CN101759184A - System for making polysilicon with assistant of hydrogen plasmas and method therefor - Google Patents
System for making polysilicon with assistant of hydrogen plasmas and method therefor Download PDFInfo
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- CN101759184A CN101759184A CN200910204974A CN200910204974A CN101759184A CN 101759184 A CN101759184 A CN 101759184A CN 200910204974 A CN200910204974 A CN 200910204974A CN 200910204974 A CN200910204974 A CN 200910204974A CN 101759184 A CN101759184 A CN 101759184A
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Abstract
The invention discloses a system for making polysilicon by using hydrogen plasmas and a method therefor, 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 manufacture method and system of polysilicon, more particularly relate to a kind of system and manufacture method 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 production method of polysilicon generally adopts siemens's improved technology, quartz sand smelted in electric arc furnace purify to 98% and generate industrial silicon, again industrial silicon is pulverized and reacted vulcanizing in the bed bioreactor at one with it with anhydrous HCl under the condition about 300 ℃, generate diffluent SiHCl3, 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, this reaction vessel seals, discharge port and opening for feed and some counter electrode are installed on the chassis, connecting diameter 5-10 millimeter on the electrode, the silicon rod of length 1.5-2.5 rice, two silicon rods on every counter electrode interconnect (see figure 1) at the other end by short silicon rod again, 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 is at the surface deposition of silicon rod, the diameter of silicon rod is increased gradually, finally reach 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 is converted to silicon tetrachloride in cracking process, and trichlorosilane is converted to the ratio of polysilicon less than 50%, and every kilogram of trichlorosilane can only obtain the following polysilicon of 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 complexity of cracking process generation, the separation costs height.
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 purpose of the present invention provides a kind of method of utilizing plasma body to produce polysilicon, this method is by 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 by 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 the back as assist gas and are converted to plasma body by plasma generator and are 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 is converted to plasma body by 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 ℃, and preferably 600～1000 ℃, particularly preferred is 700～850 ℃.
Further, the vapour deposition of implementing on the silicon plug under the air pressure of 0.5～1 crust, preferred 0.85～0.95 crust (bar) (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, described plasma body is chosen as the stronger negative hydrogen plasma of reductibility.
Further, unstripped gas and assist gas carried out preheating by the reduction furnace reacted tail gas before entering plasma producing apparatus.
Further, the silicon plug is the HIGH-PURITY SILICON plug of resistivity 20-150 Ω cm in the reduction furnace.
Further, described 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, 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 dichlorosilane, in Trichloromonosilane and the silicon tetrachloride one or more, it is characterized in that the gas feed device of plasma producing apparatus by 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 flow control 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 Controlling 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 by 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 discharge nozzle, 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 by specific embodiment and in conjunction with the accompanying drawings plasma body production equipment of the present invention and method being 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, discharge nozzle 4, electrode 5 and silicon core 6, and this reduction furnace is airtight, feed-pipe 3, discharge nozzle 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 comprising the above-mentioned prior art structure of (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, primary heater unit be set, carry out preheating to entering body of heater inside and/or entering plasma generator gas inside temperature by the reduction furnace reacted tail gas.Reduction furnace and plasma generator pressure inside can be regulated by pressure regulating device.In one embodiment, plasma producing apparatus 7 by inlet pipe 8 with hydrogen be selected from helium, neon, argon gas, the assist gas of one or more in the krypton gas infeeds wherein, 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 by 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 unstripped gas in the feed-pipe (close the flow control valve that leads to the unstripped gas on the gas mixer and open the flow control 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 flow control 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 unstripped gas gas mixer on flow control valve simultaneously close the flow control 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 by 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 by 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 unstripped gas is about 3: 1, raises gradually along with sedimentary, in sedimentary latter stage, is increased to about 6: 1.Can be by 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 is 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, in the sedimentary later stage, unstripped gas all directly can be fed reduction furnace.
