CN106115709A - A kind of polycrystalline reduction method - Google Patents
A kind of polycrystalline reduction method Download PDFInfo
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- CN106115709A CN106115709A CN201610465438.6A CN201610465438A CN106115709A CN 106115709 A CN106115709 A CN 106115709A CN 201610465438 A CN201610465438 A CN 201610465438A CN 106115709 A CN106115709 A CN 106115709A
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- chassis
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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
Abstract
A kind of method of polycrystalline reduction, uses following polycrystalline silicon reducing furnace；Reduction furnace includes that chassis and body of heater, described body of heater are the top on chassis, and body of heater is the cylindric reaction chamber adding spherical top；Chassis is discoid, and raw material gas inlet and offgas outlet are distributed on chassis, uniform 30 50 pairs of electrodes on chassis, described half electrode homogeneous vertical on chassis is installed, second half electrode is interspersed for vertically-mounted electrode on lifting electrode, with chassis, and the bottom of lifting electrode is far from chassis 3 10cm；The upper end position of lifting electrode is concordant with spherical top intersection with cylindric；On the circumference of the different radii that raw material gas inlet and offgas outlet are distributed on chassis, when the circumference of a radius arranges raw material gas inlet, the circumference of adjacent radius is arranged offgas outlet；Being provided with temperature sensor in the plan-position, upper end of lifting electrode, the flow controlling unstripped gas makes the temperature of sensor reach 910 935 DEG C.
Description
One, technical field
The present invention relates to a kind of at polycrystalline silicon reducing furnace and the method that carries out polycrystalline reduction.
Two, background technology
The technique of production of polysilicon has the most in the world: improved Siemens, silane thermal decomposition process and fluidized bed process.Wherein improve west
MENZI method is the main technique of current production of polysilicon, the 80% of the Liang Zhan world production of polysilicon total amount of its production polysilicon,
The most important equipment of this process is polycrystalline silicon reducing furnace, and its reduction power consumption exceedes the total power consumption of whole polysilicon production process 60%.
Therefore, the fluidal texture in reduction furnace is carried out in-depth study, and then the Novel reducing furnace of exploitation low energy consumption has important
Science and practical value.
In traditional polycrystalline-silicon reducing furnace structure, the import of its unstripped gas and offgas outlet are distributed on chassis, this knot
Structure require nozzle of air supply is set, additionally must control induction air flow ratio reach sufficiently large could realize to reduction furnace top area mixing
The renewal of gas, the shortcoming of this structure maximum is to easily cause reduction furnace top area to produce dead band, owing to top gas can not get
Effectively updating, therefore top area can produce district of localized hyperthermia, and district of this localized hyperthermia can cause the generation of silica flour, and silica flour is very
Being readily adhered to reduction furnace internal face, reduce reduction furnace inner surface heat radiant reflectance, ultimately resulting in reduction power consumption increases.
Novel reducing furnace offgas outlet after existing improvement is distributed on top, and in solving tradition reduction furnace, local temperature is high
Problem, it is to avoid produce silica flour in reduction furnace, tentatively solves the problem that reduction power consumption is too high.But offgas outlet is distributed on top
Structure reduction control on need.
The chassis of reducing furnace electrode improved divides the arrangement of 3 circumference, the silicon rod on each circumference all in arranged in regular hexagon shape, from
Center have the most successively 3 to, 3 to, 6 to equally distributed electrode；Maximum between the most adjacent two electrodes in Novel reducing furnace chassis
Spacing is 220mm；The most adjacent three pairs of silicon rods all constitute a regular hexagon, and each orthohexagonal central distribution an air inlet
Mouthful, its air inlet sum is 13.
In Novel polysilicon reduction furnace, gaseous mixture is essentially all and flows up along silicon rod surface, and this is due to more
Near silicon rod surface, its temperature is the highest, and density is the lowest；Additionally on reduction furnace axial direction, there is also temperature difference, this temperature
Degree difference also makes reactor produce density contrast in the axial direction, and polycrystalline silicon reducing furnace indexes difference rush in the density of varying cross-section plane
Make gaseous mixture from chassis air inlet mouth to the flat push type flowing taking over a business gas outlet.
