CN103386347A - Low-temperature ball-milling experimental apparatus - Google Patents
Low-temperature ball-milling experimental apparatus Download PDFInfo
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- CN103386347A CN103386347A CN2013103300164A CN201310330016A CN103386347A CN 103386347 A CN103386347 A CN 103386347A CN 2013103300164 A CN2013103300164 A CN 2013103300164A CN 201310330016 A CN201310330016 A CN 201310330016A CN 103386347 A CN103386347 A CN 103386347A
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Abstract
The invention relates to a low-temperature ball-milling experimental apparatus which comprises a planetary low-temperature ball mill arranged in a sealed box, wherein a low-temperature gas generating device is connected onto an air inlet through a pipeline with a gas temperature control device, cooling gas is discharged from an exhaust port formed in the top of the sealed box, a drive device is arranged at the rear end of the sealed box and drives the planetary type low-temperature ball mill to rotate through a transmission device arranged at the bottom of the sealed box, and the transmission device is arranged in a base. Through the low-temperature ball-milling experimental apparatus, low-temperature gas generated by the low-temperature gas generating device is introduced into the sealed box, the low temperature of low-temperature ball milling is obtained by using the low-temperature gas when the drive mechanism drives the planetary type low-temperature ball mill, a ball milling tank is pre-cooled, and thus the function of saving energy is achieved, the gas is exhausted by the exhaust port in the top of the sealed box, and the low-temperature ball-milling experimental apparatus capable of accurately, efficiently and rapidly preparing relatively fine and passivated nano powder particles is realized.
Description
Technical field
The present invention relates to a kind of can be the low temperature ball milling experimental system of being on active service under-120 ℃～-196 ℃ in normal pressure, operating temperature, is specifically related to a kind of low temperature ball milling experimental provision.
Background technology
Planetary ball mill is mainly for powders such as pulverizing, grinding, dispersed metal, nonmetal, organic, Chinese herbal medicines and design, its operation principle is utilized the rolling at a high speed in grinding pot of abrasive material and powder exactly, and material is produced strong shear, impacts, rolls the purpose that reaches pulverizing, grinding, dispersion, emulsifying material.Planetary ball mill is equipped with four ball grinders on same rotating disk, when dial rotation, ball grinder in turntable shaft revolution again around the Pivot Point Center rotation, make planetary motion.In tank, abrading-ball can collide mutually in high-speed motion, grinds and biased sample.
Yet the actual ball mill grinding process of powder is but very complicated.As take a certain independent particle as research object, in mechanical milling process, it can be subject to grinding the effect of compression repeatedly, causes the crack extesion that is present on this particle surface (intrinsic or newly-generated), and then causes it broken or produce plastic deformation.When this particle was constantly pulverized, the new particle of certain one-level of generation just was difficult to further levigate, and this is because the lip-deep crackle of new grain is thinner, and the cause that also reduced of crackle probability that a certain minimum fracture strength occurs.When shattering process was proceeded, required finished breaking stress may increase to and make particle produce the degree of plastic deformation.At this moment, along with the generation of plastic deformation, particle just can be by not levigate.Therefore, have a granularity limiting value during grinding material.That is to say, when the grinding of material entered into the scope of ultra-fine grinding, the pulverization of ball mill was just more and more difficult.All have the grinding limit of a reality in most of grinding systems, this limit depends on that mainly the grinding product particle produces the tendency of again building up, and the physical equilibrium of setting up between accumulation and fragmentation.Therefore, long prolongation Ball-milling Time is skimble-skamble, only can cause the increase of energy consumption, because meticulous particle can't store the elastic energy that makes crack extesion required effectively.
Summary of the invention
The object of the invention is to address the above problem, a kind of low temperature ball milling experimental provision is provided, this device carries out ball milling refinement or alloying to the powder of different materials at low temperatures, can prepare more tinyly, the nano-powder particles of passivation, have accurately, efficiently, the characteristics such as quick.
