CN104549658B - Cold field plasma discharge assisted high energy ball milled powder device - Google Patents
Cold field plasma discharge assisted high energy ball milled powder device Download PDFInfo
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- CN104549658B CN104549658B CN201410815093.3A CN201410815093A CN104549658B CN 104549658 B CN104549658 B CN 104549658B CN 201410815093 A CN201410815093 A CN 201410815093A CN 104549658 B CN104549658 B CN 104549658B
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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
- 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
- B02C17/14—Mills in which the charge to be ground is turned over by movements of the container other than by rotating, e.g. by swinging, vibrating, tilting
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
- B02C23/06—Selection or use of additives to aid 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
- B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
- B02C23/18—Adding fluid, other than for crushing or disintegrating by fluid energy
- B02C23/24—Passing gas through crushing or disintegrating zone
-
- 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 provides a cold field plasma discharge assisted high energy ball milled powder device. The device comprises a vibrating type high energy ball milled main machine, an additionally-arranged cold field plasma power supply, a discharge ball milled pot, a discharge electrode bag, an atmosphere-controllable system and a cooling system. The method comprises the following steps: utilizing dielectric barrier discharge to generate plasmas, introducing a dielectric barrier discharge electrode bar into a high-speed vibrating ball-milling tank, on one hand, requiring a solid insulating medium on the outer layer of the electrode bar to simultaneously bear high-voltage discharge and mechanical shock failure of the grinding ball, and on the other hand, requiring the high-speed vibrating ball milling device to uniformly process the powder. The method is based on the ordinary ball milling technology; the processing efficiency and the effect of the ball mill can be greatly improved by the following steps: under a non-heat-balance discharge condition of the pressure that the discharge space pressure is set to be about 102-106 Pa, introducing the discharge plasmas to input another effective energy to the processed powder, promoting the powder to be processed to be subjected to combined action of the mechanical stress effect and the heat effect of the external electric field, and further accelerating refining of the powder and promoting the alloying progress.
Description
Technical field
The invention belongs to machine-building and powder metallurgical technology, are related to a kind of high-energy ball milling device, and in particular to one
Plant awkward silence at a meeting plasma auxiliary high-energy ball milling powder body device.
Background technology
The method that common high-energy ball milling prepares alloy powder is that prepared by current nano and micro materials and mechanical alloying is the most frequently used
One of technology, usually rotated using high energy ball mill or vibrated metal or alloy powder fining to micro-meter scale is received, i.e.,：
Two or more powder is put in the ball grinder of high energy ball mill simultaneously carries out ball milling, powder abrasive particle Jing calenderings, pressure
Close, pulverize, then the repetitive process (i.e. cold welding-crushing-cold welding be repeated) for pressing, powder grain and particle size can be made
Constantly refinement, can finally obtain a micron superfine alloy powder of receiving for tissue and distributed components.Usual high energy ball mill is only
It is simple by rotation or vibrating ball grinding jar, powder, that is, only machinery is processed using the mechanical energy of abrading-ball in ball grinder
Stress field facilitates powder to have an effect.However, the application of current mechanical alloying is concentrated mainly on planetary and stirring-type ball
Grinding machine aspect, this mechanical alloying has that energy consumption is big, the low shortcoming of efficiency.
Plasma generator typically under negative pressure (vacuum), to reacting gas environment high-frequency electric field is applied, and gas exists
Ionize under the excitation of high-frequency electric field, produce plasma.The activity of these ions is very high, and its energy be enough to destroy almost all of
Chemical bond, in any exposed material surface chemical reaction is caused, so that the structure of material surface, composition and group become
Change, be met the surface of actual requirement.Meanwhile, plasma reaction speed is fast, treatment effeciency is high, and modified occurs over just
Material surface, does not affect on the performance of material internal bulk material, is preferable surface modified method.Plasma surface changes
Property have been widely used in the materials of shape such as film like, block and graininess, and material of different shapes must be adopted
Different corona treatment modes, such as film like material (including thin film, fabric, non-woven fabrics, silk screen), because it can be into
Coil packing, therefore Reel-to-reel type batch processing can be adopted；Lump material is due to putting one by one therefore flat suitable for multilamellar
Plate electrode process.And application of the plasma in terms of powder particle is processed is less, particularly plasma is incorporated into into high energy
Difficulty in ball mill apparatus is bigger.This is mainly due to two aspects：One is that the reunion between microgranule makes because powder body is piled up
The microparticle surfaces that must be not exposed in plasma atmosphere cannot be processed, it is difficult to realized that microgranule is all processed, caused microgranule
Process incomplete, uneven, poor processing effect；Two is the common work of the high velocity impact of abrading-ball and electrion in high-energy ball milling tank
Serious with the destruction to sparking electrode, electrode life-span in ball grinder is very short.Therefore, a kind of effective plasmaassisted is needed badly
High-energy ball milling processes the device of powder body material.
The A of CN 1718282 disclose a kind of high energy ball mill method with plasma aid, and it is mainly described in general milling
How to improve on the basis of machine and realize plasma discharge aid in ball milling effect, but the specific configuration for main ball mill,
The structure design of electric discharge ball grinder, the particularly selection of medium blocking discharge electrode rod and design are not done further open.And it is real
On border, plasma auxiliary high-energy ball mill is in additional plasma electrical source, electric discharge ball grinder and medium blocking discharge electrode rod
Etc. aspect there are various technical barriers, during particularly electrode bar introduces ball grinder, exist cooperate, localized high intensity
The problems such as disruptive discharge and plasma discharge strength control, and electrode bar itself has and is limited to material and structure brought
The problem in various impact life-spans, is all that foregoing invention patent is unsolved.
A the and CN1011239336 A of CN 101239334 individually disclose a kind of plasma auxiliary high-energy roller ball mill
Device and a kind of plasmaassisted stirring ball mill device, it is mainly converted in conventional rollers and agitating ball mill
, but this two bulbs mill mechanical can be less, and grinding efficiency is low, is not only difficult to the regulation of long scope ballmilling energy,
And it is not suitable for the high efficiency thinning effect under plasmaassisted.And vibration type ball mill device can simultaneously pass through exciting block
Two aspects of amplitude and drum's speed of rotation realize the long range regulation of ballmilling energy jointly.
The A of CN 101239335 disclose a kind of plasma auxiliary high-energy planetary ball mill device, and it is in conventional planetary ball
On the basis of grinding machine, add in the ball grinder that luck of being expert at turns and be circumscribed with the electrode bar of plasma electrical source to improve planetary ball mill
The grinding efficiency of machine.But the rotation and revolution of ball grinder are realized because planetary ball mill is confidential, introduced electrode in ball grinder
Extremely unstable；Additionally, collision of the electrode bar in ball grinder to abrading-ball produces serious inhibition, to planetary knot
The ball milling advantage of structure produces inhibition.
The A of CN 102500451 and the U of CN 202398398 disclose a kind of auxiliary ball milling dielectric barrier discharge electrode rod, it
It is that tubulose politef block media layer is arranged in tubular conductive electrode layer, screw thread cooperation is obviated between two pipes；And
This electrode bar can be only applied on the ball grinder that two ends are all through holes.In reality processing assembling process, this cooperation is all the time
Residual air be cannot be avoided in discharge process to the infringement of electrode bar, the actual life of its electrode bar cannot be carried significantly
It is high.
US 6126097 and US 6334583 disclose a kind of planetary ball high-energy ball milling device and prepare nanometer powder
Method, describes a kind of structure of common planetary formula ball mill and its application in terms of nanometer powder preparation, but the invention is special
Profit is limited only to planetary ball mill field, and is not related to the application of additional plasma electric field.
