CN110548447B - Apparatus and method for preparing conductive paste - Google Patents
Apparatus and method for preparing conductive paste Download PDFInfo
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- CN110548447B CN110548447B CN201910856794.4A CN201910856794A CN110548447B CN 110548447 B CN110548447 B CN 110548447B CN 201910856794 A CN201910856794 A CN 201910856794A CN 110548447 B CN110548447 B CN 110548447B
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- 238000000034 method Methods 0.000 title claims description 54
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 145
- 239000007788 liquid Substances 0.000 claims abstract description 131
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 84
- 238000002156 mixing Methods 0.000 claims abstract description 84
- 239000012530 fluid Substances 0.000 claims abstract description 47
- 238000003756 stirring Methods 0.000 claims abstract description 44
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 38
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 38
- 238000002360 preparation method Methods 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 49
- 239000000725 suspension Substances 0.000 claims description 31
- 238000000967 suction filtration Methods 0.000 claims description 26
- 238000003860 storage Methods 0.000 claims description 23
- 239000007791 liquid phase Substances 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 18
- 229910002804 graphite Inorganic materials 0.000 claims description 17
- 239000010439 graphite Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 13
- 238000009210 therapy by ultrasound Methods 0.000 claims description 13
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 10
- 239000002002 slurry Substances 0.000 claims description 10
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 8
- 150000001298 alcohols Chemical class 0.000 claims description 7
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 6
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 238000007667 floating Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000004005 microsphere Substances 0.000 claims description 5
- 238000005273 aeration Methods 0.000 claims description 4
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- 238000005406 washing Methods 0.000 claims description 4
- 206010040844 Skin exfoliation Diseases 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 229910021383 artificial graphite Inorganic materials 0.000 claims description 3
- 238000004299 exfoliation Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 229910021382 natural graphite Inorganic materials 0.000 claims description 3
- 238000010008 shearing Methods 0.000 claims description 3
- 239000012141 concentrate Substances 0.000 claims description 2
- 239000000654 additive Substances 0.000 abstract description 4
- 239000002270 dispersing agent Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 230000000996 additive effect Effects 0.000 abstract description 3
- 238000003828 vacuum filtration Methods 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 32
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 239000000523 sample Substances 0.000 description 7
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 239000013543 active substance Substances 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 2
- 238000005276 aerator Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 230000032798 delamination Effects 0.000 description 2
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- 238000009826 distribution Methods 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
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- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
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- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
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- 230000002349 favourable effect Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000010943 off-gassing Methods 0.000 description 1
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- 238000003921 particle size analysis Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
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- 238000001179 sorption measurement Methods 0.000 description 1
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/82—Combinations of dissimilar mixers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Conductive Materials (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation device and a preparation method of conductive paste, wherein the preparation device comprises: the mixing container is used for mixing the gas-liquid mixed fluid with the treatment object, a gas-liquid mixed fluid pipeline is used for conveying the gas-liquid mixed fluid into the mixing container, a stirring device and/or at least one ultrasonic unit and a vacuum filtration device. According to the preparation method, the graphene and/or carbon nano tube and the gas-liquid mixed fluid are mixed at low concentration and then concentrated, so that the conductive paste containing micro bubbles can be rapidly produced in a large scale, the micro bubbles can be spontaneously adsorbed around the graphene and/or carbon nano tube, and the graphene and/or carbon nano tube can be uniformly and stably dispersed in the conductive paste, so that the effect of using no or very little dispersing agent or additive is achieved.
Description
Technical Field
The present invention relates to the preparation of conductive paste, and more particularly, to a preparation apparatus and a preparation method of conductive paste containing fine bubbles and having a conductive component including graphene and/or carbon nanotubes.
Background
Graphene is widely favored in conductive paste of batteries because of the characteristics of ultra-high conductivity, ultra-thin two-dimensional property, high chemical stability and the like. And when the graphene is applied to the electrode, the graphene and the active substance can be contacted through a 'surface-point', so that the conductivity of the whole electrode is greatly improved. And the graphene has a lower conductivity threshold, so that the use amount of the conductive agent in the whole electrode can be greatly reduced, more active substances are used and densely stacked, and the mass specific capacity and the volume specific capacity of the battery are improved. Meanwhile, the carbon nano tube has higher conductivity and can be contacted with an active substance through a line-point type, but graphene and the carbon nano tube are easy to agglomerate, stack and even precipitate in the conductive paste due to stronger van der Waals force and high specific surface area, so that the storage and practical application of the conductive paste are greatly limited. To improve the stability of the graphene slurry, it is generally necessary to add a large amount of dispersant or additive. Such conductive pastes with dispersants or additives, when practically applied to battery electrodes, can seriously affect the contact of graphene with active materials and thus the conductivity thereof.
