Device for quickly and uniformly depositing thin film on inner wall of hollow cathode slender tube barrel part based on water cooling and magnetic confinement and use method

Abstract

The invention discloses a device for quickly and uniformly depositing a thin film on the inner wall of a hollow cathode slender tube barrel based on water cooling and magnetic confinement and a use method. The method belongs to the field of surface treatment. The method solves the problem that the hollow cathode target deforms and loses efficacy due to the fact that an existing method is limited by too high local temperature of a hollow cathode port. According to the device, water cooling and magnetic confinement are combined. The method comprises the following steps: cleaning the inner wall of the slender pipe barrel by self-glow; cleaning the inner wall of the slender pipe barrel part through hollow cathode enhanced glow; and depositing the inner wall of the pipe barrel. The hollow cathode target material is prevented from deforming and losing efficacy due to local overheating, the coating is more uniform in cooperation with a reciprocating mechanism, rapid and uniform deposition of a metal film on the inner wall, with the inner diameter being 6 mm, of a long and thin pipe barrel piece can be achieved, surface temperature changes can be controlled, and the mechanical property of the material is ensured. Compared with a traditional method, the ion source is generated in the tube, energy loss is avoided, the sputtering efficiency is improved, the coating uniformity can be regulated and controlled through reciprocating mechanism stepping sputtering, and the requirements of different industries for the thickness and uniformity of the film layer on the inner wall of the thin tube are met.

Description

Technical Field

[0001] The invention belongs to the field of surface treatment, and in particular relates to a device for quickly and evenly depositing a thin film on the inner wall of a hollow cathode slender tube based on water cooling and magnetic confinement and a method for using the device. Background Art

[0002] With the development of social science and technology, the demand for tubular materials in production and life is increasing, and the performance requirements for the inner wall film of slender tubular parts are getting higher and higher. Tubular materials play an important role in many key fields such as industrial manufacturing, medical care, electronic information, aerospace, and national defense. For example, sleeve bearings, oil pipelines, engine cylinders, cardiovascular stents, gun barrels, etc. Different application scenarios have different performance requirements for the inner tube coating. For example, the coating on the inner bore of artillery and firearm barrels needs to withstand extremely high temperatures, pressures and wear, and also needs to withstand the high temperature, high pressure, and high-speed gunpowder gas generated by the propellant. Therefore, great requirements are placed on the high temperature resistance, high pressure resistance, wear resistance and other properties of the inner wall coating of the tube in this case.

[0003] At present, the methods for coating the inner wall of slender tubes include immersion plating, electroplating, physical vapor deposition (PVD) and chemical vapor deposition (CVD), among which electroplating is the most widely used. However, with the development of science and technology, the coating formed by electroplating has poor bonding with the substrate and low density, which can hardly meet the growing demand. In addition, when electron beam coating is used, the coating uniformity is poor.

[0004] PVD technology has the advantages of being environmentally friendly and having a small restriction on the types of coatings that can be plated. However, in conventional PVD technology, arc ion plating or magnetron sputtering requires a built-in magnetic field and a water-cooling structure, and the volume and size of the target are limited. For slender tubes, it is impossible to build the target in while retaining a large target-substrate distance, and discharge is extremely difficult. Also due to the limitation of the space inside the tube, the remaining space after arc ion plating or magnetron sputtering target is very small, and the anode cannot be built in. Only a two-pole discharge method can be used, in which the target is connected to the positive electrode and the slender tube is connected to the positive electrode of the power supply, which limits the effective regulation of plasma energy. The hollow cathode discharge method is simple in device, and the target can be placed inside the slender tube while performing three-stage discharge. However, during the hollow cathode discharge process, the plasma is concentrated at the tube mouth, and the local plasma density and energy are very high, resulting in local overheating, deformation and failure of the hollow cathode target port. Therefore, how to reduce the plasma energy and heat input at the port position while maintaining the port plasma density and ionization rate, and enhance the cooling capacity of the hollow cathode target has become a key issue that limits the further application of this method in the field of inner wall coating of slender tubes, and it needs to be solved urgently. Summary of the invention

[0005] The purpose of the present invention is to solve the problem that the method of hollow cathode discharge coating in a slender tube is limited by the local excessive temperature of the hollow cathode port, which leads to deformation and failure of the hollow cathode target, and to provide a device and a method for quickly and uniformly depositing a thin film on the inner wall of a hollow cathode slender tube based on water cooling and magnetic constraint.

