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CN113495095A - Silicon wafer metal impurity detection sample protection device and silicon wafer metal impurity detection method - Google Patents

Silicon wafer metal impurity detection sample protection device and silicon wafer metal impurity detection method
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Publication number
CN113495095A
CN113495095ACN202010258528.4ACN202010258528ACN113495095ACN 113495095 ACN113495095 ACN 113495095ACN 202010258528 ACN202010258528 ACN 202010258528ACN 113495095 ACN113495095 ACN 113495095A
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China
Prior art keywords
sample
silicon wafer
protection device
metal impurity
impurity detection
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Chinese (zh)
Inventor
陈宇驰
张俊宝
陈猛
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Shanghai Chaosi Semiconductor Co ltd
Chongqing Advanced Silicon Technology Co ltd
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Shanghai Chaosi Semiconductor Co ltd
Chongqing Advanced Silicon Technology Co ltd
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Priority to CN202010258528.4ApriorityCriticalpatent/CN113495095A/en
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Abstract

Translated fromChinese

本发明公开了一种硅片金属杂质检测样品保护装置及硅片金属杂质检测方法,通过本发明公开的方案,可以将金属杂质检测样品放置在保护装置容纳腔中的自动进样器上,由于洁净气流循环系统可以为该保护装置内部输入洁净气流,并采用了一定风速的排风,所以使得自动进样器附近空间不受周围的大气波动影响,且该保护装置将金属杂质检测样品与外部污染源隔离,提升了检测的稳定性和准确性。

Figure 202010258528

The invention discloses a silicon wafer metal impurity detection sample protection device and a silicon wafer metal impurity detection method. Through the scheme disclosed in the invention, the metal impurity detection sample can be placed on the automatic sampler in the accommodating chamber of the protection device. The clean airflow circulation system can input clean airflow into the protection device, and adopts a certain wind speed to exhaust air, so that the space near the autosampler is not affected by the surrounding atmospheric fluctuations, and the protection device separates the metal impurity detection sample from the outside. Isolation of pollution sources improves the stability and accuracy of detection.

Figure 202010258528

Description

Silicon wafer metal impurity detection sample protection device and silicon wafer metal impurity detection method
Technical Field
The invention relates to the technical field of silicon wafer metal impurity detection for integrated circuits, in particular to a silicon wafer metal impurity detection sample protection device and a silicon wafer metal impurity detection method.
Background
In the large-scale integrated circuit manufacturing process, along with the continuous reduction of the size of a device, the line width of a semiconductor is narrower and narrower, and the cleaning degree of a silicon wafer has larger and larger influence on the yield of the device, especially on metal impurities of the silicon wafer. Metallic contamination of the superstate level can already cause device failures of different degrees, reducing the yield of the production line. Different metal pollution can cause defects of devices with different reasons, and the pollution of alkali metals such as sodium, potassium, calcium, magnesium and the like can cause GOI (Gate Oxide Integrity) deterioration; contamination with heavy metals such as cupronickel can shorten minority carrier lifetime and increase leakage current. Therefore, the metal impurities of the silicon wafer must be analyzed before the silicon wafer is shipped and taken off line.
At present, the most advanced metal impurity analysis tool in a silicon wafer production factory is an inductively coupled plasma mass spectrometer (ICP-MS), a silicon wafer sample preparation system is used as an aid, metal impurities on a silicon wafer are recovered in a recovery liquid by a gas phase decomposition method, and the recovery liquid is analyzed by the ICP-MS.
In the method, the interior of the ICP-MS and the interior of the silicon wafer sample preparation system respectively belong to a closed clean space, so that the sample preparation process of the silicon wafer sample preparation system and the sample entering the ICP-MS are not influenced by the external environment. However, because of more analysis elements, one recycling solution sample needs 5 to 7 minutes for ICP-MS analysis, and other samples are exposed to the atmosphere in a laboratory in the time period, so that the cleanliness of the sample is inevitably influenced by the environment in the laboratory, and the accuracy of analysis of metal impurities in the silicon wafer is influenced. Meanwhile, the laboratory environment is greatly influenced by personnel, so that the detection limit is high.
