CN101759184B - System for making polysilicon with assistance of hydrogen plasmas and method therefor - Google Patents
System for making polysilicon with assistance of hydrogen plasmas and method therefor Download PDFInfo
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- CN101759184B CN101759184B CN2009102049740A CN200910204974A CN101759184B CN 101759184 B CN101759184 B CN 101759184B CN 2009102049740 A CN2009102049740 A CN 2009102049740A CN 200910204974 A CN200910204974 A CN 200910204974A CN 101759184 B CN101759184 B CN 101759184B
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Abstract
The invention discloses a method for making polysilicon by using hydrogen plasmas, wherein the method includes that one or more of dichlorosilane, silicochloroform and silicon tetrachloride is (are) used as the raw gas; hydrogen is used as the reducing gas; or one or more of helium, neon, argon and krypton is (are) used as the assistant gas; the assistant gas and the raw gas are mixed and then transformed into plasmas in a plasma generator; the plasmas are conveyed into a reducing furnace and deposited to make polysilicon ingots on a silicon core in the reducing furnace. In addition, the invention also discloses the polysilicon reducing furnace applying the method. Compared with the prior art, the invention obviously reduces the reaction temperature, improves the once through yield of the polysilicon and the deposition rate of silicon rods, and greatly reduces the energy consumption; a high-voltage device for high voltage start is saved due to adoption of the plasmas, and the system is started easily at low voltage; and the constant voltage operation in the reducing furnace can be realized. Integrating the system and the method, the invention reduces the production cost and the probability of potential safety hazard remarkably.
Description
Technical field
The present invention relates to a kind of method of manufacture and system of polysilicon, more particularly relate to a kind of system and method for manufacture of utilizing hydrogen plasma secondary combined Siemens Method to carry out production of polysilicon.
Background technology
As everyone knows, world today's information and control techniques have obtained develop rapidly, and what it relied on is the various device chips that silicon chip is made, and the starting materials of silicon chip is exactly a polysilicon.
At present; The working method of polysilicon generally adopts siemens's improved technology; Silica sand smelted in electric arc furnace purify to 98% and generate industrial silicon; With the industrial silicon pulverizing and in a sulfuration bed bioreactor, reacting with it with anhydrous HCl under the condition about 300 ℃, generate diffluent SiHCl3 again, form gaseous mixture (H2, HCl, SiHCl3, SiCl4, Si) simultaneously.Above-mentioned gaseous mixture is then further purified, decomposed, and the SiHCl3 that purifies after purifying adopts high temperature reduction technology, with high-purity SiHCl3 reduce deposition and generate polysilicon in H2 atmosphere.
Above-mentioned chemical vapor deposition processes carries out in reduction furnace, and this reaction vessel seals, and discharge port and opening for feed and some counter electrode are installed on the chassis; The silicon rod that is connecting diameter 5-10 millimeter, length 1.5-2.5 rice on the electrode; Two silicon rods on every counter electrode interconnect (see figure 1) at the other end through short silicon rod again, and when applying the high pressure of 12kV on the counter electrode, the breakdown conduction of silicon rod also is heated to 1080-1100 ℃ and reacts; Through hydrogen reduction; Silicon increases the diameter of silicon rod at the surface deposition of silicon rod gradually, finally reaches the 120-200 millimeter.Generally, produce the high purity silicon rods of diameter 120-200 millimeter, the required reaction times is approximately 150-300 hour.
Yet there is following shortcoming in this method: 1, and the efficient of thermo-cracking is low, and the part trichlorosilane converts silicon tetrachloride in cracking process, and trichlorosilane converts the ratio of polysilicon into less than 50%, and every kilogram of trichlorosilane can only obtain the polysilicon below the 100g.Silicon tetrachloride is through after separating, and synthesizing trichlorosilane is as starting material again, such working cycle power consumption power consumption, inefficiency.2, the exhaust gas component of cracking process generation is complicated, and separation costs is high.
