CN115636415B - Polysilicon acid washing impurity removing equipment and impurity removing method - Google Patents
Polysilicon acid washing impurity removing equipment and impurity removing method Download PDFInfo
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- CN115636415B CN115636415B CN202211327763.8A CN202211327763A CN115636415B CN 115636415 B CN115636415 B CN 115636415B CN 202211327763 A CN202211327763 A CN 202211327763A CN 115636415 B CN115636415 B CN 115636415B
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- 239000002253 acid Substances 0.000 title claims abstract description 112
- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 80
- 229920005591 polysilicon Polymers 0.000 title claims abstract description 58
- 239000012535 impurity Substances 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000005406 washing Methods 0.000 title claims description 34
- 230000002378 acidificating effect Effects 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 9
- 238000005554 pickling Methods 0.000 claims description 107
- 239000000463 material Substances 0.000 claims description 66
- 238000005243 fluidization Methods 0.000 claims description 65
- 238000005520 cutting process Methods 0.000 claims description 55
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- 238000006243 chemical reaction Methods 0.000 claims description 21
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- 230000000903 blocking effect Effects 0.000 claims description 14
- 238000007873 sieving Methods 0.000 claims description 12
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- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
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Abstract
The invention provides polysilicon acid cleaning and impurity removing equipment and an impurity removing method, which solve the problems of polysilicon acidic impurity residues and the like. The invention has the advantages of good impurity removing effect, stable structure and the like.
Description
Technical Field
The invention belongs to the technical field of polysilicon recovery, and particularly relates to polysilicon acid washing impurity removing equipment.
Background
Polycrystalline silicon is a form of elemental silicon, and when molten elemental silicon solidifies under supercooling conditions, silicon atoms are arranged in the form of diamond lattices into a number of crystal nuclei, which if grown into grains with different crystal face orientations, combine to crystallize into polycrystalline silicon. The polycrystalline silicon wafer has obvious polycrystalline characteristics relative to the monocrystalline silicon wafer. The existing polysilicon recovery generally needs to remove quartz, metal ions and the like on the surface of a silicon material, firstly uses alkali liquor to remove quartz and the like, then uses acid mixed liquor to carry out acid washing, is soaked to be neutral by deionized water flushing liquor, and finally is dried and stored in a classified mode. However, in the actual treatment process, the conventional pickling impurity removal equipment has poor temperature control effect on the pickling process, and cannot ensure that metal impurities are fully reacted and dissolved. In addition, in the actual pickling impurity removal process, when the equipment is continuously fed, the internal acidity cannot be regulated, so that the metal impurities react unevenly, and more impurities still exist in silicon material particles at the bottom of the equipment.
In order to solve the defects existing in the prior art, long-term exploration is performed, and various solutions are proposed. For example, chinese patent literature discloses an acid cleaning and impurity removal method, apparatus, and polysilicon purification method, system [200910177449.4], comprising the steps of: slowing down the cooling process of discharging the metallurgical silicon, and selecting a plurality of acids to carry out acid washing operation on the silicon powder according to a certain sequence after the cooled metallurgical silicon is crushed into silicon powder with a certain granularity.
The problem that the internal temperature control effect of equipment is poor in the pickling process is solved to a certain extent by the scheme, but the scheme still has a plurality of defects, such as excessive impurity residues of silicon materials positioned at the bottom of the equipment.
Disclosure of Invention
The invention aims to solve the problems and provides polysilicon acid pickling impurity removal equipment which is reasonable in design and capable of effectively reducing impurity residues of bottom silicon materials.
Another object of the present invention is to provide a polysilicon acid cleaning and impurity removing method with good impurity removing effect, aiming at the above problems.
In order to achieve the above purpose, the present invention adopts the following technical scheme: the utility model provides a polycrystalline silicon pickling edulcoration equipment, includes crushing subassembly, crushing subassembly is connected with the pickling box, and the built-in heating element of pickling box has a plurality of independent pickling chambeies in the pickling box, installs centrifugal sieve material subassembly and with the fluidization component who sets up in the pickling intracavity respectively in the pickling chamber, and the pickling box is equipped with automatic acid supplementing subassembly and temperature and pressure balance subassembly. After the polycrystalline silicon fragments are crushed, the silicon particles are conducted into the acid washing cavity, the fluidization component drives the particles to flow and fully react with the acid liquor, uneven reaction caused by sedimentation of the silicon is avoided, the temperature and pressure balance component maintains the temperature and pressure in the acid washing cavity to be constant, and the reaction rate of metal impurities is ensured.
In the above-mentioned polycrystalline silicon pickling edulcoration equipment, smash the subassembly and include smashing the barrel, smash barrel entrance and be provided with one-way feed assembly, smash barrel exit and be provided with and carry the material subassembly, smash barrel inside and set up cutting assembly and grinding assembly. The crushing component further crushes the crushed flaky polycrystalline silicon to obtain the particle diameter meeting the fluidization reaction.
In the polysilicon acid washing impurity removing device, the cutting assembly comprises a cutting motor, and the cutting motor is in transmission connection with the cutting blade through the synchronous transmission assembly; the synchronous transmission assembly comprises a transmission gear and a transmission toothed ring which are concentrically arranged, a plurality of driven gears which are symmetrically arranged opposite to the center of the transmission gear and the transmission toothed ring are meshed and transmitted between the transmission gear and the transmission toothed ring, the driven gears are connected with the cutting blade, the transmission gear is connected with a plurality of reversing gears which are meshed and transmitted, and the reversing gears are connected with the transmission toothed ring through a driving gear and a cutting motor; the cutting blade is discoid and the upper end is provided with relative central symmetry and is the cutting protruding of triangle form, and the cutting blade is provided with the sawtooth along circumference, smashes the inside toper boss that is used for rotating installation cutting blade that is provided with of barrel, and cutting blade bottom is provided with the conical surface that covers in the toper boss outside. The plurality of cutting blades synchronously rotate to break the hard polycrystalline silicon wafer, so that the subsequent grinding is convenient.
