CN112473966A - Three-electrode discharge plasma auxiliary ball-milling tank - Google Patents
Three-electrode discharge plasma auxiliary ball-milling tank Download PDFInfo
- Publication number
- CN112473966A CN112473966A CN202011177316.XA CN202011177316A CN112473966A CN 112473966 A CN112473966 A CN 112473966A CN 202011177316 A CN202011177316 A CN 202011177316A CN 112473966 A CN112473966 A CN 112473966A
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- cover plate
- electrode
- ball milling
- discharge plasma
- discharge
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- 238000000498 ball milling Methods 0.000 title claims abstract description 50
- 229910052751 metal Inorganic materials 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims abstract description 5
- 230000007704 transition Effects 0.000 claims abstract description 4
- 238000007789 sealing Methods 0.000 claims description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 239000004519 grease Substances 0.000 claims description 6
- 229920001296 polysiloxane Polymers 0.000 claims description 6
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 2
- 239000011324 bead Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 210000002381 plasma Anatomy 0.000 description 26
- 239000000843 powder Substances 0.000 description 11
- 230000005684 electric field Effects 0.000 description 8
- 230000004888 barrier function Effects 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 239000007772 electrode material Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 229910001415 sodium ion Inorganic materials 0.000 description 3
- 239000011232 storage material Substances 0.000 description 3
- 238000005551 mechanical alloying Methods 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C19/00—Other disintegrating devices or methods
- B02C19/18—Use of auxiliary physical effects, e.g. ultrasonics, irradiation, for disintegrating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/10—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with one or a few disintegrating members arranged in the container
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C19/00—Other disintegrating devices or methods
- B02C19/18—Use of auxiliary physical effects, e.g. ultrasonics, irradiation, for disintegrating
- B02C2019/183—Crushing by discharge of high electrical energy
Abstract
The invention discloses a three-electrode discharge plasma auxiliary ball-milling tank which comprises a connecting cylinder body, a rear cover plate, a front cover plate and three parallel electrode rods. The electrode bar is connected with the inner circular hole of the rear cover plate in a transition fit mode, the conductive electric core of the electrode bar is connected to the positive electrode of the plasma power supply, the whole metal cylinder is connected to the negative electrode of the plasma power supply, and the discharge of different electrode bars is mutually independent. The device is simple and practical, local high-intensity discharge can be easily realized by adjusting the power within the working voltage range of the plasma power supply, and the gas ionization rate and the ball milling energy efficiency in the ball milling tank are greatly improved; meanwhile, the multi-electrode discharge can also effectively prevent the discharge interruption phenomenon caused by the damage of a single electrode rod in the ball milling process, remarkably reduce the failure rate of the plasma auxiliary ball mill and promote the application of the plasma auxiliary ball mill in the actual production.
Description
Technical Field
The invention belongs to the technical field of powder metallurgy and mechanical alloying, and particularly relates to a three-electrode discharge plasma auxiliary ball-milling tank and application thereof in the aspects of preparing lithium ion battery electrode materials, sodium ion battery electrode materials, hydrogen storage materials, hard alloys and the like.
Background
In recent years, the dielectric barrier discharge plasma auxiliary ball milling technology is a novel and efficient external field auxiliary ball milling method for realizing mechanical alloying, the ball milling process is usually carried out in the atmosphere of oxygen, argon, ammonia, hydrogen and the like, and the applied high-frequency high-voltage electric field can ionize the gas to form low-temperature plasma with high energy density. The electron temperature of the low-temperature plasma is extremely high, the electron temperature can instantaneously heat the micro-area of the powder to melt or sputter the surface layer of the powder, and the macroscopic temperature of the whole discharge space is kept near the room temperature, so that the workpiece cannot be burnt. The synergistic effect of the plasma and the mechanical force of the ball mill ensures that the powder can easily reach the nanoscale size under the mechanism action of melting-thermal explosion-quenching, and has high powder refining efficiency; meanwhile, the plasma can also carry out thinning, etching, doping and other treatments on the laminar material, so that various defects such as dislocation, atom vacancy, lattice distortion and the like can be generated in the crystal lattices of the powder particles, and the defects greatly improve the activity of the powder. At present, the method is widely applied to the preparation of nano-powder such as electrode materials of lithium ion batteries and sodium ion batteries, hydrogen storage materials, hard alloys and the like.
