CN107604431A - N-type monocrystalline silicon manufacturing method and apparatus - Google Patents
N-type monocrystalline silicon manufacturing method and apparatus Download PDFInfo
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Abstract
The present invention provides a kind of n-type monocrystalline silicon manufacture method, and in silicon single-crystal pullup growth course, the rate of temperature fall of 1300 DEG C of 1100 DEG C of temperature ranges is controlled in 3 DEG C/min, 1 DEG C/min；Rate of temperature fall in 600 DEG C of 400 DEG C of temperature ranges is controlled in 3 DEG C/min, 1.5 DEG C/min.Present invention also offers the device for realizing this method, a circular radiating disk is disposed in the upper cavity of body of heater, the temperature range of corresponding silicon single crystal bar is 600 DEG C 400 DEG C, it is double helix radiating tube inside circular radiating disk, each lead into cooling water and argon gas, an annular temperature control disk is installed in the bottom of body of heater, and the temperature range of corresponding silicon single crystal bar is 1300 DEG C 1100 DEG C, and the part argon gas of circular radiating disk outflow is entered in annular temperature control disk by current divider.Using the manufacturing method and apparatus of the present invention, improve the effective depth of body of heater, and avoid OSF generation.
Description
Technical field
The present invention relates to a kind of manufacturing method and apparatus of n-type monocrystalline silicon, the monocrystal rod cooling control technology more particularly in vertical pulling method monocrystalline silicon growing technique, preparation has the monocrystalline silicon without stacking fault.
Background technology
Monocrystalline silicon is the basic material of most semiconductor electronic component manufactures, and in the manufacturing process of monocrystalline silicon, most-often used is vertical pulling method（Czochralski, abridge CZ）.In vertical pulling method, polysilicon is to be filled in quartz glass crucibles（Also referred to as silica crucible）In, then heat melting and form melted silicon, seed crystal is contacted with melted silicon, and promote crystal growth by slowly rotating up lifting, silicon is in seed crystal and the interface solidification and crystallization of melted silicon, formation monocrystal silicon.After neck grows up to, by reducing the rate of pulling, reducing melt temperature to expand crystal diameter, aimed dia is made up to.Then the rate of pulling and melt temperature and the melt level for compensating decline are controlled, keeps the isodiametric growth of crystal.Before crystal growth terminates, complete to finish up by way of accelerating the rate of pulling, heat crucible, crystal is separated with remaining melted silicon.
During monocrystalline silicon growing, grown-in defects, three kinds of defects therein can be produced：COP（Crystal Originated
Particle, cavity caused by the cohesion of hole）, OSF（Oxidation Induced Stacking
Fault, aoxidize the stacking fault of induction）And the caused dislocation ring cluster by silicon cohesion between lattice（Silicon type dislocation defects between lattice, I-defect）.In recent years, with the continuous progress of microelectronic technique, the requirement to silicon chip quality improves constantly, and grown-in defects be present not in the silicon wafer surface of manufacture device.Therefore, more and more method of the manufacture without grown-in defects chip is widely studied, and epitaxy single-crystal silicon chip of the manufacture with high added value is used to by the method for the high epitaxy single-crystal silicon layer of one layer of crystalline perfection of vapor deposition growth in silicon wafer surface.Epitaxially grown layer is considered as zero defect layer because its crystallinity is high, and then the device made on epitaxial layer can significantly improve its performance.Before, generally believe the crystalline perfection of epitaxial layer is not influenceed by the monocrystalline silicon piece as substrate, but as defect detecting device is more and more sensitive and flaw evaluation standard is more and more stricter, the defects of monocrystalline silicon piece is transmitted to epitaxial layer and the fact that form epitaxy defect had been found to.Increasing research shows that the grown-in defects OSF in silicon wafer is easily transmitted to epitaxial layer and forms epitaxy defect, therefore during high quality epitaxial silicon wafer is prepared, it is necessary to remove it.