In the polysilicon acid cleaning and impurity removing equipment, the grinding assembly comprises a grinding chamber arranged below the cutting assembly, a plurality of grinding disks which are arranged in a superimposed manner are rotatably arranged in the grinding chamber, leak holes are uniformly distributed in the grinding disks, grinding particle layers are distributed on one sides, opposite to the adjacent grinding disks, of the grinding disks, and a spray head for spraying grinding aid is arranged in the grinding chamber. The grinding aid is continuously sprayed in the grinding process to realize wet grinding, and silicon material particles after grinding are adhered to each other, so that the floating in the transmission process is avoided.
In the polysilicon acid washing impurity removing device, the unidirectional feeding assembly comprises a feeding hole arranged at the upper end of the crushing cylinder, the upper end of the crushing cylinder is provided with a feeding box body, the inside of the feeding box body is divided into a plurality of independent feeding cavities by a baffle plate which is obliquely arranged, one side of the feeding cavity is provided with an opening and closing hole opposite to the inner feeding cavity, the opening and closing hole is closed by a plurality of opening and closing plates which are connected in a sliding way, and a step-by-step discharging assembly is arranged between one end of the feeding box body and the feeding hole; the step-by-step discharging assembly comprises discharging guide rails arranged on two sides of the feeding hole, the discharging guide rails are respectively and slidably provided with discharging sliding blocks, the discharging guide rails extend to the upper part of the crushing cylinder, the discharging sliding blocks are rotationally connected with the feeding box body, a baffle strip for blocking the opening and closing plate from falling into the crushing cylinder is arranged at the edge opening of the feeding hole, a discharging motor is arranged at the upper end of the crushing cylinder body, a discharging gear is fixed at the output end of the discharging motor, and a discharging rack meshed with the discharging gear is arranged on the outer side of the feeding box body; the material lifting assembly comprises a material lifting barrel which is obliquely arranged, a material lifting screw rod is arranged in the material lifting barrel, and the material lifting screw rod is in transmission connection with a material lifting motor through a coupler. The unidirectional feeding component is used for controlling the feeding quantity and is matched with the centrifugal screening component to obtain the optimal screening effect.
In the polysilicon pickling impurity-removing equipment, the pickling tank body comprises a main tank body and a tank cover for sealing the upper end of the main tank body, the pickling cavities are equidistantly arranged in the main tank body and are covered with an acid-resistant surface layer, and the pickling cavities are mutually separated through a sealing component; the sealing assembly comprises a sealing plugboard arranged on the inner side of the box cover, the sealing plugboard is arranged between the pickling cavities, heat insulation layers are respectively arranged in the sealing plugboard and the pickling box, oppositely arranged sealing grooves are formed between the main box body and the side opening of the box cover, alkaline liquid is filled in the sealing grooves, and the main box body and the box cover are pressed and fixed through lock catches. The pickling box body has good sealing performance and heat preservation effect, acid liquor leakage and heat dissipation are effectively avoided, the box cover is opened to take materials, and the requirement of mass polysilicon acid washing is met.
In the polysilicon acid washing impurity removing equipment, the centrifugal material sieving component comprises a material sieving cylinder, wherein a screen is uniformly distributed on the material sieving cylinder, the material sieving cylinder is in transmission connection with the centrifugal driving component, a material blocking cylinder is arranged around the material sieving cylinder, and a material guiding component is arranged inside the material sieving cylinder; the material guiding component comprises material guiding plates which are spirally and uniformly arranged on the inner side of the material sieving cylinder, and the material guiding plates are provided with base plates which are mutually overlapped and are opposite to the center of the material sieving cylinder; the centrifugal driving assembly comprises a driving rod connected with the center of the screen cylinder, and the driving rod is in transmission connection with the servo motor; the material blocking cylinder is cone-shaped, and the diameter of the upper end of the material blocking cylinder is smaller than that of the lower end of the material blocking cylinder. After the granular silicon materials are conducted into the centrifugal screen material component, the granular silicon materials are uniformly distributed into the acid washing cavity under the centrifugal action, and the residual large-grain silicon materials are ground secondarily.
In the polysilicon pickling impurity-removing equipment, the fluidization component comprises a fluidization pipe coiled at the bottom of the pickling cavity, an upward fluidization nozzle is arranged on the surface of the fluidization pipe, a one-way valve is arranged between the fluidization nozzle and the fluidization pipe, and a dispersion pipe is reserved on the fluidization nozzle; the dispersing pipe comprises a main pipe connected with the fluidization nozzle and a branched pipe obliquely downward, and the branched pipe is symmetrically arranged relative to the center of the main pipe; the automatic acid supplementing assembly comprises an acid supplementing pipe communicated with the fluidization pipe, an evaporation tank and an acid supplementing pump are externally connected with the acid supplementing pipe, an electric heating coil pipe is mounted on the inner wall of the evaporation tank in a fitting mode, a pressure regulating valve is mounted on the acid supplementing pipe, and PH sensors are respectively arranged in the acid supplementing pipe and the acid washing cavity. The fluidization component is arranged at the bottom of the pickling cavity to avoid silicon material deposition, and is matched with the automatic acid supplementing component to continuously supply acid to the pickling cavity to ensure the impurity removal rate.
