CN115792080A - Method for testing trace ion pollution on surface of semiconductor manufacturing equipment component - Google Patents
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- CN115792080A CN115792080A CN202211547774.7A CN202211547774A CN115792080A CN 115792080 A CN115792080 A CN 115792080A CN 202211547774 A CN202211547774 A CN 202211547774A CN 115792080 A CN115792080 A CN 115792080A
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- 238000012360 testing method Methods 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 38
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 26
- 239000004065 semiconductor Substances 0.000 title claims abstract description 26
- 229920000742 Cotton Polymers 0.000 claims abstract description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000002791 soaking Methods 0.000 claims abstract description 20
- 239000000835 fiber Substances 0.000 claims abstract description 15
- 229920000728 polyester Polymers 0.000 claims abstract description 15
- 238000005070 sampling Methods 0.000 claims abstract description 14
- 238000004255 ion exchange chromatography Methods 0.000 claims abstract description 12
- 238000004140 cleaning Methods 0.000 claims abstract description 11
- 229920001903 high density polyethylene Polymers 0.000 claims description 13
- 239000004700 high-density polyethylene Substances 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 12
- 238000011109 contamination Methods 0.000 claims description 10
- 239000000356 contaminant Substances 0.000 claims description 7
- 230000003749 cleanliness Effects 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 3
- 239000012498 ultrapure water Substances 0.000 claims description 3
- 125000000129 anionic group Chemical group 0.000 claims description 2
- 125000002091 cationic group Chemical group 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 1
- 150000002500 ions Chemical class 0.000 abstract description 26
- 239000003344 environmental pollutant Substances 0.000 abstract description 10
- 231100000719 pollutant Toxicity 0.000 abstract description 9
- 238000004458 analytical method Methods 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 description 16
- 239000010453 quartz Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 150000001450 anions Chemical class 0.000 description 2
- 238000000861 blow drying Methods 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
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Abstract
The invention discloses a method for testing trace ion pollution on the surface of a semiconductor manufacturing equipment part, which is carried out in a clean room with the cleaning grade of at least 100 grades; and wiping the surface of the part to be tested by using a clean dustless polyester fiber cotton swab, sampling, soaking the cotton swab in electronic-grade water in a clean small bottle, taking out the cotton swab, and testing the ion content in the solution by using ion chromatography. The invention uses an indirect sampling mode of wiping a dust-free cotton swab to wipe out trace ions on the surface of a semiconductor manufacturing equipment part through the cotton swab, then uses electronic grade water to soak the cotton swab, finally takes out the cotton swab, and uses ion chromatography to test the ion content in the solution. The method is simple, convenient and quick to operate, and is suitable for local testing and surface trace ion pollutant analysis of large-size parts.
Description
Technical Field
The invention belongs to the technical field of semiconductor detection, relates to detection of semiconductor manufacturing equipment components, and particularly relates to a method for testing trace ion pollution on the surfaces of semiconductor manufacturing equipment components.
Background
With the rapid development of the semiconductor industry, the research on the advanced semiconductor process is more and more urgent. Since various pollutants (metal ions, particles and the like) are easily introduced in the manufacturing process, the pollutants can change the size of a device, change the cleanliness of the surface and cause a pitted surface, and therefore the cleaning link of parts is more important. The high degree of contamination allows only a small number of parts to complete the process, resulting in increased costs. In addition, mobile ionic contaminants can alter the electrical properties of the device and even cause device failure, and thus effective cleaning of semiconductor manufacturing equipment is extremely critical to the semiconductor industry.
In order to control micro-pollution in the manufacturing environment and improve the product yield, the detection of the surface micro-pollution of the manufacturing equipment parts and the surface micro-pollution after the cleaning and regeneration of the parts is very important. The detection of the pollutant components on the surface of the part can judge whether the surface pollutants are effectively removed or not, and can help to develop a cleaning regeneration process with stronger pertinence, so that the reliability of the manufacturing process is improved.
A great part of micro-pollutants on the surface of a semiconductor manufacturing equipment part belongs to anion and cation pollutants, and a quantitative analysis technology is required. Among the conventional trace ion analysis methods, ion chromatography (hereinafter referred to as "IC") is a widely used one. The IC has the advantages of low detection limit and high detection precision down to the PPb level, and meets the detection requirement of a semiconductor manufacturing factory on the micro-pollution control of the surfaces of devices and equipment.
