Film-forming thickness control method of C-type poly-p-xylylene film

By establishing a thickness control model for the deposition rotary tooling and optimizing the vapor deposition process parameters, the problem of difficult to control the film formation thickness of C-type parylene film is solved, and the precise adjustment of film thickness and the improvement of film layer quality are achieved.

CN119615102APending Publication Date: 2025-03-1410TH RES INST OF CETC
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Patent Information

Application Number
CN202411742247.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-29
Publication Date
2025-03-14

AI Technical Summary

Technical Problem

The prior art is difficult to accurately control the film forming thickness of C-type parylene film, which affects product cost and performance.

Method used

By preparing multi-sheet polyester film substrates, a thickness control model for deposition rotary tooling is established, the vapor deposition process parameters are optimized, and the high controllability of the thickness of C-type parylene film is achieved.

Benefits of technology

It realizes precise adjustment of film thickness at the nano level, improves the quality and uniformity of the film layer, reduces production costs, and broadens the application scenarios of materials.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a film forming thickness control method of a C-type poly-p-xylylene film. The method comprises the following steps: S1, preparing a plurality of polyester film substrates; s2, preparing the polyester film substrate to obtain a parylene C film thickness control standard sample; s3, measuring the thickness of the parylene C film to control the thickness of the standard sample; s4, the paraxylene Parylene C film thickness control standard samples are placed on the upper layer, the middle layer and the lower layer of a deposition rotating tool respectively, calculation is carried out on each layer according to the paraxylene Parylene C film thickness, the position and dimer loading amount data, a model is established, and a thickness control model is obtained; s5, controlling the thickness of the parylene C thin film according to the thickness control model of each layer; the technical problem that the thickness of the C-type poly-p-xylylene film is difficult to control at present can be solved.
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Description

Technical Field

[0001] The invention belongs to the technical field of drug detection, and specifically relates to a method for controlling the film thickness of a C-type polyparaxylene film. Background Art

[0002] Since the C-type polyparaxylene film is grown by vapor deposition, the film layer is denser than the air spray coating. In addition, it can reach the task part of the product and has good sealing performance for the product. The vapor deposition method and its structure make the grinding layer have excellent moisture-proof, smoke-proof, mildew-proof performance, gas isolation performance, physical and mechanical properties, optical properties, biocompatibility and electrical insulation. Therefore, it is widely used in semiconductors, integrated circuits, micro-electromechanical systems, sensors, medical devices and cultural relics protection. Especially in the field of microwave circuit protection, C-type polyparaxylene can meet the functional and protection needs of the product at the same time.

[0003] The thickness of C-type polyparaxylene film affects the cost of the product on the one hand; on the other hand, its thickness is closely related to the performance of microwave circuit components. If the thickness is too thick, it will affect the product function and cause product failure. Therefore, for the product, it is very important to control the thickness of C-type polyparaxylene film. However, since its film formation process is a gas phase process, it has always been difficult to accurately control its film thickness.

[0004] At present, the thickness control of polyparaxylene film is mainly achieved indirectly by controlling the loading amount of dimer. This method can control the film thickness to a certain extent, but does not take into account the difference in film thickness at different positions in the deposition chamber during the vapor deposition process. In addition, this control method cannot directly correspond to the film thickness and cannot fully meet the user's low cost, high reliability and design requirements. From the current publicly released papers and patents, there is no technology for thickness control of C-type polyparaxylene film. Most technologies focus on product performance analysis, film performance analysis, equipment and deposition process optimization, and do not involve C-type polyparaxylene film thickness control technology. Summary of the invention

[0005] In order to overcome the defects of the prior art, the present invention provides a method for controlling the film thickness of a C-type polyparaxylene film, which can solve the current technical problem that the thickness control of the C-type polyparaxylene film is difficult.

[0006] The object of the present invention is achieved through the following technical solutions:

[0007] A method for controlling the film thickness of a C-type polyparaxylene film comprises the following steps:

[0008] S1, preparing multiple polyester film substrates; S2, preparing the above polyester film substrates to obtain a standard sample for the thickness control of Parylene C film; S3, measuring the thickness of the above standard sample for the thickness control of Parylene C film; S4, placing the above standard sample for the thickness control of Parylene C film on the upper layer, middle layer and lower layer of the deposition rotating tooling, respectively, calculating and establishing a model for each layer according to the thickness, position and dimer loading data of the above Parylene C film, and obtaining a thickness control model;

[0009] S5. Control the thickness of the Parylene C film according to the thickness control model of each layer.

