CN110272049A - The preparation method and preparation facilities of hollow silicon core - Google Patents
The preparation method and preparation facilities of hollow silicon core Download PDFInfo
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- CN110272049A CN110272049A CN201810220009.1A CN201810220009A CN110272049A CN 110272049 A CN110272049 A CN 110272049A CN 201810220009 A CN201810220009 A CN 201810220009A CN 110272049 A CN110272049 A CN 110272049A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
- C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
- C01B33/035—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process
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Abstract
The present invention provides a kind of preparation method of hollow silicon core, comprising: bulk crystals silicon material is fitted into crucible, is in crucible in seal chamber；Seal chamber, seal pipe and silicon core are cached and are passed through protective gas into seal chamber after indoor air is discharged to maintain the micro-positive pressure environment of three；Crucible is heated, so that the bulk crystals melting silicon materials in it are liquid；Liquid silicon material after making fusing flows downwardly through nozzle ring, to form hollow silicone tube in seal pipe under self gravity and the effect of the pressure of protective gas；Length-measuring appliance, aid device and cutter device is set to be fitted to each other, to carry out linear measure longimetry to hollow silicone tube, and it is all fixed, cuts when hollow silicone tube reaches preset length value from the upward length in lower end every time, and drive downlink to be sent into silicon core and cache room, it loops back and forth like this until preparation process terminates.Correspondingly, a kind of preparation facilities of hollow silicon core is provided.The present invention can efficiently prepare large-diameter hollow silicon core.
Description
Technical field
The present invention relates to technical field of polysilicon production, and in particular to the preparation method and one kind of a kind of hollow silicon core are hollow
The preparation facilities of silicon core.
Background technique
Silicon core is the significant components in reduction furnace production polysilicon process, provides carrier for the deposition of crystalline silicon.Silicon core
Characteristic the sinking speed of crystalline silicon, the energy consumption of reduction furnace are played a crucial role.In general, the diameter of silicon core or transversal
Area is bigger, and deposition velocity is faster, and the time of high-voltage breakdown is shorter, and the energy consumption of production can also reduce relatively.
But inventors have found that round or rectangular solid silicon core for generalling use at present, if its cross section is too
Greatly, then its raw material used will be increase accordingly, and production efficiency can also decline to a great extent, and lead to that the production cost increases, so solid
The sectional area of silicon core is very restricted.
To solve the above problem existing for solid silicon core, hollow silicon core is come into being.Hollow silicon core has cross-sectional area big,
The advantages that raw material usage amount is small can solve many restrictions of the solid silicon core in preparation, use process.Domestic and international Some Enterprises
Exploitation hollow silicon core production technology is begun trying.
However, it is found by the inventors that being prepared although existing hollow silicon core production technology can prepare hollow silicon core
During hollow silicon core, problem low, at high cost that there are still production efficiencys, for example, when preparing hollow silicon core by czochralski method,
Not only production efficiency is low, and energy consumption is high, and high production cost also adds the clustered operation of each component under individual cases, technique is more
It is complicated.
Therefore the hollow silicon core for how efficiently preparing major diameter becomes ability to realize the fast-growth of polycrystalline silicon rod
Field technique personnel are difficult to the technical barrier overcome, and an important factor for limitation production of polysilicon cost.
Summary of the invention
The technical problem to be solved by the present invention is to for the drawbacks described above in the presence of the prior art, providing one kind can
The efficient method for preparing large-diameter hollow silicon core and corresponding preparation facilities.
Solving technical solution used by present invention problem is:
The present invention provides a kind of preparation method of hollow silicon core comprising following steps:
Bulk crystals silicon material is fitted into crucible, is in crucible and its interior silicon material in seal chamber；
By in seal chamber, in the seal pipe that top is connected to seal chamber bottom and top is connected to sealing bottom of the tube
Silicon core is passed through protective gas into seal chamber after caching indoor air discharge to maintain seal chamber, seal pipe and silicon core caching room
Interior micro-positive pressure environment；
Crucible is heated, so that the bulk crystals melting silicon materials in it are liquid；
Liquid crystal silicon material after making fusing flows downwardly through under self gravity and the effect of the pressure of protective gas set on earthenware
Crucible bottom and the nozzle ring extended into seal pipe, to form hollow silicone tube in seal pipe；
Using the length upward from lower end of the hollow silicone tube in length-measuring appliance monitoring seal pipe, and reach in the length
Start the aid device in seal pipe when preset length value with fixation hollow silicone tube lower part, then starts cutter device for hollow silicon
Pipe lower part is cut to conform to the finished product hollow silicon core of the preset length value, and aid device is made to drive finished product hollow after cutting
Silicon core comes downwards in silicon core caching room and places, and then makes to accommodate the reset of device uplink, and the hollow silicone tube in seal pipe
The length upward from lower end is fixed, cuts when reaching preset length value again, and drives downlink to be sent into silicon core and cache room,
It loops back and forth like this until preparation process terminates.
Optionally, by seal chamber, in the seal pipe that top is connected to seal chamber bottom and top and sealing bottom of the tube
The silicon core of connection is passed through protective gas into seal chamber after caching indoor air discharge to maintain seal chamber, seal pipe and silicon core
Cache indoor micro-positive pressure environment specifically:
The seal chamber, seal pipe and silicon core caching room are vacuumized, negative pressure will be evacuated to inside this three, then
It is passed through protective gas into the seal chamber, is stopped until seal chamber, seal pipe and silicon core cache when indoor pressure rises to positive pressure
Only, it repeats and this three vacuumize 1~3 time, finally continue to be passed through protective gas into the seal chamber, to remain close
It seals chamber, seal pipe and silicon core and caches indoor micro-positive pressure environment, until preparation process terminates.