But the raw material gas inlet of conventional multi-crystalline silicon reduction furnace and offgas outlet are distributed on chassis, this structural requirement is arranged
Nozzle of air supply, additionally must control induction air flow ratio and reach the sufficiently large renewal that could realize reduction furnace top area gaseous mixture,
Therefore the flowing in reduction furnace is substantially complete mixing flow, is the flowing of forced convertion, its axially and radially density contrast on direction
Hinder gaseous mixture on the contrary to flow to the gas outlet on chassis.Make the Density Distribution newer type reduction furnace in tradition reduction furnace more equal
Even.The turnover gas mode of tradition reduction furnace is also easy to cause raw material to make short circuit leave with rage so that unstripped gas not sufficiently reactive just directly from
Gas outlet is discharged, and causes the waste of unstripped gas, affects the sedimentation rate of polysilicon.Relatively new and old reduction furnace, Novel reducing furnace
There is the temperature difference become apparent from Temperature Distribution on the axial direction of reduction furnace, this is due in Novel polysilicon reduction furnace
Flow field is flat push type flowing, and this type of flow can control each position in reduction furnace by the operating condition changing reduction furnace
The temperature put, controlled Temperature Distribution can control the generation of silica flour in reduction furnace, it is to avoid silica flour is because being attached to reduction furnace
Destroy the burnishing surface of reduction furnace inwall on internal face, the burnishing surface of reduction furnace internal face can be preserved for a long time, add inwall
In the face of the thermal-radiating reflection of high temperature silicon rod, thus reduce the reduction power consumption of reduction furnace；And the flow field in tradition reduction furnace is complete
Mixed flow, its Temperature Distribution is more uniform, and this type of flow can not efficiently control the temperature in reduction furnace, therefore in reduction furnace
Easily producing localized high temperature regions, this localized high temperature regions can produce silica flour, and silica flour is readily adhered to reduction furnace inwall
The surface in face, causes the generation of reduction furnace internal face localized hyperthermia's point, and this localized hyperthermia's point can cause again the attached of more silica flour
, finally destroy the burnishing surface of reduction furnace internal face, thus add the reduction power consumption of reduction furnace.
Three, summary of the invention
The present invention seeks to, propose the structure of a kind of polycrystalline silicon reducing furnace and utilize this reduction furnace to carry out the work side reduced
Method.Use the lifting electrode of cross-distribution, improve the uniformity of material distribution in stove, be easily controlled each position in reduction furnace
Temperature, reduce power consumption and also ensure product quality.
The technical scheme is that, a kind of method of polycrystalline reduction, it is characterized in that using following polycrystalline silicon reducing furnace；
Reduction furnace includes that chassis and body of heater, described body of heater are the top on chassis, and body of heater is the cylindric reaction chamber adding spherical top；Chassis
For discoid, raw material gas inlet and offgas outlet are distributed on chassis, it is characterized in that on chassis, uniform 30-50 is to electrode, described
Half electrode homogeneous vertical on chassis is installed, and second half electrode is staggered point of vertically-mounted electrode on lifting electrode, with chassis
Cloth, the bottom of lifting electrode is far from chassis 3-10cm；The upper end position of lifting electrode is concordant with spherical top intersection with cylindric, former
Material gas import is arranged on chassis by the air inlet pipe of a height of 3-10cm.Raw material gas inlet and offgas outlet are distributed on chassis not
With on the circumference of radius, when the circumference of a radius arranges raw material gas inlet, the circumference of adjacent radius is arranged tail
Gas exports.The plan-position, upper end of lifting electrode is provided with temperature sensor, and the flow controlling unstripped gas makes the temperature of sensor
Reach 910-935 DEG C；Increase raw gas flow when especially temperature is less than 910 DEG C, temperature is when raising near or above 925 DEG C
Reduce the flow of material mixed gas.
The stake body of concordant lifting electrode drawn by the cylindric titanium pad that clamps with spherical top intersection of body of heater, and titanium pad is drawn
Titanium framework body for angle titanium-type material.
