CN102181925A - Growth process and device for growing IC-level silicon single crystal with low Fe content by czochralski method - Google Patents
Growth process and device for growing IC-level silicon single crystal with low Fe content by czochralski method Download PDFInfo
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- CN102181925A CN102181925A CN 201110092088 CN201110092088A CN102181925A CN 102181925 A CN102181925 A CN 102181925A CN 201110092088 CN201110092088 CN 201110092088 CN 201110092088 A CN201110092088 A CN 201110092088A CN 102181925 A CN102181925 A CN 102181925A
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Abstract
The invention relates to a growth process and device for growing an IC-level silicon single crystal with a low Fe content by a czochralski method. The method comprises the following steps of loading materials, heating the materials and pulling crystals. A diversion device, which is combined with a diversion cover and a diversion cylinder, is used in the process of pulling a single crystal silicon rod by the czochralski method and used for adjusting a position of a crucible to carry out silicon fusing and crystal pulling. The device comprises a single crystal furnace, a heater, the diversion cylinder, a quartz crucible, a graphite crucible, a thermal-insulation cover, a thermal-insulation cylinder, a tray, a cured thermal-insulation carbon felt, a curing oven bottom protective disc and a vent. By means of the process and the device disclosed by the invention, the czochralski single crystal silicon with a diameter of 150 to 200m and the Fe content of less than 5E10Atoms/cm<3> can grow, so that the czochralski single crystal silicon can meet the requirement of an integrated circuit (IC), and the material cost can be greatly reduced if the czochralski single crystal silicon is applied to the IC industry. Furthermore, because a used graphite system is not needed to be chloridized and purified, the pollution to the natural environment can be indirectly reduced.
Description
Technical field
The present invention relates to the growth technique and the device of the low Fe content silicon monocrystal of a kind of Grown by CZ Method IC level, be specially to adopt and reduce the diffuse pollution of Fe in the Grown by CZ Method silicon single-crystal process silicon single crystal ingot, the technology of the single-crystal semiconductor material of growing high-quality, the low Fe content silicon monocrystal of growth IC level makes the manufacturing cost of relevant IC grade silicon decline to a great extent in the pulling of silicon single crystal environment of routine.
Background technology
Metallic impurity in the silicon single crystal can cause the deep-Level defective in following process, have a strong impact on device performance.The manufacturing of silicon single crystal, the general at present vertical pulling method that adopts; During growing single-crystal: a because in the quartz crucible, the hot system of graphite, single crystal growing furnace as heavy metals such as Fe, Cu, Au etc. at high temperature in melting silicon, spread, cause pulling of silicon single crystal to be stain by heavy metal; B is owing to contain multiple micro heavy inpurity in the furnace atmosphere, be attached to crystal bar surface during crystal growth and in higher temperature field to the crystal bar internal divergence, thereby cause silicon single-crystal to be stain by metallic impurity.Traditional solution mainly be to use the hot system of ultra-pure graphite, not only cost is far above the hot system of conventional sun power and use the hot system of ultra-pure graphite, graphite also may pollute physical environment in the process of chloridized.
Summary of the invention
The growth technique and the device that the purpose of this invention is to provide the low Fe content silicon monocrystal of a kind of Grown by CZ Method IC level can overcome the above-mentioned defective of solution.The present invention increases unique guiding device, improves mainly that beavy metal impurity stains and diffuse pollution crystal bar in the crystal growth, being implemented in the silicon single crystal that the low levels metal of IC requirement is satisfied in growth conventional pulling of silicon single crystal environment under.But the present invention's growth diameter 150-200mm, Fe content are less than 5E10Atoms/cm
3Following pulling of silicon single crystal makes pulling of silicon single crystal satisfy the requirement of unicircuit, is used for the IC industry and can significantly reduces material cost.In addition, purify, can also reduce pollution indirectly physical environment because of used graphite system need not chlorination.
The growth technique of the low Fe content silicon monocrystal of Grown by CZ Method IC level provided by the invention comprises charging, adds the thermalization material, the crystal pulling step, use the guiding device of pod and guide shell combination in the process of described vertical pulling method pulling monocrystal silicon rod, the molten silicon in position of adjusting crucible carries out crystal pulling.
