CN109647639B - Ultrasonic atomization grading device for submicron powder and application thereof - Google Patents
Ultrasonic atomization grading device for submicron powder and application thereof Download PDFInfo
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Abstract
The invention discloses an ultrasonic atomization grading device for submicron powder and application thereof, belonging to the field of powder grading. The ultrasonic atomization grading device comprises an ultrasonic atomization device, a solution inlet, a solution outlet, a nitrogen inlet and a nitrogen outlet; a liquid whistle dispersing device is arranged behind the solution inlet and comprises a pipeline for mounting a pore plate and a pipeline for mounting a reed, and the two pipelines are connected through a flange; a silicon powder collecting device is arranged in front of the nitrogen outlet; install level sensor and transducer on ultrasonic atomization device's the container inner wall, the figure of transducer is 4 ~ 6 and evenly install on same height. The ultrasonic atomization grading device provided by the invention grades the submicron silicon powder by adopting an ultrasonic atomization grading mode, solves the problems of long grading time, low precision, complex process and the like in the conventional grading mode, and disperses the raw materials, thereby improving the grading efficiency of ultrasonic atomization grading.
Description
Technical Field
The invention belongs to the field of powder classification, and particularly relates to an ultrasonic atomization classification device for submicron powder and application thereof.
Background
The particle size of silicon powder manufactured after ball milling at present has two scales of micron scale (the particle size diameter is 1.0-5.0 μm) and submicron scale (the particle size diameter is 100 nm-1.0 μm), in order to further improve the performance of a product, the submicron silicon powder needs to be separated from the silicon powder, and the process is called as submicron grade classification of the silicon powder. Currently known methods for classifying silicon powders include centrifugal classification, microfiltration, wet electrostatic classification, cyclone classification, etc., but these methods have the following disadvantages:
1. the density gradient is not apparent when classifying submicron particles. The particle size of the particles after centrifugal classification can reach between 40 and 60 mu m, and the particle size of the particles after cyclone classification can reach about 1.7 mu m, so that the classification precision of the centrifugal classification and the cyclone classification is low, and the requirement of submicron particle classification cannot be met.
2. The process is complex and the process is discontinuous. The particle size of the particles obtained by classification by adopting a microporous filtration method can reach 0.1-20 mu m, but the particles are easy to block micropores in the classification process, so that the filter paper is frequently interrupted and replaced in the classification process, and the classification cannot be continuously carried out, thereby seriously influencing the classification efficiency.
3. The grading efficiency is low and the time consumption is long. The particle size of the particles can reach 0.1-0.4 μm after wet electrostatic classification, but the classification time needs 4-8h and takes long time because the particles move slowly in the solution.
Disclosure of Invention
The invention aims to solve the problems that: solves the problems of complex process, low grading efficiency, long time consumption, discontinuity and the like in the submicron grade grading of powder in the prior art.
In order to solve the technical problem, the invention provides an ultrasonic atomization grading device for submicron powder, which comprises an ultrasonic atomization device 1, a solution inlet 6, a nitrogen inlet 4, a solution outlet 7, a powder collecting device 2 and a nitrogen outlet 3; the ultrasonic atomization device 1 is divided into an upper part, a middle part and a lower part, wherein the upper part is conical, the middle part is cylindrical, the lower part is conical or cylindrical, the ultrasonic atomization device 1 comprises transducers 120, reaction tanks 130, partition plates 140 and cylindrical partition plates 150, the transducers 120 and the reaction tanks 130 are arranged on the inner wall of the middle part of the ultrasonic atomization device 1, the transducers 120 and the reaction tanks 130 are 4-6 and are uniformly arranged at the same height of the middle part of the ultrasonic atomization device 1, the reaction tanks 130 correspond to the transducers 120 one by one, and the reaction tanks 130 are arranged on the periphery of the transducers 120 and are open at the upper part; the cylindrical partition plate 150 is vertically fixed in the middle of the ultrasonic atomization device 1 and is coaxial with the ultrasonic atomization device 1, and the height of the bottommost end of the cylindrical partition plate 150 is lower than the highest position of the reaction tank 130; the lower part of the ultrasonic atomization device 1 is provided with a partition plate 140, and the partition plate 140 is provided with a small hole;
the solution inlet 6 is connected with a solution pipeline 8 through a liquid whistle dispersion device 5, and the solution pipeline 8 is connected with the ultrasonic atomization device 1 and extends into the ultrasonic atomization device 1 to be communicated with the bottom of each reaction tank 130; the nitrogen inlet 4 is connected with the ultrasonic atomization device 1 and is positioned below the solution inlet 6; the nitrogen outlet 3 is connected with the top of the ultrasonic atomization device 1 through the powder collecting device 2, and the solution outlet 7 is positioned at the bottom of the ultrasonic atomization device 1.
In one embodiment of the present invention, the angle between the transducer 120 and the horizontal plane is 60-70 °.
In one embodiment of the invention, the reaction tank 130 is positioned 5-10cm above the transducer.
In one embodiment of the present invention, the height ratio of the upper, middle and lower portions of the ultrasonic atomization device 1 is: 6-10: 19-25: 4-6.
In one embodiment of the present invention, the angle of the taper of the upper portion of the ultrasonic atomization device 1 is 35 to 40 °, and when the lower portion of the ultrasonic atomization device 1 is tapered, the angle of the taper of the lower portion is 20 to 25 °.