For achieving the above object, the technical solution adopted in the present invention is: comprise the planetary low temperature ball mill that is arranged in seal box, the air inlet of seal box front end is connected with the cryogenic gas generation device, the cryogenic gas generation device is connected on air inlet by the pipeline with the gas attemperating unit, and refrigerating gas is finally discharged by the exhaust outlet at the top that is opened in seal box; The rear end of seal box is equipped with drive unit, and drive unit drives planetary low temperature ball mill by the transmission device that is arranged on the seal box bottom and rotates, and the bottom of seal box is equipped with support, and transmission device is arranged in support.
Described planetary low temperature ball mill comprises that four rotating speeds are the ball grinder of 100～500r/min, each ball grinder all is contained in and draws in toilet, the top of ball grinder is provided with and cooperatively interacts the crossbeam of its sealing, tie down screw and clamping screw, four ball grinders all by floor installation in mounting disc, the coaxial planetary gear that is fixed with in the below of base, the mounting disc below is provided with transition gear co-axially fixed with it, and transition gear is meshed with each planetary gear respectively.
Described clamping screw, tie down screw and crossbeam use the 9%Ni steel to do.
The material of described ball grinder and abrading-ball is stainless steel or zirconia or aluminium oxide.
Described drive unit comprises motor and the frequency converter that is arranged in electric machine casing, and the rear end of electric machine casing seals electric machine casing by back shroud, also is equipped with on electric machine casing for the control box of controlling frequency converter and motor speed.
Described transmission mechanism comprise with motor output shaft coaxial fix the first belt wheel and with co-axially fixed the second belt wheel of transition gear, the first belt wheel is connected with the second belt wheel by belt; The diameter of the second belt wheel is greater than the first belt wheel.
Described cryogenic gas generation device comprises Dewar bottle, and the bottle mouth position of Dewar bottle is equipped with the cryogenic pumping machine, and Dewar bottle is connected with the air inlet of seal box by the low temperature thermal insulation air channel.
Described gas attemperating unit comprises power heater and the first temperature probe that is arranged on low temperature thermal insulation air channel inside.
Described low temperature thermal insulation air channel and seal box use low-temperature alloy steel 9%Ni steel to make, and shell both all is incubated by acquiring the high vacuum heat-insulation material.
Be equipped with on the inwall of described seal box for the second temperature probe of surveying sealing the temperature inside the box.
Compared with prior art, the present invention has following beneficial effect:
The cryogenic gas that the present invention produces the cryogenic gas generation device is passed in seal box, when driving mechanism drives planetary low temperature ball mill rotation, utilize cryogenic gas to obtain the cryogenic temperature of low temperature ball milling, and precooling ball grinder, reach energy-conservation effect, last gas is discharged by the steam vent at seal box top, having realized can be accurately, efficiently, the ball mill device of the nano-powder particles of more tiny, the passivation of preparation efficiently.
Further, the present invention is provided with temperature probe at low temperature thermal insulation air channel and seal box, can reasonably control cryogenic temperature.
Further, the shell of low temperature thermal insulation air channel of the present invention and seal box all is incubated by acquiring the high vacuum heat-insulation material, has reduced thermal loss.
Further, the present invention controls motor and frequency converter by controller is set, thereby the article of ball milling are regulated the rotating speed of planetary low temperature ball mill as required, with the powder that adapts to different materials, carry out ball milling refinement or alloying.
Description of drawings
Fig. 1 is overall structure schematic diagram of the present invention.
Wherein, 1 is Dewar bottle; 2 is the cryogenic pumping machine; 3 is the low temperature thermal insulation air channel; 4 is power heater; 5 is the first temperature probe; 6 is the second belt wheel; 7 is the second temperature probe; 8 is transition gear; 9 is planetary gear; 10 are mounting disc; 11 is the first belt wheel; 12 is support; 13 is motor; 14 is back shroud; 15 for drawing toilet; 16 is ball grinder; 17 is frequency converter; 18 is crossbeam; 19 is tie down screw; 20 is clamping screw; 21 is control box; 22 is exhaust outlet; 23 is seal cover.