Disclosure of Invention
Aiming at the technical problems that the conductive paste containing graphene and/or carbon nano tubes is easy to agglomerate, stack and even precipitate, the invention provides a preparation device of the conductive paste, which comprises:
the mixing container is used for mixing the gas-liquid mixed fluid and the treatment object, wherein the mixing container is provided with a conical bottom, the conical bottom is provided with an opening part, the opening part is also provided with a valve for controlling the opening and closing of the opening part, the inside of the mixing container is provided with a bearing structure, the bearing structure is used for placing a filter material, and the treatment object comprises one of raw materials with a graphite lamellar structure, graphene, carbon nano tubes or a mixture of the graphene and the carbon nano tubes;
A gas-liquid mixed fluid pipeline for conveying the gas-liquid mixed fluid to the mixing container;
The stirring device is used for stirring and mixing the gas-liquid mixed fluid and the treated object; and/or
At least one ultrasonic unit for liquid phase stripping treatment to strip the raw material with graphite lamellar structure into graphene or ultrasonically mix the gas-liquid mixed fluid with the treated matter;
the vacuum filter device comprises a liquid storage container and a vacuum pump, wherein an opening part of the liquid storage container is communicated with an opening part at the bottom of the mixing container, the liquid storage container further comprises a vacuum interface, the vacuum interface is connected with the vacuum pump through a pipeline, and the vacuum pump is used for generating negative pressure to filter liquid in the mixing container into the liquid storage container.
In some embodiments, the preparation device further comprises a micro-bubble generating device, which is communicated with the mixing container through a gas-liquid mixed fluid pipeline and is used for mixing gas and liquid to obtain a gas-liquid mixed fluid.
In some embodiments, the outer wall of the mixing vessel is further provided with a condensing means for controlling the temperature of the liquid in the mixing vessel.
In some embodiments, the liquid storage container is connected to a filtering device, and is used for delivering the filtered liquid to a liquid inlet pipeline of the micro-bubble generating device, so that the liquid can be recycled.
In some embodiments, the microbubble generation device, agitation device, and/or ultrasound unit, vacuum pump, and valve are connected to a controller by wired or wireless means.
In some embodiments, the micro-bubble generating device is configured to perform a mixing treatment of a gas and a liquid by one or more of a mechanical shearing method, an ultrasonic cavitation method, a pressurized dissolved gas and outgassing method, a micro-porous dispersed gas method, a jet aeration method, an air-floating pump gas production method, or an electrolysis method, to obtain a gas-liquid mixed fluid.
The invention also provides a preparation method for obtaining the conductive paste by using the preparation equipment, which comprises the following steps:
Adding a gas-liquid mixed fluid, graphene and/or carbon nano tubes into a mixing container in a state that a valve is closed, wherein the mass content of the graphene and/or the carbon nano tubes is between 0.1 wt and 1wt percent; the gas-liquid mixed fluid contains micro-bubbles, the particle size of the micro-bubbles is smaller than 100 mu m, and the concentration of the micro-bubbles is larger than 10 6/ml;
stirring by a stirring device and performing ultrasonic treatment by an ultrasonic unit to obtain suspension in which graphene and/or carbon nanotubes are uniformly dispersed;
And carrying out vacuum suction filtration on the suspension in the mixing container through a vacuum suction filtration device, and controlling the quantity of the suction-filtered liquid to further concentrate the suspension until the mass content is between 3 wt and 8 wt percent, so as to obtain the conductive slurry.
In some embodiments, the stirring process, the stirring rotor is rotated at a speed between 1000 rpm and 5000 rpm; ultrasonic treatment, wherein the ultrasonic power is 500W to 2000W, and the treatment time is 1 min to 60 min.
In some embodiments, the method of preparing further comprises the step of preparing graphene by a liquid phase exfoliation process comprising:
adding first fine bubble water, alcohols and raw materials with a graphite lamellar structure into a mixing container, and stirring by a stirring device;
after stirring treatment, carrying out liquid phase stripping treatment by an ultrasonic unit to obtain graphene suspension with a stripped graphite lamellar structure;
Carrying out vacuum suction filtration on the graphene suspension in the mixing container by using a vacuum suction filtration device, and filtering out water to obtain a filter material, wherein the filter material contains graphene;
adding second micro bubble water into the mixing container, and carrying out suction filtration and washing on the filter material by a vacuum suction filtration device to remove alcohol impurities in the filter material to obtain graphene;
wherein the first fine bubble water and the second fine bubble water are aqueous solutions containing fine bubbles, and the first fine bubble water and the second fine bubble water are the same or different.
In some embodiments, the alcohols include: one or more of ethanol, n-propanol, isopropanol, n-butanol, isobutanol, sec-butanol, or tert-butanol; adding alcohol with total volume content of 5-59%; the raw materials comprise one or more of natural graphite, artificial graphite, expanded graphite, graphitized carbon microspheres or expanded carbon microspheres; in the liquid phase stripping treatment, the ultrasonic power of the ultrasonic unit is 1000W to 20000W, and the treatment time is 1 min to 60 min.
