CN101624721A - Quartz glass crucible and silicon single crystal pulling method using same - Google Patents
Quartz glass crucible and silicon single crystal pulling method using same Download PDFInfo
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- CN101624721A CN101624721A CN200810210350A CN200810210350A CN101624721A CN 101624721 A CN101624721 A CN 101624721A CN 200810210350 A CN200810210350 A CN 200810210350A CN 200810210350 A CN200810210350 A CN 200810210350A CN 101624721 A CN101624721 A CN 101624721A
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Abstract
The invention provides a quartz glass crucible used for silicon single crystal pulling, in particular to a quartz glass crucible which inhibits the area of crystalline silica obtained by crystallizing amorphous silica to be less than 10% of the area of the crucible and inhibits the density of the dent generated by open bubbles on the inner surface of the crucible to be 0.01-0.2count/mm<2> and to a method which uses the quartz crucible and inhibits the melting loss speed of the inner surface of the crucible to be less than 20mu m/hr for silicon single crystal pulling, thus preventing air holes.
Description
Technical field
The present invention relates to be used to draw silicon single-crystal, and the pore of silicon single-crystal (ピ Application ホ one Le) few quartz glass crucibles and the silicon single crystal pulling method that uses this quartz glass crucibles.
Background technology
Mainly make as the silicon single-crystal that the semiconductor material of silicon wafer etc. uses by the CZ method.
This manufacture method is that the polysilicon heating and melting of putting into quartz glass crucibles is made melted silicon (シ リ コ Application melts liquid), and is that the center makes monocrystalline grow up, it is lifted the method for growing into bar-shaped monocrystalline slowly with the crystal seed that is immersed in this liquid level at high temperature.
The silicon single-crystal that lifts usually uses in melted silicon at the center of crucible, therefore, if the bubble that floats from the internal surface of crucible attached to the interface of silicon single-crystal and melted silicon, it directly enters in the silicon single-crystal as pore.
The bubble that pore is exactly in the silicon single-crystal to be comprised.
In the slicing processes of silicon single-crystal, find that leachy wafer goes out of use, therefore, pore becomes one of reason of goods yield rate reduction.
As the technology that prevents the silicon single-crystal pore, known polycrystalline silicon raw material fusion under the furnace pressure of certain limit that will join quartz crucible, and to carry out the method that the lifts (patent documentation 1: Japanese kokai publication hei 05-9097 communique) of silicon single-crystal than its high furnace pressure.
In addition, known in the stove of certain limit, depress carry out raw materials melt after, the low furnace pressure of furnace pressure with than fusion the time carries out the method (patent documentation 2: TOHKEMY 2000-169287 communique) of the single crystal pulling after the raw materials melt.
The method of existing above-mentioned anti-pore all is when carrying out the lifting of silicon single-crystal, furnace pressure when regulating the polysilicon fusion and the furnace pressure when lifting, prevent that bubble is involved in the method for silicon single-crystal, but, because raw material polysilicon fusion in quartz glass crucibles, lift silicon single-crystal by the molten silicon in this crucible, therefore, the influence of quartz glass crucibles is big.
But, at present the influence of the character pair pore of quartz glass crucibles is not fully studied.
The invention provides specific its condition of the quartz glass crucibles that prevents the silicon single-crystal pore, the quartz glass crucibles that the pore of silicon single-crystal is few.
Summary of the invention
The present invention relates to have the quartz glass crucibles that addresses the above problem of following formation.
(1) quartz glass crucibles, it is the quartz glass crucibles that is used for silicon single-crystal pullup, it is characterized in that, the area by crystalline silica that the amorphous silica crystallization is formed is suppressed at below 10% of crucible inner area, prevents the pore of silicon single-crystal.
(2) quartz glass crucibles is characterized in that, inner surface of crucible opened bubble (Open mood bubble) limitations in density of the recess that produces is at 0.01～0.2count/mm
2, prevent the pore of silicon single-crystal.
(3) method of pulling up of silicon single-crystal is characterized in that, uses the quartz glass crucibles of above-mentioned (1) or above-mentioned (2), carries out lifting of silicon single-crystal below the melting loss speed of inner surface of crucible is suppressed at 20 μ m/hr, prevents pore thus.
