An air-breathing membrane and a method of making the same

By embedding a getter film inside the stainless steel VC cavity and depositing a multilayer alloy film using magnetron sputtering, the performance degradation problem of stainless steel VC during high-temperature aging is solved, significantly extending its service life.

CN117535625BActive Publication Date: 2025-11-18GEMCH MATERIAL TECH SUZHOU
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Patent Information

Application Number
CN202311069850.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-08-24
Publication Date
2025-11-18
Estimated Expiration
2043-08-24

AI Technical Summary

Technical Problem

Stainless steel VC suffers severe performance degradation during high-temperature aging. The internal liquid reacts chemically with the contact materials, leading to a decrease in vacuum and performance failure.

Method used

A gas-absorbing film is built into the stainless steel VC cavity. Multilayer alloy films, including materials such as NiV, Pd, and TiZr, are deposited by magnetron sputtering to form a gas-absorbing film to prevent gas leakage.

Benefits of technology

It significantly improves the service life of stainless steel VC, increasing the aging time at 150℃ from 12 hours to over 100 hours.

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Abstract

The application discloses an air absorption film and a preparation method thereof, relates to the field of film coating, and aims to solve the problem of avoiding the decrease of vacuum degree of a VC cavity, and the technical scheme is as follows: a substrate is subjected to first layer film deposition, the target material is a NiV alloy target with a purity of 99.95%, or a NiCr alloy target with a purity of 99.9%, or an AgNi alloy target with a purity of 99.99%; then, second layer film deposition is carried out, the target material is a Pd target with a purity of 99.95%; then, third layer film deposition is carried out, the target material is a TiZr alloy target with a purity of 99.9%; then, fourth layer film deposition is carried out, the target material is a Pd target with a purity of 99.95%; then, fifth layer film deposition is carried out, the target material is a TiZr alloy target with a purity of 99.9%; then, sixth layer film deposition is carried out, the target material is a Pd target with a purity of 99.95%; and then, seventh layer film deposition is carried out, the target material is a NiV alloy target with a purity of 99.95%, or a NiCr alloy target with a purity of 99.9%, or an AgNi alloy target with a purity of 99.99%. The air absorption film and the preparation method thereof can guarantee the performance of the VC cavity.
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Description

Technical Field

[0001] This invention relates to the field of coating, and more specifically, to a gas-absorbing thin film and a method for preparing the same. Background Technology

[0002] As mobile phone manufacturers continuously pursue higher performance, they demand lighter, thinner, and faster phones. "Fast" refers to faster processing speeds, leading to increasingly higher power consumption from the processing chips in mobile phones. This high power consumption inevitably causes overheating issues, thus placing increasingly stringent technical requirements on high heat flux density VC liquid cooling vapor chambers (vacuum chamber heat exchanger technology).

[0003] Traditional vacuum chambers (VCs) use copper strips, which have good thermal conductivity. However, copper strips are too soft and lack sufficient support strength when thin, making it impossible to achieve thicknesses below 0.25mm. Therefore, stainless steel VC technology emerged. During high-temperature aging tests at 150℃, it was found that the performance degradation of stainless steel VCs was significantly worse than that of copper VCs. After 12 hours of aging, almost all VCs failed. Analysis showed that the liquid (water) inside the stainless steel VC reacts chemically with the contact materials, producing hydrogen gas. This leads to a decrease in the vacuum level of the VC chamber, severe performance degradation, and even failure.

[0004] Therefore, a new solution is needed to address this problem. Summary of the Invention

[0005] To address the shortcomings of existing technologies, the present invention aims to provide an air-absorbing membrane and its preparation method, which embeds the air-absorbing material within a stainless steel cavity, effectively solving the problem and significantly improving service life.

[0006] The above-mentioned technical objective of the present invention is achieved through the following technical solution: a method for preparing an air-absorbing film, comprising the following steps,

[0007] S1: Preparation of the substrate, including copper sheets, titanium sheets, aluminum sheets or copper wires, titanium wires, and aluminum wires;

[0008] S2: Clean and dry the substrate to obtain a clean substrate;

[0009] S3: Perform plasma cleaning on the substrate;

[0010] S4: Deposit the first thin film on the substrate, using a NiV alloy target with a purity of 99.95%, a NiCr alloy target with a purity of 99.9%, or an AgNi alloy target with a purity of 99.99%.

