In-line wall biased magnetron sputter coating apparatus and method
By installing ceramic insulators and a vacuum transition cavity in the magnetron sputtering coating equipment on the inner wall of the tube, independent bias control of the sample tube is achieved, solving the problem that the sample to be coated cannot be independently biased, improving the deposition quality and density of the film, and regulating the physicochemical properties and surface roughness of the film.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- WUHAN UNIV
- Filing Date
- 2023-05-25
- Publication Date
- 2026-07-14
AI Technical Summary
In magnetron sputtering deposition on the inner wall of a tube, the sample to be deposited is directly fixed on the vacuum transition cavity, and a bias voltage cannot be applied independently, which affects the deposition quality and properties of the thin film.
By installing a ceramic insulator at the other end of the sample tube, the sample tube is insulated. Combined with a vacuum transition cavity and a bias power supply, the charge state of the sample tube can be independently controlled, and a positive bias voltage can be applied to regulate the thin film deposition.
Independent bias control of the sample tube was achieved, which improved the deposition rate, quality and density of the thin film, reduced surface defects, and enabled the deposition of thin films with different properties, as well as the control of physicochemical properties and surface roughness.
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Figure CN116590678B_ABST
Abstract
Description
Technical Field
[0001] This application relates to the technical field of magnetron sputtering coating, and more particularly to a magnetron sputtering coating apparatus and method for inner wall of a tube with bias voltage. Background Technology
[0002] As is known in the art, magnetron sputtering deposition on the inner wall of a tube is a surface thin film technology, and its equipment is widely used to deposit target thin films on the inner wall of tubular samples. In the process of magnetron sputtering deposition on the inner wall of a tube, the prepared target material (usually metal or ceramic) is first placed in the sample tube to be deposited under vacuum. An external solenoid provides a parallel magnetic field to the surface of the target material. Then, by applying a certain negative voltage to the target material, a plasma field is formed inside the sample tube. Gas ions bombard the surface of the target material, and the particles generated by gas ion sputtering are deposited on the inner wall of the sample tube, ultimately forming a uniform thin film on the inner wall of the tube.
[0003] In conventional magnetron sputtering, bias voltage is one of the crucial parameters for regulating the deposition rate and quality of the film. Bias voltage refers to the voltage applied to the substrate (sample to be deposited) during magnetron sputtering. When a negative bias voltage is applied, the substrate surface attracts cations and neutral atoms from the target material. These particles bombard the substrate surface with higher energy, promoting the deposition rate and quality. Simultaneously, negative bias voltage also increases the ionization rate and activity of metal atoms, promoting film formation and improving adhesion. Furthermore, negative bias voltage effectively reduces the bombardment of the substrate by electrons and ions generated in the target material, avoiding excessive heat generation and damage to the substrate surface. Therefore, a suitable bias voltage in magnetron sputtering can improve the deposition rate and quality of the film while protecting the substrate surface, resulting in a high-quality film.
[0004] During magnetron sputtering, when a positive bias is applied to the sample, ions shuttle between the target and the deposition surface. During this process, some target ions collide with the deposition surface and interact with other atoms and ions, thus affecting the deposition and properties of the thin film. Simultaneously, some positive ions may bounce back to the target, a phenomenon known as sputtering, which is also a significant factor affecting film deposition and properties. Therefore, a positive bias can increase the ion bombardment energy, promoting ion deposition on the substrate surface. This helps improve the density and adhesion of the film, as well as enhance its thickness and uniformity. Thus, factors such as ion bombardment energy, ion bombardment angle, and sputtering need to be considered comprehensively to obtain optimal film quality and performance.
[0005] The actual effect depends on the specific experimental conditions and objectives. Potential impacts include:
[0006] A. Increase deposition rate: Positive bias can increase the electron energy in the plasma, thereby increasing the deposition rate.
[0007] B. Changing the properties of the deposited film: By adjusting the positive bias voltage, the energy distribution and trajectory of electrons in the plasma can be changed, thereby affecting the structure and properties of the deposited film.
[0008] C. Improve film quality: Positive bias can reduce the number of surface defects and impurities, thereby improving the quality of deposited films.