First mode of the present invention is to reduce the area of the crystalline silica that the amorphous silica crystallization forms, the percent crystallization in massecuite that makes crystalline silica is the quartz glass crucibles below 10%, by reducing the area of above-mentioned crystalline silica, the air holes when preventing to use this crucible.
At this, the percent crystallization in massecuite of crystalline silica calculates at the area that lifts silicon single-crystal front and back mensuration crystallization silicon-dioxide.
If the inner surface of crucible crystalline silica that exists noncrystallineization of amorphous silica to obtain, then polysilicon fusion is when soaking full melted silicon, at the bubble of the residual easily argon gas as atmosphere gas of inner surface of crucible in crucible.
Therefore, in melted silicon, sneak into above-mentioned bubble, become the reason of pore.
So, the crystallization dislocation (Knot brilliant translocation position of quartz glass crucibles of the present invention by reducing internal surface) and the area of the crystalline silica that produces, bubble is difficult to attached to inner surface of crucible.
Thus, the bubble of sneaking into melted silicon reduces, and can prevent pore.
Second mode of the present invention be make inner surface of crucible to open the recess that bubble produces be certain density (0.01～0.2count/mm
2) quartz glass crucibles, by the existence of above-mentioned recess, the generation of the pore when preventing to use this crucible.
If there is certain recess in inner surface of crucible, then can suppress the reaction of silica glass and melted silicon and the bumping of the SiO gas that generates, reduce the generation of air pocket, therefore, the bubbles volume that enters silicon single-crystal reduces, and can prevent pore.
Third Way of the present invention is suppressed at below the 20 μ m/hr by the melting loss speed with inner surface of crucible for the method for pulling up of the silicon single-crystal of the quartz crucible of above-mentioned first mode of use or second mode, can prevent the pore of silicon single-crystal.
Description of drawings
Fig. 1 is the longitudinal diagram of an embodiment of expression arc discharge device of the present invention and quartz glass crucibles producing device;
Fig. 2 is the longitudinal diagram of an embodiment of expression quartz glass crucibles of the present invention;
Fig. 3 is the longitudinal diagram of other embodiment of expression quartz glass crucibles of the present invention;
Fig. 4 is expression lifts the state of silicon single crystal ingot from the melted silicon in the quartz glass crucibles of an embodiment a longitudinal diagram.
Nomenclature
1-electrode drive mechanism, 2-carbon dioxide process carbon electrode, 3-mould (モ one Le De), 4-driving mechanism, 5-decompression path, the quartzy accumulation horizon of 6-, 10-arc discharge device, 11-quartz glass crucibles, 20--internal layer, 22-skin, the 20A-wall 20B-of portion bend, 20C-bottom, 22-natural quartz glass, 24-synthetic quartz glass.
Embodiment
Below, describe the present invention in detail with reference to embodiment.
The quartz glass crucibles of the present invention's first mode is the quartz glass crucibles that silicon single-crystal pullup is used, it is characterized in that, area by crystalline silica that the amorphous silica crystallization is obtained is suppressed at below 10% of crucible area, prevents the pore of silicon single-crystal.
When there is the crystalline silica that the amorphous silica crystallization forms in inner surface of crucible, the polysilicon fusion, when in crucible, being full of melted silicon, the bubble of the residual easily argon gas as atmosphere gas of inner surface of crucible.
Therefore, sneak into above-mentioned bubble in the melted silicon, become the reason of pore.
In the above-mentioned quartz glass crucibles of the present invention, the area constraints of the crystalline silica that amorphous silica crystallization dislocation is obtained is difficult to attached to inner surface of crucible bubble at total below 10% of internal surface, reduces the bubble of sneaking into melted silicon thus.
When above-mentioned crystalline silica surpassed 10%, the bubble that adheres to increased, so not preferred.
Reduce the amount of the crystalline silica that the crystallization dislocation of amorphous silica produces, can reduce and promote the fracture of silica glass structure, the impurity of arranging again.
In addition, the reaction of the silica glass of silicon and crucible and also be crystalline silica, but the incomplete (SiO of crystal structure at the painted spot (this is called brown ring (Block ラ ウ Application リ Application グ)) that inner surface of crucible is separated out
2-x), the crystalline silica that obtains with above-mentioned crystallization dislocation is different in fact.