In fact, oxygen plays a part of two aspects in crystal, it is beneficial aspect first, improving the mechanical strength of silicon wafer；Second, having done a kind of impurities phase causes point defect and dislocation defects etc., it is harmful aspect.Research finds, radially-arranged oxide particle（Formed by the interaction in oxygen and room）The spatial band of formation, can be that OSF rings reveal by thermal oxide.OSF is in crystal pull growth course, is formed under given conditions.In-depth study shows, parameter v/G is drawn high in specific crystal（V is pulling rate, and G is the axial-temperature gradient of near interface）Scope, OSF thermal oxides nucleation.（G. Rozgonyi,
p149, Semiconductor Silicon 2002 vol1, Electr℃hemical S℃iety pr℃eeding volume 2002-2）, patent CN99807092, CN200380102309, CN200610172531 and CN201310072159 suggested a variety of methods to eliminate OSF.For p-type crystal, the clear and definite OSF of this condition can of parameter formation is only drawn high with crystal, but it is relevant with the oxygen concentration in crystal ingot also with the thermal history evolution of crystal ingot growth for n-type crystal, OSF formation.OSF in n-type crystal, not only it is induced in p-type crystal under conditions of OSF nucleation, and can be also induced in the condition wide range that OSF is nucleated in than p-type crystal.In n-type crystal, rely solely on control crystal and draw high parameter in particular range, no OSF crystal can not be obtained.
The content of the invention
It is an object of the invention to provide a kind of method and apparatus for preparing no stacking fault n-type monocrystalline silicon, suppress the interior caused OSF due to thermal oxide induction of silicon single crystal rod.In order to suppress the OSF in n-type crystal, we have discovered that in crystal growing process, the decline for controlling crystal temperature effect is very effective, especially in following two temperature ranges：1300 DEG C -1100 DEG C and 600 DEG C -400 DEG C.In 1300 DEG C of -1100 DEG C of scopes, temperature is relatively higher, the easy fast cooling of crystal ingot, but rate of temperature fall should be relatively slower；And at 600 DEG C -400 DEG C, crystal ingot generally cooling is very slow, fast cooling is actually needed, so as to suppress OSF generation.
In order to reach object above, the present invention uses following technical scheme：In silicon single-crystal pullup growth course, the rate of temperature fall of two temperature ranges is controlled, first, in 1300 DEG C of -1100 DEG C of scopes, rate of temperature fall is controlled in 3 DEG C/min-1 DEG C/min；Second, in the range of 600 DEG C -400 DEG C, rate of temperature fall is controlled in 3 DEG C/min-1.5 DEG C/min.
Preferably, a circular radiating disk is disposed in the upper cavity of body of heater, the temperature range of its position correspondence silicon single crystal rod is 600 DEG C -400 DEG C；One annular temperature control disk is installed in the bottom of body of heater, the temperature range of its position correspondence silicon single crystal rod is 1300 DEG C -1100 DEG C.The rate of temperature fall of 1300 DEG C -1100 DEG C, 600 DEG C -400 DEG C of two temperature ranges is controlled by circular radiating disk and annular temperature control disk.
Circular radiating disk is prepared by stainless steel, and inside is double helix radiating tube, each leads into cooling water and argon gas.Argon gas is accessed by upper of furnace body, after being circulated in circular radiating disk, is entered in current divider；Current divider is arranged in body of heater, controls the part argon gas from the outflow of circular radiating disk to enter in annular temperature control disk, and the argon gas for being introduced into annular temperature control disk is discharged by the circumferential weld of current divider bottom.Annular temperature control disk occupies the area of melted silicon according to the diameter design to be grown crystal, and the inside diameter ranges of annular temperature control disk are between 250mm-450mm.The shunt volume of current divider is up to 0-80%, the cooling velocity of 1300 DEG C of -1100 DEG C of silicon single crystal bars is controlled by the flow of argon gas, this section mainly plays a part of reducing rate of temperature fall, by rate of temperature fall control in the range of 3 DEG C/min-1 DEG C/min, avoids high speed cooling band from carrying out OSF generation.
Annular temperature control disk is made up of carbon material, prevents metal approach silicon melt surface from volatilizing and produces pollution.After argon gas circulates in annular temperature control disk, discharged by the circumferential weld of annular temperature control disk bottom, flowed through on the surface of silicon melt, play the SiO gases taken up in silicon melt, reduce the effect of oxygen content in crystal.
Preferably, in silicon single crystal rod pulling process, argon gas flow control is between 200L/min-400L/min in cavity.
Preferably, in silicon single crystal rod pulling process, when crystal bar head temperature is less than 400 DEG C, the pulling growth process of crystal bar stops, and crystal bar is by lifting directly up to the region of lower temperature.
To realize the above method, present invention also offers a kind of n-type manufacturing device of single crystal silicon, and in the upper cavity of body of heater, the temperature range of corresponding silicon single crystal rod is 600 DEG C -400 DEG C of position, disposes a circular radiating disk；In the bottom of body of heater, the temperature range of corresponding silicon single crystal rod is 1300 DEG C -1100 DEG C of position, installs an annular temperature control disk.