[0006] A device for rapidly and uniformly depositing a thin film on the inner wall of a hollow cathode slender tube based on water cooling and magnetic confinement, comprising a flange, a first connection joint, a second connection joint, a third connection joint, a first water pipe, a first water outlet pipe, a second water pipe, a second water outlet pipe, a third water pipe, a cathode tube, a hollow cathode target, a magnetic plug, a magnet, an anode tube, a slender tube, a reciprocating mechanism, a hollow cathode power supply and a bias power supply;

[0007] The first connecting joint, the second connecting joint, the third connecting joint, the first water pipe, the water outlet pipe, the second water pipe, the second water outlet pipe, the third water pipe, the cathode tube, the hollow cathode target, the magnetic plug and the magnet together constitute the water cooling system of the device;

[0008] One end of the first water pipe is connected to the flange, and the other end is connected to one end of the third water pipe through a first connection joint; the other end of the third water pipe is connected to one end of the second water pipe through a second connection joint; the other end of the second water pipe is a water outlet;

[0009] One end of the first water outlet pipe is connected to the flange, and the other end is connected to one end of the second water outlet pipe through a third connecting joint; the other end of the second water outlet pipe is the water inlet of the second water delivery pipe;

[0010] The hollow cathode target is connected to the cathode tube, and the magnetic plug is connected to the magnet and is placed inside the cathode tube and at the connection between the hollow cathode target and the cathode tube; the magnetic plug is sealed and connected to the cathode tube;

[0011] The slender tube member is sleeved with a second water pipe, a cathode tube, a hollow cathode target, a magnetic plug, a magnet and an anode tube; the second water pipe, the cathode tube, the hollow cathode target, the magnetic plug, the magnet, the anode tube and the slender tube member are coaxially arranged; the length of the cathode tube and the anode tube is longer than that of the slender tube member.

[0012] Furthermore, it also includes a first insulating bracket, a second insulating bracket and a base; the first insulating bracket is fixed on the base, and the first insulating bracket supports the second water pipe and the anode tube; the second insulating bracket is fixed on the reciprocating mechanism, and the second insulating bracket supports the slender tube member; the second insulating bracket is pulled by the reciprocating mechanism to drive the slender tube member to reciprocate axially.

[0013] Furthermore, the positive output end of the bias power supply is connected to the anode tube and grounded, and the negative output end is connected to the slender tube member; the negative output end of the hollow cathode power supply is connected to the hollow cathode target material, and the positive output end is connected to the anode tube and grounded.

[0014] Furthermore, the hollow cathode target is made of Cr, Ti, Ta, Cu, Ni, Zn, Nb, Sn, Al, Fe, Mg or Zr;

[0015] Alternatively, it may be a nickel-chromium alloy, a nickel-aluminum alloy, a nickel-iron alloy, a nickel-vanadium alloy, a titanium-aluminum alloy, a titanium-aluminum-silicon alloy, a gold-tin alloy, a gold-palladium alloy, a molybdenum-niobium alloy, a ruthenium-chromium alloy, a boron-iron alloy or a silicon-iron alloy.

[0016] Furthermore, the hollow cathode power supply and the bias power supply can both be a direct current power supply, a pulse power supply, a high voltage power supply, a radio frequency power supply, an intermediate frequency power supply or a high power pulse power supply.

