CN108660509A - A kind of pulling of silicon single crystal method - Google Patents

A kind of pulling of silicon single crystal method Download PDF

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Publication number
CN108660509A
CN108660509A CN201710188098.1A CN201710188098A CN108660509A CN 108660509 A CN108660509 A CN 108660509A CN 201710188098 A CN201710188098 A CN 201710188098A CN 108660509 A CN108660509 A CN 108660509A
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silicon
pulling
single crystal
wafer
silicon single
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肖德元
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Zing Semiconductor Corp
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Zing Semiconductor Corp
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-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
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/06—Silicon
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-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
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
    • C30B15/04—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt adding doping materials, e.g. for n-p-junction
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-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
    • C30B30/00—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions
    • C30B30/04—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions using magnetic fields
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-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
    • C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • C30B33/02—Heat treatment

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The present invention provides a kind of pulling of silicon single crystal method, includes the following steps：The silicon chip that surface growth has deuterium doped silicon nitride is provided；The silicon chip is carried out with polysilicon fragment to mix fusion；Carry out seed crystal welding；Monocrystal silicon is formed using magnetic field Czochralski method is added.The present invention also provides a kind of forming methods of wafer, form wafer as original material using monocrystal silicon, wherein the monocrystal silicon is formed using above-mentioned pulling of silicon single crystal method.The pulling of silicon single crystal method of the present invention can relatively accurately control nitrogen in silicon single crystal bar and deuterium concentration and obtain good uniform doping.