The specific embodiment
The present invention is described in further detail below in conjunction with accompanying drawing:
Participate in Fig. 1, the present invention includes the planetary low temperature ball mill that is arranged in seal box, planetary low temperature ball mill comprises the ball grinder 16 that four rotating speeds are 100～500r/min, ball grinder 16 is stainless steel or zirconia or aluminium oxide with the material of abrading-ball, each ball grinder 16 all is contained in and draws in toilet 15, the top of ball grinder 16 is provided with and cooperatively interacts the crossbeam of its sealing 18, tie down screw 19 and clamping screw 20, and clamping screw 20, tie down screw 19 and crossbeam 18 use the 9%Ni steel to do; Four ball grinders 16 all by floor installation in mounting disc 10, the coaxial planetary gear 9 that is fixed with in the below of base, mounting disc 10 belows are provided with transition gear 8 co-axially fixed with it, transition gear 8 is meshed with each planetary gear 9 respectively; Be equipped with on the inwall of seal box for the second temperature probe 7 of surveying sealing the temperature inside the box, the air inlet of seal box front end is connected with the cryogenic gas generation device, the cryogenic gas generation device is connected on air inlet by the pipeline with the gas attemperating unit, and refrigerating gas is finally discharged by the exhaust outlet 22 at the top that is opened in seal box; The cryogenic gas generation device comprises Dewar bottle 1, the bottle mouth position of Dewar bottle 1 is equipped with cryogenic pumping machine 2, Dewar bottle 1 is connected with the air inlet of seal box by low temperature thermal insulation air channel 3, low temperature thermal insulation air channel 3 and seal box use low-temperature alloy steel 9%Ni steel to make, and shell both all is incubated by acquiring the high vacuum heat-insulation material; The gas attemperating unit comprises power heater 4 and the first temperature probe 5 that is arranged on low temperature thermal insulation air channel 3 inside; The rear end of seal box is equipped with drive unit, drive unit comprises motor 13 and the frequency converter 17 that is arranged in electric machine casing, the rear end of electric machine casing, also is equipped with on electric machine casing for the control box of controlling frequency converter 17 and motor 13 rotating speeds the electric machine casing sealing by back shroud 14; Drive unit drives planetary low temperature ball mill by the transmission device that is arranged on the seal box bottom and rotates, transmission mechanism comprises with motor 13 output shafts are coaxial to be fixed the first belt wheel 11 and with co-axially fixed the second belt wheel 6, the first belt wheels 11 of transition gear 8, by belt, with the second belt wheel 6, is connected; The diameter of the second belt wheel 6 is greater than the first belt wheel 11; The bottom of seal box is equipped with support 12, and transmission device is arranged in support 12.
Principle of the present invention:
In recent years, along with the continuous progress of ball grinding technique, the low temperature ball milling, also referred to as Cryomilling, is a kind of Process During High Energy Ball Milling.The low temperature ball grinding technique is high-energy ball milling in low temperature environment, can increase the fragility of material, improves the efficiency that machinery grinds, and strengthens nonequilibrium effect simultaneously in low temperature.Simultaneously, along with the development of nanometer technology and constantly progressive, for guaranteeing that nano-powder grain growth fast can not occur in densified forming process and in nano block use procedure afterwards, thereby guarantee nano structure and corresponding special specific performance, must prepare passivation, have a nanostructured powders of high thermal stability.
Low temperature ball milling experimental system of the present invention, its operating temperature is-120 ℃～-196 ℃, whole system can be divided into four major parts: (a) low temperature nitrogen generation device mainly is comprised of the Dewar bottle that liquid nitrogen is housed; (b) gas attemperating unit, mainly be comprised of netted power-adjustable heater and temperature probe; (c) planetary low temperature ball mill, the ball grinder that by 4 rotating speeds, is mainly 100～500r/min forms, and spherical tank is with the protective cover sealing and leave exhaust outlet at top for the cold air circulation.The cold air of (d) discharging enters in seal box, is used for the precooling ball grinder, and to reach energy-conservation effect, last gas is discharged by the steam vent at seal box top.