Optionally, crucible is heated specifically: the temperature of crucible is heated to 1400~1500 DEG C.
Optionally, during forming hollow silicone tube in seal pipe, through temperature-adjusting device control in seal pipe
The temperature of the hollow silicone tube formed, to ensure the viscosity of hollow silicone tube.
Optionally, during forming hollow silicone tube in seal pipe, continue to be passed through into it from the top of hollow silicone tube
Inert gas to guarantee the pressure of the hollow silicon pipe orifice drawn, and adjusts inert gas according to the specification requirement of hollow silicone tube
Flow to prepare the hollow silicone tubes of preset diameters and default wall thickness.
Optionally, the preparation method further includes following steps:
After silicon core, which caches indoor finished product hollow silicon core, reaches preset quantity, close between seal pipe and silicon core caching room
Channel；
The outlet of silicon core caching room is opened, by outlet closing after the finished product hollow silicon core to be removed in it；
Displacement preset time is carried out to silicon core caching room using protective gas；
After to the preset time, then open the channel between seal pipe and silicon core caching room.
Optionally, the crystal silicon material is electron level crystal silicon material；The size of the bulk crystals silicon material is not less than 2cm；
The bulk crystals silicon material total amount that single is added to crucible must not exceed the 3/4 of crucible volume, and the protective gas is argon gas.
The present invention also provides a kind of preparation facilities of hollow silicon core comprising seal chamber, top are connected to seal chamber bottom
Seal pipe and the silicon core caching room that be connected to sealing bottom of the tube of top, be placed in the seal chamber and loaded blocky crystalline substance
The bottom of the crucible of body silicon material, the crucible is contacted with the bottom in seal chamber, and the bottom of crucible is equipped with and prolongs into seal pipe
The nozzle ring stretched；
The preparation facilities further includes vacuum evacuation device, protective gas gas source, heating device, seal pipe lower part is arranged in
Length-measuring appliance and cutter device, and the aid device being arranged in seal pipe；
The vacuum evacuation device is used to seal chamber, seal pipe and silicon core caching indoor air and be discharged；
The protective gas gas source is connected to the top of seal chamber, indoor for caching in seal chamber, seal pipe and silicon core
Air discharge after, protective gas is passed through into seal chamber to maintain seal chamber, seal pipe and silicon core to cache indoor micro-positive pressure
Environment；
The heating device is arranged in inside seal chamber, the outside of crucible, for heating to crucible, so that its
Interior bulk crystals melting silicon materials are liquid, and the liquid crystal silicon material after fusing is acted in self gravity and the pressure of protective gas
Under, the nozzle ring set on crucible bottom is flowed downwardly through, to form hollow silicone tube in seal pipe；
The length-measuring appliance is used to monitor the length upward from lower end of the hollow silicone tube in seal pipe, and in the length
Starting aid device when reaching preset length value；The aid device is used for fixing seal under the starting of length-measuring appliance
The lower part of hollow silicone tube in managing, and start cutter device after fixing；The cutter device is used under the starting of aid device
In the finished product hollow silicon core that hollow silicone tube lower part is cut to conform to the preset length value, and start aid after cutting
Device；The aid device is under the starting of cutter device, for driving finished product hollow silicon core to come downwards in silicon core caching room simultaneously
It places, then uplink resets；
The length-measuring appliance, aid device and cutter device are fitted to each other, certainly with the hollow silicone tube in seal pipe
The upward length in lower end is fixed, cuts when reaching preset length value again, and drives downlink to be sent into silicon core and cache room, such as
This moves in circles until preparation process terminates.
Optionally, the vacuum evacuation device is specifically used for take out to the seal chamber, seal pipe and silicon core caching room true
Sky will be evacuated to negative pressure inside this three；To institute when the protective gas gas source is specifically for being in negative pressure inside the three
It states and is passed through protective gas in seal chamber, until seal chamber, seal pipe and silicon core cache stopping when indoor pressure rises to positive pressure；Institute
Vacuum evacuation device is stated to be also used to inside the three that this three vacuumize 1~3 time in repetition when positive pressure；The protection
Gas source is also used to continue at the end of vacuumizing to be passed through protective gas into the seal chamber, to maintain seal chamber, sealing
Pipe and silicon core cache indoor micro-positive pressure environment, until preparation process terminates.
Optionally, the heating device is specifically used for the temperature of crucible being heated to 1400~1500 DEG C.
Optionally, the preparation facilities further includes the temperature-adjusting device that seal pipe top is arranged in, for controlling close
The temperature of the hollow silicone tube formed in tube sealing, to ensure the viscosity of hollow silicone tube.
Optionally, the preparation facilities further includes noble gas source, for continuing from the top of hollow silicone tube into it
It is passed through inert gas, to guarantee the pressure of the hollow silicon pipe orifice drawn, and inertia is adjusted according to the specification requirement of hollow silicone tube
The flow of gas is to prepare the hollow silicone tubes of preset diameters and default wall thickness.
Optionally, the bottom of the crucible is equipped with through-hole, and the outer tube extended in oriented seal pipe is connected in through hole, close
Tube sealing covers in the outside of outer tube and spaced apart, and the middle part of outer tube is equipped with the inner tube for being upward through silicon material in crucible, and outer
Pipe and the gap location of inner pipe wall lower end form the nozzle ring extended in oriented seal pipe.