In the polysilicon pickling impurity removing device, the heating assembly comprises a heating pipe communicated with the inside of the pickling cavity, the heating pipe is externally connected with a heating box, and an electric heating pipe and a circulating fan are arranged in the heating box; the temperature and pressure balance assembly comprises a pressure relief pipe communicated with the pickling cavity, the pressure relief pipe is externally connected with a pressure relief pump and a neutralization tank, and a temperature sensor and a pressure sensor are arranged in the pickling cavity. The temperature in the pickling tank body rises, the reaction rate of acidic substances rises along with the rise of the reaction rate, and the temperature and pressure balance assembly timely discharges pressure to maintain the internal pressure within a specified range.
The polysilicon acid washing impurity removing method comprises the following steps:
s1: crushing and grinding the polycrystalline silicon fragments by utilizing a crushing assembly;
s2: the crushed polysilicon powder is input into an acid washing box body and uniformly dispersed into each acid washing cavity by a centrifugal screening component;
s3: the fluidization component is led in acid steam towards the pickling cavity to carry out fluidization reaction;
s4: the heating component and the temperature and pressure balancing component feed back to adjust the temperature and pressure in the pickling cavity;
s5: the temperature and pressure balance component pumps the inside of the pickling cavity and leads out redundant acidic substances;
s6: and drying and guiding the polysilicon powder after pickling by a heating assembly and a fluidization assembly. Compared with the conventional impurity removal method, the method combines the fluidization reaction with the acidic impurity removal, ensures that the silicon material at the bottom fully reacts with the acid liquor, further reduces the residue of metal impurities, and improves the recovery effect of the polysilicon silicon material.
Compared with the prior art, the invention has the advantages that: continuously supplementing acid in the fluidization reaction process, so that silicon material impurities in the acid washing cavity maintain a higher reaction rate, and the impurity removal effect is improved; the temperature-pressure balance component maintains the internal temperature and pressure of the pickling tank body to be constant, and ensures that the internal pickling substances are maintained to be in a fog state and fully contact and react with impurities; the polycrystalline silicon fragments are crushed before the reaction, so that the subsequent transmission processing is convenient.
Drawings
FIG. 1 is a schematic view of the comminution assembly of the present invention;
FIG. 2 is a cross-sectional view of the construction of the shredder assembly of the present invention;
FIG. 3 is a partial cross-sectional view of the cutting assembly of the present invention;
FIG. 4 is a partial cross-sectional view of the unidirectional feed assembly of the present invention;
FIG. 5 is a schematic view of the structure of the stripping assembly of the present invention;
FIG. 6 is a structural cross-sectional view of the pickling tank of the present invention;
FIG. 7 is a partial cross-sectional view of the centrifugal screen assembly of the present invention;
FIG. 8 is a partial cross-sectional view of the fluidization assembly of the present invention;
FIG. 9 is a partial cross-sectional view of the pickling tank of the present invention;
in the drawing the view of the figure, crushing assembly 1, crushing cylinder 11, unidirectional feed assembly 12, feed port 121, feed box 122, baffle 123, feed chamber 124, open-close port 125, open-close plate 126, feed assembly 13, cutting assembly 14, cutting motor 141, cutting blade 142, drive gear 143, drive gear ring 144, driven gear 145, reversing gear 146, drive gear 147, cutting projection 148, tapered boss 149, grinding assembly 15, grinding chamber 151, grinding disk 152, leak 153, abrasive particle layer 154, progressive discharge assembly 16, discharge guide 161, discharge slide 162, barrier 163, discharge motor 164, discharge gear 165, discharge rack 166, feed cylinder 167, feed screw 168, leak hole 153, abrasive particle layer 154, progressive discharge assembly 16, discharge motor 164, discharge motor 165, discharge motor 167, discharge motor 168, and feed screw 168 the material lifting motor 169, the acid washing box 2, the main box 21, the box cover 22, the sealing plugboard 23, the sealing groove 24, the lock catch 25, the heating component 3, the heating pipe 31, the heating box 32, the electric heating pipe 33, the circulating fan 34, the acid washing cavity 4, the centrifugal material sieving component 5, the material sieving cylinder 51, the screen 52, the material blocking cylinder 53, the material guiding plate 54, the base plate 55, the driving rod 56, the servo motor 57, the fluidization component 6, the fluidization pipe 61, the fluidization nozzle 62, the dispersing pipe 63, the main pipe 64, the branch pipe 65, the acid supplementing pipe 66, the evaporation tank 67, the acid supplementing pump 68, the electric heating coil 69, the pressure regulating valve 691, the automatic acid supplementing component 7, the temperature and pressure balancing component 8, the pressure releasing pipe 81, the pressure releasing pump 82 and the neutralization tank 83.
Detailed Description
The invention will be described in further detail with reference to the drawings and the detailed description.