Description

A kind of pulling of silicon single crystal method
Technical field
The present invention relates to technical field of semiconductors, more particularly to a kind of method of pulling of silicon single crystal.
Background technology
During pulling of crystals silicon growth, due to the melting of silica crucible, a part of oxygen would generally enter monocrystalline In silicon, these oxygen are primarily present in the interstitial site of silicon crystal lattice.When interstitial oxygen concentration concentration be more than a certain temperature under oxygen in silicon When solubility, interstitial oxygen concentration will precipitate in monocrystalline silicon, form oxygen precipitation defect common in monocrystalline silicon.If not to silicon Oxygen precipitation in piece is controlled, it will is caused damages to integrated circuit device.
By certain technique, highdensity oxygen precipitation is formed in wafer bulk, and forms certain depth in silicon chip surface Flawless clean area.The region will be used to manufacture device, and here it is " intrinsic gettering " techniques.With very large scale integration (ULSI) development, characteristic line breadth is smaller and smaller, this just needs to reduce the oxygen concentration in monocrystalline silicon in order to avoid in device active region Defect is formed, while the heat budget of integrated circuit technology has significant decrease than before.Therefore, oxygen precipitation is formed in wafer bulk Condition cannot be met well, to influence intrinsic gettering effect.
One of the approach for solving the problems, such as this is exactly the nitrating in pulling of silicon single crystal, this, which is primarily due to nitrogen, can promote directly Oxygen precipitation in crystal-pulling silicon gets off, to enhance the intrinsic gettering ability of silicon chip.In addition nitrating can be in czochralski silicon monocrystal Silicon chip mechanical strength is improved, void-type defect is inhibited.It is aobvious using infrared light scattering Tomography (IR-LST) and scanned infrared Micro- art (SIRM) research oxygen precipitation profile situation the result shows that, 300mm nitrating Czochralski silicon wafers are after annealing at a high temperature by a step, Highdensity oxygen precipitation can be formed in the suitable wafer bulk of nitrating concentration and forms the cleaning of one fixed width in silicon chip near surface Area.In addition, with the increase of nitrogen concentration, the oxygen precipitation radial distribution in silicon chip is more uniformly distributed.
Industrial quarters generally uses solid phase nitrating pulling of crystals method to carry out silicon single crystal nitrating, such as uses silicon nitride (Si3N4) powder Nitrating.Before seed crystal welding, by alpha-silicon nitride powders and polysilicon fragment under higher than alpha-silicon nitride powders melting temperature (>1900℃) It carries out being sufficiently mixed melting, then reduces melt temperature, carry out seed crystal welding, the temperature of silicon melt surface central area is at this time For silicon melting temperature, solid phase nitrating crystal pulling growth then can be carried out.The advantages of the method is can relatively accurately to control silicon Nitrating concentration in monocrystal rod, the disadvantage is that high purity silicon nitride (Si3N4) powder is difficult to obtain, and due to Si3N4It is difficult to melt, It is easy the residual Si in silicon melt3N4Particle brings difficulty to the dislocation-free growth of monocrystalline silicon.
Industrial quarters also has carries out silicon single crystal nitrating using gas phase nitrogen-doping pulling of crystals method.Its nitrating technique is, molten in seed crystal After connecing, the temperature of silicon melt surface central area is silicon melting temperature, is passed through high pure nitrogen or nitrogen and argon gas at this time Mixture carry out gas phase nitrogen-doping.Lead to the time of nitrogen by control to control the nitrogen concentration in silicon crystal.After nitrating, open Beginning seeding.As previously mentioned, gas phase nitrogen-doping is to be reacted with high temperature silicon melt surface by nitrogen by realize nitrating, purity is higher, together When due to nitrogen and reacting for silicon melt it is inviolent, particle will not be formed by reacting the silicon nitride of generation, can be quickly dissolved in silicon solution. The disadvantage is that due to fully relying on thermal convection current, the nitrogen concentration in silicon melt is uneven, and not easy to control.
Invention content
In view of prior art described above, the purpose of the present invention is to provide a kind of methods of pulling of silicon single crystal, for solving Variety of problems certainly in the prior art.
In order to achieve the above objects and other related objects, the present invention provides a kind of pulling of silicon single crystal method, including following step Suddenly：
The silicon chip that surface growth has deuterium doped silicon nitride is provided；
The silicon chip is carried out with polysilicon fragment to mix fusion；
Carry out seed crystal welding；
Monocrystal silicon is formed using magnetic field Czochralski method is added.
Optionally, the silicon chip that surface growth has deuterium doped silicon nitride is provided, is given birth in silicon chip surface by chemical vapor deposition Silicon nitride with deuterium doping.
Still optionally further, deuterium mixes using low-pressure chemical vapor deposition or the growth of plasma activated chemical vapour deposition method Miscellaneous silicon nitride.
Optionally, the thickness of the silicon nitride for having deuterium to adulterate is 20nm~5000nm.