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 of Cai Yonging 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 unstripped gas is mixed the back by 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 of Cai Yonging 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 of Cai Yonging 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 unstripped 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 of Cai Yonging 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 unstripped 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 of Cai Yonging 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 ℃, by the gaseous tension control device furnace pressure being set simultaneously is 0.95bar, on load voltage on electrode then, make the silicon in-core form electric current, and continue to be warming up to 1000 ℃, feed unstripped 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 production 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 above the specific embodiment of the present invention has been 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 (13)
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, be converted to plasma body by plasma producing apparatus after the assist gas of hydrogen, unstripped gas and nonessential interpolation mixes and be transported in the reduction furnace; Perhaps hydrogen is mixed with assist gas and be transported in the reduction furnace respectively with unstripped gas after the back is converted to plasma body by plasma producing apparatus, deposit polycrystal silicon ingot on the silicon core in reduction furnace, described assist gas is selected from one or more in helium, neon, argon gas and the nitrogen.
2. the method for claim 1, wherein the temperature of plasma body is 400～1200 ℃, and preferably 600～1000 ℃, particularly preferred is 700～850 ℃.
3. the method for claim 1, wherein the interior air pressure of plasma producing apparatus and reduction furnace is 0.5～1 crust, preferred especially 0.85～0.95 crust.
4. the method for claim 1, wherein the temperature of silicon plug is corresponding is heated to 600～1200 ℃, preferred especially 700～850 ℃.
5. as each described method of claim 1-4, 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.
6. as each described method of claim 1-4, wherein, the silicon plug resistivity in the reduction furnace is 20～150 Ω cm.
7. as each described method of claim 1-4, wherein, described plasma generator is wherein a kind of of electron cyclotron resonace (ECR) plasma body, inductively coupled plasma (ICP) or hot filament (HF) plasma body, preferred inductively coupled plasma (ICP).
8. device that utilizes plasma body to produce polysilicon, 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 also can be only from the chassis charging from top chassis charging simultaneously, the chassis is equipped with the tail gas relief outlet, the chassis is provided with heating electrode, on the electrode one by one correspondence be provided with the silicon plug, unstripped gas adopts dichlorosilane, in Trichloromonosilane and the silicon tetrachloride one or more, 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 by 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.
9. device as claimed in claim 8, it is characterized in that, the reaction zone inwall material of plasma producing apparatus is made up of in graphite, quartz, HIGH-PURITY SILICON, silicon carbide and the silicon nitride one or more, and interior wall construction is one or more layers material composite structure.
10. device as claimed in claim 8 is characterized in that, described plasma producing apparatus has a gas mixer before air inlet, and described mixing tank has the flow valve of controlling hydrogen, assist gas and raw material gas flow respectively.
11. device as claimed in claim 8 is characterized in that, described plasma generator has negative hydrogen plasma producer.
12. as each described device of claim 8-11, it is characterized in that, unstripped gas enters plasma producing apparatus after can all feeding gas mixer by flow valve control, or part feed gas mixer and another part directly by be arranged on stove tube top and/or the chassis opening for feed with etc. the feeding reduction furnace that is mixed of the plasma body after the conversion of three-dimensional producer, also can all directly feed reduction furnace by opening for feed.
13., it is characterized in that the resistivity that the described 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 as each described device of claim 8-11.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| 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 |
| 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 |
| CN114455587A (en) * | 2022-01-26 | 2022-05-10 | 何良雨 | High-purity polycrystalline silicon production device and method |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| ITRM20060521A1 (en) * | 2006-10-02 | 2008-04-03 | Solaria Tecnologie S R L | PROCEDURE AND EQUIPMENT FOR THE PRODUCTION OF HIGH PURITY SILICON USING MULTIPLE PRECURSORS |
| CN101239723A (en) * | 2007-02-07 | 2008-08-13 | 北京明远通科技有限公司 | Plasma producing method and device for polycrystalline silicon |
| CN201313954Y (en) * | 2008-11-03 | 2009-09-23 | 江苏中能硅业科技发展有限公司 | Reducing furnace for preparing polycrystalline silicon |
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- 2009-09-30 CN CN2009102049740A patent/CN101759184B/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN114455587A (en) * | 2022-01-26 | 2022-05-10 | 何良雨 | High-purity polycrystalline silicon production device and method |
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