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.
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.