Optionally, the upper end of said inner tube is connected with the lower end of air supply pipe, and the upper end of air supply pipe passes through the upper of seal chamber
It is connected to after side wall with noble gas source, so that inert gas is successively after air supply pipe and inner tube from the top of hollow silicone tube
In into it.
Optionally, the junction in the sealing bottom of the tube and silicon core caching ceiling portion is equipped with keeping apart in normally open
It closes, the outlet for taking out finished product hollow silicon core, and the lower part or bottom of silicon core caching room is provided on silicon core caching room
It is connected to protective gas gas source, top is connected to the exhaust line for being equipped with one-way cock；The disconnecting switch is used in silicon core
The outlet of caching room is closed when opening, and caches room with isolating seal pipe and silicon core；It is taken out in it from the outlet of silicon core caching room
Finished product hollow silicon core and after closing the outlet, the protective gas gas source, which is also used to cache interior to silicon core, is passed through preset time
Protective gas, with use protective gas to silicon core caching room carry out displacement preset time；The disconnecting switch is also used in institute
It is opened after stating preset time, to open the channel between seal pipe and silicon core caching room.
Optionally, the crystal silicon material is electron level crystal silicon material；The size of the bulk crystals silicon material is not less than 2cm；
The bulk crystals silicon material total amount that single is added to crucible must not exceed the 3/4 of crucible volume；The crucible uses high purity quartz
Crucible or silicon nitride crucible, the protective gas are argon gas；The shape of the nozzle ring is circular rings, Q-RING, triangle
Ring or polygon ring, material are ceramics；The heating method of the heating device is graphite resistance heating or induction heating；It is described to cut
The cutting mode for cutting device is machine cuts or laser cutting；The length-measuring appliance uses laser length detector.
The utility model has the advantages that
1) present invention takes the mode of gravity flow to draw downwards using the gravity of liquid crystal silicon material and the pressure of protective gas
Hollow silicone tube, simple process, hollow silicone tube ratio of briquetting is high, high-efficient；
2) viscosity of hollow silicone tube is adjusted by the way that temperature-adjusting device is arranged on seal pipe top in the present invention, it is ensured that at
Type effect；
3) present invention prevents hollow silicon under high temperature by being continually fed into inert gas inside the hollow silicone tube into seal pipe
The surface of pipe is oxidized, while inert gas also has the function of adjusting temperature, prevents the temperature for stretching out the hollow silicone tube of seal pipe
Du Taigao and violent oxidation reaction occurs with air.
Detailed description of the invention
Fig. 1 is the flow chart for the hollow silicon core preparation method that the embodiment of the present invention 1 provides；
Fig. 2 is the structural schematic diagram for the hollow silicon core preparation facilities that the embodiment of the present invention 2 provides.
In figure: 1- crucible；2- heating device；3- bulk crystals silicon material；4- seal chamber；5- top cover；6- seal chamber
Protective gas inlet line；7- outer tube；8- inner tube；9- nozzle ring；10- air supply pipe；11- inert gas import pipeline；
12- seal pipe；The hollow silicone tube of 13-；14- cutter device；15- temperature-adjusting device；16- length-measuring appliance；17- every
Leave pass；18- silicon core caches room；19- finished product hollow silicon core；20- silicon core caches room outlet；21- silicon core caches room exhaust
Pipeline；22- pressure-detecting device；23- silicon core caches room protective gas inlet line；24- accommodates device.
Specific embodiment
Technical solution in order to enable those skilled in the art to better understand the present invention, with reference to the accompanying drawings and examples to this
Invention is described in further detail.
The low, production cycle for production efficiency existing during using czochralski method to produce hollow silicon core in the prior art
The problems such as length, energy consumption are high, at high cost, the invention proposes the methods that one kind can efficiently prepare large-diameter hollow silicon core, and
Corresponding preparation facilities effectively increases the preparation efficiency of hollow silicon core, and formed product rate is high, and high production efficiency drops significantly
The low production cost of hollow silicon core.It is described in detail below by specific embodiment.
Embodiment 1:
As shown in Figure 1, including the following steps S101 to S108 the present embodiment provides a kind of preparation method of hollow silicon core.
S101. bulk crystals silicon material is fitted into crucible, crucible and its interior silicon material is made to be in seal chamber after charging
It is interior.
The crystal silicon material is electron level crystal silicon material；The size of the bulk crystals silicon material is not less than 2cm；Single is added
Bulk crystals silicon material total amount in crucible must not exceed the 3/4 of crucible volume.
S102. by seal chamber, in the seal pipe that top is connected to seal chamber bottom and top and sealing bottom of the tube connect
After logical silicon core caches indoor air discharge, protective gas is passed through into seal chamber to maintain seal chamber, seal pipe and silicon core
Cache indoor micro-positive pressure environment.
The protective gas is preferably argon gas.
This step specifically: the seal chamber, seal pipe and silicon core caching room are vacuumized, inside this three
It is evacuated to negative pressure, is then passed through protective gas into the seal chamber, until seal chamber, seal pipe and silicon core cache indoor pressure
Stopping when rising to positive pressure repeats and vacuumize 1~3 time to this three, finally continues to be passed through protection into the seal chamber
Gas, to maintain seal chamber, seal pipe and silicon core to cache indoor micro-positive pressure environment, until preparation process terminates.
S103. crucible is heated, so that the bulk crystals melting silicon materials in it are liquid.
In this step, crucible is heated specifically: the temperature of crucible is heated to 1400~1500 DEG C.