[0017] The method for using the above-mentioned device for rapidly and uniformly depositing a thin film on the inner wall of a hollow cathode elongated tube based on water cooling and magnetic confinement is implemented by the following steps:

[0018] 1. Self-glow cleaning of the inner wall of slender tubes:

[0019] The vacuum chamber is evacuated, and working gas is introduced into the vacuum chamber to maintain the vacuum chamber pressure of 1-50 Pa, the positive output end of the bias power supply is connected to the anode tube and grounded, and the negative output end is connected to the slender tube member, the voltage of the bias power supply is controlled to be -50--2000V, and the duty cycle is 5%-100%, and the inner surface of the slender tube member is self-glowing and cleaned by plasma generated by the hollow cathode discharge effect, so as to obtain the slender tube member after self-glowing cleaning;

[0020] 2. Hollow cathode enhanced glow cleaning of the inner wall of slender tube parts:

[0021] The vacuum chamber pressure is maintained at 1-50 Pa, the negative output end of the hollow cathode power supply is connected to the hollow cathode target material, the positive output end is connected to the anode tube and grounded, and the negative output end of the bias power supply is connected to the slender tube after self-glow cleaning, and the positive output end is grounded, the voltage of the hollow cathode power supply is controlled to be 400-2000V, the peak current is 0.1-100A, and the duty cycle is 0.1%-100%, the voltage of the bias power supply is -50--2000V, and the duty cycle is 5%-100%, and the hollow cathode enhanced glow cleaning is performed to obtain the slender tube after hollow cathode enhanced glow cleaning;

[0022] 3. Deposition on the inner wall of tube and barrel:

[0023] The negative output end of the hollow cathode power supply is connected to the hollow cathode target material, the positive output end is connected to the anode tube, and the negative output end of the bias power supply is connected to the slender tube after the hollow cathode enhanced glow cleaning, and the positive output end is grounded. The vacuum chamber pressure is maintained at 1-50Pa, the voltage of the hollow cathode power supply is controlled to be 400-2000V, the peak current is 0.1-100A, and the duty cycle is 0.1%-100%. The voltage of the bias power supply is -0.1-500V and the duty cycle is 5%-100%. Hollow cathode coating is carried out to complete the rapid and uniform deposition of a thin film on the inner wall of the slender tube, and the method for using the device is completed.

[0024] Furthermore, the working gas in step 1 is argon (Ar), helium (He), neon (Ne), krypton (Kr), xenon (Xe), radon (Rn), oxygen (O 2 ), nitrogen (N 2 ), hydrogen (H 2 ), methane (CH4), hydrogen sulfide (H2S), ammonia (NH3), Ar+O 2 、Ar+N 2 、Ar+H 2 , O 2 +N 2 , O 2 +CH 4 , Ar+He or Ar+Xe; when the working gas is a mixed gas, the two are mixed in any ratio.

[0025] Furthermore, the self-glow cleaning time in step 1 is 5 minutes to 700 minutes.

[0026] Furthermore, the time for the hollow cathode enhanced glow cleaning in step 2 is 5 min to 700 min.

[0027] Furthermore, the time for hollow cathode coating in step three is 10 min to 700 min.

[0028] Principles and beneficial effects of the present invention:

[0029] 1. The present invention successfully achieves plasma discharge and efficient, controlled and uniform deposition of coatings in slender tubes by applying a magnetic field and water cooling inside the hollow cathode target, effectively solving the problem of deformation and failure of hollow cathode targets caused by local overheating of hollow cathode discharge in the tube. The principle is that hollow cathode technology is a method of achieving efficient ionization discharge by reciprocating oscillation of electrons between the cathode walls. The actual hollow cathode effect is mainly concentrated at the port. In the present invention, the end of the hollow cathode target is installed on the cathode tube with a built-in magnet, together forming a water-cooled + magnetically constrained hollow cathode target. The magnetic field generated by the magnet can further constrain the movement path of the plasma, increase the probability of plasma collision, ensure the discharge intensity while reducing the discharge difficulty and heat input; the water cooling system can transfer heat and cool the hollow cathode port through circulating water, while preventing the built-in magnet from overheating, while ensuring the high-density and high-ionization rate plasma discharge at the port, enhancing the temperature control ability of the hollow cathode target, and ensuring the long-term stable operation ability of the device, avoiding local overheating deformation failure at the port position; since the opening direction of the hollow cathode can be along the axis, and its anode can be coaxially placed in the tube, the plasma generated by the two can be controllably deposited on the inner wall of the slender tube under the action of the bias electric field between the anode and the slender tube, effectively realizing the regulation of plasma energy. At the same time, by pulling and moving the slender tube, effective contact between the discharge area and different positions of the inner wall of the tube can be achieved, and uniform and efficient deposition of coatings at all positions inside the slender tube can be achieved.

[0030] 2. The present invention successfully achieves stable discharge of hollow cathode target material through water cooling. At the same time, due to the introduction of magnetic field, the control of plasma orientation is greatly improved. The method proposed by the present invention can achieve rapid and uniform deposition on the inner wall of the slender tube, and at the same time helps to control the temperature change on the surface of the slender tube, ensuring the mechanical properties of the slender tube material.

[0031] 3. In terms of uniformity, in addition to magnetic confinement control, the present invention also performs step control of the reciprocating mechanism to achieve control of the residence time of the sputtering process, thereby playing an excellent role in the uniformity of the coating.

[0032] 4. The hollow cathode target of the present invention is detachable, which improves the efficiency of experiments and production to a certain extent, and is also very advantageous in terms of target utilization. In addition, the hollow cathode target is in close contact with the magnetic plug, which ensures the stability of the hollow cathode target during experiments and production, thereby improving the accuracy of sputtering coating to a certain extent, thereby having a positive impact on the uniformity of the coating.

[0033] 5. The inner diameter of the slender tube is relatively small. Due to the limitation of the space inside the tube, there is very little space left after the arc ion plating or magnetron sputtering target is built in. The anode cannot be built in. The only way is to use a two-pole discharge method in which the target is connected to the positive electrode and the slender tube is connected to the positive electrode of the power supply, which limits the effective regulation of the plasma energy. The hollow cathode discharge method is simple to install, and the target can be placed inside the slender tube and three-stage discharge can be performed simultaneously. However, during the hollow cathode discharge process, the plasma is concentrated at the tube mouth, and the local plasma density and energy are very high, resulting in local overheating, deformation and failure of the hollow cathode target port. In the method of using the device of the present invention, the failure of the hollow cathode target is avoided by water cooling, and the obtained coating is more uniform with the cooperation of magnetic confinement and reciprocating mechanism.

[0034] 6. The inner wall film thickness of the thin tubes used in different industries has different requirements and the requirements for uniformity are generally high, and the axial uniformity requirements need to be met. The ion source of the electron beam method is provided by the plasma generated by the pre-vacuum pressure hollow cathode plasma electron source. The traditional high-power pulsed magnetron sputtering method uses a flat target or a rod-shaped target, and the plated thin tube is placed in front of the flat target or the rod-shaped target is directly inserted into the thin tube for sputtering coating. However, there are many problems when using a flat target. For example, the utilization rate of sputtering ions is low and there is a significant difference in the thickness of the coating near the tube mouth and the coating in the middle of the tube. The thickness of the coating at the tube mouth is much larger, resulting in a difference in the uniformity of the coating on the inner wall of the thin tube, and the deposition rate is relatively slow. When a rod-shaped target is directly inserted into the inside of the thin tube, the temperature inside the tube cannot be well controlled during the ignition discharge, which may cause the target to melt excessively and directly contact the inner wall of the thin tube to cause a short circuit, and the direction of sputtering cannot be controlled during sputtering, resulting in low sputtering efficiency. The electron source emits electrons and accelerates to form an electron beam. These electron beams interact with the gas during transmission in the slender tube to generate ions. The injection of electron beams in this way is a key step in initiating gas ionization to form an ion source. In the method of using the device of the present invention, a hollow cathode target material is used inside the thin tube to complete all operations, that is, the ion source is generated inside the tube, avoiding the problem of energy loss in other operations, thus solving the problem of sputtering efficiency; and the uniformity of the coating can be effectively regulated by stepping sputtering through a reciprocating mechanism.