As shown in fig. 1 and 6, a polysilicon acid cleaning and impurity removing device comprises a crushing assembly 1, wherein the crushing assembly 1 is arranged on an automatic production line, and polysilicon fragments are introduced into the inside of the crushing assembly by adopting an automatic transmission or manual transmission mode for crushing treatment. The crushing assembly 1 is connected with an acid washing box body 2 for carrying out closed acid washing treatment on polysilicon particles. The heating component 3 is arranged in the pickling tank body 2 to heat the inside, so that the reaction rate of metal impurities and acid liquor is accelerated, meanwhile, the evaporation of the acid liquor is accelerated after pickling is finished, and the acid liquor residue on the surface of the silicon material is reduced. The inside of the pickling box body 2 is provided with a plurality of independent pickling cavities 4, which can work synchronously or asynchronously, and polysilicon particles are conveyed into each pickling cavity 4 for independent pickling. The centrifugal screening component 5 and the fluidization component 6 arranged in the pickling cavity 4 are respectively arranged in the pickling cavity 4, polysilicon particles in the pickling cavity 4 are in a suspension motion state in the fluidization component 6, and the particles cannot be scattered due to the closed structure of the pickling cavity 4. The pickling tank 2 is equipped with an automatic acid replenishing assembly 7 and a temperature and pressure balancing assembly 8. The common acid liquor comprises hydrofluoric acid, nitric acid and acetic acid, the proportion of the acid liquor is selected according to different metal impurity contents, when the PH value in the acid washing cavity 4 is higher than a preset value, the automatic acid supplementing component 7 automatically supplements acid to reduce the PH value, and the temperature and pressure balance component 8 feed back to adjust the temperature and pressure in the acid washing cavity 4.
As shown in fig. 2, unlike the conventional crushing apparatus, the crushing assembly 1 comprises a closed crushing cylinder 11, and a unidirectional feeding assembly 12 is arranged at the inlet of the crushing cylinder 11 to avoid the ejection of crushed pieces in the crushing process. The outlet of the crushing cylinder 11 is provided with a lifting assembly 13 for lifting and conveying the polysilicon particles, and the processed polysilicon particles are directly conducted into the pickling tank 2. The cutting assembly 14 and the grinding assembly 15 are arranged in the crushing cylinder 11 to perform double crushing treatment on the flaky polycrystalline silicon until the particle diameter meets the fluidization reaction requirement.
As can be seen from fig. 3, the cutting assembly 14 includes a cutting motor 141, the cutting motor 141 being drivingly connected to the cutting blade 142 by a synchronous drive assembly, the synchronous drive assembly providing a relatively large circumferential rotational speed for the cutting blade 142; the synchronous transmission assembly comprises a transmission gear 143 and a transmission gear ring 144 which are concentrically arranged, a plurality of driven gears 145 which are symmetrically arranged opposite to the center of the transmission gear 143 and the transmission gear ring 144 are meshed and transmitted, the driven gears 145 are connected with the cutting blade 142, the transmission gear 143 is connected with a plurality of reversing gears 146 which are meshed and transmitted, and the reversing gears 146 and the transmission gear ring 144 are connected with the cutting motor 141 through a driving gear 147; the reversing gear 146 does not change the transmission ratio of the driven gears 145, and the reversing gear 146, the transmission gear ring 144 and the driving gear 147 are synchronously meshed for transmission, so that each driven gear 145 and the cutting blade 142 connected with the driven gear 145 have good rotation stability; the cutting blade 142 is formed in a disc shape and is provided at an upper end thereof with a cutting protrusion 148 symmetrical with respect to the center thereof and formed in a triangular shape, the cutting blade 142 is provided with serrations in a circumferential direction, and the cutting blade 142 is rotated at a high speed to crush the polycrystalline silicon wafer into fine fragments. The crushing cylinder 11 is provided inside with a tapered boss 149 for rotatably mounting the cutting blade 142, and the bottom of the cutting blade 142 is provided with a tapered surface covering the outside of the tapered boss 149. The tapered bosses 149 overlap each other to prevent debris from entering the rotational connection of the cutting blade 142 and the tapered bosses 149.
Further, the crushed polysilicon fragments can be directly subjected to acid washing or further ground to increase the contact area with acid liquor. The grinding assembly 15 comprises a grinding chamber 151 which is arranged below the cutting assembly 14 and is independent relative to the cutting assembly 14, a plurality of grinding disks 152 which are arranged in a superimposed manner are rotatably arranged in the grinding chamber 151, the grinding disks 152 are in transmission connection with the cutting motor 141, and reversing gear sets are arranged between adjacent grinding disks 152 to realize synchronous rotation and opposite rotation directions. The grinding disc 152 is uniformly provided with the leak holes 153, and the polysilicon fragments fall into the leak holes 153 and are broken along with the rotation of the grinding disc 152. An abrasive particle layer 154 is disposed on the opposite side of the adjacent grinding disc 152 for increasing the coefficient of friction, and a nozzle for spraying grinding aid is installed in the grinding chamber 151. Grinding aid is injected into the grinding chamber 151, so that the adhesion degree of polysilicon particles can be improved and fine particles can be prevented from being scattered besides the auxiliary grinding of polysilicon fragments.
As can be seen from fig. 4, since the crushing assembly 1 continuously feeds and crushes, the single feeding amount is controlled by the unidirectional feeding assembly 12, so that the crushing unevenness caused by excessive silicon material in the crushing cylinder 11 is avoided. The unidirectional feeding assembly 12 comprises a feeding hole 121 arranged at the upper end of the crushing cylinder 11, a feeding box 122 is arranged at the upper end of the crushing cylinder 11, and the feeding box 122 indirectly feeds the crushing cylinder 11. The interior of the feeding box 122 is divided into a plurality of independent feeding cavities 124 by obliquely arranged baffles 123, one side of each feeding cavity 124 is provided with an opening and closing opening 125 opposite to the inner feeding cavity 124, and the opening and closing opening 125 is closed by a plurality of opening and closing plates 126 which are connected in a sliding manner. Polysilicon fragments are placed into the feed box 122, after which the opening and closing plate 126 completely closes the opening and closing opening 125.