The invention has the beneficial technical effects that: the invention provides a preparation device of conductive paste, which is suitable for industrialized rapid mass preparation of conductive paste containing micro bubbles. According to the preparation method of the conductive paste, graphene and/or carbon nano tubes and gas-liquid mixed fluid containing micro bubbles are uniformly mixed at low concentration, and then suction filtration and concentration are carried out, so that the conductive paste with the mass content of 3-wt wt.% of graphene and/or carbon nano tubes is obtained, and the conductive paste containing micro bubbles, being uniformly dispersed and having better viscosity can be obtained. When the micro bubbles exist in the conductive paste, the micro bubbles can be spontaneously adsorbed around the graphene and/or the carbon nano tube through the high specific surface area adsorption effect of the graphene and the carbon nano tube, and the micro bubbles have the characteristic of long existence time in the liquid by utilizing the slow rising speed of the micro bubbles in the water, so that the graphene can be uniformly and stably dispersed in the conductive paste to achieve the effect of using no or a small amount of dispersing agent and additive. The method can meet the requirements of long-time storage and transportation of the conductive paste, when the conductive paste is used in the actual battery electrode preparation process, graphene and/or carbon nanotubes are easy to uniformly disperse, micro bubbles in the conductive paste spontaneously disappear in the drying process, no impurities are introduced, the contact of the graphene and active substances is not influenced, the conductivity of the graphene is reduced, and the conductive paste has good application value.
Drawings
Fig. 1 is a schematic structural view of a first embodiment of an apparatus for preparing a conductive paste according to the present invention;
fig. 2 is a schematic structural view of a second embodiment of the apparatus for preparing a conductive paste of the present invention;
Fig. 3 is a schematic structural view of a third embodiment of the apparatus for preparing a conductive paste of the present invention;
fig. 4 is a schematic structural view of a fourth embodiment of the apparatus for preparing a conductive paste of the present invention;
fig. 5 is a schematic structural view of a fifth embodiment of the apparatus for preparing a conductive paste of the present invention;
fig. 6 is a step diagram of a method for preparing a conductive paste according to an embodiment of the invention;
fig. 7 is a step diagram of a method for preparing a conductive paste according to another embodiment of the invention;
fig. 8 is a comparative photograph of graphene conductive paste and comparative graphene conductive paste obtained by the preparation method of the present invention after being left for 6 months;
symbol description in the drawings:
1. A fine bubble generation device; 11. an air intake line; 12. a liquid inlet pipeline; 13. a gas-liquid mixed fluid pipeline; 14. a liquid line;
2.A stirring device; 21 a stirring rotor;
3. an ultrasonic unit; 31. a probe-type ultrasonic device; 32 an outer wall mounted ultrasonic device;
4. a mixing vessel; 41. a filter material; 42. a load bearing structure; 43. a valve; 44. an opening part; 45. a cooling device;
5. A connecting device; 51. a vacuum connection tube;
6. An opening of the liquid storage container; 61. a vacuum interface;
7. A liquid storage container;
8. a vacuum pump;
9. a controller;
10. a filtering and recycling device;
S101-S103, S201-S206;
A, a graphene conductive slurry sample obtained by the method is prepared;
and B, comparing the graphene conductive paste samples.
Detailed Description
The apparatus and method for preparing the conductive paste of the present invention will be further described with reference to the accompanying drawings.
Example 1
The embodiment provides a preparation device of conductive paste, the structure of which is schematically shown in fig. 1, comprising:
A micro-bubble generating device 1 for mixing gas and water to generate gas-liquid mixed fluid; wherein the gas and the water enter the micro-bubble generating device 1 through the air inlet pipeline 11 and the liquid inlet pipeline 12 respectively, and after being fully mixed, the formed gas-liquid mixed fluid enters the mixing container 4 through the gas-liquid mixed fluid pipeline 13, and the gas in the gas-liquid mixed fluid exists in the form of micro-bubbles.
A mixing container 4 for mixing the gas-liquid mixed fluid and graphene, wherein the mixing container 4 has a conical bottom, the conical bottom has an opening 44, the opening 44 is further provided with a valve 43 for controlling the opening and closing of the opening 44, the mixing container 4 has a bearing structure 42 inside, and the bearing structure 42 is used for placing the filter material 41;
A stirring device 2 comprising a stirring rotor 21, wherein the stirring rotor 21 is arranged in the inner space of the mixing container 4, and when the stirring device 2 works, the stirring rotor 21 is not under the liquid level of the liquid contained in the mixing container 4;
An ultrasonic unit 3, wherein the ultrasonic unit 3 is a probe type ultrasonic device 31 arranged in the inner space of the mixing container 4;
The vacuum filtering device comprises a liquid storage container 7 and a vacuum pump 8, wherein an opening part 6 of the liquid storage container 7 is communicated with the opening part 44 at the bottom of the mixing container 4, a vacuum interface 61 is further arranged on the liquid storage container 7, and the vacuum interface 61 is connected with the vacuum pump 8 through a vacuum connecting pipe 51, so that the liquid in the mixing container can be filtered and separated by the negative pressure generated by the vacuum pump 8.
It should be noted that the number of the ultrasonic units 3 may be increased to a plurality according to the specific implementation.
