Method for identifying corrosion resistance of aluminum oxide film layer
By using the EIS impedance test method in NaCl aqueous solution, the corrosion resistance of the alumina film layer was identified, which solved the problem that the hydrochloric acid bubble method test could not identify the film layer contamination defect, and achieved more accurate and efficient film corrosion resistance detection.
Patent Information
- Application Number
- CN202510156026.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-12
- Publication Date
- 2025-04-29
AI Technical Summary
The existing hydrochloric acid bubble method test cannot fully identify the potential contamination defects of the alumina film layer when contaminated by metal ions, resulting in the corrosion resistance of the film layer being unable to accurately reflect.
The EIS impedance test method in NaCl aqueous solution was used to compare the Nyquist curve of the sample to determine whether its corrosion resistance was qualified or unqualified.
This method can more comprehensively verify the corrosion resistance of the membrane layer, which is more environmentally friendly and safe than the hydrochloric acid bubble method, and has a shorter test time, which greatly improves the testing efficiency.
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Figure CN119901665A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to performance detection of an aluminum oxide film layer, and in particular to a method for identifying the corrosion resistance of an aluminum oxide film layer. Background Art
[0002] The components of semiconductor production equipment are mainly composed of aluminum or aluminum alloys, and their surfaces must be properly treated. Oxide film is a commonly used process. The key characteristic of the oxide film is the corrosion resistance of the film layer. The better the corrosion resistance, the stronger the equipment's ability to resist ion bombardment. The method usually used to evaluate the corrosion resistance of the film layer is the hydrochloric acid bubble test. The sample to be tested is sealed with a transparent tube, 5 wt% hydrochloric acid is poured into the transparent tube, and the time for continuous bubbles to appear on the surface of the film layer is observed to determine the corrosion resistance of the film layer.
[0003] Under normal circumstances, the hydrochloric acid bubble method can accurately reflect the corrosion resistance of the film layer, but tests have shown that if the oxidizing solution is contaminated by metal ions, the film layer will be affected to a certain extent, and the results of the hydrochloric acid bubble method test cannot reflect the changes in the film layer, indicating that there are loopholes in this test method, which may cause potential defects in the film layer to fail to be identified. Summary of the invention
[0004] In view of the problem that the hydrochloric acid bubble method for testing the corrosion resistance of the film layer cannot comprehensively identify more potential contamination defects, the present invention provides a method for identifying the corrosion resistance of the aluminum oxide film layer, which can accurately identify the corrosion resistance of the aluminum oxide film layer under various conditions.
[0005] In order to achieve the above object, the present invention provides a method for identifying the corrosion resistance of an aluminum oxide film layer, which comprises the following steps: S1. Perform EIS impedance test on the sample in NaCl aqueous solution to obtain the Nyquist curve of the sample; S2. Compare the Nyquist curve of the sample with the Nyquist curve of the standard. If the slope of the Nyquist curve of the sample is greater than or equal to the slope of the Nyquist curve of the standard, the corrosion resistance of the sample is qualified, otherwise it is unqualified.
[0006] Specifically, in step S1, the concentration of the NaCl aqueous solution is 3.5 wt%.
[0007] Specifically, in step S2, the standard product is an oxide film of the gas guide disk used in the TiAL process (ALD atomic layer deposition equipment). In the physical vapor deposition process, Wafer 1200PCS can be produced (this quantity is the current basic quantity in the industry).
[0008] Through the above technical solution, the present invention achieves the following beneficial effects: 1. The method of the present invention can more comprehensively verify the corrosion resistance of the film layer.
[0009] 2. Use EIS impedance test method, the solution is sodium chloride solution, which is more environmentally friendly and safer than hydrochloric acid bubble method.
[0010] 3. Compared with the hydrochloric acid bubble method, the EIS impedance test uses an impedance generator and software fitting to obtain the performance curve. The test takes a shorter time, which greatly improves the test efficiency. BRIEF DESCRIPTION OF THE DRAWINGS
[0011] Figure 1 is the EIS impedance test result of two test pieces in Example 1 of the present invention; Figure 2 These are the EIS impedance test results of the two test pieces in Example 2 of the present invention. DETAILED DESCRIPTION
[0012] The specific embodiments of the present invention are described in detail below. It should be understood that the specific embodiments described herein are only used to illustrate and explain the present invention, and are not used to limit the present invention.