Currently, a common dielectric barrier discharge plasma assisted ball mill generally adopts a single electrode discharge mode, that is, only one electrode rod is connected in a ball milling tank, such as CN201410815093.3, CN 200810026690.2, CN 200520056595.9 and the like. However, in the single-electrode discharge mode, because the gap between the positive electrode and the negative electrode is large, the electric field intensity in the ball milling tank is low, and the gas is not completely ionized, so that the energy density of plasma is low, and the ball milling energy efficiency is influenced. In addition, in the working process, the electrode rod is in the environment of non-uniform electric field and high mechanical force action for a long time, the service life is short, and the phenomenon of discharge interruption often occurs during the operation of the ball mill, so that the failure rate of the dielectric barrier discharge plasma auxiliary ball mill in practical application is high, and the continuous use is influenced. Therefore, the improvement of the ionization rate of gas in the ball milling tank and the reduction of the failure rate of the ball mill are problems to be solved urgently in the current dielectric barrier discharge plasma auxiliary ball milling technology.
Disclosure of Invention
In order to solve the problems in the existing dielectric barrier discharge plasma auxiliary ball milling technology, the invention provides a technical scheme of a three-electrode discharge plasma auxiliary ball milling tank from the perspective of improving the ball milling tank.
The invention aims to provide a three-electrode discharge plasma auxiliary ball-milling tank, which can easily realize local high-intensity discharge by adjusting power within the working voltage range of a plasma power supply by increasing the number of electrode bars in the ball-milling tank, and greatly improve the ionization rate and ball-milling energy efficiency of gas in the ball-milling tank. And even if a single electrode bar in the ball milling tank is damaged, other electrode bars can still maintain dielectric barrier discharge, and the plasma discharge environment can be kept in the ball milling tank all the time, so that the failure rate of the dielectric barrier discharge plasma auxiliary ball mill is obviously reduced.
The purpose of the invention is realized by the following technical scheme: the utility model provides a ball-milling jar is assisted to three electrode discharge plasma, is including connecting barrel, back shroud, front shroud and parallelly connected three electrode bar, the material of connecting the barrel is the metal material, and the material of back shroud and front shroud is polytetrafluoroethylene or high-purity pottery. The surfaces of the rear cover plate, the front cover plate and the cylinder body, which are contacted with each other, are provided with an annular sealing groove and a plurality of through holes, the cover plate and the cylinder body are fixed through bolts, and an annular sealing ring and a vacuum silicone grease seal are arranged between the cover plate and the cylinder body. The back cover plate is internally provided with a plurality of round holes, the electrode rods are connected with the round holes in a transition fit mode, circular shoulders are arranged at corresponding matching positions of the electrode rods, and the matching positions are sealed by sealing rings and vacuum silicone grease.
The conductive electric cores of the three electrode bars are simultaneously connected with the positive electrode of the plasma power supply, the whole metal cylinder is connected with the negative electrode of the plasma power supply, and the discharge of different electrode bars is mutually independent. The vacuum air valve is arranged on the outer side of the front cover plate, and an air inlet and outlet hole is formed below the vacuum air valve, so that ball milling can be performed in the gas atmosphere of vacuum, oxygen, argon, ammonia, hydrogen and the like.
FIG. 2 is a cross-sectional view of a three-electrode ball mill jar, wherein the inner diameter of the ball mill jar is R, and P1, P2 and P3 correspond to the positions of three electrodes respectively. A rectangular coordinate system is established in FIG. 2, P1 is located at the position of a positive half axis R/2-2R/3 of a y axis, and P2 and P3 are positions obtained after P1 rotates clockwise and anticlockwise around the center of the ball milling pot by 60-120 degrees respectively. Assuming that the included angles between the three electrode rods and the central connecting line of the ball milling tank are all 120 degrees, the voltage on each electrode rod is respectively V1, V2 and V3, and under the voltage configuration, the electric field intensity of any point P in the ball milling tank is EPx (V1,V2,V3)(X-direction component), EPy (V1,V2,V3)(Y-direction component) and EP(resultant field strength). Due to the vectorial and symmetrical nature of the field strength, the field strength for point P1 has:
according to the principle of superposition:
according to the formulas (1-1) and (1-2), the field intensity of one point in the ball milling tank under any voltage configuration can be formed by the superposition of the field intensities generated by three electrodes under the basic voltage configuration. Because of the superposition of electric fields, the electric field intensity generated by the three electrodes is reduced relative to that of a single electrode in the central area of the ball milling tank, but the space electric field intensity generated by the three electrodes is far larger than that of the single electrode in the field area range between the electrodes and the inner wall of the ball milling tank, and the electric field distribution is more uniform. The three-electrode discharge observed in the experiment is that each electrode rod independently emits purple light beams to the wall of the ball milling tank, and the discharge phenomenon at the center of the ball milling tank is weaker, so the design of the three-electrode ball milling tank can locally increase the discharge intensity of the inner wall field of the ball milling tank, the ball milling efficiency is improved, and the treatment effect of moving powder materials along the wall is more facilitated.
