CN106290117B - Device and method for testing radiation induced gas permeation of material - Google Patents
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- 239000000463 material Substances 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 44
- 230000005855 radiation Effects 0.000 title claims abstract description 40
- 238000012360 testing method Methods 0.000 title claims abstract description 37
- 230000035699 permeability Effects 0.000 claims abstract description 24
- 238000000605 extraction Methods 0.000 claims abstract description 23
- 238000005086 pumping Methods 0.000 claims description 53
- 239000000725 suspension Substances 0.000 claims description 12
- 238000007789 sealing Methods 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 230000001105 regulatory effect Effects 0.000 claims description 8
- 238000001514 detection method Methods 0.000 claims description 7
- 238000012937 correction Methods 0.000 claims description 4
- 102100027198 Sodium channel protein type 5 subunit alpha Human genes 0.000 claims description 3
- 238000010998 test method Methods 0.000 claims description 3
- 238000005286 illumination Methods 0.000 claims description 2
- 239000007789 gas Substances 0.000 description 89
- 238000005259 measurement Methods 0.000 description 7
- 238000004949 mass spectrometry Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000001900 extreme ultraviolet lithography Methods 0.000 description 3
- 238000001459 lithography Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 238000009530 blood pressure measurement Methods 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/10—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing diffusion of components through a porous wall and measuring a pressure or volume difference
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Abstract
The invention discloses a device for testing radiation induced gas permeation of a material and a method for testing gas permeation rate, wherein the device comprises the following components: vacuum chamber system, radiation system, air extraction system, air feed system and detecting system, vacuum chamber system includes left cavity (1) and right cavity (2), radiation system includes light source (5) and lighting system, air extraction system includes three air extraction passageway, air feed system includes gas cylinder (16), relief pressure valve (17), stop valve (18) and flow controller (19) that connect in order, detecting system includes first vacuum gauge (20), second vacuum gauge (21) and mass spectrometer (22), and wherein first vacuum gauge (20), second vacuum gauge (21) are used for testing the pressure of left cavity and right cavity respectively, and mass spectrometer (22) are used for measuring the gas component and the partial pressure of right cavity. The device has simple structure and can accurately and truly measure the gas permeability of the material under radiation on line in real time.
Description
Technical Field
The invention relates to the technical field of radiation induced gas permeation measurement of materials, in particular to a device and a method for testing gas permeation caused by optical radiation films, metals and nonmetal sheets.
Background
Extreme ultraviolet lithography (EUVL) technology is one of the most promising lithography technologies for lithography nodes of 10nm and below. Since air and most materials have a strong absorption of EUV light at 13.5nm, the EUV beam needs to be placed in vacuum. Under such vacuum conditions, some gases may cause catastrophic failure of the mirror, such as water vapor (H) 2 O) causes oxidation thereof, and hydrocarbon (CxHy) causes deposition of a carbon layer on the surface thereof, so that the content of the contaminating gas in the vacuum needs to be controlled. EUV lithography machine having a large number of photoelectrodes insideThe components must be enclosed with a sealed housing to prevent the release of contaminating gases directly into the main chamber of the lithographic apparatus. Under direct or indirect irradiation of EUV light, the gas permeability of some encapsulation materials may also change, so it is necessary to study the radiation induced gas permeability change of the material.
At present, the research on the barrier property of the gas permeability of packaging materials such as foods, medicines, electronic products and the like is mainly focused at home and abroad, and a plurality of methods are adopted, such as a weighing method, a sensor method, a calcium reaction method, a radioactive tracing method, a helium mass spectrometry leak detection method and a mass spectrometry, wherein the measurement sensitivity of the first five methods is not high, and the measurement of the gas types is limited. Mass spectrometry has been increasingly used in recent years due to its high sensitivity, rapid measurement speed and unlimited types of test gases, see US patent 4944180a, chinese patent ZL 200810045129.9 and ZL201310026422.1. But convenient and fast mass spectrometer calibration and accurate partial pressure measurement have been one difficulty in mass spectrometry.
The technical problems to be solved are as follows:
(1) The mass spectrometer and the effective pumping speed of the system are calibrated in a convenient mode;
(2) Accurately and truly measuring the gas permeability of the material on line in real time;
(3) The gas permeability of the material under optical radiation is accurately and truly measured in real time on line.