S104. the liquid crystal silicon material after making fusing flows downwardly through under self gravity and the effect of the pressure of protective gas
The nozzle ring extended set on crucible bottom and into seal pipe, to form hollow silicone tube in seal pipe.
In this step, during forming hollow silicone tube in seal pipe, it can be controlled and sealed by temperature-adjusting device
The temperature of the hollow silicone tube formed in pipe, to ensure the viscosity of hollow silicone tube.
In this step, during forming hollow silicone tube in seal pipe, it can continue from the top of hollow silicone tube into it
It is passed through inert gas, to guarantee the pressure of the hollow silicon pipe orifice drawn, and inertia is adjusted according to the specification requirement of hollow silicone tube
The flow of gas is to prepare the hollow silicone tubes of preset diameters and default wall thickness.
The inert gas is preferably argon gas.
S105. the length upward from lower end using the hollow silicone tube in length-measuring appliance monitoring seal pipe.
S106. the aid started when the measured value of length-measuring appliance reaches preset length value in seal pipe is filled with fixation
Hollow silicone tube lower part, then starts cutter device.
S107., hollow silicone tube lower part is cut to conform to the finished product hollow silicon of the preset length value using cutter device
Core.
S108. make aid device that finished product hollow silicon core be driven to come downwards in silicon core caching room after cutting and place,
Then make to accommodate the reset of device uplink.
Step S106-S108 is repeated, until preparation process terminates.
In other words, abovementioned steps S105 to S108 specifically: use the hollow silicon in length-measuring appliance monitoring seal pipe
The pipe length upward from lower end, and the aid device when the length reaches preset length value in starting seal pipe is with fixation hollow
Then silicone tube lower part starts the finished product hollow silicon that hollow silicone tube lower part is cut to conform to the preset length value by cutter device
Core makes aid device that finished product hollow silicon core be driven to come downwards in silicon core caching room and places, then makes to accommodate after cutting
Device uplink resets, and when hollow silicone tube in seal pipe reaches preset length value from the upward length in lower end again is consolidated
Fixed, cutting, and drive downlink to be sent into silicon core and cache room, it loops back and forth like this until preparation process terminates.
In addition, as shown in Figure 1, the preparation method may also include the steps of S109-S112.
S109. it after silicon core, which caches indoor finished product hollow silicon core, reaches preset quantity, closes seal pipe and silicon core caches
Channel between room.
S110. the outlet of silicon core caching room is opened, by outlet closing after the finished product hollow silicon core to be removed in it.From
Silicon core caches the finished product hollow silicon core that room is taken out can remove the oxidation film on surface by pickling link, in order to avoid influence later period silicon core
Normal use.
S111. displacement preset time is carried out to silicon core caching room using protective gas.The preset time is 10~30 points
Clock.
S112. to the preset time after, then open seal pipe and silicon core caching room between channel.
After step S112, a production cycle terminates, and needs return step if continuing to produce hollow silicon core
S101。
In conclusion hollow silicon core preparation method described in the present embodiment uses electron level bulk crystals silicon material for raw material, lead to
It crosses heating crucible and crystal silicon material is molten into liquid-state silicon, and liquid-state silicon flows through nozzle ring under the action of gravity and gas pressure
Hollow silicone tube is formed in seal pipe, molding hollow silicone tube carries out length detection by length-measuring appliance, when hollow silicone tube
Length when meeting the requirement of finished product hollow silicon core, hollow silicone tube is cut into the hollow silicon of certain length by starting cutter device
Core, and be sent into silicon core caching room, to complete the preparation of a finished product hollow silicon core, the length to hollow silicone tube reaches again
It is fixed, cuts when preset length value, and drive downlink to be sent into silicon core and cache room, loop back and forth like this until preparation process
Terminate.
Embodiment 2:
As shown in Fig. 2, the present embodiment provides a kind of preparation facilities of hollow silicon core, including seal chamber 4, top and seal chamber
The silicon core caching room 18 that the seal pipe 12 of 4 bottoms connection and top are connected to 12 bottom of seal pipe.Wherein, seal chamber 4 is by pushing up
The cylinder of end opening and the top cover 5 being covered at cartridge openings are constituted.
The crucible 1 for having loaded bulk crystals silicon material 3 is placed in the seal chamber 4, the size of bulk crystals silicon material 3 is not small
In 2cm, 3 total amount of bulk crystals silicon material that single is added to crucible must not exceed the 3/4 of crucible volume；Crystal silicon material is preferably
Electron level crystal silicon material, crucible use high-purity silica pot or silicon nitride crucible.In the bottom of the crucible 1 and seal chamber 4
Bottom contact, and the bottom of crucible 1 is equipped with the nozzle ring 9 extended into seal pipe 12.
Specifically, the bottom of the crucible 1 is equipped with through-hole, and the outer tube extended in oriented seal pipe 12 is connected in through hole
7 (i.e. outer tubes 7 be connected to crucible 1 bottom), 12 sets of seal pipe is in the outside of outer tube 7 and spaced apart, preferably at outer tube 7
In the center of seal pipe 12, the middle part of outer tube 7 is equipped with the inner tube 8 for being upward through silicon material in crucible 1 (i.e. in the insertion of inner tube 8 outer tube 7
Between), and outer tube 7 and the gap location of 8 tube wall lower end of inner tube form the nozzle ring 9 extended in oriented seal pipe 12, thus outside
The drawing nozzle with certain shapes gap is formed between pipe lower end and inner tube lower end.