The dusty material of low temperature ball milling preparation of the present invention, can be metal, intermetallic compound and oxide, perhaps Inorganic Non-metallic Materials.Purity〉99.9%, grain size intervals is the 50-600 order; Secondly, low temperature nitrogen generation device of the present invention mainly forms with the Dewar bottle that liquid nitrogen is housed, the bottleneck deadend, and at the cryogenic pumping machine that bottleneck is equipped with power-adjustable, be used for extracting cryogenic gas.Have, the heater of the netted power-adjustable of cryogenic gas attemperating unit of the present invention in cryogenic piping, is used for cryogenic gas is heated to regulate its temperature again, and temperature probe is used for measuring cold-gas temperature; Finally, planetary ball mill of the present invention comprises on same rotating disk four ball grinders is housed, when dial rotation, ball grinder in the turntable shaft revolution again around the Pivot Point Center rotation, make planetary motion.In tank, abrading-ball collision mutually in high-speed motion, grind and biased sample.Ball milling hood and fully sealing, and with bottom opening and cryogenic wind-tunnel UNICOM.
The present invention can control rational cryogenic temperature, have good heat-insulating property and less thermal loss, low temperature environment in whole hermetically sealed can offer the suitable cryogenic temperature of ball grinder, and the power of regulating netted heater by temperature probe obtains required cryogenic temperature.
The course of work of the present invention is such:
At first, open the seal cover 23 on ball mill, the powder that grind is put into ball grinder assemble, assemble the complete seal cover 23 that closes.Open the cryogenic pumping machine and adjust rotating speed, the low temperature nitrogen that extracts in Dewar bottle enters in the low temperature thermal insulation air channel.Then adjust heater power according to the first temperature probe, if only need-196 ℃, heater does not start; If need interval interior temperature, need temperature probe.Cryogenic gas is along with cryogenic wind-tunnel enters the interior cooling whole system of ball mill seal cover 23, by the second temperature probe, determines that the temperature in seal box determines the ball milling temperature.So in the bottom of temperature probe, then cold air slowly flows out from seal box top aperture due to the large Probe arrangement of cold air density.Can directly discharge outdoorly, also conduit connectable enters the precooling storehouse and is used for cooling ball grinding jar in advance.Low temperature thermal insulation air channel and seal box all use low-temperature alloy steel 9%Ni steel to make, and shell all is incubated by acquiring the high vacuum heat-insulation material.Its clamping screw, tie down screw and crossbeam use the 9%Ni steel to do too, exactly in order to maintain equally the strength and toughness of steel at low temperatures, and locked ball grinder that can be intact.The material of ball grinder and abrading-ball is stainless steel, also can be the ceramic materials such as zirconia or aluminium oxide, mainly by service condition and the condition that grinds, is coordinated.
The present invention is further illustrated below by specific embodiment:
Carry out the ball milling experiment of-150 ℃ of Si powder.
At first, with the silica flour of purity＞99.9%, granularity is that 200 orders are put into stainless steel jar mill according to the ratio of grinding media to material of 10:1, ball grinder is vacuumized and passes into Ar gas prevent powder oxidation in mechanical milling process.Then assembling jig, cover seal box.Then open cryogenic pumping machine and bleeding regulating acc power; extract cryogenic gas, regulate mesh heater power, check that the temperature of low temperature the first thermal detector shows; for-170 ℃ of up and down; cold air carries out cooling to ball mill insulated hold and ball grinder along with the low temperature thermal insulation air channel enters in the ball mill seal case, then observe the second temperature probe in seal box, and displays temperature is-150 ℃; be incubated after 20 minutes; open ball mill, adjust rotating speed 300r/min, ball milling was shut down after 3 hours.Gained silica flour product is nanocrystal silicon, and through the series of experiments exploration discovery, nanocrystalline grain size significantly reduces with the prolongation of Ball-milling Time.
Embodiment 2
Carry out the ball milling experiment of-196 ℃ of fine aluminium powder.
At first, with the fine aluminium powder of purity＞99.9%, granularity is that 400 orders are put into stainless steel jar mill according to the ratio of grinding media to material of 20:1.Ball grinder is vacuumized and pass into Ar gas prevent powder oxidation in mechanical milling process.Then assembling jig, cover seal box.Then open cryogenic pumping machine and bleeding regulating acc power; extract cryogenic gas; cold air carries out cooling along with the low temperature thermal insulation air channel enters in the ball mill seal case to ball mill insulated hold and ball grinder; then observe two temperature probes; displays temperature is-196 ℃ of up and down, is incubated after 20 minutes, opens ball mill; adjust rotating speed 500r/min, ball milling was shut down after 5 hours.Gained pure aluminium powder product is nanocrystalline, and through the series of experiments exploration discovery, nanocrystalline grain size significantly reduces with the prolongation of Ball-milling Time.
