Method for analyzing particulate matters in gas transmission system component

Abstract

The invention relates to the technical field of detection. The invention discloses a method for analyzing particulate matters in a gas transmission system component. The method comprises the following steps: step 1, capturing the particulate matters; clean compressed air is connected to one end of the gas transmission system assembly, a carbon adhesive tape is placed at the other end of the gas transmission system assembly, one face of the carbon adhesive tape is bonded to the metal base, the air outlet hole is aligned to the center of the carbon adhesive tape, and a certain distance is kept between the carbon adhesive tape and the air outlet hole; the gas transmission system assembly is kept in a normally-open state, the transmission air pressure of compressed air is controlled, and the particulate matter of the gas transmission system assembly is purged and trapped for a period of time; step 2, SEM-EDS analysis is carried out; immediately transferring the captured carbon adhesive tape with the metal base into a scanning electron microscope sample bin, and vacuumizing; and performing SEM scanning electron microscope energy spectrum analysis after vacuumizing, and scanning and analyzing particles on the surface of the carbon adhesive tape.

Description

Technical Field

[0001] The present invention relates to the field of detection technology, and in particular to an analysis method for particulate matter in a gas transmission system component. Background Art

[0002] In semiconductor manufacturing, due to high cleanliness requirements, some gas transmission system components (such as diaphragm valves, pressure regulating valves, mass flow controllers, flow meters and filters, etc.) are also required to have extremely high cleanliness levels. Particles, as the most common pollutants in semiconductor manufacturing, are also present in gas transmission system components. Usually, the size and number of particles can be monitored by particle counters, but the elemental composition of the particles cannot be confirmed, which is not conducive to troubleshooting the source of particle contamination. Disassembling or destroying gas transmission system components can easily introduce additional contamination. Therefore, it is difficult to simultaneously obtain the size, number and elemental composition of particles inside gas transmission system components under non-destructive conditions. Summary of the invention

[0003] In view of the problems existing in the prior art, the present invention provides a method for analyzing particulate matter in a gas transmission system component, which solves at least one of the above-mentioned technical problems.

[0004] The technical solution of the present invention is: a method for analyzing particulate matter in a gas transmission system component, characterized in that it comprises the following steps:

[0005] Step 1: particle capture;

[0006] Connect clean compressed air to the air inlet of the gas transmission system component, place a piece of carbon tape at the air outlet of the gas transmission system component, with one side of the carbon tape bonded to the metal base; align the air hole at the air outlet with the center of the carbon tape, and keep the carbon tape 5-20mm away from the air outlet; keep the gas transmission system component in a normally open state, control the transmission pressure of compressed air at 1-20bar, and purge and capture the particles in the gas transmission system component for 10-30min;

[0007] Step 2, SEM-EDS analysis;

[0008] The captured carbon tape with metal base was immediately transferred to the SEM sample chamber and vacuumed;

[0009] After vacuuming, SEM scanning electron microscope energy spectrum analysis is performed to scan and analyze the particles on the surface of the carbon tape.

[0010] Further preferably, in step one, the gas transmission system component is a diaphragm valve, a pressure regulating valve, a mass flow controller, a flow meter or a filter.

[0011] Further preferably, in step 1, the distance between the carbon tape and the port through which the gas flows out is 5-20 mm.

[0012] Further preferably, in step 1, the transmission pressure of the compressed air is 1-20 bar.

[0013] Further preferably, in step 1, the time for purging and capturing particulate matter in the gas transmission system components is 10-30 minutes.

[0014] Further preferably, in step 2, after vacuuming, turn on the scanning electron microscope electron beam, set the acceleration voltage to 20 kV, the beam spot size to 4.0-6.0, the working distance to 10.5 mm, and in BSE mode, use carbon tape and aluminum foil as the background, adjust the brightness contrast, and make the BSE image grayscale of carbon tape and aluminum foil 1000 and 23000 respectively, set the ECD of particle detection to 0.5 μm, set the grayscale threshold range of automatic identification of particles in the BSE image to 8000-32767, and use the AZtecClean function of Oxford spectrometer to scan and analyze the particles on the surface of carbon tape.

[0015] A method for analyzing particulate matter in a gas transmission system component, characterized in that it comprises the following steps:

[0016] Step 1: particle capture;

[0017] Connect clean compressed air to the outlet of the gas transmission system component, place a piece of carbon tape at the inlet of the gas transmission system component, with one side of the carbon tape bonded to the metal base; align the air hole at the inlet with the center of the carbon tape, and keep the carbon tape 5-20mm away from the outlet; keep the gas transmission system component in a normally open state, control the transmission pressure of compressed air at 1-20bar, and purge and capture the particles in the gas transmission system component for 10-30min;

[0018] Step 2, SEM-EDS analysis;

[0019] The captured carbon tape with metal base was immediately transferred to the SEM sample chamber and vacuumed;

[0020] After vacuuming, SEM scanning electron microscope energy spectrum analysis is performed to scan and analyze the particles on the surface of the carbon tape.