Disclosure of Invention
The invention proposes a device for testing the radiogas permeation of a material, comprising: a vacuum chamber system, a radiation system, an air extraction system, an air supply system and a detection system.
Preferably, the vacuum chamber system comprises a left chamber 1 and a right chamber 2, wherein the left chamber 1 and the right chamber 2 are cylinders with the same size and are connected into a whole through knife edge flanges, a material to be measured is placed between the knife edge flanges, and a supporting grid is welded on the right chamber 2 and used for supporting the material to be measured; when the left chamber 1 and the right chamber 2 are integrated, the ultimate vacuum is 1×10 - 7 Pa。
Preferably, the radiation system comprises a light source 5 and an illumination system for generating a uniform beam of radiation onto the surface of the material 3 to be measured.
Preferably, the air extraction system comprises three air extraction channels, wherein the main pump of the first air extraction channel is a 300L/s magnetic suspension molecular pump 8 and is used for vacuumizing a left cavity; the second air extraction channel adopts a magnetic suspension molecular pump group 9 formed by connecting two stages of molecular pumps in series to vacuumize the right cavity, and the pumping speed is 600L/s and 300L/s respectively; the first air extraction channel and the second air extraction channel share the first dry mechanical pump 7 as a backing pump; the third air extraction channel adopts a second dry mechanical pump to vacuumize the gap between the metal sealing ring 24 and the rubber sealing ring 23.
Preferably, the gas supply system comprises a gas cylinder 16, a pressure reducing valve 17, a shut-off valve 18 and a flow controller 19 connected in sequence for directly charging the vacuum chamber with gas or a gas of adjustable and known flow, wherein the flow controller 19 is precisely calibrated.
Preferably, the detection system comprises a first vacuum gauge 20, a second vacuum gauge 21 and a mass spectrometer 22, wherein the first vacuum gauge 20 and the second vacuum gauge 21 are used for testing the pressure of the left chamber and the right chamber respectively, the second vacuum gauge 21 is precisely calibrated, and the mass spectrometer 22 is used for measuring the gas component and the partial pressure of the right chamber.
A method of testing the radiation induced gas permeation of a material using a device for testing the radiation induced gas permeation of a material, for testing the gas permeation rate of a material, comprising the steps of:
step S1: placing a material sample 3 to be tested, connecting the left chamber 1 and the right chamber 2 into a whole, and respectively pumping the left chamber 1 and the right chamber 2 to limit vacuum through a first pumping channel and a second pumping channel; step S2: measuring the gas pressure of the right chamber 2 with a second vacuum gauge 21; step S3: the flow controller 19 of the air supply system is regulated to charge high-purity air i into the left chamber 1 so as to achieve dynamic balance under a certain pressure; step S4: the partial pressure increase deltap of gas i in the right chamber 2 is recorded with a mass spectrometer 22 i The method comprises the steps of carrying out a first treatment on the surface of the Permeability K of the material to gas i at this pressure i (g·m -2 ·day -1 ) The method comprises the following steps:
wherein S is ei For effective pumping speed, unit m 3 /s；M i Is the molar mass of the gas i, in g/mol; a is the area of the sample, unit m 2 The method comprises the steps of carrying out a first treatment on the surface of the R is a gas constant, unit Pa.m 3 ·K -1 ·mol -1 The method comprises the steps of carrying out a first treatment on the surface of the T is the temperature, unit K;
wherein the effective pumping speed S ei Obtained by:
step SS1: the left chamber 1 and the right chamber 2 are connected into a whole without placing materials to be tested, and the system is pumped to the limit vacuum through the first pumping channel and the second pumping channel; step SS2: closing the first pumping channel and regulating the flow controller 19 to introduce a known flow Q into the vacuum chamber system i 99.99% high purity gas i; step SS3: after dynamic equilibrium is reached, the pressure P of the right chamber 2 is measured using a mass spectrometer 22 i . The effective pumping speed of the second pumping channel to the gas i is S ei ＝Q i /P i 。
Wherein, for accurately testing the partial pressure P of the gas i in the vacuum chamber i Calibration of mass spectrometer 22 is required:
step SSS1: the left chamber 1 and the right chamber 2 are connected into a whole without placing materials to be tested, and the system is pumped to the limit vacuum through the first pumping channel and the second pumping channel; step SSS2: closing the first air suction channel, and introducing 99.99% high-purity gas i into the vacuum chamber system to form dynamic balance; step SSS3: when more than 95% of the chamber is gas i, the total pressure P measured by the second vacuum gauge 21 is recorded ion And mass spectrometer 22 measures partial pressure P of gas i i . The mass spectrometer 22 tests the correction factor c=p of the partial pressure of gas i ion /P i 。
A method of testing the radiation induced gas permeation of a material using a device for testing the radiation induced gas permeation of a material, for testing the radiation induced gas permeation rate of a material, comprising the steps of:
step S1: placing a sample 3 of the material to be tested, and connecting the left chamber 1 and the right chamber 2The left chamber 1 and the right chamber 2 are pumped to the limit vacuum through the first pumping channel and the second pumping channel respectively; step S2: measuring the gas pressure of the right chamber 2 with a second vacuum gauge 21; step S3: the flow controller 19 of the air supply system is regulated to charge high-purity air i into the left chamber 1 so as to achieve dynamic balance under a certain pressure; step S4: the partial pressure increase deltap of gas i in the right chamber 2 is recorded with a mass spectrometer 22 i The method comprises the steps of carrying out a first treatment on the surface of the Permeability K of the material to gas i at this pressure i (g·m -2 ·day -1 ) The method comprises the following steps:
step S5: after the gas permeation reaches a stable state, the light source 5 is turned on to radiate the sample 3 to be tested, and the partial pressure increment delta P of the gas i in the right chamber 2 is recorded i ' permeability change ΔK of material when irradiated under the pressure gas i (g·m -2 ·day -1 ) The method comprises the following steps:
permeability K of the material when irradiated under the pressure gas i ’(g·m -2 ·day -1 ) The method comprises the following steps:
wherein S is ei For effective pumping speed, unit m 3 /s；M i Is the molar mass of the gas i, in g/mol; a is the area of the sample, unit m 2 The method comprises the steps of carrying out a first treatment on the surface of the R is a gas constant, unit Pa.m 3 ·K -1 ·mol -1 The method comprises the steps of carrying out a first treatment on the surface of the T is the temperature, unit K;
wherein the effective pumping speed S ei Obtained by:
step SS1: the left chamber 1 and the right chamber 2 are connected into a whole without the material to be tested, and the material to be tested passes through the first air extraction channel and the second air extraction channelPumping the system to a limit vacuum; step SS2: closing the first pumping channel and regulating the flow controller 19 to introduce a known flow Q into the vacuum chamber system i 99.99% high purity gas i; step SS3: after dynamic equilibrium is reached, the pressure P of the right chamber 2 is measured using a mass spectrometer 22 i . The effective pumping speed of the second pumping channel to the gas i is S ei ＝Q i /P i 。
Wherein, for accurately testing the partial pressure P of the gas i in the vacuum chamber i Calibration of mass spectrometer 22 is required:
step SSS1: the left chamber 1 and the right chamber 2 are connected into a whole without placing materials to be tested, and the system is pumped to the limit vacuum through the first pumping channel and the second pumping channel; step SSS2: closing the first air suction channel, and introducing 99.99% high-purity gas i into the vacuum chamber system to form dynamic balance; step SSS3: when more than 95% of the chamber is gas i, the total pressure P measured by the second vacuum gauge 21 is recorded ion And mass spectrometer 22 measures partial pressure P of gas i i . The mass spectrometer 22 tests the correction factor c=p of the partial pressure of gas i ion /P i 。
The device only comprises a set of vacuum chamber system consisting of a left chamber and a right chamber, and has a simple structure; the device is provided with the air supply channel with known and adjustable flow, can calibrate the effective pumping speed and the mass spectrometer of the system, and ensures the accuracy of the test result; the right chamber of the device is partitioned by a gate valve with a current-limiting small hole, so that the measurement sensitivity of the radiation permeability is improved; the device increases the radiation system and can test the permeability of the material radiation induced gas. The invention also provides a method for testing the gas permeability of the material and the gas permeability caused by the radiation of the material respectively by combining the device, and the measurement result is accurate and reliable and can be tested on line.
Drawings
FIG. 1 is an apparatus for testing the radiation induced gas permeation of materials.
Fig. 2 shows flange sealing structures of left and right vacuum chambers in an apparatus for testing material radiation induced gas permeation.