In one embodiment of the present invention, the bottom of the cylindrical partition plate 150 is lower than the highest point of the reaction tank 130, a gap is left at the top of the cylindrical partition plate 150, an airflow channel is constructed by the partition plate, a rotational flow is formed in the channel after the tangential introduction of nitrogen, and the gas is discharged from the top of the ultrasonic atomization device 1 more completely and reliably.
In an embodiment of the present invention, the cylindrical isolation plate 150 is fixed in the middle of the ultrasonic atomization device 1 by welding a plurality of solid round bars 160, and the number of the solid round bars 160 is preferably 4-8.
In one embodiment of the invention, the nitrogen inlet 4 adopts an inclined upward tangential air inlet mode which forms an angle of 15-20 degrees with the horizontal direction, and the height of the air inlet is slightly higher than the highest point of the reaction tank, so that the fog can be better driven to be discharged from the nitrogen outlet 3.
In one embodiment of the present invention, preferably, the isolation plate 140 is inclined downward from the end of the ultrasonic atomization device 1 to the small hole, the inclination angle is 2 to 20 degrees, and the diameter of the small hole is 1/30 to 1/20 of the diameter of the middle part of the ultrasonic atomization device 1; the number of the small holes is preferably 1-3, and more preferably 1.
In one embodiment of the present invention, the isolation plate 140 has a funnel shape.
In one embodiment of the invention, the liquid whistle dispersing device 5 comprises a pipe with an orifice plate 520 and a pipe with a reed 540, the two pipes being connected by a flange 530.
In an embodiment of the present invention, the orifice plate 520 is axially perpendicular to a pipeline on which the orifice plate 520 is installed, a diameter of the orifice plate 520 is equal to an inner diameter of the pipeline, the orifice plate 520 is provided with an orifice 510, a circle center of the orifice 510 is a circle center of the orifice plate, a ratio of the diameter of the orifice 510 to the diameter of the pipeline is 1/25-1/10, and the number of the orifice plates 520 is preferably 1.
In one embodiment of the present invention, the pipe with the orifice 510 is provided with a pressure gauge 580
In one embodiment of the present invention, one end of the reed 540 is fixed to the reed mounting member 550 by a bolt 570, a washer 5100, and a nut 590, the reed mounting member 550 is mounted to the flange 560 by the bolt 570, and the flange 560 is mounted in the pipe by welding.
In one embodiment of the invention, the free vibrating end of reed 540 is aligned with aperture 510 and one end is free to vibrate.
In one embodiment of the invention, the distance from reed 540 to orifice plate 520 can be varied by adjusting the thickness of shim 590, where a smaller shim 590 is used to distance reed 540 from orifice plate 520 when fluid flow is greater, and where a larger shim 590 is used to bring reed 540 closer to orifice plate 520 when fluid flow is less, to adjust the dispersion effect of the reed on the suspension.
In one embodiment of the invention, the reed 540 has a smaller width at the free vibrating end than at the fixed end.
In one embodiment of the invention, the reed 540 has a distance from the free vibrating end to the aperture 510 of 10-14 mm.
In one embodiment of the present invention, the length and thickness of the reed 540 are 38-40 mm and 0.3-0.5mm, respectively, the width of the free vibrating end is 4-5 mm, and the width of the fixed end is 6-8 mm.
In one embodiment of the present invention, a pressure gauge 580 is installed on the pipe of the orifice plate 520 to control the inlet water pressure to be 0.3-0.5 MPa.
In one embodiment of the present invention, the solution outlet 7 may connect a part of the outlet solution or the entire outlet solution with the solution inlet 6 through a pump, mix with the inlet solution, circulate into the apparatus for classification, and may classify the powder that is not completely separated again, thereby improving the utilization rate of the product and realizing continuous classification of the ultrasonic atomization classification apparatus.
The invention also provides a method for grading submicron powder by using the device.
In one embodiment of the invention, the process is directed to the classification of submicron powders such as silicon powder, silica, silicon carbide, and the like.
In one embodiment of the present invention, the method is: adding water into powder to be separated to prepare suspension, feeding the suspension from a solution inlet 6, forming jet flow through a small hole 510 in the middle of a pore plate 520, enabling the jet flow to impact a reed 540, enabling the reed 540 to vibrate and enable the powder in the suspension to be fully dispersed, enabling the dispersed suspension to enter an ultrasonic atomization device 1, shunting to enter each reaction tank 130, enabling the submicron powder and the solution to be atomized to form mist under the action of a transducer 120, enabling nitrogen to enter the ultrasonic atomization device 1 from a nitrogen inlet 4, enabling the mist to form rotational flow in a gas channel formed by the inner wall of the ultrasonic atomization device 1 and a cylindrical partition plate 150 under the action of the nitrogen, enabling the nitrogen to drive the mist to be rapidly discharged from the top of the ultrasonic atomization device 1, collecting the submicron silicon powder in the mist through a silicon powder collecting device 2, discharging the rest of nitrogen through a nitrogen outlet 3, enabling unreacted silicon powder suspension to overflow from the upper end of the reaction tank 130, is discharged through the middle of the partition plate 140 and is finally discharged through the solution outlet 7.
In one embodiment of the present invention, the submicron-sized silicon powder is collected by liquid nitrogen in the silicon powder collection device 2.
In an embodiment of the present invention, a part of the suspension discharged from the solution outlet 7 may return to the solution inlet 6, and the micro-nano particles that may not be atomized in the suspension are circularly atomized again, so as to complete the classification of the sub-micron silicon powder.