The content of the invention
The present invention seeks to be to overcome the shortcoming that mechanical alloying energy consumption is big, efficiency is low, pollute weight, using dielectric impedance
Electric discharge (dielectric barrier discharge, abbreviation DBD) receives much concern uniqueness as the one kind for producing plasma
Discharge type, medium blocking discharge electrode rod is incorporated in the ball grinder of vibration at high speed, on the one hand requires electrode bar outer layer
Solid dielectric insulation can simultaneously bear the mechanical shock destruction of electrion and abrading-ball, on the other hand require the ball of vibration at high speed
Mill apparatus can make powder-processed uniform in effect, there is provided one kind is effectively improved material mechanical alloying efficiency, prepares hard conjunction
The new awkward silence at a meeting plasma discharge auxiliary high-energy ball milling powder body device of gold, lithium ion battery, hydrogen storing alloy powder powder material.Its base
On the basis of general milling technology, by introducing discharge plasma to handled another kind of effective energy of powder body input,
Promote pending powder body to produce under plasma collective effect in mechanical stress effect and extra electric field electric discharge, accelerate the thin of powder body
Change and promote alloying process, so as to greatly improve the working (machining) efficiency and action effect of ball mill.
The technical solution adopted in the present invention is that a kind of awkward silence at a meeting plasma discharge auxiliary high-energy ball milling powder body device is wrapped
Include vibration type high-energy ball milling main frame, additional awkward silence at a meeting plasma electrical source, electric discharge ball grinder, sparking electrode rod, controllable atmosphere system
System and six ingredients of cooling system,
The structure of described vibration type high-energy ball milling main frame is dual-drum vibration mill form；
Described additional awkward silence at a meeting plasma electrical source is become civil power using the high-voltage ac power of AC-DC-AC mapping modes
For high frequency electric, wherein using frequency modulation control mode, operating frequency range is adjustable in 1～20kHz, and power supply is defeated for the conversion of DC-AC
Go out voltage range between 1～30kV；
Described electric discharge ball grinder includes connector drum, front shroud, back shroud, the plasma being connected with electric discharge ball grinder
Power cathode earthing pole；The front shroud outer face of the electric discharge ball grinder is equipped with vacuum air valve, collectively constitutes with external gas circuit
Controllable atmosphere system；
The sparking electrode rod is cylindrical bar, by its internal ferrum or the conductive core and politef material of copper product
The insulating outer layer of material is collectively constituted；Conductive core is connected with plasma electrical source positive pole high-pressure stage, used as plasma discharge
One pole, insulating outer layer exists as the dielectric barrier of electric discharge；
Described controllable atmosphere system is arranged on the top of electric discharge ball grinder tank body air inlet/outlet, can in different air pressure and
In all kinds of atmosphere of argon, nitrogen, ammonia, hydrogen, oxygen, realize that plasma implements independent regulation and control to the ball milling effect for being processed powder body；
The awkward silence at a meeting plasma asistance high-energy ball milling device is defeated to electric discharge ball grinder using additional awkward silence at a meeting plasma electrical source
The different voltage and current for entering, then adjustment is controlled to the ball grinder internal atmosphere that discharges by controllable atmosphere system, so
Sparking electrode rod in relief electric discharge ball grinder produces intensity controlled corona or glow discharge phenomenon, so as to realize to electric discharge
Processed powder body in ball grinder implements plasma field high-energy ball milling, the process of Aided Machine alloying.
A kind of awkward silence at a meeting plasma discharge auxiliary high-energy ball milling powder body device of the present invention, including vibration type high-energy ball milling master
Machine, additional awkward silence at a meeting plasma electrical source, electric discharge ball grinder, sparking electrode rod, six groups of controllable atmosphere system and cooling system
Into part, the structure of described vibration type high-energy ball milling main frame is the form of eccentric vibration mill；
Described additional awkward silence at a meeting plasma electrical source is become civil power using the high-voltage ac power of AC-DC-AC mapping modes
For high frequency electric, wherein using frequency modulation control mode, operating frequency range is adjustable in 1～20kHz, and power supply is defeated for the conversion of DC-AC
Go out voltage range between 1～30kV；
Described electric discharge ball grinder includes connector drum, front shroud, back shroud, the plasma being connected with electric discharge ball grinder
Power cathode earthing pole；The front shroud outer face of the electric discharge ball grinder is equipped with vacuum air valve, collectively constitutes with external gas circuit
Controllable atmosphere system；
The sparking electrode rod is cylindrical bar, by its internal ferrum or the conductive core and politef material of copper product
The insulating outer layer of material is collectively constituted；Conductive core is connected with plasma electrical source positive pole high-pressure stage, used as plasma discharge
One pole, insulating outer layer exists as the dielectric barrier of electric discharge；
Described controllable atmosphere system is arranged on the top of electric discharge ball grinder tank body air inlet/outlet, can in different air pressure and
In all kinds of atmosphere of argon, nitrogen, ammonia, hydrogen, oxygen, realize that plasma implements independent regulation and control to the ball milling effect for being processed powder body；
The awkward silence at a meeting plasma asistance high-energy ball milling device is defeated to electric discharge ball grinder using additional awkward silence at a meeting plasma electrical source
The different voltage and current for entering, then adjustment is controlled to the ball grinder internal atmosphere that discharges by controllable atmosphere system, so
Sparking electrode rod in relief electric discharge ball grinder produces intensity controlled corona or glow discharge phenomenon, so as to realize to electric discharge
Processed powder body in ball grinder implements plasma field high-energy ball milling, the process of Aided Machine alloying.
Awkward silence at a meeting plasma discharge auxiliary high-energy ball milling powder body device of the present invention, is further characterized in that, and described
The conductive core of internal ferrum or copper product collectively constitutes the insulating outer layer of sparking electrode rod, is high-purity alpha-alumina ceramic material；
The insulating outer layer of the high-purity alpha-alumina ceramic material, is shaped using Direct precipitation mode or differential arc oxidation mode.
The insulating outer layer of the sparking electrode rod is cased with a metal sleeve with mesh.
The end flanges of cylinder two of the electric discharge ball grinder are connected respectively by sealing ring, bolt with front shroud, back shroud sealing
Connect, front shroud, the center of back shroud are respectively equipped with through hole and blind hole for fixing sparking electrode rod.
The embedded rustless steel sleeve of through hole of the front shroud of the electric discharge ball grinder and sealing rubber ring, the back shroud inner side
The blind hole in face is embedded with rustless steel sleeve gasket；Wherein front shroud includes polyfluortetraethylene plate and ceramic wafer, and back shroud includes polytetrafluoro
Vinyl plate and ceramic wafer.
Outside the sparking electrode rod inside ferrum or the conductive core fastening end of copper product and the insulation of polytetrafluoroethylmaterial material
Layer is coordinated using screw thread, and discharge end is coordinated using polished rod structure with insulating outer layer, between the cooperation of conductive core and insulating outer layer
Heat-resistant adhesive is filled with gap, and conductive core top is engaged with spherical structure with insulating outer layer medium；
Wherein, polished rod, spherical interface cooperation of the sparking electrode rod using conductive core and insulating outer layer, suppresses micro- putting
The unlimited enhancing of electricity so that dielectric barrier discharge will not change into spark discharge or arc discharge, such that it is able to avoid ball milling body
The scaling loss of system.
Described controllable atmosphere system is discharged and is input into by the ball grinder setup of entrances and exits ball valve that discharges, control gas,
Gas is by air relief valve and the pressure and flow of effusion meter control input；Powder body is filtered using filter, powder is reduced because of air-flow
The discharge of effect；It is connected with the ball valve of ball grinder as gas circuit using metal hose, reduces impact of the ball milling vibration to gas circuit.
Awkward silence at a meeting plasma discharge auxiliary high-energy ball milling powder body device of the present invention, by the use of dielectric barrier discharge as plasma
Body, by dielectric overlay on the electrode that discharge space is placed, when applying sufficiently high alternating voltage on sparking electrode, forms and is situated between
Gas or formation between matter barrier discharge breakdown electrode is very uniform, careless and sloppy, stable, and the glow discharge under low pressure seemingly, structure
Into a kind of unique discharge type by a large amount of trickle Fast pulsed discharge passages.Medium blocking discharge electrode rod is incorporated at a high speed
In the ball grinder of vibration, on the one hand require that the solid dielectric insulation of electrode bar outer layer can be while bear electrion and abrading-ball
Mechanical shock is destroyed, and on the other hand requiring the ball mill device of high speed vibration can make powder-processed uniform in effect, there is provided a kind of
It is effectively improved the novel high-energy ball mill device of material mechanical alloying efficiency and its prepares hard alloy, lithium ion battery, hydrogen storage
The application process of alloy powder material.Discharge space air pressure is set to 10 by it based on the basis of general milling technology2~
106Thermal nonequilibrium discharge condition under Pa or so air pressure, it is another to handled powder body input by introducing discharge plasma
Effective energy is planted, promotes pending powder body under mechanical stress effect and additional discharge plasma collective effect, accelerate powder body
Refinement and promote alloying process, so as to greatly improve the working (machining) efficiency and action effect of ball mill.