Therefore,, shorten the depositing time of polysilicon, improve productive rate, the present invention proposes and adopted plasma to assist to carry out the system and method that polysilicon is made in chemical vapour deposition in order to reduce production costs and significantly to increase reduction rate.This method has avoided original direct feeding high-voltage power supply by force to the mode of silicon plug heating on the one hand, has simplified required control panel greatly, has improved the deposition effect of elemental silicon on the silicon core on the other hand, has reduced production cost.
Summary of the invention
One of the object of the invention provides a kind of method of utilizing plasma body to produce polysilicon; This method is through with being incorporated in the polycrystalline silicon reducing furnace after the unstripped gas plasma; Thereby improve the reducing power of hydrogen; Fast reaction speed also reduces temperature of reaction, helps to improve the deposition effect of polysilicon on the silicon plug.
Another object of the present invention provides the system that a kind of plasma body is produced polysilicon; This system is through being provided with the plasma producing apparatus of gas mixer on the inlet of reduction furnace; And take stove tube top and/or chassis to distinguish the mode of charging; Significantly improve the deposition of silicon, increased productive rate.
To achieve these goals, the present invention has adopted following technical scheme:
A kind of method of utilizing plasma body to produce polysilicon; Unstripped gas adopts hydrogen as reducing gas; In dichlorosilane, Trichloromonosilane and the silicon tetrachloride one or more are as unstripped gas, and wherein one or more in the helium of hydrogen and unstripped gas or nonessential interpolation, neon, argon gas, the krypton gas mix as assist gas and then convert plasma body into through plasma generator and be transported in the reduction furnace; Or hydrogen mixed with above-mentioned assist gas be transported to respectively in the reduction furnace with unstripped gas after the back converts plasma body into through plasma generator, deposit polycrystal silicon ingot on the silicon core in reduction furnace, wherein the temperature of silicon plug is heated to 600～1200 ℃.
Further, the temperature of plasma body is 400～1200 ℃, preferably 600～1000 ℃, and especially preferably 700～850 ℃.
Further; The vapour deposition of under the air pressure of 0.5～1 crust, preferred 0.85～0.95 crust (bar), implementing on the silicon plug (that is to say; Air pressure in plasma producing apparatus and the reduction furnace is 0.5～1 crust; Preferred especially 0.85～0.95 crust), the temperature of silicon plug is corresponding to be heated to 600～1200 ℃, preferred 700～850 ℃.
Further, said plasma body is chosen as the stronger negative hydrogen plasma of reductibility.
Further, unstripped gas and assist gas carried out preheating through the reduction furnace reacted tail gas before getting into plasma producing apparatus.
Further, the silicon plug is the HIGH-PURITY SILICON plug of resistivity 20-150 Ω cm in the reduction furnace.
Further, said plasma generator is wherein a kind of device of electron cyclotron resonace (ECR) plasma body, inductively coupled plasma (ICP) or hot filament (HF) plasma body.
Further, plasma type preferably adopts inductively coupled plasma (ICP).
A kind of device that utilizes plasma body to produce polysilicon; Comprise the stove tube that has refrigerating unit, the stove tube is arranged on the chassis, and stove tube top and/or chassis are provided with the gas feed device; The chassis is provided with heating electrode; On the electrode one by one correspondence be provided with the silicon plug, reducing gas adopts hydrogen, unstripped gas adopts one or more in dichlorosilane, Trichloromonosilane and the silicon tetrachloride; It is characterized in that the gas feed device of plasma producing apparatus through being arranged on stove tube top and/or chassis feeds reduction furnace with hydrogen and unstripped gas or nonessential assist gas according to the geometric centre position of arranging along the silicon plug.
Further, plasma producing apparatus is provided with a gas mixer before air inlet, and mixing tank has the regulating valve of controlling hydrogen, assist gas and raw material gas flow respectively.
Further, plasma producing apparatus preferably has negative hydrogen plasma generating unit.