The current commonly used testing means for micro-pollution on the surface of the part is an integral soaking method, namely, the part is wholly soaked in a solution, the part is taken out after a certain time, and the soaking solution passes through IC (integrated circuit) for testing, so that the micro-pollution content on the surface of the part can be obtained. However, the size of the parts of the semiconductor manufacturing equipment is often large, a proper vessel is difficult to find for soaking, and the blank of the process is difficult to control; some parts only need to test the ionic pollutants in the polluted area and cannot be directly soaked; in addition, the long-time integral soaking can corrode the surface of the part, and the integral soaking cannot be directly carried out. These have all prevented effective performance of the micro-contamination test on the surface of the component. Therefore, the development of a method for testing the trace ion pollution on the surface of the semiconductor manufacturing equipment component is of great significance.
Disclosure of Invention
The invention provides a brand-new testing method for the trace ion pollution on the surface of the semiconductor manufacturing equipment part, which aims at the defects of the trace ion pollution on the surface of the existing semiconductor manufacturing equipment part, completely abandons the existing mode that the detection can be realized only by soaking the whole part to be detected, adopts an indirect sampling mode of wiping the surface by using a dust-free cotton swab to realize the detection, and improves the application range.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the invention provides a method for testing trace ion pollution on the surface of a semiconductor manufacturing equipment part, which has the following technical characteristics: in a clean room having a cleanliness class of at least 100; and wiping the surface of the part to be tested by using a clean dustless polyester fiber cotton swab, sampling, soaking the cotton swab in electronic-grade water in a clean small bottle, taking out the cotton swab, and testing the ion content in the solution by using ion chromatography.
Preferably, the cationic contaminants comprise Li + 、Na + 、NH 4 + 、K + 、Mg 2+ 、Ca 2+ (ii) a The anionic contaminant comprises F - 、Cl - 、NO 2 - 、Br - 、NO 3 - 、PO 4 3- 、SO 4 2- 。
The cotton swab head of the polyester fiber cotton swab is made of one hundred percent of polyester fiber.
The dust-free polyester fiber cotton swab cleaning process comprises the following steps: before using, the cotton swab needs to be washed with electronic grade water for 2 times, then the electronic grade water is used for ultrasonic treatment for 20min, and the steps are repeated for 5 times; and then rinsed 2 times with electronic grade water and soaked in electronic grade water for at least 1 week, removed and placed in a clean vial for use, and rinsed 6 times with electronic grade water before each use.
The vial used in the test procedure was a HDPE vial, which was cleaned as follows: washing with electronic grade water for 2 times, filling with electronic grade water, performing ultrasound for 20min, repeating twice, washing with electronic grade water for 2 times, filling with electronic grade water, storing, washing with electronic grade water for at least 2 times before each use, and blow-drying with high pressure air gun.
In the detection process, the sampling process is operated as follows: the method comprises the steps of slightly wiping the front surface and the back surface of a part to be tested on the surface of the part to be tested by using a dust-free polyester fiber cotton swab in opposite wiping directions, calculating the area of a wiping area, then placing the part into another clean HDPE empty bottle, adding 20-40 ml of electronic grade water, covering the bottle with a cover, soaking for 5 minutes, taking out the cotton swab, and testing the ion content in a solution by using ion chromatography.
In the detection process, a blank test step is required to be carried out at the same time: a dust-free polyester fiber cotton swab is placed in a clean empty bottle, 20-40 mL of electronic grade water is added, a cover is covered, after 5 minutes of soaking, the cotton swab is taken out, and the ion content in the solution is tested by using ion chromatography.
After the detection is finished, calculating the content of trace ion pollutants on the surface of the part to be detected according to the following formula:
wherein: the unit of surface contaminant concentration is: 10 12 molecules/cm 2 ；
C p The concentration in ppb of the test parts is reported as the value after;
C B the concentration in ppb, which is the blank of the overall process, is recorded as the previous value;
v is the volume of ultrapure water for soaking the cotton swab to be measured, and the unit is L;
N A avogalois constants: 6.022 × 10 23 ；
M is relative molecular mass, unit: g/mol;
s is the wiping area in cm 2 。
The invention has the following beneficial effects:
in the aspect of effect, the invention utilizes an indirect sampling mode of wiping a dust-free cotton swab to wipe out trace ions on the surface of a semiconductor manufacturing equipment part through the cotton swab, then uses electronic grade water to soak the cotton swab, finally takes out the cotton swab, and uses ion chromatography to test the ion content in the solution. The sampling mode is suitable for local test sampling, is also suitable for surface trace element pollutant analysis of large-size parts, has a wide application range, and overcomes the defects that the current soaking sampling mode is small in application range and can damage the parts.
In the aspect of operation, the cleaning treatment mode of the cotton swab and the small bottle and the component surface wiping sampling mode used in the sampling process are simple and easy to master, and the rapid detection is facilitated.
Drawings
FIG. 1 is a schematic view of the direction of swab wiping sampling.
