CN104775150A - Gallium-doping process in vertical-czochralski-method monocrystalline silicon growth - Google Patents
Gallium-doping process in vertical-czochralski-method monocrystalline silicon growth Download PDFInfo
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Abstract
The invention discloses a gallium-doping process in vertical-czochralski-method monocrystalline silicon growth, and relates to the technical field of monocrystalline silicon growth. The process is carried out under an environmental temperature of 20-25 DEG C. The process comprises the following steps: A, weighing is carried out, wherein 0.8-1g of metal gallium is weighed and placed in an alloy spoon; B, melting is carried out, wherein the alloy spoon is placed in a melting furnace, the temperature in the melting furnace is controlled at 50-60 DEG C, and a melting time is 4-7min, such that a molten liquid is obtained; C, fast cooling is carried out, wherein a groove is formed on the end face of a seed crystal, corrosion cleaning is carried out, the molten liquid is poured onto the end face of the seed crystal, the seed crystal with the end face oriented vertically upwards is held with a fixture and is placed in a freezer for cooling for more than 3min under a cooling temperature of -10 DEG C to 0 DEG C; and D, storage is carried out, wherein the seed crystal is fetched from the freezer and is stored in a special-purposed container for later use. With the heavy doping process, gallium doping amount accuracy can be improved, and an alloy addition step before subsequent seeding and diameter-enlarging steps of vertical-czochralski-method monocrystalline silicon growth can be eliminated, such that production efficiency can be greatly improved.
Description
Technical field
The invention belongs to monocrystalline silicon growing Technology field, relate to the charging process in vertical pulling method monocrystalline silicon growing process, specifically doping agent in a kind of charging process--the doping process of gallium.
Background technology
At present, vertical pulling method monocrystalline silicon growing flow process is roughly: reinforced-fusing-seeding-shouldering-isodiametric growth-ending process, wherein crystal silicon raw material and doping agent are mainly put into charging bucket by addition step.The kind of doping agent is fixed according to conduction type N or P, and the doping agent of P type is generally gallium, and N-type doping agent is generally phosphorus.When taking gallium as doping agent, the doping way of doping agent divides two kinds: one is that crystal silicon raw material and gallium are put into charging bucket simultaneously, then the second step of monocrystalline silicon growing is carried out--fusing step, fusing point due to gallium is 29.76 °, gallium can melt in advance, and then stick in charging bucket and cause doping inaccurate, have a strong impact on silicon rod quality.Another way is: first crystal silicon raw material is put into charging bucket and carry out fusing step, then gallium is put into by Reasonable adjustment temperature, and after this adds alloy step, carry out seeding-shouldering step, this way can reduce working efficiency undoubtedly, and operation easier increases.
Summary of the invention
The present invention is in order to solve the problem, devise mixing in a kind of vertical pulling method monocrystalline silicon growing and transfer technique, this heavy doping technique can improve the accuracy of gallium doping, the alloy step that adds in vertical pulling method monocrystalline silicon growing process can also be omitted, greatly enhances productivity.
The technical solution used in the present invention is: mixing in a kind of vertical pulling method monocrystalline silicon growing transfers technique, and key is: described technique is carry out within 20-25 DEG C in envrionment temperature, and its processing step comprises:
A, to weigh: according to processing requirement, take gallium 0.8-1 gram and be placed in alloy spoon;
B, fusing: above-mentioned alloy spoon is put into smelting furnace, control in-furnace temperature 50-60 DEG C, fusing time 4-7min obtains fused solution;
C, fast cooling: slot on seed crystal end face, carry out corrosion cleaning afterwards, poured into by fused solution on seed crystal end face, and then clamp seed crystal with clamper vertically upward with end face and put into refrigeration chamber cooling, cooling time is greater than 3min, cooling temperature-10-0 DEG C;
D, deposit, for subsequent use: seed crystal is taken out in refrigeration chamber, deposits in special container, for subsequent use.
The described seed crystal side of being seed crystal, its end face is square.
Described mode of grooving is 4*3, and groove depth is less than 1mm.
Described corrosion cleaning comprises the steps:
1), seed crystal is put into the plastics casing being furnished with analytical pure nitric acid and analytical pure hydrofluoric acid, wherein, analytical pure nitric acid and analytical pure hydrofluoric acid volume ratio are (6-8): 1, stir with plastic strip, corrode evenly to make seed crystal face;
2), after corrosion is qualified, drag in water rapidly, in order to avoid cause oxidation;
3), seed crystal is dried pack.
