CN112473966B - Three-electrode discharge plasma auxiliary ball milling tank - Google Patents
Three-electrode discharge plasma auxiliary ball milling tank Download PDFInfo
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- CN112473966B CN112473966B CN202011177316.XA CN202011177316A CN112473966B CN 112473966 B CN112473966 B CN 112473966B CN 202011177316 A CN202011177316 A CN 202011177316A CN 112473966 B CN112473966 B CN 112473966B
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- cover plate
- ball milling
- electrode
- milling tank
- cylinder body
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- 238000000498 ball milling Methods 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims abstract description 4
- 239000002184 metal Substances 0.000 claims abstract description 4
- 230000007704 transition Effects 0.000 claims abstract description 4
- 230000005684 electric field Effects 0.000 claims description 9
- 238000007789 sealing Methods 0.000 claims description 9
- 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
- 239000002131 composite material Substances 0.000 claims 1
- 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 10
- 230000004888 barrier function Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000007772 electrode 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
- 239000000956 alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 210000004027 cell Anatomy 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
- 239000007769 metal material Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- 239000013078 crystal Substances 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
- 238000004880 explosion Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 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
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
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
Landscapes
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Crushing And Grinding (AREA)
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 electrode rods which are connected in parallel. The electrode rod is connected with the round hole in the rear cover plate in a transition fit manner, the conductive electric core of the electrode rod is simultaneously connected with the anode of the plasma power supply, the whole metal cylinder body is connected with the cathode of the plasma power supply, and the discharge of different electrode rods is mutually independent. The device is simple and practical, can easily realize local high-intensity discharge by adjusting power in the working voltage range of the plasma power supply, and greatly improves the gas ionization rate and the ball milling energy efficiency in the ball milling tank; meanwhile, the multi-electrode discharge can also effectively prevent discharge interruption phenomenon caused by single electrode rod damage in the ball milling process, obviously reduce the failure rate of the plasma auxiliary ball mill and promote the application of the plasma auxiliary ball mill in 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-assisted 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 alloy and the like.
Background
In recent years, the dielectric barrier discharge plasma assisted ball milling technology is a novel and efficient external field assisted ball milling method for realizing mechanical alloying, the ball milling process is usually carried out in an atmosphere of oxygen, argon, ammonia, hydrogen and the like, and the gas is ionized to form low-temperature plasma with high energy density under the action of an external high-frequency high-voltage electric field. The electron temperature of the low-temperature plasma is extremely high, and the electron temperature can instantly heat the micro-area of the powder to enable the surface layer of the powder to be melted or sputtered, while the macroscopic temperature of the whole discharge space is kept near the room temperature, so that the workpiece is not burnt. The synergistic effect of the plasmas and the mechanical force of the ball mill ensures that the powder is extremely easy to reach the nanoscale scale under the action of a mechanism of melting, thermal explosion and quenching, and has high powder refining efficiency; meanwhile, plasma can also carry out thinning, etching, doping and other treatments on lamellar materials, so that various defects such as dislocation, atomic vacancy, lattice distortion and the like can be generated in crystal lattices of 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 alloy and the like.
The conventional dielectric barrier discharge plasma auxiliary ball mill generally adopts a single-electrode discharge mode, namely, 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, the gap between the positive electrode and the negative electrode is large, so that the electric field intensity in the ball milling tank is low, and the gas is not completely ionized, so that the energy density of the plasma is low, and the ball milling energy efficiency is affected. In addition, in the working process, the electrode rod is in an environment with a non-uniform electric field and high mechanical force for a long time, the service life of the electrode rod is short, and the phenomenon of discharge interruption frequently occurs when the ball mill runs, so that the dielectric barrier discharge plasma assisted ball mill has high failure rate in practical application and affects continuous use. Therefore, the method improves the ionization rate of the gas in the ball milling tank and reduces the failure rate of the ball mill, and is a problem to be solved in the current dielectric barrier discharge plasma assisted ball milling technology.
Disclosure of Invention
In order to solve the problems in the prior 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 angle 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 in the working voltage range of a plasma power supply by increasing the number of electrode rods in the ball milling tank, and greatly improve the ionization rate and the ball milling energy efficiency of gas in the ball milling tank. And even if a single electrode rod in the ball milling tank is damaged, other electrode rods can still maintain dielectric barrier discharge, and the environment of plasma discharge can be always maintained in the ball milling tank, so that the failure rate of the dielectric barrier discharge plasma auxiliary ball mill is obviously reduced.