Beneficial effect, the installation of the lifting electrode of reduction furnace structure of the present invention significantly improves the uniform of material distribution in stove
Property, is easily controlled the temperature of each position in reduction furnace easily by the applying of unstripped gas etc., and controlled Temperature Distribution can be controlled
The generation of silica flour in reduction furnace processed, it is to avoid silica flour is because being attached on the internal face of reduction furnace destroy the polishing of reduction furnace inwall
Face, can preserve the burnishing surface of reduction furnace internal face for a long time, adds internal face (being silver-plated) thermal-radiating to high temperature silicon rod
Reflection, thus reduce the reduction power consumption of reduction furnace；Temperature Distribution is more uniform, and this type of flow of the present invention can be controlled effectively
Temperature in reduction furnace processed, will not produce localized high temperature regions, and the reduction power consumption of reduction furnace is lower than prior art.Especially silicon rod
Growth quality more easy to control.The most hemispheric dome is conducive to the uniform balance of growth and tail gas stream.Due to lifting electricity
The alternatively distributed effect being alternately distributed and passing in and out gas of pole is more preferable, more improves the uniformity of material distribution in stove.Controlled
Temperature Distribution can control in reduction furnace silica flour in the uniform generation of electrode, it is to avoid silica flour is because being attached on the internal face of reduction furnace
And destroy the burnishing surface of reduction furnace inwall, the burnishing surface of reduction furnace internal face can be preserved for a long time, add internal face to high temperature
The thermal-radiating reflection of silicon rod, thus reduce the reduction power consumption of reduction furnace, efficiently control the temperature in reduction furnace, work of the present invention
In industry, the reduction power consumption of reduction furnace is 59～62kW h/kg.
Four, accompanying drawing explanation
Fig. 1 is present configuration schematic diagram.
Fig. 2 is the chassis top view of stove of the present invention.
Five, detailed description of the invention
As it can be seen, furnace bottom 1 in figure, electrode suppor 2, stove foot 3, furnace wall 4, gas outlet 5, air inlet pipe 6, sight glass 7,9, stove
The standby gas outlet of wall 8, air inlet pipe mounting disc 10, electrode 11, lifting electrode 12, lifting electrode installation site 13, lifting electrode peace
Dress support 14, hemisphere top furnace chamber 15.
The present invention includes: chassis and body of heater, and described body of heater is the top on chassis, and body of heater is the cylindric reaction adding spherical top
Chamber；Chassis is discoid, and raw material gas inlet and offgas outlet are distributed on chassis, on chassis uniform 30-50 to electrode (depending on stove
The size of body, also includes lifting electrode), described half electrode homogeneous vertical on chassis is installed, and second half electrode is lifting electricity
On pole, with chassis, vertically-mounted electrode is interspersed, and the bottom of lifting electrode is far from chassis 3-10cm, especially 5-6cm；Lifting electricity
The upper end position of pole is concordant with spherical top intersection with cylindric, and raw material gas inlet is by a height of 3-10cm, especially 5-6cm
Air inlet pipe is arranged on chassis.The distance of adjacent raw material gas inlet is 8-12cm, air inlet pipe 6 straight that raw material gas inlet is installed
Footpath is 4-6mm；Furnace wall internal face is silver-plated, reflection thermal-radiating to high temperature silicon rod, and electrode 11, lifting electrode 12 are in pairs
Install；The plan-position, upper end of lifting electrode is provided with temperature sensor, and the flow controlling unstripped gas makes the temperature of sensor reach
To 910-935 DEG C；Increase raw gas flow when especially temperature is less than 910 DEG C, temperature subtracts when raising near or above 925 DEG C
The flow of few material mixed gas.
On the circumference of the different radii that raw material gas inlet and offgas outlet are distributed on chassis, cloth on the circumference of a radius
When putting raw material gas inlet, the circumference of adjacent radius is arranged offgas outlet.The interval that the radius of adjacent circumferential increases is permissible
Being identical, or radius is the biggest, the interval that radius increases is smaller.
The stake body of concordant lifting electrode drawn by the cylindric titanium pad that clamps with spherical top intersection of body of heater, and titanium pad is drawn
Titanium framework body for angle titanium-type material.
