CN1718282A - High energy ball mill method with plasma aid - Google Patents
High energy ball mill method with plasma aid Download PDFInfo
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- CN1718282A CN1718282A CN 200510036231 CN200510036231A CN1718282A CN 1718282 A CN1718282 A CN 1718282A CN 200510036231 CN200510036231 CN 200510036231 CN 200510036231 A CN200510036231 A CN 200510036231A CN 1718282 A CN1718282 A CN 1718282A
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Abstract
A plasma aided high-energy ball grinding method includes such steps as installing the front cover plate and rod electrode of ball grinder, respectively connecting the ball grinder and rod electrode to the poles of plasma power supply, loading the powder to be ground in the ball grinder, pumping negative pressure, filling discharging gas medium, turning on the plasma power supply, regulating discharge parameters for corona discharge or glow discharge, and turning on the motor to drive the vibration exciting block for ball grinding.
Description
Technical field
The micro-powder that the present invention relates to receive preparation and mechanical alloying method provide a kind of high energy ball mill method with plasma aid especially.
Background technology
The method that high-energy ball milling prepares alloy powder is one of the most frequently used technology of present nano and micro materials preparation and mechanical alloying, it normally utilizes high energy ball mill to rotate or vibrates the metal or alloy powder fining to receiving micro-meter scale, that is: the ball grinder of two or more powder being put into simultaneously high energy ball mill carries out high-energy ball milling, powder particle is through calendering, pressing, pulverize, the repetitive process of pressing (being carrying out repeatedly of cold welding-pulverizing-cold welding) again, the continuous refinement of powder grain and particle size can be made, micron superfine alloy powder of receiving can be obtained to organize at last with distributed components.Because this method can utilize mechanical energy to make powder realize alloying, rather than with heat energy or electric energy, is also referred to as mechanical alloying so high-energy ball milling prepares the method for alloy powder.At present, high-energy ball-milling process is increasingly extensive in the application in investigation of materials field, utilizing high energy ball mill can prepare compound between simple metal nanometer powder, nano metal, receive a micron composite, nano ceramic material etc., is a new way of nano and micro materials preparation.
As a kind of solid-state New Machining Technology, high-energy ball-milling process shows certain mandatory and non-equilibrium property, and it is exactly in fact a process that energy is forced to processed powder.And usually high energy ball mill is just simple by rotating or the vibratory milling jar, utilizes in the ball grinder mechanical energy of abrading-ball to handle powder, and this influences working (machining) efficiency to a great extent.Because existing high energy ball mill working (machining) efficiency is low, generally need the long period, some product synthetic even need hundreds of hour, the ball milling utensil that causes thus is very serious to the pollution of product powder.For these reasons, high energy ball mill is restricted in the preparation and the production in enormous quantities application facet of actual nano and micro materials, and application in this respect at present still mainly concentrates on laboratory research.High energy ball mill commonly used now comprises the planet gear type ball mill, shimmy formula ball mill, oscillatory type ball mill, stirring ball mill and roller milling machine.Wherein, the planet gear type ball mill is relative higher with the input of shimmy formula ball mill mechanical energy, but it is little to have a processing capacity, and the equipment operation complexity is difficult for improved shortcoming.Stirring ball mill is relative low with the input of roller milling machine mechanical energy, the shortcoming that equipment maintenance cost is high.The oscillatory type ball mill is to use one of more ball mill, and its major advantage is: the powder processing capacity is big, and operating procedure is convenient, and the ball grinder running orbit is simple, and equipment cost is low, realizes technological improvement easily.But its shortcoming is: influenced by the ball grinder amplitude, the mechanical energy that powder is imported is not very high, and the product powder diameter is substantially in micron grade, and the powder reunion is serious, and particle diameter distributes wide, is difficult to obtain the powder of particle diameter in nano-scale; Working (machining) efficiency is low, and when being applied to mechanical alloying, the processing required time is longer.
Summary of the invention
Purpose of the present invention is exactly shortcoming and the problem that exists in the above-mentioned existing ball grinding technique in order to overcome, providing a kind of can strengthen handling the effective energy input of powder, the refinement of powder quick and promote mechanical alloying process improves the high energy ball mill method with plasma aid of working (machining) efficiency greatly.