[0010] In one embodiment, in S1 above, the preparation of the polyester film substrate comprises the following steps: A1, cutting the polyester film; A2, washing the polyester film three times with ethanol and drying it in an oven at 50-60° C. for 28-32 minutes; A3, applying a release agent to all surfaces of the polyester film substrate, twice on each surface;

[0011] A4. Dry the polyester film coated with the release agent at 45-55° C. for 4-6 minutes to obtain the above-mentioned polyester film substrate.

[0012] In one embodiment, in the above A1, the size of the above polyester film after cutting is (100±1) mm×(100±1) mm.

[0013] In one embodiment, in the above A3, the preparation of the above release agent includes the following steps: B1, mixing deionized water and micro-90 cleaning solution in a volume ratio of 2:100; B2, stirring for 13 to 17 minutes and standing for 25 to 35 minutes to obtain the above release agent.

[0014] In one embodiment, in the above S2, the preparation of the above-mentioned Parylene C film thickness control standard sample comprises the following steps: C1, placing the above-mentioned polyester film substrate on the upper, middle and lower trays of the above-mentioned deposition rotating tooling respectively; C2, loading C-type polyparaxylene dimer, and depositing Parylene C film on the polyester film substrate, so as to obtain the above-mentioned Parylene C film thickness control standard sample.

[0015] In one embodiment, in the above C1, two sheets of the above polyester film substrates are placed on each tray and are symmetrically arranged.

[0016] In one embodiment, the second-order polynomial thickness control mathematical model formula for depositing the upper layer of the rotary tooling is:

[0017] τ=0.265m-0.0000742m 2 -0.432

[0018] Where: τ is the film thickness in μm, m is the dimer loading in g.

[0019] In one embodiment, the second-order polynomial thickness control mathematical model formula of the layer in the deposition rotary tooling is:

[0020] τ=0.253m-0.0000481m 2 +0.143

[0021] Where: τ is the film thickness in μm, m is the dimer loading in g.

[0022] In one embodiment, the second-order polynomial thickness control mathematical model formula of the layer in the deposition rotary tooling is:

[0023] τ=0.27m+0.000186m 2 +0.419

[0024] Where: τ is the film thickness in μm, m is the dimer loading in g.

[0025] The beneficial effects of the present invention are:

[0026] The present invention provides a method for controlling the film thickness of a C-type polyparaxylene film, which can effectively solve the above-mentioned problems. By optimizing the vapor deposition process parameters, including but not limited to key factors such as precursor gas flow rate, deposition temperature, and reaction chamber pressure, the present invention achieves a high degree of controllability of the deposition thickness of the C-type polyparaxylene film. This technological advancement not only allows the film thickness to be precisely adjusted at the nanometer level, but also greatly improves the quality of the film layer, ensuring its uniformity and density, which is crucial to improving the performance of the final product.

[0027] In addition, the application of this technology has also brought about a significant improvement in production efficiency, reduced production costs, and broadened the application scenarios of C-type polyparaxylene film materials. For example, in microelectronics manufacturing, this high-quality film can be used as an effective insulating layer or protective layer to enhance the reliability and service life of the equipment; in the biomedical field, it can be used to manufacture implantable medical devices to improve their biocompatibility and functionality.

[0028] In conclusion, this invention not only promotes the development of materials science by improving the deposition technology of C-type polyparaxylene film, but also provides strong support for technological innovation in multiple industries. With the deepening of research and the continuous improvement of technology, it is expected that more new products based on this technology will be launched in the future, contributing to the progress of human society. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] The present invention will be described in more detail below based on embodiments and with reference to the accompanying drawings, wherein:

[0030] Figure 1 This is the fitting result of the thickness control function of the standard sample on the tray of type C xylene in the embodiment of the present invention;

[0031] Figure 2 This is the fitting result of the thickness control function of the standard sample of the tray in type C xylene in the embodiment of the present invention;

[0032] Figure 3 This is the fitting result of the thickness control function of the standard sample of the tray in type C xylene in the embodiment of the present invention. DETAILED DESCRIPTION

[0033] The present invention will be further described below in conjunction with the accompanying drawings.