Further, to produce the silicon plug that the device of polysilicon also is provided with in gaseous tension system and the reduction furnace be the HIGH-PURITY SILICON plug of resistivity 20-150 Ω cm for above-mentioned plasma body.
Compared with prior art, the present invention has the following advantages: 1) the present invention has significantly reduced temperature of reaction, has shortened the reactive deposition time, has greatly reduced energy consumption, and has realized atmospheric operation; The use of high-pressure electric control device when 2) the present invention has saved high voltage startup through the introducing of plasma body can be used the higher higher polycrystalline silicon rod of silicon plug production purity of purity; Comprehensively both have reduced production cost significantly, have reduced the probability of occurrence of potential safety hazard.
Description of drawings
Fig. 1 is the device synoptic diagram that siemens's legal system is equipped with polysilicon in the prior art.
Wherein, 1 is furnace shell, and 2 is the chassis, and 3 is that feed-pipe, 4 is that extraction line, 5 is that electrode, 6 is the silicon core.
Fig. 2 is the synoptic diagram of the auxiliary vapor phase growing apparatus of polysilicon hydrogen plasma of one of embodiment of the present invention.
Wherein, 7 is plasma producing apparatus; 8 is inlet pipe; 9 is gas mixer; 10 is the variable valve on each inlet pipe.
Embodiment
Below through concrete embodiment and combine accompanying drawing that plasma body production equipment of the present invention and method are elaborated, but these embodiment only are illustrative purposes, are not intended to scope of the present invention is carried out any qualification.
Referring to Fig. 1, Fig. 1 is equipped with the device synoptic diagram of polysilicon for siemens's legal system in the prior art.Wherein, this device comprises stove tube 1, chassis 2, feed-pipe 3, extraction line 4, electrode 5 and silicon core 6, and this reduction furnace is airtight, feed-pipe 3, extraction line 4 and electrode 5 are installed on the chassis 2 and/or on the furnace shell top, silicon core 6 is connected on the electrode 5.Fig. 2 is the synoptic diagram of polysilicon plasma body production equipment of the present invention.Except the structure that comprises above-mentioned prior art (as shown in Figure 1); Respectively at stove tube top and/or the chassis plasma producing apparatus 7 up and down has been installed along the geometric centre position that the silicon core is arranged; Further can before the plasma producing apparatus inlet mouth, preheating unit be set, carry out preheating to getting into body of heater inside and/or getting into plasma generator gas inside temperature through the reduction furnace reacted tail gas.Reduction furnace and plasma generator pressure inside can be regulated through pressure regulating device.In one embodiment; Plasma producing apparatus 7 infeeds hydrogen and one or more the assist gas that is selected from helium, neon, argon gas, the krypton gas wherein through inlet pipe 8; And the plasma body that will be transformed into and unstripped gas feed in the reduction furnace according to the geometric centre position of arranging along the silicon plug through feed-pipe 3; The feed-pipe 3 of this moment is preferably the feed-pipe of concentric sleeve type; Insert the plasma gun 11 of plasma generator 7 in feed-pipe 3 inner cores, plasma in the plasma gun 11 and the virgin gas in the feed-pipe (close the regulating valve that leads to the virgin gas on the gas mixer and open the regulating valve that leads on the feed-pipe 3 simultaneously) infeed in the stove together.Preferably, plasma producing apparatus 7 is provided with a gas mixer 9 before air inlet, and mixing tank has the regulating valve 10 of controlling hydrogen, assist gas and/or raw material gas flow respectively, referring to Fig. 2.In another embodiment; Plasma producing apparatus 7 infeeds wherein (unlatching lead to virgin gas gas mixer on regulating valve simultaneously close the regulating valve that lead to feed-pipe 3 on) with in the helium of hydrogen and unstripped gas or nonessential interpolation, neon, argon gas, the krypton gas one or more as assist gas through inlet pipe 8, and the plasma body that will be transformed into is that feed-pipe 3 feeds in the reduction furnace according to the geometric centre position of arranging along the silicon plug through the gas feed device that is arranged on stove tube top and/or chassis.In addition, the top of body of heater also can be provided with above-mentioned plasma producing apparatus and gas mixer etc. symmetrically, thereby forms new embodiment (not shown).