Disclosure of Invention
The invention provides a silicon wafer metal impurity detection sample protection device and a silicon wafer metal impurity detection method, aiming at the problems of inaccurate detection result and high detection limit caused by insufficient clean protection of a sample in the existing silicon wafer metal impurity detection process.
In order to achieve the purpose, the invention adopts the following specific technical scheme:
a silicon chip metal impurity detection sample protection device comprises a protection shell with a containing cavity, an automatic sample injector for containing a silicon chip metal impurity detection sample, an automatic sample injection pipe, a shielding piece and a clean airflow circulating system;
an operation opening communicated with the containing cavity and a first through hole matched with the outer diameter of the automatic sampling tube are formed in the outer surface of the protective shell, the area of the operation opening is smaller than that of the shielding piece, and the clean airflow circulating system comprises a fan filter unit and an exhaust fan which are arranged on the protective shell;
in the protection user state, the auto-sampler is located in the chamber that holds of protection casing, with the auto-sampler pipe that the auto-sampler is connected passes first through-hole is connected with outside test analysis appearance, shelter from the piece set up in on the protection casing and will the operation mouth shelters from, fan filter unit will clean air current input hold the chamber, the exhaust fan will clean air current in the protection casing is discharged.
Optionally, a filter screen made of polytetrafluoroethylene material is arranged in the fan filter unit.
Optionally, the area of the air outlet of the fan filter unit is 900cm2~1200cm2
Optionally, the autosampler has a cable, still be formed with on the protection casing with the external diameter assorted second through-hole of cable, in the protection user state, the cable passes the second through-hole is connected with external power source.
Optionally, the shielding sheet is a polyethylene film sheet.
Optionally, the protection casing includes the shell body and sets up interior casing in the shell body, hold the chamber by interior casing encloses to establish and forms, the bottom of interior casing is the board of punching a hole for bear the weight of autosampler, the exhaust fan with the shell body with the interior casing encloses the interlayer space connection of establishing, in order to discharge clean air current in the interlayer space.
Optionally, the fan filter unit and the exhaust fan are arranged on the top layer of the outer shell.
Optionally, the outer housing and the inner housing are made of polypropylene material.
Optionally, the outer casing is 600mm ~ 700mm long, 600mm ~ 700mm wide, and the height is 1000 mm's cuboid, the interior casing is 500mm ~ 600mm long, 500mm ~ 600mm wide, 500mm ~ 600mm high cuboid, the adjacent surface of cuboid passes through polypropylene plastic welding technique and splices mutually.
Further, the invention also provides a silicon wafer metal impurity detection method, which comprises the following steps:
s1: a silicon wafer sample preparation system is used for preparing a silicon wafer metal impurity detection sample;
s2: opening an operation window of the silicon wafer sample preparation system, taking out a prepared silicon wafer metal impurity detection sample from the silicon wafer sample preparation system through the operation window, and covering a sample bottle containing the silicon wafer metal impurity detection sample;
s3: opening a clean air flow circulating system in any one of the monocrystalline silicon metal impurity detection sample protection devices;
s4: transporting the capped sample vial to the vicinity of the protective device;
s5: when the working time of the clean air flow circulating system reaches a preset time threshold, taking down a shielding sheet for shielding the operation port, placing the capped sample bottle on the automatic sample injector, and after opening a cap covered on the sample bottle, shielding the operation port by using the shielding sheet;
s6; and the automatic sample injector sends the monocrystalline silicon metal impurity detection sample into the test analyzer through the automatic sample injection pipe for test analysis to obtain a detection result.
The clean gas in the inner shell can reach the following parameters when the working time of the clean gas flow circulating system reaches a preset time threshold: the humidity is less than 45 percent, the 0.1um particles < =1ea/m3, the content of lithium sodium magnesium aluminum potassium calcium titanium vanadium chromium manganese iron cobalt nickel zinc molybdenum tungsten in the gas is less than 1ng/L respectively, and the content of ammonium chloride fluorine chlorine bromine nitrite nitrate radical sulfate radical phosphate radical ions is less than 1 ng/L.
