CN114965663A - System and method for detecting metal element impurities on surface of polycrystalline silicon substrate - Google Patents

System and method for detecting metal element impurities on surface of polycrystalline silicon substrate Download PDF

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CN114965663A
CN114965663A CN202210469892.4A CN202210469892A CN114965663A CN 114965663 A CN114965663 A CN 114965663A CN 202210469892 A CN202210469892 A CN 202210469892A CN 114965663 A CN114965663 A CN 114965663A
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polycrystalline silicon
digestion
inert gas
impurities
leaching solution
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罗李斌
蓝元柯
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Zing Semiconductor Corp
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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    • G01N27/62Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G01N27/626Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas
    • 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
    • G01N1/40Concentrating samples
    • G01N1/4044Concentrating samples by chemical techniques; Digestion; Chemical decomposition
    • 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
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

The invention provides a polycrystalline silicon-based surface metal element impurity detection system which comprises a pretreatment part and a detection part, wherein the pretreatment part at least comprises a digestion unit and a concentration unit, and the system also comprises an inert gas protection device which provides inert gas protection for the digestion unit and the concentration unit. The invention also provides a corresponding method for detecting the metal element impurities on the surface of the polycrystalline silicon substrate.

Description

System and method for detecting metal element impurities on surface of polycrystalline silicon substrate
Technical Field
The invention belongs to the technology of impurity detection of semiconductor materials, and particularly relates to a method and equipment for detecting metal element impurities on a polycrystalline silicon-based surface.
Background
The polysilicon is divided into electronic grade and solar grade according to different purity requirements.
At present, the standard method for detecting the surface metal impurities of electronic grade polysilicon in China is GBT 24579-.
The plasma mass spectrometer is a mature polycrystalline silicon impurity element analyzer, has the advantage of low detection limit, but cannot directly analyze a solid sample, and impurities contained in solutes in the dissolving process are often higher than inherent impurities in an object to be detected, so that the interference is serious, the reproducibility is poor, digestion pretreatment is required, and leaching is performed during detection.
However, the current detection method still cannot meet the requirement of detecting high-purity polycrystalline silicon. In the semiconductor manufacturing industry, the existence of metal impurities can affect the performance of products, so that the introduction of impurity elements on the surface of a silicon wafer in the whole production process of the silicon wafer can reduce the qualification rate of chips of electronic components manufactured in the later period. Specific contamination problems may lead to different defects of the semiconductor device, for example, alkali metal and alkaline earth metal (Na, K, Ca, Mg, Ba, etc.) contamination may lead to a reduction in the breakdown voltage of the element; contamination with transition metals and heavy metals (Fe, Cr, Ni, Cu, Mn, Pb, etc.) can shorten the lifetime of the device or increase the dark current when the device is operated.
Based on the above, the present application provides a technical solution to solve the above technical problems.
Disclosure of Invention
The invention provides a system for detecting metallic element impurities on a polycrystalline silicon-based surface.
The invention provides a method for detecting metallic element impurities on the surface of a polycrystalline silicon base.
The invention provides a system for detecting metallic element impurities on a polysilicon-based surface, which comprises a pretreatment part and a detection part,
the pretreatment part at least comprises a digestion unit and a concentration unit,
the device also comprises an inert gas protection device which provides inert gas protection for the digestion unit and the concentration unit.
In a preferred embodiment of the invention, the inert gas blanketing means is in gas-path communication with the digestion unit and the concentration unit via a digestion tube having two gas-path interfaces.
In a preferred embodiment of the invention, the inert gas protection device is arranged in a ventilation subsystem of the detection system for detecting the metal element impurities on the surface of the polycrystalline silicon.
The second aspect of the present invention provides a method for detecting metal element impurities on a polysilicon-based surface, which is applicable to the system for detecting metal element impurities on a polysilicon-based surface of the present invention, and the method includes:
providing a polysilicon-based sample to be detected;
carrying out a pretreatment step on the polycrystalline silicon-based sample, wherein the pretreatment step comprises first digestion, concentration or a combination thereof to obtain a pretreated polycrystalline silicon-based sample; wherein the pretreatment process is carried out under the protection of inert gas;
the pretreated polycrystalline silicon-based sample is used for subsequent detection of surface metal element impurities.