In the present embodiment, the shape of nozzle ring 9 can be circular rings, Q-RING, triangular loop or polygon ring, material
It can be the ceramic materials such as silicon nitride or corundum.The material of outer tube 7 and inner tube 8 may be the ceramic material such as silicon nitride or corundum
Material.
The preparation facilities further includes vacuum evacuation device (not shown), protective gas gas source (not shown), lazy
Property gas source (not shown), heating device 2, the length-measuring appliance 16 and cutter device that 12 lower part of seal pipe is set
14, the temperature-adjusting device 15 on 12 top of seal pipe is set, and the aid device 24 being arranged in seal pipe 12.
In the present embodiment, protective gas and inert gas are all made of argon gas.Mechanical severing device can be used in cutter device 14
Or laser cutting device, preferably laser cutting device, it is radiated at workpiece surface using high energy laser beam, makes irradiated area
Local melting, gasification, to achieving the purpose that cutting, due to laser cutting be it is contactless, silicone tube itself is rushed without machinery
Pressure not will cause silicone tube fracture.Laser length detector can be used in length-measuring appliance 16.
Wherein, the air that the vacuum evacuation device is used to cache seal chamber 4, seal pipe 12 and silicon core in room 18 is discharged.
The protective gas gas source (not shown) is by being provided with the seal chamber protective gas inlet line 6 of valve and sealing
The protective gas inlet communication of the cylinder upper side wall of chamber 4, for the sky in seal chamber 4, seal pipe 12 and silicon core caching room 18
Gas discharge after, protective gas is passed through into seal chamber 4 with maintain seal chamber 4, seal pipe 12 and silicon core caching room 18 in it is micro- just
Pressure ring border.
Specifically, the vacuum evacuation device is used to take out to the seal chamber 4, seal pipe 12 and silicon core caching room 18 true
Sky will be evacuated to negative pressure inside this three；To described close when the protective gas gas source is for being in negative pressure inside the three
It is passed through protective gas in envelope chamber 4, until stopping when the pressure in seal chamber 4, seal pipe 12 and silicon core caching room 18 rises to positive pressure；
The vacuum evacuation device is also used to inside the three vacuumize 1~3 time (preferably to this three in repetition when positive pressure
3 times)；The protective gas gas source is also used to continue at the end of vacuumizing to be passed through protective gas into the seal chamber 4, with dimension
The micro-positive pressure environment in seal chamber 4, seal pipe 12 and silicon core caching room 18 is held, until preparation process terminates.
The heating device 2 is arranged in inside seal chamber 4, the outside of crucible 1 has for heating to crucible 1
Body is to be heated to 1400~1500 DEG C, so that the bulk crystals silicon material 3 in it is molten into liquid.Liquid crystal silicon material after fusing
Under self gravity and the effect of the pressure of protective gas, the nozzle ring 9 set on 1 bottom of crucible is flowed downwardly through, thus sealing
Hollow silicone tube 13 is formed in pipe 12.
In the present embodiment, the heating method of heating device 12 can be graphite (C/C) resistance heating or induction heating.
During forming hollow silicone tube 13, temperature-adjusting device 15 for control formed in seal pipe 12 it is hollow
The temperature of silicone tube 13, to ensure the viscosity of hollow silicone tube 13.In the present embodiment, the heating method of temperature-adjusting device 15 is using electricity
Heating or radiant heating, preferably radiant heating.
During forming hollow silicone tube 13, noble gas source is used to continue from the top of hollow silicone tube 13 into it
It is passed through inert gas, to guarantee the pressure of 13 inner hole of hollow silicone tube drawn, and is adjusted according to the specification requirement of hollow silicone tube 13
The flow of inert gas is to prepare the hollow silicone tubes 13 of preset diameters and default wall thickness.
Specifically, the upper end of inner tube 8 is connected with the lower end of air supply pipe 10 by flange, and the upper end of air supply pipe 10 is across close
It is connected to by being provided with the inert gas import pipeline 11 of valve with noble gas source after sealing the cylinder upper side wall of chamber 4,
So that inert gas successively enters in it after air supply pipe 10 and inner tube 8 from the top of hollow silicone tube 13, guarantee to pull out empty
The pressure of heart silicone tube inner hole, convenient for adjusting the diameter and wall thickness that pull out hollow silicone tube, moreover it is possible under the fixed function of air supply pipe 10
Inner tube 8 is set to be placed in the center of outer tube 7.
The length-measuring appliance 16 is used to monitor hollow silicone tube 13 in seal pipe 12 length upward from lower end, and
Starting aid device 24 when the length reaches preset length value, for example, when the lower end of hollow silicone tube is by length-measuring appliance
After portion's detection mouth, length-measuring appliance starts to measure hollow silicon length of tube；The aid device 24 is filled in linear measure longimetry
It sets under 16 starting, for the lower part of silicone tube 13 hollow in fixing seal pipe 12, and starts cutter device 14 after fixing；Institute
Cutter device 14 is stated under the starting of aid device 24, for hollow 13 lower part of silicone tube to be cut to conform to the preset length value
Finished product hollow silicon core 19, and after cutting starting aid device 24；Aid the opening in cutter device 14 of device 24
Under dynamic, for driving finished product hollow silicon core 19 to come downwards in silicon core caching room 18 and placing, then uplink resets.
As it can be seen that silicon core caching room 18 is for storing finished product hollow silicon core 19.Device 24 is accommodated to remove with aid and unclamp function
Other than energy, also have the function of to move up and down, can be moved between seal pipe 12 and silicon core caching room 18, to realize cutting process
In hollow silicone tube 13 fixation, and cutting after by finished product hollow silicon core 19 be delivered to silicon core caching room 18 in.