Key of the present invention is: change traditional inertial thinking, is fused in seed crystal by doping agent-gallium, instead of adds in charging process and neither add before postorder seeding-shouldering step.Like this, both to have avoided in the fusing step in monocrystalline silicon growing process the inaccurate problem of add-on that is that cause because gallium fusing point is low, and control difficulty can have been reduced again, enhance productivity.
The invention has the beneficial effects as follows: 1, the enforcement of this technique makes " adding alloy " step in follow-up crystal pulling technique omit, and substantially increases working efficiency, this effect is difficult to before being expect; 2, this technique effectively prevent the reinforced inaccurate problem produced after traditional crystal silicon raw material feeds in raw material-melts together with gallium, makes the add-on of doping agent accurate, and then improves the quality of silicon single crystal.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
Mixing in vertical pulling method monocrystalline silicon growing transfers a technique, and described technique is carry out within 20-25 DEG C in envrionment temperature, and its processing step comprises:
A, to weigh: according to processing requirement, take gallium 0.8-1 gram and be placed in alloy spoon;
B, fusing: above-mentioned alloy spoon is put into smelting furnace, control in-furnace temperature 50-60 DEG C, fusing time 4-7min obtains fused solution;
C, fast cooling: slot on seed crystal end face, carry out corrosion cleaning afterwards: 1), seed crystal is put into the plastics casing being furnished with analytical pure nitric acid and analytical pure hydrofluoric acid, wherein, analytical pure nitric acid and analytical pure hydrofluoric acid volume ratio are (6-8): 1, stir with plastic strip, corrode evenly to make seed crystal face; 2), after corrosion is qualified, drag in water rapidly, in order to avoid cause oxidation; 3), seed crystal is dried pack; After being taken out by seed crystal in bag, poured into by fused solution on seed crystal end face, then clamp seed crystal with clamper vertically upward with end face and put into refrigeration chamber cooling, cooling time is greater than 3min, cooling temperature-10-0 DEG C;
D, deposit, for subsequent use: seed crystal is taken out in refrigeration chamber, deposits in special container, for subsequent use.
Like this, in vertical pulling method monocrystalline silicon growing process, the following step is carried out successively: 1, reinforced: crystal silicon raw material is put into quartz crucible; 2, melt: when add crystal silicon raw material in quartz crucible after, single crystal growing furnace cuts out and vacuumizes and makes it to maintain certain pressure range, is then heated to temperature of fusion more than 1420 DEG C, by crystal silicon melting sources; 3, seeding: after the temperature-stable of melted silicon, takes out seed crystal and slowly immerses melted silicon in special container; 4, shouldering; 5, isodiametric growth; 6, finish up; 7, cool.After having grown brilliant body part, if crystal bar and liquid level separated at once, so thermal stresses will make crystal bar appear as mistake and slip line.So in order to avoid this problem and occur, the diameter of crystal bar slowly must be reduced, until become a cusp and separating with liquid level.This process is called ending.
Visible, the seeding in vertical pulling method monocrystalline silicon growing process, " adding alloy " step before shouldering step, on the basis ensureing crystal bar quality, can be omitted, while improving resistivity accuracy rate, substantially increase production efficiency by this doped gallium technique.
Claims (4)
1. mixing in vertical pulling method monocrystalline silicon growing transfers a technique, it is characterized in that: described technique is carry out within 20-25 DEG C in envrionment temperature, and its processing step comprises:
A, to weigh: according to processing requirement, take gallium 0.8-1 gram and be placed in alloy spoon;
B, fusing: above-mentioned alloy spoon is put into smelting furnace, control in-furnace temperature 50-60 DEG C, fusing time 4-7min obtains fused solution;
C, fast cooling: slot on seed crystal end face, carry out corrosion cleaning afterwards, poured into by fused solution on seed crystal end face, and then clamp seed crystal with clamper vertically upward with end face and put into refrigeration chamber cooling, cooling time is greater than 3min, cooling temperature-10-0 DEG C;
D, deposit, for subsequent use: seed crystal is taken out in refrigeration chamber, deposits in special container, for subsequent use.