[0009] However, in current magnetron sputtering coating on the inner wall of a tube, the sample to be coated is directly fixed on the vacuum transition cavity and in direct contact with the ground, making it impossible to directly and independently feed in a bias voltage. Therefore, unlike conventional magnetron sputtering, where the sample to be coated is clamped on a sample holder insulated from the cavity, it is not possible to achieve independent input bias voltage for the sample to be coated. Summary of the Invention
[0010] In view of this, this application provides a magnetron sputtering coating apparatus and method for the inner wall of a tube with bias voltage, which can more easily achieve the input bias voltage to the sample tube by adding a ceramic insulating component to make the sample tube to be coated insulated, thereby controlling the surface charge state of the sample tube.
[0011] In a first aspect, this application provides a biased magnetron sputtering coating apparatus for the inner wall of a tube, comprising:
[0012] A vacuum electrode is installed at one end of the sample tube to be coated, and the electrode is connected to the target material placed in the sample tube.
[0013] A ceramic insulating component is installed at the other end of the sample tube;
[0014] A vacuum transition chamber is used to introduce or extract process gas into the sample tube to maintain the gas pressure inside the sample tube within the pressure range required for glow discharge.
[0015] An electromagnet is used to generate a magnetic field on the surface of the target material when energized.
[0016] The sputtering power supply is electrically connected at one end to the vacuum electrode and at the other end to the vacuum transition cavity;
[0017] A bias power supply, one end of which is electrically connected to the sample tube, and the other end of which is electrically connected to the vacuum transition chamber;
[0018] The sputtering power supply provides power to the target material. Under the action of the magnetic field, atoms on the surface of the target material are sputtered by gas ions. At the same time, the bias power supply provides a positive bias to the sample tube, thereby causing particles to deposit into a film on the inner wall of the sample tube.
[0019] Optionally, the vacuum transition chamber is provided with an inlet pipe for introducing process gas.
[0020] Optionally, the vacuum transition chamber is provided with an extraction pipeline for extracting process gases.
[0021] Optionally, the vacuum transition cavity is provided with a measurement interface for measuring the vacuum level.
[0022] Optionally, the vacuum transition cavity is grounded.
[0023] Optionally, the ceramic insulating component includes a first vacuum flange, a tubular ceramic component, and a second vacuum flange connected in sequence, with its internal space achieving vacuum sealing, and the first vacuum flange and the second vacuum flange being electrically insulated.
[0024] Secondly, this application provides a coating method using the biased magnetron sputtering coating equipment for the inner wall of a tube as described above, comprising:
[0025] Process gas is introduced into the vacuum transition cavity and extracted from the vacuum transition cavity, so that the gas pressure in the sample tube to be plated is within the gas pressure range required for glow discharge.
[0026] The sputtering power supply supplies power to the target material, the process gas is ionized, and positive ions bombard the target material surface under the action of an electromagnetic field to form sputtered particles;
[0027] By providing a positive bias voltage to the sample tube using the bias power supply, and simultaneously applying an independently controllable positive bias voltage to the sample tube while sputtered particles from the target form a film on the sample surface, it is possible to deposit thin films with different properties and better quality. The physicochemical properties and surface roughness of the thin film can be controlled. This results in thin films with fewer defects, or the deposition of dense / columnar multilayer composite thin films. The above-described solution of the present invention includes at least the following beneficial effects:
[0028] Under suitable process gas pressure and magnetic field, the charge state between the target material and the sample tube to be coated is independently controlled, achieving magnetron sputtering coating. During the sputtering coating process, an independently controlled positive pressure is applied to the sample tube, allowing for the deposition of thin films with different properties and better quality. The physicochemical properties and surface roughness of the thin films can be controlled. Process development can lead to the preparation of thin films with denser structures and better crystallinity, as well as thin films with smoother surfaces and fewer defects. Alternatively, it can allow for the deposition of dense / columnar composite thin films using different processes. Attached Figure Description
[0029] The technical solution and other beneficial effects of this application will become apparent from the following detailed description of specific embodiments in conjunction with the accompanying drawings.
[0030] Figure 1 This is a schematic diagram of a vacuum coating device for the inner wall of a tube with a bias device, as disclosed in an embodiment of this application.
[0031] Figure 2 This is a plan view of the ceramic insulating component structure disclosed in the embodiments of this application;
[0032] Figure 3 This is an example of a three-dimensional cross-sectional view of a vacuum coating apparatus for the inner wall of a tube with a bias device, as disclosed in the embodiments of this application.
[0033] Figure 4 This is an example of a TiZrV monolayer thin film deposited as disclosed in the embodiments of this application;
[0034] Figure 5 This is an example of a dense TiZr film deposited according to the embodiments of this application.
[0035] Figure 6 Examples of deposited TiN columnar / dense multilayer films disclosed in the embodiments of this application.