Advantageous effects
According to the silicon wafer metal impurity detection sample protection device and the silicon wafer metal impurity detection method, metal impurity detection samples can be placed on the automatic sample injector in the accommodating cavity of the protection device, clean air flow can be input into the protection device through the clean air flow circulating system, and air exhaust with a certain air speed is adopted, so that the space near the automatic sample injector is not influenced by surrounding atmospheric fluctuation, the metal impurity detection samples are isolated from an external pollution source through the protection device, and the stability and accuracy of detection are improved.
Drawings
Fig. 1 is a schematic view of a part of a structure of a silicon wafer metal impurity detection sample protection device according to a first embodiment of the present invention.
Fig. 2 is a schematic view of the airflow direction in the protection device according to the first embodiment of the present invention.
Fig. 3 is a schematic flow chart of a method for detecting metal impurities in a silicon wafer according to a second embodiment of the present invention.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The embodiment provides a silicon chip metal impurity detection sample protection device, and a partial structure thereof please refer to fig. 1, including a protection housing having a containing cavity, an autosampler tube, a shielding sheet and a clean airflow circulation system, wherein an operation port penetrating through the containing cavity and a first throughhole 11 matching with the outer diameter of the autosampler tube are formed on the outer surface of the protection housing, the area of the operation port is smaller than that of the shielding sheet, the clean airflow circulation system includes an FFU (Fan Filter Unit) 12 and anexhaust Fan 13 arranged on the protection housing, and a detector can put a metal impurity detection sample on the autosampler in the containing cavity through the operation port.
In a protection use state, the automatic sample injector is located in the containing cavity of the protection shell, the automatic sample injection pipe connected with the automatic sample injector penetrates through the first through hole to be connected with an external test analyzer, the shielding sheet is arranged on the protection shell and shields the operation opening to prevent external pollution from entering the containing cavity to pollute a sample, meanwhile, the fan filter unit inputs clean air flow into the containing cavity, the exhaust fan exhausts the clean air flow in the protection shell to keep the protection shell in positive pressure to the external environment so as to reduce pollution of atmospheric quality fluctuation around the protection shell to the sample on the automatic sample injector, such as passing of people and the like.
In practical application, when a silicon wafer metal impurity detection sample needs to be protected to prevent the silicon wafer metal impurity detection sample from being polluted, a metal-free organic matter-free volatilization particle-free protective shell which is independent from the atmospheric environment of a laboratory and is shown in fig. 1 can be built based on an automatic sample injector connected with an automatic sample injection pipe, namely the protective shell is built around the automatic sample injector to protect the silicon wafer metal impurity detection sample.
The fan filter unit in this embodiment is provided with the filter screen to the filtering impurity, filter screen are made by the polytetrafluoroethylene material in this embodiment, replace the quartz filter screen by polytetrafluoroethylene material filter screen and can stop hydrofluoric acid fog in the sample to corrode quartzy release metal ion. Optionally, the area of the air outlet of the fan filter unit in this embodiment may be 900cm2~1200cm2Of course, in other embodiments, the area of the air outlet of the fan filter unit may also be other values.
In some embodiments, the battery is disposed in the autosampler, and the autosampler does not need to be connected to an external power source, but in other embodiments, the autosampler has a cable, and the protective housing should further have a second throughhole 15 matching with the outer diameter of the cable, and in the protective use state, the cable passes through the second throughhole 15 and is connected to the external power source, so as to supply power to the autosampler. In fig. 1, the first through hole is disposed on a side surface of the protection housing, and the second throughhole 15 is disposed on a surface of the protection housing opposite to the operation opening, and it should be noted that the first throughhole 11 and the second throughhole 15 may be disposed at flexible positions, for example, may be disposed on the same surface. The sizes of the first throughhole 11 and the second throughhole 15 in this embodiment may also be flexibly set, for example, the diameter of the first throughhole 11 may be 3cm, and the diameter of the second throughhole 15 may be 6 cm.
The shielding sheet in the embodiment can be a polyethylene film, specifically, 6 polyethylene films with the length of 600-700 mm, the width of 100mm and the thickness of 5mm can be used as shielding in the operation opening.
In one example, the protective housing may be directly formed by a single housing, in which case a carrier plate for placing the autosampler may be provided in the middle of the housing, the carrier plate having punched holes thereon, the exhaust fan being provided at the bottom of the single housing, and the fan filter unit being provided at the top of the single housing.