Compared with the prior art, the invention has the following advantages and gain effects:
under the same working voltage, compared with a single-electrode discharge mode, the three electrode rods connected in parallel can realize discharge with higher strength, and the gas is fully ionized to generate more high-activity plasmas in the ball-milling tank, so that the crushing and the refining of powder are promoted. Under the action of plasma, various defects are generated on the surface of the powder, the activity of the powder is improved, and the powder has obvious advantages in the aspects of preparing electrode materials of lithium ion batteries and sodium ion batteries, hydrogen storage materials, hard alloys and the like. Meanwhile, the three-electrode discharge can also effectively prevent the phenomenon of plasma discharge interruption in the ball milling process, remarkably reduce the failure rate of the ball mill and promote the application of the ball mill in actual production.
Drawings
Fig. 1 is a schematic structural diagram of an embodiment of the present invention.
Figure 2 is a cross section of a three electrode rod ball mill pot.
Fig. 3 is a side view (rear cover portion) of an embodiment of the present invention.
Fig. 4 is a side view (front cover portion) of an embodiment of the present invention.
The various components in the figure are as follows: the connecting cylinder comprises a connecting cylinder body 1, a rear cover plate 2, a front cover plate 3, an electrode rod 4, a conductive battery core 5, a bolt 6, a small sealing ring 7, a round hole 8, a large sealing ring 9, an air hole and a vacuum air valve 10.
Detailed Description
The three-electrode discharge plasma auxiliary ball-milling tank comprises a connecting cylinder body 1, a rear cover plate 2, a front cover plate 3 and three parallel electrode rods 4, as shown in figure 1. The connecting cylinder 1 is made of metal, and the front cover plate 3 and the rear cover plate 2 are made of polytetrafluoroethylene or high-purity ceramic. The conductive electric core of the parallel electrode rod 4 is simultaneously connected with the positive electrode of the plasma power supply, the whole metal tank body is connected with the negative electrode of the plasma power supply, and the discharge of different electrodes is mutually independent.
The surfaces of the front cover plate 3 and the rear cover plate 2, which are in contact with the connecting cylinder body 1, are provided with an annular sealing groove and a plurality of through holes, the front cover plate and the rear cover plate are respectively fixed with the connecting cylinder body through symmetrically distributed bolts 6, and the contact part between the cover plate and the cylinder body is sealed by an annular sealing ring and vacuum silicone grease, as shown in figure 1.
Fig. 3 and 4 are side views of the present invention, a plurality of circular holes are arranged in the back cover plate 2, the electrode rod is connected with the circular holes in a transition fit manner, the electrode rod is provided with a shoulder at the corresponding matching position, and the matching position is sealed by a sealing ring and vacuum silicone grease, as shown in fig. 3. A vacuum air valve is arranged on the outer side of the front cover plate 3, and an air inlet and an air outlet are arranged below the vacuum air valve, so that ball milling can be carried out in a gas atmosphere of vacuum, oxygen, argon, ammonia, hydrogen and the like, as shown in fig. 4.
The above embodiments are only preferred embodiments of the present invention, but the embodiments of the present invention are not intended to limit the scope of the present invention, and all equivalent changes, modifications, substitutions, combinations, and simplifications made according to the content and principle of the present invention as described in the claims of the present application should be included in the equivalent substitution ways within the scope of the present invention.
Claims (7)
1. A three-electrode discharge plasma auxiliary ball-milling tank comprises a connecting cylinder body (1), a rear cover plate (2), a front cover plate (3) and three parallel electrode rods (4); the rear cover plate (2) and the front cover plate (3) are arranged at two ends of the connecting cylinder body (1), and the three electrode rods (4) are connected in parallel and fixed on the rear cover plate (2) and the front cover plate (3).