[0036] The components in the diagram are labeled as follows:
[0037] 1-Vacuum electrode; 2-Sample tube; 3-Electromagnet; 4-Target material; 5-Evacuation line; 6-Inlet line; 7-Measurement interface; 8-Vacuum transition chamber; 9-Ceramic insulator; 10-Sputtering power supply; 11-Bias power supply; 12-First vacuum flange; 13-Tubular ceramic; 14-Second vacuum flange. Detailed Implementation
[0038] The technical solutions in the embodiments of this application will be clearly and completely described below with reference to the embodiments of this application. Obviously, the described embodiments are only some embodiments of this application, and not all embodiments. Based on the embodiments of this application, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this application.
[0039] In the description of this application, it should be understood that the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated. Therefore, features defined as "first" or "second" may explicitly or implicitly include one or more of the stated features. In the description of this application, "multiple" means two or more, unless otherwise explicitly specified.
[0040] In the description of this application, it should be noted that, unless otherwise expressly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection, an electrical connection, or a connection that allows communication between them; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication between two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this application according to the specific circumstances.
[0041] The following disclosure provides many different embodiments or examples for implementing different structures of this application. To simplify the disclosure, specific examples of components and arrangements are described below. Of course, these are merely examples and are not intended to limit the scope of this application. Furthermore, reference numerals and / or letters may be repeated in different examples; such repetition is for simplification and clarity and does not in itself indicate a relationship between the various embodiments and / or arrangements discussed. In addition, various specific examples of processes and materials are provided in this application, but those skilled in the art will recognize the application of other processes and / or the use of other materials.
[0042] Magnetron sputtering coating equipment
[0043] The biased magnetron sputtering coating apparatus for the inner wall of a tube disclosed in this application includes:
[0044] Vacuum electrode 1 is installed at one end of sample tube 2 to be plated, and target material 4 is placed inside the sample tube 2.
[0045] Ceramic insulating component 9 is installed at the other end of the sample tube 2.
[0046] The vacuum transition chamber 8 is used to introduce or extract process gas into the sample tube 2 to maintain the gas pressure inside the sample tube 2 within the gas pressure range required for glow discharge.
[0047] Electromagnet 3 is used to generate a magnetic field outside the sample tube 2 after being energized;
[0048] The sputtering power supply 10 is electrically connected at one end to the aforementioned vacuum electrode 1 and at the other end to the vacuum transition cavity 8.
[0049] The bias power supply 11 is electrically connected at one end to the sample tube 2 and at the other end to the vacuum transition chamber 8.
[0050] The sputtering power supply 10 provides power to the target material 4. Under the action of the magnetic field, the atoms on the surface of the target material 4 are sputtered by gas ions. At the same time, the bias power supply 11 provides a positive bias to the sample tube 2, thereby causing the particles to be deposited on the inner wall of the sample tube 2 to form a film.
[0051] Based on the preceding description of "vacuum transition chamber 8, used to introduce or extract process gas into the sample tube 2", those skilled in the art can directly and without doubt determine that the coating pipe, ceramic insulating component 9, and the interior of the vacuum transition chamber 8 form a complete and sealed vacuum space.
[0052] As an example, the vacuum transition chamber 8 is provided with an inlet pipe 6 for introducing process gas.
[0053] Thus, through the air inlet pipe 6, process gas can be easily introduced into the vacuum transition chamber 8.
[0054] As an example, the vacuum transition chamber 8 is provided with an extraction line 5 for extracting process gases.
[0055] Thus, through the extraction pipe 5, the process gas can be easily extracted from the vacuum transition chamber 8.
[0056] As an example, the vacuum transition cavity 8 is provided with a measurement interface 7 for measuring the vacuum level.
[0057] As an example, the aforementioned vacuum transition cavity 8 is grounded.
[0058] As an example, the ceramic insulator 9 includes a first vacuum flange 12, a tubular ceramic 13 and a second vacuum flange 14 connected in sequence, with its internal space being vacuum sealed, and the first vacuum flange 12 and the second vacuum flange 14 being electrically insulated.
[0059] Here, the first vacuum flange 12, the tubular ceramic 13, and the second vacuum flange 14 are connected in sequence to form a "sandwich" structural combination.
[0060] Magnetron sputtering coating method
[0061] This application provides a coating method using the biased magnetron sputtering coating equipment for the inner wall of a tube as described above, including:
[0062] Process gas is introduced into the vacuum transition chamber 8 and extracted from the vacuum transition chamber 8, so that the gas pressure in the sample tube 2 to be plated is within the gas pressure range required for glow discharge.