Example 2
The present embodiment provides an apparatus for preparing a conductive paste, the structure of which is schematically shown in fig. 2, which is different from the apparatus for preparing a conductive paste according to embodiment 1 in that the ultrasonic unit 3 in the present embodiment is an outer wall-mounted ultrasonic device 32 mounted on the mixing vessel 4.
Example 3
The present embodiment provides an apparatus for preparing a conductive paste, the structure of which is schematically shown in fig. 3, which is different from the apparatus for preparing a conductive paste of embodiment 1 in that it further comprises a controller 9, and the controller 9 is in signal connection with the micro-bubble generating apparatus 1, the stirring apparatus 2, the ultrasonic unit 3, the valve 43 and the vacuum pump 8 through wired or wireless means. The working parameters and the starting and closing of the signal connection device or equipment can be controlled by a program in the controller 9, so that the aim of automatic production is fulfilled.
Example 4
The embodiment provides a device for preparing a conductive paste, the structure of which is schematically shown in fig. 4, which is different from the device for preparing a conductive paste according to embodiment 1 in that a cooling device 45 is further disposed on the outer wall of the mixing container 4, and the cooling device 45 is a manner of cooling with flowing water to keep the temperature of the liquid in the mixing container 4 not higher than a certain value. When the mixing vessel is subjected to ultrasonic treatment, a large amount of heat is generated to raise the temperature of the liquid in the mixing vessel 4, and in particular, when the liquid contains an organic solution, evaporation loss of the liquid is accelerated and the concentration of fine bubbles in the liquid is affected. In practice, therefore, the ultrasound process may be carried out by intermittent ultrasound treatment, and the cooling device 45 may also be used to control the temperature of the liquid in the mixing vessel 4 to not more than 50 ℃.
Example 5
The present embodiment provides a device for preparing a conductive paste, whose structure is schematically shown in fig. 5, and is different from the device for preparing a conductive paste according to embodiment 4 in that a liquid pipeline 14 is disposed at the bottom of the liquid storage container 7 to convey the recovered liquid in the liquid storage container 7 into a filtering and recovering device 10, and the recovered liquid after filtering and recovering treatment is re-introduced into the micro-bubble generating device 1 through a liquid inlet pipeline 12, and is mixed with gas again to form a gas-liquid mixed fluid. This embodiment includes the filtration recovery device 10, and is particularly suitable for the case where the liquid contains a nonaqueous solvent. The waste liquid can be recycled, and the influence of liquid discharge on the environment is avoided.
Example 6
The embodiment provides a method for preparing an inventive conductive paste, which includes steps as shown in fig. 6, including steps S101 to S103:
s101: adding a gas-liquid mixed fluid, graphene and/or carbon nano tubes into the mixing container 4 in a state that the valve 43 is closed, wherein the mass content of the graphene and/or the carbon nano tubes is between 0.1 wt and 1 wt percent; in the mass content range, the suspension of the graphene and/or carbon nano tube and the gas-liquid mixed fluid shows lower viscosity (less than 1000 mPa s), and is easy to uniformly disperse by ultrasonic and stirring;
S102: stirring by a stirring device 2 and carrying out ultrasonic treatment by an ultrasonic unit 3 to obtain suspension with uniformly dispersed graphene and/or carbon nano tubes;
S103: and carrying out vacuum suction filtration on the suspension in the mixing container 4 by a vacuum suction filtration device, and controlling the quantity of the suction-filtered liquid, wherein the suspension is further concentrated to a mass content of 3 wt-8 wt%, so as to obtain the conductive slurry.
The preparation method of this example is further described below by way of specific embodiments, wherein the preparation device of the conductive paste in example 4 uses inert gas argon as a gas source, and organic solution N-methylpyrrolidone (NMP) as a liquid, and the method further includes steps 1) to 4):
Step 1) in the state that the valve 43 is closed, the micro-bubble generating device 1 is opened, argon and NMP enter the micro-bubble generating device 1 through the air inlet pipeline 11 and the liquid inlet pipeline 12 respectively, and after being fully mixed, the formed gas-liquid mixed fluid enters the mixing container 4 through the gas-liquid mixed fluid pipeline 13. The level of the liquid added to the interior of the mixing vessel 4 is between 1/3 and 1/2 of the height of the mixing vessel;
Step 2), starting the stirring device 2, setting the rotating speed of the stirring rotor 21 to be between 1000 and 5000 revolutions per minute, slowly adding graphene with the mass content of 0.1-1% into the mixing container 4, and stirring for 30 min to obtain suspension;
Step 3), starting an ultrasonic unit 3, performing ultrasonic treatment, setting the ultrasonic power to be 500W-2000W and the treatment time to be 1 min-60 min, so that graphene is fully dispersed in a gas-liquid mixed fluid;
After the ultrasonic treatment of the step 4) is finished, a valve 43 and a vacuum pump 8 are opened, vacuum suction filtration is carried out on the suspension in the mixing container 4, after the suspension is filtered by a filter material 41, liquid NMP in the suspension enters the liquid storage container 7 through an opening part 44 at the bottom of the mixing container 4, the amount of the suction filtered liquid is controlled, and the graphene suspension in the mixing container is further concentrated until the mass content is 3 wt-8 wt%, namely the conductive slurry.