Optionally, when the silicon chip being carried out mixing fusion with polysilicon fragment, in the pre- constant temperature higher than silicon nitride fusing point Degree carries out mixing fusion.
Still optionally further, the predetermined temperature is 1420~1500 DEG C.
Optionally, when carrying out seed crystal welding, reducing melt temperature makes the temperature of silicon melt surface central area to silicon fusing point Temperature.
Optionally, using adding magnetic field Czochralski method to form monocrystal silicon, including step：Use seed crystal with predetermined pulling rate to Upper crystal pulling reduces pulling rate and enters shouldering step when seed crystal length reaches predetermined length；In the monocrystalline for forming predetermined diameter After silicon ingot, into turning the isometrical step of shoulder；After monocrystal silicon diameter is stablized relatively, into the automatic equal diameter control stage.
When still optionally further, using magnetic field Czochralski method formation monocrystal silicon is added, used magnetic field intensity is 1000- 5000 Gausses.
When optionally, using the pulling of silicon single crystal method, it is passed through gas, the gas includes argon gas.
In order to achieve the above objects and other related objects, the present invention also provides a kind of forming methods of wafer, using monocrystalline Silicon ingot forms wafer as original material, wherein the monocrystal silicon is formed using above-mentioned pulling of silicon single crystal method.
Optionally, a concentration of the 1 × 10 of the wafer nitrogen atom13~1 × 1016/cm3。
Optionally, the wafer containing D-atom a concentration of 1 × 1012~1 × 1016/cm3。
Optionally, the forming method of the wafer includes carrying out cutting thin, surface grinding, throwing successively to the monocrystal silicon Light, edge treated and cleaning treatment are to form wafer.
As described above, the pulling of silicon single crystal method of the present invention, has the advantages that：
The present invention adds magnetic Czochralski monocrystalline method (MCZ) to carry out silicon single crystal nitrating and deuterium using solid phase nitrating, can be relatively accurate Nitrogen and deuterium concentration in ground control silicon single crystal bar and the good uniform doping of acquisition.Thus the monocrystal rod or silicon of method production Chip nitrogen atom concentration is 1 × 1013~1 × 1016/cm3；Concentration containing D-atom is 1 × 1012~1 × 1016/cm3Between In range.
By carrying out high temperature long term annealing to N doping monocrystalline silicon piece, deep close to the surface of manufacture integrated circuit device Silicon chip COP (Crystal Originated Particle) defect is eliminated in degree about 0.5 micron range.In superficial layer In COP density reduce to internal about 50% or less.Silicon chip surface is also lacked without BMD (Bulk Micro Defect) It falls into.
To D-atom is added in the silicon of molten, D-atom is made to be stored in the gap of monocrystal silicon, can reduce oxygen and The content of carbon impurity, after forming wafer using the method for the present invention pulled crystal silicon ingot, when forming device on wafer, deuterium can It diffuses out, and is actively combined with gate dielectric layer and the dangling bonds at interface, form relatively stable structure, to Penetrating for hot carrier is avoided, leakage current is reduced, improves the performance and reliability of device.
Description of the drawings
Fig. 1 is shown as the schematic diagram of pulling of silicon single crystal method provided in an embodiment of the present invention.
Specific implementation mode
Illustrate that embodiments of the present invention, those skilled in the art can be by this specification below by way of specific specific example Disclosed content understands other advantages and effect of the present invention easily.The present invention can also pass through in addition different specific realities The mode of applying is embodied or practiced, the various details in this specification can also be based on different viewpoints with application, without departing from Various modifications or alterations are carried out under the spirit of the present invention.It should be noted that in the absence of conflict, following embodiment and implementation Feature in example can be combined with each other.
It should be noted that the diagram provided in following embodiment only illustrates the basic structure of the present invention in a schematic way Think, component count, shape and size when only display is with related component in the present invention rather than according to actual implementation in schema then Draw, when actual implementation kenel, quantity and the ratio of each component can be a kind of random change, and its assembly layout kenel It is likely more complexity.
The present embodiment will provide a kind of method of pulling of silicon single crystal, add magnetic Czochralski monocrystalline method (MCZ) using solid phase nitrating Carry out silicon single crystal nitrating and deuterium.Before seed crystal welding, surface growth there are into the silicon chip and polycrystalline of the silicon nitride film of deuterium doping simultaneously Silicon fragment under higher than silicon nitride melting temperature (>1900 DEG C) it carries out being sufficiently mixed melting, melt temperature is then reduced, seed is carried out Brilliant welding, the temperature of silicon melt surface central area is silicon melting temperature at this time, then can be carried out solid phase nitrating and mixes Deuterium plus magnetic field crystal pulling growth, can relatively accurately control nitrogen in silicon single crystal bar and deuterium concentration and good uniform doping Property.