In another preferred example, the protective casing comprises an outer casing and an inner casing disposed in the outer casing, that is, as shown in fig. 1, in which case the receiving cavity is defined by the inner casing, the bottom layer of the inner casing is aperforated plate 14 for carrying the autosampler, and the exhaust fan is connected with the interlayer space defined by the outer casing and the inner casing to exhaust the clean air flow in the interlayer space, for this example, it is preferred that a fan filter set and an exhaust fan are disposed on the top layer of the outer casing, the FFU of this example can feed clean air with a wind speed of 2m/s-4m/s to the inner casing, the air flow flows from the top downwards to the interlayer through the perforated holes of the bottom plate, and then is exhausted by the acid exhaust fan with a wind speed of 8-12m/s, in which case the air flow direction in the protective device can be shown in fig. 2, it should be noted that, for this example, in order to connect the automatic sample feeding tube connected to the automatic sample feeder in the inner housing with an external test analyzer, first throughholes 11 should be formed in the inner housing and the outer housing, respectively, so that the automatic sample feeding tube can pass through the protection device. Similarly, when the cable of the auto-sampler needs to be connected to an external power source, the inner housing and the outer housing should be provided with the second throughholes 15, respectively.
Optionally, the outer shell and the inner shell in the embodiment are made of polypropylene materials, and optionally, the outer shell is a cuboid with the length of 600 mm-700 mm, the width of 600 mm-700 mm and the height of 1000mm, the inner shell is a cuboid with the length of 500 mm-600 mm, the width of 500 mm-600 mm and the height of 500 mm-600 mm, and the clean room with the size is also a cuboid with the protection device capable of easily controlling the gas flow direction and free of ambient atmosphere pollution. The polypropylene material is clean and has excellent mechanical property, and the clean area is firm and the inside is not polluted. The thickness of the polypropylene plate used in the embodiment can be 20mm, and the polypropylene plastic welding technology is used for splicing adjacent plates, so that volatile metal ions brought by metal screws are prevented from polluting samples.
Example 2
The present embodiment provides a method for detecting metal impurities in a silicon wafer, please refer to fig. 3, which includes the following steps:
s1: and the silicon wafer sample preparation system is used for preparing a silicon wafer metal impurity detection sample.
S2: and opening an operation window of the silicon wafer sample preparation system, taking the prepared silicon wafer metal impurity detection sample out of the silicon wafer sample preparation system through the operation window, and capping a sample bottle containing the silicon wafer metal impurity detection sample.
After the silicon wafer metal impurity detection sample is prepared in the silicon wafer sample preparation system, the operation window of the silicon wafer sample preparation system can be opened within 5 minutes, the sample plate loaded with a plurality of recovery liquid sample bottles is covered with covers, and the operation window of the silicon wafer sample preparation system is closed within 5 seconds.
S3: and opening a clean air flow circulating system in the monocrystalline silicon metal impurity detection sample protection device.
The protective device for the monocrystalline silicon metal impurity detection sample in this step may be any one of the protective devices in the above embodiments.
S4: the capped sample bottles are transported to the vicinity of the protective device.
For example, the sample vial may be brought within 30mm of the guard by moving the cart. Specifically, the moving cart should be first pushed to within 30mm from the operating area of the silicon wafer sampling system, the operating window of the silicon wafer sampling system should be opened, the sample tray covered with the cover should be moved to the cart within 5 seconds, and the operating window of the silicon wafer sampling system should be closed, and then the moving cart should be moved to the vicinity of the protection device.
S5: the shielding piece for shielding the operation port is taken down when the working time of the clean air flow circulating system reaches a preset time threshold value, the capped sample bottle is placed on the automatic sample injector, and the shielding piece is used for shielding the operation port after the cover covered on the sample bottle is opened.
The preset time threshold in this embodiment can be flexibly set, for example, can be set to 5 minutes.
S6; the automatic sample injector sends the monocrystalline silicon metal impurity detection sample into a test analyzer through an automatic sample injection pipe for test analysis, and a detection result is obtained.
Example 3
To verify the effectiveness of the protocol provided in this example, the following example tests a sample of metal impurities from a single crystal silicon wafer.
