CN104357901A - Method for reducing oxygen donor content of Czochralski monocrystal - Google Patents
Method for reducing oxygen donor content of Czochralski monocrystal Download PDFInfo
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- CN104357901A CN104357901A CN201410616737.6A CN201410616737A CN104357901A CN 104357901 A CN104357901 A CN 104357901A CN 201410616737 A CN201410616737 A CN 201410616737A CN 104357901 A CN104357901 A CN 104357901A
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Abstract
The invention discloses a method for reducing an oxygen donor content of a Czochralski monocrystal. The method comprises the steps of seeding, shouldering, rotating, obtaining equal diameter, ending and oxygen controlling. The method disclosed by the invention has the advantages as follows: the furnace pressure is reduced to accelerate the pumping of a main pump, increase argon flow, exhaust the SiO volatile gas more quickly, and reduce the content of oxygen which is fed to the molten silicon; the revolving speed of a crucible where the monocrystal grows is reduced, reaction between the molten silicon and the quartz crucible can be slowed down, and the oxygen content in the molten silicon can be reduced, so that the content of oxygen fed to the monocrystal can be reduced, and further the type P monocrystal donor effect can be fundamentally reduced; the revolving speed of the seed crystal can be increased, the latent heat release of crystallization can be quickened, and the cooling speed can be increased, so that the monocrystal can quickly pass through the oxygen donor forming area to reduce the oxygen donor effect.
Description
Technical field:
The present invention relates to a kind of production method of monocrystalline, particularly relate to a kind of method reducing pulling of crystals oxygen alms giver.
Background technology:
Oxygen is topmost impurity in vertical pulling (CZ) silicon single-crystal.Oxygen concn in silicon is generally 10
17~ 10
18cm
3the order of magnitude, is present in silicon crystal lattice with gap state.Oxygen is introduced in crystal growing process, due to thermal history impact, because head of single crystal is in high-temperature time length, cooling slowly in crystal temperature-fall period, the oxygen (aobvious electroactive) originally existed with gap form can assemble the aobvious electroactive SiO of generation at about 450 DEG C
4 2-, provide electronics to become oxygen alms giver.
P type 8 inches of monocrystalline oxygen alms givers are subject to influence of oxygen content, because the segregation coefficient of oxygen is greater than 1, so the oxygen in crystal is (its change curve also by crystal pulling process, constantly separate out, liquid level constantly volatilizees impact by the oxygen in crucible) that linearly decline.Head of single crystal oxygen level is high, easily assembles producing oxygen alms giver.
And oxygen alms giver easily brings out fault, defect, cause the warpage of silicon chip, introduce a large amount of secondary defects, affect single-chip mechanical property, have destruction to the electric property of silicon materials and device, reduce the efficiency of conversion of single crystal battery sheet.Comparatively non-oxygen alms giver monocrystalline unit price is low by about 20% for oxygen alms giver monocrystalline, commercially competitiveless, benefit is lower.Current most domestic monocrystalline producer still rests on single generation processing, manufacturing aspect, and the impact of monocrystalline production technique on quality is but seldom studied.
Summary of the invention:
The object of the present invention is to provide a kind of method reducing pulling of crystals oxygen alms giver, effectively can reduce oxygen alms giver effect, improve vertical pulling P type 8 inches of monocrystalline production qualification rates.
Oxygen alms giver is the SiO formed by interstitial oxygen concentration and Siliciumatom acting in conjunction
4 2-electronics is provided to form oxygen alms giver effect, the formation of oxygen alms giver and Crystal Rotation and crucible rotation have direct relation, the rotating speed of crucible is larger, the rotating speed of seed crystal is less, inert gas flow is less, furnace pressure is more large more easily forms oxygen alms giver, and oxygen alms giver easily brings out fault, defect, affect single-chip mechanical property, reduce the efficiency of conversion of single crystal battery sheet.
The present invention, from the root producing oxygen alms giver, by reducing furnace pressure, increasing inert gas flow in crystal pulling process, can accelerate SiO rate of volatilization in crystal pulling process, thus minimizing enters molten Oxygen in silicon content; The precipitation of oxygen in quartz crucible is reduced by the rotating speed reducing crucible; The rotating speed increasing seed crystal changes the thermal history of monocrystalline, thus reduces oxygen alms giver effect, improves monocrystalline qualification rate, reduces costs simultaneously.