The length-measuring appliance 16, aid device 24 and cutter device 14 are fitted to each other, with the sky in seal pipe 12
Heart silicone tube 13 is fixed when reaching preset length value again from the upward length in lower end, cuts, and downlink is driven to be sent into silicon
Core caches room 18, loops back and forth like this until preparation process terminates.
In addition, the junction at 18 top of 12 bottom of seal pipe and silicon core caching room is equipped with the disconnecting switch in normally open
17；Appropriate position on silicon core caching room 18 is provided with the outlet 20 for taking out finished product hollow silicon core 19, and silicon core caches room
18 lower part or bottom cache room protective gas inlet line 23 and protective gas gas source by being provided with the silicon core of valve
Connection；The top of silicon core caching room 18 caches chamber gas outlet line 21 with the silicon core for being equipped with one-way cock and is connected to, single due to being equipped with
To valve, gas can only cache room 18 from silicon core and flow out from inside to outside, avoid air from entering silicon core by exhaust line 21 and cache room
In 18；Silicon core caching is additionally provided with pressure-detecting device 22 on room 18.The disconnecting switch 17 is used for going out in silicon core caching room
Mouth 20 is closed when opening, and caches room 18 with isolating seal pipe 12 and silicon core；Silicon core caching room outlet 20 take out its at
Product hollow silicon core 19 and close it is described outlet 20 during, air can by outlet 20 scurry into silicon core cache room 18 in, therefore
After the outlet 18 of silicon core caching room is closed, the protective gas gas source, which is also used to cache in room 18 to silicon core, is passed through preset time
Protective gas, to use protective gas to carry out displacement preset time to silicon core caching room 18, the preset time is 10~30
Minute；The disconnecting switch 17 is also used to open after the preset time, caches room to open seal pipe 12 and silicon core
Channel between 18 then proceedes to prepare hollow silicone tube.
As it can be seen that the preparation process of above-mentioned hollow silicon core preparation facilities may be summarized to be charging, material, drawing silicon core, output
Product and the big step of pickling five, are described in detail below.
A charging
High-purity bulk crystals silicon material is fitted into crucible, the size of block material is not less than 2cm, the dress of single crystal silicon material
Entering amount must not exceed at the 3/4 of crucible volume, and after charging, the top cover of seal chamber is installed, so that crucible and its interior
Silicon material is in seal chamber, and checks that leakproofness is good, then opens the valve in vacuum lines, negative by being evacuated in system
Pressure, then the valve in seal chamber protective gas inlet line is opened, it is passed through protective gas to system, when the pressure in system rises
When to positive pressure, the valve in protective gas inlet line is closed, the valve in vacuum lines is closed after repeating vacuum pumping 3 times
Door is continued to be passed through protective gas into seal cavity with positive pressure environment in maintenance system by protective gas inlet line, be prevented
Air is scurried into seal pipe.
B material
The heating device on the outside of crucible is opened, the temperature of crucible is heated to 1400~1500 DEG C, so that in crucible
Crystal silicon material is molten into liquid.
C drawing silicon core
Liquid silicon material after fusing enters the gap between inner and outer pipes under the effect of the pressure of gravity and protective gas,
Hollow silicone tube is formed by nozzle ring downwards, the temperature of hollow silicone tube is controlled by the temperature-adjusting device on seal pipe top,
To ensure the viscosity of hollow silicone tube, the valve on inert gas import pipeline is opened, by air supply pipe to leading to inside hollow silicone tube
Enter inert gas, while different rulers are prepared according to the inert gas flow that the specification requirement of hollow silicone tube adjustment flows through air supply pipe
Very little and thickness hollow silicone tube.During drawing hollow silicone tube, protection gas is continually fed into seal chamber, it can be ensured that sealing
Chamber, seal pipe and silicon core cache indoor micro-positive pressure environment, prevent air anti-channeling.Certainly, brilliant by being added constantly into crucible
Body silicon material can continuous output hollow silicon core.
D output product
Enter in seal pipe by the hollow silicone tube that nozzle ring is formed, when the lower end of hollow silicone tube is filled by linear measure longimetry
After setting upper detection mouth, length-measuring appliance starts to measure hollow silicon length of tube, when the length of hollow silicone tube reaches pre-
If length value, that is, when meeting product requirement, hollow silicone tube lower part is fixed in the starting of aid device in seal pipe, cutter device with
Start, hollow silicone tube is cut into the finished product hollow silicon core of certain length, device is accommodated after cutting and drives finished product hollow
Silicon core comes downwards in silicon core caching room, and finished product hollow silicon core is put into silicon core caching room, and then, aid device goes upward to sealing
It is resetted in pipe, repeats silicone tube next time and fix.
After silicon core, which caches indoor finished product hollow silicon core, reaches certain amount, close between seal pipe and silicon core caching room
Disconnecting switch, open silicon core caching room outlet, finished product hollow silicon core is taken out, be then shut off silicon core caching room outlet, open
Silicon core caches the valve in room protective gas inlet line, carries out displacement 10min to caching room, turns off the room protection of silicon core caching
Then valve on gas feed pipeline opens the disconnecting switch between silicon core caching room and seal pipe.
E pickling
When the temperature for the finished product hollow silicon core taken out from silicon core caching room is too high, exposure is easy in air in silicon core table
Face forms oxidation film, influences the normal use of later period silicon core, it is therefore desirable to pickling is carried out to finished product hollow silicon core, to remove finished product
The oxidation film on hollow silicon core surface.Wherein, pickling solution can be 10-20% hydrofluoric acid solution or hydrochloric acid solution.