In a preferred embodiment of the present invention, the polysilicon-based sample to be detected is an electronic grade polysilicon-based sample.
In a preferred embodiment of the present invention, the pressure of the inert gas is controlled in multiple stages, and the multiple stages of control at least include gas pressure stabilization control and gas pressure fine control.
In a preferred embodiment of the invention, the inert gas is used for enabling the pretreatment process to be carried out under the inert protective gas by adopting an in-line sealing mode; the straight-cutting sealing mode comprises an air inlet and an air outlet, and the inert gas is introduced into the digestion pipe through the air inlet.
In a preferred embodiment of the present invention, the pretreated polysilicon-based sample is leached to obtain a first leaching solution;
and the first leaching solution is used for subsequent detection of surface metal element impurities.
In a preferred embodiment of the present invention, performing a second digestion on the first leaching solution to obtain a second leaching solution, wherein the second leaching solution is used for subsequent surface metal element impurity detection.
In a preferred embodiment of the invention, the first leaching solution is subjected to second digestion to obtain a second leaching solution, and the second leaching solution is used for detection by plasma mass spectrometry.
In a preferred embodiment of the present invention, the pressure of the inert gas is not higher than 0.1 MPa.
The invention can bring at least one of the following beneficial effects:
the invention mainly aims at a method for detecting metallic element impurities on the surface of an electronic grade polysilicon base;
the main improvement method of the invention is that the inert gas (such as nitrogen) is introduced by using an inert gas protection device to prevent the particles in the air from entering the digestion solution, thereby achieving the purpose of eliminating the environmental pollution;
the invention can effectively improve the digestion and evaporation rate and shorten the pretreatment time after using an inert gas protection device (such as nitrogen);
in a preferred embodiment of the invention, the digestion solution is used for improving the problem of blockage of an ICPMS sample feeding system caused by direct sample feeding of the soaking solution.
Drawings
The foregoing features, technical features, advantages and embodiments are further described in the following detailed description of the preferred embodiments, which is to be read in connection with the accompanying drawings.
Fig. 1 is an example of the device for detecting the metallic element impurities on the surface of the polycrystalline silicon base, and particularly shows one embodiment of the digestion pipe.
Detailed Description
Various aspects of the invention are described in further detail below.
In the current polysilicon detection, the following scenes are common and cause new problems, and the processing scheme of corresponding solving measures is adopted for solving the new problems:
scene one, problem of pretreatment in standard method for detecting metal impurities on surface of electronic-grade polysilicon
At present, the standard method for detecting the surface metal impurities of electronic grade polysilicon in China comprises GBT 245782-2009 acid leaching-inductively coupled plasma mass spectrometer determination of the surface metal impurities of the polysilicon, and the detection limit of the metal elements of iron, chromium, nickel, zinc, copper and sodium in the GBT 245782-2009 method for detecting the surface metal is 10 pptw.
The method belongs to an open closed method. The polycrystalline silicon is opened to contact with ambient air in the digestion process, and after digestion is finished, a closed environment is used for drying to remove silicon. The pretreatment of the polycrystalline silicon sample is to perform operations such as digestion, concentration and the like in an open digestion tube, and when the open digestion tube is used for analyzing the sample, the blank sample always has the problem of overhigh content of elements such as Fe, Ca, Na and the like.
An improved route to the open-closed process includes:
a protective cover adding method. The method is carried out in the protective cover from the beginning of the digestion of the polycrystalline silicon to the evaporation of the digestion solution, and the volatilized acid liquid and water vapor are condensed on the bottle wall and basically cannot drop into the digestion tube.
A bottle cap opening method can also be adopted. The method is carried out from the beginning of polysilicon digestion to the evaporation of the digestion solution, the whole process is carried out by covering a bottle cap with a hole, and liquid is condensed in the bottle cap and flows back to the digestion tube.