The argon gas in this embodiment may also replace other gas types, including: one or more of oxygen, nitrogen, hydrogen, argon, helium, carbon dioxide, or ozone.
The NMP in this example may also be replaced with other common solvents including one of water, N-dimethylformamide, ethanol, isopropanol, butanone, or toluene.
The graphene added in step 2) of the present embodiment may be replaced by carbon nanotubes or a mixture of graphene and carbon nanotubes.
The conductive paste obtained by vacuum filtration concentration in step 4) of this embodiment is thinner in the fluid state (viscosity is less than 2000 mPa ·s) when the mass concentration of graphene and/or carbon nanotubes is less than 3 wt%, and thicker in the apparent viscosity (viscosity is greater than 3000 mPa ·s) when the mass concentration thereof is greater than 5 wt%, so that the mass concentration of the conductive paste after concentration is preferably 3 wt to 5 wt%, and the conductive paste has a preferable apparent viscosity in this mass concentration range, preferably the mass concentration of graphene and/or carbon nanotubes is 4 wt%. The viscosity test adopts a rotary viscometer to test a rotor No. 4, and the torque is as follows: 40 to 60 N.m.
In this embodiment, the liquid NMP separated by vacuum filtration in the liquid storage container 7 can be recycled again after entering the filtering device 10 through the liquid pipeline 14, and then is mixed with gas again in the liquid inlet pipeline 12 of the micro-bubble generating device 1 to form a gas-liquid mixed fluid, so that the waste of liquid is avoided, and particularly, the influence of the discharge on the environment is also avoided for the organic solvent.
According to the preparation method, a mode of concentration after dilution is adopted, graphene and/or carbon nanotubes are firstly dispersed in a gas-liquid mixed fluid in a low concentration, the graphene and/or the carbon nanotubes are fully mixed and dispersed in the gas-liquid mixed fluid in a stirring and/or ultrasonic mode to obtain a uniformly dispersed suspension of low-concentration graphene and/or carbon nanotubes, then partial moisture in the suspension is removed by a suction filtration method, the suspension is concentrated to obtain the conductive slurry containing micro bubbles, the mass concentration of the conductive slurry is 3 wt-8 wt%, and the method is favorable for uniform dispersion of graphene and/or carbon nanotubes and avoids caking caused by uneven dispersion in the mixing process.
Example 7
The embodiment provides a method for preparing an inventive conductive paste, which includes steps as shown in fig. 7, including steps S201 to S206:
S201: adding first fine bubble water, alcohols and raw materials with a graphite lamellar structure into a mixing container 4, and stirring by a stirring device 2;
s202: carrying out liquid phase stripping treatment through an ultrasonic unit 3 to obtain graphene suspension with a stripped graphite lamellar structure;
S203: carrying out vacuum suction filtration on the graphene suspension in the mixing container 4 by a vacuum suction filtration device, and obtaining a filter material after water is filtered out by suction;
s204: adding second fine bubble water into the mixing container 4, and carrying out suction filtration and washing on the filter material through a vacuum suction filtration device;
S205: adding a gas-liquid mixed fluid into a mixing container 4, and performing stirring treatment of a stirring device 2 and ultrasonic treatment of an ultrasonic unit 3 to obtain graphene suspension of 0.1-1 wt%;
S206: and carrying out vacuum suction filtration on the suspension, controlling the quantity of the suction-filtered liquid, and further concentrating the graphene suspension in the mixing container 4 to 3 wt-8 wt% to obtain the graphene conductive slurry.
The difference between this embodiment and embodiment 6 is that this embodiment includes a process of performing ultrasonic liquid phase exfoliation treatment to prepare graphene using the preparation apparatus of the conductive paste of the present invention.