The present invention is implemented by following technical scheme: a kind of method reducing pulling of crystals oxygen alms giver, comprises seeding step, shouldering step, turns shoulder step, isometrical step, finishing steps and control oxygen step,
Wherein, in described shouldering step, furnace pressure is 10-14Torr, and the rotating speed of seed crystal is 10-12rpm, and the rotating speed of crucible is 10-12rpm, and inert gas flow is 80-100slpm
In described turn of shoulder step, described furnace pressure is 10-14Torr, and the rotating speed of described seed crystal is 10-12rpm, and the rotating speed of described crucible is 10-12rpm, and described inert gas flow is 80-100slpm;
In described isometrical step, described furnace pressure is 10-14torr, and the rotating speed of described seed crystal is 10-12rpm, and the rotating speed of described crucible is 8-10rpm, and described inert gas flow is 80-100slpm;
Preferably, in described shouldering step, described furnace pressure is 12Torr, and the rotating speed of described seed crystal is 12pm, and the rotating speed of described crucible is 12pm, and described inert gas flow is 100slpm; In described turn of shoulder step, described furnace pressure is 12Torr, and the rotating speed of described seed crystal is 12rpm, and the rotating speed of described crucible is 10rpm, and described inert gas flow is 80slpm; In described isometrical step, described furnace pressure is 12torr, the rotating speed of described seed crystal is 12rpm, the rotating speed of described crucible is 8rpm, described inert gas flow is 80slpm.
Described rare gas element is argon gas.
The invention has the advantages that: the present invention adopts and reduces furnace pressure quickening main pump pumping speed, increases argon flow amount, takes away SiO volatilization gas faster, reduce the content entering molten Oxygen in silicon; The rotating speed of the crucible of reduction single crystal growing, slows down molten silicon and quartz crucible reacts, and reduces the content entering molten Oxygen in silicon, thus minimizing enters oxygen level in monocrystalline, reduces P type monocrystalline oxygen alms giver effect from root; Increase the rotating speed of seed crystal, accelerate latent heat release, improve speed of cooling, allow monocrystalline quickly through oxygen alms giver forming region, reduce oxygen alms giver effect.
Embodiment:
Embodiment 1: a kind of method reducing vertical pulling P type 8 inches of monocrystalline oxygen alms givers, comprises seeding step, shouldering step, turns shoulder step, isometrical step, finishing steps and control oxygen step.
Wherein, in described shouldering step, furnace pressure is 10Torr, and the rotating speed of seed crystal is 10rpm, and the rotating speed of crucible is 10rpm, and inert gas flow is 80s lpm;
In described turn of shoulder step, furnace pressure is 10Torr, and the rotating speed of seed crystal is 10rpm, and the rotating speed of crucible is 10rpm, and inert gas flow is 80slpm;
In described isometrical step, furnace pressure is 10torr, and the rotating speed of seed crystal is 10rpm, and the rotating speed of crucible is 8rpm, and inert gas flow is 80slpm.
Wherein rare gas element is argon gas.
Detect the monocrystalline that embodiment 1 method is produced, wherein the oxygen level at the isometrical 80mm place of monocrystalline is down to 18.9ppma by 20ppma.Oxygen alms giver monocrystalline ratio is down to 1% by 13.28%.
100 monocrystalline that random selecting embodiment 1 method is produced detect RRV value.Carrying out apart from head of single crystal 100mm place cutting (front 100mm exists a large amount of defect, oxygen is high) detection RRV value (radial resistivity evenness) and calculating mean value, detected result is: RRV mean value is 6.1%, the monocrystalline produced than existing methods reduces by 99.5%, and RRV is evenly distributed, anaerobic alms giver.
Embodiment 2: a kind of method reducing vertical pulling P type 8 inches of monocrystalline oxygen alms givers, comprises seeding step, shouldering step, turns shoulder step, isometrical step, finishing steps and control oxygen step.
Wherein, in described shouldering step, furnace pressure is 14Torr, and the rotating speed of seed crystal is 12rpm, and the rotating speed of crucible is 12rpm, and inert gas flow is 100slpm;
In described turn of shoulder step, furnace pressure is 14Torr, and the rotating speed of seed crystal is 12rpm, and the rotating speed of crucible is 12rpm, and inert gas flow is 100slpm;
In described isometrical step, furnace pressure is 14torr, and the rotating speed of seed crystal is 12rpm, and the rotating speed of crucible is 10rpm, and inert gas flow is 100slpm.
Wherein rare gas element is argon gas.
Detect the monocrystalline that embodiment 2 method is produced, wherein the oxygen level at the isometrical 80mm place of monocrystalline is down to 19.1ppma by 20ppma.Oxygen alms giver monocrystalline ratio is down to 1.1% by 13.28%.