It is double helix radiating tube inside circular radiating disk, each leads into cooling water and argon gas；Argon gas is accessed by upper of furnace body, after being circulated in circular radiating disk, is entered in current divider；Current divider is arranged in body of heater, controls the part argon gas from the outflow of circular radiating disk to enter in annular temperature control disk.
Compared with prior art, n-type monocrystalline silicon manufacturing method and apparatus provided by the invention, by controlling the rate of temperature fall of 1300 DEG C -1100 DEG C and 600 DEG C -400 DEG C of two temperature ranges, it can improve the effective depth of body of heater, and avoid OSF generation.
Brief description of the drawings
Fig. 1 is circular radiating disk of the present invention, current divider and annular temperature control dish structure schematic diagram.
In figure：1 circular radiating disk, 2 argon gas, 3 current dividers, 4 circumferential welds, 5 annular temperature control disks, 6 circumferential welds, 7 silicon single crystal rods.
Embodiment
Silicon single crystal rod 7 for growing 8 inches, 28 inches of silica crucible is used, adds 140Kg polycrystalline silicon raw materials, heating fusing is carried out after vacuumizing, forms melted silicon.
N-type monocrystalline silicon growing device in the upper cavity of body of heater as shown in figure 1, dispose a circular radiating disk 1；One annular temperature control disk 5 is installed in the bottom of body of heater.The inside of circular radiating disk 1 is double helix radiating tube, each leads into cooling water and argon gas 2；Argon gas 2 is accessed by upper of furnace body, after being circulated in circular radiating disk 1, is entered in current divider 3；Current divider 3 is arranged in body of heater, controls the part argon gas flowed out from circular radiating disk 1 to enter in annular temperature control disk 5.The argon gas for being introduced into annular temperature control disk 5 is discharged by the circumferential weld 4 of the bottom of current divider 3；After argon gas circulates in annular temperature control disk 5, discharged by the circumferential weld 6 of the annular bottom of temperature control disk 5, flowed through on the surface of silicon melt.
Crystal bar is tested by growing, the R type thermocouples made using platinum-rhodium alloy, measure draws the temperature profile of crystal bar, and determines crystal bar corresponding height from silicon melt level at 1300 DEG C, 1100 DEG C, 600 DEG C, 400 DEG C according to temperature profile.Based on temperature profile, it may be determined that and annular heat dissipation plate 1 and annular temperature control disk 5 are controlled from the height of silicon melt level, so that the temperature range of the position correspondence silicon single crystal rod of circular radiating disk is 600 DEG C -400 DEG C；The temperature range of the position correspondence silicon single crystal rod of annular temperature control disk is 1300 DEG C -1100 DEG C.
The rate of temperature fall in the range of 600 DEG C -400 DEG C of circular radiating disk raising is used alone, the internal diameter of circular radiating disk is 260mm, center and liquid level center superposition.According to thermocouple measurement result, when boule temp is 1300 DEG C, 1100 DEG C, 600 DEG C, 400 DEG C, the height corresponding to liquid level is respectively 45mm, 190mm, 560mm, 780mm.Circular radiating disk is arranged on the height apart from liquid level 550mm-750mm, to improve rate of temperature fall of the crystal bar in the range of 600 DEG C -400 DEG C.After installing circular radiating coil pipe additional, when boule temp is 400 DEG C, the height apart from liquid level is down to 690mm.
Annular temperature control disk, which is used alone, reduces the cooling velocity of 1300 DEG C of -1100 DEG C of silicon single crystal bars, and the internal diameter of annular temperature control disk is 260mm, center and liquid level center superposition, is placed in the height apart from liquid level 50mm-200mm.After installing annular temperature control disk additional, during 1100 DEG C of boule temp, carried apart from the height of liquid level to 240mm.
Heat dissipation plate and temperature control disk are used simultaneously, using water cooling and argon gas flow-dividing control, cooling velocity in the range of 1300 DEG C -1100 DEG C of silicon single crystal bar and the rate of temperature fall in the range of 600 DEG C -400 DEG C can be controlled simultaneously.
Embodiment 1
Using simultaneously using the method for heat dissipation plate and temperature control disk, 8 inches of growth<100>The n-type silicon monocrystalline in direction, resistivity are 10-15 ohmcms, and the pull rate of crystal is arranged to 1.2mm/min.In 1300 DEG C of -1100 DEG C of scopes, argon gas flow velocity 20%, rate of temperature fall is controlled in 2.5 DEG C/min；In the range of 600 DEG C -400 DEG C, using water cooling and argon gas dual-cooled, rate of temperature fall is controlled in 1.8 DEG C/min.After boule growth success, cut from crystal bar diverse location and take out test piece, be placed into oxidation furnace, 60min oxidation is carried out at 1100 DEG C.Afterwards, do not find OSF in all test pieces, show that OSF original positions defect is all not present in whole crystal bar.