Purpose of the present invention is achieved through the following technical solutions: this high energy ball mill method with plasma aid, and its step comprises:
(1) installs the front shroud and the electrode bar of ball grinder, and described ball grinder is connected with the two poles of the earth of plasma electrical source respectively with electrode bar;
(2) in ball grinder, pack into abrading-ball and pending powder, and electrode bar contacts with pending powder with abrading-ball, builds the back shroud of ball grinder;
(3) by vacuum valve airtight ball grinder is taken out negative pressure to 0.01~0.1Pa, perhaps feed the discharge gas medium by vacuum valve again after taking out negative pressure, pressure is 0.01~0.1MPa;
(4) connect plasma electrical source, regulate discharge parameter according to discharge gas medium and pressure thereof, voltage is 3~30kv, frequency is 5~40kHz, realize corona discharge or glow discharge, and start drive motors and drive the exciting piece, make frame and the ball grinder that is fixed on the frame vibrates simultaneously, thereby change the relative position of abrading-ball in electrode bar and the ball grinder, carry out corona discharge or glow discharge plasma auxiliary high-energy ball milling.
Corona discharge plasma mainly applies to auxiliary powder refinement, and glow discharge plasma mainly applies to the Aided Machine alloying.
For realizing the present invention better, described abrading-ball cumulative volume accounts for ball grinder volume 70~75%, wherein the abrading-ball of diameter 20~22mm accounts for total abrading-ball quantity 10~15%, diameter 15~18mm abrading-ball account for total abrading-ball quantity 75~80%, the abrading-ball of diameter 10mm accounts for total abrading-ball quantity 10%, and described pending powder pine volume accounts for 30%~130% of space between the abrading-ball.
Described exciting piece adopts double-amplitude 5mm~10mm, motor speed 930~1400r/min.
Described discharge gas medium is argon gas, nitrogen, ammonia, or other organic gas are as methane, and according to the needs of different discharge gas media, the output voltage range of plasma electrical source is 1~30kv, and frequency range is 1~40kHz.
Described plasma is a kind of highly active atmosphere of high-energy that has, because it has the microcosmic particle that is in excitation state in a large number, make plasma the time with neutral particle or nanometer powder collision, so it not only can be used as a kind of thermal source, the energy of warm-up movement is provided, and main is to change excitation energy, ionization energy, luminous energy into, thereby material surface is caused bombardment, perhaps activate the chemism of gas phase, nanometer powder, bring out the conventional chemical process that is difficult to take place down.And when the reaction powder left plasma, cooldown rate is very big (can to reach 10
5K/s), the process of this quenching can make and handle the special state that powder is in a kind of similar " freezing ", and this acquisition to nano particle is very favourable.And corona discharge plasma has certain ultrasonic wave effect, and it is more even to make the processing powder accept energy, narrow diameter distribution after the powder refinement.When the discharge gas medium is organic gas, can realize simultaneously in-situ-surface modifying to powder at the refinement powder.
Operation principle of the present invention is: from the angle of energy input, on the basis of existing oscillatory type ball mill, ball grinder is improved, described ball grinder and electrode bar are connected the two poles of the earth of described plasma electrical source respectively, because described ball grinder, abrading-ball is conductive material, as stainless steel or carbide alloy, can be used as an electrode integral body, thereby corona discharge or glow discharge between electrode and the abrading-ball in the realization mechanical milling process, plasma is incorporated into ball grinder inside, with mechanical energy single in the former ball milling process and plasma is organic combines, strengthen handling the effective energy input of powder, powder is carried out Combined Processing.
The present invention compared with prior art has following advantage and beneficial effect:
(1) the powder heating is fast, and distortion is big, and the refinement required time is short.Under the same process parameter, the product powder diameter that adopts this method to carry out the auxiliary ball milling of plasma can both reach nanoscale, and narrow diameter distribution, and the product powder diameter of general milling is at micron order, and particle diameter distributes wide.
(2) promote mechanical alloying process, the plasma auxiliary high-energy ball milling, it is the energy of composite plasma body on the basis of conventional mechanical energy, this Combined Processing to powder, in efficient refinement powder, must increase the surface energy and the interface energy of powder, strengthen the reactivity of powder, and the pure fuel factor of plasma also be favourable to promotion diffusion and alloying reaction.