The method that adopts cryogenic gas generation device of the present invention to cool to planetary low temperature ball mill, obviously be better than in prior art directly adding the cooling means of liquid nitrogen in ball grinder.Reason is as follows:
If one adds liquid nitrogen, very easily introduce impurity, aluminium powder can generate AlN with the nitrogen reaction in mechanical milling process;
Two, because the liquid nitrogen addition is limited, so Ball-milling Time can not be long.Simultaneously, due to system at normal temperatures and pressures, the ball grinder temperature can not be constant, can be along with the increase of time temperature rise, therefore affect the accuracy of experimental result and the effect after the powder ball milling.
Claims (10)
1. low temperature ball milling experimental provision, it is characterized in that: comprise the planetary low temperature ball mill that is arranged in seal box, the air inlet of seal box front end is connected with the cryogenic gas generation device, the cryogenic gas generation device is connected on air inlet by the pipeline with the gas attemperating unit, and refrigerating gas is finally discharged by the exhaust outlet (22) at the top that is opened in seal box; The rear end of seal box is equipped with drive unit, and drive unit drives planetary low temperature ball mill by the transmission device that is arranged on the seal box bottom and rotates, and the bottom of seal box is equipped with support (12), and transmission device is arranged in support (12).
2. low temperature ball milling experimental provision according to claim 1, it is characterized in that: described planetary low temperature ball mill comprises that four rotating speeds are the ball grinder of 100～500r/min (16), each ball grinder (16) all is contained in and draws in toilet (15), the top of ball grinder (16) is provided with and cooperatively interacts the crossbeam of its sealing (18), tie down screw (19) and clamping screw (20), four ball grinders (16) all by floor installation in mounting disc (10), the coaxial planetary gear (9) that is fixed with in the below of base, mounting disc (10) below is provided with transition gear co-axially fixed with it (8), transition gear (8) is meshed with each planetary gear (9) respectively.
3. low temperature ball milling experimental provision according to claim 2, is characterized in that: described clamping screw (20), tie down screw (19) and crossbeam (18) use 9%Ni steel work.
4. low temperature ball milling experimental provision according to claim 2 is characterized in that: described ball grinder (19) is stainless steel or zirconia or aluminium oxide with the material of abrading-ball.
5. low temperature ball milling experimental provision according to claim 2, it is characterized in that: described drive unit comprises motor (13) and the frequency converter (17) that is arranged in electric machine casing, the rear end of electric machine casing, also is equipped with on electric machine casing for the control box of controlling frequency converter (17) and motor (13) rotating speed the electric machine casing sealing by back shroud (14).
6. low temperature ball milling experimental provision according to claim 5, it is characterized in that: described transmission mechanism comprise with motor (13) output shaft coaxial fix the first belt wheel (11) and with co-axially fixed the second belt wheel of transition gear (8) (6), the first belt wheel (11) is connected with the second belt wheel (6) by belt; The diameter of the second belt wheel (6) is greater than the first belt wheel (11).
7. low temperature ball milling experimental provision according to claim 1, it is characterized in that: described cryogenic gas generation device comprises Dewar bottle (1), the bottle mouth position of Dewar bottle (1) is equipped with cryogenic pumping machine (2), and Dewar bottle (1) is connected with the air inlet of seal box by low temperature thermal insulation air channel (3).
8. low temperature ball milling experimental provision according to claim 7 is characterized in that: described gas attemperating unit comprises and is arranged on low temperature thermal insulation air channel (3) inner power heater (4) and the first temperature probe (5).
9. according to claim 7 or 8 described low temperature ball milling experimental provisions, it is characterized in that: described low temperature thermal insulation air channel (3) and seal box use low-temperature alloy steel 9%Ni steel to make, and shell both all is incubated by acquiring the high vacuum heat-insulation material.
10. low temperature ball milling experimental provision according to claim 1, is characterized in that: be equipped with on the inwall of described seal box for the second temperature probe (7) of surveying sealing the temperature inside the box.