Second, problem in detection of metal impurities on surface of electronic-grade polysilicon in standard detection method
GBT 24579-A2009 acid leaching-inductively coupled plasma mass spectrometer determination of metal impurities on polysilicon surface, serial no: GBT 245782-
Name: determination of metal impurities on polycrystalline silicon surface by acid leaching-inductively coupled plasma mass spectrometer
The following steps are described: the sample is soaked for 60min at 70 ℃ by a mixture (1:1:1:50) of nitric acid, hydrofluoric acid, hydrogen peroxide and water, the leaching solution is collected to an open bottle, heated and evaporated at 110-115 ℃ by a hot plate, 10mL of 5% dilute nitric acid is added after cooling to dissolve residues, and the sample leaching solution is analyzed by ICP/MS.
The technical problem of the invention is that:
(1) fine polysilicon particles are remained in the leaching solution after the leaching solution is evaporated to dryness, and an analysis sample can block an instrument sample introduction system;
(2) the sample leaching solution is susceptible to interference of environmental factors in the process of open evaporation to dryness.
It is generally accepted in the art that the shielding gas may introduce new impurities that may affect the results and therefore this approach is not adopted (national standards, for example). However, the inventor of the present invention finds, through a large number of experiments and analyses, that the detection result is not affected by adding the inert gas protection device to the digestion tube. In particular, when the pressure of the inert gas takes a specific value, no additional significant sources of error are introduced.
The technical concept adopted by the invention comprises the following steps: the existing detection standard gas protection of metal impurities on the surface of electronic-grade polysilicon is improved by introducing inert gas protection through a ventilation system modification and other means (not limited to the means, but the means is more economical). The technical scheme can control the stable reaction speed and stably discharge the silicon substrate, and ensures consistent influence on results.
The invention solves the defects existing in the technical problems that: (1) fine polysilicon particles are left in the leaching solution after the leaching solution is evaporated to dryness, and an analysis sample can block a sample injection system of an instrument to cause the risk of downtime of the instrument; (2) the sample leaching solution is susceptible to interference of environmental factors in the process of open evaporation to dryness.
In conclusion, compared with the prior art, the scheme has the advantages that:
(1) reducing the risk of the sample factors to the breakdown of the instrument;
(2) the influence of environmental factors on the sample is reduced;
(3) the protection device improves the pretreatment efficiency.
Unless defined or stated otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In addition, any methods and materials similar or equivalent to those described herein can be used in the methods of the present invention.
Method
Pretreatment section
The invention discloses a method for detecting metallic element impurities on a polycrystalline silicon-based surface, which comprises the following steps: a polysilicon-based sample to be tested is provided. Carrying out a pretreatment step on the polycrystalline silicon-based sample, wherein the pretreatment step comprises first digestion, concentration or a combination thereof to obtain a pretreated polycrystalline silicon-based sample; wherein the pretreatment process is carried out under the protection of nitrogen. The pretreated polycrystalline silicon-based sample is used for subsequent detection of surface metal element impurities.
Preferably, the polysilicon-based sample to be detected is an electronic grade polysilicon-based sample. It should be understood that the polysilicon-based samples to be tested of the present invention may be applied to other grades of polysilicon-based samples.
The nitrogen gas may be replaced with other inert gases as long as it does not limit the object of the present invention.
In order to control a stable reaction rate and to stably discharge the silicon substrate, and to ensure a uniform effect on the result, the flow rate of the inert gas, particularly nitrogen, is preferably not higher than 0.1 MPa. Preferably not higher than 0.08MPa, 0.06MPa, 0.04MPa, 0.02MPa and a range between any two points. Most preferably not more than 0.02 Mpa.
Detecting part
The subsequent surface elemental metal impurity detection comprises plasma mass spectrometry.
Leaching the pretreated polycrystalline silicon-based sample to obtain a first leaching solution;
and the first leaching solution is used for subsequent detection of surface metal element impurities.
And carrying out second digestion on the first leaching solution to obtain a second leaching solution, wherein the second leaching solution is used for subsequent surface metal element impurity detection.
And carrying out second digestion on the first leaching solution to obtain a second leaching solution, wherein the second leaching solution is used for detecting by a plasma mass spectrometry.
System for controlling a power supply
Pretreatment unit
The invention relates to a system for detecting metallic element impurities on a polysilicon-based surface, which comprises a pretreatment part and a detection part,
the pretreatment part at least comprises a digestion unit and a concentration unit,
the device also comprises an inert gas protection device which provides inert gas protection for the digestion unit and the concentration unit.
