a filter bucket, a stainless steel filter screen, a filter flask and a negative pressure suction filter port. One of the cores of the device is: the stainless steel filter screen is densely combined with the filter funnel plane; the mesh number of the stainless steel filter screen is 100-500 meshes.
And during suction filtration, a vacuum pump is connected with a negative pressure suction filtration port, and a suction filtration experiment is performed.
2. Determination of carbon nanotube slurry particle size D90
The dispersion of the carbon nanotube slurry is achieved based on continuous motion friction of the beads. As shown in fig. 2, the balls continuously move for friction, and seamless friction can be realized during double ball friction, namely nano dispersion is achieved; when three balls are rubbed, a dispersion limit blind area is easy to appear, and an agglomeration range of slurry particles is formed. Thus, during grinding of the slurry, the overall particle D90 (the size of the mesh through which 90% of the particles pass) size of the slurry is directly substantially consistent with the size of the dispersion limit dead zone.
There are four mathematical models according to the ball motion friction described above: 1) single ball rolling, 2) double ball friction stripping, 3) three ball friction and 4) four ball friction. Four balls are rubbed, the structure is loose, and the contact interface is unstable; three ball friction can form the fixed knot that stands immediately constructs, and the probability of motion together is very big, appears friction contact's limit space, disperses limit blind area promptly. According to calculation, the limit distance of the dispersion blind area is 0.07D, namely 0.07 times of the diameter of the ball.
In actual operation, the corresponding filter media may be selected with reference to the following table 1:
table 1 list of ball diameter, dispersion limit area D90 and screen mesh number
| Ball diameter (mm) | Limit area-D90 (μm) | Screen (mesh) |
| 1.4 | 98 | 140--106 |
| 1.2 | 84 | 160--96 |
| 1.0 | 70 | 200--75 |
| 0.8 | 56 | 250--58 |
| 0.6 | 42 | 325--45 |
| 0.4 | 28 | 400--38 |
| 0.3 | 21 | 500--25 |
| 0.2 | 14 | 800--18 |
3. Filter screen filtration large particle test
1) 20ml of carbon tube slurry with 1.0mm ball dispersed is selected, and the slurry is filtered on a negative pressure filter device by a vacuum suction filtration method (the filter screen is selected to be 200 meshes, the aperture is 75 um), and the suction filtration is carried out for 3-5 minutes. And visually observing whether large particles and residual phenomena exist through a filter screen. The surface of the filter screen has no residue, which indicates that the dispersion is qualified, the filter screen has residue blocking, and indicates that the dispersion granularity is larger and the filter screen is unqualified.
Table 2 experimental list of 200 mesh screen filtering 1.0mm ball mill dispersed carbon nanotube slurry
| Grinding of the dispersed sample/hour/100 kg | Screen residue | Whether or not to pass |
| 1 | Residual, large particles | Whether or not |
| 2 | Residue of | Whether or not |
| 2.5 | No residue | Is that |
| 3 | Has residues and particles | Whether or not |
2) 20ml of carbon tube slurry with 0.6mm spherical beads dispersed is selected, and the slurry is filtered on a negative pressure filter device by a vacuum suction filtration method (a filter screen is selected to be 325 meshes, the aperture is 45 um), and the suction filtration is carried out for 3-5 minutes. And visually observing whether large particles and residual phenomena exist through a filter screen. The surface of the filter screen has no residue, which indicates that the dispersion is qualified, the filter screen has residue blocking, and indicates that the dispersion granularity is larger and the filter screen is unqualified.
Table 3 Experimental list of 325 mesh Screen filtering 0.6mm ball milling dispersed carbon nanotube slurry
| Grinding of the dispersed sample/hour/100 kg | Screen residue | Whether or not to pass |
| 1 | Residual, large particles | Whether or not |
| 2 | Without any means for | Is that |
| 2.5 | Residue of | Whether or not |
Example 2
The method for judging whether the dispersion of the carbon nano tube slurry meets the standard by in-situ identification of the particle size comprises the following steps: carrying out suction filtration on the carbon nano tube slurry by using a negative pressure filter device, if the surface of the filter material has no residue after the suction filtration is finished, indicating that the dispersion reaches the standard, and if the slurry has a blocking net remained on the filter material, indicating that the dispersion granularity is larger and does not reach the standard; wherein, the following relation is satisfied between the filter pore diameter R and the ball diameter D of the slurry: r=0.07 d·a, where a=15/14.
Preferably, the carbon nanotube slurry is used in an amount of 20mL.
Preferably, the duration of the suction filtration is 3-5 min.
Preferably, the negative pressure filtering device comprises a filter flask 1, a negative pressure suction port 2, a filter funnel 3 and a filter material 4, wherein the negative pressure suction port 2 is positioned at the side end of the filter flask 1, the filter funnel 3 is arranged at the top end of the filter flask 1, the filter material 4 is fixed in the filter funnel 3 and intercepts at least one cross section of the filter funnel 3, and a vacuum pump is connected to the negative pressure suction port 2.
Preferably, the filter medium 4 is a stainless steel filter screen.
Preferably, the stainless steel filter screen is closely attached to the surface of the filter bucket 3.
The foregoing describes the embodiments of the present invention in detail, but the description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modification, equivalent replacement, improvement, etc. made within the scope of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. The method for judging whether the dispersion of the carbon nano tube slurry meets the standard by in-situ identification of the particle size is characterized by comprising the following steps: carrying out suction filtration on the carbon nano tube slurry by using a negative pressure filter device, if the surface of the filter material has no residue after the suction filtration is finished, indicating that the dispersion reaches the standard, and if the slurry has a blocking net remained on the filter material, indicating that the dispersion granularity is larger and does not reach the standard; wherein, the following relation is satisfied between the filter pore diameter R and the ball diameter D of the slurry: r=0.07 d·a, where a=15/14.
2. The method for determining whether the dispersion of the carbon nanotube slurry meets the standard by in-situ identification of particle size according to claim 1, wherein the amount of the carbon nanotube slurry is 20mL.
3. The method for determining whether the dispersion of the carbon nanotube slurry meets the standard by in-situ identification of particle size according to claim 1, wherein the duration of suction filtration is 3-5 min.
4. The method for in-situ identification of particle size to determine whether dispersion of carbon nanotube slurry meets standards according to claim 1, wherein the negative pressure filtering device comprises a filter flask (1), a negative pressure suction filter port (2), a filter funnel (3) and a filter medium (4), wherein the negative pressure suction filter port (2) is positioned at the side end of the filter flask (1), the filter funnel (3) is arranged at the top end of the filter flask (1), the filter medium (4) is fixed in the filter funnel (3) and intercepts at least one cross section of the filter funnel (3), and a vacuum pump is connected to the negative pressure suction filter port (2).
5. The method for determining whether the dispersion of the carbon nanotube slurry meets the standard according to the in-situ identification particle size of claim 4, wherein the filter material (4) is a stainless steel filter screen.
6. The method for judging whether the dispersion of the carbon nano tube slurry meets the standard or not according to the in-situ identification particle size of claim 5, wherein the stainless steel filter screen is tightly attached to the surface of the filter bucket (3).
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