CN114235737A - Method for detecting carbon content in polycrystalline silicon - Google Patents

Method for detecting carbon content in polycrystalline silicon Download PDF

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CN114235737A
CN114235737A CN202111580332.8A CN202111580332A CN114235737A CN 114235737 A CN114235737 A CN 114235737A CN 202111580332 A CN202111580332 A CN 202111580332A CN 114235737 A CN114235737 A CN 114235737A
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carbon content
polycrystalline
sample rod
rod
single crystal
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刘翠
杨伟
李阳
于生海
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Xinjiang Daqo New Energy Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3563Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
    • 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
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34Purifying; Cleaning
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44Sample treatment involving radiation, e.g. heat
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3563Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
    • G01N2021/3572Preparation of samples, e.g. salt matrices

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  • Spectroscopy & Molecular Physics (AREA)
  • Molecular Biology (AREA)
  • Biomedical Technology (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention relates to a method for detecting the carbon content in polycrystalline silicon. A method for detecting the carbon content in polycrystalline silicon comprises the following steps: (1) sampling to obtain a polycrystalline sample rod; (2) cleaning the polycrystalline sample rod to obtain a cleaned polycrystalline sample rod; (3) the cleaned polycrystalline sample rod is arranged in a zone melting furnace, and the furnace is firstly vacuumized and then filled with argon, heated and drawn into a single crystal rod; (4) and (3) preparing the single crystal rod into a single crystal wafer, and measuring the carbon content. The method for detecting the carbon content in the polycrystalline silicon can reduce the influence of the detection process to the lowest level, so that the detection result fully reflects the actual carbon content in the polycrystalline silicon material.