[0034] Example

[0035] (1) First, cut 54 pieces of polyester film of 100 mm × 100 mm.

[0036] (2) Wash the polyester film three times with ethanol and dry it in an oven at 55°C for 30 min.

[0037] (3) Deionized water and micro-90 cleaning solution were prepared in a volume ratio of 2:100, stirred clockwise for 15 minutes, and allowed to stand for 30 minutes before use.

[0038] (4) Dip a brush into the coating agent and apply it twice on the polyester film substrate.

[0039] (5) Dry the polyester film substrate coated with the release agent in an oven at 50° C. for 5 minutes.

[0040] (6) The polyester film substrates are marked as 10-1, 10-2, 10-3, 20-1, 20-2, 20-3, ..., 90-3, and each number corresponds to two polyester film substrates.

[0041] (7) Place the polyester film substrate on the upper, middle and lower trays of the equipment tooling respectively. Two sets of polyester film substrates are required to be placed on each tray and arranged symmetrically, with two 10-1s placed on the upper tray, two 10-2s placed on the middle tray, and two 10-3s placed on the lower tray, with the marked side facing up.

[0042] (8) The evaporation chamber of the equipment is loaded with 10 g of C-type polyparaxylene dimer, and a Parylene C film is deposited on a polyester film substrate.

[0043] (9) Prepare 20g, 30g, 40g, 50g, 60g, 70g, 80g and 90g of Parylene C film thickness control standard samples respectively.

[0044] (10) Use a cutter to cut off about 1 cm from one side of a Parylene C film thickness control standard sample.

[0045] (11) Manually peel off the Parylene C film layer on the marked surface along the edge cut by the scissors.

[0046] (12) Use a micrometer to randomly measure 6 points in the middle of the film layer and record them.

[0047] (13) The remaining 53 film thickness control standard samples were tested.

[0048] (14) Remove the maximum and minimum values ​​of each set of data, and then take the average value of the remaining 10 sets of data.

[0049] (15) Complete the preprocessing of the remaining data.

[0050] (16) Fit the thickness control function of the standard sample on the tray, and the results are as follows Figure 1 The results are shown.

[0051] (17) The thickness control function of the standard sample of the pallet is fitted, and the results are as follows: Figure 2 The results are shown.

[0052] (18) Fit the thickness control function of the standard pallet sample, and the results are as follows: Figure 3 The results are shown.

[0053] (19) The error of the thickness control function was analyzed.

[0054] (20) The thickness of Parylene C film at dimer loadings of 15 g, 75 g, and 100 g was compared and verified, thus completing the standard construction.

[0055] The present invention provides a method for controlling the film thickness of a C-type polyparaxylene film, which can effectively solve the above-mentioned problems. By optimizing the vapor deposition process parameters, including but not limited to key factors such as precursor gas flow rate, deposition temperature, and reaction chamber pressure, the present invention achieves a high degree of controllability of the deposition thickness of the C-type polyparaxylene film. This technological advancement not only allows the film thickness to be precisely adjusted at the nanometer level, but also greatly improves the quality of the film layer, ensuring its uniformity and density, which is crucial to improving the performance of the final product.

[0056] In addition, the application of this technology has also brought about a significant improvement in production efficiency, reduced production costs, and broadened the application scenarios of C-type polyparaxylene film materials. For example, in microelectronics manufacturing, this high-quality film can be used as an effective insulating layer or protective layer to enhance the reliability and service life of the equipment; in the biomedical field, it can be used to manufacture implantable medical devices to improve their biocompatibility and functionality.

[0057] In conclusion, this invention not only promotes the development of materials science by improving the deposition technology of C-type polyparaxylene film, but also provides strong support for technological innovation in multiple industries. With the deepening of research and the continuous improvement of technology, it is expected that more new products based on this technology will be launched in the future, contributing to the progress of human society.

[0058] In the description of the present invention, it is necessary to understand that the terms "upper", "lower", "bottom", "top", "front", "back", "inside", "outside", "left", "right", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present invention.

