CN104108718A - Method and device for quickly depositing polysilicon - Google Patents
Method and device for quickly depositing polysilicon Download PDFInfo
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- CN104108718A CN104108718A CN201410376132.4A CN201410376132A CN104108718A CN 104108718 A CN104108718 A CN 104108718A CN 201410376132 A CN201410376132 A CN 201410376132A CN 104108718 A CN104108718 A CN 104108718A
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Abstract
The invention relates to a method and device for quickly depositing and growing polysilicon in a chemical vapor deposition furnace. According to the method and device, silicon cores (1) or silicon plates and cross beams (2) in groups are connected to form a sheet(plate)-shaped inverted U-shaped device in the chemical vapor deposition reaction furnace. The large-surface-area device can be used as the initial base for producing polysilicon by siliceous gas deposition; and the device can also be used as an electric heating unit, so that the reaction furnace can quickly enter the heavy-current high-mixed-gas-flow large-solid/gas-contact-surface state after being started, thereby quickly depositing and growing the polysilicon in the reaction furnace.
Description
Technical field
A kind of method and apparatus of polysilicon fast deposition relates in chemical vapour deposition reactor furnace, produces the Technology of polysilicon with the mixed gas of silicon-containing gas or silicon-containing gas and hydrogen.Polysilicon is the key foundation material of photovoltaic cell, semiconducter device.
Background technology
At present, the mainstream technology of producing polysilicon is improved Siemens, at improved Siemens, produce in the process of polysilicon, various to the Reaktionsofen of excellent bell-jar (9 pairs rod and more than) in, adopt the inverted U-shaped silicon core (1) of the silicon core (1) that is arranged on electrode (4) graphite base (3) on Reaktionsofen chassis and crossbeam (2) overlap joint composition right.It is the electric heating body of conduct assurance reduction reaction temperature both, the matrix of growing as polysilicon deposition again, as shown in Figure 1.
In bell-jar Reaktionsofen, according to processing requirement, be provided with and multipairly by 2 silicon cores (1) and crossbeam (2), be connected to form inverted U-shaped silicon core to (Fig. 1).When Reaktionsofen opens stove, by the electrode on Reaktionsofen chassis (4) to inverted U-shaped silicon core to adding the high voltage electric of about 10KV, after certain hour, silicon core (1) will be breakdown, flows through silicon core upper current value is increased gradually.Now, control current value size, by the temperature on silicon core (1) at 1020--1150 ℃.Until all inverted U-shaped silicon core in Reaktionsofen is to all breakdown, and while being heated to 1020-1150 ℃, it is complete that Reaktionsofen opens stove, opens the intake valve of hydrogen and trichlorosilane gas.Now, hydrogen and trichlorosilane gas start, on silicon core (1) surface, gas-phase chemical reaction occurs, silicon is at silicon core (1) surface deposition, polysilicon starts in the upper growth of silicon core (1), along with the diameter of the growth silicon rod in reaction times increases gradually, until silicon rod diameter while reaching processing requirement, is closed mixed gas intake valve, disconnect the power supply of this Reaktionsofen, Reaktionsofen blowing out.Under normal circumstances, during Reaktionsofen blowing out, silicon rod diameter is 110-200mm, and the production cycle of Reaktionsofen is 100-250 hours.
In Reaktionsofen, hydrogen and trichlorosilane be in reaction and the deposition of silicon on silicon core (1) on silicon core (1) surface, involves gas boundary layer that a series of chemical reaction, Siliciumatom penetrate solid (silicon core or silicon rod) surface, Siliciumatom at the crystal growing process on gas-solid surface.According to gas-solid reaction principle, the factor that affects gas-solid reaction mainly contains temperature of reaction, pressure, gaseous component, solid surface is long-pending and gas flow rate etc.In other words, in Reaktionsofen, the sedimentation rate of polysilicon on silicon rod is mainly subject to temperature, pressure, gaseous component, the surface-area of silicon rod, the impact of gas flow in Reaktionsofen.At present, in the production process of polysilicon, the temperature in Reaktionsofen, pressure, gaseous component are constant substantially.But the surface-area of silicon rod is along with the variation of silicon rod diameter changes (3.14 times of rate of change that surface-area rate of change is diameter).In the starting stage of Reaktionsofen operation, the diameter of silicon rod is very little, and the surface-area of silicon rod is very little, and the sedimentation rate of polysilicon is just very little.