In addition, a step-by-step discharging assembly 16 is arranged between one end of the feeding box 122 and the feeding hole 121; the progressive discharging assembly 16 includes discharging guide rails 161 symmetrically disposed at both sides of the feed inlet 121, the discharging guide rails 161 are slidably provided with discharging sliders 162, and the sliding track of the discharging sliders 162 is limited by the discharging guide rails 161. The discharging guide rail 161 extends above the crushing cylinder 11, the discharging slide block 162 is rotatably connected with the feeding box 122, and the feeding box 122 can rotate from a horizontal state to a vertical state, and then is slidably inserted into the feeding hole 121.
The side opening of the feed port 121 is provided with a stopper bar 163 that blocks the opening and closing plate 126 from falling into the pulverizing cylinder 11, and when the feed port 121 is vertically lowered, the opening and closing plate 126 is housed one by one and opens the opening and closing plate 125 under the restriction of the stopper bar 163. The upper end of the crushing cylinder 11 is provided with a discharging motor 164 to drive the feeding box 122 to turn over and vertically lift, the output end of the discharging motor 164 is fixedly provided with a discharging gear 165, and the outer side of the feeding box 122 is provided with a discharging rack 166 which is meshed with the discharging gear 165 for transmission. When the discharge gear 165 is rotated by the discharge motor 164, the feed box 122 is slidably inserted into the feed port 121. As shown in fig. 5, the material lifting assembly 13 comprises a material lifting cylinder 167 which is obliquely arranged, a material lifting screw 168 is installed in the material lifting cylinder 167, and the material lifting screw 168 is in transmission connection with a material lifting motor 169 through a coupling. The lower end of the lifting cylinder 167 is communicated with the bottom of the crushing cylinder 11, and the slurry mixed with the grinding aid and the polysilicon is conducted to the next processing platform.
In addition, unlike the conventional pickling mode, the closed pickling tank 2 is adopted to improve the acid liquor utilization rate. The pickling tank 2 includes a main tank 21 and a tank cover 22 closing the upper end of the main tank 21, and the main tank 21 and the tank cover 22 are opened and closed by lifting or turning. The pickling cavities 4 are equidistantly arranged in the main box body 21, and the inner side of the pickling cavities is covered with an acid-resistant surface layer to avoid corrosion inside the pickling box body 2. The pickling cavities 4 are separated from each other by the sealing assembly, so that the reaction effect of metal impurities in each pickling cavity 4 is conveniently detected, and the acid injection quantity and the temperature are timely adjusted; the sealing assembly comprises a sealing plugboard 23 arranged on the inner side of the box cover 22, the sealing plugboard 23 further improves the sealing effect of the box cover 22 and the main box body 21, the sealing plugboard 23 is arranged between the pickling cavities 4, heat insulation layers are respectively arranged inside the sealing plugboard 23 and inside the pickling box body 2, oppositely arranged sealing grooves 24 are formed between the side openings of the main box body 21 and the box cover 22, alkaline liquid is injected into the sealing grooves 24 to prevent pollution to the outside caused by acid steam loss, and the main box body 21 and the box cover 22 are tightly pressed and fixed through lock catches 25 so that the main box body 21 can bear larger internal pressure.
In fig. 6, a centrifugal screen assembly 5 is integrally installed inside a tank cover 22, the centrifugal screen assembly 5 comprises a screen material cylinder 51, a screen mesh 52 is uniformly distributed on the screen material cylinder 51 so that silicon material particles are uniformly dispersed into an acid washing cavity 4, and the screen material cylinder 51 is in transmission connection with a centrifugal driving assembly to provide centrifugal driving torque for the screen material cylinder 51. A blocking cylinder 53 is arranged around the screen cylinder 51 to limit scattered particles and concentrate the scattered particles into the pickling chamber 4. A material guiding component is arranged inside the screen material cylinder 51; the guide assembly includes a guide plate 54 uniformly arranged inside the screen cylinder 51 in a spiral shape, and polysilicon particles are blocked by the guide plate 54 during the falling process inside the screen cylinder 51 so as to be uniformly guided out from the surface of the screen 52. The guide plate 54 has a base plate 55 overlapped with each other and opposed to the center of the screen cylinder 51, the base plate 55 being opposed to an inlet located at the top of the screen cylinder 51; the centrifugal driving assembly comprises a driving rod 56 in transmission connection with the center of the screen cylinder 51, and the driving rod 56 is in transmission connection with a servo motor 57; the material blocking cylinder 53 is cone-shaped, and the diameter of the upper end of the material blocking cylinder 53 is smaller than that of the lower end. The servo motor 57 drives the driving rod 56 to rotate, and the toothed ring meshed with the driving rod 56 is arranged at the upper end of the screen material cylinder 51, so that normal feeding of the center of the upper end of the screen material cylinder 51 is not affected.