[0059] Although the present invention is described herein with reference to specific embodiments, it should be understood that these embodiments are merely examples of the principles and applications of the present invention. It should therefore be understood that many modifications may be made to the exemplary embodiments and that other arrangements may be devised without departing from the spirit and scope of the present invention as defined by the appended claims. It should be understood that the different dependent claims and features described herein above may be combined in a manner different from that described in the original claims. It will also be understood that the features described in conjunction with the individual embodiments may be used in other embodiments described above.

Claims

1. A method for controlling the film thickness of a C-type polyparaxylene film, characterized in that: The steps include: S1, preparing multiple polyester film substrates; S2, preparing the polyester film substrate to obtain a Parylene C film thickness control standard sample; S3, measuring the thickness of the Parylene C film thickness control standard sample; S4, placing the p-xylene Parylene C film thickness control standard samples on the upper layer, middle layer and lower layer of the deposition rotary tooling, respectively, calculating and establishing a model for each layer according to the p-xylene Parylene C film thickness, position, and dimer loading data, to obtain a thickness control model; S5. Controlling the thickness of the Parylene C film according to the thickness control model of each layer.

2. The method for controlling the film thickness of a C-type polyparaxylene film according to claim 1, characterized in that: In S1, the preparation of the polyester film substrate comprises the following steps: A1. Cutting polyester film; A2. Wash the polyester film three times with ethanol and dry it in an oven at 50-60°C for 28-32 minutes; A3. Apply the release agent to all sides of the polyester film substrate, twice on each side; A4. Dry the polyester film coated with the release agent at 45-55° C. for 4-6 minutes to obtain the polyester film substrate.

3. The method for controlling the film thickness of a C-type polyparaxylene film according to claim 2, characterized in that: In A1, the size of the polyester film after cutting is (100±1) mm×(100±1) mm.

4. The method for controlling the film thickness of a C-type polyparaxylene film according to claim 2, characterized in that: In A3, the preparation of the release agent comprises the following steps: B1. Mix deionized water and micro-90 cleaning solution in a volume ratio of 2:

100. B2. Stir for 13 to 17 minutes and let stand for 25 to 35 minutes to obtain the release agent.

5. The method for controlling the film thickness of a C-type polyparaxylene film according to claim 1, characterized in that: In S2, the preparation of the Parylene C film thickness control standard sample comprises the following steps: C1. placing the polyester film substrate on the upper, middle and lower trays of the deposition rotary tooling respectively; C2. Load C-type poly(p-xylene) dimer and deposit a Parylene C film on a polyester film substrate to obtain the Parylene C film thickness control standard sample.

6. The method for controlling the film thickness of a C-type polyparaxylene film according to claim 5, characterized in that: In C1, two sheets of the polyester film substrate are placed on each tray and arranged symmetrically.

7. The method for controlling the film thickness of a C-type polyparaxylene film according to claim 1, characterized in that: In S3, the preparation of the Parylene C film thickness control standard sample comprises the following steps: D1. Subtract 0.9-1.1 cm from one side of the Parylene C film thickness control standard sample using a cutting machine; D2. Manually peel off the Parylene C film along the cutting edge; D3. Use a micrometer to randomly measure 5 to 7 points in the middle of the film layer to complete the thickness measurement.

8. The method for controlling the film thickness of a C-type polyparaxylene film according to claim 1, characterized in that: The second-order polynomial thickness control mathematical model for the upper layer of the deposition rotary tooling is: τ=0.265m-0.0000742m 2 -0.432, where: τ is the film thickness in μm, and m is the dimer loading in g.

9. The method for controlling the film thickness of a C-type polyparaxylene film according to claim 1, characterized in that: The second-order polynomial thickness control mathematical model of the layer in the deposition rotary tooling is: τ=0.253m-0.0000481m 2 +0.143 Where: τ is the film thickness in μm, m is the dimer loading in g.

10. The method for controlling the film thickness of a C-type polyparaxylene film according to claim 1, characterized in that: The second-order polynomial thickness control mathematical model of the layer in the deposition rotary tooling is: τ=0.27m+0.000186m 2 +0.419 Where: τ is the film thickness in μm, m is the dimer loading in g.