The preparation method of the present embodiment is described in detail below by way of specific embodiments, wherein the graphene preparation apparatus of embodiment 1 is further described by taking air as an air source, and the method includes steps 1) to 7):
Step 1) in the state that the valve 43 is closed, the micro-bubble generating device 1 is started, air and water enter the micro-bubble generating device 1 through the air inlet pipeline 11 and the liquid inlet pipeline 12 respectively, after being fully mixed, first micro-bubble water is formed and enters the mixing container 4 through the gas-liquid mixed fluid pipeline 13, and the liquid level of liquid added into the mixing container 4 is between 1/3 and 1/2 of the height of the mixing container;
Step 2), starting the stirring device 2, setting the rotating speed of the stirring rotor 21 to be between 1000 and 5000 revolutions per minute, adding 30% of isopropanol and 10% of isobutanol into the mixing container 4, slowly adding the preparation raw material expanded graphite, and stirring for 30 min to obtain a suspension;
Step 3), starting an ultrasonic unit 3, performing liquid phase stripping treatment, setting the ultrasonic power to be 1000-20000W, and setting the treatment time to be 1-60 min;
After the liquid phase stripping treatment is finished, opening a valve 43 and a vacuum pump 8, carrying out vacuum suction filtration on the suspension in the mixing container 4, filtering the suspension by a filter material 41, and allowing water to enter the liquid storage container 7 through an opening part 44 at the bottom of the mixing container 4, wherein the filter material 41 is obtained;
step 5), starting the micro-bubble generating device 1 again, enabling the first micro-bubble water to enter the mixing container 4 again, and sequentially closing the micro-bubble generating device 1, the vacuum pump 8 and the valve 43 after performing vacuum pumping, filtering and washing on the filter material for 10 min;
Step 6) starting the micro-bubble generating device 1, adding a certain amount of second micro-bubble water into the mixing container 4, starting the stirring device 2 and the ultrasonic unit 3, wherein the rotating speed of the stirring rotor 21 is set to be 1000-5000 r/min, the ultrasonic power is set to be 500-2000W in ultrasonic treatment, and the treatment time is 1-60 min, so as to obtain the conductive paste with the mass concentration of 0.1-1%;
Step 7) starting a vacuum suction filtration device, filtering out a part of liquid into a liquid storage container, and further concentrating the conductive paste until the mass concentration of graphene is 3 wt-8 wt%, wherein the mass concentration of graphene in the conductive paste for battery electrode preparation is more preferably 4 wt-5 wt%, and the conductive paste has a better viscosity of 2500-3000 mPa.s in the concentration range.
In this embodiment, the first fine bubble water and the second fine bubble water are both aqueous solutions containing fine bubbles, and belong to a gas-liquid mixed fluid in which the liquid is water, wherein the particle size of the fine bubbles is less than 100 μm, and the concentration of the fine bubbles is more than 10 6/ml. The first fine bubble water and the second fine bubble water may be the same fine bubble water generated by the same fine bubble generating device under the same conditions, or may be fine bubble water with different particle diameters and different concentration states of fine bubbles generated by the same fine bubble generating device under different conditions or different fine bubble generating devices. The first micro bubble water is mainly used for an ultrasonic liquid phase stripping process, and the smaller the particle size of micro bubbles is, the easier the micro bubbles penetrate into raw material gaps of a graphene lamellar structure, so that the liquid phase stripping treatment process is benefited; the second fine bubble water is mainly used for dispersing graphene and/or carbon nanotubes, and the smaller the diameter of fine bubbles adsorbed and dispersed around graphene and/or carbon nanotubes, the longer the time of existence in water, the more stable, and therefore, the fine bubbles in the first fine bubble water and the second fine bubble water are preferably 10 nm to 1 μm in particle size, and from the viewpoint of convenience of practical production, the first fine bubble water and the second fine bubble water are preferably the same.
The preparation raw materials added in the step 2) can be replaced by other raw materials with graphite structures, including: one or more of natural graphite, artificial graphite, expanded graphite, or graphitized carbon microspheres.
The gas air may also replace other gas types in step 1), including: one or more of oxygen, nitrogen, hydrogen, argon, helium, carbon dioxide, or ozone.
The alcohols added in step 2) may further comprise: one or more of ethanol, n-propanol, isopropanol, n-butanol, isobutanol, sec-butanol, or tert-butanol; the total volume content of the added alcohols is 0.05 to 59%.
Preferably, in the step 3), the power of the ultrasonic liquid phase stripping treatment is 10000W to 15000W, the ultrasonic time is 30 to 40min, and the ultrasonic is stopped for 5min at intervals, namely every 2 to 5min.
Preferably, in the step 6), the power of the ultrasonic treatment is 1000W, and the ultrasonic time is 20-30 min.
According to the preparation method, the raw material containing the graphite lamellar structure can be subjected to ultrasonic liquid phase stripping treatment through the preparation equipment to obtain the conductive slurry, wherein micro bubbles contained in the liquid phase can be adsorbed on the raw material containing the graphite lamellar structure or the periphery of graphene formed by stripping in the liquid phase in the process of stripping, when the ultrasonic liquid phase stripping treatment is carried out, a large amount of ultrasonic energy can generate ultrasonic cavitation phenomenon, so that micro bubbles in water vibrate and grow under the action of an ultrasonic field and continuously gather acoustic field energy, when the energy reaches a certain threshold value, cavitation bubbles rapidly collapse and close, and the process can occur in the process of stripping graphene, thereby being beneficial to deeper stripping of the raw material containing the graphite lamellar structure into graphene.
In this embodiment, before the liquid phase stripping treatment or the ultrasonic treatment, carbon nanotubes may be further added into the mixing container 4 to prepare a conductive paste in which graphene and carbon nanotubes are mixed.