[0063] The sputtering power supply 10 supplies power to the target material 4. Under the action of the magnetic field, atoms on the surface of the target material 4 escape to form sputtered ions.
[0064] The bias power supply 11 provides a positive bias voltage to the sample tube 2, thereby causing the sputtered ions to deposit into a film on the inner wall of the sample tube 2.
[0065] It is worth adding that, in this coating method, in addition to the general control of process gas pressure, magnetic field strength, sputtering power supply 10 and other parameters, bias control in the vacuum coating technology of the inner wall of the tube can also be achieved by adjusting the voltage and frequency of the input bias power supply 11.
[0066] To more clearly illustrate the magnetron sputtering coating method, several common or widely used application scenarios are listed below. It should be noted that these common application scenarios should not be used as the basis for determining the essential features for understanding the technical problem claimed to be solved in this application; they are merely examples.
[0067] Example 1
[0068] Please refer to Figure 4 A 1m long, 30mm inner diameter stainless steel tube was used as sample tube 2. Sample tube 2 was ultrasonically cleaned for 30 minutes each in a water bath containing alkaline cleaning solution, alcohol, and deionized water, and then dried with dry nitrogen. A 2mm thick TiZrV target wire 4 was then inserted through the sample tube, with the tip of the target wire 4 connected to the vacuum electrode 1. The tube was then slowly lowered into the electromagnet 3, with one sealed end connected to the vacuum electrode 1 and the other end connected to the ceramic insulator 9. A pulsed DC sputtering power supply 10 was used as the sputtering power source for the target 4, with its negative terminal connected to the vacuum electrode 1 and its positive terminal connected to the vacuum transition cavity 8. A positive voltage power supply 11 was used as the bias power supply 11, with its positive terminal connected to the sample tube and its negative terminal connected to the vacuum transition cavity 8.
[0069] The molecular pump unit is turned on, and the vacuum transition chamber 8, ceramic insulating component 9, and the internal space of the sample tube are evacuated through the evacuation pipe by 1×10. -5 At Pa, the flow controller was turned on, and argon gas at 5 sccm was introduced through the injection pipe. At this time, the internal gas pressure was maintained at 1 Pa as observed at the vacuum detection port. The sputtering power supply 10 was set to output -600V and 5kHz, and the bias power supply 11 was set to output 80V. The coating was carried out for 5 hours. The TiZrV thin film on the inner wall of the tube was detected, and its cross-section showed a clear and dense structure.
[0070] Example 2
[0071] Please refer to Figure 5 A 1m long, 35mm inner diameter stainless steel tube was used as sample tube 2. Sample tube 2 was ultrasonically cleaned for 30 minutes each in a water bath containing alkaline cleaning solution, alcohol, and deionized water, and then dried with dry nitrogen. A 5mm diameter TiZr alloy target 4 was then inserted through the sample tube, with the top of target 4 connected to vacuum electrode 1. The tube was then slowly lowered into electromagnet 3, with one sealed end connected to vacuum electrode 1 and the other end connected to ceramic insulator 9. A pulsed DC sputtering power supply 10 was used as the sputtering power supply for target 4, with its negative terminal connected to vacuum electrode 1 and its positive terminal connected to vacuum transition cavity 8. A positive voltage power supply 11 was used as the bias power supply 11, with its positive terminal connected to the sample tube and its negative terminal connected to vacuum transition cavity 8.
[0072] The molecular pump unit was turned on, and the vacuum transition chamber 8, ceramic insulating component 9, and the internal space of the sample tube were evacuated through the evacuation pipe to a depth of 5×10 mm. -5 At Pa, the flow controller was turned on, and 8 sccm of argon gas was introduced through the injection pipe. At this time, the internal gas pressure was maintained at 1.5 Pa by the vacuum detection port. The sputtering power supply 10 was set to output -500V and 10kHz, and the bias power supply 11 was set to output 90V. The coating was carried out for 4 hours. The TiZr film on the inner wall of the tube was examined, and the cross-section of the film showed that the film had a distinctly dense structure. The thickness deviation of the film sample taken from the inner wall of the tube was within 10%.