Described charging back with the flow velocity applying argon gas of 20～150L/h to furnace pressure 3500Pa～4000Pa.
The described thermalization material power that adds is 900-2500kw, and change work stone English crucible upper edge is lower than well heater upper edge 10-25mm.
Described crystal pulling process is control crystalline pulling rate, argon gas flow velocity, the brilliant commentaries on classics and the crucible commentaries on classics, and accent crucible position keeps the distance between guide shell lower edge and the liquid level, process adjustments, ending and cooling routinely.Promptly being cooled to liquid level after changing material has condensate depression, behind the silicon temperature-stable fusion, falls seed crystal to being higher than liquid level 120～150mm place's preheating 30～40 minutes; Draw thin footpath, crystalline substance changes 1～8 rev/min, soaks to melt to lift after 25～40 minutes, and pulling rate 6～17mm/ minute, thin electrical path length was not less than 170mm, diameter≤4mm; And control furnace chamber pressure 3500Pa～4000Pa isodiametric growth,
Described crystal pulling process utilizes the angle (60 ° to 90 °) of guide shell that argon gas stream in the stove is directly blown crystal ingot external diameter and molten silicon contact position, i.e. periphery, crystallization forward position.
After describedization material finished, the distance between guide shell lower edge and the fusion silicon liquid level transferred to 5-15mm.
Described control crystal pulling rate is that control pulling rate scope is 0.7-0.9mm/min in isometrical process;
Described control argon gas flow velocity is to promote argon gas at isodiametric growth 20mm place to 30-150L/h;
Described control crystalline substance transfers 5-14 rev/min to; The isometrical crucible of described control transfers 0-1 rev/min to;
The polysilicon parameter that the present invention uses must not be lower than routine, and its purity requirement is: B≤0.1ppba, D≤0.9ppba, C≤0.5ppma.Boron dope agent purity is 9-11N.Atom number in the single crystal silicon material is 0.5*10
23Individual/cubic centimetre.
The device of the growth of the low Fe content silicon monocrystal of a kind of Grown by CZ Method IC level provided by the invention mainly comprises protection plate and venting hole at the bottom of single crystal growing furnace, well heater, guide shell, quartz crucible, plumbago crucible, insulation cover, heat-preservation cylinder, pallet, curing heat preservation carbon felt, the curing oven.
The present invention has realized that under conventional pulling of silicon single crystal environment growth satisfies the silicon single crystal of the low levels heavy metal that IC requires.But the present invention's growth diameter 150-200mm, Fe content are less than 5E10Atoms/cm
3Following pulling of silicon single crystal makes pulling of silicon single crystal satisfy the requirement of unicircuit, is used for the IC industry and can significantly reduces material cost.In addition, purify, can also reduce pollution indirectly physical environment because of used graphite system need not chlorination.The present invention makes the section minority carrier life time distribution of crystal bar be tending towards evenly realizing silicon single crystal lattice high integrality and highly purified product up-gradation.
Description of drawings
Fig. 1 is the device synoptic diagram of the growth of the low Fe content silicon monocrystal of Grown by CZ Method IC level.
Fig. 2 is to use the assay figure of the inventive method iron level.
Embodiment
The present invention is described in detail as follows with reference to accompanying drawing:
As shown in the figure, 1. crystal rising rotating mechanism, 2. silicon single crystal, 3. pod, 4. guide shell, 5. quartzy earthenware misfortune, 6. molten silicon, 7. plumbago crucible, 8. well heater, 9. the graphite insulation is disclosed, 10. exhaust outlet, 11. heating electrodes, 12. crucible rising rotating mechanisms.
Apparatus of the present invention mainly comprise protection plate and venting hole at the bottom of single crystal growing furnace, well heater, guide shell, quartz crucible, plumbago crucible, insulation cover, heat-preservation cylinder, pallet, curing heat preservation carbon felt, the curing oven.