The device comprises a left chamber, a right chamber, a 3-material to be tested, a 4-supporting grid, a 5-light source, a 6-light beam, a 7-first dry mechanical pump, an 8-magnetic suspension molecular pump, a 9-magnetic suspension molecular pump set, a 10-three-way valve, an 11-angle valve, a 12-angle valve, a 13-gate valve, a 14-gate valve with a flow-limiting small hole, a flow-limiting small hole on a 15-gate valve, a 16-gas cylinder, a 17-pressure-reducing valve, a 18-stop valve, a 19-flow controller, a 20-first vacuum gauge, a 21-second vacuum gauge, a 22-mass spectrometer, a 23-rubber seal ring, a 24-metal seal ring, a 25-third air suction channel and a 26-flange bolt.
Detailed Description
The invention is described in detail below with reference to the attached drawings and examples:
as shown in fig. 1 and 2, the apparatus for testing the radiation induced gas permeation of a material of the present invention includes a vacuum chamber system, a radiation system, a pumping system, a gas supply system, and a detection system.
The vacuum chamber system comprises a left chamber 1, a right chamber 2, a material to be tested 3, a support grid 4, a rubber sealing ring 23, a metal sealing ring 24, a third air suction channel 25 and flange bolts 26. The material 3 to be measured is arranged between the flanges of the left chamber and the right chamber, the flanges are sealed by adopting rubber rings 23, the left chamber and the right chamber are sealed by adopting oxygen-free copper metal rings 24, and a gap between the two seals is vacuumized by adopting a channel 25. The outer wall of the vacuum chamber system is uniformly wrapped with a baking heating belt, so that the vacuum chamber system can be baked, and the highest temperature can reach 200 ℃. When the material 3 to be measured is not put in, the left chamber 1 and the right chamber 2 can be connected into a vacuum chamber through metal sealing, and the ultimate vacuum can reach 1 multiplied by 10 -7 Pa. After the material to be measured 3 is placed, the left chamber 1 and the right chamber 2 can be separated. The material 3 to be measured may be a film, a metal or a non-metal sheet.
The radiation system is used for carrying out optical radiation on the material 3 to be tested in the vacuum chamber, and comprises a light source 5 and a light beam 6. Typical sources of radiation are EUV light, excimer laser and CO 2 Laser light, etc., also includes light sources of the remaining wavelengths.
The pumping system comprises: the first dry mechanical pump 7, the magnetic suspension molecular pump 8, the magnetic suspension molecular pump group 9, the three-way valve 10, the angle valve 11, the angle valve 12, the gate valve 13, the gate valve 14 with the flow-limiting small hole, the flow-limiting small hole 15 and the third air extraction channel 25 form three air extraction channels. The first air extraction channel consists of a first dry mechanical pump 7, a magnetic suspension molecular pump 8, a three-way valve 10, an angle valve 11 and a gate valve 13, and is used for vacuumizing the left chamber 1, and the typical pumping speed of the magnetic suspension molecular pump 8 is 300L/s. The second air extraction channel consists of a first dry mechanical pump 7, a magnetic suspension molecular pump group 9, a three-way valve 10, an angle valve 12, a gate valve 14 with a flow-limiting small hole and a flow-limiting small hole 15, wherein the magnetic suspension molecular pump group 9 consists of two stages of molecular pumps which are connected in series, and typical pumping speeds are 600L/s and 300L/s respectively. The right cavity 2 can be vacuumized by opening the gate valve 14, and the right cavity 2 can be vacuumized by closing the gate valve 14 through the flow limiting small hole 15, wherein the diameter of the flow limiting small hole can be 5-50 mm. The third pumping channel 25 uses a second dry mechanical pump to pump vacuum to the gap between the two sealing rings of fig. 2.
The air supply system comprises two air supply channels consisting of an air bottle 16, a pressure reducing valve 17, a stop valve 18 and a flow controller 19, and can supply air directly through the stop valve 18 or through the flow controller 19. Wherein the flow control range of the flow controller 19 is 1×10 -2 ～1×10 -5 Pa·m 3 S, and is precisely calibrated for filling the vacuum chamber with a gas of adjustable and known flow rate.