100 monocrystalline that random selecting embodiment 2 method is produced detect RRV value.Cutting detection (front 100mm exists a large amount of defect, oxygen is high) RRV value (radial resistivity evenness) is being carried out and calculating mean value apart from head of single crystal 100mm place, detected result is: RRV mean value is 6.3%, the monocrystalline produced than existing methods reduces by 99.3%, and RRV is evenly distributed, anaerobic alms giver.
Embodiment 3: a kind of method reducing vertical pulling P type 8 inches of monocrystalline oxygen alms givers, comprises seeding step, shouldering step, turns shoulder step, isometrical step, finishing steps and control oxygen step.
Wherein, in described shouldering step, furnace pressure is 12Torr, and the rotating speed of seed crystal is 11rpm, and the rotating speed of crucible is 11rpm, and inert gas flow is 90slpm;
In described turn of shoulder step, furnace pressure is 12Torr, and the rotating speed of seed crystal is 11rpm, and the rotating speed of crucible is 11rpm, and inert gas flow is 90slpm;
In described isometrical step, furnace pressure is 12torr, and the rotating speed of seed crystal is 11rpm, and the rotating speed of crucible is 9rpm, and inert gas flow is 90slpm.
Wherein rare gas element is argon gas.
Detect the monocrystalline that embodiment 3 method is produced, wherein the oxygen level at the isometrical 80mm place of monocrystalline is down to 19.05ppma by 20ppma.Oxygen alms giver monocrystalline ratio is down to 1.05% by 13.28%.
100 monocrystalline that random selecting embodiment 3 method is produced detect RRV value.Cutting detection (front 100mm exists a large amount of defect, oxygen is high) RRV value (radial resistivity evenness) is being carried out and calculating mean value apart from head of single crystal 100mm place, detected result is: RRV mean value is 6.25%, the monocrystalline produced than existing methods reduces by 99.35%, and RRV is evenly distributed, anaerobic alms giver.
Embodiment 4: a kind of method reducing vertical pulling P type 8 inches of monocrystalline oxygen alms givers, comprises seeding step, shouldering step, turns shoulder step, isometrical step, finishing steps and control oxygen step.
Wherein, in described shouldering step, furnace pressure is 12Torr, and the rotating speed of seed crystal is 12pm, and the rotating speed of crucible is 12pm, and inert gas flow is 100slpm;
In described turn of shoulder step, described furnace pressure is 12Torr, and the rotating speed of described seed crystal is 12rpm, and the rotating speed of described crucible is 10rpm, and described inert gas flow is 80slpm;
In described isometrical step, described furnace pressure is 12torr, the rotating speed of described seed crystal is 12rpm, the rotating speed of described crucible is 8rpm, described inert gas flow is 80slpm.
Wherein rare gas element is argon gas.
Detect the monocrystalline that embodiment 4 method is produced, wherein the oxygen level at the isometrical 80mm place of monocrystalline is down to 19ppma by 20ppma.Oxygen alms giver monocrystalline ratio is down to 1% by 13.28%.
100 monocrystalline that random selecting embodiment 4 method is produced detect RRV value.Cutting detection (front 100mm exists a large amount of defect, oxygen is high) RRV value (radial resistivity evenness) is being carried out and calculating mean value apart from head of single crystal 100mm place, detected result is: RRV mean value is 6.2%, the monocrystalline produced than existing methods reduces by 99.4%, and RRV is evenly distributed, anaerobic alms giver.
Claims (3)
1. reduce a pulling of crystals oxygen alms giver's method, comprise seeding step, shouldering step, turn shoulder step, isometrical step, finishing steps and control oxygen step, it is characterized in that:
In described shouldering step, furnace pressure is 10-14Torr, and the rotating speed of seed crystal is 10-12rpm, and the rotating speed of crucible is 10-12rpm, and inert gas flow is 80-100slpm
In described turn of shoulder step, described furnace pressure is 10-14Torr, and the rotating speed of described seed crystal is 10-12rpm, and the rotating speed of described crucible is 10-12rpm, and described inert gas flow is 80-100slpm;
In described isometrical step, described furnace pressure is 10-14torr, and the rotating speed of described seed crystal is 10-12rpm, and the rotating speed of described crucible is 8-10rpm, and described inert gas flow is 80-100slpm.
2. a kind of method reducing pulling of crystals oxygen alms giver according to claims 1, it is characterized in that: in described shouldering step, described furnace pressure is 12Torr, and the rotating speed of described seed crystal is 12rpm, the rotating speed of described crucible is 12rpm, and described inert gas flow is 100slpm; In described turn of shoulder step, described furnace pressure is 12Torr, and the rotating speed of described seed crystal is 12rpm, and the rotating speed of described crucible is 10rpm, and described inert gas flow is 80slpm; In described isometrical step, described furnace pressure is 12torr, the rotating speed of described seed crystal is 12rpm, the rotating speed of described crucible is 8rpm, described inert gas flow is 80slpm.
