CN105483817A - Monocrystalline silicon growth ultrasonic wave oxygen control method - Google Patents

Monocrystalline silicon growth ultrasonic wave oxygen control method Download PDF

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CN105483817A
CN105483817A CN201510899269.2A CN201510899269A CN105483817A CN 105483817 A CN105483817 A CN 105483817A CN 201510899269 A CN201510899269 A CN 201510899269A CN 105483817 A CN105483817 A CN 105483817A
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ultrasonic wave
silicon
crystal
melt
oxygen
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CN105483817B (en
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张俊宝
宋洪伟
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Shanghai Chaosi Semiconductor Co.,Ltd.
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SHANGHAI ADVANCED SILICON TECHNOLOGY Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02Elements
    • C30B29/06Silicon

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  • Crystallography & Structural Chemistry (AREA)
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  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention discloses a monocrystalline silicon growth ultrasonic wave oxygen control method. In a device of the monocrystalline silicon growth ultrasonic wave oxygen control method, the surface of silicon melt is provided with a set of ultrasonic wave, and a set of ultrasonic wave vibration heads are uniformly distributed on a circle coaxial to silicon single crystal rods and a crucible; the distance between each pair of ultrasonic wave vibration heads is controlled to be 1.5 to 2 times of the distance from a corresponding ultrasonic wave vibration head to the crucible wall; the ultrasonic wave vibration heads are made of a high-purity quartz material, and are stretched to be 10 to 15mm below the surface of the silicon melt; and the depth is maintained in the process of crystal growth. In silicon single crystal equal-diameter growth process, ultrasonic wave oscillation is introduced so as to inhibit heat natural convection in a high oxygen concentration zone around the crucible, accelerate flow of the silicon melt from the center to the surrounding caused by crystal rotation, promote volatilization of oxygen on a free surface, reduce solubility of Si-O gas in the silicon melt, promote volatilization of Si-O on the surface of the silicon melt, and control oxygen content of obtained crystals.

Description

Monocrystalline silicon growing ultrasonic wave control oxygen technology
Technical field
The present invention relates to a kind of monocrystalline silicon growing ultrasonic wave control oxygen technology, be specifically related to the control of oxygen level in silicon melt, particularly in silicon melt, introduce ultrasonic wave, silicon melt is vibrated, reduce the solubleness of oxygen element in silicon melt.
Background technology
In the manufacturing process of silicon single crystal, the most often use vertical pulling method (Czochralski, abbreviation CZ), in vertical pulling method, polysilicon is filled in quartz glass crucibles (also claiming quartz crucible), and then heating and melting forms melted silicon, immerse in melted silicon after seed crystal on rotary pulling, silicon, at the interface solidification and crystallization of seed crystal and molten solution, forms silicon single crystal rod (ingot).
Oxygen is that in CZ method silicon single-crystal, content is the highest, and a kind of impurity that behavior is the most complicated, its content can up to 3 × 10 18/ cm 3.Oxygen is the element of silicon single-crystal most study, to the control of its content, is one of research topic important in silicon materials field always.In silicon monocrystal growth process, silicon reacts with the quartz crucible containing silicon, and generating silicon monoxide and enter melt, is the main source of Oxygen in silicon.Main and the temperature of the dissolution rate of quartz crucible, furnace chamber internal pressure, quartz crucible surface state, the factors such as the boundary layer thickness on crucible/melt interface are relevant.Temperature is higher, and pressure is lower, surface irregularity is larger, and the dissolution rate of crucible is faster.According to the test data that CHANEL and YARKER provides, the dissolution rate of quartz crucible is 1.5mg/cm 2h.There are three concentration gradient distributed areas in the oxygen be dissolved in silicon melt, i.e. three frictional belt: the frictional belt being respectively quartz crucible and melt interface are hyperoxia districts in quartz crucible.Oxygen enters melt inside by the thermal natural convection of melt.Two is frontier districts of crystal and melt interface, Shi Zhongyang district.Oxygen enters into crystal by thermal natural convection and forced convection by frictional belt.Three is melt and gas interface frictional belt, is oxygen-depleted zone.Oxygen is volatilized by frictional belt.The oxygen of about more than 99% evaporate in furnace chamber from bath surface, and only the oxygen of small portion enters in crystal.Visible, oxygen mixes the concentration of crystal, depends on the area at three diffusion boundary layers and three interfaces.Boundary layer thickness depends on melt thermal convection, and interfacial area depends on the diameter etc. of charge amount and crucible size and shape and crystal.The ratio that wherein interfacial area and the melt free surface of crucible and melt are amassed is the important factor determining to enter oxygen level in crystal.In crystal growing process, along with the growth of crystal, crystal weight constantly increases, and the melt weight in crucible reduces thereupon.So the distribution of oxygen in crystal is uneven, be generally crystal head content high, afterbody content is low.Position, germ nucleus content is high, and edge content is low.