Referring to Fig. 1, a kind of pulling of silicon single crystal method provided in this embodiment, includes the following steps：
S1 provides the silicon chip that surface growth has deuterium doped silicon nitride；
S2 carries out the silicon chip with polysilicon fragment to mix fusion；
S3 carries out seed crystal welding；
S4 is used plus magnetic field Czochralski method forms monocrystal silicon.
In step sl, there can be the silicon nitride that deuterium adulterates in silicon chip surface growth by chemical vapor deposition (CVD).Electricity Low-pressure chemical vapor deposition (LPCVD) or plasma activated chemical vapour deposition may be used in the silicon nitride film of the deuterium doping of sub- grade (PECVD) technology deposits obtain on a silicon substrate, such as：
3 SiD4(gas)+4ND3(gas)→Si3N4(solid)+12D2(gas)
3 SiCl4(gas)+4ND3(gas)→Si3N4(solid)+12DCl(gas)
3 SiCl2D2(gas)+4ND3(gas)→Si3N4(solid)+6DCl(gas)+6D2(gas)
The silicon nitride film and silicon substrate of deuterium doping remain the D-atom for having certain amount wherein.
Preferably, the thickness of the silicon nitride of deuterium doping that has of growth can be 20nm~5000nm to the present embodiment.
In step s 2, when the silicon chip being carried out mixing fusion with polysilicon fragment, pre- higher than silicon nitride fusing point Constant temperature degree carries out mixing fusion.The present embodiment is preferably, described pre- when the silicon chip is carried out mixing fusion with polysilicon fragment Constant temperature degree is 1420~1500 DEG C.
In step s3, when carrying out seed crystal welding, reducing melt temperature makes the temperature of silicon melt surface central area to silicon Near melting temperature.
In step s 4, using adding magnetic field Czochralski method to form monocrystal silicon, specially：Use seed crystal with predetermined pulling rate Upward crystal pulling reduces pulling rate and enters shouldering step when seed crystal length reaches predetermined length；It is dropped in the shouldering step Low pulling rate maintains a linear rate of temperature fall, after forming the monocrystal silicon of predetermined diameter, into turning the isometrical step of shoulder；Wait for monocrystalline It is rapidly lifted up after silicon ingot growth in thickness to pre-provisioning request, cool down in time, be simultaneously stopped linear cooling, gives crucible rising Rate slowly adjusts casting speed control according to diameter change rate speed, after monocrystal silicon diameter is stablized relatively, opens automatic etc. Diameter controls program, into the automatic equal diameter control stage.
Wherein, the diameter of monocrystal silicon can be controlled by pulling rate and predetermined temperature.
In the present embodiment, when using adding magnetic field Czochralski method to form monocrystal silicon, used magnetic field intensity can be 1000- 5000 Gausses.
In the present embodiment, when using the pulling of silicon single crystal method, whole process can be passed through gas, and the gas includes argon Gas.Some impurity and reaction product gas can be taken away by being passed through argon gas, such as CO, CO2、O2, SiO etc..
In addition, the present embodiment also provides a kind of forming method of wafer.
This method using above-mentioned pulling of silicon single crystal method after obtaining monocrystal silicon, using the monocrystal silicon as original material Material forms wafer.
In the present embodiment, the concentration of the wafer nitrogen atom of formation can be 1 × 1013~1 × 1016/cm3。
In the present embodiment, concentration of the wafer containing D-atom of formation can be 1 × 1012~1 × 1016/cm3。
Specifically, the forming method of the wafer includes carrying out cutting thin, surface grinding, throwing successively to the monocrystal silicon Light, edge treated and cleaning treatment are to form wafer.
In conclusion method using the present invention, can relatively accurately control nitrogen in silicon single crystal bar and deuterium concentration and Obtain good uniform doping.Thus the monocrystal rod or silicon wafer nitrogen atom concentration of method production are 1 × 1013~1 × 1016/cm3；Concentration containing D-atom is 1 × 1012~1 × 1016/cm3Between.
By carrying out high temperature long term annealing (such as 1150~1200 DEG C, 1~2h) to N doping monocrystalline silicon piece, close to system The case depth for making integrated circuit device is about silicon chip COP (Crystal Originated in 10-30 micron ranges Particle) defect is eliminated.COP density in superficial layer is reduced to internal about 50% or less.Silicon chip surface There is no BMD (Bulk Micro Defect) defect.
To D-atom is added in the silicon of molten, D-atom is made to be stored in the gap of monocrystal silicon, can reduce oxygen and The content of carbon impurity, after forming wafer using the method for the present invention pulled crystal silicon ingot, when forming device on wafer, deuterium can It diffuses out, and is actively combined with gate dielectric layer and the dangling bonds at interface, form relatively stable structure, to Penetrating for hot carrier is avoided, leakage current is reduced, improves the performance and reliability of device.
So the present invention effectively overcomes various shortcoming in the prior art and has high industrial utilization.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe The personage for knowing this technology can all carry out modifications and changes to above-described embodiment without violating the spirit and scope of the present invention.Cause This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as At all equivalent modifications or change, should by the present invention claim be covered.