Detailed Description
The present invention will now be described in detail with reference to the embodiments and the accompanying drawings, but it should be understood that the following detailed description is illustrative and not restrictive, and should not be taken to limit the scope of the invention. The following examples are carried out on the premise of the technical scheme of the invention, and give detailed implementation modes and specific operation processes. The raw materials and equipment used in the invention can be obtained from the market.
The test of the trace ion contamination on the surface of the quartz cavity component in the embodiment comprises the following procedures:
1. ware cleaning process
1. HDPE bottle: washing with electronic grade water for 2 times, filling with electronic grade water, performing ultrasound for 20min, repeating twice, washing with electronic grade water for 2 times, filling with electronic grade water, storing, washing with electronic grade water for at least 2 times before each use, and blow-drying with high pressure air gun.
2. Cleaning a cotton swab:
the cotton bud head is made of one hundred percent polyester fiber.
Placing the cotton swab for wiping in a cleaned HDPE bottle, washing with electronic grade water for 2 times, filling with electronic grade water for ultrasonic treatment for 20min, repeating for 5 times, washing with electronic grade water for 2 times, filling with electronic grade water for soaking for 1-2 weeks, taking out, washing with electronic grade water for 6 times, and placing in the cleaned HDPE empty bottle for later use.
2. Testing of
1. Full process blank (MB) test:
and (3) taking out a clean cotton swab in the HDPE bottle in a 100-grade clean room, placing the clean HDPE empty bottle in the cleaned clean HDPE empty bottle, adding 20-40 mL of electronic grade water, covering the clean HDPE empty bottle with a cover, soaking for 5 minutes, taking out the cotton swab, and testing the ion content in the solution by using ion chromatography.
2. Testing of a quartz cavity sample part:
and taking out another clean cotton swab in the HDPE bottle in a 100-grade clean room, lightly wiping the surface of the part to be detected, calculating the area of a wiping area, then placing the part into another cleaned clean HDPE empty bottle, adding 20-40 mL of electronic grade water, covering a cover, soaking for 5 minutes, taking out the cotton swab, and testing the ion content in the solution by using ion chromatography. The schematic diagram of the wiping direction of the cotton swab is shown in fig. 1, and the wiping directions of the front surface and the back surface of the component to be detected are opposite.
3. Ions tested:
cation: li + 、Na + 、NH 4 + 、K + 、Mg 2+ 、Ca 2+ ；
Anion: f-, cl - 、NO 2- 、Br - 、NO 3 - 、PO 4 3- 、SO 4 2- 。
4. Concentration calculation
And taking the difference value of the two test results, and calculating the result through the following formula, wherein the result is the content of trace ion pollution on the surface of the quartz cavity component:
wherein: c p The concentration in ppb of the test parts is reported as the value after;
C B the concentration in ppb, which is the blank of the overall process, is recorded as the previous value;
v is the volume of ultrapure water for soaking the cotton swab to be measured, and the unit is L;
N A is the Avogadro constant: 6.022 × 10 23 ；
M is relative molecular mass, unit: g/mol;
s is the wiping area in cm 2 。
The detection results for each test ion are shown in table 1 below:
TABLE 1 summary of the results of the different ion measurements
| Serial number | Testing ions | Method detection limit | Test results | Unit |
| 1 | Li + | 8.7 | / | 10 12 molecules/cm 2 |
| 2 | Na + | 15.7 | 851.3 | 10 12 molecules/cm 2 |
| 3 | NH 4 + | 20.1 | 40.1 | 10 12 molecules/cm 2 |
| 4 | K + | 18.5 | / | 10 12 molecules/cm 2 |
| 5 | Mg 2+ | 14.9 | / | 10 12 molecules/cm 2 |
| 6 | Ca 2+ | 13.5 | 52.7 | 10 12 molecules/cm 2 |
| 7 | F - | 1.3 | / | 10 12 molecules/cm 2 |
| 8 | Cl - | 0.3 | 176.8 | 10 12 molecules/cm 2 |
| 9 | NO 2 - | 4.5 | 48.6 | 10 12 molecules/cm 2 |
| 10 | Br - | 0.4 | / | 10 12 molecules/cm 2 |
| 11 | NO 3 - | 3.2 | 36.7 | 10 12 molecules/cm 2 |
| 12 | PO 4 3- | 1.0 | / | 10 12 molecules/cm 2 |
| 13 | SO 4 2- | 0.3 | 26.8 | 10 12 molecules/cm 2 |
Note: in the table, "/" indicates that the detection limit is lower.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are given by way of illustration of the principles of the present invention, and that various changes and modifications may be made without departing from the spirit and scope of the invention as defined by the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. A method for testing trace ion pollution on the surface of a semiconductor manufacturing equipment component is characterized by comprising the following steps: in a clean room having a cleanliness class of at least class 100; and wiping the surface of the part to be tested by using a clean dustless polyester fiber cotton swab, sampling, soaking the cotton swab in electronic-grade water in a clean small bottle, taking out the cotton swab, and testing the ion content in the solution by using ion chromatography.