The aim of the invention is achieved by the following technical scheme: the utility model provides a three electrode discharge plasma assists ball-milling jar, includes connecting barrel, back shroud, front shroud and parallelly connected three electrode stick, the material of connecting the barrel is the metal material, and the material of back shroud and front shroud is polytetrafluoroethylene or high purity ceramic. The surface that back shroud, front shroud and barrel contacted all is equipped with an annular seal groove and a plurality of through-holes, through bolt fastening apron and barrel, and is equipped with annular seal circle and vacuum silicone grease seal between apron and the barrel. The rear cover plate is internally provided with a plurality of round holes, the electrode bars are connected with the round holes in a transition fit manner, shoulders are arranged at corresponding matching positions of the electrode bars, and the matching positions are sealed by adopting sealing rings and vacuum silicone grease.
The conductive cells of the three electrode bars are simultaneously connected with the positive electrode of the plasma power supply, the whole metal cylinder body is connected with the negative electrode of the plasma power supply, and the discharge of the different electrode bars is mutually independent. The outside of the front cover plate is provided with a vacuum air valve, and an air inlet and outlet hole is arranged below the vacuum air valve, so that ball milling can be performed in the atmosphere of vacuum, oxygen, argon, ammonia, hydrogen and the like.
Fig. 2 is a cross-sectional view of a three-electrode ball-milling pot, wherein the inner diameter of the ball-milling pot is set to be R, and the positions of P1, P2 and P3 respectively correspond to the positions of three electrodes. In FIG. 2, a rectangular coordinate system is established, P1 is positioned at the position of a positive half axis R/2-2R/3 of a y axis, and P2 and P3 are respectively positions obtained after P1 rotates clockwise and anticlockwise by 60-120 degrees around the center of the ball milling tank. Assuming that the included angles between the three electrode bars and the central connecting line of the ball milling tank are 120 DEG, setting the voltage on each electrode bar as V1, V2 and V3 respectively, and setting the electric field intensity of any point P in the ball milling tank as E under the voltage configuration Px (V1,V2,V3) (X-direction component), E Py (V1,V2,V3) (Y-direction component) and E P (resultant field strength). Because of the vectoriality and symmetry of the field strength, the field strength at the P1 point is:
the method can be obtained according to the superposition principle:
the field intensity of one point in the ball milling tank under any voltage configuration can be overlapped by the field intensity generated by three electrodes under the basic voltage configuration, which is obtained by the formulas (1-1) and (1-2). Because of the superposition of the electric fields, the electric field intensity generated by the three electrodes is reduced relative to that of the single electrode in the central area of the ball milling tank, but the space electric field intensity generated by the three electrodes is far greater than that generated by the single electrode in the field area 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 by the experiment is that each electrode rod independently emits a purple light beam to the tank wall, and the central discharge phenomenon of the ball milling tank is weaker, so that the design of the three-electrode ball milling tank can locally increase the discharge intensity of the field on the inner wall 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, three electrode rods are connected in parallel, so that higher-intensity discharge can be realized, and gas is fully ionized to enable more high-activity plasmas to be generated in the ball milling tank, so that crushing and refinement 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 preparation method has obvious advantages in the aspects of preparing electrode materials, hydrogen storage materials, hard alloy and the like of lithium ion batteries and sodium ion batteries. Meanwhile, the three-electrode discharge can also effectively prevent the plasma discharge from being interrupted in the ball milling process, obviously reduce the fault rate of the ball mill and promote the application of the ball mill in actual production.
Drawings
Fig. 1 is a schematic structural view of an embodiment of the present invention.
Fig. 2 is a cross section of a ball milling pot for a three electrode rod.
Fig. 3 is a side view (back cover portion) of an embodiment of the present invention.
Fig. 4 is a side view (front cover plate portion) of an embodiment of the present invention.