In one embodiment of the invention, when a jet is formed and impacts reed 540, reed 540 is excited to vibrate laterally, radiating sound waves into the surrounding liquid, and the sound wave field creates a strong alternating pressure on the suspension, thereby allowing the powder in the suspension to be dispersed sufficiently.
In one embodiment of the invention, the suspension has a mass concentration of 0.1 to 0.5%.
In one embodiment of the present invention, the solution inlet 4 has an inlet water pressure of 0.3 to 0.5 MPa.
In one embodiment of the present invention, the N is2The flow rate/flow of the water is 3-15L/min.
In one embodiment of the invention, the frequency of the transducer is 1.7MHz or 2.4 MHz.
The invention has the beneficial effects that:
1) the liquid in the liquid whistle dispersion device forms jet flow to impact the metal reed whistle, so that the reed is excited to vibrate and act on the liquid-solid medium, and the liquid whistle dispersion device plays a role in fully dispersing and depolymerizing particles such as silicon powder.
2) The inlet water pressure is intelligently controlled by pressure, the feeding flow rate is automatically adjusted, or the position of the reed is changed, so that the generated jet flow can cause the resonance of the reed, and the optimal dispersion effect of the silicon powder and the like is achieved.
3) The reed of the invention adopts a structure with a narrower free vibration end, and can increase the resonance effect and better disperse the solid powder in the suspension compared with the common reed.
4) A plurality of transducers in the ultrasonic atomization device are used simultaneously and are blocked by the reaction tank, so that ultrasonic waves are limited in the reaction tank, the energy density of the ultrasonic waves is improved, and the atomization effect is enhanced; and a plurality of transducers are combined, so that the grading efficiency and the atomization result can be improved, and the grading time is shortened.
5) The height of the reaction tank of the ultrasonic atomization device is 5-10mm higher than that of the transducer, so that the best atomization effect of the submicron silicon powder and water is ensured.
6) Adopt the liquid nitrogen to collect the submicron order silica flour in the fog among the silica flour collection device, the collection effect is better, and the nitrogen gas entry is the tangential air inlet to design ultrasonic atomization device upper end and be the toper structure, set up the division board in ultrasonic atomization device, form annular gas passageway, be favorable to atomizing back gaseous better, faster discharge ultrasonic atomization device, shorten the classification time.
7) Generally, during continuous operation, the flow direction of nitrogen is influenced by opening the solution outlet, so that the grading efficiency is influenced, and therefore, the solution outlet can only be opened intermittently, and complete continuous operation cannot be formed.
8) The solution outlet is arranged to connect part of the outlet solution with the solution inlet, so that the suspension is fully dispersed and atomized, the product utilization rate is improved, the ultrasonic atomization classification of continuous feeding and discharging is realized, and the classification efficiency is high.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
FIG. 2 is a schematic view of the nitrogen inlet of the present invention.
Fig. 3 is a schematic view of the structure of the liquid whistle dispersing device of the present invention.
Fig. 4 is a schematic view of an orifice plate in a liquid whistle dispensing device of the present invention.
Fig. 5 is a schematic structural view of an ultrasonic atomizing device according to the present invention.
Fig. 6 is a schematic top view of the three-dimensional structure of the ultrasonic atomization device of the present invention.
1-ultrasonic atomization device, 110-fog, 120-transducer, 130-reaction tank, 140-isolation plate, 150-cylindrical isolation plate, 2-powder collection device, 3-nitrogen outlet, 4-nitrogen inlet, 5-liquid whistle dispersion device, 510-small hole, 520-pore plate, 530-flange, 540-reed, 550-reed mounting piece, 560-flange, 570-bolt, 580-pressure gauge, 590-nut, 5100-gasket, 6-solution inlet, and 7-solution outlet.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to specific embodiments and the accompanying drawings. In which like parts are designated by like reference numerals. It should be noted that the words "front", "rear", "left", "right", "upper" and "lower" used in the following description refer to directions in the drawings.
Grading efficiency: the material in the silicon powder collecting device is subjected to particle size measurement every five minutes, when the particle size distribution of particles is unchanged, the device is determined to reach a stable working state, the particle size with the particle classification efficiency of 50 percent is set as a cutting particle size, and the formula of the classification efficiency is as follows:
in the formula: dp-particle size, nm;
Δη(Dp) Particle diameter DpClassification efficiency,%;
ms、mc-the mass flow of fine and coarse particles, kg/s;
fs(Dp)、fc(Dp) Particle size is particle size DpConcentration in the fine and coarse mass flow.
D when Δ η is 50%pIn order to measure the important index of the grading performance of the device, the invention measures the D after grading50The data of (1).