Because present media barrier discharge plasma has the advantage of following uniqueness, when consideration is drawn in high-energy ball milling
When entering plasma, dielectric barrier discharge plasma is obviously exactly one and preferably selects：
First, dielectric barrier discharge plasma can occur at ambient pressure, meet guarantor of the ball milling needs in certain pressure
The condition carried out under shield atmosphere；
Secondly, dielectric barrier discharge inhibits the unlimited enhancing of micro discharge due to dielectric layer so that dielectric barrier discharge is not
Spark discharge or arc discharge can be changed into, it is ensured that plasma is not the hot plasma strong to material damage power, so as to can
To avoid the scaling loss of ball milling system；
Third, dielectric barrier discharge can uniformly spread out in dielectric layer surface, the uniform accepting medium resistance of ball milling powder physical ability is made
The effect of gear discharge plasma；
Finally, under certain condition, dielectric barrier discharge can produce quasi- aura or glow discharge such that it is able to realize
Efficient ball milling in reaction atmosphere, promotes pending powder body under mechanical stress effect and additional discharge plasma collective effect,
Accelerate the refinement of powder body and promote alloying process, so as to greatly improve the working (machining) efficiency and action effect of ball mill.
Description of the drawings
Fig. 1 is awkward silence at a meeting plasma discharge auxiliary high-energy ball milling powder body device structural representation of the present invention；
Fig. 2 a and Fig. 2 b are vibration type ball mill bitubular mill main frame of the present invention and eccentric mill main machine structure schematic diagram；
Fig. 3 is awkward silence at a meeting plasma discharge auxiliary high-energy ball mill device electric discharge ball grinder structural representation of the present invention；
Fig. 4 is present invention electric discharge ball grinder and sparking electrode rod mounting structure schematic diagram；
Fig. 5 is sparking electrode rod structural representation of the present invention；
Fig. 6 is present invention electric discharge ball grinder and metal sleeve sparking electrode rod scheme of installation is housed；
Fig. 7 is the controllable atmosphere system of the present invention and electric discharge ball grinder mounting structure schematic diagram；
Fig. 8 a, Fig. 8 b are that the resting state in mechanical milling process of the present invention and ball milling state medium barrier discharge plasma shine
Piece；
Fig. 9 is the W-C-10Co powder (BPR=50 that difference Ball-milling Time of the invention is obtained:1) XRD spectrum；
Figure 10 is the W-C-10Co powder heat scan DSC curves of DBDP ball millings 3h of the present invention；
Figure 11 a, Figure 11 b are the scanning of the W-C-10Co-1.2VC mixed-powders after DBDP auxiliary high-energies ball milling 3h of the present invention
Electronic Speculum pattern picture.
In figure, 1. vibration type high-energy ball milling main frame, 2. additional awkward silence at a meeting plasma electrical source, 3. discharge ball grinder, 4. discharges
Electrode bar, 5. can control atmosphere system, 6. cooling system, 7. abrading-ball, 31. cylinders, 32. front shrouds, 33. back shrouds, 34. grades from
Daughter power ground pole, 35. plasma electrical source high-pressure stages, 36. tank body air inlet/outlets, 41. conductive cores, 42. insulating outer layers,
311. flanges, 312. sealing rings, 313. bolts, 321. through holes, 322. rustless steel sleeves, 323. sealing rubber rings, 324. vacuum
Air valve, 325. polyfluortetraethylene plates, 326. ceramic wafers, 331. blind holes, 332. rustless steel sleeve gaskets, 333. polyfluortetraethylene plates,
334. ceramic wafers, 411. fastening ends, 412. discharge ends, 413. spherical structures, 421. metal sleeves, 51. air relief valve, 52. flows
Meter, 56. unloaders, 541. ball valves, 542. ball valves, 551. filters, 552. filters, 571. metal hoses, 572. metals are soft
Pipe.
Specific embodiment
With reference to the accompanying drawings and detailed description the present invention is described in detail.
A kind of awkward silence at a meeting plasma discharge auxiliary high-energy ball milling powder body device, as shown in figure 1, including vibration type high-energy ball milling
Main frame 1, additional awkward silence at a meeting plasma electrical source 2, electric discharge ball grinder 3, sparking electrode rod 4, controllable atmosphere system 5 and cooling system
6 six ingredients.
As shown in Fig. 2 a embodiments, the structure of vibration type high-energy ball milling main frame 1 of the present invention is dual-drum vibration mill form, is vibrated
Formula high-energy ball milling main frame 1 may also be employed the form of eccentric vibration mill as shown in Figure 2 b.
The additional awkward silence at a meeting plasma electrical source 2 of the present invention adopts the high-voltage ac power of AC-DC-AC mapping modes, by city
Electricity is changed into high frequency electric, and the wherein conversion of DC-AC adopts frequency modulation control mode, and operating frequency range is adjustable in 1～20kHz, electricity
Source output voltage range is between 1～30kV.
As shown in figure 3, the electric discharge ball grinder 3 of the present invention, including connector drum 31, front shroud 32, back shroud 33, with electric discharge
The plasma electrical source minus earth pole 34 of the connection of ball grinder 3；The outer face of front shroud 32 of the electric discharge ball grinder 3 is equipped with vacuum
Air valve 324, with external gas circuit controllable atmosphere system 5 has been collectively constituted；31 liang of end flanges 311 of cylinder of electric discharge ball grinder 3 are led to
Cross sealing ring 312, bolt 313 to be tightly connected with front shroud 32, back shroud 33 respectively, front shroud 32, the centre bit of back shroud 33
Put the through hole 321 and blind hole 331 being respectively equipped with for fixing sparking electrode rod 4.
As shown in figure 4, the through hole 321 of the front shroud 32 of electric discharge ball grinder 3 embeds rustless steel sleeve 322 and sealing rubber ring
323, the blind hole 331 of the medial surface of the back shroud 33 is embedded with rustless steel sleeve gasket 332；Wherein front shroud 32 includes politef
Plate 325 and ceramic wafer 326, back shroud 33 includes polyfluortetraethylene plate 333 and ceramic wafer 334.
As shown in figure 5, the sparking electrode rod 4 of the present invention is cylindrical bar, by its internal ferrum or the conduction electricity of copper product
The insulating outer layer 42 of core 41 and polytetrafluoroethylmaterial material is collectively constituted；Internal conductive core 41 is just high with plasma electrical source
Pressure pole 35 is connected, and used as a pole of plasma discharge, insulating outer layer 42 exists as the dielectric barrier of electric discharge；Electric discharge electricity
The fastening end 411 of conductive core 41 and the insulating outer layer 42 of polytetrafluoroethylmaterial material of the inside ferrum of pole rod 4 or copper product uses screw thread
Coordinate, discharge end 412 is coordinated using polished rod structure with insulating outer layer 42, in conductive core 41 and the fit clearance of insulating outer layer 42
In be filled with heat-resistant adhesive, and the top of conductive core 41 is engaged with spherical structure 413 with the medium of insulating outer layer 42.
Wherein, polished rod, spherical interface cooperation of the sparking electrode rod 4 using conductive core 41 and insulating outer layer 42, suppression
The unlimited enhancing of micro discharge processed so that dielectric barrier discharge will not change into spark discharge or arc discharge, such that it is able to avoid
The scaling loss of ball milling system.
The present invention collectively constitutes the insulating outer layer 42 of sparking electrode rod 4 with the conductive core 41 of internal ferrum or copper product, is
High-purity alpha-alumina ceramic material；The high-purity alpha-alumina ceramic material of insulating outer layer 42, using Direct precipitation mode or the differential of the arc
Mode of oxidizing shapes；Using the sparking electrode rod 4 of the insulating outer layer 42 of high-purity alpha-alumina ceramic material, as shown in fig. 6, putting
The insulating outer layer 42 of electric electrode bar 4 is cased with a metal sleeve 421 with mesh.