It can be seen that the fluidization assembly 6 as shown in fig. 8 comprises a fluidization tube 61 coiled at the bottom of the pickling chamber 4, the fluidization tube 61 being externally connected to an air injection line, and the injection of acid vapor through the fluidization tube 61 has a higher reaction rate than conventional acid solutions. The surface of the fluidization pipe 61 is provided with upward fluidization nozzles 62, the fluidization nozzles 62 are arranged at the bottom of the pickling cavity 4 in a matrix, and a one-way valve is arranged between the fluidization nozzles 62 and the fluidization pipe 61 to ensure that the fluidization nozzles 62 jet air unidirectionally. The fluidization jets 62 leave a dispersion tube 63; the dispersing pipe 63 comprises a main pipe 64 connected with the fluidization nozzle 62 and a branched pipe 65 inclined downwards, wherein the branched pipe 65 is arranged symmetrically relative to the center of the main pipe 64 and used for guiding steam to be transmitted to the bottom of the pickling chamber 4, so that uneven reaction caused by deposition of part of polysilicon particles on the bottom of the pickling chamber 4 is avoided.
The automatic acid supplementing assembly 7 and the fluidization pipe 61 share the fluidization nozzle 62, the automatic acid supplementing assembly 7 comprises an acid supplementing pipe 66 communicated with the fluidization pipe 61, the fluidization pipe 61 can be filled with hydrofluoric acid and nitric acid to integrally adjust the internal PH value except for high-temperature steam to improve the reaction rate of metal impurities, and the acid liquor ratio is adjusted for different metal impurities. The acid supplementing pipe 66 is externally connected with the evaporation tank 67 and the acid supplementing pump 68, the electric heating coil 69 is attached to the inner wall of the evaporation tank 67, acid liquid is injected into the evaporation tank 67, and acid gas is generated under the heating action of the electric heating coil 69. The acid supplementing pipe 66 is provided with a pressure regulating valve 691, and PH sensors are respectively arranged on the acid supplementing pipe 66 and the acid washing cavity 4. The pressure regulating valve 691 maintains the constant pressure in the acid replenishing pipe 66, and the PH sensor feeds back and regulates the PH value in the pickling chamber 4.
As is apparent from fig. 9, the heating assembly 3 comprises a heating pipe 31 communicated with the interior of the pickling chamber 4, and an isolating layer and a heat conducting layer are arranged between the heating pipe 31 and the pickling chamber 4 to indirectly heat the interior of the pickling chamber 4. The heating pipe 31 is externally connected with a heating box 32, an electric heating pipe 33 and a circulating fan 34 are arranged in the heating box 32; the temperature and pressure balance assembly 8 comprises a pressure relief pipe 81 communicated with the pickling cavity 4, the pressure relief pipe 81 is externally connected with a pressure relief pump 82 and a neutralization tank 83, and a temperature sensor and a pressure sensor are arranged inside the pickling cavity 4. The pressure release pipe 81 discharges the excess gas from the inside, and the neutralization tank 83 stores a high-concentration alkaline solution therein to neutralize acidic substances.
The polysilicon acid washing impurity removing method comprises the following steps:
s1: crushing and grinding the polycrystalline silicon fragments by using a crushing assembly 1;
s2: the crushed polysilicon powder is input into the pickling box body 2 and uniformly dispersed into each pickling cavity 4 by the centrifugal screening component 5;
s3: the fluidization component 6 is led into the acid washing cavity 4 by acid steam for fluidization reaction;
s4: the heating component 3 and the temperature and pressure balance component 8 feed back to adjust the temperature and pressure in the pickling cavity 4;
s5: the temperature and pressure balance component 8 pumps the inside of the pickling cavity 4 and leads out redundant acidic substances;
s6: the polysilicon powder after the pickling is dried by the heating unit 3 and the fluidizing unit 6 and is discharged.
Example 1
The crushing assembly 1 crushes and grinds the polycrystalline silicon fragments, then the polycrystalline silicon particles are guided into the pickling tank body 2, the fluidization assembly 6 is filled with acid steam, the polycrystalline silicon particles float under the fluidization effect, and metal impurities on the surface react with acid substances.
And then high-temperature steam is introduced into the fluidization component 6 to remove acid and rinse the surface of the polysilicon, the redundant solution is led out through the temperature-pressure balance component 8, the pickling tank 2 is opened after the acidic substances in the pickling tank 2 are completely led out, and the polysilicon particles after the impurity removal is completed are led out.
Example two
The structure, principle, implementation steps and implementation steps of the embodiment are similar to those of the embodiment, except that the centrifugal screen material component 5 in the embodiment centrifugally separates polysilicon particles led into the pickling tank body 2, larger polysilicon fragments are suspended in the pickling cavity 4 by the centrifugal screen material component 5, and when the pickling cavity 4 is filled with acid gas, the centrifugal screen material component 5 drives the polysilicon fragments to rotate at a high speed, so that the polysilicon fragments and metal impurities on the surfaces of the polysilicon fragments are in contact reaction with acid liquor.
Example III
The structure, principle, implementation steps and implementation steps of the embodiment are similar to those of the embodiment, and the difference is that the fluidization component 6 and the automatic acid supplementing component 7 in the embodiment are matched to continuously inject acid steam towards the acid washing cavity 4, after the reaction is completed, the surface of the polysilicon particles is washed by the temperature and pressure balancing component 8, then the interior of the acid washing box 2 is heated by the heating component 3, and meanwhile, the fluidization component 6 continuously injects high-temperature air to keep the interior polysilicon particles in a boiling state, so that the interior moisture is fully evaporated, and drier polysilicon particles are obtained.
In summary, the principle of this embodiment is as follows: the crushing assembly 1 further crushes the polycrystalline silicon fragments and guides the crushed polycrystalline silicon fragments into the acid washing cavity 4, the fluidization assembly 6 keeps polycrystalline silicon particles in a suspension state, the automatic acid supplementing assembly 7 introduces acid steam to react with metal impurities on the surfaces of the polycrystalline silicon particles, and the temperature and pressure balancing assembly 8 keeps the internal temperature and pressure constant, so that the metal impurities and the acidic substances have higher reaction rate.