As shown in fig. 1, an ultrasonic atomization classification device for submicron powder,
in order to solve the technical problem, the invention provides an ultrasonic atomization grading device for submicron powder, which comprises an ultrasonic atomization device 1, a solution inlet 6, a nitrogen inlet 4, a solution outlet 7, a powder collecting device 2 and a nitrogen outlet 3; the ultrasonic atomization device 1 is divided into an upper part, a middle part and a lower part, wherein the upper part is conical, the middle part is cylindrical, the lower part is conical or cylindrical, the ultrasonic atomization device 1 comprises transducers 120, reaction tanks 130, partition plates 140 and cylindrical partition plates 150, the transducers 120 and the reaction tanks 130 are arranged on the inner wall of the middle part of the ultrasonic atomization device 1, the transducers 120 and the reaction tanks 130 are 4-6 and are uniformly arranged at the same height of the middle part of the ultrasonic atomization device 1, the reaction tanks 130 correspond to the transducers 120 one by one, and the reaction tanks 130 are arranged on the periphery of the transducers 120 and are open at the upper part; the cylindrical partition plate 150 is vertically fixed in the middle of the ultrasonic atomization device 1 and is coaxial with the ultrasonic atomization device 1, and the height of the bottommost end of the cylindrical partition plate 150 is lower than the highest position of the reaction tank 130; the lower part of the ultrasonic atomization device 1 is provided with a partition plate 140, and the partition plate 140 is provided with a small hole;
the solution inlet 6 is connected with a solution pipeline 8 through a liquid whistle dispersion device 5, and the solution pipeline 8 is connected with the ultrasonic atomization device 1 and extends into the ultrasonic atomization device 1 to be communicated with the bottom of each reaction tank 130; the nitrogen inlet 4 is connected with the ultrasonic atomization device 1 and is positioned below the solution inlet 6; the nitrogen outlet 3 is connected with the top of the ultrasonic atomization device 1 through the powder collecting device 2, and the solution outlet 7 is positioned at the bottom of the ultrasonic atomization device 1.
Furthermore, transducer 120 installation angle is 60 ~ 70 with the horizontal plane contained angle, can effectively solve the problem of installing transducer atomization efficiency is not high on the wall.
Furthermore, the height of the reaction tank is controlled to be 5-10cm higher than the transducer, the shallower the liquid level is, the better the ultrasonic atomization effect is, but when the liquid level is too shallow, the atomization of the submicron silicon powder is affected.
Furthermore, the nitrogen inlet 4 adopts an upward tangential air inlet mode with an inclination of 15-20 degrees with the horizontal direction, and the height is slightly higher than the highest point of the reaction tank.
Further, the height ratio of the upper part, the middle part and the lower part of the ultrasonic atomization device 1 is as follows: 6-10: 19-25: 4-6.
Further, the angle of the taper of the upper part of the ultrasonic atomization device 1 is 35-40 °, and when the lower part of the ultrasonic atomization device 1 is tapered, the angle of the taper of the lower part is 20-25 °.
Furthermore, the bottom of the cylindrical partition plate 150 is lower than the highest position of the reaction tank 130, a gap is reserved at the top of the cylindrical partition plate 150, an airflow channel is formed by the partition plate, a rotational flow is formed in the channel after nitrogen is introduced tangentially, and gas is discharged from the top of the ultrasonic atomization device 1 more completely and reliably.
Further, division plate 140 welds in the reaction tank below, prevents to generate fog 110 and gets into ultrasonic atomization device 1 bottom, leads to letting in nitrogen gas and can't effectively discharge fog 110, influences hierarchical effect.
Furthermore, the isolation plate 140 is inclined downwards from the end connected with the ultrasonic atomization device 1 to the small holes, the inclination angle is 2-20 degrees, the diameter of the small holes is 1/30-1/20 of the diameter of the middle part of the ultrasonic atomization device 1, and the number of the small holes is preferably 1-3, and more preferably 1.
Further, as shown in fig. 3, the liquid whistle dispersing device 5 includes a pipe to which the orifice 520 is mounted and a pipe to which the reed 540 is mounted, and the two pipes are connected by a flange 530.
Further, the orifice plate 520 is axially perpendicular to a pipeline on which the orifice plate 520 is mounted, the diameter of the orifice plate 520 is equal to the inner diameter of the pipeline, the orifice plate 520 is provided with an orifice 510, the circle center of the orifice 510 is the circle center of the orifice plate, the ratio of the diameter of the orifice 510 to the diameter of the pipeline is 1/25-1/10, and the number of the orifice plates 520 is preferably 1.
Further, a pressure gauge 580 is installed on the pipeline provided with the orifice plate 520, and the water pressure at the inlet is controlled to be 0.3-0.5 MPa.
Further, the reed 540 is fixed to the reed mounting member 550 at one end and can freely vibrate at one end.
Further, one end of the reed 540 is fixed on the reed mounting member 550 by a bolt 570, a washer 5100 and a nut 590, the reed mounting member 550 is mounted on the flange 560 by the bolt 570, and the flange 560 is mounted in the pipeline by welding.
Further, the distance from reed 540 to orifice plate 520 can be varied by adjusting the thickness of shim 590, where a smaller shim 590 is used when the liquid flow rate is greater and reed 540 is farther from orifice plate 520, and where a larger shim 590 is used when the liquid flow rate is less and reed 540 is closer to orifice plate 520, to adjust the dispersion effect of the reed on the suspension.
Further, the length and the thickness of the reed 540 are 40 mm and 0.3mm respectively, the width of the free vibration end is 4mm, the width of the fixed end is 6mm, and the distance from the free vibration end of the reed 540 to the small hole 510 is 10-14 mm.
As shown in fig. 1, a powder collecting device 2 is arranged in front of the nitrogen outlet 3, and liquid nitrogen is used for collecting submicron-grade silicon powder in the mist.
Further, a solution outlet 7 connects part of the outlet solution with a solution inlet 6 through a pipeline, and the micro-nano particles which are not atomized in the suspension are circularly atomized again, so that the utilization rate of the product is improved, and the continuous production of the ultrasonic atomization grading device is realized.