Description

Method for detecting carbon content in polycrystalline silicon
Technical Field
The invention belongs to the technical field of polycrystalline silicon, and particularly relates to a method for detecting carbon content in polycrystalline silicon.
Background
Polycrystalline silicon material is a raw material for producing czochralski crystal or zone-melting single crystal in photovoltaic industry and semiconductor industry, and contains carbon impurities, wherein carbon is harmful impurity and seriously influences the electrical property of silicon. Except that the raw material silicon powder contains carbon, pipelines, graphite materials adopted by silicon material deposition and the like in the production process are all introduction sources of carbon.
At present, in the process of detecting the carbon content in polycrystalline silicon, each family still adopts a graphite heater as a preheater, the cleaning process still only adopts an acid cleaning mode, and nitrogen is used for drying after acid cleaning. The process has the following problems: 1) zone-melting polycrystal appearance stick adopts graphite pre-heater to preheat polycrystal appearance stick, and the principle adopts the eddy current effect that copper heating coil arouses, heats for graphite pre-heater, and carbon impurity can volatilize under high temperature state in the pre-heater, produces carbon pollution to polycrystal appearance stick. 2) The polycrystalline sample rod is obtained by drilling, oil stains can be left on the surface of the polycrystalline sample rod by a drilling machine of the drilling equipment, the sample rod is generally cleaned in an acid cleaning mode in the industry, and the acid cleaning can only remove impurities such as metal on the surface of the polycrystalline sample rod without oil removal effect. 3) After the polycrystalline sample rod is acid-washed, each family uses nitrogen for blow-drying, the purity of the nitrogen cannot meet the purity requirement of the polycrystalline sample rod, and the polycrystalline sample rod is polluted by accompanying oil in a nitrogen gas source. 4) After the polycrystalline sample rod zone-melts the single crystal, the single crystal has more dislocation, and the detection result of the carbon content is influenced.
In view of this, the invention provides a novel method for detecting carbon content in polysilicon, which can effectively avoid the introduction of carbon in the detection process, thereby resulting in accurate detection results.
Disclosure of Invention
The invention aims to provide a method for detecting the carbon content in polycrystalline silicon, which can reduce the influence of a detection process to the lowest level, so that the detection result fully reflects the actual carbon content in the polycrystalline silicon material.
In order to realize the purpose, the adopted technical scheme is as follows:
a method for detecting the carbon content in polycrystalline silicon comprises the following steps:
(1) sampling to obtain a polycrystalline sample rod;
(2) cleaning the polycrystalline sample rod to obtain a cleaned polycrystalline sample rod;
(3) the cleaned polycrystalline sample rod is arranged in a zone melting furnace, and the furnace is firstly vacuumized and then filled with argon, heated and drawn into a single crystal rod;
(4) and (3) preparing the single crystal rod into a single crystal wafer, and measuring the carbon content.
Further, in the step (1), the diameter of the polycrystalline sample rod is 20-25 mm.
Further, in the step (2), after the polycrystalline sample rod is cleaned to remove oil stains, the polycrystalline sample rod is cleaned to remove metal impurities on the surface, and then is cleaned by pure water.
Further, in the step (2), a mixed solution of concentrated nitric acid and hydrofluoric acid is used as a cleaning agent to remove metal impurities on the surface.
Still further, the volume ratio of the concentrated nitric acid to the hydrofluoric acid is 1: 5.
Further, in the step (3), a quartz-coated graphite heater or a tantalum heater is used as a preheater.
Furthermore, in the step (3), the surface of the single crystal rod is smooth and has no bamboo joints.
Further, in the step (4), an infrared spectrometer is used for measuring the carbon content.
Compared with the prior art, the invention has the beneficial effects that:
the polycrystalline silicon material used in the photovoltaic industry and the semiconductor industry contains carbon, and the carbon is also introduced in the czochralski or zone-melting process, so that the introduction of the carbon in the detection link needs to be reduced in order to better evaluate the content level of the carbon in the polycrystalline silicon material. According to the technical scheme, the carbon content in the polycrystalline silicon can be reduced to be below 0.10ppma through the 4 technologies, the influence of the detection process is reduced to the lowest level, and the actual carbon content in the polycrystalline silicon material is fully reflected by the detection result.
Detailed Description
In order to further illustrate the method for detecting the carbon content in polysilicon according to the present invention to achieve the intended purpose of the invention, the following detailed description is given to the method for detecting the carbon content in polysilicon according to the present invention, and the specific implementation manner, structure, features and efficacy thereof, in combination with the preferred embodiments. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
The method for detecting the carbon content in polysilicon according to the present invention will be further described in detail with reference to the following specific embodiments:
aiming at the following problems in the existing polysilicon carbon content detection technology, 1) at present, graphite heaters are still adopted by various families as pre-heaters, and carbon is introduced; 2) the cleaning process still only adopts an acid cleaning mode, and carbon introduced in the sample drilling process is not effectively removed; 3) blowing the acid-washed waste water by nitrogen gas to introduce new carbon impurities; 4) single crystal dislocations affect the results of the detection of carbon content. The novel method for detecting the carbon content in the polycrystalline silicon is provided, so that the introduction of carbon in a detection link can be effectively avoided, and the carbon content in the polycrystalline silicon material can be more accurately evaluated. The technical scheme of the invention is as follows:
a method for detecting the carbon content in polycrystalline silicon comprises the following steps:
(1) sampling to obtain a polycrystalline sample rod;
(2) cleaning the polycrystalline sample rod to obtain a cleaned polycrystalline sample rod;
(3) the cleaned polycrystalline sample rod is arranged in a zone melting furnace, and the furnace is firstly vacuumized and then filled with argon, heated and drawn into a single crystal rod;
(4) and (3) preparing the single crystal rod into a single crystal wafer, and measuring the carbon content.
Preferably, in the step (1), the diameter of the polycrystalline rod is 20-25 mm.
Preferably, in the step (2), after the polycrystalline sample rod is cleaned to remove oil stains, the polycrystalline sample rod is cleaned to remove metal impurities on the surface, and then is cleaned by pure water. Before cleaning the polycrystalline sample rod, cleaning by adopting a cleaning agent to remove oil stains, and removing carbon introduced by sample drilling equipment.
More preferably, in the step (2), a mixed solution of concentrated nitric acid and hydrofluoric acid is used as a cleaning agent to remove metal impurities on the surface.
Further preferably, the volume ratio of the concentrated nitric acid to the hydrofluoric acid is 1: 5.
Preferably, in the step (3), a quartz-coated graphite heater or a tantalum heater is used as a preheater. The heating device of the polycrystalline sample rod is changed into a device method without introducing carbon, and the quartz wrapped graphite heater or the tantalum heater is used as a preheater, so that the introduction of carbon in the heating process during zone melting of polycrystalline silicon can be reduced.
Preferably, in the step (3), the surface of the single crystal rod is smooth and has no bamboo joints. The crystal pulling process is optimized, the bamboo joint phenomenon on the surface of the single crystal after crystal pulling is reduced, the surface of the single crystal rod is smooth, and no bamboo joint is taken as a standard, so that the detection result of carbon content influenced by single crystal dislocation can be reduced.
Preferably, in the step (4), the carbon content is determined by an infrared spectrometer.
Example 1.
The improvement of the embodiment is mainly as follows: during zone melting of the polycrystalline sample rod, a quartz wrapped graphite heater or a tantalum heater is used as a preheater. Secondly, cleaning by adding a cleaning agent in the cleaning process, removing oil stains, and cleaning metal impurities on the surface of the polycrystalline sample rod by using mixed acid of hydrofluoric acid and nitric acid. And thirdly, a link of drying the polycrystalline sample rod by using nitrogen is eliminated, and residual moisture on the surface of the polycrystalline sample rod is extracted by adopting a vacuumizing mode when a zone melting furnace replaces air. And fourthly, optimizing the crystal pulling process, reducing the bamboo joint phenomenon on the surface of the single crystal after crystal pulling, and taking the smooth surface and no bamboo joint of the single crystal rod as the standard.
The specific operation steps are as follows:
(1) and drilling the polycrystalline silicon material by using a drilling machine to drill a polycrystalline sample rod with the diameter of 20-25 mm.
(2) Cleaning the polycrystalline sample rod, comprising the following steps: cleaning by adding a cleaning agent in the process of cleaning the polycrystalline sample rod, and removing oil stains (only by adopting the conventional cleaning agent capable of removing the oil stains in the field); then adopting a volume ratio of 1:5, cleaning metal impurities on the surface of the polycrystalline sample rod by using mixed acid of concentrated nitric acid and concentrated hydrofluoric acid, and finally cleaning by using pure water.
(3) And (3) installing the polycrystalline sample rod in a zone melting furnace, vacuumizing the furnace, and filling argon to replace air.
The link of blowing the polycrystalline sample rod by nitrogen is eliminated, the residual moisture on the surface of the polycrystalline sample rod is extracted by adopting a vacuumizing mode when a zone melting furnace replaces air, and the drying step can be omitted.
(4) The polycrystalline sample rod is heated and zone-melted to form a single crystal rod.
During zone melting of the polycrystalline sample rod, the preheater adopts a quartz wrapped graphite heater or adopts a tantalum heater as the preheater.
Optimizing a crystal pulling process, reducing the bamboo joint phenomenon on the surface of the single crystal after crystal pulling, and taking the smooth surface of the single crystal rod without bamboo joints as a standard. The bamboo joint phenomenon on the surface of the single crystal is eliminated by optimizing the process parameters of different rotating speeds and pulling speeds of the upper shaft and the lower shaft. In the present example, a Danish PVA zone melting furnace is adopted, and the zone melting process parameters are as follows: the rotation speed of the upper shaft is 0.55RPM, the rotation speed of the lower shaft is 25RPM, the feed of the upper shaft is 0.80mm/min, and the feed of the lower shaft is 5 mm/min.
(5) Slicing and polishing the single crystal bar into single crystal chips by a cutting machine and a grinding and polishing machine.
(6) And detecting the carbon content of the single crystal wafer by adopting an infrared spectrometer.
The test results of the test methods before and after the modification are shown in table 1.
TABLE 1
Figure BDA0003425849480000051
As can be seen from Table 1, the carbon content before modification is between 0.20 and 0.20ppma and the carbon content after modification is between 0.01 and 0.10 ppma. The technical scheme of the invention reduces the influence of sample preparation and sampling on the detection result, so that the detection result is closer to the actual carbon content in the polysilicon material.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.