[0011] S5: Deposit a second thin film on the substrate, using a Pd target with a purity of 99.95%;

[0012] S6: Deposit a third thin film on the substrate using a TiZr alloy target with a purity of 99.9%;

[0013] S7: The substrate is subjected to a fourth thin film deposition, and the target material is a Pd target with a purity of 99.95%;

[0014] S8: Deposit the fifth thin film on the substrate using a TiZr alloy target with a purity of 99.9%;

[0015] S9: The substrate is subjected to a sixth thin film deposition, and the target material is a Pd target with a purity of 99.95%;

[0016] S10: Deposit a seventh thin film on the substrate, using a NiV alloy target with a purity of 99.95%, a NiCr alloy target with a purity of 99.9%, or an AgNi alloy target with a purity of 99.99%.

[0017] The present invention is further configured such that the thin film deposition method is magnetron sputtering.

[0018] The present invention is further configured such that, in S4, the thin film deposition power density is 4 W / cm². 2 Ar gas flow rate 30 sccm, deposition time 30 s.

[0019] The present invention is further configured such that, in S5, the thin film deposition power density is 2 W / cm². 2 Ar gas flow rate 30 sccm, deposition time 80 s.

[0020] The present invention is further configured such that, in S6, the thin film deposition power density is 3 W / cm². 2 Ar gas flow rate 30 sccm, deposition time 20 s.

[0021] The present invention is further configured such that, in S7, the thin film deposition power density is 2 W / cm². 2 Ar gas flow rate 30 sccm, deposition time 100 s.

[0022] The present invention is further configured such that, in S8, the thin film deposition power density is 3 W / cm². 2 Ar gas flow rate 30 sccm, deposition time 20 s.

[0023] The present invention is further configured such that, in S9, the thin film deposition power density is 2 W / cm². 2 Ar gas flow rate 30 sccm, deposition time 120 s.

[0024] The present invention is further configured such that, in S10, the thin film deposition power density is 4 W / cm². 2Ar gas flow rate 30 sccm, deposition time 10 s.

[0025] The present invention also provides an air-absorbing film, which is obtained by the above-described preparation method.

[0026] In summary, the present invention has the following beneficial effects: after the gas-absorbing film prepared by the preparation process of the present invention is placed in the VC cavity, the aging time at 150°C is increased from 12 hours to more than 100 hours, thus improving the service life. Detailed Implementation

[0027] The present invention will now be described in detail with reference to the embodiments.

[0028] This invention provides a novel method for manufacturing an air-absorbing film, comprising the following steps:

[0029] S1: Preparation of the substrate, including copper sheets, titanium sheets, aluminum sheets or copper wires, titanium wires, aluminum wires, substrate composition and form including but not limited to these.

[0030] S2: The substrate is cleaned using industrial alcohol as the cleaning solution and an ultrasonic cleaner as the cleaning equipment. After ultrasonic cleaning, the substrate is removed and wiped dry with a dust-free cloth to obtain a clean substrate.

[0031] S3: The substrate is subjected to plasma cleaning. The plasma cleaning working pressure is 10 Pa, the gas is 99.999% high-purity argon, the voltage is 100 V, and the cleaning time is 3 minutes.

[0032] S4: Deposit the first thin film on the substrate using magnetron sputtering. The target material is a 99.95% pure NiV alloy target, a 99.9% pure NiCr alloy target, or a 99.99% pure AgNi alloy target, with a power density of 4 W / cm². 2 Ar gas flow rate 30 sccm, deposition time 30 s.

[0033] S5: A second thin film is deposited on the substrate using magnetron sputtering with a 99.95% pure Pd target and a power density of 2 W / cm³. 2 Ar gas flow rate 30 sccm, deposition time 80 s.

[0034] S6: A third thin film is deposited on the substrate using magnetron sputtering with a TiZr alloy target of 99.9% purity and a power density of 3 W / cm³. 2 Ar gas flow rate 30 sccm, deposition time 20 s.

[0035] S7: Deposit the fourth thin film on the substrate using magnetron sputtering with a 99.95% pure Pd target and a power density of 2 W / cm³. 2 Ar gas flow rate 30 sccm, deposition time 100 s.

[0036] S8: Deposit the fifth thin film on the substrate using magnetron sputtering with a TiZr alloy target of 99.9% purity and a power density of 3 W / cm³. 2 Ar gas flow rate 30 sccm, deposition time 20 s.