(3) utilize the inventive method, when the discharge gas medium is organic gas, can realize simultaneously in-situ-surface modifying powder at the refinement powder.
(4) technology of the present invention is easy to realize that the working (machining) efficiency height can effectively shorten powder refinement and mechanical alloying required time, and energy savings can make high-energy ball-milling process realize real material preparation and production in enormous quantities, has a extensive future.
Description of drawings
Fig. 1 realizes plasma auxiliary high-energy ball mill device external structure schematic diagram of the present invention.
Fig. 2 is the structural representation of ball grinder shown in Figure 1.
Fig. 3 is the side view of ball grinder shown in Figure 2.
Fig. 4 uses the inventive method and common vibratory milling method ball milling TiO
2ESEM pattern contrast.
Fig. 5 is the ESEM pattern contrast of using the inventive method and common vibratory milling method ball milling Fe.
Fig. 6 is the X diffraction pattern contrast of using the inventive method and common vibratory milling method ball milling W-C system.
The specific embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment one
As shown in Figure 1, realize plasma auxiliary high-energy ball mill device of the present invention, comprise drive motors 1, ball grinder 2, frame 3, base 4, ball grinder 2 is installed on the frame 3, its inside is placed with abrading-ball 5, and frame 3 is installed on the base 4 by spring 6, and its arranged outside has exciting piece 7, drive motors 1 is installed on the base 4, and is connected with frame 3, exciting piece 7 respectively by elastic coupling 8.
Shown in Fig. 2,3, abrading-ball 5 is placed in the ball grinder 2, ball grinder 2 also is connected with electrode bar 9, plasma electrical source 10, ball grinder 2 comprises cylindrical shell 2-1, front shroud 2-1, back shroud 2-3, the flange at cylindrical shell 2-1 two ends is tightly connected with front shroud 2-2, back shroud 2-3 respectively by sealing ring 2-4, bolt 2-5, any bolt 2-5 of front shroud 2-2 is connected with a utmost point of plasma electrical source 10, front shroud 2-2 is provided with electrode perforations 2-2-1, the inboard of electrode perforations 2-2-1 is provided with concave station, and back shroud 2-3 medial surface is provided with blind hole 2-3-1.
The outer surface of electrode bar 9 is provided with clad 11, the concave station of clad 11 respective electrode perforation is provided with shoulder, be provided with gasket seal 12 between concave station and the shoulder, electrode bar 9 front end 9-1 expose and are connected with another utmost point of plasma electrical source 10, and front end 9-1 is threaded and nut 13, nut 13 is close to the lateral surface of protecgulum 2-2, and electrode bar 9 rear end 9-2 penetrate the electrode perforations 2-2-1 of front shroud 2-2 and embed in the blind hole 2-3-1 of back shroud 2-3.
Front shroud 2-2 also is provided with vacuum valve 2-2-2, can take out negative pressure by vacuum valve 2-2-2, also can feed discharge gas medium argon gas, nitrogen, ammonia or organic gas (as methane) and realize milling atmosphere in the ball grinder.
Cylindrical shell 2-1, abrading-ball 5 materials are stainless steel or carbide alloy, and the material of electrode bar 9 is stainless steels, and the material of front shroud 2-2, back shroud 2-3, electrode bar clad 11 is polytetrafluoroethylene (PTFE).The output voltage range of plasma electrical source 10 is 1~30kv, and frequency range is 1~40kHz.
As shown in Figure 1, 2, the step of this high energy ball mill method with plasma aid is:
(1) install the front shroud and the electrode bar of ball grinder, and described ball grinder is connected with the two poles of the earth of plasma electrical source respectively with electrode bar, ball grinder selects for use stainless steel material to make internal diameter 150mm, high 145mm, the thick 6mm of tank skin.