This example tests 1 sample of single crystal silicon wafers 200mm in diameter for metal impurities. And (3) preparing samples by using a silicon wafer sample preparation system, wherein the interior of the silicon wafer sample preparation system is kept independent of the outside in the sample preparation process. The sample was taken using 500ul VPD and the final sample size was 500 ul. The outer housing dimensions of the protective device used were 600MM 1000MM, the inner housing dimensions 500MM long, 500MM wide and 500MM high. The FFU with the filter screen made of polytetrafluoroethylene is carried, and the effective air outlet area is 900mm2. An autosampler online with ICP-MS was placed directly below the center of the FFU. And 5 minutes after the sampling of the silicon wafer sample preparation system is finished, opening an operation window of the silicon wafer sample preparation system, covering a cover on a sample tray loaded with the sample bottle, and closing the operation window of the silicon wafer sample preparation system. And opening the FFU of the purification room to keep the air speed at 2m/s, opening the exhaust fan, adjusting the air speed to 8m/s, and purging for 5 minutes. And (3) moving the sample tray to a position 10mm away from the clean room by using the chemical trolley, lifting the polyethylene shield, putting the sample tray on an automatic sample injector in the clean room from the chemical trolley, and opening the cover.
ICP-MS was started for measurement. The content of all impurity elements of the sample is detected to be below E8Atoms/cm 2. The detection limit is below E7Atoms/cm 2. In the detection process, the detection result is not influenced by the walking operation of personnel indoors and the like. Meanwhile, the phenomenon of signal fluctuation is not found in the detection process, and the stability and the accuracy of detection are greatly improved.
Example 4
This example tests 10 samples of single crystal silicon wafers 200mm in diameter for metal impurities. Preparing samples by using a silicon wafer sample preparation system, and keeping the silicon wafer preparation in the sample preparation processThe interior of the sample system is independent of the outside. The sample was taken using 800ul VPD and the final sample size was 800 ul. The size of the outer shell using the protection device is 700MM 1000MM, and the size of the inner shell is 600MM in length, 600MM in width and 600MM in height. The carrying filter screen is an FFU made of polytetrafluoroethylene material, and the effective air outlet area of the FFU is 1000mm2. An autosampler online with ICP-MS was placed directly below the center of the FFU. And opening an operation window of the silicon wafer sample preparation system 1 minute after the silicon wafer sample preparation system finishes sampling, and covering a sample tray loaded with the sample bottle with a cover. And opening the FFU of the purification room to keep the air speed at 2m/s, opening the exhaust fan, adjusting the air speed to 8m/s, and purging for 6 minutes. And (3) moving the sample tray to a position 20mm away from the clean room by using the chemical trolley, lifting the polyethylene shield, putting the sample tray on an automatic sample injector in the clean room from the chemical trolley, and opening the cover.
ICP-MS was started for measurement. The content of all impurity elements of the sample is detected to be below E8Atoms/cm 2. The detection limit is below E7Atoms/cm 2. In the detection process, the detection result is not influenced by the walking operation of personnel indoors and the like. Meanwhile, the phenomenon of signal fluctuation is not found in the detection process, and the stability and the accuracy of detection are greatly improved.
Example 5
50 samples of single crystal silicon wafers 200mm in diameter were tested for metal impurities. And (3) preparing samples by using a silicon wafer sample preparation system, wherein the interior of the silicon wafer sample preparation system is kept independent of the outside in the sample preparation process. The sample was taken using 200ul VPD and the final sample size was 1000 ul. The outer housing dimensions of the protective device used were 600MM 1000MM, the inner housing dimensions were 550MM long, 550MM wide and 550MM high. The FFU with the filter screen made of polytetrafluoroethylene is carried, and the effective air outlet area is 900mm2. An autosampler online with ICP-MS was placed directly below the center of the FFU. And after the sampling of the silicon wafer sample preparation system is finished, opening an operation window of the silicon wafer sample preparation system, and covering a sample tray loaded with the sample bottle with a cover. And opening the FFU of the purification room to keep the air speed at 3m/s, opening the exhaust fan, adjusting the air speed to 10m/s, and purging for 8 minutes. Moving the sample tray to a position 10mm away from the purification room by using the chemical cart, opening the polyethylene shield, and placing the sample tray into the automatic sample introduction chamber from the chemical cartThe container is closed and the lid is opened.