The detection system comprises a first vacuum gauge 20, a second vacuum gauge 21 and a mass spectrometer 22. The first vacuum gauge 20 is a composite gauge, and has a measuring range of 1.2X10 5 Pa～1×10 -8 Pa for measuring the pressure of the left chamber 1. The second vacuum gauge 21 is a cold cathode ion gauge, and has a measurement range of 1×10 -2 Pa～1×10 -8 Pa for measuring the pressure of the right chamber 2, and is precisely calibrated. The mass spectrometer 22 is used for measuring the gas composition and partial pressure of the right chamber 2, and the lower limit of partial pressure measurement is 1×10 -10 Pa。
By adopting the device for testing the radiation induced gas permeation of the material, the invention firstly provides a method for conveniently calibrating a mass spectrometer. Step S1: the left chamber 1 and the right chamber 2 are connected into a whole without placing materials to be tested, and the system is pumped to the limit vacuum through the first pumping channel and the second pumping channel; step S2: closing the first air suction channel, and introducing 99.99% high-purity gas i (such as He gas) into the vacuum chamber system to form a dynamic flatBalance (2); step S3: when 95% or more of the gas i in the chamber is present (partial pressure ratio P measured by the mass spectrometer 22) 18 /P i < 0.05), the total pressure P measured by the second vacuum gauge 21 is recorded ion And mass spectrometer 22 measures partial pressure P of gas i i . The mass spectrometer 22 tests the correction factor c=p of the partial pressure of gas i ion /P i 。
By adopting the device for testing the radiation induced gas permeation of the material, the invention also provides a method for conveniently calibrating the effective pumping speed of the system. Step S1: the left chamber 1 and the right chamber 2 are connected into a whole without placing materials to be tested, and the system is pumped to the limit vacuum through the first pumping channel and the second pumping channel; step S2: closing the first pumping channel and regulating the flow controller 19 to introduce a known flow Q into the vacuum chamber system i 99.99% of high purity gas i (e.g., he gas); step S3: after dynamic equilibrium is reached, the pressure P of the right chamber 2 is measured using a mass spectrometer 22 i . The effective pumping speed of the second pumping channel to the gas i is S ei ＝Q i /P i 。
The invention also provides a method for testing the permeability of the material under different pressure gases by adopting the device for testing the radiation induced gas permeation of the material. Step S1: placing a material sample 3 to be tested, connecting the left chamber 1 and the right chamber 2 into a whole, and respectively pumping the left chamber 1 and the right chamber 2 to limit vacuum through a first pumping channel and a second pumping channel; step S2: measuring the gas pressure of the right chamber 2 by using a vacuum gauge 21; step S3: the flow controller 19 of the air supply system is regulated to charge high-purity air i into the left chamber 1 so as to achieve dynamic balance under a certain pressure; step S4: the partial pressure increase deltap of gas i in the right chamber 2 is recorded with a mass spectrometer 22 i . Permeability K of the material to gas i at that pressure i (g·m -2 ·day -1 ) The method comprises the following steps:
wherein M is i Is the molar mass of the gas i, in g/mol; a is the area of the sample, unit m 2 The method comprises the steps of carrying out a first treatment on the surface of the R is a gas constant, unit Pa.m 3 ·K -1 ·mol -1 The method comprises the steps of carrying out a first treatment on the surface of the T is the temperature in K.
With the device for testing the radiation induced gas permeation of the material, the invention also provides a method for testing the radiation induced gas permeation rate of the material. The steps S1-S4 are the same as above on the basis of the step of testing the permeability of the material under different pressure gases. Step S5: after the gas permeation reaches a stable state, the light source 5 is turned on to radiate the sample 3 to be tested, and the partial pressure increment delta P of the gas i in the right chamber 2 is recorded i '. Similarly, the permeability change ΔK of a material when irradiated under the pressure gas i (g·m -2 ·day -1 ) The method comprises the following steps:
permeability K of the material when irradiated under the pressure gas i ’(g·m -2 ·day -1 ) The method comprises the following steps:
wherein M is i Is the molar mass of the gas i, in g/mol; a is the area of the sample, unit m 2 The method comprises the steps of carrying out a first treatment on the surface of the R is a gas constant, unit Pa.m 3 ·K -1 ·mol -1 The method comprises the steps of carrying out a first treatment on the surface of the T is the temperature in K.
The above specific embodiments are used for further detailed description of the objects, technical solutions and advantageous effects of the present invention. It should be noted that the present invention is applicable to the field of space technology for testing the permeability change of a space material due to light irradiation, in addition to the radiation induced gas permeability of a test material in the field of semiconductor lithography.