The specific embodiments described herein are offered by way of example only to illustrate the spirit of the invention. Those skilled in the art may make various modifications or additions to the described embodiments or substitutions thereof without departing from the spirit of the invention or exceeding the scope of the invention as defined in the accompanying claims.
Although the pulverizing assembly 1, pulverizing bowl 11, unidirectional feed assembly 12, feed port 121, feed box 122, baffle 123, feed cavity 124, open and close port 125, open and close plate 126, lifter assembly 13, cutting assembly 14, cutting motor 141, cutting blade 142, drive gear 143, drive ring 144, driven gear 145, reversing gear 146, drive gear 147, cutting projection 148, tapered boss 149, grinding assembly 15, grinding chamber 151, grinding disk 152, leak 153, abrasive particle layer 154, progressive discharge assembly 16, discharge rail 161, discharge slide 162, barrier 163, discharge motor 164, discharge gear 165, discharge rack 166, lifter bowl 167, and grinding wheel assembly a lifting screw 168, a lifting motor 169, a pickling tank 2, a main tank 21, a tank cover 22, a sealing plugboard 23, a sealing groove 24, a lock catch 25, a heating component 3, a heating pipe 31, a heating tank 32, an electric heating pipe 33, a circulating fan 34, a pickling chamber 4, a centrifugal screen component 5, a screen cylinder 51, a screen 52, a baffle cylinder 53, a guide plate 54, a base plate 55, a driving rod 56, a servo motor 57, a fluidization component 6, a fluidization pipe 61, a fluidization nozzle 62, a dispersion pipe 63, a main pipe 64, a branch pipe 65, a acid supplementing pipe 66, an evaporation tank 67, an acid supplementing pump 68, an electric heating coil 69, a pressure regulating valve 691, an automatic acid supplementing component 7, a temperature-pressure balancing component 8, a pressure releasing pipe 81, a pressure releasing pump 82, a neutralization tank 83 and the like, but does not exclude the possibility of using other terms. These terms are used merely for convenience in describing and explaining the nature of the invention; they are to be interpreted as any additional limitation that is not inconsistent with the spirit of the present invention.
Claims (6)
1. The utility model provides a polycrystalline silicon pickling edulcoration equipment, includes crushing subassembly (1), crushing subassembly (1) be connected with pickling box (2), pickling box (2) built-in heating element (3), its characterized in that, pickling box (2) inside have a plurality of independent pickling chambeies (4), pickling chambeies (4) install centrifugal sieve material subassembly (5) respectively and with set up fluidization subassembly (6) in pickling chambeies (4), pickling box (2) be equipped with automatic acid supplementing subassembly (7) and temperature and pressure balance subassembly (8); the pickling box body (2) comprises a main box body (21) and a box cover (22) for sealing the upper end of the main box body (21), the pickling cavities (4) are equidistantly arranged in the main box body (21) and are covered with an acid-resistant surface layer, and the pickling cavities (4) are separated from each other through a sealing assembly; the sealing assembly comprises sealing plugboards (23) arranged on the inner side of the box cover (22), the sealing plugboards (23) are arranged between the pickling cavities (4), heat insulation layers are respectively arranged in the sealing plugboards (23) and the pickling box body (2), sealing grooves (24) which are oppositely arranged are formed between the main box body (21) and the edge opening of the box cover (22), alkaline liquid is injected into the sealing grooves (24), and the main box body (21) and the box cover (22) are tightly fixed through lock catches (25); the centrifugal screen material component (5) comprises a screen material cylinder (51), wherein a screen mesh (52) is uniformly distributed on the screen material cylinder (51), the screen material cylinder (51) is in transmission connection with the centrifugal driving component, a material blocking cylinder (53) is arranged around the screen material cylinder (51), and a material guiding component is arranged inside the screen material cylinder (51); the material guiding assembly comprises material guiding plates (54) which are spirally and uniformly arranged on the inner side of the material sieving cylinder (51), and the material guiding plates (54) are provided with base plates (55) which are mutually overlapped and are opposite to the center of the material sieving cylinder (51); the centrifugal driving assembly comprises a driving rod (56) in transmission connection with the center of the screen cylinder (51), and the driving rod (56) is in transmission connection with a servo motor (57); the material blocking cylinder (53) is cone-shaped, and the diameter of the upper end of the material blocking cylinder (53) is smaller than that of the lower end; the fluidization assembly (6) comprises a fluidization pipe (61) coiled at the bottom of the pickling cavity (4), upward fluidization nozzles (62) are arranged on the surface of the fluidization pipe (61), one-way valves are arranged between the fluidization nozzles (62) and the fluidization pipe (61), and a dispersion pipe (63) is reserved on the fluidization nozzles (62); the dispersing pipe (63) comprises a main pipe (64) connected with the fluidization nozzle (62) and a branched pipe (65) which is inclined downwards, and the branched pipe (65) is arranged symmetrically relative to the center of the main pipe (64); the automatic acid supplementing assembly (7) comprises an acid supplementing pipe (66) communicated with the fluidization pipe (61), the acid supplementing pipe (66) is externally connected with an evaporation tank (67) and an acid supplementing pump (68), an electric heating coil pipe (69) is attached to the inner wall of the evaporation tank (67), a pressure regulating valve (691) is arranged on the acid supplementing pipe (66), and a PH sensor is arranged in each of the acid supplementing pipe (66) and the acid washing cavity (4); the heating assembly (3) comprises a heating pipe (31) communicated with the inside of the pickling cavity (4), the heating pipe (31) is externally connected with a heating box (32), and an electric heating pipe (33) and a circulating fan (34) are arranged in the heating box (32); the temperature and pressure balance assembly (8) comprises a pressure relief pipe (81) communicated with the pickling cavity (4), the pressure relief pipe (81) is externally connected with a pressure relief pump (82) and a neutralization tank (83), and a temperature sensor and a pressure sensor are arranged in the pickling cavity (4).