The thermal field device that is fit to the low Fe content silicon monocrystal of growth IC level is installed in the burner hearth of described single crystal growing furnace, and graphite heat-preservation cylinder 9 is installed at well heater 8 peripheral places, and heat-preservation cylinder 9 outsides are installed and solidified heat preservation carbon felt; Graphite heat-preservation cylinder 9 is located at the bottom of the curing oven under the graphite on the protection plate in the bayonet socket of pallet, graphite heat-preservation cylinder 9 upper edges are also by the following bayonet socket location of graphite upper tray, pod 3 be positioned at guide shell 4 directly over be fixed on the monocrystalline body of heater, guide shell 4 upper edges are located by the upper latch notch in the graphite upper tray, and last insulation cover is by the top outer bayonet socket location of graphite upper tray.The plumbago crucible bar supports plumbago crucible 7, and quartz crucible 5 is located in the plumbago crucible 7, and quartz crucible 5 upper edges exceed plumbago crucible 7 upper edges.
The source of silicon single crystal, specification etc., the method for inspection: adopt U.S. SDI Fax230 surface photovoltage tester, under clean 10 grades of ultra-clean chambers, constant temperature, constant humidity environment, test according to SEMIMF391-0708, YS/T697 standard.
Application Example 1
The method of Grown by CZ Method gallium-mixing silicon monocrystal of the present invention is described in detail as follows: comprise steps such as charging, heating, crystal pulling:
The first step: according to a conventional method the single crystal growing furnace prepurging is handled, vacuumized, and when confirming trouble free, blow-on, charging add 42 kilograms of polysilicons and 1.6 and restrain galliums, and the centre that gallium is put polycrystalline silicon raw material to the quartzy crucible, applying argon gas is to furnace pressure 2000Pa.
Second step: low crucible position material, adding thermalization material power is 1600kw, crucible transfers zero to, collapses in the to be confirmedization material behind the material, and the crucible veer is transferred to 1 rev/min, changes material and finishes, 1500 ℃ of molten silicon temperature.
The 3rd step: change material and finish, the heating power electrically-controlled controller is adjusted into automatically, being cooled to liquid level has condensate depression, and silicon temperature-stable fusion after 30 minutes is reduced to seed crystal apart from fusion silicon liquid level 90mm place's preheating 30 minutes, begin to descend and draw thin footpath, this moment, brilliant modulation to 7 was changeed, and soaked to melt to lift after 30 minutes, and pulling rate is 5.5mm/ minute, thin electrical path length is not less than 160mm, diameter=2mm～3mm.
The 4th step: changeed the shoulder pulling rate 2.4mm/ minute, and changeed shoulder 1/2 post-tensioning velocity modulation to 1.2mm/ minute.
The 5th step: isodiametric growth, furnace pressure transfers to 2500Pa, pulling rate 0.9mm/ minute, the argon gas stream velocity modulation is to 25L/h, and brilliant the commentaries on classics in 30 rev/mins regulated, and transfers the crucible position to keep between guide shell lower edge and the liquid level apart from 15mm, crucible changes at 1 rev/min, process adjustments, ending and cooling routinely.Detect and measurement result:
42 kilograms of charging capacitys are at Φ 16 " the Φ 150mm of growth under the thermal field device, P type＜100〉crystal orientation; The resistivity of silicon single crystal bar: head p≤3 Ω .cm, afterbody p 〉=0.5 Ω cm.Interstitial oxygen content is [Oi]≤17.5ppma, and the displacement carbon content is [Cs]≤0.5ppma, non-equilibrium minority carrier life time τ 〉=150 μ s, dislocation desity EPD≤500/cm2.
Figure 2 shows that Fe content and the distribution results thereof of using SDI Fax230 surface photovoltage tester to detect the monocrystalline of growing with present method.Critical data is among Fig. 2,314 of test point, 314 of high-quality points; Fe content is maximum 21.33E10cm-3, minimum 4.556E10cm-3, and average is 8.880E10cm-3.