The inventors have found that although the use of an inert gas such as nitrogen to protect from impurities in the ambient air can avoid interfering with the experiments, the use of nitrogen is believed by those skilled in the art to introduce new impurities in electronic grade material testing, but the inventors have conducted extensive and intensive experiments to confirm that the protection of nitrogen at low flow rates does not have a major effect on the recovery of heavy metals.
In a preferred embodiment, the inert gas blanket is in gas communication with the digestion unit and the concentration unit via a digestion tube having two gas path connections.
The inventor finds that after the digestion tube in the prior art is replaced by the digestion tubes with the two air path interfaces, the pretreatment process can be protected conveniently in a direct-insertion sealing mode, so that the digestion tube cannot be influenced by external air.
Preferably, the in-line sealing means may be achieved by a digestion tube having an inlet and an outlet. In practice, only the tube cap of the digestion tube needs to be replaced to obtain it (such as shown in the exemplary embodiment of fig. 1).
In a preferred embodiment, the inert gas protection device is arranged in a ventilation subsystem of the detection system for detecting the metal element impurities on the surface of the polycrystalline silicon.
The inventors have found that this integration with existing ventilation systems results in a reduction in the overall cost of the inert gas protection arrangement. For example, in combination with each other under HOOD experimental conditions.
Detection unit
The detection unit of the device comprises a sample leaching unit and a sample digestion unit.
Unless explicitly stated or limited otherwise, the term "or" as used herein includes the relationship of "and". The "sum" is equivalent to the boolean logic operator "AND", the "OR" is equivalent to the boolean logic operator "OR", AND "is a subset of" OR ".
It will be understood that, although the terms first, second, etc. may be used herein to describe various elements, these elements should not be limited by these terms. These terms are only used to distinguish one element from another. Thus, a first element could be termed a second element without departing from the teachings of the present inventive concept.
As used herein, the terms "comprising," "including," or "including" mean that the various ingredients may be used together in a mixture or composition of the invention. Thus, the terms "consisting essentially of and" consisting of are encompassed by the terms "comprising," including, "or" including.
The terms "connected," "communicating," and "connecting" are used broadly and encompass, for example, a fixed connection, a connection through an intervening medium, a connection between two elements, or an interaction between two elements, unless expressly stated or limited otherwise. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art as the case may be.
Other aspects of the invention will be apparent to those skilled in the art in view of the disclosure herein.
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following description will be made with reference to the accompanying drawings. It is obvious that the drawings in the following description are only some examples of the invention, and that for a person skilled in the art, other drawings and embodiments can be derived from them without inventive effort.
It should be noted that the drawings provided in the following embodiments are only for illustrating the basic idea of the present application, and the drawings only show the components related to the present application rather than the number, shape and size of the components in actual implementation, and the type, amount and ratio of the components in actual implementation may be changed arbitrarily, and the layout of the components may be more complicated. For example, the thicknesses of elements in the drawings may be exaggerated for clarity.
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The experimental methods of the following examples, which are not specified under specific conditions, are generally determined according to national standards. If there is no corresponding national standard, it is carried out according to the usual international standards, to the conventional conditions or to the conditions recommended by the manufacturer. Unless otherwise indicated, all parts are parts by weight and all percentages are percentages by weight.
National standards mainly referred to in this context are for example: GBT 24579-2009 acid leaching-inductively coupled plasma mass spectrometer (ICP-ICP) for measuring metal impurities on the surface of polysilicon.
Example 1
(1) Adding HF and HNO again after the leaching solution is evaporated to dryness 3 Digesting the leaching solution by the mixed solution;
(2) when the concentration is started in the experiment, inert gas with a certain flow rate, which can be high-purity nitrogen (0.02MPa), is introduced into an opening of one of the gas paths.