Usually, playing heater stage, the volume ratio of hydrogen and virgin gas is about 3: 1, raises gradually along with sedimentary, in sedimentary latter stage, is increased to about 6: 1.Can be through the adjusting of unstripped gas variable valve 9 realizations to the unstripped gas air input; Can select unstripped gas is fed gas mixer and hydrogen and assist gas mixing post plasmaization fully or partly; Also can select unstripped gas is all directly fed in the reduction furnace by opening for feed up and down, preferably, when playing stove, unstripped gas all fed the gas mixer post plasmaization; Reactive behavior and sedimentation velocity when having improved stove; Reduce the ratio that feeds unstripped gas in the gas mixer after the reaction beginning gradually,, can unstripped gas all directly be fed reduction furnace in the sedimentary later stage.
Plasma producing apparatus preferably has negative hydrogen plasma producer.
Embodiment 1
1) having adopted resistivity is the HIGH-PURITY SILICON plug of 20 Ω cm.
2) the ICP generating unit frequency that adopts is that 40.68MHz, power are 100kW.
3) air pressure in plasma producing apparatus and the reduction furnace is controlled at 0.95bar.
4) unstripped gas employing dichlorosilane and silicon tetrachloride volume ratio are 1: 2 gaseous mixture.
5) above-mentioned silicon core is connected on the electrode on chassis in the reduction furnace structure of the present invention; Feeding earlier when playing stove is heated up with the plasma body that is transformed after auxiliary gas mixes by hydrogen makes the silicon core be heated to about 400 ℃; On load voltage on electrode then; Make the silicon in-core form electric current, and continue to be warming up to 600 ℃, cut off auxiliary gas charging more gradually and virgin gas is mixed the back through gas mixer with hydrogen feeding plasma producing apparatus.Hydrogen flow rate is controlled to be 30m
3/ h deposits 100 hours then, obtains the silicon rod that diameter is 100mm.
Embodiment 2
1) having adopted resistivity is the HIGH-PURITY SILICON plug of 50 Ω cm.
2) the ICP generating unit frequency that adopts is that 40.68MHz, power are 100kW.
3) air pressure in plasma producing apparatus and the reduction furnace is controlled at 0.95bar.
4) unstripped gas employing dichlorosilane and silicon tetrachloride volume ratio are 1: 5 gaseous mixture.
5) above-mentioned silicon core is connected on the electrode on chassis in the reduction furnace structure of the present invention; Feeding earlier when playing stove is heated up with the plasma body that is transformed after auxiliary gas mixes by hydrogen makes the silicon core be heated to about 500 ℃; Loading current on electrode then, and continue to be warming up to 700 ℃.Hydrogen flow rate is controlled to be 40 cubic metres/hour, deposits 100 hours then, obtains diameter and be 120 millimeters silicon rod.
1) adopting resistivity is the HIGH-PURITY SILICON plug of 70 Ω cm.
2) the ICP generating unit frequency that adopts is that 40.68MHz, power are 100kW.
3) air pressure in plasma producing apparatus and the reduction furnace is controlled at 0.95bar.
4) unstripped gas employing dichlorosilane and silicon tetrachloride volume ratio are 1: 8 gaseous mixture.
5) above-mentioned silicon core is connected on the electrode on chassis in the reduction furnace structure of the present invention; Feeding earlier when playing stove is heated up with the plasma body that is transformed after auxiliary gas mixes by hydrogen makes the silicon core be heated to about 600 ℃; And continue to be warming up to 800 ℃, feed virgin gas again.Hydrogen flow rate is controlled to be 30 cubic metres/hour, deposits 100 hours then, obtains diameter and be 100 millimeters silicon rod.