[0037] S9: A sixth thin film is deposited on the substrate using magnetron sputtering with a 99.95% pure Pd target and a power density of 2 W / cm³. 2 Ar gas flow rate 30 sccm, deposition time 120 s.

[0038] S10: Deposit the seventh thin film on the substrate using magnetron sputtering. The target material is a NiV alloy target with a purity of 99.95%, a NiCr alloy target with a purity of 99.9%, or an AgNi alloy target with a purity of 99.99%, and the power density is 4 W / cm². 2 Ar gas flow rate 30 sccm, deposition time 10 s.

[0039] Specific implementation examples:

[0040] Example 1:

[0041] S1: Prepare copper sheets, 50*50*0.1mm in size.

[0042] S2: The substrate is cleaned using industrial alcohol as the cleaning solution and an ultrasonic cleaner as the cleaning equipment. After ultrasonic cleaning, the substrate is removed and wiped dry with a dust-free cloth to obtain a clean substrate.

[0043] S3: The substrate is subjected to plasma cleaning. The plasma cleaning working pressure is 10 Pa, the gas is 99.999% high-purity argon, the voltage is 200 V, and the cleaning time is 3 minutes.

[0044] S4: Deposit the first thin film on the substrate using magnetron sputtering with a 99.95% pure NiV alloy target and a power density of 5 W / cm³. 2 Ar gas flow rate 30 sccm, deposition time 50 s.

[0045] S5: A second thin film is deposited on the substrate using magnetron sputtering with a 99.95% pure Pd target and a power density of 5 W / cm³. 2Ar gas flow rate 40 sccm, deposition time 100 s.

[0046] S6: A third thin film is deposited on the substrate using magnetron sputtering with a TiZr alloy target of 99.9% purity and a power density of 3 W / cm³. 2 Ar gas flow rate 30 sccm, deposition time 50 s.

[0047] S7: Deposit the fourth thin film on the substrate using magnetron sputtering with a 99.95% pure Pd target and a power density of 5 W / cm³. 2 Ar gas flow rate 40 sccm, deposition time 100 s.

[0048] S8: Deposit the fifth thin film on the substrate using magnetron sputtering with a TiZr alloy target of 99.9% purity and a power density of 3 W / cm³. 2 Ar gas flow rate 30 sccm, deposition time 50 s.

[0049] S9: A sixth thin film is deposited on the substrate using magnetron sputtering with a 99.95% pure Pd target and a power density of 5 W / cm³. 2 Ar gas flow rate 40 sccm, deposition time 100 s.

[0050] S10: Deposit the seventh thin film on the substrate using magnetron sputtering with a 99.99% AgNi alloy target and a power density of 3 W / cm³. 2 Ar gas flow rate 50 sccm, deposition time 10 s.

[0051] Example 2:

[0052] S1: Prepare titanium sheets, 50*50*0.1mm in size.

[0053] S2: The substrate is cleaned using industrial alcohol as the cleaning solution and an ultrasonic cleaner as the cleaning equipment. After ultrasonic cleaning, the substrate is removed and wiped dry with a dust-free cloth to obtain a clean substrate.

[0054] S3: The substrate is subjected to plasma cleaning. The plasma cleaning working pressure is 30Pa, the gas is 99.999% high-purity argon, the voltage is 200V, and the cleaning time is 5 minutes.

[0055] S4: The substrate is subjected to the first thin film deposition, which is performed by magnetron sputtering using a NiCr alloy target with a purity of 99.9% and a power density of 4 W / cm³. 2 Ar gas flow rate 30 sccm, deposition time 50 s.

[0056] S5: A second thin film is deposited on the substrate using magnetron sputtering with a 99.95% pure Pd target and a power density of 5 W / cm³. 2 Ar gas flow rate 40 sccm, deposition time 80 s.

[0057] S6: Deposit a third thin film on the substrate using magnetron sputtering with a TiZr alloy target of 99.9% purity and a power density of 2 W / cm³. 2 Ar gas flow rate 30 sccm, deposition time 50 s.

[0058] S7: Deposit the fourth thin film on the substrate using magnetron sputtering with a 99.95% pure Pd target and a power density of 5 W / cm³. 2 Ar gas flow rate 40 sccm, deposition time 200 s.