Oxygen is in interstitial site in silicon crystal lattice, to the effect of dislocation nail nipping bundle, increases the physical strength of crystal, avoids silicon chip, in device heat treatment process, deformation occurs.In silicon single-crystal, the oxygen of high-content is in hypersaturated state, at a proper temperature can precipitation precipitating with the form that oxygen and silicon form complexing body.The complex compound that oxygen and silicon are formed is very complicated, and form is different at different temperatures, also not identical to silicon single-crystal performance impact.The precipitation of oxygen can be used to form controllable lattice imperfection, is used for inducing fault and dislocation loop, carries out Intrinsic gettering, form clean area on polished section surface to metallic impurity and satiety point defect.Oxygen precipitation forms Thermal donor at 450 DEG C of temperature, and its concentration reaches as high as and reaches 5 × 10 15/ cm 3.The verity of silicon single-crystal resistance is gently mixed in impact, and P type resistivity is raised, and N-type resistivity reduces, therefore gently mixes silicon single crystal flake needs and heat-treat at 650 DEG C of temperature, to eliminate the impact of Thermal donor.The defect that oxygen precipitation induces produces adverse influence to the yield rate of unicircuit.Particularly along with the development of unicircuit, integrated level improves constantly, and live width constantly reduces, and this impact is more outstanding.
Traditional control oxygen level, mainly controls in monocrystalline growing process.Comprise little feeding quantity, for the crucible of intended size, it is low that little feeding quantity will obtain oxygen level, and the heating power that little feeding quantity needs is low, and volumetric ratio diminishes, and little with the contact area of crucible, in melt, the meltage of oxygen is relatively little.The thermal convection of little feeding quantity melt weakens.This makes oxygen concn will change to the transmission in melt centre, is namely changed to flooding mechanism by convection mechanism.The transmission speed of oxygen reduces, and oxygen can be volatilized fully, and the oxygen concn in melt is reduced, thus in crystal, oxygen concn reduces.Control unmelted polycrystalline silicon temperature, reduce temperature during silicon fusing, the dissolution rate of quartz crucible can be reduced, thus reduce the oxygen level in melted silicon.Increase the Melt Stability time, stablize for a long time and the oxygen of nearly 95% can be made to evaporate from melt free surface with the form of silicon monoxide, form a trim point.Adopt heat reflection cover, or claim heat shielding, reduce actual thermal power, simultaneously because heat shielding can help crystals cooled, crucible can be made to be set in higher zero position, accelerate the Ar gas velocity of bath surface, accelerate silicon monoxide to volatilize from bath surface, reduce the oxygen level in crystal.Control the speed of growth of crystal, the change of oxygen concn and the speed of growth is not a linear relationship.In minor diameter crystal (3 inches or 4 inches) situation, the silicon single-crystal that pulling rate grows within the scope of 3.54 inches to 4.72 inch per hours is hyperoxia.Therefore speed that major diameter single crystal silicon rod is is grown generally lower than 3.54 inch per hours.Reduce furnace inner gas pressure, low pressure is conducive to making silicon monoxide effectively from melt free surface volatilization, thus the oxygen concn in melt is reduced, and the oxygen concn therefore in crystal is also along with reduction.Crucible rotation has larger impact to oxygen level in crystal, increases the dissolution rate that crucible rotation can accelerate crucible, thus the oxygen level in melt is increased.It should be noted that the oxygen level of crystal ingot afterbody is usually higher, this is that crucible is in very high position and heating power is very high, and crucible has very high dissolution rate because melt remaining in crucible constantly reduces.When crystal growth covers melt most surfaces gradually, the minimizing of free surface causes oxygen to reduce from bath surface evaporation rate, thus adds oxygen concn in melt.But simultaneously in crucible, melt amount is little, the contact area of crucible also melt is little, and the amount of dissolving also reduces, and