Application Example 2
Well heater external diameter 495mm, internal diameter 458mm, electrode spacing 320mm.Well heater virtual height 330mm, the well heater total height is 480mm.The single crystal growing furnace internal diameter is Φ=620mm.The peripheral 15mm of well heater installs the graphite heat-preservation cylinder in the place, and the quartz crucible upper edge exceeds plumbago crucible upper edge 25mm.
Operation steps:
The first step: with the single crystal growing furnace prepurging, vacuumize according to a conventional method, vaccum leakage rate reaches 1Pa/3 minute, blow-on, charging (pack into 42 kilograms of polysilicons and 1.6 gram galliums), the centre of gallium being put polycrystalline silicon raw material to the quartzy crucible.Applying argon gas is to furnace pressure 1900Pa, and argon flow amount is transferred to a times of common process flow, and the argon gas stream velocity modulation is to 35L/h.And the large-scale furnace pressure that other usual methods are used can not guarantee the resistivity distribution of gallium-mixing silicon monocrystal under major diameter.
Second step: low crucible position material, adding thermalization material power is 1600kw, and crucible transfers zero to, collapses in the to be confirmedization material behind the material, and the crucible veer is transferred to 0.5 rev/min, changes material and finishes, and molten silicon temperature reaches 1500 ℃.
The 3rd step: change material and finish, apart from 5mm, the automatically controlled incision of heating power is automatic between guide shell lower edge and the liquid level, and being cooled to liquid level has condensate depression, silicon temperature-stable fusion is after 35 minutes, seed crystal is reduced to apart from fusion silicon liquid level 100mm place's preheating 30 minutes, descend and to draw thin footpath, brilliant modulation to 8 this moment rev/min, soak to melt and lift after 35 minutes, pulling rate is 1.5mm/ minute, and thin electrical path length is not less than 160mm, diameter 2.5mm;
The 4th step: change the shoulder pulling rate, changeed the shoulder pulling rate 2mm/ minute, change shoulder 1/2 post-tensioning velocity modulation to 1.2mm/ minute;
The 5th step: isodiametric growth, furnace pressure transfers to 2500Pa, pulling rate 0.9mm/ minute, the argon gas stream velocity modulation is to 25L/h, and brilliant the commentaries on classics in 30 rev/mins regulated, and transfers the crucible position to keep between guide shell lower edge and the liquid level apart from 15mm, crucible changes at 1 rev/min, process adjustments, ending and cooling routinely.
The measuring result is with embodiment 1.
Claims (10)
1. the growth technique of the low Fe content silicon monocrystal of a Grown by CZ Method IC level, it is characterized in that it comprises charging, adds the thermalization material, the crystal pulling step, use the guiding device of pod and guide shell combination in the process of vertical pulling method pulling monocrystal silicon rod, the molten silicon in position of adjusting crucible carries out crystal pulling.
2. according to the described growth technique of claim 1, it is characterized in that described charging back with the flow velocity applying argon gas of 20～150L/h to furnace pressure 3500Pa～4000Pa.
3. according to the described growth technique of claim 1, it is characterized in that the described thermalization material power that adds is 900-2500kw, and change work stone English crucible upper edge is lower than well heater upper edge 10-25mm.
4. according to the described growth technique of claim 1, it is characterized in that described crystal pulling process is control crystalline pulling rate, argon gas flow velocity, the brilliant commentaries on classics and the crucible commentaries on classics, transfer the distance between maintenance guide shell lower edge, crucible position and the liquid level, process adjustments, ending and cooling routinely, promptly after changing material, be cooled to liquid level condensate depression is arranged, behind the silicon temperature-stable fusion, seed crystal falls to being higher than liquid level 120～150mm place's preheating 30～40 minutes; Draw thin footpath, crystalline substance changes 1～8 rev/min, soaks to melt to lift after 25～40 minutes, and pulling rate 6～17mm/ minute, thin electrical path length was not less than 170mm, diameter≤4mm; And control furnace chamber pressure 3500Pa～4000Pa isodiametric growth,
5. according to the described growth technique of claim 4, it is characterized in that describedization material finishes after, the distance between guide shell lower edge and the fusion silicon liquid level is 5-15mm.