It is understood that the principle that embodiment of above is intended to be merely illustrative of the present and the exemplary implementation that uses
Mode, however the present invention is not limited thereto.For those skilled in the art, essence of the invention is not being departed from
In the case where mind and essence, various changes and modifications can be made therein, these variations and modifications are also considered as protection scope of the present invention.
Claims (16)
1. a kind of preparation method of hollow silicon core, which comprises the steps of:
Bulk crystals silicon material is fitted into crucible, is in crucible and its interior silicon material in seal chamber；
By in seal chamber, in the seal pipe that top is connected to seal chamber bottom and top and the silicon core that is connected to of sealing bottom of the tube
Protective gas is passed through into seal chamber to maintain seal chamber, seal pipe and silicon core caching indoor after caching indoor air discharge
Micro-positive pressure environment；
Crucible is heated, so that the bulk crystals melting silicon materials in it are liquid；
Liquid crystal silicon material after making fusing flows downwardly through under self gravity and the effect of the pressure of protective gas set on crucible bottom
Portion and the nozzle ring extended into seal pipe, to form hollow silicone tube in seal pipe；
Using the length upward from lower end of the hollow silicone tube in length-measuring appliance monitoring seal pipe, and reach default in the length
Start the aid device in seal pipe when length value with fixation hollow silicone tube lower part, then starting cutter device will be under hollow silicone tube
Portion is cut to conform to the finished product hollow silicon core of the preset length value, makes to accommodate device drive finished product hollow silicon core after cutting
It comes downwards in silicon core caching room and places, then make to accommodate the reset of device uplink, and the hollow silicone tube in seal pipe is under
It holds upward length to be fixed, cut when reaching preset length value again, and drives downlink to be sent into silicon core and cache room, so
It moves in circles until preparation process terminates.
2. preparation method according to claim 1, which is characterized in that by seal chamber, top is connected to seal chamber bottom
Seal pipe in and top cached after indoor air is discharged with the silicon core that be connected to of sealing bottom of the tube and be passed through guarantor into seal chamber
Shield gas is to maintain seal chamber, seal pipe and silicon core to cache indoor micro-positive pressure environment specifically:
The seal chamber, seal pipe and silicon core caching room are vacuumized, negative pressure will be evacuated to inside this three, then to institute
It states and is passed through protective gas in seal chamber, until seal chamber, seal pipe and silicon core cache stopping when indoor pressure rises to positive pressure, then
Repeat this three vacuumize 1~3 time, finally continue to be passed through protective gas into the seal chamber, with maintain seal chamber,
Seal pipe and silicon core cache indoor micro-positive pressure environment, until preparation process terminates.
3. preparation method according to claim 1, which is characterized in that heat to crucible specifically:
The temperature of crucible is heated to 1400~1500 DEG C.
4. preparation method according to claim 1, which is characterized in that during forming hollow silicone tube in seal pipe,
By the temperature for the hollow silicone tube that temperature-adjusting device control is formed in seal pipe, to ensure the viscosity of hollow silicone tube.
5. preparation method according to claim 1, which is characterized in that during forming hollow silicone tube in seal pipe,
Continue to be passed through inert gas into it from the top of hollow silicone tube, with the pressure for the hollow silicon pipe orifice that guarantee is drawn, and according to
The specification requirement of hollow silicone tube adjusts the flow of inert gas to prepare the hollow silicone tube of preset diameters and default wall thickness.
6. preparation method according to claim 1, which is characterized in that the preparation method further includes following steps:
After silicon core, which caches indoor finished product hollow silicon core, reaches preset quantity, close logical between seal pipe and silicon core caching room
Road；
The outlet of silicon core caching room is opened, by outlet closing after the finished product hollow silicon core to be removed in it；
Displacement preset time is carried out to silicon core caching room using protective gas；
After to the preset time, then open the channel between seal pipe and silicon core caching room.
7. preparation method according to claim 1 to 6, which is characterized in that the crystal silicon material is that electron level is brilliant
Body silicon material；The size of the bulk crystals silicon material is not less than 2cm；The bulk crystals silicon material total amount to crucible is added in single must not
More than the 3/4 of crucible volume, the protective gas is argon gas.
8. a kind of preparation facilities of hollow silicon core, which is characterized in that the sealing being connected to including seal chamber, top with seal chamber bottom
The silicon core that pipe and top are connected to sealing bottom of the tube caches room, is placed in the seal chamber and has loaded bulk crystals silicon material
Crucible, the bottom of the crucible contacts with the bottom in seal chamber, and the bottom of crucible is equipped with the ring extended into seal pipe
Shape nozzle；
The preparation facilities further includes vacuum evacuation device, protective gas gas source, heating device, the length that seal pipe lower part is arranged in
Measuring device and cutter device, and the aid device being arranged in seal pipe；
The vacuum evacuation device is used to seal chamber, seal pipe and silicon core caching indoor air and be discharged；
The protective gas gas source is connected to the top of seal chamber, for caching indoor sky in seal chamber, seal pipe and silicon core
After gas discharge, protective gas is passed through into seal chamber to maintain seal chamber, seal pipe and silicon core to cache indoor micro-positive pressure environment；
The heating device is arranged in inside seal chamber, the outside of crucible, for heating to crucible, so that in it
Bulk crystals melting silicon materials are liquid, liquid crystal silicon material after fusing under self gravity and the effect of the pressure of protective gas,
The nozzle ring set on crucible bottom is flowed downwardly through, to form hollow silicone tube in seal pipe；
The length-measuring appliance is used to monitor the length upward from lower end of the hollow silicone tube in seal pipe, and reaches in the length
Starting aid device when preset length value；The aid device is under the starting of length-measuring appliance, in fixing seal pipe
The lower part of hollow silicone tube, and start cutter device after fixing；For the cutter device under the starting of aid device, being used for will
Hollow silicone tube lower part is cut to conform to the finished product hollow silicon core of the preset length value, and starting aid dress after cutting
It sets；The aid device is under the starting of cutter device, for driving finished product hollow silicon core to come downwards in silicon core caching room and pacifying
It puts well, then uplink resets；
The length-measuring appliance, aid device and cutter device are fitted to each other, with the hollow silicone tube in seal pipe from lower end
Upward length is fixed when reaching preset length value again, cuts, and drives downlink to be sent into silicon core and cache room, so follows
Ring is back and forth until preparation process terminates.