[0059] S8: Deposit the fifth thin film on the substrate using magnetron sputtering with a TiZr alloy target of 99.9% purity and a power density of 2 W / cm³. 2 Ar gas flow rate 30 sccm, deposition time 50 s.

[0060] S9: A sixth thin film is deposited on the substrate using magnetron sputtering with a 99.95% pure Pd target and a power density of 5 W / cm³. 2 Ar gas flow rate 40 sccm, deposition time 300 s.

[0061] S10: Deposit the seventh thin film on the substrate using magnetron sputtering with a 99.99% AgNi alloy target and a power density of 3 W / cm³. 2 Ar gas flow rate 60 sccm, deposition time 15 s.

[0062] Thickness and aging tests were conducted on Examples 1 and 2, and the test results are shown in Table 1 below.

[0063] Table 1: Thickness and Aging Test Results

[0064] Case Total film thickness 150℃ aging test Implementation Case 1 3.2um 100H Implementation Case 2 5.9um 120H

[0065] The above description is merely a preferred embodiment of the present invention. The scope of protection of the present invention is not limited to the above embodiments. All technical solutions falling within the scope of the present invention's concept are within the scope of protection of the present invention. It should be noted that for those skilled in the art, any improvements and modifications made without departing from the principles of the present invention should also be considered within the scope of protection of the present invention.

Claims

1. A method for preparing an air-absorbing membrane, characterized in that: Includes the following steps, S1: Preparation of the substrate, including copper sheets, titanium sheets, aluminum sheets or copper wires, titanium wires, and aluminum wires; S2: Clean and dry the substrate to obtain a clean substrate; S3: Perform plasma cleaning on the substrate; S4: Deposit the first thin film on the substrate, using a NiV alloy target with a purity of 99.95%, a NiCr alloy target with a purity of 99.9%, or an AgNi alloy target with a purity of 99.99%. S5: Deposit a second thin film on the substrate, using a Pd target with a purity of 99.95%; S6: Deposit a third thin film on the substrate using a TiZr alloy target with a purity of 99.9%; S7: Deposit the fourth thin film on the substrate, using a Pd target with a purity of 99.95%; S8: Deposit the fifth thin film on the substrate, using a TiZr alloy target with a purity of 99.9%; S9: The substrate is subjected to a sixth thin film deposition, and the target material is a Pd target with a purity of 99.95%; S10: Deposit a seventh thin film on the substrate, using a NiV alloy target with a purity of 99.95%, a NiCr alloy target with a purity of 99.9%, or an AgNi alloy target with a purity of 99.99%.

2. The method for preparing an air-absorbing film according to claim 1, characterized in that: The thin films were all deposited using magnetron sputtering.

3. The method for preparing an air-absorbing film according to claim 1 or 2, characterized in that: In S4, the thin film deposition power density is 4 W / cm². 2 Ar gas flow rate 30 sccm, deposition time 30 s.

4. The method for preparing an air-absorbing film according to claim 1 or 2, characterized in that: In S5, the thin film deposition power density is 2 W / cm². 2 Ar gas flow rate 30 sccm, deposition time 80 s.

5. A method for preparing an air-absorbing film according to claim 1 or 2, characterized in that: In S6, the thin film deposition power density is 3 W / cm². 2 Ar gas flow rate 30 sccm, deposition time 20 s.

6. A method for preparing an air-absorbing film according to claim 1 or 2, characterized in that: In S7, the thin film deposition power density is 2 W / cm². 2 Ar gas flow rate 30 sccm, deposition time 100 s.

7. The method for preparing an air-absorbing film according to claim 1 or 2, characterized in that: In S8, the thin film deposition power density is 3 W / cm². 2 Ar gas flow rate 30 sccm, deposition time 20 s.

8. A method for preparing an air-absorbing film according to claim 1 or 2, characterized in that: In S9, the thin film deposition power density is 2 W / cm². 2 Ar gas flow rate 30 sccm, deposition time 120 s.

9. A method for preparing an air-absorbing film according to claim 1 or 2, characterized in that: In S10, the thin film deposition power density is 4 W / cm². 2 Ar gas flow rate 30 sccm, deposition time 10 s.

10. A breathable membrane, characterized in that: Obtained by the preparation method described in any one of claims 1-9.

Citation Information

Patent Citations

  • Self-air-suction vacuum plating method

    CN101492807A

  • Thin-film getter with high gas absorption performance and preparation method thereof

    CN103182297A