(2) in ball grinder, pack into abrading-ball and pending powder, the abrading-ball cumulative volume accounts for ball grinder volume 70%, wherein the abrading-ball of diameter 20mm accounts for total abrading-ball quantity 10%, the abrading-ball of diameter 15mm accounts for total abrading-ball quantity 80%, the abrading-ball of diameter 10mm accounts for total abrading-ball quantity 10%, pending powder pine volume accounts for 30% of space between the abrading-ball, and electrode bar contacts with pending powder with abrading-ball, builds the back shroud of ball grinder;
(3) by vacuum valve airtight ball grinder is taken out negative pressure to 0.1Pa;
(4) connect plasma electrical source, regulate discharge parameter according to discharge gas medium and pressure thereof, voltage is 15kv, when frequency is 25kHz, realizes corona discharge, and the startup drive motors drives the exciting piece, adopt the 5mm double-amplitude, motor speed 1400r/min makes frame and the ball grinder that is fixed on the frame vibrates simultaneously, thereby change the relative position of abrading-ball in electrode bar and the ball grinder, carry out corona discharge plasma auxiliary high-energy ball milling.
Embodiment two
Adopt the device of embodiment one, the process conditions of this high energy ball mill method with plasma aid are identical with enforcement one substantially, difference is: the abrading-ball cumulative volume accounts for ball grinder volume 75%, wherein the abrading-ball of diameter 22mm accounts for total abrading-ball quantity 15%, the abrading-ball of diameter 18mm accounts for total abrading-ball quantity 75%, diameter 10mm abrading-ball account for total abrading-ball quantity 10%, pending powder pine volume accounts for 130% of space between the abrading-ball; Ball grinder is taken out negative pressure to 0.01Pa; Discharge voltage is 3kv, and frequency is 5kHz, realizes corona discharge; The exciting piece adopts 10mm double-amplitude, motor speed 930r/min.
Embodiment three
Adopt the device of embodiment one, the process conditions of this high energy ball mill method with plasma aid are identical with enforcement one substantially, difference is: the abrading-ball cumulative volume accounts for ball grinder volume 72%, wherein the abrading-ball of diameter 20mm accounts for total abrading-ball quantity 12%, the abrading-ball of diameter 18mm accounts for total abrading-ball quantity 78%, diameter 10mm abrading-ball account for total abrading-ball quantity 10%, pending powder pine volume accounts for 80% of space between the abrading-ball; Ball grinder is taken out negative pressure to 0.05Pa; Discharge voltage is 10kv, and frequency is 20kHz, realizes corona discharge; The exciting piece adopts 8mm double-amplitude, motor speed 930r/min.
Embodiment four
Adopt the device of embodiment one, the process conditions of this high energy ball mill method with plasma aid are identical with enforcement one substantially, and difference is: discharge voltage is 30kv, and frequency is 40kHz, realizes glow discharge.
Embodiment five
Adopt the device of embodiment one, the process conditions of this high energy ball mill method with plasma aid are identical with enforcement two substantially, and difference is: discharge voltage is 10kv, and frequency is 20kHz, realizes glow discharge.
Embodiment six
Adopt the device of embodiment one, the process conditions of this high energy ball mill method with plasma aid are identical with enforcement three substantially, and difference is: discharge voltage is 25kv, and frequency is 30kHz, realizes glow discharge.
Embodiment seven
Adopt the device of embodiment one, the process conditions of this high energy ball mill method with plasma aid are identical with enforcement one substantially, and difference is: ball grinder feeds discharge gas medium argon gas by vacuum valve after taking out negative pressure again, and pressure is 0.01MPa.
Embodiment eight
Adopt the device of embodiment one, the process conditions of this high energy ball mill method with plasma aid are identical with enforcement two substantially, and difference is: ball grinder feeds discharge gas medium ammonia by vacuum valve after taking out negative pressure again, and pressure is 0.1MPa.
Embodiment nine
Adopt the device of embodiment one, the process conditions of this high energy ball mill method with plasma aid are identical with enforcement three substantially, and difference is: ball grinder feeds discharge gas medium nitrogen by vacuum valve after taking out negative pressure again, and pressure is 0.01MPa.
Embodiment ten
Adopt the device of embodiment one, the process conditions of this high energy ball mill method with plasma aid are identical with enforcement three substantially, and difference is: ball grinder feeds discharge gas medium methane by vacuum valve after taking out negative pressure again, and pressure is 0.05MPa.
Adopt the device of embodiment one, the process conditions of this high energy ball mill method with plasma aid are identical with enforcement four substantially, and difference is: ball grinder feeds discharge gas medium argon gas by vacuum valve after taking out negative pressure again, and pressure is 0.01MPa.