Embodiment 2
Using simultaneously using the method for heat dissipation plate and temperature control disk, 8 inches of growth<100>The n-type silicon monocrystalline in direction, resistivity are 10-15 ohmcms, and the pull rate of crystal is arranged to 1.2mm/min.In 1300 DEG C of -1100 DEG C of scopes, argon gas flow velocity 40%, rate of temperature fall is controlled in 2.0 DEG C/min；In the range of 600 DEG C -400 DEG C, using water cooling and argon gas dual-cooled, rate of temperature fall is controlled in 2.0 DEG C/min.After boule growth success, cut from crystal bar diverse location and take out test piece, be placed into oxidation furnace, 60min oxidation is carried out at 1100 DEG C.Afterwards, do not find OSF in all test pieces, show that OSF original positions defect is all not present in whole crystal bar.
Embodiment 3
Using simultaneously using the method for heat dissipation plate and temperature control disk, 8 inches of growth<100>The n-type silicon monocrystalline in direction, resistivity are 10-15 ohmcms, and the pull rate of crystal is arranged to 1.5mm/min.In 1300 DEG C of -1100 DEG C of scopes, argon gas flow velocity 60%, rate of temperature fall is controlled in 1.5 DEG C/min；In the range of 600 DEG C -400 DEG C, using water cooling and argon gas dual-cooled, rate of temperature fall is controlled in 3.0 DEG C/min.After boule growth success, cut from crystal bar diverse location and take out test piece, be placed into oxidation furnace, 60min oxidation is carried out at 1100 DEG C.Afterwards, do not find OSF in all test pieces, show that OSF original positions defect is all not present in whole crystal bar.
Embodiment 4
Using simultaneously using the method for heat dissipation plate and temperature control disk, 12 inches of growth<100>The n-type silicon monocrystalline in direction, resistivity are 10-15 ohmcms, and the pull rate of crystal is arranged to 1.2mm/min.In 1300 DEG C of -1100 DEG C of scopes, argon gas flow velocity 60%, rate of temperature fall is controlled in 2.5 DEG C/min；In the range of 600 DEG C -400 DEG C, using water cooling and argon gas dual-cooled, rate of temperature fall is controlled in 2.0 DEG C/min.After boule growth success, cut from crystal bar diverse location and take out test piece, be placed into oxidation furnace, 60min oxidation is carried out at 1100 DEG C.Afterwards, do not find OSF in all test pieces, show that OSF original positions defect is all not present in whole crystal bar.
Embodiment 5
Using simultaneously using the method for heat dissipation plate and temperature control disk, 12 inches of growth<100>The n-type silicon monocrystalline in direction, resistivity are 10-15 ohmcms, and the pull rate of crystal is arranged to 1.2mm/min.In 1300 DEG C of -1100 DEG C of scopes, argon gas flow velocity 60%, rate of temperature fall is controlled in 2.8 DEG C/min；In the range of 600 DEG C -400 DEG C, using water cooling and argon gas dual-cooled, rate of temperature fall is controlled in 2.0 DEG C/min.After boule growth success, cut from crystal bar diverse location and take out test piece, be placed into oxidation furnace, 60min oxidation is carried out at 1100 DEG C.Afterwards, do not find OSF in all test pieces, show that OSF original positions defect is all not present in whole crystal bar.
Comparative example 1
Using the method for embodiment 1,8 inches are grown<100>The n-type silicon monocrystalline in direction, resistivity are 10-15 ohmcms, and the pull rate of crystal is arranged to 1.2mm/min.Heat dissipation plate is not provided with above crystal bar in cavity, in 1300 DEG C of -1100 DEG C of scopes, rate of temperature fall is controlled in 2.5 DEG C/min；In the range of 600 DEG C -400 DEG C, rate of temperature fall is 1.1 DEG C/min.After boule growth success, cut from crystal bar diverse location and take out test piece, be placed into oxidation furnace, 60min oxidation is carried out at 1100 DEG C.There is substantial amounts of OSF to be observed at the top of crystal bar, or even in crystal bar afterbody also with the presence of OSF.