it is that oxygen level is very high that these factors are combined the effect caused, and conventional art still shows thorough solution.Increase crucible diameter size, for given feeding quantity and crystalline size, large crucible size has larger effective volatilization its own face, and simultaneously because volumetric ratio is little, thermal convection is also little, and the transmission speed of oxygen is also lower.Ideally, crucible diameter and crystal diameter are than being 3:1 or larger.Crystal rotation, crystal rotation can not the oxygen level of effective influence crystal, but has important impact for the distributing homogeneity of oxygen in crystal.The rotating drive melt of crystal flows to growth interface from center, its radial evenly increase.Usually represent with ORG, require ORG≤5%, but brilliant turning is subject to crucible size, crystalline size, crystal orientation, liquid level position, the impact of the many factors such as the speed of growth, but brilliant turning accelerates to there will be the plotted point that crystalline substance turns and crucible turns, and cause crystal facet width to become large, profile is irregular, circularity is deteriorated, the cooling of melt simultaneously can be accelerated, and time serious, melt there will be swing, and even crystal can depart from from melt.As mentioned above, utilize and change monocrystalline growing process, although have certain effect to the control of oxygen level in growing single-crystal, the amplitude controlled is little, only can control within the scope of several ppm.The another kind of method controlling oxygen level is magnetic field crystal pulling method, pulling technique under the action of a magnetic field that horizontal magnetic field, vertical magnetic field or horizontal and vertical combine, suppress velocity of flow and the fluctuation of melt, thus bath surface is stable, temperature fluctuation is little, can obtain the oxygen span of control of 4ppm.But it is huge that the weak point of magnetic field crystal pulling is facility investment, power consumption is large, is difficult to obtain high magneticstrength.
Summary of the invention
The object of the present invention is to provide a kind of monocrystalline silicon growing ultrasonic wave control oxygen technology, be specifically related to introduce one group of ultrasonic wave on the surface of silicon melt in crystal pulling process, silicon melt is impelled to flow to quartz crucible wall by superfield ripple, expand the low-oxygen area surface-area of silicon melt, hyperoxia district silicon melt is stirred simultaneously, reduce the solubleness of oxygen in melt, accelerate dissolution oxygen in the volatilization of free surface, thus reaches the effect controlling oxygen concn in silicon single-crystal.
In order to reach the above object, present invention process technology realizes by the following method: introduce one group of ultrasonic wave on the surface of silicon melt, see shown in Fig. 1 and Fig. 2.The ultrasonic wave head that shakes is evenly distributed on the coaxial circle 3 of quartz crucible 1 and silicon list rod 2.The distance that ultrasonic wave is shaken between head be shake head to sidewall of crucible distance 1.5-2.0 doubly.Ultrasonic wave is shaken and 7 to be made up of high purity quartz material, extend into the following 10-15mm in silicon melt 6 surface, and in crystal growing process, remains the same degree of depth.In silicon single-crystal isodiametric growth process, introduce ultra-sonic oscillation, ul-trasonic irradiation district 8 and high oxygen concentration district partly overlap, suppress the hot natural convection in the high oxygen concentration district near crucible, accelerate the brilliant silicon melt quoted from center to the flowing of surrounding, promote that oxygen is in the volatilization of free surface, reduces the solubleness of the Si-O gas in melt simultaneously, further promotion Si-O in the volatilization of bath surface, thus controls the oxygen level in crystal.The oxygen level crystal is controlled from face.
Hyperacoustic range of frequency is 500kHz-2.0MHz.Frequency, more than the ultrasonic wave of 500kHz, relative to the ultrasonic wave of lower frequency, to stirring and the mobilization reinforcement of melt, and reduces the cavatition of silicon melt, can not cause the gasification of silicon melt self, therefore can not introduce defect in crystal growth.