[0021] Further preferably, in step 1, the gas transmission system component is a filter.

[0022] Further preferably, in step 2, after vacuuming, turn on the scanning electron microscope electron beam, set the acceleration voltage to 20 kV, the beam spot size to 4.0-6.0, the working distance to 10.5 mm, and in BSE mode, use carbon tape and aluminum foil as the background, adjust the brightness contrast, and make the BSE image grayscale of carbon tape and aluminum foil 1000 and 23000 respectively, set the ECD of particle detection to 0.5 μm, set the grayscale threshold range of automatic identification of particles in the BSE image to 8000-32767, and use the AZtecClean function of Oxford spectrometer to scan and analyze the particles on the surface of carbon tape.

[0023] Compared with the prior art, the present invention has the following beneficial effects:

[0024] The present invention provides a method for analyzing particulate matter in gas transmission system components, which mainly includes the steps of capturing particulate matter, scanning electron microscope analysis, etc. SEM-EDS is used for statistical analysis and detection. The AZtecClean function of the Oxford spectrometer can manually set the category of particulate matter according to the element and display it, and can obtain the particle size distribution above the set minimum detection particle size, as well as element information.

[0025] 1. It can effectively count the number, size and elemental composition of particles in gas transmission system components.

[0026] 2. The one-time preparation success rate is high and has a certain degree of repeatability.

[0027] 3. The method is simple to operate, highly efficient, and can automatically test particulate matter with low labor intensity. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 A schematic diagram of a specific embodiment 1 of the present invention;

[0029] Figure 2 is a scanning electron microscope photograph of the results of specific embodiment 1;

[0030] Figure 3 is a histogram of the number of particles of different particle sizes according to the results of specific embodiment 1;

[0031] Figure 4 Element information diagram of particles obtained from the results of specific Example 1;

[0032] Figure 5 Element information diagram of particles obtained from the results of specific Example 1;

[0033] Figure 6 Element information diagram of particles obtained from the results of specific Example 1;

[0034] Figure 7is a scanning electron microscope photograph of the results of specific embodiment 2;

[0035] Figure 8 is a histogram of the number of particles of different particle sizes according to the results of specific embodiment 2;

[0036] Fig. 9 Element information diagram of particles obtained from the specific example 2;

[0037] Fig.10 Element information diagram of particles obtained from the specific example 2;

[0038] Fig.11 Element information diagram of particles obtained from the specific example 2;

[0039] Fig.12 is a scanning electron microscope photograph of the result of specific embodiment 3;

[0040] Fig.13 is a histogram of the number of particles of different particle sizes according to the results of specific embodiment 3;

[0041] Fig.14 Element information diagram of particles obtained from the specific example 3;

[0042] Fig.15 Element information diagram of particles obtained from the specific example 3;

[0043] Fig.16 The scanning electron microscope photograph of the result of the comparative example;

[0044] Fig.17 The following is a comparison table of the number of particles of different particle sizes showing the results of comparative examples. DETAILED DESCRIPTION

[0045] See also Figure 1 ,Specific embodiment 1, the gas transmission system component is a diaphragm valve;

[0046] A method for analyzing particulate matter in a gas transmission system component comprises the following steps:

[0047] Step 1: particle capture;

[0048] Connect clean compressed air to the air inlet of the gas transmission system component, place a piece of carbon tape at the air outlet of the gas transmission system component, with one side of the carbon tape bonded to the metal base; align the air hole at the air outlet with the center of the carbon tape, and keep the carbon tape 5-20mm away from the air outlet; keep the gas transmission system component in a normally open state, control the transmission pressure of compressed air at 1-20bar, and purge and capture the particles in the gas transmission system component for 10-30min;

[0049] Step 2, SEM-EDS analysis;

[0050] The captured carbon tape with metal base was immediately transferred to the SEM sample chamber and vacuumed;

[0051] After vacuuming, SEM scanning electron microscope energy spectrum analysis is performed to scan and analyze the particles on the surface of the carbon tape.

[0052] In step one, the gas delivery system component is a diaphragm valve.

[0053] In step 2, after vacuuming, turn on the electron beam of the scanning electron microscope, set the acceleration voltage to 20kv, the beam spot size to 4.0-6.0, the working distance to 10.5mm, and in BSE mode, use carbon tape and aluminum foil as the background, adjust the brightness contrast, make the BSE image grayscale of carbon tape and aluminum foil 1000 and 23000 respectively, set the ECD of particle detection to 0.5μm, set the grayscale threshold range of automatic identification of particles in BSE image to 8000-32767, and use the AZtecClean function of Oxford spectrometer to scan and analyze the particles on the surface of carbon tape. Environment: Class 1000 / Class 100 / Class 10.