[0073] Example 3
[0074] Please refer to Figure 6 A 1m long, 35mm inner diameter stainless steel tube was used as sample tube 2. Sample tube 2 was ultrasonically cleaned for 30 minutes each in a water bath containing alkaline cleaning solution, alcohol, and deionized water, and then dried with dry nitrogen. A 5mm diameter titanium target 4 was then inserted through the sample tube, with the top of the target 4 connected to the vacuum electrode 1. The tube was then slowly lowered into the electromagnet 3, with one sealed end connected to the vacuum electrode 1 and the other end connected to the ceramic insulator 9. A pulsed DC sputtering power supply 10 was used as the sputtering power supply for the target 4, with its negative terminal connected to the vacuum electrode 1 and its positive terminal connected to the vacuum transition cavity 8. A positive voltage power supply 11 was used as the bias power supply 11, with its positive terminal connected to the sample tube and its negative terminal connected to the vacuum transition cavity 8.
[0075] The molecular pump unit was turned on, and the vacuum transition chamber 8, ceramic insulating component 9, and the internal space of the sample tube were evacuated through the evacuation pipe to a depth of 5×10 mm. -5 At Pa, the flow controller was turned on, and 6 sccm of argon and 4 sccm of nitrogen were introduced through the gas injection pipe. At this time, the internal gas pressure was maintained at 1.5 Pa by the vacuum detection port. The sputtering power supply 10 was set to output -600V and 10kHz, and the bias power supply was not turned on. The deposition time was 3 hours, and the first TiN film was deposited. The sputtering power supply was kept on, and the bias power supply 11 was turned on to output 80V. The deposition time was 2 hours, and the second TiN film was deposited. The TiN film on the inner wall of the tube was examined. The cross-section of the film showed that the film thickness was about 1.2 μm, and it had a clear two-layer structure. The first layer was a columnar structure, and the second layer was a dense structure.
[0076] The above description is merely a preferred embodiment of this application, but the scope of protection of this application is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the scope of the technology disclosed in this application should be included within the scope of protection of this application.
Claims
1. A magnetron sputtering coating apparatus for the inner wall of a tube with bias voltage, characterized in that, include: A vacuum electrode is installed at one end of the sample tube to be coated, and the electrode is connected to the target material placed inside the sample tube. A ceramic insulating component is installed at one end in the sample tube and at the other end in the vacuum transition chamber; the ceramic insulating component includes a first vacuum flange, a tubular ceramic component, and a second vacuum flange connected in sequence, and its internal space is vacuum sealed, while the first vacuum flange and the second vacuum flange are electrically insulated. A vacuum transition chamber is used to introduce or extract process gas into the sample tube to maintain the gas pressure inside the sample tube within the pressure range required for glow discharge. An electromagnet is used to generate a magnetic field on the surface of the target material when energized. The sputtering power supply is electrically connected at one end to the vacuum electrode and at the other end to the vacuum transition cavity; A bias power supply, one end of which is electrically connected to the sample tube, and the other end of which is electrically connected to the vacuum transition chamber; In this process, the sputtering power supply powers the target material, causing the process gas to ionize into positive ions. Under the influence of an electromagnetic field, the positive ions bombard the surface of the target material, sputtering particles from the target material to form a film on the sample surface. Simultaneously, the bias power supply provides a positive bias voltage to the sample tube, thereby further controlling the deposition of particles on the inner wall of the sample tube to form a film.
2. The biased magnetron sputtering coating equipment for the inner wall of a tube according to claim 1, characterized in that, The vacuum transition cavity is equipped with an inlet pipe for introducing process gas.
3. The biased magnetron sputtering coating equipment for the inner wall of a tube according to claim 1, characterized in that, The vacuum transition chamber is equipped with an extraction pipeline for extracting process gases.
4. The biased magnetron sputtering coating equipment for the inner wall of a tube according to claim 1, characterized in that, The vacuum transition cavity is equipped with a measurement interface for measuring vacuum level.
5. The biased magnetron sputtering coating equipment for the inner wall of a tube according to claim 1, characterized in that, The vacuum transition cavity is grounded.
6. A method for coating using the biased magnetron sputtering coating equipment for the inner wall of a pipe as described in claim 1, characterized in that, include: Process gas is introduced into the vacuum transition cavity and extracted from the vacuum transition cavity, so that the gas pressure in the sample tube to be plated is within the gas pressure range required for glow discharge. The sputtering power supply supplies power to the target material, causing the process gas to ionize into positive ions. Under the action of the electromagnetic field, the positive ions bombard the surface of the target material, and the target material sputters particles to form a film on the sample surface. The bias power supply provides a positive bias voltage to the sample tube, thereby further controlling the deposition of particles on the inner wall of the sample tube to form a film.