ICP-MS was started for measurement. The content of all impurity elements of the sample is detected to be below E8Atoms/cm 2. The detection limit is below E7Atoms/cm 2. In the detection process, the detection result is not influenced by the walking operation of personnel indoors and the like. Meanwhile, the phenomenon of signal fluctuation is not found in the detection process, and the stability and the accuracy of detection are greatly improved.
Example 6
10 samples of single crystal silicon wafers 300mm in diameter were tested for metal impurities. And (3) preparing samples by using a silicon wafer sample preparation system, wherein the interior of the silicon wafer sample preparation system is kept independent of the outside in the sample preparation process. The sample was taken using 200ul VPD and the final sample size was 1000 ul. The outer housing dimensions of the protective device used were 600MM 1000MM, the inner housing dimensions 500MM long, 500MM wide and 500MM high. The carrying filter screen is an FFU made of polytetrafluoroethylene material, and the effective air outlet area of the FFU is 1200mm2. An autosampler online with ICP-MS was placed directly below the center of the FFU. And 3 minutes after the sampling of the silicon wafer sample preparation system is finished, opening an operation window of the silicon wafer sample preparation system, and covering a sample tray loaded with the sample bottle with a cover. And opening the FFU of the purification room to keep the air speed at 4m/s, opening the exhaust fan, adjusting the air speed to 12m/s, and purging for 10 minutes. And (3) moving the sample tray to a position 30mm away from the clean room by using the chemical trolley, lifting the polyethylene shield, putting the sample tray on an automatic sample injector in the clean room from the chemical trolley, and opening the cover.
ICP-MS was started for measurement. The content of all impurity elements of the sample is detected to be below E7Atoms/cm 2. The detection limit is below E6Atoms/cm 2. In the detection process, the detection result is not influenced by the walking operation of personnel indoors and the like. Meanwhile, the phenomenon of signal fluctuation is not found in the detection process, and the stability and the accuracy of detection are greatly improved.
Example 7
10 samples of single crystal silicon wafers 300mm in diameter were tested for metal impurities. And (3) preparing samples by using a silicon wafer sample preparation system, wherein the interior of the silicon wafer sample preparation system is kept independent of the outside in the sample preparation process. The sample was taken using 200ul VPD and the final sample size was 1000 ul. The size of the outer shell using the protection device is 800MM 1000mm, the size of the inner shell is 700mm in length, 700mm in width and 500mm in height. The carrying filter screen is an FFU made of polytetrafluoroethylene material, and the effective air outlet area of the FFU is 1200mm2. An autosampler online with ICP-MS was placed directly below the center of the FFU. And opening an operation window of the silicon wafer sample preparation system 10 minutes after the sampling of the silicon wafer sample preparation system is finished, and covering a sample tray loaded with the sample bottle with a cover. And opening the FFU of the purification room to keep the air speed at 4m/s, opening the exhaust fan, adjusting the air speed to 12m/s, and purging for 3 minutes. And (3) moving the sample tray to a position 40mm away from the clean room by using the chemical trolley, lifting the polyethylene shield, putting the sample tray on an automatic sample injector in the clean room from the chemical trolley, and opening the cover.
ICP-MS was started for measurement. Through detection, the content of all impurity elements of the sample is above E8Atoms/cm 2. The detection limit is above E8Atoms/cm 2. Meanwhile, the phenomenon of signal fluctuation exists in the detection process.
Therefore, preferably, the outer shell is a cuboid with the length of 600 mm-700 mm, the width of 600 mm-700 mm and the height of 1000mm, and the inner shell is a cuboid with the length of 500 mm-600 mm, the width of 500 mm-600 mm and the height of 500 mm-600 mm.