Embodiment 4
1) adopting resistivity is the HIGH-PURITY SILICON plug of 100 Ω cm.
2) the ICP generating unit frequency that adopts is that 40.68MHz, power are 100kW.
3) air pressure in plasma producing apparatus and the reduction furnace is controlled at 0.95bar.
4) unstripped gas employing dichlorosilane and Trichloromonosilane volume ratio are 1: 4 gaseous mixture.
5) above-mentioned silicon core is connected on the electrode on chassis in the reduction furnace structure of the present invention; Feeding earlier when playing stove is heated up with the plasma body that is transformed after auxiliary gas mixes by hydrogen makes the silicon core be heated to about 700 ℃; And continue to be warming up to 800 ℃, feed virgin gas again.Hydrogen flow rate is controlled to be 40 cubic metres/hour, deposits 100 hours then, obtains diameter and be 180 millimeters silicon rod.
1) adopting resistivity is the HIGH-PURITY SILICON plug of 150 Ω cm.
2) the ICP generating unit frequency that adopts is that 40.68MHz, power are 100kW.
3) air pressure in plasma producing apparatus and the reduction furnace is controlled at 0.95bar.
4) unstripped gas employing dichlorosilane and Trichloromonosilane volume ratio are 1: 9 gaseous mixture.
5) above-mentioned silicon core is connected on the electrode on chassis in the reduction furnace structure of the present invention; Feeding earlier when playing stove is heated up with the plasma body that is transformed after auxiliary gas mixes by hydrogen makes the silicon core be heated to about 700 ℃; Through the gaseous tension gear furnace pressure being set simultaneously is 0.95bar, and on load voltage on electrode makes the silicon in-core form electric current then; And continue to be warming up to 1000 ℃, feed virgin gas again.Hydrogen flow rate is controlled to be 30 cubic metres/hour, deposits 100 hours then, obtains diameter and be 180 millimeters silicon rod.
Table 1 is the comparing result of method for preparing polysilicon of the present invention and prior art working method.
Table 1
| Title | Prior art | The present invention |
| Unit power consumption | 100-150kWh/kg | 60-90kWh/kg |
| Sedimentation rate | 0.8～1.2mm/h | 1～1.8mm/h |
| Operational condition | 1000～1150 ℃, 0.3～0.6MPa, 5～10kV opens stove | 600～950 ℃, normal pressure need not high pressure and opens stove |
The method of utilizing plasma body to produce polysilicon among the present invention has reduced the production cost of polysilicon significantly, has greatly shortened depositing time, productivity is improved greatly, and make production process safer.
Although the preceding text specific embodiments of the invention has given to describe in detail and explanation; But should indicatedly be; We can carry out various equivalences to above-mentioned embodiment according to conception of the present invention and change and modification; When the function that it produced does not exceed spiritual that specification sheets and accompanying drawing contain yet, all should be within protection scope of the present invention.
Claims (15)
1. method of utilizing plasma body to produce polysilicon; Unstripped gas adopts one or more in dichlorosilane, Trichloromonosilane and the silicon tetrachloride; Reducing gas adopts hydrogen; It is characterized in that, convert plasma body into through plasma producing apparatus after the assist gas of hydrogen, unstripped gas and nonessential interpolation mixes and be transported in the reduction furnace; Perhaps hydrogen being mixed with assist gas is transported in the reduction furnace respectively with unstripped gas after the back converts plasma body into through plasma producing apparatus; Deposit polycrystal silicon ingot on the silicon core in reduction furnace; Said assist gas is selected from one or more in helium, neon, argon gas and the krypton gas; Wherein the temperature of plasma body is 400～1200 ℃, and the air pressure in plasma producing apparatus and the reduction furnace is 0.5～1 crust, and the temperature of silicon plug is corresponding is heated to 600～1200 ℃.