2. mixing in a kind of vertical pulling method monocrystalline silicon growing according to claim 1 transfers technique, it is characterized in that: the described seed crystal side of being seed crystal, and its end face is square.
3. mixing in a kind of vertical pulling method monocrystalline silicon growing according to claim 1 transfers technique, it is characterized in that: described mode of grooving is 4*3, and groove depth is less than 1mm.
4. mixing in a kind of vertical pulling method monocrystalline silicon growing according to claim 1 transfers technique, it is characterized in that: described corrosion cleaning comprises the steps:
1), seed crystal is put into the plastics casing being furnished with analytical pure nitric acid and analytical pure hydrofluoric acid, wherein, analytical pure nitric acid and analytical pure hydrofluoric acid volume ratio are (6-8): 1, stir with plastic strip, corrode evenly to make seed crystal face;
2), after corrosion is qualified, drag in water rapidly, in order to avoid cause oxidation;
3), seed crystal is dried pack.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111424314A (en) * | 2020-04-30 | 2020-07-17 | 包头美科硅能源有限公司 | Gallium-silicon alloy manufacturing furnace for gallium-doped monocrystalline silicon and manufacturing method thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1114885A1 (en) * | 1999-05-28 | 2001-07-11 | Shin-Etsu Handotai Co., Ltd | CZ SINGLE CRYSTAL DOPED WITH Ga AND WAFER AND METHOD FOR PRODUCTION THEREOF |
| CN101148777A (en) * | 2007-07-19 | 2008-03-26 | 任丙彦 | Method and device for growing gallium-mixing silicon monocrystal by czochralski method |
| CN101319364A (en) * | 2008-06-03 | 2008-12-10 | 天津市环欧半导体材料技术有限公司 | Process for preparing gallium doped elementarysubstance solar energy single crystal |
| CN101555621A (en) * | 2009-05-18 | 2009-10-14 | 浙江大学 | Method for growing silicon single crystal by nitrogen-doped inoculating crystal |
| CN101597788A (en) * | 2009-06-24 | 2009-12-09 | 浙江大学 | Under nitrogen, melt the method that polysilicon prepares the nitrating casting monocrystalline silicon |
| CN101787566A (en) * | 2010-03-25 | 2010-07-28 | 杭州海纳半导体有限公司 | Gallium doping method of Czochralski silicon monocrystalline and doping device thereof |
| CN102409395A (en) * | 2011-11-15 | 2012-04-11 | 浙江长兴众成电子有限公司 | Gallium element doping device and method for Czochralski silicon |
-
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- 2015-04-01 CN CN201510151623.3A patent/CN104775150A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1114885A1 (en) * | 1999-05-28 | 2001-07-11 | Shin-Etsu Handotai Co., Ltd | CZ SINGLE CRYSTAL DOPED WITH Ga AND WAFER AND METHOD FOR PRODUCTION THEREOF |
| CN101148777A (en) * | 2007-07-19 | 2008-03-26 | 任丙彦 | Method and device for growing gallium-mixing silicon monocrystal by czochralski method |
| CN101319364A (en) * | 2008-06-03 | 2008-12-10 | 天津市环欧半导体材料技术有限公司 | Process for preparing gallium doped elementarysubstance solar energy single crystal |
| CN101555621A (en) * | 2009-05-18 | 2009-10-14 | 浙江大学 | Method for growing silicon single crystal by nitrogen-doped inoculating crystal |
| CN101597788A (en) * | 2009-06-24 | 2009-12-09 | 浙江大学 | Under nitrogen, melt the method that polysilicon prepares the nitrating casting monocrystalline silicon |
| CN101787566A (en) * | 2010-03-25 | 2010-07-28 | 杭州海纳半导体有限公司 | Gallium doping method of Czochralski silicon monocrystalline and doping device thereof |
| CN102409395A (en) * | 2011-11-15 | 2012-04-11 | 浙江长兴众成电子有限公司 | Gallium element doping device and method for Czochralski silicon |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111424314A (en) * | 2020-04-30 | 2020-07-17 | 包头美科硅能源有限公司 | Gallium-silicon alloy manufacturing furnace for gallium-doped monocrystalline silicon and manufacturing method thereof |
| CN111424314B (en) * | 2020-04-30 | 2021-07-20 | 包头美科硅能源有限公司 | Gallium-silicon alloy manufacturing furnace for gallium-doped monocrystalline silicon and manufacturing method thereof |
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