As shown in fig. 7, the controllable atmosphere system 5 of the present invention is arranged on the upper of the electric discharge tank body air inlet/outlet 36 of ball grinder 3
Side, can realize plasma to being processed the ball milling effect of powder body in different air pressure and all kinds of atmosphere of argon, nitrogen, ammonia, hydrogen, oxygen
Fruit applies independent regulation and control；Controllable atmosphere system 5 is by the setup of entrances and exits ball valve 541,542 of ball grinder 3 that discharges, control gas row
Go out and be input into, gas is by air relief valve 51 and the pressure and flow of the control input of effusion meter 52；Filtered using filter 551,552
Powder body, reduces powder because of the discharge of airflow function；Using metal hose 571,572 as gas circuit and ball grinder ball valve 541,
542 connections, reduce impact of the ball milling vibration to gas circuit.
Awkward silence at a meeting plasma discharge auxiliary high-energy ball mill device of the present invention is using additional awkward silence at a meeting plasma electrical source 2 to electric discharge
The different voltage and current of the input of ball grinder 3, then by 5 pairs of electric discharge internal atmosphere (gases of ball grinder 3 of controllable atmosphere system
Type and air pressure) be controlled adjustment, the sparking electrode rod 4 then allowed in electric discharge ball grinder 3 produce intensity controlled corona or
Person's glow discharge phenomenon, so as to realize that the processed powder body to discharging in ball grinder implements plasma field high-energy ball milling, auxiliary
The process of mechanical alloying.
Fig. 8 a, Fig. 8 b are the dielectric barrier discharge plasma photos in mechanical milling process of the present invention.
Apparatus of the present invention are operated by following steps：
(1) load abrading-ball and pending powder in ball grinder, and medium blocking discharge electrode rod is arranged on into ball milling
The center of tank, makes electrode bar and abrading-ball and pending powder contact, is then sealed and is consolidated using the end cap of ball grinder
It is fixed；
(2) negative pressure is evacuated to the ball grinder of good seal by vacuum valve, needed for being then passed through by vacuum valve again
Discharge gas medium, such as：Argon, nitrogen, argon, methane or oxygen etc..Wherein, be passed through gas pressure can whole-process control 0.01
～1MPa scopes；
(3) ball milling tank and electrode bar conductive core are connected respectively with the positive and negative two-stage of plasma electrical source, wherein, electricity
Pole rod conductive core connects the positive pole of plasma electrical source, and ball milling tank connects the negative pole of plasma electrical source；
(4) power supply of plasma is connected, the electric discharge of plasma electrical source is adjusted according to discharge gas medium and its pressure
Parameter voltages are 3～30KV, and frequency is 5～40KHz, forms electric field, and starts ball mill.With ball mill frequency of vibration or
The change of rotating speed, so as to change the relative position of abrading-ball in electrode bar and ball grinder, carry out corona discharge or glow discharge etc. from
Daughter auxiliary high-energy ball milling.Wherein, corona plasma is mainly used and adjuvant powders refinement, and glow discharge plasma master
To use and Aided Machine alloying.
The present invention relative to prior art, in electric discharge ball grinder, medium blocking discharge electrode rod and atmosphere control system etc.
The design of aspect, with unique structure and advantage.
The electric discharge ball grinder of the present invention includes cylinder, front shroud (bilayer), back shroud (bilayer), and ball grinder connects plasma
Both the negative pole of power supply, sleeve and abrading-ball are turned on, and can be considered collectively as a pole of plasma discharge；Wherein front shroud and
Back shroud includes respectively polytetrafluoroethylene floor and ceramic layer；Ball grinder cylinder is made up of stainless steel casing liner hard alloy layer,
For electrically conductive body, described forward and backward cover plate is total to using insulant such as double-deck politef, lucite and ceramic wafers
With making, when such as politef and ceramic wafer are combined, the former prevents abrading-ball from smashing as internal layer, and the latter strengthens as outer layer to be covered
Plate intensity；The flange at cylinder two ends is tightly connected respectively by sealing ring, the bolt of more than 8 with front shroud, back shroud, protecgulum
Plate, the center of back shroud are respectively provided with through hole and blind hole for fixed electrode rod；
The embedded rustless steel internal ring of the through hole of front shroud of the present invention and sealing rubber ring, the blind hole of back shroud medial surface is also embedded
There is metal sleeve, the insert structure is prevented effectively from infringement of the electrode bar point discharge to forward and backward cover plate；The upper setting of front shroud
There is vacuum air valve made by stainless steel material, be easy to be controlled the vacuum in ball grinder；
The core apparatus of awkward silence at a meeting plasma discharge auxiliary high-energy ball milling powder body device of the present invention are dielectric barrier discharge electricity
Pole rod, by the discharge voltage and power that control plasma, and then the discharge effect of coordination electrode rod.But, electrode bar
Block media layer is in discharge process, while by destroying that the mechanical collision and electric field of abrading-ball discharge, work bad border is extremely disliked
It is bad, various forms of destructions are generally occurred within use：(1) dielectric impedance layer surface is susceptible to pin hole or duck eye shape hits
Wear；(2) dielectric barrier with the cooperation of ball grinder two ends end cap at easily occur puncturing cavity；(3) block media layer is because of office
Overheated cracking and the large area of producing in portion burns out.These destructions have had a strong impact on the application that discharge plasma aids in ball grinding technique.
Solve puncturing and destroy to dielectric barrier in electrode layer work, it is necessary to design and produce electrode bar rational in infrastructure, keep away
Exempt to discharge and there is the uneven of discharge electric field and thermal field in block media layer in mechanical milling process.Wherein, dielectric barrier is most weak
Link is the position at the top of the shaft shoulder and axle.This is mainly localized high intensity electric field causes block media layer to puncture, and this
Plant localized high intensity electric field and be attributed to again at screw thread cooperation and cooperation and there is breath residual.
The medium blocking discharge electrode rod of the present invention adopts cylindrical bar, its by core conductive material ferrum, copper etc. and
Insulant politef or high-purity alpha-alumina ceramics of outer layer etc. are collectively constituted.The inner conductive battery core and plasma
Body positive source is connected, and used as a pole of plasma discharge, and exterior insulation material is deposited as the dielectric barrier of electric discharge
.The present invention specifically includes following three kinds of structures in terms of medium blocking discharge electrode rod service life is improved：
(1) electrode bar described in is collectively constituted by internal ferrum or copper core and outside politef, wherein, fastening end with it is outer
Layer teflon insulation coordinates with the use of screw thread, and discharge end adopts polished rod structure (abandoning helicitic texture), and in electrode
It is sufficient filling with heat-resistant adhesive and avoids air from existing in layer and the fit clearance of politef, while top of electrodes adopts spherical structure
It is engaged with outer layer insulation medium, it is to avoid the electric field of the localized high intensity value that point discharge is caused occurs；
(2) electrode bar described in is made up of internal ferrum or copper core and outside politef, wherein, by politef
(dielectric barrier) is deposited directly to electrode layer, and formation is fitted close completely, there is no the dielectric insulation layer in any gap；
(3) electrode bar described in is collectively constituted by internal ferrum or copper core and outside high-purity alpha-alumina ceramics, the two employing
The mode such as Direct precipitation or differential arc oxidation is made, wherein, to prevent cracking destruction of the ceramics in abrading-ball collision process, in electrode
Add a metal sleeve with mesh between rod and ball grinder, as shown in fig. 6, abrading-ball runs between sleeve and ball grinder.
Add a metal sleeve with mesh between electrode bar and ball grinder, between sleeve and ball grinder, ball grinder connects abrading-ball
The negative pole of plasma electrical source, ball grinder, abrading-ball and sleeve three conducting, can be considered collectively as one of plasma discharge
Pole.Electrode bar in the middle of the positive pole female connector cylinder of plasma electrical source, electrode bar is still by ferrum, copper core and high-purity alpha-alumina ceramic layer
Constitute.So plasma discharge will be carried out between sleeve and electrode bar, and the powder body of ball milling can pass through the mesh on sleeve
Discharge plasma process is obtained in sleeve.The design parameter of metal sleeve 421 is generally：Sleeve thickness 3mm, external diameter
40mm, hole diameter 3mm, less than minimum ball radius.Therefore, powder body can be freed in and out during ball milling and abrading-ball cannot
Into in sleeve, mechanical impact effect would not be produced to electrode bar.