2. A three-electrode discharge plasma auxiliary ball milling pot as claimed in claim 1, wherein the conductive cell (5) of the electrode rod is connected to the positive electrode of the plasma power supply at the same time, the whole cylinder is connected to the negative electrode of the plasma power supply, and the discharges of different electrode rods are independent.
3. The three-electrode discharge plasma-assisted ball milling pot according to claim 1, wherein the connecting cylinder is made of metal.
4. The three-electrode discharge plasma-assisted ball milling jar according to claim 1, wherein the back cover plate and the front cover plate are made of polytetrafluoroethylene or high-purity ceramic.
5. A three-electrode discharge plasma auxiliary ball milling pot according to claim 1, characterized in that the contact surfaces of the rear cover plate (2) and the front cover plate (3) with the connecting cylinder (1) are provided with an annular sealing groove and a plurality of through holes, the cover plate and the cylinder are fixed by bolts (6), and the contact part of the cover plate and the cylinder is sealed by an annular sealing ring (9) and vacuum silicone grease.
6. The three-electrode discharge plasma auxiliary ball milling pot according to claim 1, wherein three circular holes (8) are formed in the rear cover plate, the included angle between the connecting line of the adjacent two circular holes and the center of the cover plate ranges from 60 degrees to 120 degrees, and the distance between the circular hole and the center of the cover plate is about 1/2-2/3 of the inner diameter R of the ball milling pot; the electrode rod is connected with the round hole in a transition fit mode, a circular bead is arranged at the corresponding fit position of the electrode rod, and the fit position is sealed by a sealing ring (7) and vacuum silicone grease.
7. A three-electrode discharge plasma auxiliary ball-milling tank is characterized in that a vacuum air valve is arranged on the outer side of a front cover plate, and an air inlet and outlet hole is formed below the vacuum air valve, so that ball-milling can be performed in vacuum, oxygen, argon, ammonia or hydrogen atmosphere.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011177316.XA CN112473966B (en) | 2020-10-29 | 2020-10-29 | Three-electrode discharge plasma auxiliary ball milling tank |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011177316.XA CN112473966B (en) | 2020-10-29 | 2020-10-29 | Three-electrode discharge plasma auxiliary ball milling tank |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112473966A true CN112473966A (en) | 2021-03-12 |
| CN112473966B CN112473966B (en) | 2023-12-15 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011177316.XA Active CN112473966B (en) | 2020-10-29 | 2020-10-29 | Three-electrode discharge plasma auxiliary ball milling tank |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116213041A (en) * | 2021-12-02 | 2023-06-06 | 山东理工大学 | Multi-energy field coupling reaction device for material preparation and mechanochemical reaction |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080050291A1 (en) * | 2004-10-18 | 2008-02-28 | Yutaka Electronics Industry Co.,Ltd. | Plasma Generation Device |
| CN101239335A (en) * | 2008-03-07 | 2008-08-13 | 华南理工大学 | Plasma auxiliary high-energy planetary ball mill device |
| CN103846111A (en) * | 2012-11-30 | 2014-06-11 | 神华集团有限责任公司 | Plasma processing apparatus for powder or particles |
| CN104549658A (en) * | 2014-12-24 | 2015-04-29 | 华南理工大学 | Application method of cold field plasma discharge assisted high energy ball milled powder and plasma assisted high energy ball milling device |
-
2020
- 2020-10-29 CN CN202011177316.XA patent/CN112473966B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080050291A1 (en) * | 2004-10-18 | 2008-02-28 | Yutaka Electronics Industry Co.,Ltd. | Plasma Generation Device |
| CN101239335A (en) * | 2008-03-07 | 2008-08-13 | 华南理工大学 | Plasma auxiliary high-energy planetary ball mill device |
| CN103846111A (en) * | 2012-11-30 | 2014-06-11 | 神华集团有限责任公司 | Plasma processing apparatus for powder or particles |
| CN104549658A (en) * | 2014-12-24 | 2015-04-29 | 华南理工大学 | Application method of cold field plasma discharge assisted high energy ball milled powder and plasma assisted high energy ball milling device |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116213041A (en) * | 2021-12-02 | 2023-06-06 | 山东理工大学 | Multi-energy field coupling reaction device for material preparation and mechanochemical reaction |
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| CN112473966B (en) | 2023-12-15 |
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