The relationship characteristic of ultrasonic frequency f and wave of oscillation amplitude D is also, formula (1) and (2)
(1)
In formula, I is the ultrasonic wave sound intensity.The decay characteristics equation of ultrasonic wave pressure I is
(2)
In formula, I 0for the sound intensity of a position that shakes, μ is the reduction coefficient of ultrasonic wave in silicon melt, and x is the distance of pickup ponints and the head that shakes.
The invention is characterized in: ultrasonic wave pressure is less than 1000Pa in the intensity at light ring place, silicon monocrystal growth interface.Therefore, ultrasonic wave for the stirring of the higher silicon melt of oxygen level near crucible and mobilization strong, and less for the effect at silicon list growth interface place.Due to hyperacoustic directivity, the silicon melt flowing that ultrasonic wave causes is reverse with hot natural convection, inhibits hot natural convection, prevents oxygen to be diffused into crystal growth interface from high concentration region.The silicon melt that ultrasonic wave causes simultaneously flows consistent with the silicon melt flow direction that Crystal Rotation causes, facilitate silicon melt to flow from crystal growth interface to low oxygen concentration district, the impurity element of enrichment on growth interface and oxygen etc. is made to be diffused into low oxygen concentration district, oxygen diffuses out melt with Si-O gas form, plays the effect controlling oxygen level.
The invention is characterized in: the ultrasonic wave angle of divergence of head in silicon melt of shaking is 60o, and the angle of shake head and silicon melt static surface is 60-90o.Ultrasonic wave carries out rectilinear propagation with the angle of divergence in silicon melt, the angle of an angle of divergence and the silicon melt static surface of shaking, ultrasonic wave can be made better to act on high oxygen concentration district near crucible, suppress thermal natural convection, promote that the silicon melt of Crystal Rotation formation is by the flowing of center to surrounding, reduces the oxygen level of crystal further simultaneously.
Hyperacoustic composition comprises: sinusoidal wave 60-100%, square wave 0-30%, zigzag wave 0-20%.Square wave and zigzag wave, when misoperation, at melt in the stronger standing wave of middle generation and resonance effect, can affect the stability of melt.
The method that frequency and amplitude are selected is: after unmelted polycrystalline silicon, carry out static, after silicon liquid surface is static, adopt fixed amplitude, frequency sweeping is carried out to melt, determine that ultrasonic wave pressure is less than 1000Pa in the intensity at light ring place, silicon monocrystal growth interface, and using this frequency and amplitude as ultrasonic wave control oxygen frequency and amplitude; After frequency and amplitude are determined, close ultrasonic wave, start seeding process.
The technology of the present invention, it is characterized in that hyperacoustic input be crystal turn shoulder terminate after isodiametric growth start before input; Because the oxygen level in crystal is under normal circumstances that head is high and afterbody is low, in crystal growing process, ultrasonic amplitude progressively can be reduced, to reduce hyperacoustic sound intensity.After isodiametric growth terminates, before crystal ending starts, stop ultrasonic wave input.
Accompanying drawing explanation
Fig. 1 is that ultrasonic wave of the present invention is shaken a site plan;
Fig. 2 is ultrasonic wave of the present invention propagation schematic diagram in the melt.
Embodiment
In growing single-crystal silicon growth technique, after polysilicon all melts, static more than 3h.After silicon liquid surface is static, the head that the ultrasonic wave adopting high purity quartz material to make shaken extend in melt with certain angle (60-90o), and the deep degree of depth is 10-15mm, and the ultrasonic wave angle of divergence is 60o.Measuring the ultrasonic wave sound intensity in crystal growth light ring predetermined position, when intensity is more than 1000Pa, making intensity be less than 1000Pa by regulating frequency and amplitude.When controlling that oxygen concn is at lower concentration in crystal, adopting higher frequency and less amplitude, when oxygen concn in control crystal is in relatively high density, adopting lower frequency and larger amplitude.
After determining ultrasonic amplitude and frequency, turn before after shoulder terminates isodiametric growth starts at crystal, open ultrasonic wave input, start isodiametric growth of crystal simultaneously.Because the oxygen level in crystal is under normal circumstances that head is high and afterbody is low, in crystal growing process, ultrasonic amplitude progressively can be reduced, to reduce hyperacoustic sound intensity.After isodiametric growth terminates, before crystal ending starts, the ripple that stops oscillation inputs.