6. according to the described growth technique of claim 4, it is characterized in that described control crystal pulling rate is that control pulling rate scope is 0.7-0.9mm/min in isometrical process;
7. according to the described growth technique of claim 4, it is characterized in that described control argon gas flow velocity is to promote argon gas at isodiametric growth 20mm place to 30-150L/h;
8. according to the described growth technique of claim 4, it is characterized in that described control crystalline substance transfers 5-14 rev/min to; The isometrical crucible of described control transfers 0-1 rev/min to;
9. according to the described growth technique of claim 1, it is characterized in that the purity of the polycrystalline silicon raw material that uses is: B≤0.1ppba, D≤0.9ppba, C≤0.5ppma; Boron dope agent purity is 9-11N; Atom number in the single crystal silicon material is 0.5*10
23Individual/cubic centimetre.
10. a Grown by CZ Method IC level is hanged down the device of the growth of Fe content silicon monocrystal, mainly comprise protection plate and venting hole at the bottom of single crystal growing furnace, well heater, guide shell, quartz crucible, plumbago crucible, insulation cover, heat-preservation cylinder, pallet, curing heat preservation carbon felt, the curing oven, it is characterized in that the peripheral place's installation of well heater graphite heat-preservation cylinder, the heat-preservation cylinder outside is installed and is solidified heat preservation carbon felt; The graphite heat-preservation cylinder is located at the bottom of the curing oven under the graphite on the protection plate in the bayonet socket of pallet, graphite heat-preservation cylinder upper edge is also by the following bayonet socket location of graphite upper tray, pod be positioned at guide shell directly over be fixed on the monocrystalline body of heater, the guide shell upper edge is located by the upper latch notch in the graphite upper tray, and last insulation cover is by the top outer bayonet socket location of graphite upper tray.The plumbago crucible bar supports plumbago crucible, and quartz crucible is located in the plumbago crucible, and the quartz crucible upper edge exceeds the plumbago crucible upper edge.
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Cited By (7)
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| CN103668440A (en) * | 2013-12-16 | 2014-03-26 | 上海申和热磁电子有限公司 | Monocrystal silicon czochralski method heat shield adjustment process |
| CN104593863A (en) * | 2015-01-05 | 2015-05-06 | 英利集团有限公司 | Single-crystal furnace |
| CN108179463A (en) * | 2017-12-28 | 2018-06-19 | 锦州神工半导体有限公司 | The flow-guiding structure of major diameter single crystal drawing process and method of river diversion in vertical pulling method |
| CN110685011A (en) * | 2019-10-21 | 2020-01-14 | 大同新成新材料股份有限公司 | Intelligent processing equipment for producing single-product silicon thermal field crucible and processing method thereof |
| CN112281207A (en) * | 2020-10-09 | 2021-01-29 | 西安奕斯伟硅片技术有限公司 | Heat preservation cover for reducing heat loss of crystal pulling furnace and crystal pulling furnace |
| CN114277433A (en) * | 2021-12-24 | 2022-04-05 | 宁夏中欣晶圆半导体科技有限公司 | Growth method of single crystal annealing product applied to Hanhong single crystal furnace |
| CN114277434A (en) * | 2021-12-29 | 2022-04-05 | 西安奕斯伟材料科技有限公司 | Thermal field adjusting device and method for single crystal growth |
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| CN112281207A (en) * | 2020-10-09 | 2021-01-29 | 西安奕斯伟硅片技术有限公司 | Heat preservation cover for reducing heat loss of crystal pulling furnace and crystal pulling furnace |
| CN114277433A (en) * | 2021-12-24 | 2022-04-05 | 宁夏中欣晶圆半导体科技有限公司 | Growth method of single crystal annealing product applied to Hanhong single crystal furnace |
| CN114277434A (en) * | 2021-12-29 | 2022-04-05 | 西安奕斯伟材料科技有限公司 | Thermal field adjusting device and method for single crystal growth |
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Application publication date: 20110914 |