While the present invention has been described with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, which are illustrative and not restrictive, and it will be apparent to those skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (10)

Translated fromChinese
1.一种硅片金属杂质检测样品保护装置,其特征在于,包括具有容纳腔的保护壳体、用于盛放硅片金属杂质检测样品的自动进样器、自动进样管、遮挡片以及洁净气流循环系统;1. a silicon wafer metal impurity detection sample protection device, is characterized in that, comprises the protective casing with accommodating cavity, the automatic sample injector that is used to hold the silicon wafer metal impurity detection sample, automatic sampling tube, shielding sheet and Clean air circulation system;所述保护壳体外表面上形成有与所述容纳腔贯通的操作口以及与所述自动进样管的外径相匹配的第一通孔,所述操作口的面积小于所述遮挡片的面积,所述洁净气流循环系统包括设置在所述保护壳体上的风机过滤机组以及排风机;The outer surface of the protective shell is formed with an operation port passing through the accommodating cavity and a first through hole matching the outer diameter of the automatic sampling tube, and the area of the operation port is smaller than the area of the shielding sheet , the clean air circulation system includes a fan filter unit and an exhaust fan arranged on the protective casing;在保护使用状态,所述自动进样器位于所述保护壳体的容纳腔中,与所述自动进样器连接的自动进样管穿过所述第一通孔与外部的测试分析仪连接,所述遮挡片设置于所述保护壳体上并将所述操作口遮挡,所述风机过滤机组将洁净气流输入所述容纳腔,所述排风机将所述保护壳体内的洁净气流排出。In a protected use state, the autosampler is located in the accommodating cavity of the protective casing, and the autosampler connected to the autosampler is connected to an external test analyzer through the first through hole The shielding sheet is arranged on the protective casing and shields the operation port, the fan filter unit inputs the clean air flow into the accommodating cavity, and the exhaust fan discharges the clean air flow in the protective casing.2.如权利要求1所述的硅片金属杂质检测样品保护装置,其特征在于,所述风机过滤机组中设置有由聚四氟乙烯材料制成的过滤网。2 . The sample protection device for detecting metal impurities in silicon wafers according to claim 1 , wherein the fan filter unit is provided with a filter screen made of polytetrafluoroethylene material. 3 .3.如权利要求1所述的硅片金属杂质检测样品保护装置,其特征在于,所述风机过滤机组的出风口面积为900cm2~1200cm23 . The sample protection device for detecting metal impurities in silicon wafers according to claim 1 , wherein the area of the air outlet of the fan filter unit is 900 cm2 to 1200 cm2 . 4 .4.如权利要求1所述的硅片金属杂质检测样品保护装置,其特征在于,所述自动进样器具有电缆,所述保护壳体上还形成有与所述电缆的外径相匹配的第二通孔,在保护使用状态,所述电缆穿过所述第二通孔与外部电源连接。4 . The sample protection device for detecting metal impurities in silicon wafers according to claim 1 , wherein the automatic sampler has a cable, and the protection shell is further formed with a matching outer diameter of the cable. 5 . The second through hole, in the protected use state, the cable passes through the second through hole and is connected to an external power source.5.如权利要求1所述的硅片金属杂质检测样品保护装置,其特征在于,所述遮挡片为聚乙烯膜片。5 . The sample protection device for detecting metal impurities in silicon wafers according to claim 1 , wherein the shielding sheet is a polyethylene film sheet. 6 .6.如权利要求1-5任一项所述的硅片金属杂质检测样品保护装置,其特征在于,所述保护壳体包括外壳体和设置在所述外壳体内的内壳体,所述容纳腔由所述内壳体围设而成,所述内壳体的底层为冲孔板,用于承载所述自动进样器,所述排风机与所述外壳体和所述内壳体围设出的隔层空间连接,以排出所述隔层空间中的洁净气流。6 . The sample protection device for silicon wafer metal impurity detection according to claim 1 , wherein the protective casing comprises an outer casing and an inner casing disposed in the outer casing, and the accommodating The cavity is surrounded by the inner shell, the bottom layer of the inner shell is a punching plate, which is used to carry the automatic sampler, and the exhaust fan is surrounded by the outer shell and the inner shell. The provided interlayer space is connected to discharge the clean air flow in the interlayer space.7.