Embodiment 1,
Growth diameter is 2 inches of silicon single crystal.The diameter of quartz crucible is 155mm, and a spot diameter that shakes is 135mm, and a spacing of shaking is 20mm.After polysilicon all melts, static 3h.After silicon liquid surface is static, the head that the ultrasonic wave adopting high purity quartz material to make shaken extend in melt with the angle of 90o, and the deep degree of depth is 10mm.Adopting 100% sine wave, measure the ultrasonic wave sound intensity in crystal growth light ring predetermined position, when intensity is more than 1000Pa, making intensity be less than 1000Pa by regulating frequency and amplitude.Determine that ultrasonic amplitude is after 1500kHz, close ultrasonic wave.Turn before after shoulder terminates isodiametric growth starts at crystal, start ultrasonic wave input, start isodiametric growth of crystal simultaneously.In crystal growing process, progressively can reduce ultrasonic amplitude, to reduce hyperacoustic sound intensity.After isodiametric growth terminates, before crystal ending starts, the ripple that stops oscillation inputs.After crystal growth, detect silicon single-crystal head, the oxygen level of middle part and afterbody is respectively 7.5ppm, 7.3ppm and 6.9ppm.The silicon single-crystal of contrast growth, parameter is identical with embodiment, does not just adopt ultrasonic wave to control oxygen concn, after crystal growth, detect silicon single-crystal head, the oxygen level of middle part and afterbody is respectively 8.0ppm, 7.3ppm and 6.5ppm, oxygen level is higher than the concentration adopting ultrasonic wave control oxygen.
Embodiment 2,
Growth diameter is 4 inches of silicon single crystal.The diameter of quartz crucible is 210mm, and a spot diameter that shakes is 190mm, and a spacing of shaking is 20mm.After polysilicon all melts, static 3h.After silicon liquid surface is static, the head that the ultrasonic wave adopting high purity quartz material to make shaken extend in melt with the angle of 60o, and the deep degree of depth is 10mm.The ultrasonic wave composition adopted comprises: sinusoidal wave 60%, square wave 20%, and zigzag wave 20% measures the ultrasonic wave sound intensity in crystal growth light ring predetermined position, when intensity is more than 1000Pa, makes intensity be less than 1000Pa by regulating frequency and amplitude.Determine that ultrasonic amplitude is after 1500kHz, close ultrasonic wave.Turn before after shoulder terminates isodiametric growth starts at crystal, start ultrasonic wave input, start isodiametric growth of crystal simultaneously.In crystal growing process, progressively can reduce ultrasonic amplitude, to reduce hyperacoustic sound intensity.After isodiametric growth terminates, before crystal ending starts, the ripple that stops oscillation inputs.After crystal growth, detect silicon single-crystal head, the oxygen level of middle part and afterbody is respectively 7.6ppm, 7.2ppm and 6.8ppm.
Embodiment 3,
Growth diameter is 4 inches of silicon single crystal.The diameter of quartz crucible is 210mm, and a spot diameter that shakes is 190mm, and a spacing of shaking is 40mm.After polysilicon all melts, static 3h.After silicon liquid surface is static, the head that the ultrasonic wave adopting high purity quartz material to make shaken extend in melt with the angle of 90o, and the deep degree of depth is 10mm.The ultrasonic wave composition adopted comprises: sinusoidal wave 60%, square wave 30%, and zigzag wave 10% measures the ultrasonic wave sound intensity in crystal growth light ring predetermined position, when intensity is more than 1000Pa, makes intensity be less than 1000Pa by regulating frequency and amplitude.Determine that ultrasonic amplitude is after 1000kHz, close ultrasonic wave.Turn before after shoulder terminates isodiametric growth starts at crystal, start ultrasonic wave input, start isodiametric growth of crystal simultaneously.In crystal growing process, progressively can reduce ultrasonic amplitude, to reduce hyperacoustic sound intensity.After isodiametric growth terminates, before crystal ending starts, the ripple that stops oscillation inputs.After crystal growth, detect silicon single-crystal head, the oxygen level of middle part and afterbody is respectively 7.3ppm, 7.3ppm and 6.6ppm.