Therefore, in augmenting response stove, the initial surface area of polysilicon deposition growing substrate is one of approach improving polysilicon deposition speed in Reaktionsofen.For example 1, patent CN101432460A has announced and has adopted large-area silicone tube to replace 2 silicon cores (1) and crossbeam (2) to be connected to form inverted U-shaped silicon core (1) method of (Fig. 1) is prepared to polysilicon, due to much bigger than silicon core (1) of the initial surface area of silicone tube, thereby can improve the embryo deposit speed of polysilicon.But there is following shortcoming in the method: 1., when Reaktionsofen shove charge, the air in silicone tube is difficult for being divided before Reaktionsofen starts, and can form potential safety and hidden danger of quality.When slight, reduce the quality of polysilicon product, when serious, cause raw Reaktionsofen blast.2. silicone tube need to adopt ad hoc approach and equipment to prepare, and its production cost is unknown, and can cause existing a large amount of silicon cores (1) producing apparatus idle.For example 2, CN201010604262 has announced a kind of method and apparatus that increases reactor for polycrystalline silicon silicon core radical.The method is on an electrode (4) graphite base (3), with 2 and above silicon core (1), be evenly distributed on the concentric(al) circles of different diameter of electrode (4), then with graphite, do crossbeam (2) electrode (4) is connected to the silicon core (1) on another upper graphite base.The method and device can improve the embryo deposit area of polysilicon, thereby improve the sedimentation velocity of polysilicon.But there is following shortcoming in the method: 1. silicon core (1) grows in the process of large diameter silicon rod at polysilicon deposition, and silicon rod center can exist larger cavity, hazardous chemical (hydrogen, silicon-containing gas, hydrogenchloride etc.) abrim in cavity.This can form polycrystalline silicon rod come out of the stove, deposit or last handling process in potential safety hazard.2. graphite is done silicon core (1) connecting cross beam (2), can increase the carbon content in polysilicon product, thereby reduces quality product.
Therefore, still need a kind of method and apparatus that increases polysilicon embryo deposit surface of the base body.The method, guaranteeing that quality product does not reduce and do not cause under the condition of potential safety hazard, can improve the embryo deposit speed of polysilicon significantly, can avoid again causing the idle of a large amount of existing installations, reduces the production comprehensive cost of polysilicon.
Summary of the invention
The present invention is a kind of method and apparatus of polysilicon fast deposition.Adopt present method and device, guaranteeing quality product and do not forming under the condition of potential safety hazard, the solution polysilicon embryo deposit slow technical problem of growing.
The technical solution used in the present invention is: on a graphite base (3), vertically settle silicon core (1) or a slice silicon plate of one group of parallel arranged, by shorter siliceous crossbeam (2), connect one group of silicon core (1) or a slice silicon plate settled by same way on another graphite base (3), form an inverted U-shaped device (Fig. 2).It is upper that graphite base (3) is placed on electrode (4), and electrode (4) is arranged on the chassis of Reaktionsofen.It is upper that the inverted U-shaped device of such sheet (Fig. 2) is placed in two electrodes (4), and it is right that these two electrodes (4) are mutually electrode (4), is connected respectively with power supply.Initial substrate (electric heating body) with the inverted U-shaped device of this sheet (Fig. 2) as polysilicon deposition growth, replace by 2 silicon cores (1) and crossbeam (2) overlap joint, forming inverted U-shaped device (Fig. 1) in chemical vapour deposition reactor furnace, just can improve exponentially surface-area and the loaded current ability of polysilicon deposition growing substrate, improve exponentially in other words the embryo deposit speed of polycrystalline silicon rod, thereby the polysilicon fast deposition growth that silicon-containing gas in Reaktionsofen and hydrogen reaction or silicon-containing gas cracking are produced, the energy-efficient ground production run of realization response stove, finally reach the object reducing costs.