[0013] Example 1 Two groups of test pieces were made using the same oxidation bath solution ((NH4)2C2H2(OH)2(COO)2 12~15g / L, (NH4)3BO3 120~160g / L, (NH4)2C2H4(COO)2 21~28g / L), with one piece in each group. The corrosion resistance was tested using the hydrochloric acid bubble method and the EIS impedance test method (in 3.5wt% NaCl aqueous solution) in turn. The results are as follows: Results of the hydrochloric acid method: The time corresponding to the oxide film baseline is 5 minutes; the time corresponding to test piece 1 and test piece 2 is 8 minutes 15 seconds and 8 minutes 10 seconds respectively.
[0014] The results of EIS impedance are: Figure 1 It can be seen that the performance of the two test pieces tested by the EIS impedance test method is basically the same, significantly higher than the baseline, and consistent with the conclusion of the hydrochloric acid method. The test data shows that the corrosion resistance of the film layer meets the requirements, proving that the two methods are consistent in identifying good film layers.
[0015] Example 2 Two groups of test pieces were made using contaminated bath liquid (standard solution: (NH4)2C2H2(OH)2(COO)2 12~15g / L, (NH4)3BO3 120~160g / L, (NH4)2C2H4(COO)2 21~28g / L. The source of contamination came from the machined products. They were not rinsed in time after machining, resulting in residual cutting fluid and metal elements in the products). The test results were tested using the hydrochloric acid bubble method. The results showed that the film had good corrosion resistance. Using the EIS impedance test (in a 3.5wt% NaCl aqueous solution), the Nyquist plot showed that the slopes of test pieces 3 and 4 were smaller than the baseline, indicating that the corrosion resistance of the film was poor, indicating that the bath liquid had an impact on the film during the oxidation process.
[0016] The hydrochloric acid results are as follows: the time corresponding to the oxide film baseline is 5 minutes; the time corresponding to test piece 3 and test piece 4 is 8 minutes 20 seconds and 8 minutes 25 seconds respectively; And from Figure 2 From the EIS curve, it can be seen that the slope of the curve corresponding to test piece 3 and test piece 4 is lower than the baseline, indicating that the corrosion resistance of test piece 3 and test piece 4 is worse than that of the baseline test piece. Combined with the bath solution, the hydrochloric acid method failed to truly identify the abnormal oxide film (using this batch of contaminated bath solution, an oxide film is generated on the surface of the gas guide disk used in the TiAL process (ALD atomic layer deposition equipment). In the physical vapor deposition process, only 650 PCS of Wafers (this number is significantly lower than the current industry basic number of 1200 PCS) were produced, and the equipment became abnormal, and the number of particles increased sharply. Analysis showed that it was caused by corrosion on the surface of the gas guide disk). Further EIS testing is required to effectively determine the characteristics of the film layer.
[0017] It can be seen from the above embodiments that, under special circumstances, the hydrochloric acid bubble method cannot accurately reflect the corrosion resistance of the oxide film, and the EIS impedance test method can confirm the corrosion resistance of the film layer on a larger scale, thereby avoiding the potential characteristics of the poor corrosion resistance of the oxide film made of unqualified oxidation tank liquid from not being fully identified.
[0018] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, a variety of simple modifications can be made to the technical solution of the present invention, and these simple modifications all belong to the protection scope of the present invention.
[0019] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.
[0020] In addition, various embodiments of the present invention may be arbitrarily combined, and as long as they do not violate the concept of the present invention, they should also be regarded as the contents disclosed by the present invention.
Claims
1. A method for identifying the corrosion resistance of an aluminum oxide film, characterized in that: The steps include: S1. Perform EIS impedance test on the sample in NaCl aqueous solution to obtain the Nyquist curve of the sample; S2. Compare the Nyquist curve of the sample with the Nyquist curve of the standard. If the slope of the Nyquist curve of the sample is greater than or equal to the slope of the Nyquist curve of the standard, the corrosion resistance of the sample is qualified, otherwise it is unqualified.
2. The identification method according to claim 1, characterized in that: In step S1, the concentration of the NaCl aqueous solution is 3.5 wt%.
3. The identification method according to claim 1, characterized in that: In step S2, the standard product is an oxide film of an air guide disk used in the TiAL process.