[0054] The results of specific example 1 are shown in Figure 2 , Figure 3 , Figure 4 , Figure 5 as well as Figure 6 .

[0055] Figure 2 This is a scanning electron microscope photo. Figure 3 It is the particle number histogram of different particle sizes. Figures 4 to 6 It is the element information diagram of the particles. The vertical axis is the number of particles of the corresponding element. The horizontal axis is the mass percentage content of the current element in the particles containing a certain element.

[0056] In specific embodiment 2, the gas transmission system component is a filter, and positive blowing is used as an example;

[0057] A method for analyzing particulate matter in a gas transmission system component, characterized in that it comprises the following steps:

[0058] Step 1: particle capture;

[0059] Connect clean compressed air to the outlet of the gas transmission system component, place a piece of carbon tape at the inlet of the gas transmission system component, with one side of the carbon tape bonded to the metal base; align the air hole at the outlet with the center of the carbon tape, and keep the carbon tape 5-20mm away from the outlet; keep the gas transmission system component in a normally open state, control the transmission pressure of compressed air at 1-20bar, and purge and capture the particles in the gas transmission system component for 10-30min;

[0060] Step 2, SEM-EDS analysis;

[0061] The captured carbon tape with metal base was immediately transferred to the SEM sample chamber and vacuumed;

[0062] After evacuation, turn on the electron beam of the scanning electron microscope, set the acceleration voltage to 20 kV, the beam spot size to 4.0-6.0, and the working distance to 10.5 mm. In BSE mode, use carbon tape and aluminum foil as the background, adjust the brightness contrast, and make the BSE image grayscale of carbon tape and aluminum foil 1000 and 23000 respectively. Set the ECD of particle detection to 0.5 μm, and set the grayscale threshold range of automatic identification of particles in the BSE image to 8000-32767. Use the AZtecClean function of the Oxford spectrometer to scan and analyze the particles on the surface of the carbon tape.

[0063] In step 1, the gas delivery system component is the filter. Environment: Class 1000 / Class 100 / Class 10.

[0064] The analysis results of specific embodiment 2 are shown in Figure 7 , Figure 8 , Fig. 9 , Fig.10 as well as Fig.11 .

[0065] Figure 7 This is a scanning electron microscope photo. Figure 8 It is the particle number histogram of different particle sizes. Figures 9 to 11 It is the element information diagram of the particles. The vertical axis is the number of particles of the corresponding element. The horizontal axis is the mass percentage content of the current element in the particles containing a certain element.

[0066] Specific embodiment 3, the gas transmission system component is a filter, and backflushing is used as an example;

[0067] A method for analyzing particulate matter in a gas transmission system component comprises the following steps:

[0068] Step 1: particle capture;

[0069] Connect clean compressed air to the outlet of the gas transmission system component, place a piece of carbon tape at the inlet of the gas transmission system component, with one side of the carbon tape bonded to the metal base; align the air hole at the inlet with the center of the carbon tape, and keep the carbon tape 5-20mm away from the outlet; keep the gas transmission system component in a normally open state, control the transmission pressure of compressed air at 1-20bar, and purge and capture the particles in the gas transmission system component for 10-30min;

[0070] Step 2, SEM-EDS analysis;

[0071] The captured carbon tape with metal base was immediately transferred to the SEM sample chamber and vacuumed;

[0072] After evacuation, turn on the electron beam of the scanning electron microscope, set the acceleration voltage to 20 kV, the beam spot size to 4.0-6.0, and the working distance to 10.5 mm. In BSE mode, use carbon tape and aluminum foil as the background, adjust the brightness contrast, and make the BSE image grayscale of carbon tape and aluminum foil 1000 and 23000 respectively. Set the ECD of particle detection to 0.5 μm, and set the grayscale threshold range of automatic identification of particles in the BSE image to 8000-32767. Use the AZtecClean function of the Oxford spectrometer to scan and analyze the particles on the surface of the carbon tape.

[0073] Gas delivery system components are filters. Environment: Class 1000 / Class 100 / Class 10.

[0074] The analysis results of specific embodiment 3 are shown in Fig.12 , Fig.13 , Fig.14 as well as Fig.15 .

[0075] Fig.12 This is a scanning electron microscope photo. Fig.13 It is the particle number histogram of different particle sizes. Figure 14 to Figure 15 It is the element information diagram of the particles. The vertical axis is the number of particles of the corresponding element. The horizontal axis is the mass percentage content of the current element in the particles containing a certain element.