The present invention is not limited to the above-mentioned embodiments, and any changes or substitutions that can be easily understood by those skilled in the art within the technical scope of the present invention are intended to be included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (3)
1. A test method based on a device for testing the radiation-induced gas permeation of a material, characterized in that the device for testing the radiation-induced gas permeation of a material comprises: the device comprises a vacuum chamber system, a radiation system, an air extraction system, an air supply system and a detection system; the vacuum chamber system comprises a left chamber (1) and a right chamber (2), wherein the left chamber (1) and the right chamber (2) are cylinders with the same size and are connected into a whole through knife edge flanges, a material to be detected is placed between the knife edge flanges, and a supporting grid is welded on the right chamber (2) and used for supporting the material to be detected; when the left chamber (1) and the right chamber (2) are integrated, the ultimate vacuum is 1 multiplied by 10 -7 Pa; the air extraction system comprises three air extraction channels, wherein a main air extraction pump of the first air extraction channel is a 300L/s magnetic suspension molecular pump (8) and is used for vacuumizing a left cavity; the second air extraction channel adopts a magnetic suspension molecular pump group (9) formed by connecting two stages of molecular pumps in series to vacuumize the right cavity, and the pumping speed is 600L/s and 300L/s respectively; the first air suction channel and the second air suction channel share a first dry mechanical pump (7) as a backing pump; the third air suction channel adopts a second dry mechanical pump to vacuumize a gap between the metal sealing ring (24) and the rubber sealing ring (23); the gas supply system comprises a gas cylinder (16), a pressure reducing valve (17), a stop valve (18) and a flow controller (19) which are connected in sequence, wherein the flow controller (19) is accurately calibrated; the detection system comprises a first vacuum gauge (20), a second vacuum gauge (21) and a mass spectrometer (22), wherein the first vacuum gauge (20) and the second vacuum gauge (21) are respectively used for testing the pressure of a left chamber and a right chamber, the second vacuum gauge (21) is accurately calibrated, and the mass spectrometer (22) is used for measuring the gas component and the partial pressure of the right chamber;
the method comprises the following steps:
step S1: placing a material (3) to be tested, connecting the left chamber (1) and the right chamber (2) into a whole, and respectively pumping the left chamber (1) and the right chamber (2) to limit vacuum through a first pumping channel and a second pumping channel; step S2: measuring right cavity with second vacuum gauge (21)The gas pressure of the chamber (2); step S3: a flow controller (19) of the air supply system is regulated to charge high-purity air i into the left cavity (1) so as to achieve dynamic balance under a certain pressure; step S4: recording the partial pressure delta P of the gas i in the right chamber (2) by using a mass spectrometer (22) i The method comprises the steps of carrying out a first treatment on the surface of the Permeability K of the material to gas i at this pressure i (g·m -2 ·day -1 ) The method comprises the following steps:
wherein S is ei For effective pumping speed, unit m 3 /s；M i Is the molar mass of the gas i, in g/mol; a is the area of the sample, unit m 2 The method comprises the steps of carrying out a first treatment on the surface of the R is a gas constant, unit Pa.m 3 ·K -1 ·mol -1 The method comprises the steps of carrying out a first treatment on the surface of the T is the temperature, unit K;
wherein the effective pumping speed S ei Obtained by:
step SS1: the method comprises the steps that a material to be tested is not placed in the system, a left chamber (1) and a right chamber (2) are connected into a whole, and the system is pumped to a limit vacuum through a first pumping channel and a second pumping channel; step SS2: closing the first pumping channel, regulating the flow controller (19) to introduce a known flow Q into the vacuum chamber system i 99.99% high purity gas i; step SS3: after dynamic balance is achieved, a mass spectrometer (22) is adopted to measure the pressure P of the right chamber (2) i The effective pumping speed of the second pumping channel to the gas i is S ei ＝Q i /P i ；
Wherein, for accurately testing the partial pressure P of the gas i in the vacuum chamber i The spectrometer (22) needs to be calibrated:
step SSS1: the method comprises the steps that a material to be tested is not placed in the system, a left chamber (1) and a right chamber (2) are connected into a whole, and the system is pumped to a limit vacuum through a first pumping channel and a second pumping channel; step SSS2: closing the first air suction channel, and introducing 99.99% high-purity gas i into the vacuum chamber system to form dynamic balance; step SSS3: when more than 95% of the chamber is gas i, the total pressure P measured by the second vacuum gauge (21) is recorded ion And a mass spectrometer (22) for measuring the partial pressure P of the gas i i Mass spectrumThe meter (22) measures a correction factor c=p of the partial pressure of the gas i ion /P i 。
2. A method according to claim 1, characterized in that the radiation system comprises a light source (5) and an illumination system for generating a uniform beam of radiation onto the surface of the material (3) to be measured.