Comparative example 2
Using the method for embodiment 1,8 inches are grown<100>The n-type silicon monocrystalline in direction, resistivity are 10-15 ohmcms, and the pull rate of crystal is arranged to 1.5mm/min.Radiating tube is not provided with above crystal bar in cavity, in 1300 DEG C of -1100 DEG C of scopes, rate of temperature fall is 3.1 DEG C/min；In the range of 600 DEG C -400 DEG C, rate of temperature fall is 1.8 DEG C/min.After boule growth success, cut from crystal bar diverse location and take out test piece, be placed into oxidation furnace, 60min oxidation is carried out at 1100 DEG C.Whole crystal bar is all found to have OSF presence, especially at center wafer R/2（R is the radius of chip）, intensive OSF defects are found.
Claims (9)
1. a kind of manufacture method of n-type monocrystalline silicon, it is characterised in that in silicon single-crystal pullup growth course, the rate of temperature fall of two temperature ranges is controlled, first, in 1300 DEG C of -1100 DEG C of scopes, rate of temperature fall is controlled in 3 DEG C/min-1 DEG C/min；Second, in the range of 600 DEG C -400 DEG C, rate of temperature fall is controlled in 3 DEG C/min-1.5 DEG C/min.
2. n-type monocrystalline silicon manufacture method according to claim 1, it is characterised in that in the upper cavity of body of heater, the temperature range of corresponding silicon single crystal rod is 600 DEG C -400 DEG C of position, disposes a circular radiating disk（1）；In the bottom of body of heater, the temperature range of corresponding silicon single crystal rod is 1300 DEG C -1100 DEG C of position, installs an annular temperature control disk（5）.
3. n-type monocrystalline silicon manufacture method according to claim 2, it is characterised in that circular radiating disk（1）Prepared by stainless steel, inside is double helix radiating tube, each leads into cooling water and argon gas（2）.
4. n-type monocrystalline silicon manufacture method according to claim 3, it is characterised in that argon gas（2）Accessed by upper of furnace body, in circular radiating disk（1）After interior circulation, current divider is entered（3）In；Current divider（3）In body of heater, current divider（3）Shunt volume up to 0-80%, control from circular radiating disk（1）The part argon gas of outflow enters annular temperature control disk（5）In, it is introduced into annular temperature control disk（5）Argon gas pass through current divider（3）The circumferential weld of bottom（4）Discharge；Argon gas is in annular temperature control disk（5）After interior circulation, pass through annular temperature control disk（5）The circumferential weld of bottom（6）Discharge, flows through on the surface of silicon melt.
5. the n-type monocrystalline silicon manufacture method according to claim 2,3 or 4, it is characterised in that annular temperature control disk（5）It is made up of carbon material, annular temperature control disk（5）The area of melted silicon is occupied according to the diameter design to be grown crystal, annular temperature control disk（5）Inside diameter ranges between 250mm-450mm.
6. the n-type monocrystalline silicon manufacture method according to claim any one of 1-5, it is characterised in that in silicon single crystal rod pulling process, argon gas flow control is between 200L/min-400L/min in cavity.
7. the n-type monocrystalline silicon manufacture method according to claim any one of 1-6, it is characterised in that in silicon single crystal rod pulling process, when crystal bar head temperature is less than 400 DEG C, the pulling growth process of crystal bar stops, and crystal bar is by lifting directly up to the region of lower temperature.
8. a kind of n-type manufacturing device of single crystal silicon for realizing claim 1 methods described, it is characterised in that in the upper cavity of body of heater, the temperature range of corresponding silicon single crystal rod is 600 DEG C -400 DEG C of position, disposes a circular radiating disk（1）；In the bottom of body of heater, the temperature range of corresponding silicon single crystal rod is 1300 DEG C -1100 DEG C of position, installs an annular temperature control disk（5）.
9. n-type manufacturing device of single crystal silicon according to claim 8, it is characterised in that circular radiating disk（1）Inside is double helix radiating tube, each leads into cooling water and argon gas（2）；Argon gas（2）Accessed by upper of furnace body, in circular radiating disk（1）After interior circulation, current divider is entered（3）In；Current divider（3）In body of heater, control from circular radiating disk（1）The part argon gas of outflow enters annular temperature control disk（5）In.
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| CN109537045A (en) * | 2018-12-29 | 2019-03-29 | 徐州晶睿半导体装备科技有限公司 | For the heat exchanger of silicon ingot growth, the growth furnace of silicon ingot and the method for preparing silicon ingot |
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| CN113235157A (en) * | 2021-06-24 | 2021-08-10 | 连城凯克斯科技有限公司 | Monocrystalline silicon growth furnace with double pulling auxiliary chambers |
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