From the point of view of the experimental result of above-mentioned three kinds improved sparking electrode rods, 1000rpm/min is reached in motor speed, in tank
When abrading-ball weight reaches 7.5kg, the electrode bar life-span prepared by latter two method can reach 30～50h or so, and this is that other are common
Electrode bar is incomparable.
Additionally, the present invention is relative to prior art, the design in terms of controllable atmosphere system, with unique structure and
Advantage.The system is achieved through the following technical solutions：
(1) gas is by air relief valve 51 and the pressure and flow of the control input of effusion meter 52.
(2) discharge the setup of entrances and exits ball valve 541 and 542 of ball grinder 3, and control gas is discharged and input.
(3) it is used to filter powder body using filter 551 and 552, powder is reduced because of the discharge of the effect of air-flow, due to filtering
Device crosses rate precision and is not up to nanoscale, therefore using double filtration mode.
(4) unloader 56, can be in the case of ventilation by the height of adjusting nut by adjusting nut above
Spring pressure in regulating valve.When gas pressure exceed spring pressure when, spring by jack-up, outside aerofluxuss (off-load)；Work as gas
When pressure is less than spring pressure, this valve closure.Realize controlling the purpose of electric discharge ball grinder internal pressure with this.
(5) part installed with ball grinder adopts metal hose 571 and 572, it is therefore an objective to reduce vibrations to other portions of gas circuit
Divide the impact of (the particularly spring section of unloader).Valve member beyond hose segment all should be fixed, and reduce the impact of vibrations.
(6) require that input air pressure is slightly larger than specified control air pressure when using, to ensure the flowing of gas in electric discharge ball grinder
It is pure with atmosphere.So as to realize the impact of the plasma such as species and air-flow of gas.
The controllable atmosphere system realizes the impact of different air pressure and atmosphere plasma strength of discharge and thickness, from
And for the different atmosphere parameter that provides of plasmaassisted ball milling of different powder body.
The present invention compared with prior art, obtains following advantage and beneficial effect in terms of Mechanical Alloying：
(1) powder heating is fast, and deformation is big, short the time required to refinement.Under same process parameter, carried out using this method etc.
The product powder diameter of gas ions auxiliary ball milling is attained by nanoscale, and narrow diameter distribution, and the product powder of general milling
Particle diameter is in micron order, particle diameter distribution width.
(2) mechanical alloying process is promoted, plasma auxiliary high-energy ball milling is combined on the basis of conventional mechanical energy
The energy of plasma, this Combined Processing to powder while efficiently refinement powder body, necessarily increases the surface energy of powder body
And interface energy, strengthen the reactivity of powder body, and the pure heat effect of plasma is also to promotion diffusion and alloying reaction
Favourable.
(3) the inventive method is utilized, when discharge gas medium is organic gas, it is right to realize simultaneously in refinement powder body
The in-situ-surface modifying of powder body.
(4) technique of the invention is easily achieved, high in machining efficiency, can effectively shorten needed for powder refining and mechanical alloying
Time, energy saving can make high-energy ball-milling process realize that real material is prepared and produced in enormous quantities, have a extensive future.
Plasmaassisted ball milling can fining metal powder body more more efficient than general milling, especially plasmaassisted ball milling is
The effective way of high-efficiency production of nano metal-powder.Result of the test shows：Room temperature general milling iron powder 60h, iron powder refine to most
Little value, the dimension limit is more than 1 μm；- 20 DEG C of low temperature ball milling 30h, iron powder is refined to less than 1 μm；24kV plasmaassisteds
Grinding efficiency highest, is only obtained the nanometer iron powder of mean diameter 103.9nm with 10h.For aluminium powder and tungsten powder, as a result and ferrum
Similar, the general milling 15h of powder, most of aluminium powder is between 10-50 μm, and plasmaassisted ball milling 15h, obtain average grain
Footpath is the aluminium powder of 128.7nm；General milling 3h, between 0.5-3 μm, using plasma auxiliary ball milling 3h is obtained Tungsten Powder Size
To the tungsten powder of mean diameter 101.9nm.During plasmaassisted ball milling simple metal, plasma " thermal explosion " effect is affected
Be metal material thermal property.The fusing point and boiling point of metal is higher, and heat conductivity, specific heat, heat of fusion, heat of gasification are bigger,
It is more difficult to induce " Explosion ", this also directly affects the content of below 10nm powder body in plasmaassisted ball milling metal dust.
Fusing point such as tungsten is high, and below the 10nm tungsten nanoparticle contents that plasma generation " thermal explosion " effect is obtained only have 10.5%.
Although aluminum thermal conductivity ratio ferrum is big, because its fusing point is too low, plasma produces below the 10nm aluminum that " thermal explosion " effect is obtained
Nanoparticle content is 27.3%, below 10nm nanoparticle contents (25.2%) slightly larger than in iron powder.
Plasmaassisted ball milling can promote mechano-chemical reation than general milling more efficiently activating reaction powder body,
Such as plasmaassisted ball milling W powder+graphite powder only 3h, just can effective activation powder body, follow-up 1100 DEG C of insulations 1h processes and just makes W
All carbonization synthesizes particle size in 100nm to powder, and, in the nanometer WC powder body of 50nm or so, carburizing temperature is than normal for average grain size
Rule carburizing temperature have dropped 500 DEG C.The activation mechanism of plasmaassisted ball milling, is on the one hand that the dielectric impedance of plasma is put
Electrical effect and shock effect cause powder body itself interior energy to increase, and more imitate mainly due to the dielectric barrier discharge in mechanical milling process
Should so that define the fine composite construction of nanometer scale between reaction powder body.This fine composite construction on the one hand can be significantly
The temperature needed for following reaction is reduced, reaction on the other hand can be promoted to carry out perfect so that product is pure.
Discharge plasma aids in ball milling as a kind of new technique, it have substantially reduce reaction activity, crystal grain thinning,
Powder activity is greatly improved and improves the combination at interface between particle distribution uniformity and reinforcement and matrix, promote solid ionic
Diffusion, induces low-temp reaction, is a kind of energy-conservation, efficient material preparation technology so as to improve the performance of each side of material.
It is by providing a kind of effective energy input that can be increased to processing powder, the refinement and promotion mechanical alloying of powder quick
Process, greatly improves the working (machining) efficiency of ball mill, and it is one and is related to the association areas such as machinery, material and electric power, with wider
Wide research space.At present, the present invention has wide commercial Application in directions such as hard alloy, lithium ion battery, hydrogen bearing alloys
Prospect.
Awkward silence at a meeting plasma discharge auxiliary high-energy ball milling powder body device of the present invention, sparking electrode rod uses cylindrical bar,
It is by conductive material ferrum, the copper etc. of core and the common group such as insulant politef or high-purity alpha-alumina ceramics of outer layer
Into, inner conductive battery core is connected with plasma electrical source positive pole high-pressure stage, as a pole of plasma discharge, and it is outside exhausted
Edge material exists as the dielectric barrier of electric discharge.And the life-span of electrode bar and performance directly determine the work efficiency of ball mill,
Therefore, we list three sections of electrode bars designed in patent of the present invention and ordinary electrode rod (iron core is directly squeezed into be had
In the politef with blind hole of interference fit), it is operated life span comparison.The working condition for adopting for：15KV's puts
Piezoelectric voltage, the discharge current of 1.5A, exciting block adopts double-amplitude 8mm, ratio of grinding media to material to adopt 50:1, abrading-ball is using hard alloy or not
Rust Steel material.As shown in table 1.
