CN111270300A - Preparation method of gas-phase doped zone-melting silicon single crystal - Google Patents

Preparation method of gas-phase doped zone-melting silicon single crystal Download PDF

Info

Publication number
CN111270300A
CN111270300A CN201811476667.3A CN201811476667A CN111270300A CN 111270300 A CN111270300 A CN 111270300A CN 201811476667 A CN201811476667 A CN 201811476667A CN 111270300 A CN111270300 A CN 111270300A
Authority
CN
China
Prior art keywords
single crystal
polycrystal
resistivity
silicon single
gas
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201811476667.3A
Other languages
Chinese (zh)
Inventor
王永涛
尚锐刚
刘建涛
李明飞
鲁进军
张建
闫志瑞
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Grinm Semiconductor Materials Co Ltd
Original Assignee
Grinm Semiconductor Materials Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Grinm Semiconductor Materials Co Ltd filed Critical Grinm Semiconductor Materials Co Ltd
Priority to CN201811476667.3A priority Critical patent/CN111270300A/en
Publication of CN111270300A publication Critical patent/CN111270300A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • 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
    • C30B13/00Single-crystal growth by zone-melting; Refining by zone-melting
    • C30B13/08Single-crystal growth by zone-melting; Refining by zone-melting adding crystallising materials or reactants forming it in situ to the molten zone
    • C30B13/10Single-crystal growth by zone-melting; Refining by zone-melting adding crystallising materials or reactants forming it in situ to the molten zone with addition of doping materials
    • C30B13/12Single-crystal growth by zone-melting; Refining by zone-melting adding crystallising materials or reactants forming it in situ to the molten zone with addition of doping materials in the gaseous or vapour state
    • 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

Abstract

The invention discloses a preparation method of a gas-phase doped zone-melting silicon single crystal, which comprises the following steps: (1) pulling the primary polycrystal into a monocrystal or polycrystal according to a normal zone melting crystal pulling process; (2) grinding the drawn single crystal or polycrystal into cone, notching, cleaning and drying; (3) and (3) charging the treated single crystal or polycrystal into a furnace, setting the doping flow according to the target resistivity, and finishing the pulling of the single crystal according to the normal gas phase doping zone melting crystal pulling process. According to the method for preparing the gas phase doping zone melting silicon single crystal, impurities in the silicon core are uniformly distributed in the whole single crystal or polycrystal formed by drawing as much as possible through first drawing instead of being limited in the silicon core, so that the fluctuation of the central resistivity of the gas phase doping zone melting silicon single crystal caused by nonuniform stirring of the silicon core impurities is reduced, the nonuniformity of the axial resistivity and the radial resistivity of the single crystal is effectively reduced, and the target resistivity hit rate and the stability of the gas phase doping zone melting silicon single crystal are improved.