Therefore, the area of brown ring is not included in above-mentioned 10% in the present invention.
The quartz glass crucibles of the present invention's second mode is characterized in that, with the limitations in density of opening the recess that bubble produces of inner surface of crucible at 0.01～0.2count/mm
2, prevent the pore of silicon single-crystal.
In the lifting of silicon single-crystal, sometimes the boiling that produces SiO gas owing to the variation of temperature and pressure, if but, then can suppress the bumping of the SiO gas that the reaction of silica glass and melted silicon generates at the recess that inner surface of crucible exists the size of certain density to be fit to.
Preferred especially crucible bottom surface has the recess of certain density.
Mainly by opening bubble formation, size is roughly 0.2～2.0mm to recess.
The density of opening the recess of bubble generation is preferably 0.01～2.0count/mm
2, 0.03～1.5count/mm more preferably
2, 0.05～1.0count/mm more preferably
2
If be lower than 0.01count/mm
2, then do not have this effect, if greater than 0.2count/mm
2, the particle that produces when then bubble breaks reduces the yield rate of silicon single-crystal.
Recess that bubble the produces inner surface of crucible melting loss in the lifting of single crystal silicon of opening of inner surface of crucible makes air entrapment appear at the surface to form, therefore, need only the number of bubbles that the melting loss scope is comprised and be controlled at above-mentioned density.
The condition that vacuumizes when number of bubbles can be made crucible by adjusting etc. is controlled.
The present invention comprises and uses above-mentioned quartz glass crucibles, with the melting loss speed control of inner surface of crucible 20 μ m/hr with lift down silicon single-crystal method.
By using above-mentioned quartz glass crucibles, the melting loss speed of inner surface of crucible is suppressed at 20 μ m/hr lifts silicon single-crystal to get off, can prevent the pore of silicon single-crystal.
SiO gas is mainly by the reaction of the silica glass of melted silicon and crucible and produce.
Therefore, by with the melting loss speed limit of inner surface of crucible in above-mentioned scope, can suppress the generation of SiO gas, can prevent the pore of silicon single-crystal.
When the melting loss speed of inner surface of crucible during faster than above-mentioned scope, it is insufficient to suppress the effect that SiO gas produces.
Obtain the low crucible of melting loss speed of inner surface of crucible, the viscosity that improves silica glass is important.
Preferred 8.6～the 9.2P of viscosity (1550 ℃ time log η) of the silica glass of this moment.Particularly, by fusion heating under high temperature more, reduce OH base concentration or use the methods such as raw material powder that reduced impurity, the melting loss speed of inner surface of crucible is also different because of the condition that lifts of silicon single-crystal, but use the little crucible of melting loss speed of inner surface of crucible, adjusting lifts condition, and the melting loss speed that makes inner surface of crucible is to get final product below the 20 μ m/hr.
As the little crucible of melting loss speed, 1450～1650 ℃ of preferred melting loss temperature and OH base concentration are the quartz crucible of 1～150ppm.
Use the quartz glass crucibles of this condition, making melting loss speed is that the following condition of lifting of 20 μ m/hr is not particularly limited, but is 0.40～66.7kPa as a routine preferred pressure.
Fig. 1 represents an example of the producing device of spendable quartz glass crucibles in the present invention, this device mainly by the mould 3 that the round-ended cylinder shape is arranged, mould 3 is constituted around the driving mechanism 4 of its axis rotation, the arc discharge device 10 that is used for heating mould 3 inboards.
Mould 3 is for example formed by carbon, and portion is formed with a plurality of decompression paths 5 to the mold inside opening within it.
Connect the not shown mechanism of decompressor on the decompression path 5, in mould 3 rotations, can carry out air-breathing from its inner face by decompression path 5.At the inner face of mould 3, can form quartzy accumulation horizon 6 by piling up quartz powder.
This quartz accumulation horizon 6 remains on the inner-wall surface by the centrifugal force of the rotation generation of mould 3.
Reduce pressure by decompression path 5 when utilizing the quartzy accumulation horizon 6 of 10 pairs of maintenances of arc discharge device to heat, quartzy thus accumulation horizon 6 fusings form quartz glass layers.