Wherein, described silicon core (1) is in groups: 1. adopt the circular silicon core (1) of 3-13 Φ (5-10) mm to become one group, silicon core (1) lower end is the small column that has certain taper, and silicon core (1) upper end is the small column that has a small stair, as shown in Figure 3; 2. adopting 3-13 cross sections is that the square silicon core (1) of thick (5-10) * wide (5-10) mm is one group, and silicon core (1) lower end is the small column that has certain taper, and silicon core (1) upper end is the small column that has a small stair, as shown in Figure 3.
Wherein, described silicon plate is: 1. cross section is the long silicon plate of thick (5-10) * wide (30-130) mm, and there are a plurality of small columns silicon plate lower end, and also there are a plurality of small columns upper end.As shown in Figure 4; 2. cross section is the long silicon plate of thick (5-10) * wide (30-130) mm, and there is the small stair of a protrusion at the upper and lower two ends of silicon plate, and small stair two ends are half-cylindrical, as shown in Figure 5.
Wherein, the crossbeam (2) of described connection silicon core (1) or silicon plate is: 1. cross section is the short silicon plate of thick (5-10) mm * wide (30-150) mm, and two ends all have one group of small sircle hole, as shown in Figure 6; 2. cross section is the short silicon plate of thick (5-10) mm * wide (30-150) mm, and it is semi-cylindrical bar shape trench hole that two ends all have two ends, as shown in Figure 7.
Wherein, the graphite base (3) of described arrangement silicon core (1) is: lower end has the taper concentric with electrode (4) circle hole, and upper end has by the center of circle, along a plurality of conicles or the circular hole of the symmetrical insertion silicon core (1) of diametric(al), as shown in Figure 8.
Wherein, the graphite base (3) of described arrangement silicon plate is: 1. lower end has the taper circle hole concentric with electrode (4), upper end has by the center of circle, along a plurality of conicles or the circular hole of the symmetrical embedding silicon plate lower end small column of diametric(al), as shown in Figure 8; 2. lower end has the taper circle hole concentric with electrode (4), and upper end has by the center of circle, along the bar shape trench hole of the symmetrical embedding silicon plate of diametric(al), and the specification of slotted eye is wide (5-10) mm * length (30-130) mm * degree of depth, as shown in Figure 9.
Wherein, described silicon core (1) group with the mode of connection of graphite base (3) is: the lower end of one group of silicon core (1) is vertically inserted in the conicle or circular hole of graphite base (3) upper end, and fixing.
Wherein, the mode of connection of described silicon plate and graphite base (3) is: 1. the lower end of silicon plate is vertically inserted in the conicle or circular hole of graphite base (3) upper end, and fixing; 2. silicon plate lower end is vertically inserted in the bar shape trench hole of graphite base (3) upper end, fixing.
Wherein, described silicon core (1) group with the mode of connection of crossbeam (2) is: by the circular hole of one end of the small cylinder stemple (2) in one group of vertical silicon core (1) upper end step, silicon core (1) head exposes certain length.
Wherein, the mode of connection of described silicon plate and crossbeam (2) is: 1. by the circular hole of small column stemple (2) one end of silicon plate upper end and expose certain length; 2. by the bar shape trench hole of protrusion step stemple (2) one end of silicon plate upper end and expose certain length.
Wherein, described silicon-containing gas is: SiHCl
3, SiCl
4, SiH
2cl
2, SiH
4gas.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the inverted U-shaped device of 2 silicon cores (1) in chemical vapour deposition reactor furnace, crossbeam (2), graphite base (3) and electrode (4) formation.
Fig. 2 is the schematic diagram that has the inverted U-shaped device of 5 circles or square silicon core (1), crossbeam (2), graphite base and motor (4) formation on each graphite base (3).
Fig. 3 is the schematic diagram of circular or square silicon core (1) and syndeton in groups.
Fig. 4 is silicon plate and the syndeton schematic diagram that all there is small column at upper and lower two ends.
Fig. 5 is silicon plate and the syndeton schematic diagram that there is a protrusion step upper end.
Fig. 6 is that two ends all have the schematic diagram of the crossbeam of aperture (2) and syndeton in groups.
Fig. 7 is the two ends crossbeam (2) that all has bar shape trench hole and the schematic diagram of syndeton.
Fig. 8 settles the graphite base (3) of silicon core (1)/silicon plate and the schematic diagram of syndeton in groups.
Fig. 9 settles the graphite base (3) of another kind of silicon plate and the schematic diagram of syndeton.