2. The polysilicon acid cleaning and impurity removing device according to claim 1, wherein the crushing assembly (1) comprises a crushing cylinder (11), a unidirectional feeding assembly (12) is arranged at the inlet of the crushing cylinder (11), a lifting assembly (13) is arranged at the outlet of the crushing cylinder (11), and a cutting assembly (14) and a grinding assembly (15) are arranged inside the crushing cylinder (11).
3. A polysilicon acid cleaning and impurity removing device according to claim 2, wherein the cutting assembly (14) comprises a cutting motor (141), and the cutting motor (141) is in transmission connection with the cutting blade (142) through a synchronous transmission assembly; the synchronous transmission assembly comprises a transmission gear (143) and a transmission toothed ring (144) which are concentrically arranged, a plurality of driven gears (145) which are symmetrically arranged relative to the center of the transmission gear (143) and the transmission toothed ring (144) are meshed and transmitted, the driven gears (145) are connected with a cutting blade (142), the transmission gear (143) is connected with a plurality of reversing gears (146) which are meshed and transmitted, and the reversing gears (146) and the transmission toothed ring (144) are connected with a cutting motor (141) through a driving gear (147); the utility model provides a cutting blade (142) be discoid and upper end be provided with relative center symmetry and be cutting protruding (148) of triangle form, cutting blade (142) be provided with the sawtooth along circumference, crushing barrel (11) inside be provided with conical boss (149) that are used for rotating installation cutting blade (142), cutting blade (142) bottom be provided with the conical surface that covers in conical boss (149) outside.
4. A polysilicon acid cleaning and impurity removing device according to claim 3, wherein the grinding assembly (15) comprises a grinding chamber (151) arranged below the cutting assembly (14), a plurality of grinding discs (152) which are arranged in a superimposed manner are rotatably arranged in the grinding chamber (151), leakage holes (153) are uniformly distributed in the grinding discs (152), grinding particle layers (154) are distributed on the opposite sides of the adjacent grinding discs (152), and a spray head for spraying grinding aid is arranged in the grinding chamber (151).
5. The polysilicon acid cleaning and impurity removing device according to claim 2, wherein the unidirectional feeding component (12) comprises a feeding hole (121) arranged at the upper end of the crushing cylinder (11), a feeding box body (122) is arranged at the upper end of the crushing cylinder (11), the inside of the feeding box body (122) is divided into a plurality of independent feeding cavities (124) by a baffle plate (123) which is obliquely arranged, an opening and closing hole (125) opposite to the inner feeding cavities (124) is formed in one side of the feeding cavities (124), the opening and closing hole (125) is closed by a plurality of opening and closing plates (126) which are connected in a sliding mode, and a step-by-step discharging component (16) is arranged between one end of the feeding box body (122) and the feeding hole (121); the progressive discharging assembly (16) comprises discharging guide rails (161) arranged on two sides of a feeding hole (121), discharging guide rails (161) are respectively and slidably provided with discharging sliding blocks (162), the discharging guide rails (161) extend to the upper part of the crushing cylinder body (11), the discharging sliding blocks (162) are rotationally connected with a feeding box body (122), a blocking strip (163) for blocking an opening and closing plate (126) to fall into the crushing cylinder body (11) is arranged at the edge of the feeding hole (121), a discharging motor (164) is arranged at the upper end of the crushing cylinder body (11), a discharging gear (165) is fixed at the output end of the discharging motor (164), and a discharging rack (166) meshed with the discharging gear (165) is arranged on the outer side of the feeding box body (122); the lifting assembly (13) comprises a lifting cylinder (167) which is obliquely arranged, a lifting screw (168) is mounted in the lifting cylinder (167), and the lifting screw (168) is in transmission connection with a lifting motor (169) through a coupler.
6. A method for pickling and removing impurities from polysilicon, which adopts the polysilicon pickling and removing equipment as set forth in any one of claims 1 to 5, and is characterized by comprising the following steps:
s1: crushing and grinding the polycrystalline silicon fragments by utilizing a crushing assembly (1);
s2: the crushed polysilicon powder is input into an acid washing box body (2) and is evenly dispersed into each acid washing cavity (4) by a centrifugal screening component (5);
s3: the fluidization component (6) is led into acid steam towards the pickling cavity (4) for fluidization reaction;
s4: the heating component (3) and the temperature and pressure balance component (8) feed back to adjust the internal temperature and pressure of the pickling cavity (4);
s5: the temperature and pressure balance component (8) pumps the inside of the pickling cavity (4) and leads out redundant acidic substances;
s6: the polysilicon powder after the pickling is dried by a heating component (3) and a fluidization component (6) and is led out.
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| CN101597063A (en) * | 2008-06-06 | 2009-12-09 | 佳科太阳能硅(厦门)有限公司 | The removal method of boron impurities in metallurgical silicon |
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