3. the method for any one reduction pulling of crystals oxygen alms giver according to claims 1 or 2, it is characterized in that, described rare gas element is argon gas.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105019017A (en) * | 2015-06-30 | 2015-11-04 | 内蒙古中环光伏材料有限公司 | Method used for reducing oxygen content of czochralski silicon |
| TWI628318B (en) * | 2015-10-15 | 2018-07-01 | 上海新昇半導體科技有限公司 | Method for forming monocrystalline silicon ingot and wafer |
| CN109097825A (en) * | 2018-08-29 | 2018-12-28 | 内蒙古中环协鑫光伏材料有限公司 | A kind of process for preventing pulling of crystals growth from shaking |
| CN109415842A (en) * | 2016-06-27 | 2019-03-01 | 胜高股份有限公司 | The manufacturing method of monocrystalline silicon |
| CN110249080A (en) * | 2016-12-20 | 2019-09-17 | 胜高股份有限公司 | The manufacturing method of monocrystalline silicon |
| CN110387574A (en) * | 2018-04-19 | 2019-10-29 | 台湾积体电路制造股份有限公司 | The control method and semiconductor equipment of chemical concentrations in electrolyte |
| CN112334605A (en) * | 2018-06-25 | 2021-02-05 | 硅电子股份公司 | Method for producing a single crystal of semiconductor material, device for carrying out said method and silicon semiconductor wafer |
| CN113417003A (en) * | 2021-06-22 | 2021-09-21 | 宁夏中欣晶圆半导体科技有限公司 | Large-diameter monocrystalline silicon production method and device capable of reducing oxygen content in head |
| WO2022148402A1 (en) * | 2021-01-08 | 2022-07-14 | 隆基绿能科技股份有限公司 | Crystal pulling process for single-crystal silicon |
| CN115323488A (en) * | 2022-08-16 | 2022-11-11 | 三一集团有限公司 | Process method and production system for pulling straight-pulling monocrystalline silicon |
| CN115404541A (en) * | 2022-10-18 | 2022-11-29 | 四川晶科能源有限公司 | Crystal pulling method |
| WO2023208156A1 (en) * | 2022-04-29 | 2023-11-02 | Tcl中环新能源科技股份有限公司 | Method for reducing oxygen content of monocrystalline silicon, and crystal bar |
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| CN105019017A (en) * | 2015-06-30 | 2015-11-04 | 内蒙古中环光伏材料有限公司 | Method used for reducing oxygen content of czochralski silicon |
| TWI628318B (en) * | 2015-10-15 | 2018-07-01 | 上海新昇半導體科技有限公司 | Method for forming monocrystalline silicon ingot and wafer |
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| CN110387574B (en) * | 2018-04-19 | 2021-10-26 | 台湾积体电路制造股份有限公司 | Method for controlling chemical concentration in electrolyte and semiconductor device |
| CN110387574A (en) * | 2018-04-19 | 2019-10-29 | 台湾积体电路制造股份有限公司 | The control method and semiconductor equipment of chemical concentrations in electrolyte |
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| CN112334605A (en) * | 2018-06-25 | 2021-02-05 | 硅电子股份公司 | Method for producing a single crystal of semiconductor material, device for carrying out said method and silicon semiconductor wafer |
| CN109097825A (en) * | 2018-08-29 | 2018-12-28 | 内蒙古中环协鑫光伏材料有限公司 | A kind of process for preventing pulling of crystals growth from shaking |
| WO2022148402A1 (en) * | 2021-01-08 | 2022-07-14 | 隆基绿能科技股份有限公司 | Crystal pulling process for single-crystal silicon |
| CN113417003A (en) * | 2021-06-22 | 2021-09-21 | 宁夏中欣晶圆半导体科技有限公司 | Large-diameter monocrystalline silicon production method and device capable of reducing oxygen content in head |
| WO2023208156A1 (en) * | 2022-04-29 | 2023-11-02 | Tcl中环新能源科技股份有限公司 | Method for reducing oxygen content of monocrystalline silicon, and crystal bar |
| CN115323488A (en) * | 2022-08-16 | 2022-11-11 | 三一集团有限公司 | Process method and production system for pulling straight-pulling monocrystalline silicon |
| CN115404541A (en) * | 2022-10-18 | 2022-11-29 | 四川晶科能源有限公司 | Crystal pulling method |
| CN115404541B (en) * | 2022-10-18 | 2023-08-25 | 四川晶科能源有限公司 | Crystal pulling method |
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Application publication date: 20150218 |