Embodiment
Below in conjunction with accompanying drawing, describe a kind of typical specific embodiments of method and apparatus of polysilicon fast deposition in detail.Other in essence identical specific embodiments belong to the scope of the method and apparatus of described a kind of polysilicon fast deposition, do not repeat one by one for this reason.
Fig. 2 is the schematic diagram that has the inverted U-shaped depositing base (electric heating body) of 5 circles or square silicon core (1) formation on each graphite base (3).A kind of specific implementation process of method and apparatus of polysilicon fast deposition is as follows:
1. choose suitable 10 circles or square silicon core (1).
2. every silicon core (1) lower end is processed into the cone of certain taper, this circular cone physical efficiency is closely inserted conicle or the circle interior (Fig. 3, Fig. 8) of graphite base (3) upper end.
3. every silicon core (1) upper end is processed into the right cylinder of a small stair, in the circular hole of the arbitrary end of the tight stemple of this cylinder physical efficiency (2) (Fig. 3, Fig. 6).
4. crossbeam (2) two ends are processed respectively to 5 small sircle holes, in small sircle hole, can closely embed silicon core (1) upper end small cylinder (Fig. 6).The decoration form of 5 small sircle holes is: from the center of central axis shown in Fig. 6, symmetrical along the upper and lower both direction of vertical axis.
5. graphite base (3) is processed into, lower end has one and justifies hole with electrode (4) taper concentric and energy intercalation electrode (4) upper end cone, upper end has 5 roundlet taper holes or circular hole, can closely insert the small cone body of silicon core (1) lower end in roundlet taper hole or circular hole.The distribution mode of 5 roundlet taper holes or circular hole is: by electrode (4) center of circle, along diametric(al) symmetrical (Fig. 8).
6. by 2 graphite bases (3) of preparing on request, be arranged on reposefully respectively on the paired electrode (4) on Reaktionsofen chassis.
7. by the lower end of 10 silicon cores (1) of preparation on request, vertically insert respectively in 5 roundlet taper holes or circular hole of 2 graphite bases (3) upper end, fixing.
8. by electrode (4) to 5 silicon cores (1) upper end small cylinder on a upper graphite base (3), in 5 small sircle holes of stemple (2) one end, and expose certain length.
9. by the small cylinder of 5 the silicon cores (1) on another graphite base (3), in 5 small sircle holes of stemple (2) the other end, and expose certain length.
10. by electrode (4) to be connected with power supply respectively (Fig. 2).
In chemical vapour deposition reactor furnace, the silicon chip (plate) of this high surface area being formed by connecting by 5 silicon cores (1) and crossbeam (2) and Graphite Electrodes (4) have just formed the initial substrate of electrically heated loop and polysilicon deposition.On such electrically heated loop, apply the high voltage electric of 10KV left and right, breakdown through certain hour silicon chip (plate), thereby regulate temperature to 1020-1150 ℃ of controlling in current value control Reaktionsofen, now, pass into the mixed gas of silicon-containing gas or silicon-containing gas and hydrogen, in Reaktionsofen, start to occur chemical gas phase reaction, polysilicon starts to deposit on depositing base.Because this silicon chip (plate) is that 5 silicon cores (1) form, with by singly propping up the initial substrate that silicon core (1) forms, compare, it has the current carrying capacity of 5 times and the gas-solid reaction area of 5 times, Reaktionsofen just can promptly improve 5 times by the flow of the mixed gas of current value, silicon-containing gas flow or silicon-containing gas and hydrogen after starting, thereby the sedimentation rate of polysilicon on embryo deposit matrix improves 5 times.In other words, in chemical vapour deposition reactor furnace, adopt the inverted U-shaped device (Fig. 2) of this (plate) shape, just can improve exponentially the embryo deposit speed of polysilicon, thereby make polysilicon fast deposition growth in Reaktionsofen.The method and apparatus of this kind of polysilicon fast deposition is applicable to various to excellent Reaktionsofen, is also applicable to Reaktionsofen and produces polysilicon under various pressure.