Taking submicron grade of silicon powder as an example, the working process of the invention is as follows:
adding water into powder to be separated to prepare suspension, feeding the suspension from a solution inlet 6, forming jet flow through a small hole 510 in the middle of a pore plate 520, enabling the jet flow to impact a reed 540, enabling the reed 540 to vibrate and enable the powder in the suspension to be fully dispersed, enabling the dispersed suspension to enter an ultrasonic atomization device 1, shunting to enter each reaction tank 130, enabling the submicron powder and the solution to be atomized to form mist under the action of a transducer 120, enabling nitrogen to enter the ultrasonic atomization device 1 from a nitrogen inlet 4, enabling the mist to form rotational flow in a gas channel formed by the inner wall of the ultrasonic atomization device 1 and a cylindrical partition plate 150 under the action of the nitrogen, enabling the nitrogen to drive the mist to be rapidly discharged from the top of the ultrasonic atomization device 1, collecting the submicron silicon powder in the mist through a silicon powder collecting device 2, discharging the rest of nitrogen through a nitrogen outlet 3, enabling unreacted silicon powder suspension to overflow from the upper end of the reaction tank 130, is discharged through the middle part of the separation plate 140 and is finally discharged from the solution outlet 7, and finally the grading of the submicron-grade silicon powder is completed.
Example 1
Raw material to be separated: the particle size range of the raw silicon powder is 0-600nm, and the median particle size is 300 nm.
The height ratio of the upper part, the middle part and the lower part of the ultrasonic atomization device 1 is 6: 19: 4, wherein the height of the middle part is 0.5m, the diameter is 0.5m, the angle of the upper part cone is 35 degrees, the lower part cone is 20 degrees, the number of the small holes of the isolation plate 140 is 1, and the diameter is 2 cm.
Preparing the silicon powder to be classified into suspension with the concentration of 0.1%, wherein the flow is 40L/h, feeding the silicon powder suspension from a solution inlet 6, the inlet water pressure of the solution inlet 6 is 0.5MPa, the suspension passes through a small hole 510 in the middle of a pore plate 520 at high speed to form jet flow and generate hydraulic change, the jet flow impacts a reed 540, the length and the thickness of the reed are 40 mm and 0.3mm respectively, the width of a vibration end is 4mm, the width of the fixed end is 6mm, the distance from the small hole is 14mm, the jet flow excites the reed 540 to vibrate transversely, sound waves are radiated to surrounding liquid, and a sound wave field generates strong alternating pressure on a liquid-solid medium to fully disperse the silicon powder in the suspension; the dispersed suspension enters the ultrasonic atomization device 1, is shunted to enter each reaction tank 130, submicron powder and solution are atomized to form mist under the action of 6 transducers 120 with power of 24W, frequency of 2.4MHz and installation angle of 60 degrees, meanwhile, nitrogen enters the ultrasonic atomization device 1 from a nitrogen inlet 4, the flow of the nitrogen is 10L/min, the mist forms rotational flow in a gas channel formed by the inner wall of the ultrasonic atomization device 1 and a cylindrical partition plate 150 under the action of the nitrogen, the nitrogen drives the mist to be rapidly discharged from the top of the ultrasonic atomization device 1, the submicron silicon powder in the mist is collected by a silicon powder collection device 2, the rest nitrogen is discharged from a nitrogen outlet 3, unreacted silicon powder suspension overflows from the upper end of the reaction tank 130, is discharged from the middle part of the partition plate 140 and is finally discharged from a solution outlet 7, and finally finishing the grading of the submicron silicon powder after the outlet flow is stable.
After being debugged on site and 45-50min later, the silicon powder collecting device reaches a stable working state, and the cutting particle size of the suspension liquid is 70nm when the suspension liquid is stable.
Example 2
Raw material to be separated: the particle size range of the raw silicon powder is 0-600nm, and the median particle size is 300 nm.
The height ratio of the upper part, the middle part and the lower part of the ultrasonic atomization device 1 is 6: 19: 4, wherein the height of the middle part is 0.5m, the diameter is 0.5m, the angle of the upper part cone is 35 degrees, the lower part cone is 20 degrees, the number of the small holes of the isolation plate 140 is 1, and the diameter is 2 cm.
Preparing the silicon powder to be classified into suspension with the concentration of 0.1%, wherein the flow rate is 40L/min, feeding the silicon powder suspension from a solution inlet 6, the inlet water pressure of the solution inlet 6 is 0.3MPa, the suspension passes through a small hole 510 in the middle of a pore plate 520 at high speed to form jet flow and generate hydraulic change, the jet flow impacts a reed 540, the length and the thickness of the reed are 40 mm and 0.3mm respectively, the width of a vibration end is 4mm, the width of the fixed end is 6mm, the distance from the small hole is 14mm, the jet flow excites the reed 540 to vibrate transversely, sound waves are radiated to surrounding liquid, and a sound wave field generates strong alternating pressure on a liquid-solid medium to fully disperse the silicon powder in the suspension; the dispersed suspension enters the ultrasonic atomization device 1, is shunted to enter each reaction tank 130, submicron powder and solution are atomized to form mist under the action of 6 transducers 120 with power of 24W, frequency of 2.4MHz and installation angle of 70 degrees, meanwhile, nitrogen enters the ultrasonic atomization device 1 from a nitrogen inlet 4, the flow of the nitrogen is 3L/min, the mist forms rotational flow in a gas channel formed by the inner wall of the ultrasonic atomization device 1 and a cylindrical partition plate 150 under the action of the nitrogen, the nitrogen drives the mist to be rapidly discharged from the top of the ultrasonic atomization device 1, the submicron silicon powder in the mist is collected by a silicon powder collection device 2, the rest nitrogen is discharged from a nitrogen outlet 3, unreacted silicon powder suspension overflows from the upper end of the reaction tank 130, is discharged from the middle part of the partition plate 140 and is finally discharged from a solution outlet 7, and finally, grading the submicron silicon powder.