Embodiment 1：
Step 1, electrode bar is collectively constituted using inner copper core and outside politef, wherein, fastening end and outer strata
Tetrafluoroethene insulation with the use of screw thread coordinate, discharge end adopt polished rod structure (abandoning helicitic texture), and electrode layer with
Heat-resistant adhesive is sufficient filling with the fit clearance of politef avoids air from existing, at the same top of electrodes using spherical structure with it is outer
Layer dielectric is engaged.Electrode bar is arranged in the ball grinder of 4L, and loads abrading-ball and pending powder in ball grinder
End, and by the center of medium blocking discharge electrode baseball grinding jar, electrode bar and abrading-ball and pending powder contact are made, then
Sealed and fixed using the end cap of ball grinder.Wherein, a diameter of 25mm of electrode bar, abrading-ball adopts Hardmetal materials, weight
7.5 kilograms, ratio of grinding media to material is 50:1；
Step 2, negative pressure is evacuated to the ball grinder of good seal by vacuum valve, needed for being then passed through by vacuum valve again
Electric discharge argon.Wherein, gas pressure is passed through to 0.1MPa；
Step 3, ball milling tank and electrode bar conductive core are connected respectively with the positive and negative two-stage of plasma electrical source, its
In, electrode bar conductive core connects the positive pole of plasma electrical source, and ball milling tank connects the negative pole of plasma electrical source；And adopt
15KV discharge voltage, the discharge current of 1.5A, exciting block adopt double-amplitude 8mm, the rotating speed of 1200rpm, start ball mill.
As a result show, the service life of electrode bar can reach 20 hours or so.
Embodiment 2：
Step 1, step 2, with example 1；
Step 3, with example 1, but drum's speed of rotation adopts 960rpm.
As a result show, the service life of electrode bar can reach 30 hours or so.
Embodiment 3：
Step 1, with example 1, but ball milling volume adopts 0.15L, electrode bar diameter to adopt 20mm, and abrading-ball is stainless steel
Material；
Step 2, with example 1；
Step 3, with example 1, but discharge current adopts 1.0A, drum's speed of rotation to adopt 960rpm.
As a result show, the service life of electrode bar can reach 35 hours or so.
Embodiment 4：
Step 1, electrode bar is collectively constituted using inner copper core and outside politef, wherein, politef (is situated between
Matter barrier layer) it is deposited directly on electrode layer.By electrode bar be arranged on 4L ball grinder in, and in ball grinder load abrading-ball and
Pending powder, and by the center of medium blocking discharge electrode baseball grinding jar, electrode bar is made with abrading-ball and pending powder
End contact, is then sealed and is fixed using the end cap of ball grinder.Wherein, a diameter of 25mm of electrode bar, abrading-ball adopts hard
Alloy material, weighs 7.5 kilograms, and ratio of grinding media to material is 50:1；
Step 2, negative pressure is evacuated to the ball grinder of good seal by vacuum valve, needed for being then passed through by vacuum valve again
Electric discharge argon.Wherein, gas pressure is passed through to 0.1MPa；
Step 3, ball milling tank and electrode bar conductive core are connected respectively with the positive and negative two-stage of plasma electrical source, its
In, electrode bar conductive core connects the positive pole of plasma electrical source, and ball milling tank connects the negative pole of plasma electrical source；And adopt
15KV discharge voltage, the discharge current of 1.5A, exciting block adopt double-amplitude 8mm, the rotating speed of 1200rpm, start ball mill.
As a result show, the service life of electrode bar can reach 15 hours or so.
Embodiment 5：
Step 1, step 2, with example 4；
Step 3, with example 4, but drum's speed of rotation adopts 960rpm.
As a result show, the service life of electrode bar can reach 25 hours or so.
Embodiment 6：
Step 1, with example 4, but ball milling volume adopts 0.15L, electrode bar diameter to adopt 20mm, and abrading-ball is stainless steel
Material；
Step 2, with example 4；
Step 3, with example 4, but discharge current adopts 1.0A, drum's speed of rotation to adopt 960rpm.
As a result show, the service life of electrode bar can reach 30 hours or so.
Embodiment 7：
Step 1, electrode bar is collectively constituted using inner copper core and external ceramic, one is added between electrode bar and ball grinder
The individual metal sleeve with mesh, abrading-ball runs between sleeve and ball grinder.Electrode bar is arranged in the ball grinder of 4L, and
Load abrading-ball and pending powder in ball grinder, and by the center of medium blocking discharge electrode baseball grinding jar, make electrode
Rod and abrading-ball and pending powder contact, are then sealed and are fixed using the end cap of ball grinder.Wherein, electrode bar is a diameter of
25mm, abrading-ball adopts Hardmetal materials, weighs 7.5 kilograms, and ratio of grinding media to material is 50:1；
Step 2, negative pressure is evacuated to the ball grinder of good seal by vacuum valve, needed for being then passed through by vacuum valve again
Electric discharge argon.Wherein, gas pressure is passed through to 0.1MPa；
Step 3, ball milling tank and electrode bar conductive core are connected respectively with the positive and negative two-stage of plasma electrical source, its
In, electrode bar conductive core connects the positive pole of plasma electrical source, and ball milling tank connects the negative pole of plasma electrical source；And adopt
15KV discharge voltage, the discharge current of 1.5A, exciting block adopt double-amplitude 8mm, the rotating speed of 1200rpm, start ball mill.
As a result show, the service life of electrode bar can reach 25 hours or so.
Embodiment 8：
Step 1, step 2, with example 7；
Step 3, with example 7, but drum's speed of rotation adopts 960rpm.
As a result show, the service life of electrode bar can reach 36 hours or so.
Embodiment 9：
Step 1, with example 7, but ball milling volume adopts 0.15L, electrode bar diameter to adopt 20mm, and abrading-ball is stainless steel
Material；
Step 2, with example 7；
Step 3, with example 7, but discharge current adopts 1.0A, drum's speed of rotation to adopt 960rpm.
As a result show, the service life of electrode bar can reach 40 hours or so.
Embodiment of the present invention employs high rotating speed (960～1200rpm), high abrading-ball packing ratio and (accounts for ball grinder
The 65 of volume～75%) and hard alloy abrading-ball, increase to the oscillation intensity and impulsive force of electrode bar to test electrode bar
Service life.From the point of view of the life-span of never isostructural electrode bar, in the present invention designed three kinds of electrode bars substantially close to or reach
To the continuous service life of 30 hours, significantly larger than the electrode bar life-span of common process.For using the slow-speed of revolution, low ratio of grinding media to material
Ball milling parameter, the life-span of electrode bar will also greatly improve.This greatly improves the operational efficiency of ball mill and increased industry should
With the probability promoted.
Table 1：The service life contrast of different structure designs electrode bar
The embodiment of hard alloy is prepared using plasmaassisted ball milling of the present invention
In order to further verify the feasibility and odds for effectiveness of apparatus of the present invention, we employ high-melting-point, high rigidity
WC-Co hard alloy material is used as ball milling object of study.Existing high-energy ball milling method prepares the research of nanosized hardmetal powder
Mainly include：Powder processed, three processes of carbonization and molding, wherein, powder processed and carbonisation are prepared by whole WC-Co series hard metals
Important foundation link.Its concrete operation step is as follows：(1) ultra-fine W, C mixture is prepared first with high-energy ball milling method；
(2) W, C mixture to preparing is carbonized, and generates ultrafine tungsten carbide (WC)；(3) Co is added on the basis of the WC for generating
High-energy ball milling is carried out again, makes WC and Co mix homogeneously.But this method remains a need for longer Ball-milling Time, and answering of preparing
Close powder decarburization serious.Using the discharge plasma auxiliary ball grinding method of the present invention, coordinate compacting sintering, can be with carburizing sintering
Integrated synthetic method prepares the WC-Co hard alloy with high-strength tenacity, overcomes that CEMENTED CARBIDE PRODUCTION process is loaded down with trivial details, energy consumption is big
Defect, and effectively increase the degree of purity of product.
It is achieved through the following technical solutions using dielectric barrier discharge plasma auxiliary high-energy ball milling：
(1) abrading-ball and W, C, Co grain growth inhibitor of certain proportioning and mixing for extra benefit carbon are loaded in ball grinder
The raw materials such as powder are closed, and is mixed into appropriate ball milling controlling agent (dehydrated alcohol etc.)；
(2) by electrode bar is through ball milling can end and is implanted in ball grinder, ball milling can end is buckled, then end cap and electricity
Pole rod is connected respectively with the two poles of the earth of plasma electrical source, wherein, electrode bar connects the positive pole high-pressure stage of plasma electrical source, front shroud
Connect the negative pole earth polar of plasma electrical source；
(3) negative pressure is taken out extremely to closed ball grinder by vacuum valveOr taking out negative pressure extremelyAgain discharge gas medium is passed through by vacuum valve later, the pressure in the ball grinder is
(4) power supply of plasma is connected, discharge parameter is adjusted according to discharge gas medium and its pressure, make plasma
The voltage of power supply isFrequency isCorona discharge is realized, and starts ball mill work, ball grinder
Collide motion with abrading-ball, so as to change the relative position of abrading-ball in electrode bar and ball grinder, carry out different types of corona
Discharge plasma high-energy ball milling, obtains W-C-Co base alloy powders；
(5) it is the W-C-Co base alloy powders is compressing, obtain green compact；
(6) green compact are sintered in thermal source environment and prepares W-C-Co hard alloys.