3. The method according to any one of claims 1 to 2, characterized in that after said step S4, the method further comprises the steps of:
step S5: after the gas permeation is stabilized, a light source (5) is turned on to radiate the material (3) to be tested, and the partial pressure increment delta P of the gas i in the right chamber (2) is recorded i ' permeability change ΔK of material when irradiated under the pressure gas i (g·m -2 ·day -1 ) The method comprises the following steps:
permeability K of the material when irradiated under the pressure gas i ’(g·m -2 ·day -1 ) The method comprises the following steps:
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107219149A (en) * | 2017-07-07 | 2017-09-29 | 金华职业技术学院 | A kind of device for measuring carbon monoxide transmitance |
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| CN113466101B (en) * | 2021-06-24 | 2023-05-12 | 华中科技大学 | Permeability detection apparatus and detection method |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103115858A (en) * | 2013-01-24 | 2013-05-22 | 电子科技大学 | Measuring device and measuring method for measuring gas permeability of material |
| CN103616317A (en) * | 2013-12-16 | 2014-03-05 | 南京工业大学 | Full-automatic equipment and method for measuring helium diffusion coefficient of material for reactor |
| WO2015041115A1 (en) * | 2013-09-19 | 2015-03-26 | 独立行政法人産業技術総合研究所 | Gas permeability measuring device |
| CN105223126A (en) * | 2015-11-05 | 2016-01-06 | 中国科学院光电研究院 | A kind of polymkeric substance irradiation damage proving installation and method of testing |
| CN105300869A (en) * | 2015-12-10 | 2016-02-03 | 电子科技大学 | Device and method for measuring gas permeability of material by virtue of differential vacuum gauge |
| CN105547956A (en) * | 2015-12-10 | 2016-05-04 | 电子科技大学 | Device and method for measuring gas permeability of thin film by using vacuometer |
| CN105928855A (en) * | 2016-04-20 | 2016-09-07 | 中国原子能科学研究院 | Measuring apparatus and method for surface micropressure tritium absorption rate constant of material |
| CN206223611U (en) * | 2016-10-19 | 2017-06-06 | 中国科学院光电研究院 | A kind of material radiation causes the test device of gas infiltration |
-
2016
- 2016-10-19 CN CN201610911295.7A patent/CN106290117B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103115858A (en) * | 2013-01-24 | 2013-05-22 | 电子科技大学 | Measuring device and measuring method for measuring gas permeability of material |
| WO2015041115A1 (en) * | 2013-09-19 | 2015-03-26 | 独立行政法人産業技術総合研究所 | Gas permeability measuring device |
| CN103616317A (en) * | 2013-12-16 | 2014-03-05 | 南京工业大学 | Full-automatic equipment and method for measuring helium diffusion coefficient of material for reactor |
| CN105223126A (en) * | 2015-11-05 | 2016-01-06 | 中国科学院光电研究院 | A kind of polymkeric substance irradiation damage proving installation and method of testing |
| CN105300869A (en) * | 2015-12-10 | 2016-02-03 | 电子科技大学 | Device and method for measuring gas permeability of material by virtue of differential vacuum gauge |
| CN105547956A (en) * | 2015-12-10 | 2016-05-04 | 电子科技大学 | Device and method for measuring gas permeability of thin film by using vacuometer |
| CN105928855A (en) * | 2016-04-20 | 2016-09-07 | 中国原子能科学研究院 | Measuring apparatus and method for surface micropressure tritium absorption rate constant of material |
| CN206223611U (en) * | 2016-10-19 | 2017-06-06 | 中国科学院光电研究院 | A kind of material radiation causes the test device of gas infiltration |
Non-Patent Citations (1)
| Title |
|---|
| 陈进新 等.极紫外光刻动态气体锁抑制率的理论研究.《激光与光电子学进展》.2016,第0534011-0534019页. * |
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