After being debugged on site and 45-50min later, the silicon powder collecting device reaches a stable working state, and 50% of the suspension liquid has a cutting particle size of 75nm when the suspension liquid is stable.
Example 3
Raw material to be separated: the particle size range of the raw silicon powder is 0-600nm, and the median particle size is 300 nm.
The height ratio of the upper part, the middle part and the lower part of the ultrasonic atomization device 1 is 6: 19: 4, wherein the height of the middle part is 0.5m, the diameter is 0.5m, the angle of the upper part cone is 35 degrees, the lower part cone is 20 degrees, the number of the small holes of the isolation plate 140 is 1, and the diameter is 2 cm.
Preparing the silicon powder to be classified into suspension with the concentration of 0.3%, wherein the flow is 40L/h, feeding the silicon powder suspension from a solution inlet 6, the inlet water pressure of the solution inlet 6 is 0.5MPa, the suspension passes through a small hole 510 in the middle of a pore plate 520 at high speed to form jet flow and generate hydraulic change, the jet flow impacts a reed 540, the length and the thickness of the reed are 40 mm and 0.3mm respectively, the width of a vibration end is 4mm, the width of the fixed end is 6mm, the distance from the small hole is 14mm, the jet flow excites the reed 540 to vibrate transversely, sound waves are radiated to surrounding liquid, and a sound wave field generates strong alternating pressure on a liquid-solid medium to fully disperse the silicon powder in the suspension; the dispersed suspension enters the ultrasonic atomization device 1, is shunted to enter each reaction tank 130, submicron powder and solution are atomized to form mist under the action of 6 transducers 120 with power of 24W, frequency of 2.4MHz and installation angle of 60 degrees, meanwhile, nitrogen enters the ultrasonic atomization device 1 from a nitrogen inlet 4, the flow of the nitrogen is 15L/min, the mist forms a rotational flow in a gas channel formed by the inner wall of the ultrasonic atomization device 1 and a cylindrical partition plate 150 under the action of the nitrogen, the nitrogen drives the mist to be rapidly discharged from the top of the ultrasonic atomization device 1, the submicron silicon powder in the mist is collected by a silicon powder collection device 2, the rest of the nitrogen is discharged from a nitrogen outlet 3, unreacted silicon powder suspension overflows from the upper end of the reaction tank 130, is discharged from the middle part of the partition plate 140 and is finally discharged from a solution outlet 7, and finally finishing the grading of the submicron silicon powder after the outlet flow is stable.
After on-site debugging, the silicon powder collecting device reaches a stable working state after 40-45min, and the cutting particle size of the suspension liquid is 65nm when the suspension liquid is stable.
Example 4
Raw material to be separated: the particle size range of the raw silicon powder is 0-1000nm, and the median particle size is 500 nm.
The height ratio of the upper part, the middle part and the lower part of the ultrasonic atomization device 1 is 6: 19: 4, wherein the height of the middle part is 0.5m, the diameter is 0.5m, the angle of the upper part cone is 35 degrees, the lower part cone is 20 degrees, the number of the small holes of the isolation plate 140 is 1, and the diameter is 2 cm.
Preparing the silicon powder to be classified into suspension with the concentration of 0.1%, wherein the flow is 40L/h, feeding the silicon powder suspension from a solution inlet 6, the inlet water pressure of the solution inlet 6 is 0.5MPa, the suspension passes through a small hole 510 in the middle of a pore plate 520 at high speed to form jet flow and generate hydraulic change, the jet flow impacts a reed 540, the length and the thickness of the reed are 40 mm and 0.3mm respectively, the width of a vibration end is 4mm, the width of the fixed end is 7mm, the distance from the small hole is 14mm, the jet flow excites the reed 540 to vibrate transversely, sound waves are radiated to surrounding liquid, and a sound wave field generates strong alternating pressure on a liquid-solid medium to fully disperse the silicon powder in the suspension; the dispersed suspension enters the ultrasonic atomization device 1, is shunted to enter each reaction tank 130, submicron powder and solution are atomized to form mist under the action of 6 transducers 120 with power of 24W, frequency of 2.4MHz and installation angle of 60 degrees, meanwhile, nitrogen enters the ultrasonic atomization device 1 from a nitrogen inlet 4, the flow of the nitrogen is 10L/min, the mist forms rotational flow in a gas channel formed by the inner wall of the ultrasonic atomization device 1 and a cylindrical partition plate 150 under the action of the nitrogen, the nitrogen drives the mist to be rapidly discharged from the top of the ultrasonic atomization device 1, the submicron silicon powder in the mist is collected by a silicon powder collection device 2, the rest nitrogen is discharged from a nitrogen outlet 3, unreacted silicon powder suspension overflows from the upper end of the reaction tank 130, is discharged from the middle part of the partition plate 140 and is finally discharged from a solution outlet 7, and finally finishing the grading of the submicron silicon powder after the outlet flow is stable.
After field debugging, the silicon powder collecting device reaches a stable working state after 50-55min, and the cutting particle size of the suspension liquid is 100nm when the suspension liquid is stable.