After the cooling quartz glass crucibles is taken out from mould 3, carry out shaping, manufacture quartz glass crucibles thus.
Arc discharge device 10 possess by highly purified carbon being of forming bar-shaped a plurality of carbon dioxide process carbon electrodes 2, the electrode travel mechanism 1 that moves it when keeping these carbon dioxide process carbon electrodes 2, be used for each carbon dioxide process carbon electrode 2 alive supply units (diagram slightly).
Carbon dioxide process carbon electrode 2 is 3 in this example, but as long as carry out arc-over between carbon dioxide process carbon electrode 2, can for 2 also can be for more than 4.
Shape to carbon dioxide process carbon electrode 2 is also unrestricted.
Carbon dioxide process carbon electrode 2 is configured to more towards the approaching more each other mode of front end.
Power supply can be that to exchange also can be direct current, in this embodiment, connects each phase of three-phase alternating current on three carbon dioxide process carbon electrodes 2.
Fig. 2 represents an example of quartz glass crucibles.
This quartz glass crucibles 20 is made of the 20A of wall portion, bend 20B, bottom 20C, is formed by natural quartz glass 22.
Quartz glass crucibles of the present invention, an embodiment as shown in Figure 2 can form following mode, the mode that the integral body of crucible (or part) is formed by above-mentioned natural quartz glass 22; At least the upper layer of crucible has the mode that easy crystalline above-mentioned silica glass forms by not adding crystallization promoter; The 20A of wall portion, the bend 20B of crucible or mode of forming by natural quartz glass 22 of the outer surface layer of the 20A of wall portion etc. at least.
Fig. 3 represents other embodiment of quartz glass crucibles.
This quartz glass crucibles 20 is made of the 20A of wall portion, bend 20B, bottom 20C, and interior surface layers is formed by synthetic quartz glass 24, and outer surface layer is formed by natural quartz glass 22.
In addition, quartz glass crucibles of the present invention can be as shown in Figure 3, and the interior surface layers of quartz glass crucibles is formed by synthetic quartz glass 24, and the outer surface layer of crucible is formed by natural quartz glass 22.
When making this quartz glass crucibles, pile up crystallization natural quartz powder at the internal surface of rotating mold, (interior all sides) piles up crystallization synthetic quartz powder thereon, and makes at above-mentioned second-order transition temperature (1710 ℃～1780 ℃, preferred 1730 ℃～1750 ℃) heating and melting.
What formed by natural quartz glass 22 also can not be the entire exterior surface layer of crucible, and the outer surface layer of the 20A of wall portion just.
This is because the intensity of the 20A of wall portion is even more important.
The median size of synthetic quartz powder is 350 microns, and particle size range is 60～600um.
The median size of natural quartz powder is 250 microns, and particle size range is 50～500um.
Existing quartz glass crucibles is easy in order to make from the taking-up of mould, and the crucible outside has the crystal quartz layer of the semi-melting state of 100 μ m～300 μ m.
In addition, in quartz glass parts, it is very slow that the crystallization of depth direction (thickness direction) is compared with the crystallization on surface, and the crystalline state on surface is had influence more by force.
The quartz glass crucibles of the unsettled crystal structure in surface, only otherwise eliminate the instability structure on surface, at depth direction with regard to uncrystallizableization.
Therefore, can remove the residual crystal quartz layer of quartz glass crucibles outside surface, crystalline above-mentioned silica glass forms the crucible outside surface by having easily.
Such quartz glass crucibles, crystallization promptly carries out to depth direction from the crucible outside surface, consequently, obtains thick and uniform crystallizing layer, and the intensity of crucible improves.
If use above-mentioned quartz glass crucibles 11 of the present invention, because the intensity of crucible is kept under the high temperature in use, and can not produce in the sidewall of crucible portion, sink to, therefore can obtain high monocrystalline yield rate.
At this, the yield rate of monocrystalline is DF (Dislocation Free) rate of monocrystalline, is to be shown in the mcl stretched portion that lifts with percentage table not comprise direction cross section, footpath and the weight of the part corresponding with lifting direction of principal axis length of part of dislocation (moving of translocation arranged) is arranged with respect to the gross weight that is filled in the polycrystalline silicon raw material in the quartz glass crucibles.