In order to more clearly clarify the technical idea of the present invention, the fine bubbles according to the present invention are further explained below. The type of the bubbles is defined according to the bubble particle size in the international standard of Micro bubbles ISO 20480-1:2017, wherein the bubbles with the particle size smaller than 100 μm are Micro bubbles (Fine bubbles), the bubbles with the particle size between 1 and 100 μm are Micro bubbles (Micro bubbles), and the bubbles with the particle size smaller than 1 μm are ultra Micro bubbles (ultra bubbles). The term "fine bubbles" in the present invention is consistent with this standard, and means bubbles having a bubble size of less than 100. Mu.m. In the present invention, the characteristic that the smaller the diameter of fine bubbles is, the longer the time of existence in water is, the more stable the present invention is. More preferably, the fine bubbles in the conductive paste of the present invention are ultrafine bubbles having a particle diameter of less than 1 μm. The test for bubble particle size can be performed using either a malvern Nanosight NS500 or IZON qNano nm particle size analysis device. The particle diameter value of the fine bubbles or the ultra fine bubbles in the present invention means the particle diameter value of D50 (D50 is the particle diameter at which the cumulative distribution of particles is 50%, also called median diameter or median diameter).
At present, the technology of generating micro-bubbles in liquid is mature, and the gas-liquid dispersion method adopted by the micro-bubble generating device mainly comprises the following steps according to the generation principle of micro-bubbles:
(1) Pressurizing and dissolving gas and releasing gas method: the gas is forced to dissolve in the liquid by pressurization to form a supersaturated state, and then the depressurized gas is released again to generate a large number of microbubbles, the size and strength of which depend on various conditions in releasing air and the surface tension of water.
(2) The air-floating pump air-producing method comprises the following steps: the impeller component is directly adopted to directly disperse air to generate micro bubbles, or the pressure dissolved air and the impeller are combined to disperse air, and three processes of gas-liquid mixing, pressurizing dissolved air and depressurizing released air are simultaneously realized in one pump, so that the bubble generation efficiency is improved.
(3) High-speed rotary cutting method: the gas-liquid two-phase enters the hollow part of the device to rotate, the specific gravity difference enables the gas to form a negative pressure gas shaft on the central shaft, the gas of the negative pressure gas shaft is cut off to become micro bubbles when passing through a gap between the external liquid and the internal high-speed rotating liquid, a large number of micro bubbles can be rapidly generated, and the uniformity of the bubble concentration is better.
(3) Jet aeration method: micro-bubbles are generated mainly through a jet aerator. The jet aerator has small nozzle diameter and high flow speed, and the liquid flow can form partial vacuum after entering the air chamber. At this time, the gas may enter the gas chamber through the gas suction pipe, be mixed with the liquid, and then form fine bubbles in the liquid after passing through the mixing pipe and the diffusion pipe.
(4) Microporous dispersed gas process: when compressed gas passes through a micropore medium, the gas is cut into tiny bubbles by micropores, the mode is relatively simple, the smaller the pore diameter of the micropore medium is, the narrower the distribution is, and the smaller and more concentrated the particle size of the formed bubbles are.
(5) Ultrasonic cavitation method: the liquid generates negative pressure through ultrasonic cavitation, gas originally dissolved in the liquid is released in the form of micro bubbles, and the control of bubble collapse can be realized, so that the method has a good prospect in the application aspect of precise bubble control.
(6) Mechanical shearing method: the gas is typically entrained into the swirling water flow by a pump, and the swirling is then broken down to crush the bubbles, which are then discharged through an outlet nozzle as fine bubbles.
(7) Electrolytic method: the main principle is that tiny bubbles are generated on the positive and negative plates by utilizing the mode of electrolyzing water by the electrodes. The micro-bubbles generated by the method have the advantages of diameter of 20-60 mu m, better size controllability, larger energy consumption, smaller bubble yield and the like.
The microbubble generation device of the prior art generally uses one or more microbubble generation methods, and can obtain a gas-liquid mixed fluid containing microbubbles with a particle size ranging from 10nm to 100 μm.
Example 8
In order to prove that the preparation method of the conductive paste has excellent stability, the preparation method in the embodiment 6 is adopted, 0.5wt.% of graphene suspension is obtained in the step S101, and the graphene conductive paste with the graphene content of 4wt.% is obtained after vacuum suction filtration, and is marked as a sample A. The gas-liquid mixed fluid in the step S101 is generated by adopting a micro-bubble generating device of a gas-floating pump gas generating method, namely, air and water are fully mixed by the gas-floating pump, and then are connected with an aeration device after pressurization and pressure release processes, the particle size range of micro-bubbles in the obtained gas-liquid mixed fluid is 10nm to 1 mu m, and the bubble concentration is in the order range of 10 6~109/ml. The bubbles are small in particle size, and belong to ultrafine bubbles and can be also called ultrafine bubble water. Adding deionized water into graphene conductive paste purchased in the market to prepare graphene conductive paste with the same mass content, and marking as a sample B. Samples a and B were placed in an ultrasonic apparatus and subjected to the same ultrasonic dispersion treatment, and then placed together for 6 months, as shown in fig. 8. As can be seen from the figure, the graphene conductive paste (sample a) obtained by the method of the present invention is still uniformly dispersed without obvious precipitation delamination, while the comparative sample (sample B) shows obvious delamination.
The foregoing description of the preferred embodiments of the invention is not intended to limit the scope of the invention, but rather to limit the scope of the invention in any way.