Claims (3)
1. a method for polycrystalline reduction, is characterized in that using following polycrystalline silicon reducing furnace；Reduction furnace includes chassis and body of heater,
Described body of heater is the top on chassis, and body of heater is the cylindric reaction chamber adding spherical top；Chassis is discoid, raw material gas inlet and
Offgas outlet is distributed on chassis, and on chassis, uniform 30-50 is to electrode, and described half electrode homogeneous vertical on chassis is installed,
Second half electrode is interspersed for vertically-mounted electrode on lifting electrode, with chassis, and the bottom of lifting electrode is far from chassis 3-10cm；
The upper end position of lifting electrode is concordant with spherical top intersection with cylindric, and raw material gas inlet is by the air inlet pipe of a height of 3-10cm
It is arranged on chassis；On the circumference of the different radii that raw material gas inlet and offgas outlet are distributed on chassis, at the circle of a radius
When arranging raw material gas inlet on week, the circumference of adjacent radius is arranged offgas outlet；Upper transverse plane position at lifting electrode
Having installed temperature sensor, the flow controlling unstripped gas makes the temperature of sensor reach 910-935 DEG C.
The method of polycrystalline reduction the most according to claim 1, it is characterized in that reaching so that the temperature of sensor 910 DEG C-
925℃。
The method of polycrystalline reduction the most according to claim 1, is characterized in that increasing flow of feed gas when temperature is less than 910 DEG C
Amount, temperature reduces the flow of material mixed gas when raising near or above 925 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610465438.6A CN106115709B (en) | 2016-06-23 | 2016-06-23 | A kind of polycrystalline reduction method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610465438.6A CN106115709B (en) | 2016-06-23 | 2016-06-23 | A kind of polycrystalline reduction method |
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| CN106115709A true CN106115709A (en) | 2016-11-16 |
| CN106115709B CN106115709B (en) | 2018-04-06 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6063370A (en) * | 1983-09-16 | 1985-04-11 | Hitachi Koki Co Ltd | Apparatus for manufacturing amorphous silicon hydride |
| CN201105991Y (en) * | 2007-10-23 | 2008-08-27 | 四川永祥多晶硅有限公司 | Polycrystalline silicon hydrogen reducing furnace |
| CN201105990Y (en) * | 2007-10-23 | 2008-08-27 | 四川永祥多晶硅有限公司 | Polycrystalline silicon hydrogen reducing furnace |
| CN201473328U (en) * | 2009-08-10 | 2010-05-19 | 上海森和投资有限公司 | Tail gas outlet structure of polysilicon hydrogen reducing furnace |
| CN201512418U (en) * | 2009-09-24 | 2010-06-23 | 上海森松压力容器有限公司 | Polycrystalline silicon reducing furnace |
| CN104724705A (en) * | 2015-03-27 | 2015-06-24 | 中国恩菲工程技术有限公司 | Chassis assembly for polycrystalline silicon reduction furnace |
-
2016
- 2016-06-23 CN CN201610465438.6A patent/CN106115709B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6063370A (en) * | 1983-09-16 | 1985-04-11 | Hitachi Koki Co Ltd | Apparatus for manufacturing amorphous silicon hydride |
| CN201105991Y (en) * | 2007-10-23 | 2008-08-27 | 四川永祥多晶硅有限公司 | Polycrystalline silicon hydrogen reducing furnace |
| CN201105990Y (en) * | 2007-10-23 | 2008-08-27 | 四川永祥多晶硅有限公司 | Polycrystalline silicon hydrogen reducing furnace |
| CN201473328U (en) * | 2009-08-10 | 2010-05-19 | 上海森和投资有限公司 | Tail gas outlet structure of polysilicon hydrogen reducing furnace |
| CN201512418U (en) * | 2009-09-24 | 2010-06-23 | 上海森松压力容器有限公司 | Polycrystalline silicon reducing furnace |
| CN104724705A (en) * | 2015-03-27 | 2015-06-24 | 中国恩菲工程技术有限公司 | Chassis assembly for polycrystalline silicon reduction furnace |
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| CN106115709B (en) | 2018-04-06 |
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