Claims (8)

1. A method for detecting the carbon content in polycrystalline silicon is characterized by comprising the following steps:
(1) sampling to obtain a polycrystalline sample rod;
(2) cleaning the polycrystalline sample rod to obtain a cleaned polycrystalline sample rod;
(3) the cleaned polycrystalline sample rod is arranged in a zone melting furnace, and the furnace is firstly vacuumized and then filled with argon, heated and drawn into a single crystal rod;
(4) and (3) preparing the single crystal rod into a single crystal wafer, and measuring the carbon content.
2. The detection method according to claim 1,
in the step (1), the diameter of the polycrystalline sample rod is 20-25 mm.
3. The detection method according to claim 1,
and (2) after the polycrystalline sample rod is cleaned to remove oil stains, cleaning to remove metal impurities on the surface, and then cleaning with pure water.
4. The detection method according to claim 3,
in the step (2), a mixed solution of concentrated nitric acid and hydrofluoric acid is used as a cleaning agent to remove metal impurities on the surface.
5. The detection method according to claim 4,
the volume ratio of the concentrated nitric acid to the hydrofluoric acid is 1: 5.
6. The detection method according to claim 1,
in the step (3), a quartz-coated graphite heater or a tantalum heater is used as a preheater.
7. The detection method according to claim 1,
in the step (3), the surface of the single crystal rod is smooth and has no bamboo joint.
8. The detection method according to claim 1,
in the step (4), an infrared spectrometer is adopted to determine the carbon content.
CN202111580332.8A 2021-12-22 2021-12-22 Method for detecting carbon content in polycrystalline silicon Pending CN114235737A (en)

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