Claims (14)

1. a kind of pulling of silicon single crystal method, which is characterized in that the described method comprises the following steps：
The silicon chip that surface growth has deuterium doped silicon nitride is provided；
The silicon chip is carried out with polysilicon fragment to mix fusion；
Carry out seed crystal welding；
Monocrystal silicon is formed using magnetic field Czochralski method is added.
2. pulling of silicon single crystal method according to claim 1, it is characterised in that：There is provided surface growth has deuterium doped silicon nitride Silicon chip, by chemical vapor deposition silicon chip surface growth have deuterium adulterate silicon nitride.
3. pulling of silicon single crystal method according to claim 2, it is characterised in that：Using low-pressure chemical vapor deposition or wait from The growth of daughter chemical vapor deposition method has the silicon nitride that deuterium adulterates.
4. pulling of silicon single crystal method according to claim 1, it is characterised in that：The thickness of the silicon nitride for thering is deuterium to adulterate For 20nm~5000nm.
5. pulling of silicon single crystal method according to claim 1, it is characterised in that：The silicon chip and polysilicon fragment are carried out When mixing fusion, mixing fusion is carried out in the predetermined temperature higher than silicon nitride fusing point.
6. pulling of silicon single crystal method according to claim 5, it is characterised in that：The predetermined temperature is 1420~1500 ℃。
7. pulling of silicon single crystal method according to claim 1, it is characterised in that：When carrying out seed crystal welding, melt temperature is reduced Degree makes the temperature of silicon melt surface central area to silicon melting temperature.
8. pulling of silicon single crystal method according to claim 1, it is characterised in that：Monocrystalline silicon is formed using magnetic field Czochralski method is added Ingot, including step：It uses seed crystal with the upward crystal pulling of predetermined pulling rate, when seed crystal length reaches predetermined length, reduces crystal pulling Rate enters shouldering step；After the monocrystal silicon for forming predetermined diameter, into turning the isometrical step of shoulder；Wait for monocrystal silicon diameter phase After stabilization, into the automatic equal diameter control stage.
9. pulling of silicon single crystal method according to claim 1, it is characterised in that：Monocrystalline silicon is formed using magnetic field Czochralski method is added When ingot, used magnetic field intensity is 1000-5000 Gausses.
10. pulling of silicon single crystal method according to claim 1, it is characterised in that：When using the pulling of silicon single crystal method, It is passed through gas, the gas includes argon gas.
11. a kind of forming method of wafer forms wafer using monocrystal silicon as original material, it is characterised in that：The list Crystal silicon ingot is used and is formed according to claim 1-10 any one of them pulling of silicon single crystal methods.
12. the forming method of wafer according to claim 11, it is characterised in that：The wafer nitrogen atom it is a concentration of 1×1013~1 × 1016/cm3。
13. the forming method of wafer according to claim 11, it is characterised in that：The wafer is containing a concentration of of D-atom 1×1012~1 × 1016/cm3。
14. the forming method of wafer according to claim 11, it is characterised in that：The forming method of the wafer includes pair The monocrystal silicon carries out cutting successively thin, surface grinding, polishing, edge treated and cleaning treatment to form wafer.
CN201710188098.1A 2017-03-27 2017-03-27 A kind of pulling of silicon single crystal method Pending CN108660509A (en)

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CN110133023A (en) * 2019-05-17 2019-08-16 西安奕斯伟硅片技术有限公司 Polysilicon selection method, polysilicon and its application in vertical pulling method

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CN102486999A (en) * 2010-12-01 2012-06-06 中芯国际集成电路制造(北京)有限公司 Forming method of grid oxidation layer
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110133023A (en) * 2019-05-17 2019-08-16 西安奕斯伟硅片技术有限公司 Polysilicon selection method, polysilicon and its application in vertical pulling method
CN110133023B (en) * 2019-05-17 2022-04-26 西安奕斯伟材料科技有限公司 Method for selecting polycrystalline silicon, polycrystalline silicon and use thereof in Czochralski method

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