2. the method for claim 1, wherein the temperature of plasma body is 600～1000 ℃.
3. method as claimed in claim 2, wherein, the temperature of plasma body is 700～850 ℃.
4. the method for claim 1, wherein the interior air pressure of plasma producing apparatus and reduction furnace is 0.85～0.95 crust.
5. the method for claim 1, wherein the temperature of silicon plug is corresponding is heated to 700～850 ℃.
6. like each described method of claim 1-5, wherein, hydrogen and unstripped gas are being reduced the preheating of stove reacted tail gas earlier before the input plasma producing apparatus or before the input reduction furnace.
7. like each described method of claim 1-5, wherein, the silicon plug resistivity in the reduction furnace is 20～150 Ω cm.
8. like each described method of claim 1-5, wherein, said plasma generator is wherein a kind of of Ecr plasma, inductively coupled plasma or hot filament plasma body.
9. method as claimed in claim 8, wherein, said plasma generator is an inductively coupled plasma.
10. device that utilizes plasma body to produce polysilicon; Be used to implement the method for claim 1, comprise the stove tube that has refrigerating unit, the stove tube is installed on the chassis; Stove tube top and/or chassis are equipped with the gas feed device; Can be from also only charging of top chassis charging simultaneously from the chassis, the chassis is equipped with the tail gas relief outlet, and the chassis is provided with heating electrode; On the electrode one by one correspondence be provided with the silicon plug; Unstripped gas adopts one or more in dichlorosilane, Trichloromonosilane and the silicon tetrachloride, and reducing gas adopts hydrogen, it is characterized in that; The geometric centre position of arranging along the silicon plug is provided with plasma producing apparatus, the gas feed device of plasma producing apparatus through being arranged on stove tube top and/or chassis with the assist gas of hydrogen and unstripped gas or nonessential interpolation according to the geometric centre position feeding reduction furnace of arranging along the silicon plug.
11. device as claimed in claim 10; It is characterized in that; The reaction zone inwall material of plasma producing apparatus is made up of in graphite, quartz, HIGH-PURITY SILICON, silit and the silicon nitride one or more, and interior wall construction is one or more layers material composite structure.
12. device as claimed in claim 10 is characterized in that, said plasma producing apparatus has a gas mixer before air inlet, and said mixing tank has the flow valve of controlling hydrogen, assist gas and raw material gas flow respectively.
13. device as claimed in claim 10 is characterized in that, said plasma generator has negative hydrogen plasma producer.
14. like each described device of claim 10-13; It is characterized in that; Unstripped gas gets into plasma producing apparatus after can all feeding gas mixer through flow valve control; Or part feed gas mixer and another part directly through being arranged on plasma body after opening for feed and the plasma generator conversion on stove tube top and/or the chassis feeding reduction furnace that is mixed, also can be all directly by opening for feed feeding reduction furnace.
15., it is characterized in that the resistivity that the said device that utilizes plasma body to produce polysilicon also is provided with silicon plug in Pneumatic controller and the reduction furnace is 20-150 Ω cm like each described device of claim 10-13.
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| KR101543495B1 (en) | 2012-06-14 | 2015-08-11 | 주식회사 엘지화학 | Apparatus for manufacturing polysilicon comprising plasma generator and method for manufacturing polysilicon using the same |
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| CN106283180A (en) * | 2015-05-21 | 2017-01-04 | 丁欣 | The manufacture method of polysilicon and the manufacture method of monocrystal silicon |
| CN107515274A (en) * | 2016-06-15 | 2017-12-26 | 上海韵申新能源科技有限公司 | A kind of polycrystalline silicon production system quality evaluating method and device |
| CN107473228A (en) * | 2017-10-12 | 2017-12-15 | 亚洲硅业（青海）有限公司 | A kind of nanoscale crystalline silicon and preparation method thereof |
| CN114455587B (en) * | 2022-01-26 | 2023-07-21 | 何良雨 | High-purity polysilicon production device and method |
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