2. The method of claim 1, wherein the step of testing the surface of the semiconductor manufacturing equipment component for trace ion contamination comprises:
wherein the cationic contaminants comprise Li + 、Na + 、NH 4 + 、K + 、Mg 2+ 、Ca 2+ (ii) a The anionic contaminant comprises F - 、Cl - 、NO 2 - 、Br - 、NO 3 - 、PO 4 3- 、SO 4 2- 。
3. The method of claim 1, wherein the testing for trace ion contamination on the surface of a component of semiconductor manufacturing equipment comprises:
wherein, the cotton swab head of the polyester fiber cotton swab is made of one hundred percent of polyester fiber.
4. The method of claim 1, wherein the testing for trace ion contamination on the surface of a component of semiconductor manufacturing equipment comprises:
wherein, the dust-free polyester fiber cotton swab has the following cleaning process: before using, the cotton swab needs to be washed with electronic grade water for 2 times, then the electronic grade water is used for ultrasonic treatment for 20min, and the steps are repeated for 5 times; and then rinsed 2 times with electronic grade water and soaked in electronic grade water for at least 1 week, removed and placed in a clean vial for use, and rinsed 6 times with electronic grade water before each use.
5. The method of claim 1, wherein the step of testing the surface of the semiconductor manufacturing equipment component for trace ion contamination comprises:
wherein the vial is an HDPE bottle and the cleaning process is as follows: washing with electronic grade water for 2 times, ultrasonic treating with electronic grade water for 20min, repeating twice, washing with electronic grade water for 2 times, filling with electronic grade water, storing, washing with electronic grade water for at least 2 times before each use, and drying with high pressure air gun.
6. The method of claim 1, wherein the step of testing the surface of the semiconductor manufacturing equipment component for trace ion contamination comprises:
wherein, the operation of the sampling process is as follows: lightly wiping the surface of the part to be tested by adopting a dust-free polyester fiber cotton swab, calculating the area of a wiping area, then placing the part into another clean HDPE empty bottle, adding 20-40 ml of electronic grade water, covering the bottle with a cover, soaking for 5 minutes, taking out the cotton swab, and testing the ion content in the solution by using ion chromatography.
7. The method of claim 6, wherein the step of testing the surface of the semiconductor manufacturing equipment component for trace ion contamination comprises the steps of:
wherein, the wiping directions of the dust-free polyester fiber cotton swab on the front surface and the back surface of the component to be detected are opposite.
8. The method of claim 1, further comprising a blank testing step of: a dust-free polyester fiber cotton swab is placed in a clean empty bottle, 20-40 mL of electronic grade water is added, a cover is covered, after 5 minutes of soaking, the cotton swab is taken out, and the ion content in the solution is tested by using ion chromatography.
9. The method of claim 8, wherein the trace ion contamination on the surface of the device under test is calculated according to the following formula:
wherein: the unit of surface contaminant concentration is: 10 12 molecules/cm 2 ；
C p The concentration in ppb of the test parts is reported as the value after;
C B the concentration in ppb, which is the blank of the overall process, is recorded as the previous value;
v is the volume of ultrapure water for soaking the cotton swab to be measured, and the unit is L;
N A avogalois constants: 6.022 × 10 23 ；
M is relative molecular mass, unit: g/mol;
s is the wiping area in cm 2 。
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|---|---|---|---|---|
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| CN113484446A (en) * | 2021-08-04 | 2021-10-08 | 上海富乐德智能科技发展有限公司 | Method for testing micro-pollution on surface of packaging bag for clean room |
| CN113533489A (en) * | 2021-08-09 | 2021-10-22 | 上海富乐德智能科技发展有限公司 | Method for testing micro-pollution in through hole of semiconductor equipment part |
-
2022
- 2022-12-05 CN CN202211547774.7A patent/CN115792080A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000002632A (en) * | 1998-04-13 | 2000-01-07 | Shimizu Corp | Contaminant defection method |
| KR20060032908A (en) * | 2004-10-13 | 2006-04-18 | 동부아남반도체 주식회사 | Method for measuring the degree of contamination using wiper |
| US20070274814A1 (en) * | 2006-05-26 | 2007-11-29 | Atsuko Kawasaki | Local clean robot-transport plant and robot-transport manufacturing method |
| CN105825902A (en) * | 2015-01-08 | 2016-08-03 | 哈电集团（秦皇岛）重型装备有限公司 | Method for detecting cleanliness of surfaces of AP1000 nuclear power equipment parts |
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