For the present invention, step (1) described W, C, Co, VC or V is better achieved2O5Each raw material is according to WC-XCo-YVC or WC-
XCo-Y V2O5Carry out proportioning (addition of grain growth inhibitor oxide form according to its carbonization after form corresponding carbide institute
The amount for needing is added), wherein, the span of X is 3<X<20, Y span is 0.09<Y<2.4, described X, Y is equal
It is weight percentage.
The amount of C is in addition to the theoretical carbon amounts required for W carbonizations in mixed-powder, also mends carbon amounts including extra, itself and C
The mass ratio of raw material is 7.5%～15%.
The compressing mode is single way stempressing, and unit pressure is
The thermal source environment is vacuum/low-pressure sintering furnace, and the temperature of thermal source environment is
The present invention has the advantage that compared with the conventional art for preparing hard alloy：
(1) deformation of W, C, Co raw material is big, the refinement time is short, the lamella words time is short, compared with other ball grinding methods, the method
Powder refining can faster be made to nanoscale；
(2) the method is conducive to the carrying out of carburizing reagent, after processing for W, C, Co raw material, drastically increases powder
Surface energy, interface energy, reactivity of body etc., and the heat effect of plasma is for the diffusion between W, C, Co and solid-state reaction
Favorably, the sinter molding of follow-up hard alloy is conducive to；
(3) directly W, C, Co alloy powder is pressed into into green compact, with the technology of carburizing sintering integration traditional handicraft is replaced
It is middle that first W powder is carbonized, then WC, Co mixed-powder is made into green sintering forming technique.The present invention only exist once from room temperature to
The heating process of high temperature, and the sintering of the carbonization of W powder and mixed-powder each experience is once from room temperature to high temperature in traditional handicraft
Heating process, thus energy consumption can be substantially reduced.
(4) present invention during dielectric barrier discharge plasma ball milling W, C, Co by adding grain growth inhibitor
(VC or V2O5), with traditional handicraft first by W carbonizations, again by grain growth inhibitor with WC, Co-compared with ball milling, it is of the invention
The distributing homogeneity of grain growth inhibitor can be increased, and the suppression grown up to WC grain can be just played in the forming process of WC
Make and use, the effect for suppressing WC grain to grow up is good；Meanwhile, the step of reduce high temperature cabonization, largely reduce cost.
We when impact of the different Ball-milling Times to crystallite dimension is investigated, as shown in figure 9, can from XRD spectrum
Go out, the diffraction maximum of DBDP ball millings to mixed powder during 6h is still mainly W, generates without WC, illustrates DBDP ball millings 6h also not
It is carbonized as W is made.With the increase of Ball-milling Time, there is widthization in the diffraction maximum of W, especially apparent in the widthization of 0.5h.Use Voigt
Function method calculates (211) face of W, the crystallite dimension change of ball milling 0.5h it is obvious that reach 43nm or so, the crystalline substance of ball milling 1h to 6h
Particle size decreases, but changes unobvious.Illustrate that DBDP ball millings can rapidly refine W crystallite dimensions to a maintenance level, its
Efficiency is much higher than common high-energy ball milling.
The DSC curve of the W-C-10Co mixed-powders of observation DBDP ball milling 3h, as shown in Figure 10, we can be found that
650 DEG C or so of endothermic peak is that carbon reduces a small amount of WO generated because of oxidation in ball-milled powder3The oxygen adsorbed with powder surface,
Generate CO or CO2Effusion.And DSC curve also has an exothermic peak in the range of 831～875 DEG C, the carbonization of tungsten may be correspond to
Reaction.In order to study the phase in version process at the reaction peak, select to be heated again in Thermal Synthetic Analysis instrument at 700 DEG C and 900 DEG C
Close powder.As a result find, when the XRD spectrum of the mixed-powder not heated and the mixed-powder of DBDP ball milling 3h are heated to 700 DEG C
XRD spectrums be all mainly W peaks, but be heated to when 700 DEG C α-Co peaks and occur.This is because with the rising of temperature, W and Co crystal grain is long
Big the reason for.It is also shown by Figure 10, mixed-powder is heated to have WC to generate when 900 DEG C, but while there is decarburization phase W2C、Co6W6C
And simple substance W.The process can be represented with formulas below：
W+C→WC (1)
2W+C→W2C (2)
6W+6Co+C→Co6W6C (3)
Continue to raise heating-up temperature, 1100 DEG C are heated in DSC and are not incubated, the XRD spectrum of the composite powder for obtaining
Solution, mesophase W2C is completely transformed into WC, decarburization phase Co6W6C becomes apparent from, and still suffers from a small amount of W.Corresponding reaction equation can be with table
It is shown as
W2C+C→2WC (4)
WC+5W+6Co→Co6W6C (5)
There is no mesophase Co during decarburization phase in version from unlike other results of study3W3The appearance of C, reason can
Can be DBDP ball millings powder activity it is higher, ball milling and taking is more easy to adsorb the oxygen in air during powder, and the flowing of DSC equipment
Atmosphere can take away the CO formed in heating process2, so that lacking, carbon is more serious, powder direct reaction is formed more towards decarburization
Co6W6C phases, without generating phosphorus content Co is compared6W6C high Co3W3C phases.
In addition, above-mentioned process also demonstrates that carbon content is wayward when completing carburizing reagent in the atmosphere that flows, and is unfavorable for
Form the WC without decarburization phase, it should avoid preparing WC-Co composite powder end using flowing atmosphere.Therefore, using identical ball milling powder
End is heated to 1000 DEG C in low-pressure sintering furnace and is incubated 1h.As a result prove to be obtained without decarburization phase under such process conditions
WC-10Co composite powders.Its reason is low pressure sintering stove heat to be carried out in closed atmosphere, will not be because of CO2Loss and
Cause scarce carbon.Meanwhile, with the growth of temperature retention time, uneven carbon further spreads, with Co6W6C reacts at high temperature generation
WC and Co, its reaction equation can be expressed as
Co6W6C+5C→6WC+6Co (6)
Additionally, based on previous work, we also add grain growth inhibitor in WC-Co hard alloy preparation with
Refinement WC grain, prepares high-performance carbide.With the addition of the W-C-Co powder body of VC as object of study, DBDP auxiliary high-energies
Ball milling not exclusively refines simple substance powder body to the action effect that with the addition of the W-C-Co mixed powders of grain growth inhibitor, also makes
Graphite it is fine and closely woven be coated on W particle surfaces, powder granule is superimposed in sheet, as shown in fig. 11a.DBDP auxiliary high-energy ball millings pair
The refining efficiency of W powder presents rule first quick and back slow, and the addition of VC can promote refinements of the W in mechanical milling process.Little through 3
When ball milling after, its W crystallite dimension is about 23nm.Different sintering process are taken to prepare WC-10Co-0.6VC hard alloys,
Find after test properties：, due to applying external pressure in holding stage, its liquid phase Co flows sample prepared by low pressure sintering
Fully, not only preferably it is filled with the hole caused because gas is escaped, moreover it is possible to be uniformly distributed between hard phase WC, play
Good cementation, as shown in figure 11b.Sample prepared by 4MPa pressure is loaded at 1340 DEG C, its consistency reaches
99%, Rockwell hardness reaches HRA91.8, and cross-breaking strength TRS reaches 3348MPa.The fracture apperance for analyzing the sample can be with
It was found that, the fracture mode of hard alloy is grain boundary fracture.