1. Cleaning and digesting the tube: the digestion tube is cleaned by nitric acid (70% nitric acid and equal volume of DIW ultrapure water) and then by DIW;
2. checking and accepting the digestion tube: adding 1mL of 2% dilute nitric acid to rinse the digestion tube, and measuring by utilizing ICP-MS;
3. weighing \ soaking: using tweezers to weigh 30g +/-1 g of electronic grade polysilicon solid to be measured, adding the electronic grade polysilicon solid into a 150ml bottle, and adding HF + HNO 3 +H 2 O 2 +H 2 Digesting in O (v/v ═ 1:1:1:50) digestion solution at constant temperature of 70 ℃ for 60 min;
4. transferring: transferring all digestion solution to a digestion tube with 30ml for evaporation;
5. concentrating and adding acid for digestion: adjusting the temperature of the graphite digestion furnace to 150 ℃, heating, adjusting the gas flow, adding 1ml of HF + HNO after the solution is distilled to dryness 3 (v/v ═ 1:1) and continuing to evaporate;
6. measuring: adding 1ml of 2% dilute nitric acid to measure the constant volume;
7. data processing, concentration calculation formula: c (ppt) ═ sample check concentration (ppt) x volumetric volume (1 ml)/sample mass (g).
See the performance examples for their performance.
Comparative examples 1 to 3
The inventor also compares the open and closed type, the protective cover method and the bottle cap hole opening mode in the first scene. The other test conditions are the same, but the pretreatment modes of the sample are respectively open and closed, a protective cover adding method and a bottle cap hole opening mode.
See the performance examples for their performance.
Examples of Performance
The results of the tests of the control, example and comparative examples 1 to 3 were subjected to performance analysis:
(1) and (5) analyzing the detection result, and referring to tables 1-3.
TABLE 1 analysis of comparative results of example 1 and comparative examples 1 to 3
Figure BDA0003626069240000091
TABLE 2 analysis of the results of the measurement of the blank control group and comparative examples 1 to 3
Figure BDA0003626069240000101
Figure BDA0003626069240000102
TABLE 3 test results (full program white and MDL data) of the examples
Element(s) 2A-1.3ML 10A-1.3ML 10B-1.3ML 2A 0.8g 10B-2.5ML 12B-1.5ML 2A-1.6ML
Na 0.439 0.499 0.524 2.403 0.318 0.18 0.537
Al 0.807 0.454 0.879 0.990 1.285 0.403 1.003
K 0.17 0.112 0.277 1.386 0.326 0.185 0.728
Cr 1.632 2.226 1.758 4.470 2.891 0.301 2.542
Fe 0.956 0.859 1.033 1.924 1.285 0.71 1.447
Ni 0.082 0.055 0.247 0.208 0.247 0.082 0.411
Cu 0.56 0.43 0.32 5.294 0.52 0.51 0.71
Zn 0.141 0.188 0.705 3.019 0.705 0.611 1.174
Element(s) 10B-QB- 1.3ML 12B-QB- 0.8ML 2B-QB- 1.3ML 10A-QB- 1.6ML 10B Mean value of MDL
Na 0.516 1.854 0.481 0.279 0.568 0.717 2.0
Al 2.764 1.59 1.013 0.571 0.488 1.021 2.0
K 2.017 0.735 0.57 0.427 0.445 0.615 1.7
Cr 9.517 0.45 1.415 11.8 0.832 3.320 10.9
Fe 3.173 2.809 1.673 3.568 0.27 1.642 3.1
Ni 0.827 0.108 0.28 0.243 0.176 0.247 0.6
Cu 0.478 0.856 0.879 0.363 0.008 0.911 4.2
Zn 0.383 1.265 0.383 0.383 0.031 0.749 2.4
MDL refers to: detection limit.
(2) Blank labeling recovery experiment is carried out on polycrystalline silicon sample
The experimental conditions adopted were:
1. cleaning and digesting the tube: the digestion tube is washed with nitric acid (70% nitric acid plus an equal volume of DIW) and then with DIW;
2. checking and accepting the digestion tube: adding 1mL of 2% dilute nitric acid to rinse the digestion tube, and measuring by utilizing ICP-MS;
3. acid/label addition apparatus: taking 10ml of HF + HNO3 digestion solution, and covering a gas path protective cover;
4. acid-dispelling and concentration: adjusting the temperature of the graphite digestion furnace to 150 ℃, heating, adjusting the gas flow, and finishing the distillation of the solution;
4. measuring: adding 2% dilute nitric acid to measure the volume
5. Data processing
The results obtained are shown in table 4 below:
TABLE 4 blank spiking recovery Experimental data
Figure BDA0003626069240000121
And (4) conclusion:
through the experimental data of the standard recovery rates of 50ppt and 100ppt, the nitrogen protection can be used for avoiding the interference of impurities in the ambient air to the experiment. It has been demonstrated that the protection of nitrogen at low flow rates does not have a major impact on heavy metal recovery. In summary, through the analysis of the data, it can be seen that: compared with different protection devices, the nitrogen protection real blank is the best choice. And the nitrogen protection device can well ensure less pollution, so that the detection result is closer to an accurate value.