embodiment 1
This routine reactor is 9 pairs of excellent bell-jar Reaktionsofens, and silicon core (1) diameter is 8mm, is highly 2000mm, the inverted U-shaped device (Fig. 1) that adopts 2 silicon cores (1) and crossbeam (2) and graphite base (3) to form.After Reaktionsofen starts, temperature of reaction is 1020-1150 ℃, the gentle mixed gas initial flow of trichlorosilane is 20Nm3/h, along with the Reaktionsofen prolongation of working time, under the constant condition of temperature of reaction, the flow of mixed gas progressively strengthens, when Reaktionsofen moves to the processing condition of setting, and blowing out.Adopt a kind of method and apparatus of polysilicon fast deposition, the inverted U-shaped device (Fig. 2) being formed by 12 silicon cores (1), after Reaktionsofen starts, temperature of reaction is controlled at 1020-1150 ℃, mixed gas flow initial flow is 120 Nm3/h, under the constant condition of temperature of reaction, the flow of mixed gas progressively strengthens.When Reaktionsofen moves to the blowing out condition identical with the former, blowing out.Both compare, and adopt device of the present invention (Fig. 2), and the Reaktionsofen production cycle shortens 24%, and current consumption reduces 20000Kwh, and straight power consumption reduces 5%, and comprehensive power consumption reduces by 12%.
embodiment 2
This routine reactor is 12 pairs of excellent bell-jar Reaktionsofens, and silicon core (1) diameter is 8mm, and length is 2500mm, the inverted U-shaped device (Fig. 1) that adopts 2 silicon cores (1) and crossbeam (2) and graphite base (3) to form.After Reaktionsofen starts, temperature of reaction is 1020-1150 ℃, the gentle mixed gas initial flow of trichlorosilane is 35Nm3/h, along with the Reaktionsofen prolongation of working time, under the constant condition of temperature of reaction, the flow of mixed gas progressively strengthens, blowing out when Reaktionsofen moves to the processing condition of setting.Adopt a kind of method and apparatus of polysilicon fast deposition, the inverted U-shaped device (Fig. 2) being formed by 20 silicon cores (1), after Reaktionsofen starts, temperature of reaction is controlled at 1020-1150 ℃, mixed gas flow initial flow is 450 Nm3/h, under the constant condition of temperature of reaction, the flow of mixed gas progressively strengthens.When Reaktionsofen moves to the blowing out condition identical with the former, blowing out.Both compare, and adopt device of the present invention (2), and the Reaktionsofen production cycle shortens 50%, and current consumption reduces by 100,000 Kwh, and straight power consumption reduces 11%, and comprehensive power consumption reduces by 30%.
Claims (12)
1. the method and apparatus of a polysilicon fast deposition is: in airtight chemical vapour deposition reactor furnace, on a graphite base (3), vertically settle silicon core (1) or a slice silicon plate of one group of parallel arranged, by shorter siliceous crossbeam (2), connect one group of silicon core (1) or a slice silicon plate settled by same way on another graphite base (3), form the inverted U-shaped device (Fig. 2) of a sheet (plate) shape; It is upper that graphite base (3) is placed on electrode (4), and electrode (4) is arranged on the chassis of Reaktionsofen; It is upper that the inverted U-shaped device of such sheet (plate) shape (Fig. 2) is placed in two electrodes (4), and it is right that these two electrodes (4) are mutually electrode (4), is connected respectively with power supply.
2. wherein, the feature of described silicon core (1) is in groups: adopt the circular silicon core (1) of 3-13 Φ (5-10) mm to become one group, silicon core (1) lower end is the small column that has certain taper, and silicon core (1) upper end is the small column (Fig. 3) that has a small stair; Adopting 3-13 cross sections is that the square silicon core (1) of (5-10) * (5-10) mm is one group, and silicon core (1) lower end is the small column that has certain taper, and silicon core (1) upper end is the small column (Fig. 3) that has a small stair.
3. wherein, the feature of described silicon plate is: cross section is the long silicon plate of thick (5-10) * wide (30-130) mm, and there are a plurality of small columns silicon plate lower end, and also there are a plurality of small columns (Fig. 4) upper end; Cross section is the long silicon plate of thick (5-10) * wide (30-130) mm, and there is the small stair of a protrusion at the upper and lower two ends of silicon plate, and small stair two ends are half-cylindrical (Fig. 5).