Embodiment 4,
Growth diameter is 8 inches of silicon single crystal.The diameter of quartz crucible is 406mm, and a spot diameter that shakes is 370mm, and a spacing of shaking is 40mm.After polysilicon all melts, static 3h.After silicon liquid surface is static, the head that the ultrasonic wave adopting high purity quartz material to make shaken extend in melt with the angle of 60o, and the deep degree of depth is 10mm.The ultrasonic wave composition adopted comprises: sinusoidal wave 60%, square wave 30%, and zigzag wave 10% measures the ultrasonic wave sound intensity in crystal growth light ring predetermined position, when intensity is more than 1000Pa, makes intensity be less than 1000Pa by regulating frequency and amplitude.Determine that ultrasonic amplitude is after 1000kHz, close ultrasonic wave.Turn before after shoulder terminates isodiametric growth starts at crystal, start ultrasonic wave input, start isodiametric growth of crystal simultaneously.In crystal growing process, progressively can reduce ultrasonic amplitude, to reduce hyperacoustic sound intensity.After isodiametric growth terminates, before crystal ending starts, the ripple that stops oscillation inputs.After crystal growth, detect silicon single-crystal head, the oxygen level of middle part and afterbody is respectively 7.9ppm, 7.3ppm and 7.0ppm.The silicon single-crystal of contrast growth, parameter is identical with embodiment, does not just adopt ultrasonic wave to control oxygen concn, after crystal growth, detect silicon single-crystal head, the oxygen level of middle part and afterbody is respectively 9.1ppm, 8.3ppm and 8.0ppm, oxygen level is far above the concentration adopting ultrasonic wave control oxygen.
Embodiment 5,
Growth diameter is 8 inches of silicon single crystal.The diameter of quartz crucible is 598mm, and a spot diameter that shakes is 520mm, and a spacing of shaking is 70mm.After polysilicon all melts, static 3h.After silicon liquid surface is static, the head that the ultrasonic wave adopting high purity quartz material to make shaken extend in melt with the angle of 90o, and the deep degree of depth is 15mm.The ultrasonic wave composition adopted comprises: sinusoidal wave 60%, square wave 30%, and zigzag wave 10% measures the ultrasonic wave sound intensity in crystal growth light ring predetermined position, when intensity is more than 1000Pa, makes intensity be less than 1000Pa by regulating frequency and amplitude.Determine that ultrasonic amplitude is after 600kHz, close ultrasonic wave.Turn before after shoulder terminates isodiametric growth starts at crystal, start ultrasonic wave input, start isodiametric growth of crystal simultaneously.In crystal growing process, progressively can reduce ultrasonic amplitude, to reduce hyperacoustic sound intensity.After isodiametric growth terminates, before crystal ending starts, the ripple that stops oscillation inputs.After crystal growth, detect silicon single-crystal head, the oxygen level of middle part and afterbody is respectively 7.8ppm, 7.5ppm and 6.5ppm.
Embodiment 6,
Growth diameter is 12 inches of silicon single crystal.The diameter of quartz crucible is 610mm, and a spot diameter that shakes is 550mm, and a spacing of shaking is 60mm.After polysilicon all melts, static 3h.After silicon liquid surface is static, the head that the ultrasonic wave adopting high purity quartz material to make shaken extend in melt with the angle of 60o, and the deep degree of depth is 10mm.The ultrasonic wave composition adopted comprises: sinusoidal wave 60%, square wave 30%, and zigzag wave 10% measures the ultrasonic wave sound intensity in crystal growth light ring predetermined position, when intensity is more than 1000Pa, makes intensity be less than 1000Pa by regulating frequency and amplitude.Determine that ultrasonic amplitude is after 500kHz, close ultrasonic wave.Turn before after shoulder terminates isodiametric growth starts at crystal, start ultrasonic wave input, start isodiametric growth of crystal simultaneously.In crystal growing process, progressively can reduce ultrasonic amplitude, to reduce hyperacoustic sound intensity.After isodiametric growth terminates, before crystal ending starts, the ripple that stops oscillation inputs.After crystal growth, detect silicon single-crystal head, the oxygen level of middle part and afterbody is respectively 7.8ppm, 7.3ppm and 6.5ppm.The silicon single-crystal of contrast growth, parameter is identical with embodiment, does not just adopt ultrasonic wave to control oxygen concn, after crystal growth, detect silicon single-crystal head, the oxygen level of middle part and afterbody is respectively 9.5ppm, 8.6ppm and 7.5ppm, oxygen level is far above the concentration adopting ultrasonic wave control oxygen.