[0076] Comparative Example: In this comparative example, no gas transmission system components are used, and the following steps are included:

[0077] Environment: Level 1000 / Level 100 / Level 10;

[0078] Place a piece of carbon tape at the outlet of clean compressed air / high-purity nitrogen, with one side of the carbon tape bonded to a metal base of the same size. Align the air hole at the outlet with the center of the carbon tape, and keep the carbon tape 5-20mm away from the air hole at the outlet. Turn on the compressed air / high-purity nitrogen, control the air pressure at 1-20bar, and purge and capture the particles in the pipeline for 10-30min.

[0079] The captured carbon tape with metal base was immediately transferred to the SEM sample chamber and vacuumed;

[0080] After evacuation, turn on the electron beam of the scanning electron microscope, set the acceleration voltage to 20kv, the beam spot size to 4.0-6.0, the working distance to 10.5mm, and in BSE mode, use carbon tape and aluminum foil as the background, adjust the brightness contrast, and make the BSE image grayscale of carbon tape and aluminum foil 1000 and 23000 respectively, set the ECD of particle detection to 0.5μm, set the grayscale threshold range of automatic identification of particles in BSE images to 8000-32767, and use the AZtecClean function of the Oxford spectrometer to scan and analyze the particles on the surface of the carbon tape. The analysis results are shown in the table. Fig.16 , Fig.17 .

[0081] Fig.16 This is a scanning electron microscope photo. Fig.17 The following is a comparison table of the number of particles of different particle sizes. It can be seen from the comparative examples that no additional particles are introduced by this method.

[0082] The above are only preferred embodiments of the present invention. It should be pointed out that, for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A method for analyzing particulate matter in a gas transmission system component, characterized in that: The steps include: Step 1: particle capture; Connect clean compressed air to the air inlet of the gas transmission system component, place a piece of carbon tape at the air outlet of the gas transmission system component, with one side of the carbon tape bonded to the metal base; align the air hole at the air outlet with the center of the carbon tape, and keep the carbon tape 5-20mm away from the air outlet; keep the gas transmission system component in a normally open state, control the transmission pressure of compressed air at 1-20bar, and purge and capture the particles in the gas transmission system component for 10-30min; Step 2, SEM-EDS analysis; The captured carbon tape with metal base was immediately transferred to the SEM sample chamber and vacuumed; After vacuuming, SEM scanning electron microscope energy spectrum analysis is performed to scan and analyze the particles on the surface of the carbon tape.

2. The method for analyzing particulate matter in a gas transmission system component according to claim 1, characterized in that: In step one, the gas delivery system component is a diaphragm valve, a pressure regulating valve, a mass flow controller, a flow meter, or a filter.

3. The method for analyzing particulate matter in a gas transmission system component according to claim 1, characterized in that: In step 2, after vacuuming, turn on the electron beam of the scanning electron microscope, set the acceleration voltage to 20 kV, the beam spot size to 4.0-6.0, the working distance to 10.5 mm, and in BSE mode, use carbon tape and aluminum foil as the background, adjust the brightness contrast, and make the BSE image grayscale of carbon tape and aluminum foil 1000 and 23000 respectively, set the ECD of particle detection to 0.5 μm, set the grayscale threshold range of automatic identification of particles in the BSE image to 8000-32767, and use the AZtecClean function of the Oxford spectrometer to scan and analyze the particles on the surface of the carbon tape.

4. A method for analyzing particulate matter in a gas transmission system component, characterized in that: The steps include: Step 1: particle capture; Connect clean compressed air to the outlet of the gas transmission system component, place a piece of carbon tape at the inlet of the gas transmission system component, with one side of the carbon tape bonded to the metal base; align the air hole at the inlet with the center of the carbon tape, and keep the carbon tape 5-20mm away from the outlet; keep the gas transmission system component in a normally open state, control the transmission pressure of compressed air at 1-20bar, and purge and capture the particles in the gas transmission system component for 10-30min; Step 2, SEM-EDS analysis; The captured carbon tape with metal base was immediately transferred to the SEM sample chamber and vacuumed; After vacuuming, SEM scanning electron microscope energy spectrum analysis is performed to scan and analyze the particles on the surface of the carbon tape.

5. The method for analyzing particulate matter in a gas transmission system component according to claim 1, characterized in that: In step one, the gas delivery system component is a filter.

6. The method for analyzing particulate matter in a gas transmission system component according to claim 1, characterized in that: In step 2, after vacuuming, turn on the electron beam of the scanning electron microscope, set the acceleration voltage to 20 kV, the beam spot size to 4.0-6.0, the working distance to 10.5 mm, and in BSE mode, use carbon tape and aluminum foil as the background, adjust the brightness contrast, and make the BSE image grayscale of carbon tape and aluminum foil 1000 and 23000 respectively, set the ECD of particle detection to 0.5 μm, set the grayscale threshold range of automatic identification of particles in the BSE image to 8000-32767, and use the AZtecClean function of the Oxford spectrometer to scan and analyze the particles on the surface of the carbon tape.

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