Based on the present application, one skilled in the art should appreciate that one aspect described herein may be implemented independently of any other aspects and that two or more of these aspects may be combined in various ways. For example, an apparatus may be implemented and/or a method practiced using any number and aspects set forth herein. Additionally, such an apparatus may be implemented and/or such a method may be practiced using other structure and/or functionality in addition to one or more of the aspects set forth herein.
It should be noted that the above embodiments can be freely combined as necessary. The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
All documents referred to herein are incorporated by reference into this application as if each were individually incorporated by reference. Furthermore, it should be understood that various changes or modifications can be made by those skilled in the art after reading the above disclosure of the present invention, and these equivalents also fall within the scope of the appended claims of the present application.

Claims (10)

1. A system for detecting metallic element impurities on the surface of polycrystalline silicon comprises a pretreatment part and a detection part, and is characterized in that,
the pretreatment portion includes at least a digestion unit and a concentration unit,
the device also comprises an inert gas protection device which provides inert gas protection for the digestion unit and the concentration unit.
2. The polysilicon-based surface metallic element impurity detection system of claim 1, wherein the inert gas shield is in gas communication with the digestion unit and the concentration unit via a digestion tube having two gas path interfaces.
3. The system for detecting metallic impurities on a polysilicon-based surface according to claim 1,
the inert gas protection device is arranged in a ventilation subsystem of the detection system for detecting the metal element impurities on the surface of the polycrystalline silicon base.
4. A method for detecting metallic element impurities on a polycrystalline silicon-based surface, which is applied to the system for detecting metallic element impurities on a polycrystalline silicon-based surface according to claims 1 to 3, and comprises the following steps:
providing a polysilicon-based sample to be detected;
carrying out a pretreatment step on the polycrystalline silicon-based sample, wherein the pretreatment step comprises first digestion, concentration or a combination thereof to obtain a pretreated polycrystalline silicon-based sample; wherein the pretreatment process is carried out under the protection of inert gas;
the pretreated polycrystalline silicon-based sample is used for subsequent detection of surface metal element impurities.
5. The method for detecting metallic element impurities on the surface of polycrystalline silicon according to claim 4, wherein the polycrystalline silicon-based sample to be detected is an electronic grade polycrystalline silicon-based sample.
6. The method for detecting metallic element impurities on a polysilicon-based surface according to claim 4,
the pressure of the inert gas is controlled in a multi-stage mode, and the multi-stage control at least comprises stable air pressure control and precise air pressure control; or
The inert gas is used for carrying out the pretreatment process under the inert protective gas by adopting a direct-insertion sealing mode; the straight-cutting sealing mode comprises an air inlet and an air outlet, and the inert gas is introduced into the digestion pipe through the air inlet.
7. The method for detecting metallic element impurities on a polysilicon-based surface according to claim 4,
leaching the pretreated polycrystalline silicon-based sample to obtain a first leaching solution;
and the first leaching solution is used for subsequent detection of surface metal element impurities.
8. The method for detecting metallic element impurities on a polysilicon-based surface according to claim 7,
and carrying out second digestion on the first leaching solution to obtain a second leaching solution, wherein the second leaching solution is used for subsequent surface metal element impurity detection.
9. The method for detecting the impurities of the metal elements on the base surface of the polycrystalline silicon as claimed in claim 7, wherein the first leaching solution is subjected to second digestion to obtain a second leaching solution, and the second leaching solution is used for detection by a plasma mass spectrometry.
10. The method for detecting metallic element impurities on the surface of polycrystalline silicon based according to any one of claims 4 to 9, wherein the pressure of the inert gas is not higher than 0.1 MPa.
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CN117191932A (en) * 2023-11-06 2023-12-08 山东有研艾斯半导体材料有限公司 Method and system for testing metal recovery rate of silicon wafer surface

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