Above-mentioned embodiment is several examples of the present invention, is not intended to limit enforcement and the interest field of the present invention,
Equivalence changes and modification that all contents according to described in the present patent application scope of patent protection are made, all should be included in Shen of the present invention
Please be in the scope of the claims.
Claims (8)
1. it is a kind of awkward silence at a meeting plasma discharge auxiliary high-energy ball milling powder body device, including vibration type high-energy ball milling main frame (1), additional
Awkward silence at a meeting plasma electrical source (2), electric discharge ball grinder (3), sparking electrode rod (4), controllable atmosphere system (5) and cooling system
(6) six ingredients, it is characterised in that
The structure of described vibration type high-energy ball milling main frame (1) is dual-drum vibration mill form；
Described additional awkward silence at a meeting plasma electrical source (2) is become civil power using the high-voltage ac power of AC-DC-AC mapping modes
For high frequency electric, wherein using frequency modulation control mode, operating frequency range is adjustable in 1～20kHz, and power supply is defeated for the conversion of DC-AC
Go out voltage range between 1～30kV；
Described electric discharge ball grinder (3) includes connector drum (31), front shroud (32), back shroud (33), with electric discharge ball grinder (3)
The plasma electrical source minus earth pole (34) of connection；Front shroud (32) outer face of electric discharge ball grinder (3) is equipped with vacuum
Air valve (324), with external gas circuit controllable atmosphere system (5) has been collectively constituted；
The sparking electrode rod (4) is cylindrical bar, by its internal ferrum or the conductive core (41) and polytetrafluoroethyl-ne of copper product
The insulating outer layer (42) of alkene material is collectively constituted；Conductive core (41) is connected with plasma electrical source positive pole high-pressure stage (35), makees
For a pole of plasma discharge, dielectric barrier presence of the insulating outer layer (42) as electric discharge；
Described controllable atmosphere system (5), can be in difference installed in the top of electric discharge ball grinder (3) tank body air inlet/outlet (36)
In air pressure and all kinds of atmosphere of argon, nitrogen, ammonia, hydrogen, oxygen, realize that plasma implements independent tune to the ball milling effect for being processed powder body
Control；
The awkward silence at a meeting plasma asistance high-energy ball milling device is using additional awkward silence at a meeting plasma electrical source (2) to electric discharge ball grinder (3)
The different voltage and current of input, then ball grinder (3) internal atmosphere that discharges is controlled by controllable atmosphere system (5)
Adjustment, the sparking electrode rod (4) then allowed in electric discharge ball grinder (3) produces intensity controlled corona or glow discharge phenomenon,
So as to realize that the processed powder body to discharging in ball grinder implements the mistake of plasma field high-energy ball milling, Aided Machine alloying
Journey.
2. it is a kind of awkward silence at a meeting plasma discharge auxiliary high-energy ball milling powder body device, including vibration type high-energy ball milling main frame (1), additional
Awkward silence at a meeting plasma electrical source (2), electric discharge ball grinder (3), sparking electrode rod (4), controllable atmosphere system (5) and cooling system
(6) six ingredients, it is characterised in that
The structure of described vibration type high-energy ball milling main frame (1) is the form of eccentric vibration mill；
Described additional awkward silence at a meeting plasma electrical source (2) is become civil power using the high-voltage ac power of AC-DC-AC mapping modes
For high frequency electric, wherein using frequency modulation control mode, operating frequency range is adjustable in 1～20kHz, and power supply is defeated for the conversion of DC-AC
Go out voltage range between 1～30kV；
Described electric discharge ball grinder (3) includes connector drum (31), front shroud (32), back shroud (33), with electric discharge ball grinder (3)
The plasma electrical source minus earth pole (34) of connection；Front shroud (32) outer face of electric discharge ball grinder (3) is equipped with vacuum
Air valve (324), with external gas circuit controllable atmosphere system (5) has been collectively constituted；
The sparking electrode rod (4) is cylindrical bar, by its internal ferrum or the conductive core (41) and polytetrafluoroethyl-ne of copper product
The insulating outer layer (42) of alkene material is collectively constituted；Conductive core (41) is connected with plasma electrical source positive pole high-pressure stage (35), makees
For a pole of plasma discharge, dielectric barrier presence of the insulating outer layer (42) as electric discharge；
Described controllable atmosphere system (5), can be in difference installed in the top of electric discharge ball grinder (3) tank body air inlet/outlet (36)
In air pressure and all kinds of atmosphere of argon, nitrogen, ammonia, hydrogen, oxygen, realize that plasma implements independent tune to the ball milling effect for being processed powder body
Control；
The awkward silence at a meeting plasma asistance high-energy ball milling device is using additional awkward silence at a meeting plasma electrical source (2) to electric discharge ball grinder (3)
The different voltage and current of input, then ball grinder (3) internal atmosphere that discharges is controlled by controllable atmosphere system (5)
Adjustment, the sparking electrode rod (4) then allowed in electric discharge ball grinder (3) produces intensity controlled corona or glow discharge phenomenon,
So as to realize that the processed powder body to discharging in ball grinder implements the mistake of plasma field high-energy ball milling, Aided Machine alloying
Journey.
3. awkward silence at a meeting plasma discharge auxiliary high-energy ball milling powder body device according to claim 1, it is characterised in that with institute
The conductive core (41) for stating internal ferrum or copper product collectively constitutes the insulating outer layer (42) of sparking electrode rod (4), is high purity oxygen
Change aluminum ceramic material；The insulating outer layer (42) of the high-purity alpha-alumina ceramic material, using Direct precipitation mode or differential of the arc oxygen
Change mode shapes.
4. awkward silence at a meeting plasma discharge auxiliary high-energy ball milling powder body device according to claim 3, it is characterised in that described
The insulating outer layer (42) of sparking electrode rod (4) is cased with a metal sleeve with mesh (421).
5. awkward silence at a meeting plasma discharge auxiliary high-energy ball milling powder body device according to claim 1, it is characterised in that described
Electric discharge ball grinder (3) the end flanges (311) of cylinder (31) two by sealing ring (312), bolt (313) respectively with front shroud
(32), back shroud (33) is tightly connected, and front shroud (32), the center of back shroud (33) are respectively equipped with for fixed electric discharge electricity
The through hole (321) and blind hole (331) of pole rod (4).
6. awkward silence at a meeting plasma discharge auxiliary high-energy ball milling powder body device according to claim 5, it is characterised in that described
Embedded rustless steel sleeve (322) of the through hole (321) of the front shroud (32) of electric discharge ball grinder (3) and sealing rubber ring (323), it is described
The blind hole (331) of back shroud (33) medial surface is embedded with rustless steel sleeve gasket (332)；Wherein front shroud (32) is including politef
Plate (325) and ceramic wafer (326), back shroud (33) includes polyfluortetraethylene plate (333) and ceramic wafer (334).
7. awkward silence at a meeting plasma discharge auxiliary high-energy ball milling powder body device according to claim 1, it is characterised in that described
Outside the internal ferrum of sparking electrode rod (4) or conductive core (41) fastening end (411) of copper product and the insulation of polytetrafluoroethylmaterial material
Layer (42) is coordinated using screw thread, and discharge end (412) is coordinated using polished rod structure and insulating outer layer (42), conductive core (41) with
Heat-resistant adhesive, and conductive core (41) top are filled with the fit clearance of insulating outer layer (42) with spherical structure (413) and insulation
Outer layer (42) medium is engaged；
Wherein, polished rod, spherical interface cooperation of the sparking electrode rod (4) using conductive core (41) and insulating outer layer (42),
Suppress the unlimited enhancing of micro discharge so that dielectric barrier discharge will not change into spark discharge or arc discharge, such that it is able to keep away
The scaling loss of ball milling free system.
8. awkward silence at a meeting plasma discharge auxiliary high-energy ball milling powder body device according to claim 1, it is characterised in that described
Controllable atmosphere system (5) by discharge ball grinder (3) setup of entrances and exits ball valve (541,542), control gas discharge and it is defeated
Enter, gas is by air relief valve (51) and the pressure and flow of effusion meter (52) control input；Filtered using filter (551,552)
Powder body, reduces powder because of the discharge of airflow function；Using metal hose (571,572) as gas circuit and the ball valve of ball grinder
(541,542) connect, reduce impact of the ball milling vibration to gas circuit.
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