Comparative example 1
Raw material to be separated: the particle size range of the raw silicon powder is 0-600nm, and the median particle size is 300 nm.
When the inlet water pressure of the solution inlet 6 is 0.2MPa, and the rest devices and conditions are the same as those in the embodiment 1, silicon powder classification is carried out according to the method in the embodiment 1, silicon powder is separated, the silicon powder is debugged on site, after 60-65min, the silicon dioxide powder collecting device reaches a stable working state, and 50% of cutting particle size of the suspension liquid is 120nm when the silicon dioxide powder collecting device is stable.
Comparative example 2
Raw material to be separated: the particle size range of the raw silicon powder is 0-600nm, and the median particle size is 300 nm.
When the number of transducers in the ultrasonic atomization classification apparatus 1 was 3, the rest of the apparatus was the same as in example 1. Silicon powder classification is carried out according to the mode of the embodiment 1, silicon powder materials are separated, after on-site debugging is carried out, the silicon powder collecting device reaches a stable working state after 70-75min, and 50% of cutting particle size of suspension liquid is 70nm when the suspension liquid is stable.
Comparative example 3
Raw material to be separated: the particle size range of the raw silicon powder is 0-600nm, and the median particle size is 300 nm.
When the position of the transducer in the ultrasonic atomization classification device 1 is at the bottom or at the installed angle level, the rest of the components in the device are unchanged, and the silicon powder classification is performed in the manner of example 1.
When the transducer is arranged at the bottom of the ultrasonic atomization grading device 1, after 50-55min, the silicon powder collecting device reaches a stable working state, and 50% of the cutting particle size of the suspension liquid is 180nm when the suspension liquid is stable;
when the transducer is horizontally arranged in the ultrasonic atomization grading device 1, after 50-55min, the mass flow of the suspension liquid in the silicon powder collecting device is kept stable, and 50% of the cutting particle size of the suspension liquid is 240nm when the suspension liquid is stable.
Comparative example 4
Raw material to be separated: the particle size range of the raw silicon powder is 0-600nm, and the median particle size is 300 nm.
N2The outlet was not modified and the tangential inlet was used, the rest of the apparatus being identical to that of example 1. Silicon powder classification was performed as in example 1, the silicon powder material was separated, and it was determined that after 55-60min, the silicon powder collection device reached a steady state operation with 50% of the cut particle size of the suspension at steady state of 70 nm.
Comparative example 5
Raw material to be separated: the particle size range of the raw silicon powder is 0-600nm, and the median particle size is 300 nm.
When the ultrasonic atomization classification device does not have the baffle 140, the rest of the device is the same as the embodiment 1. Silicon powder classification was carried out as in example 1, separating the silicon powder mass, wherein the solution outlet 7 was opened once at 0.5h intervals and the excess suspension was drained off.
Through determination, after 70-75min, the silicon powder collecting device reaches a stable working state, and 50% of the suspension liquid has a cutting particle size of 80nm when the suspension liquid is stable.
Comparative example 6
Raw material to be separated: the particle size range of the raw silicon powder is 0-600nm, and the median particle size is 300 nm.
When the ultrasonic atomization classifying device does not have the baffle 150, the rest of the device is the same as that of the embodiment 1. Silicon powder classification was performed as in example 1, the silicon powder material was separated, and it was determined that after 75-80min, the silicon powder collection device reached a steady state operation with 50% of the cut particle size of the suspension at steady state being 90 nm.
Comparative example 7
Raw material to be separated: the particle size range of the raw silicon powder is 0-600nm, and the median particle size is 300 nm.
When the upper end of the ultrasonic atomizing device 1 is not tapered, the nitrogen gas outlet is discharged from the upper side, and the rest of the device is the same as that of example 1. Silicon powder classification was performed as in example 1, separating the silicon powder material. Through determination, after 55-60min, the silicon powder collecting device reaches a stable working state, and 50% of the suspension liquid has a cutting particle size of 70nm when the suspension liquid is stable.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (14)
1. An ultrasonic atomization grading device of submicron powder is characterized by comprising an ultrasonic atomization device (1), a solution inlet (6), a nitrogen inlet (4), a solution outlet (7), a powder collecting device (2) and a nitrogen outlet (3);
the ultrasonic atomization device (1) is divided into an upper part, a middle part and a lower part, the upper part is conical, the middle part is cylindrical, the lower part is conical or cylindrical, the ultrasonic atomization device (1) comprises transducers (120), reaction tanks (130), partition plates (140) and cylindrical partition plates (150), the transducers (120) and the reaction tanks (130) are arranged on the inner wall of the middle part of the ultrasonic atomization device (1), the number of the transducers (120) and the number of the reaction tanks (130) are 4-6 and are uniformly arranged at the same height of the middle part of the ultrasonic atomization device (1), the reaction tanks (130) are in one-to-one correspondence with the transducers (120), and the reaction tanks (130) are arranged on the periphery of the transducers (120) and have open upper parts; the cylindrical partition plate (150) is vertically fixed in the middle of the ultrasonic atomization device (1) and is coaxial with the ultrasonic atomization device (1), and the bottommost end of the cylindrical partition plate (150) is lower than the highest position of the reaction tank (130); the lower part in the ultrasonic atomization device (1) is provided with a partition plate (140), and the partition plate (140) is provided with a small hole;
the solution inlet (6) is connected with a solution pipeline (8) through a liquid whistle dispersion device (5), and the solution pipeline (8) is connected with the ultrasonic atomization device (1) and extends into the ultrasonic atomization device (1) to be communicated with the bottom of each reaction tank (130); the nitrogen inlet (4) is connected with the ultrasonic atomization device (1) and is positioned below the solution inlet (6); the nitrogen outlet (3) is connected with the top of the ultrasonic atomization device (1) through the powder collecting device (2), and the solution outlet (7) is positioned at the bottom of the ultrasonic atomization device (1).