9. preparation facilities according to claim 8, which is characterized in that the vacuum evacuation device is specifically used for the sealing
Chamber, seal pipe and silicon core caching room are vacuumized, and will be evacuated to negative pressure inside this three；The protective gas gas source is specifically used
It is passed through protective gas into the seal chamber when inside the three being in negative pressure, until seal chamber, seal pipe and silicon core are slow
Deposit stopping when indoor pressure rises to positive pressure；The vacuum evacuation device is also used to inside the three repeat in when positive pressure to this
Three vacuumize 1~3 time；The protective gas gas source is also used to continue at the end of vacuumizing to lead into the seal chamber
Enter protective gas, to maintain seal chamber, seal pipe and silicon core to cache indoor micro-positive pressure environment, until preparation process terminates.
10. preparation facilities according to claim 8, which is characterized in that the heating device is specifically used for the temperature of crucible
Degree is heated to 1400~1500 DEG C.
11. preparation facilities according to claim 8, which is characterized in that further include the temperature tune that seal pipe top is arranged in
Regulating device, for controlling the temperature of the hollow silicone tube formed in seal pipe, to ensure the viscosity of hollow silicone tube.
12. preparation facilities according to claim 8, which is characterized in that further include noble gas source, be used for from hollow silicon
The top of pipe continues to be passed through inert gas into it, to guarantee the pressure of the hollow silicon pipe orifice drawn, and according to hollow silicone tube
Specification requirement adjustment inert gas flow to prepare the hollow silicone tubes of preset diameters and default wall thickness.
13. preparation facilities according to claim 12, which is characterized in that the bottom of the crucible is equipped with through-hole, and logical
The outer tube extended in oriented seal pipe, outside and spaced apart, the middle part of outer tube of the sealed tube in outer tube are connected at hole
Equipped with the inner tube for being upward through silicon material in crucible, and outer tube and the gap location of inner pipe wall lower end form in oriented seal pipe and extend
Nozzle ring.
14. preparation facilities according to claim 13, which is characterized in that the lower end phase of the upper end of said inner tube and air supply pipe
Even, and the upper end of air supply pipe is connected to after the upper side wall of seal chamber with noble gas source, so that inert gas successively passes through
Enter in it after crossing air supply pipe and inner tube from the top of hollow silicone tube.
15. preparation facilities according to claim 8, which is characterized in that the sealing bottom of the tube and silicon core cache ceiling portion
Junction be equipped with the disconnecting switch in normally open, silicon core caching is provided on room for taking out finished product hollow silicon core
Outlet, and the lower part of silicon core caching room or bottom are connected to protective gas gas source, top and the exhaust for being equipped with one-way cock
Pipeline connection；The disconnecting switch is used to close when the outlet of silicon core caching room is opened, and is cached with isolating seal pipe and silicon core
Room；After taking out the finished product hollow silicon core in it from the outlet of silicon core caching room and close the outlet, the protective gas gas source
It is also used to cache the protective gas that interior is passed through preset time to silicon core, to use protective gas to replace silicon core caching room
Preset time；The disconnecting switch is also used to open after the preset time, caches room to open seal pipe and silicon core
Between channel.
16. the preparation facilities according to any one of claim 8-15, which is characterized in that the crystal silicon material is electron level
Crystal silicon material；The size of the bulk crystals silicon material is not less than 2cm；The bulk crystals silicon material total amount to crucible is added not in single
Obtain 3/4 more than crucible volume；The crucible uses high-purity silica pot or silicon nitride crucible, and the protective gas is argon gas；
The shape of the nozzle ring is circular rings, Q-RING, triangular loop or polygon ring, and material is ceramics；The heating device
Heating method be graphite resistance heat or induction heating；The cutting mode of the cutter device is that machine cuts or laser are cut
It cuts；The length-measuring appliance uses laser length detector.
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| CN116607207A (en) * | 2023-07-20 | 2023-08-18 | 山东豪迈机械制造有限公司 | Manufacturing equipment and manufacturing method of tubular silicon core |
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Application publication date: 20190924 Assignee: Xinte silicon based new materials Co.,Ltd. Assignor: XINTE ENERGY Co.,Ltd. Contract record no.: X2022990000325 Denomination of invention: Preparation method and device of hollow silicon core Granted publication date: 20210302 License type: Common License Record date: 20220627 Application publication date: 20190924 Assignee: Inner Mongolia Xinte silicon material Co.,Ltd. Assignor: XINTE ENERGY Co.,Ltd. Contract record no.: X2022990000326 Denomination of invention: Preparation method and device of hollow silicon core Granted publication date: 20210302 License type: Common License Record date: 20220627 |