Description

Preparation method of gas-phase doped zone-melting silicon single crystal
Technical Field
The invention relates to a preparation method of a silicon single crystal, in particular to a preparation method of a gas-phase doped zone-melting silicon single crystal.
Background
In the process of pulling the zone-melting silicon single crystal, a certain amount of impurities are required to be doped in order to obtain certain electrical properties so as to improve the electrical activity of the zone-melting silicon single crystal. At present, the main doping methods of the zone-melting silicon single crystal are Neutron Transmutation Doping (NTD), gas phase doping, and the like. Among them, the single crystal obtained by Neutron Transmutation Doping (NTD) has the best nonuniformity of axial and radial resistivities, but is gradually replaced by the gas phase doping technology due to the defects of long production period, high production cost, limitation of neutron irradiation, and the like. However, with the development of integrated circuit technology, the requirement for the nonuniformity of the resistivity of the silicon wafer is higher and higher, and how to improve the nonuniformity of the resistivity of the gas-phase doped zone-melting silicon single crystal is very important.
At present, the high nonuniformity of the resistivity of the gas-phase doped zone-melting silicon single crystal is mainly reflected in large fluctuation of the resistivity of a central point. The polycrystalline rod used by the zone-melting silicon single crystal is prepared on a silicon core through chemical vapor deposition, the resistivity of the polycrystal mainly comes from the silicon core, the resistivity of the silicon core is generally 50-100 omega cm, the target resistance of the gas-phase doped silicon single crystal is generally within 100 omega cm, and if the impurities in the silicon core are not uniformly distributed in the single crystal drawing process, the fluctuation of the resistivity is inevitably caused. For this reason, those skilled in the art are constantly improving the doping process, including eccentric pulling, forward and reverse pulling, etc., but the results are very poor.
Disclosure of Invention
The invention aims to provide a preparation method of a gas-phase doped zone-melting silicon single crystal, which is used for improving the target resistivity hit rate and stability of the gas-phase doped zone-melting silicon single crystal.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing a gas phase doped zone-melting silicon single crystal comprises the following steps:
(1) pulling the primary polycrystal into a monocrystal or polycrystal according to a normal zone melting crystal pulling process;
(2) grinding the drawn single crystal or polycrystal into cone, notching, cleaning and drying;
(3) and (3) charging the treated single crystal or polycrystal into a furnace, setting the doping flow according to the target resistivity, and finishing the pulling of the single crystal according to the normal gas phase doping zone melting crystal pulling process.
The invention has the advantages that:
according to the method for preparing the gas phase doping zone melting silicon single crystal, impurities in the silicon core are uniformly distributed in the whole single crystal or polycrystal formed by drawing as much as possible through first drawing instead of being limited in the silicon core, so that the fluctuation of the central resistivity of the gas phase doping zone melting silicon single crystal caused by nonuniform stirring of the silicon core impurities is reduced, the nonuniformity of the axial resistivity and the radial resistivity of the single crystal is effectively reduced, and the target resistivity hit rate and the stability of the gas phase doping zone melting silicon single crystal are improved.
Drawings
FIG. 1 is a schematic view of a process flow of a gas-phase doped float-zone silicon single crystal according to the present invention.
FIG. 2 is a result of measuring the resistivity at the axial center point of the gas phase doped zone-melting silicon single crystal prepared in comparative example 1.
FIG. 3 shows the results of measuring the resistivity at the axial center point of the gas phase doped zone-melting silicon single crystal produced in example 1.
Detailed Description
The present invention is further illustrated by the following figures and examples, which are not meant to limit the scope of the invention.
Example 1
By using the method, the primary polycrystalline silicon is pulled into the silicon single crystal, and then the silicon single crystal is grinded, grooved, corroded and dried to prepare the 5-inch N-type <111> air-doped silicon single crystal with the target resistivity of 65-85 omega cm. The flow rate of the doping gas (phosphine) is 30mL/min, the flow of the carrier gas argon is 1L/min, the flow rate of the mixed gas entering the furnace is 100mL/min, and the pressure entering the furnace is 3 bar.
Comparative example 1
The primary polysilicon was directly prepared into a 5-inch air-doped silicon single crystal under the same conditions as in example 1.
The stability of the resistivity of the axial center point and the nonuniformity of the radial resistivity of the gas-doped silicon single crystal prepared by the two methods are evaluated, and particularly as shown in fig. 2, fig. 3 and table 1, the axial and radial uniformity of the resistivity of the gas-phase doped zone-melting silicon single crystal prepared by the method are obviously improved.
TABLE 1
Preparation method Target resistivity Measured resistivity Single crystal bulk non-uniformity (RRV)
Example 1 65-85Ω·cm 68-80Ω·cm 11.6%
Comparative example 1 65-85Ω·cm 65-84Ω·cm 19.9%

Claims (1)

1. A preparation method of a gas-phase doped zone-melting silicon single crystal is characterized by comprising the following steps:
(1) pulling the primary polycrystal into a monocrystal or polycrystal according to a normal zone melting crystal pulling process;
(2) grinding the drawn single crystal or polycrystal into cone, notching, cleaning and drying;
(3) and (3) charging the treated single crystal or polycrystal into a furnace, setting the doping flow according to the target resistivity, and finishing the pulling of the single crystal according to the normal gas phase doping zone melting crystal pulling process.
CN201811476667.3A 2018-12-04 2018-12-04 Preparation method of gas-phase doped zone-melting silicon single crystal Pending CN111270300A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811476667.3A CN111270300A (en) 2018-12-04 2018-12-04 Preparation method of gas-phase doped zone-melting silicon single crystal

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811476667.3A CN111270300A (en) 2018-12-04 2018-12-04 Preparation method of gas-phase doped zone-melting silicon single crystal

Publications (1)

Publication Number Publication Date
CN111270300A true CN111270300A (en) 2020-06-12

Family

ID=70994862

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811476667.3A Pending CN111270300A (en) 2018-12-04 2018-12-04 Preparation method of gas-phase doped zone-melting silicon single crystal

Country Status (1)

Country Link
CN (1) CN111270300A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114855262A (en) * 2022-07-05 2022-08-05 江苏鑫华半导体科技股份有限公司 Pretreatment method for zone-melting polycrystalline silicon rod
CN115558999A (en) * 2022-10-09 2023-01-03 包头美科硅能源有限公司 Method for improving resistivity hit degree of large-size N-type single crystal

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09286688A (en) * 1996-04-22 1997-11-04 Komatsu Electron Metals Co Ltd Method for doping gas to silicon single crystal
CN1267751A (en) * 2000-03-30 2000-09-27 天津市半导体材料厂 Vertical pulling and zone melting process of producing monocrystalline silicon
CN101565185A (en) * 2008-04-23 2009-10-28 信越化学工业株式会社 Method of manufacturing polycrystalline silicon rod
CN102534752A (en) * 2012-03-08 2012-07-04 天津市环欧半导体材料技术有限公司 Czochralski zone melting gas doping method for preparing zone-melted silicon single crystal
CN102534749A (en) * 2012-02-14 2012-07-04 天津市环欧半导体材料技术有限公司 Method for preparing 6-inch N type solar silicon single crystals by Czochralski and float zone methods
CN102534751A (en) * 2012-03-08 2012-07-04 天津市环欧半导体材料技术有限公司 Casting zone melting gas doping method for preparing zone-melted silicon single crystal
CN107109692A (en) * 2015-01-06 2017-08-29 信越化学工业株式会社 The manufacture method and solar cell of study on floating zone silicon used for solar batteries