The individual components in the figure are as follows: the device comprises a connecting cylinder body 1, a rear cover plate 2, a front cover plate 3, an electrode rod 4, a conductive cell 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 electrode rods 4 which are connected in parallel, as shown in figure 1. Wherein, the material of connecting cylinder 1 is metal material, and the material of front shroud 3, back shroud 2 can be polytetrafluoroethylene or high-purity pottery. The conductive cells of the parallel electrode bars 4 are 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 adopting an annular sealing ring and vacuum silicone grease, as shown in figure 1.
Fig. 3 and 4 are side views of the invention, a plurality of round holes are arranged in the rear cover plate 2, electrode rods are connected with the round holes in a transition fit manner, shoulders are arranged at corresponding matching positions of the electrode rods, and sealing rings and vacuum silicone grease seal are adopted at the matching positions, as shown in fig. 3. The outside of the front cover plate 3 is provided with a vacuum air valve, and an air inlet and outlet hole is arranged below the vacuum air valve, so that ball milling can be performed in the atmosphere of vacuum, oxygen, argon, ammonia, hydrogen and the like, as shown in fig. 4.
The foregoing embodiment is only one preferred embodiment of the present invention, but the embodiment of the present invention is not intended to limit the scope of the novel invention, and all equivalent changes, modifications, substitutions, combinations, and simplifications made according to the contents and principles of the present invention as described in the claims are intended to be included in the scope of the present invention.
Claims (1)
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 electrode rods (4) which are connected in parallel; 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);
the inner diameter of the ball milling tank is set to be R, the positions of P1, P2 and P3 corresponding to three electrodes respectively, a rectangular coordinate system is established, P1 is positioned at the position of a positive half axis R/2-2R/3 of a y axis, P2 and P3 are respectively positions obtained by rotating P1 clockwise and anticlockwise around the center of the ball milling tank by 120 DEG, when the included angles of the three electrode bars and the connecting line of the center of the ball milling tank are 120 DEG, the voltage on each electrode bar is V1, V2 and V3 respectively, and under the voltage configuration, the electric field intensity of any point P in the ball milling tank is X-direction component E Px (V1,V2,V3) Component E in Y direction Py (V1,V2,V3) Composite field strength E P Because of the vectoriality and symmetry of the field strength, the field strength for the P1 point is:
the method can be obtained according to the superposition principle:
the field intensity of one point in the ball milling tank under any voltage configuration is formed by superposition of field intensities generated by three electrodes under basic voltage configuration, wherein the field intensities are obtained by the formulas (1-1) and (1-2);
the conductive electric core (5) of the electrode rod is connected with the positive electrode of the plasma power supply at the same time, the whole cylinder body is connected with the negative electrode of the plasma power supply, and the discharge of different electrode rods is mutually independent;
the connecting cylinder body is made of metal;
the rear cover plate and the front cover plate are made of polytetrafluoroethylene or high-purity ceramic;
the surfaces of the rear cover plate (2) and the front cover plate (3) which are contacted with the connecting cylinder body (1) are provided with an annular sealing groove and a plurality of through holes, the cover plate and the connecting cylinder body are fixed through bolts (6), and the contact part of the cover plate and the connecting cylinder body is sealed by adopting an annular sealing ring (9) and vacuum silicone grease;
three round holes (8) are formed in the rear cover plate, the included angle between the connecting lines of two adjacent round holes and the center of the rear cover plate ranges from 60 degrees to 120 degrees, and the distance between the round holes and the center of the rear cover plate is 1/2 to 2/3 of the inner diameter R of the ball milling tank; the electrode rod is connected with the round hole in a transition fit way, a shoulder is arranged at a corresponding fit position of the electrode rod, and the fit position is sealed by a sealing ring (7) and vacuum silicone grease;
the outer side of the front cover plate is provided with a vacuum air valve, and an air inlet and outlet hole is arranged 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 |
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| Publication Number | Publication Date |
|---|---|
| CN112473966A CN112473966A (en) | 2021-03-12 |
| CN112473966B true CN112473966B (en) | 2023-12-15 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202011177316.XA Active CN112473966B (en) | 2020-10-29 | 2020-10-29 | Three-electrode discharge plasma auxiliary ball milling tank |
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| Country | Link |
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| CN (1) | CN112473966B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006114450A (en) * | 2004-10-18 | 2006-04-27 | Yutaka Electronics Industry Co Ltd | Plasma generating device |
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- 2020-10-29 CN CN202011177316.XA patent/CN112473966B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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