如权利要求6所述的硅片金属杂质检测样品保护装置,其特征在于,所述风机过滤机组和所述排风机设置于所述外壳体的顶层上,所述外壳体和所述内壳体由聚丙烯材料制成。7 . The sample protection device for detecting metal impurities in silicon wafers according to claim 6 , wherein the fan filter unit and the exhaust fan are arranged on the top layer of the outer casing, and the outer casing and the inner The housing is made of polypropylene material.8.如权利要求8所述的硅片金属杂质检测样品保护装置,其特征在于,所述外壳体是长为600 mm~700mm,宽为600 mm~700mm,高为1000mm的长方体,所述内壳体是长为500 mm~600mm,宽为500 mm~600mm,高为500 mm~600mm的长方体,所述长方体的相邻面通过聚丙烯塑料焊接技术相拼接。8 . The sample protection device for detecting metal impurities in silicon wafers according to claim 8 , wherein the outer casing is a rectangular parallelepiped with a length of 600 mm to 700 mm, a width of 600 mm to 700 mm and a height of 1000 mm. The shell is a rectangular parallelepiped with a length of 500 mm to 600 mm, a width of 500 mm to 600 mm and a height of 500 mm to 600 mm, and the adjacent faces of the rectangular parallelepiped are joined together by polypropylene plastic welding technology.9.一种硅片金属杂质检测方法,其特征在于,包括以下步骤:9. A silicon wafer metal impurity detection method, characterized in that, comprising the following steps:S1:硅片制样系统制作硅片金属杂质检测样品;S1: The silicon wafer sample preparation system prepares the silicon wafer metal impurity detection sample;S2:打开所述硅片制样系统的操作窗,通过所述操作窗从所述硅片制样系统中取出制备完成的硅片金属杂质检测样品,并对盛放所述硅片金属杂质检测样品的样品瓶加盖;S2: Open the operation window of the silicon wafer sample preparation system, take out the prepared silicon wafer metal impurity detection sample from the silicon wafer sample preparation system through the operation window, and detect the metal impurities in the silicon wafer The sample vial is capped;S3:打开如权利要求1-9中任一项所述的单晶硅金属杂质检测样品保护装置中的洁净气流循环系统;S3: open the clean air circulation system in the sample protection device for detecting single crystal silicon metal impurities as described in any one of claims 1-9;S4:将已加盖的所述样品瓶运送至所述保护装置附近;S4: transport the capped sample bottle to the vicinity of the protection device;S5:在所述洁净气流循环系统的工作时长达到预设时长阈值时取下遮挡所述操作口的遮挡片,并将已加盖的所述样品瓶放在所述自动进样器上,并在打开盖于所述样品瓶上的盖子后,使用所述遮挡片遮挡所述操作口;S5: when the working duration of the clean air circulation system reaches a preset duration threshold, remove the shielding sheet that shields the operation port, and place the capped sample bottle on the automatic sampler, and After opening the cap on the sample bottle, use the shielding sheet to cover the operation port;S6;所述自动进样器通过所述自动进样管将所述单晶硅金属杂质检测样品送入所述测试分析仪进行测试分析,得到检测结果。S6; the automatic sampler sends the single crystal silicon metal impurity detection sample into the testing analyzer for testing and analysis through the automatic sampling tube to obtain a testing result.10.如权利要求8所述的硅片金属杂质检测样品保护装置,其特征在于,所述内壳体内洁净气体在所述洁净气流循环系统的工作时长达到预设时长阈值时能达到如下参数:湿度小于45%,0.1um颗粒<=1ea/m3,气体中锂钠镁铝钾钙钛钒铬锰铁钴镍铜锌钼钨含量各小于1ng/L,铵根氯氟溴亚硝酸根硝酸根硫酸根磷酸根各离子含量小于1ng/L。10 . The protection device for silicon wafer metal impurity detection samples according to claim 8 , wherein the clean gas in the inner casing can reach the following parameters when the operating duration of the clean airflow circulation system reaches a preset duration threshold: 10 . The humidity is less than 45%, 0.1um particles are less than 1ea/m3, the content of lithium sodium magnesium aluminum potassium calcium titanium vanadium chromium manganese iron cobalt nickel copper zinc molybdenum tungsten in the gas is less than 1ng/L, ammonium chloride, fluorine, bromine, nitrite, nitrate The content of each ion of sulfate phosphate is less than 1ng/L.
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