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09286688A (en) * 1996-04-22 1997-11-04 Komatsu Electron Metals Co Ltd Method for doping gas to silicon single crystal
CN1267751A (en) * 2000-03-30 2000-09-27 天津市半导体材料厂 Vertical pulling and zone melting process of producing monocrystalline silicon
CN101565185A (en) * 2008-04-23 2009-10-28 信越化学工业株式会社 Method of manufacturing polycrystalline silicon rod
CN102534749A (en) * 2012-02-14 2012-07-04 天津市环欧半导体材料技术有限公司 Method for preparing 6-inch N type solar silicon single crystals by Czochralski and float zone methods
CN102534752A (en) * 2012-03-08 2012-07-04 天津市环欧半导体材料技术有限公司 Czochralski zone melting gas doping method for preparing zone-melted silicon single crystal
CN102534751A (en) * 2012-03-08 2012-07-04 天津市环欧半导体材料技术有限公司 Casting zone melting gas doping method for preparing zone-melted silicon single crystal
CN107109692A (en) * 2015-01-06 2017-08-29 信越化学工业株式会社 The manufacture method and solar cell of study on floating zone silicon used for solar batteries

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114855262A (en) * 2022-07-05 2022-08-05 江苏鑫华半导体科技股份有限公司 Pretreatment method for zone-melting polycrystalline silicon rod
CN115558999A (en) * 2022-10-09 2023-01-03 包头美科硅能源有限公司 Method for improving resistivity hit degree of large-size N-type single crystal

Similar Documents

Publication Publication Date Title
CN106128938B (en) A kind of VDMOS device method that thick-layer extension is prepared on thin Sb substrates
KR101303422B1 (en) Method for Manufacturing Single Crystal Ingot and Single Crystal Ingot, Wafer manufactured by the same
CN104960100B (en) A kind of processing method improving silicon single crystal rod utilization rate
CN111270300A (en) Preparation method of gas-phase doped zone-melting silicon single crystal
KR102275678B1 (en) Method for manufacturing n-type silicon single crystal, n-type silicon single crystal ingot, silicon wafer, and epitaxial silicon wafer
JP2007314374A (en) Manufacturing method of fz single crystal silicon using silicon crystal rod manufactured by cz method as raw material
CN102978699A (en) Growth of boron and gallium co-doped heavy doped p-type monocrystalline silicon and doping method thereof
CN103337506A (en) Preparation technology of silicon epitaxial wafer for CCD device
CN113584585B (en) Production method of heavily As-doped silicon single crystal capable of reducing head resistivity
CN112048761B (en) Large-diameter monocrystalline silicon shouldering growth process
TW201907057A (en) Method for manufacturing n-type single crystal, n-type single crystal ingot, tantalum wafer and epitaxial wafer
EP3814555B1 (en) Sample rod resistivity measurement during single crystal silicon ingot production
DE112010004657B4 (en) Single-crystal manufacturing apparatus and a single-crystal production method
US10954606B2 (en) Methods for modeling the impurity concentration of a single crystal silicon ingot
CN104465721A (en) Silicon carbide epitaxial material and preparing method thereof
CN103996608B (en) The method improving epilayer resistance rate uniformity
JP2019202913A (en) Method of measuring resistivity of raw material crystal and method of manufacturing fz silicon single crystal
CN114959878A (en) Method for improving axial resistivity uniformity of CZ method high-resistance semiconductor single crystal
JP2005035816A (en) Method for manufacturing silicon single crystal and silicon single crystal
EP3814557B1 (en) Growth of plural sample rods to determine impurity build-up during production of single crystal silicon ingots
CN114318507B (en) Drawing method of heavy arsenic-doped large-diameter low-resistance silicon single crystal
CN102623285A (en) Silicon electrode plate for plasma etching
CN115194566B (en) Method for positioning equal-diameter zero position of monocrystalline silicon crystal bar
JP6963265B1 (en) Manufacturing method of silicon epitaxial wafer
CN202297858U (en) Crucible for improving uniformity of melt concentration

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
CB02 Change of applicant information
CB02 Change of applicant information

Address after: 101300 south side of Shuanghe Road, Linhe Industrial Development Zone, Shunyi District, Beijing

Applicant after: Youyan semiconductor silicon materials Co.,Ltd.

Address before: 101300 south side of Shuanghe Road, Linhe Industrial Development Zone, Shunyi District, Beijing

Applicant before: GRINM SEMICONDUCTOR MATERIALS Co.,Ltd.

RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20200612