The present invention comprises the manufacture method of the silicon single-crystal that has used this above-mentioned quartz glass crucibles.
Among Fig. 4, an embodiment of silicon single-crystal manufacture method is described.
When using the quartz glass crucibles 11 of this embodiment to carry out silicon single-crystal pullup, in quartz glass crucibles 11 with after the polysilicon fusion, to be immersed among the melted silicon Y by the seed crystal (diagram slightly) that silicon single-crystal constitutes, make quartz glass crucibles 11 when rotating around the crucible axis C, lift seed crystal, form silicon single crystal ingot I thus.
At this moment, the temperature during preferred silicon material fusion is 1420～1600 ℃.
The Si liquation is immersed in the crystallization of silicon Si kind, lift kind of a crystallization while rotating upward, cultivate silicon single-crystal.
In lifting, because silica glass is dissolved in the Si liquation, so the characteristic of quartz crucible has big influence to the characteristic and the yield rate of silicon single-crystal.
Argon partial pressure is preferably 0.40～66.7kPa in the stove when at this moment, lifting silicon.
Temperature when in addition, lifting silicon single-crystal is preferably 1420～1550 ℃.
Embodiment
Embodiments of the invention and comparative example are shown below in the lump.
(embodiment 1～3, comparative example 1～6)
Use the quartz glass crucibles (bore is 28 inches) of proterties shown in the table 1, with furnace pressure 40torr, argon atmosphere gas, lift the time (draw き Xia Time Inter) 100hr, lift silicon single-crystal.
Its result is as shown in table 1.
In addition, in the table 1, inner face crystallization rate (%) is that the silicon metal that produces of the crystallization of amorphous silicon is in the shared ratio of inner surface of crucible.
Open bubble density (count/mm
2) be the inner surface of crucible density of opening the recess of bubble generation.
Melting loss speed (μ m/h) is the speed that the thickness of inner surface of crucible reduces.
Pore containing ratio (%) is the contained stomatal number of a wafer.
Embodiment 1～3 is a quartz glass crucibles of the present invention, and comparative example 1～6 is the outer quartz glass crucibles of the scope of the invention.
Inner face crystallization rate is the inner surface of crucible before and after using by visual inspection, and the area of measuring crystallization calculates.
Opening bubble density is measured by polarized light microscope observing crucible inner face.
Fusion speed is to be calculated by the crucible weight difference before and after using or the thickness difference of transparent layer etc.
The pore containing ratio is to calculate by all silicon wafers after the visual inspection section.
As shown in table 1, when using quartz glass crucibles of the present invention, the pore of silicon single-crystal is especially few, the fabrication yield height of silicon single-crystal.
On the other hand, in the comparative example, the pore of silicon single-crystal is all many, and the yield rate that silicon single-crystal is made is all low.
Table 1
| Inner face crystallization rate (%) | Open bubble density (count/mm 2) | Melting loss speed (μ m/h) | Bubble containing ratio (%) | Single crystal yield rate (%) | |
| Embodiment 1 | ??4 | ??0.05 | ??4 | ??0.001 | ??88 |
| Embodiment 2 | ??10 | ??0.2 | ??20 | ??0.002 | ??90 |
| Embodiment 3 | ??5 | ??0.01 | ??10 | ??0.001 | ??92 |
| Comparative example 1 | ??28 | ??0.07 | ??17 | ??0.16 | ??90 |
| Comparative example 2 | ??7 | ??0.005 | ??18 | ??0.15 | ??86 |
| Comparative example 3 | ??6 | ??0.5 | ??17 | ??0.17 | ??50 |
| Comparative example 4 | ??6 | ??0.05 | ??27 | ??0.25 | ??79 |
| Comparative example 5 | ??90 | ??0.005 | ??30 | ??0.62 | ??76 |
| Comparative example 6 | ??90 | ??1.1 | ??18 | ??0.22 | ??47 |
Claims (8)
1. quartz glass crucibles, it is the quartz glass crucibles that lifts that is used for silicon single-crystal, it is characterized in that, the area by crystalline silica that the amorphous silica crystallization is formed is suppressed at below 10% of crucible area, prevents the pore of silicon single-crystal.