Claims (8)
1. An apparatus for producing a conductive paste, comprising:
the mixing container is used for mixing the gas-liquid mixed fluid and the treatment object, wherein the mixing container is provided with a conical bottom, the conical bottom is provided with an opening part, the opening part is also provided with a valve for controlling the opening and closing of the opening part, the inside of the mixing container is provided with a bearing structure, the bearing structure is used for placing a filter material, and the treatment object comprises one of raw materials with a graphite lamellar structure, graphene, carbon nano tubes or a mixture of the graphene and the carbon nano tubes;
a gas-liquid mixed fluid pipeline for conveying the gas-liquid mixed fluid into the mixing container;
The stirring device is used for stirring and mixing the gas-liquid mixed fluid and the treatment object; and/or at least one ultrasonic unit for liquid phase stripping treatment, stripping the raw material with the graphite lamellar structure into graphene, or ultrasonically mixing the gas-liquid mixed fluid with the treated object;
The vacuum suction filtration device comprises a liquid storage container and a vacuum pump, wherein the opening part of the liquid storage container is communicated with the opening part at the bottom of the mixing container, the liquid storage container also comprises a vacuum interface, the vacuum interface is connected with the vacuum pump through a pipeline, and the vacuum pump is used for generating negative pressure to suction-filter liquid in the mixing container into the liquid storage container;
The preparation equipment also comprises a micro-bubble generating device which is communicated with the mixing container through the gas-liquid mixed fluid pipeline and is used for mixing gas and liquid to obtain the gas-liquid mixed fluid;
the outer wall of the mixing vessel is also provided with a condensing device for controlling the temperature of the liquid in the mixing vessel.
2. The apparatus for preparing a conductive paste according to claim 1, wherein the liquid storage container is connected to a filtering means for delivering the filtered liquid to a liquid inlet line of the micro bubble generating means so that the liquid can be recycled.
3. The apparatus for preparing a conductive paste according to claim 1, wherein the micro bubble generating means, the stirring means, and/or the ultrasonic unit, the vacuum pump, and the valve are connected to a controller by wired or wireless means.
4. The apparatus for producing a conductive paste according to claim 1, wherein said fine bubble generating means is for performing a mixing treatment of a gas and a liquid by one or more of a mechanical shearing method, an ultrasonic cavitation method, a pressurized dissolved gas releasing method, a microporous dispersion gas method, a jet aeration method, or an air-floating pump gas generating method to obtain said gas-liquid mixed fluid.
5. A production method for obtaining a conductive paste using the production apparatus according to any one of claims 1 to 4, comprising the steps of:
Adding a gas-liquid mixed fluid, graphene and/or carbon nano tubes into a mixing container in a state that a valve is closed, wherein the mass content of the graphene and/or the carbon nano tubes is between 0.1 wt and 1wt percent; the gas-liquid mixed fluid contains micro bubbles, the particle size of the micro bubbles is smaller than 100 mu m, and the concentration of the micro bubbles is larger than 10 6/ml;
stirring by a stirring device and performing ultrasonic treatment by an ultrasonic unit to obtain a suspension in which the graphene and/or the carbon nanotubes are uniformly dispersed;
and carrying out vacuum suction filtration on the suspension in the mixing container through a vacuum suction filtration device, and controlling the quantity of the suction-filtered liquid to further concentrate the suspension until the mass content is between 3 wt and 8 wt percent to obtain the conductive slurry.
6. The method of producing a conductive paste according to claim 5, wherein the stirring treatment is performed at a rotation speed of a stirring rotor of between 1000 rpm and 5000 rpm; the ultrasonic treatment is carried out with ultrasonic power of 500W to 2000W and treatment time of 1 to 60 min.
7. The method for preparing a conductive paste according to claim 5, further comprising a step of preparing the graphene by a liquid phase exfoliation treatment, comprising:
Adding first fine bubble water, alcohols and raw materials with a graphite lamellar structure into the mixing container, and stirring by the stirring device;
After the stirring treatment, carrying out liquid phase stripping treatment by the ultrasonic unit to obtain graphene suspension with the stripped graphite lamellar structure;
Carrying out vacuum suction filtration on the graphene suspension in the mixing container through the vacuum suction filtration device, and filtering out water to obtain a filter material, wherein the filter material contains the graphene;
Adding second fine bubble water into the mixing container, and carrying out suction filtration and washing on the filter material through the vacuum suction filtration device to remove the alcohol impurities in the filter material to obtain the graphene;
wherein the first fine bubble water and the second fine bubble water are aqueous solutions containing fine bubbles, and the first fine bubble water and the second fine bubble water are the same or different.
8. The method of preparing a conductive paste according to claim 7, wherein the alcohols include: one or more of ethanol, n-propanol, isopropanol, n-butanol, isobutanol, sec-butanol, or tert-butanol; adding the alcohol in a total volume content of 5 to 59%; the raw materials comprise one or more of natural graphite, artificial graphite, expanded graphite, graphitized carbon microspheres or expanded carbon microspheres; in the liquid phase stripping treatment, the ultrasonic power of the ultrasonic unit is 1000W to 20000W, and the treatment time is 1 min to 60min.
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