Claims (7)

1. a monocrystalline silicon growing ultrasonic wave control oxygen technology; Introduce one group of ultrasonic wave on the surface of silicon melt, the ultrasonic wave head that shakes is evenly distributed on on silicon list rod and the coaxial circle of crucible; The distance that ultrasonic wave is shaken between head be shake head to sidewall of crucible distance 1.5-2.0 doubly; The ultrasonic wave head that shakes is made up of high purity quartz material, extend into below silicon melt surface 10-15mm, and in crystal growing process, remains the same degree of depth; In silicon single-crystal isodiametric growth process, introduce ultra-sonic oscillation, suppress the hot natural convection in the high oxygen concentration district near crucible, accelerate the brilliant silicon melt quoted from center to the flowing of surrounding, promote that oxygen is in the volatilization of free surface, reduce the solubleness of the Si-O gas in melt simultaneously, promote that Si-O is in the volatilization of bath surface, thus control the oxygen level in crystal.
2. a kind of monocrystalline silicon growing ultrasonic wave control oxygen technology according to claim 1, is characterized in that: hyperacoustic range of frequency is 500kHz-2.0MHz.
3. a monocrystalline silicon growing ultrasonic wave control oxygen technology, is characterized in that: the relationship characteristic of ultrasonic frequency f and wave of oscillation amplitude D is also, formula (1) and (2)
(1)
In formula, I is the ultrasonic wave sound intensity;
The decay characteristics equation of ultrasonic wave pressure I is:
(2)
In formula, I 0for the sound intensity of a position that shakes, μ is the reduction coefficient of ultrasonic wave in silicon melt, and x is the distance of pickup ponints and the head that shakes; Feature of the present invention is also: ultrasonic wave pressure is less than 1000Pa in the intensity at light ring place, silicon monocrystal growth interface.
4. a monocrystalline silicon growing ultrasonic wave control oxygen technology, is characterized in that: the ultrasonic wave angle of divergence of head in silicon melt of shaking is 60o, and the angle of shake head and silicon melt static surface is 60-90o.
5. a monocrystalline silicon growing ultrasonic wave control oxygen technology, is characterized in that: hyperacoustic composition comprises: sinusoidal wave 60-100%, square wave 0-30%, zigzag wave 0-20%.
6. a monocrystalline silicon growing ultrasonic wave control oxygen technology, the method that frequency and amplitude are selected is: after unmelted polycrystalline silicon, carry out static, after silicon liquid surface is static, adopt fixed amplitude, frequency sweeping is carried out to melt, determines that ultrasonic wave pressure is less than 1000Pa in the intensity at light ring place, silicon monocrystal growth interface, and using this frequency and amplitude as ultrasonic wave control oxygen frequency and amplitude; After frequency and amplitude are determined, close ultrasonic wave, start seeding process.
7. a monocrystalline silicon growing ultrasonic wave control oxygen technology, it is characterized in that hyperacoustic input be crystal turn shoulder terminate after isodiametric growth start before input; In crystal growing process, progressively can reduce ultrasonic amplitude, to reduce hyperacoustic pressure; After isodiametric growth terminates, before crystal ending starts, stop ultrasonic wave input.
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CN105887198A (en) * 2016-06-16 2016-08-24 江苏中电振华晶体技术有限公司 Device and method for clearing away bubbles in sapphire crystal melt material
CN108166055A (en) * 2017-12-21 2018-06-15 重庆超硅半导体有限公司 A kind of integrated circuit large size single crystal silicon growth liquid stream control technology
CN108691009A (en) * 2017-03-31 2018-10-23 环球晶圆股份有限公司 Method for producing silicon single crystal
TWI761454B (en) * 2017-03-31 2022-04-21 環球晶圓股份有限公司 Method of manufacturing silicon single crystal
CN114855263A (en) * 2022-04-01 2022-08-05 上海新昇半导体科技有限公司 Crystal growth method and growth device

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