2. The ultrasonic atomization and classification device for submicron powders according to claim 1, characterized in that the installation angle of the transducer (120) is 60-70 ° with respect to the horizontal plane.
3. An ultrasonic atomization classification device of submicron powders in accordance with claim 1 or 2 characterized by that the nitrogen inlet (4) is installed in the tangential direction with an inclination of 15-20 ° from the horizontal and with a height higher than the highest point of the reaction tank.
4. An ultrasonic atomization classification device of submicron powder according to claim 1 or 2, characterized in that the liquid whistle dispersion device (5) comprises a pipe with a hole plate (520) and a pipe with a reed (540), the two pipes are connected by a flange (530), wherein the hole plate (520) is perpendicular to the pipe with the hole plate (520), the diameter of the hole plate (520) is equal to the inner diameter of the pipe, and the hole plate (520) is provided with a small hole (510); one end of the reed (540) is fixed on the reed mounting piece (550), and the other end can freely vibrate.
5. An ultrasonic atomization classification device of submicron powder according to claim 3, characterized in that the liquid whistle dispersion device (5) comprises a pipe with a hole plate (520) and a pipe with a reed (540), the two pipes are connected by a flange (530), wherein the hole plate (520) is perpendicular to the pipe with the hole plate (520), the diameter of the hole plate (520) is equal to the inner diameter of the pipe, and the hole plate (520) is provided with a small hole (510); one end of the reed (540) is fixed on the reed mounting piece (550), and the other end can freely vibrate.
6. The ultrasonic atomization grading device of submicron powders according to claim 4, characterized in that the free vibrating end of the reed (540) is aligned with the small hole (510).
7. The ultrasonic atomization grading device of submicron powders according to claim 4, characterized in that the width of the free vibrating end of the reed (540) is smaller than the fixed end.
8. The ultrasonic atomization grading device of submicron powders according to claim 6, characterized in that the reed (540) has a smaller width at the free vibrating end than at the fixed end.
9. The ultrasonic atomization and classification device for submicron powders according to any one of claims 1, 2 or 5 to 8, characterized in that the solution outlet (7) is divided into two outlets, one of which is connected to the solution inlet (6) by a pump and the other is connected to the outside.
10. An ultrasonic atomizing classification device for submicron powders in accordance with claim 3 characterized in that said solution outlet (7) is divided into two outlets, one of which is connected to the solution inlet (6) by a pump and the other is connected to the outside.
11. The ultrasonic atomization classification device of submicron powders in accordance with claim 4, characterized in that the solution outlet (7) is divided into two outlets, one of which is connected to the solution inlet (6) by a pump and the other is connected to the outside.
12. A method for classifying submicron powders, characterized in that the method uses the ultrasonic atomization classifying device of submicron powders as any one of claims 1 to 11 as a classifying device, adds water into the powders to be separated to prepare suspension, feeds the suspension from a solution inlet (6), feeds the suspension dispersed by a liquid whistle dispersing device (5) into an ultrasonic atomization device (1), shunts the suspension into each reaction tank (130), under transducer (120) effect, submicron powder and solution are atomized and form the fog, and the fog forms the whirl at the inner wall of ultrasonic atomization device (1) under the nitrogen gas effect, and nitrogen gas drives the fog and discharges and collect submicron powder from ultrasonic atomization device (1) top fast, and unreacted silica flour suspension overflows from reaction tank (130) upper end, finally is discharged by solution outlet (7).
13. The method of classifying submicron powders according to claim 12, wherein said method is: adding water into powder to be separated to prepare suspension, sending the suspension into a solution inlet (6), forming jet flow through a small hole (510) in the middle of a pore plate (520) to impact a reed (540), vibrating the reed (540) to fully disperse the powder in the suspension, enabling the dispersed suspension to enter an ultrasonic atomization device (1), shunting to enter each reaction tank (130), atomizing the submicron powder and the solution to form mist under the action of a transducer (120), meanwhile, enabling nitrogen to enter the ultrasonic atomization device (1) from a nitrogen inlet (4), enabling the mist to form rotational flow in a gas channel formed by the inner wall of the ultrasonic atomization device (1) and a cylindrical partition plate (150) under the action of the nitrogen, driving the mist to be rapidly discharged from the top of the ultrasonic atomization device (1) by the nitrogen, and collecting the submicron silicon powder in the mist by a silicon powder collecting device (2), the rest nitrogen is discharged from a nitrogen outlet (3), and the unreacted silicon powder suspension overflows from the upper end of the reaction tank (130), is discharged through the middle part of the partition plate (140), and is finally discharged from a solution outlet (7).
14. The method for the classification of submicron powders according to claim 13, characterized in that the collection of submicron powders is carried out by liquid nitrogen in the collection device of silicon powders (2).
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JP2003190838A (en) * | 2001-12-28 | 2003-07-08 | Kawasaki Heavy Ind Ltd | Cyclone type fine powder catcher |
CN104690278A (en) * | 2013-12-09 | 2015-06-10 | 青岛平度市旧店金矿 | Novel metal powder processing method through ultrasonic atomization process |
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