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| CN103831440A (en) * | 2014-03-24 | 2014-06-04 | 山东大学 | Method for smashing amorphous band Fe78Si9B13 |
| CN105107580A (en) * | 2015-09-21 | 2015-12-02 | 江苏天鹏机电制造有限公司 | Planetary ball mill |
| CN105289801A (en) * | 2015-12-10 | 2016-02-03 | 重庆润际远东新材料科技有限公司 | Silica powder production method |
| CN105689067A (en) * | 2016-04-09 | 2016-06-22 | 长沙米淇仪器设备有限公司 | Variable-frequency planetary ball mill |
| CN107008539A (en) * | 2017-05-24 | 2017-08-04 | 湖北馥雅食品科技有限公司 | Lowtemperaturepulverizer for high-lipid material |
| CN107116490A (en) * | 2017-05-05 | 2017-09-01 | 江苏锋泰工具有限公司 | The SHS preparation methods of multi-block type diamond segment |
| CN108236997A (en) * | 2016-12-23 | 2018-07-03 | 卡梅德生物科技（天津）有限公司 | A kind of use for laboratory minigrinder |
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| CN109724899A (en) * | 2017-10-30 | 2019-05-07 | 中核四0四有限公司 | A kind of determination method of dry ball milling terminal |
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| CN103831440A (en) * | 2014-03-24 | 2014-06-04 | 山东大学 | Method for smashing amorphous band Fe78Si9B13 |
| CN105107580A (en) * | 2015-09-21 | 2015-12-02 | 江苏天鹏机电制造有限公司 | Planetary ball mill |
| CN105289801A (en) * | 2015-12-10 | 2016-02-03 | 重庆润际远东新材料科技有限公司 | Silica powder production method |
| CN105689067A (en) * | 2016-04-09 | 2016-06-22 | 长沙米淇仪器设备有限公司 | Variable-frequency planetary ball mill |
| CN108236997A (en) * | 2016-12-23 | 2018-07-03 | 卡梅德生物科技（天津）有限公司 | A kind of use for laboratory minigrinder |
| CN107116490B (en) * | 2017-05-05 | 2020-02-21 | 江苏锋泰工具有限公司 | SHS preparation method of segment type diamond tool bit |
| CN107116490A (en) * | 2017-05-05 | 2017-09-01 | 江苏锋泰工具有限公司 | The SHS preparation methods of multi-block type diamond segment |
| CN108855426A (en) * | 2017-05-11 | 2018-11-23 | 刘志红 | A kind of adjustable planetary ball mill of rotational velocity |
| CN107008539A (en) * | 2017-05-24 | 2017-08-04 | 湖北馥雅食品科技有限公司 | Lowtemperaturepulverizer for high-lipid material |
| CN109724899A (en) * | 2017-10-30 | 2019-05-07 | 中核四0四有限公司 | A kind of determination method of dry ball milling terminal |
| CN109724899B (en) * | 2017-10-30 | 2021-08-17 | 中核四0四有限公司 | Method for judging dry method ball milling end point |
| CN111282688A (en) * | 2020-02-20 | 2020-06-16 | 西南石油大学 | Integrated intelligent grinding and screening instrument |
| CN111282688B (en) * | 2020-02-20 | 2021-09-17 | 西南石油大学 | Integrated intelligent grinding and screening instrument |
| CN111841770A (en) * | 2020-07-27 | 2020-10-30 | 安徽阖煦微波技术有限公司 | Ball milling device and method for preparing microwave gyromagnetic ferrite material |
| CN112892808A (en) * | 2021-01-14 | 2021-06-04 | 杨锦宏 | Extraction element is smashed to plant negative pressure |
| CN113426531A (en) * | 2021-07-08 | 2021-09-24 | 刘恒瑞 | Multifunctional grinding equipment for medical molecule biological experiment samples |
| CN113426531B (en) * | 2021-07-08 | 2022-07-01 | 刘恒瑞 | Multifunctional grinding equipment for medical molecule biological experiment samples |
| CN116351519A (en) * | 2023-05-12 | 2023-06-30 | 邹平伟佳新型材料科技有限公司 | Liquid nitrogen cooling ball mill |
| CN116351519B (en) * | 2023-05-12 | 2023-08-15 | 邹平伟佳新型材料科技有限公司 | Liquid nitrogen cooling ball mill |
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