4. wherein, the feature of the crossbeam (2) of described connection silicon core (1) or silicon plate is: cross section is the short silicon plate of thick (5-10) mm * wide (30-150) mm, and two ends all have one group of small sircle hole (Fig. 6); Cross section is the short silicon plate of thick (5-10) mm * wide (30-150) mm, and it is semi-cylindrical bar shape trench hole (Fig. 7) that two ends all have two ends.
5. wherein, the feature of the graphite base (3) of described arrangement silicon core (1) is: lower end has the taper concentric with electrode (4) circle hole, and upper end has by the center of circle, along a plurality of roundlet taper holes or the circular hole (8) of the symmetrical insertion silicon core (1) of diametric(al).
6. wherein, the feature of the graphite base (3) of described arrangement silicon plate is: lower end has the taper concentric with electrode (4) circle hole, and upper end has by the center of circle, along a plurality of roundlet taper holes or the circular hole (Fig. 8) of the symmetrical embedding silicon plate lower end small column of diametric(al); Lower end has the taper circle hole concentric with electrode (4), and upper end has by the center of circle, along the bar-shaped trough of the symmetrical embedding silicon plate of diametric(al), and the specification of bar-shaped trough is wide (5-10) mm * length (30-130) mm * degree of depth (Fig. 9).
7. wherein, described silicon core (1) group with the feature of the mode of connection of graphite base (3) is: the lower end of one group of silicon core (1) is vertically inserted in the roundlet taper hole or circular hole of graphite base (3) upper end, and fixing.
8. wherein, the feature of the mode of connection of described silicon plate and graphite base (3) is: the lower end of silicon plate is vertically inserted in the roundlet taper hole or circular hole of graphite base (3) upper end, and fixing; The lower end of silicon plate is vertically inserted in graphite base (3) bar-shaped trough, fixing.
9. wherein, described silicon core (1) group with the feature of the mode of connection of crossbeam (2) is: by the circular hole of one end of the small cylinder stemple (2) in one group of vertical silicon core (1) upper end step, silicon core (1) head exposes certain length.
10. wherein, the feature of the mode of connection of described silicon plate and crossbeam (2) is: by the circular hole of small column stemple (2) one end of silicon plate upper end and expose certain length; By in the bar shape trench hole of protrusion step stemple (2) one end of silicon plate upper end and expose certain length.
11. wherein, and the feature of described silicon-containing gas is: SiHCl
3, SiCl
4, SiH
2cl
2, SiH
4gas.
The method and apparatus of 12. 1 kinds of polysilicon fast deposition is applicable to the reaction type of furnace of various reaction pressures and excellent number.
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| CN201410376132.4A CN104108718A (en) | 2014-08-02 | 2014-08-02 | Method and device for quickly depositing polysilicon |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105460939A (en) * | 2016-02-04 | 2016-04-06 | 洛阳金诺机械工程有限公司 | Hollow silicon core and silicon core assembly thereof |
| CN105502407A (en) * | 2016-02-04 | 2016-04-20 | 洛阳金诺机械工程有限公司 | Silicon core used in polycrystalline silicon production and silicon core component thereof |
| CN105600788A (en) * | 2016-03-08 | 2016-05-25 | 洛阳金诺机械工程有限公司 | Silicon core assembly |
| CN110395735A (en) * | 2018-04-24 | 2019-11-01 | 内蒙古盾安光伏科技有限公司 | The also original production of polysilicon |
-
2014
- 2014-08-02 CN CN201410376132.4A patent/CN104108718A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105460939A (en) * | 2016-02-04 | 2016-04-06 | 洛阳金诺机械工程有限公司 | Hollow silicon core and silicon core assembly thereof |
| CN105502407A (en) * | 2016-02-04 | 2016-04-20 | 洛阳金诺机械工程有限公司 | Silicon core used in polycrystalline silicon production and silicon core component thereof |
| CN105600788A (en) * | 2016-03-08 | 2016-05-25 | 洛阳金诺机械工程有限公司 | Silicon core assembly |
| CN105600788B (en) * | 2016-03-08 | 2018-02-02 | 洛阳金诺机械工程有限公司 | A kind of silicon core assembly |
| CN110395735A (en) * | 2018-04-24 | 2019-11-01 | 内蒙古盾安光伏科技有限公司 | The also original production of polysilicon |
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