Adopt the device of embodiment one, the process conditions of this high energy ball mill method with plasma aid are identical with enforcement five substantially, and difference is: ball grinder feeds discharge gas medium ammonia by vacuum valve after taking out negative pressure again, and pressure is 0.1MPa.
Adopt the device of embodiment one, the process conditions of this high energy ball mill method with plasma aid are identical with enforcement six substantially, and difference is: ball grinder feeds discharge gas medium nitrogen by vacuum valve after taking out negative pressure again, and pressure is 0.04MPa.
Embodiment 14
Adopt the device of embodiment one, the process conditions of this high energy ball mill method with plasma aid are identical with enforcement six substantially, and difference is: ball grinder feeds discharge gas medium methane by vacuum valve after taking out negative pressure again, and pressure is 0.05MPa.
Adopt the auxiliary common vibratory milling of the present invention and no plasma respectively to TiO
2, Fe and W-C system are carried out ball milling, and relatively:
Fig. 4 is that embodiment seven application the inventive method are carried out the auxiliary ball milling of corona discharge and common vibratory milling method ball milling purity is 99.0%, and granularity is 200 order TiO
2ESEM pattern contrast, ball milling time 1h, wherein (a) auxiliary ball milling, (b) common vibratory milling.Visible plasma auxiliary high-energy ball-milled powder granularity evenly distributes about 150nm, and common vibratory milling powder size is distributed in 1-2 μ m.
Fig. 5 is that embodiment seven application the inventive method are carried out the auxiliary ball milling of corona discharge and common vibratory milling method ball milling purity is 98.0%, granularity is the ESEM pattern contrast of 100 order Fe, ball milling time 1h, wherein (a) auxiliary ball milling, (b) common vibratory milling.It is evenly laminar that visible plasma auxiliary high-energy ball-milled powder becomes, and distortion is big, and sheet thickness is much smaller than common vibratory milling result.
Fig. 6 is that embodiment 11 uses the X diffraction pattern contrast that the inventive method is carried out auxiliary ball milling of glow discharge and common vibratory milling method ball milling W-C system, wherein W purity is 99.0%, and granularity is 300 orders, and C purity is 99.9%, granularity is 100 orders, ball milling time 17h.W has appearred in visible plasma auxiliary high-energy ball-milled powder
2The diffraction maximum of C phase, and common vibratory milling powder does not have cenotype to produce.
As mentioned above, can realize the present invention preferably.
Claims (4)
1, a kind of high energy ball mill method with plasma aid is characterized in that step comprises:
(1) installs the front shroud and the electrode bar of ball grinder, and described ball grinder is connected with the two poles of the earth of plasma electrical source respectively with electrode bar;
(2) in ball grinder, pack into abrading-ball and pending powder, and electrode bar contacts with pending powder with abrading-ball, builds the back shroud of ball grinder;
(3) by vacuum valve airtight ball grinder is taken out negative pressure to 0.01~0.1Pa, perhaps feed the discharge gas medium by vacuum valve again after taking out negative pressure, pressure is 0.01~0.1MPa;
(4) connect plasma electrical source, regulate discharge parameter according to discharge gas medium and pressure thereof, voltage is 3~30kv, frequency is 5~40kHz, realize corona discharge or glow discharge, and start drive motors and drive the exciting piece, make frame and the ball grinder that is fixed on the frame vibrates simultaneously, thereby change the relative position of abrading-ball in electrode bar and the ball grinder, carry out corona discharge or glow discharge plasma auxiliary high-energy ball milling.
2, by the described a kind of high energy ball mill method with plasma aid of claim 1, it is characterized in that: described abrading-ball cumulative volume accounts for ball grinder volume 70~75%, wherein the abrading-ball of diameter 20~22mm accounts for total abrading-ball quantity 10~15%, diameter 15~18mm abrading-ball account for total abrading-ball quantity 75~80%, diameter 10mm abrading-ball account for total abrading-ball quantity 10%, described pending powder pine volume accounts for 30%~130% of space between the abrading-ball.
3, by the described a kind of high energy ball mill method with plasma aid of claim 1, it is characterized in that: described exciting piece adopts double-amplitude 5mm~10mm, motor speed 930~1400r/min.
4, by the described a kind of high energy ball mill method with plasma aid of claim 1, it is characterized in that: described discharge gas medium is argon gas, nitrogen, ammonia or organic gas methane.
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