2. quartz glass crucibles is characterized in that, with the limitations in density of opening the recess that bubble produces of inner surface of crucible at 0.01～0.2count/mm
2, prevent the pore of silicon single-crystal.
3. the method for pulling up of silicon single-crystal is characterized in that, uses the quartz glass crucibles of claim 1 or 2, and the melting loss speed of inner surface of crucible is suppressed at below the 20 μ m/hr, carries out lifting of silicon single-crystal, prevents pore thus.
4. the described quartz glass crucibles of claim 2, wherein, the size of recess is 0.2～2.0mm.
5. the described quartz glass crucibles of claim 2, wherein, recess is present in the crucible surface one side.
6. the method for pulling up of the described silicon single-crystal of claim 3, wherein, argon partial pressure is 0.40～66.7kPa in the stove when lifting silicon.
7. the method for pulling up of the described silicon single-crystal of claim 3, wherein, the temperature when lifting silicon single-crystal is 1420～1550 ℃.
8. the method for pulling up of the described silicon single-crystal of claim 3, wherein, the temperature during the silicon material fusion is 1420～1600 ℃.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811832A (en) * | 2010-05-10 | 2010-08-25 | 宁波宝斯达坩埚保温制品有限公司 | Quartz crucible inner surface treatment process |
| CN102080256A (en) * | 2011-03-02 | 2011-06-01 | 镇江荣德新能源科技有限公司 | Quartz crucible |
| CN103201226A (en) * | 2010-11-05 | 2013-07-10 | 信越半导体股份有限公司 | Quartz glass crucible, method for producing same, and method for producing monocrystalline silicon |
| CN103526280A (en) * | 2013-10-12 | 2014-01-22 | 南通路博石英材料有限公司 | Preparation method of crystal pulling quartz glass crucible with groove on inner surface |
| CN104711674A (en) * | 2013-12-09 | 2015-06-17 | 有研新材料股份有限公司 | Method for reducing density of micro-pinholes in monocrystalline Czochralski silicon |
| CN114616361A (en) * | 2019-11-11 | 2022-06-10 | 环球晶圆日本股份有限公司 | Method for producing silicon single crystal |
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2008
- 2008-07-10 CN CN200810210350A patent/CN101624721A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811832A (en) * | 2010-05-10 | 2010-08-25 | 宁波宝斯达坩埚保温制品有限公司 | Quartz crucible inner surface treatment process |
| CN103201226A (en) * | 2010-11-05 | 2013-07-10 | 信越半导体股份有限公司 | Quartz glass crucible, method for producing same, and method for producing monocrystalline silicon |
| CN103201226B (en) * | 2010-11-05 | 2015-08-05 | 信越半导体股份有限公司 | The manufacture method of quartz glass crucibles and manufacture method and silicon single crystal |
| US9376336B2 (en) | 2010-11-05 | 2016-06-28 | Shin-Etsu Handotai Co., Ltd. | Quartz glass crucible, method for producing the same, and method for producing silicon single crystal |
| CN102080256A (en) * | 2011-03-02 | 2011-06-01 | 镇江荣德新能源科技有限公司 | Quartz crucible |
| CN102080256B (en) * | 2011-03-02 | 2013-03-27 | 镇江荣德新能源科技有限公司 | Quartz crucible |
| CN103526280A (en) * | 2013-10-12 | 2014-01-22 | 南通路博石英材料有限公司 | Preparation method of crystal pulling quartz glass crucible with groove on inner surface |
| CN104711674A (en) * | 2013-12-09 | 2015-06-17 | 有研新材料股份有限公司 | Method for reducing density of micro-pinholes in monocrystalline Czochralski silicon |
| CN104711674B (en) * | 2013-12-09 | 2017-06-06 | 有研半导体材料有限公司 | A kind of method of the micro- stomatal frequency in reduction pulling of silicon single crystal inside |
| CN114616361A (en) * | 2019-11-11 | 2022-06-10 | 环球晶圆日本股份有限公司 | Method for producing silicon single crystal |
| CN114616361B (en) * | 2019-11-11 | 2023-12-26 | 环球晶圆日本股份有限公司 | Method for producing silicon single crystal |
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Application publication date: 20100113 |