[0035] 7. Compared with traditional methods, such as electron beam method, high-power pulse magnetron sputtering method of planar target or rod-shaped target, the ion source of the present invention is generated in the tube, which avoids energy loss and improves sputtering efficiency. The coating uniformity can be regulated by reciprocating mechanism step sputtering to meet the requirements of different industries for the thickness and uniformity of the film layer on the inner wall of the capillary tube. The method of the present invention, with its advantages of high ionization rate, high deposition rate, etc., will become a reliable method in the field of coating the inner wall of the capillary tube in the future.

[0036] The invention is suitable for quickly and evenly depositing a thin film on the inner wall of a slender tube. BRIEF DESCRIPTION OF THE DRAWINGS

[0037] Figure 1 It is a schematic diagram of the device for rapidly and uniformly depositing a thin film on the inner wall of a hollow cathode slender tube member based on water cooling and magnetic confinement of the present invention, wherein 1 represents a flange, 2 represents a first connection joint, 3 represents a second connection joint, 4 represents a first water pipe, 5 represents a first water outlet pipe, 6 represents a second water pipe, 7 represents a cathode tube, 8 represents a hollow cathode target, 9 represents a magnetic plug, 10 represents a magnet, 11 represents an anode tube, 12 represents a slender tube member, 13 represents a reciprocating mechanism, 14 represents a first insulating bracket, 15 represents a base, 16 represents a hollow cathode power supply, 17 represents a bias power supply, 18 represents a third connection joint, 19 represents a second insulating bracket, 20 represents a second water outlet pipe, and 21 represents a third water pipe;

[0038] Figure 2 This is a cross-sectional electron microscope image of a metal Cr film deposited on the inner wall of a slender tube with an inner diameter of 6 mm in this embodiment;

[0039] Figure 3 This is the surface morphology of the metal Cr film plated in this embodiment;

[0040] Figure 4 This is the indentation morphology of the metal Cr film plated in this embodiment;

[0041] Figure 5 The discharge voltage and current waveforms of the hollow cathode power supply used for thin film deposition on the inner wall of a slender tubular member. DETAILED DESCRIPTION

[0042] Specific implementation method 1: Figure 1 As shown, in this embodiment, a device for quickly and uniformly depositing a thin film on the inner wall of a hollow cathode slender tube member based on water cooling and magnetic confinement comprises a flange 1, a first connecting joint 2, a second connecting joint 3, a third connecting joint 18, a first water pipe 4, a first water outlet pipe 5, a second water pipe 6, a second water outlet pipe 20, a third water pipe 21, a cathode tube 7, a hollow cathode target 8, a magnetic plug 9, a magnet 10, an anode tube 11, a slender tube member 12, a reciprocating mechanism 13, a hollow cathode power supply 16 and a bias power supply 17;

[0043] The first connecting joint 2, the second connecting joint 3, the third connecting joint 18, the first water pipe 4, the water outlet pipe 5, the second water pipe 6, the second water outlet pipe 20, the third water pipe 21, the cathode tube 7, the hollow cathode target 8, the magnetic plug 9 and the magnet 10 together constitute the water cooling system of the device;

[0044] One end of the first water pipe 4 is connected to the flange 1, and the other end is connected to one end of the third water pipe 21 through the first connection joint 2; the other end of the third water pipe 21 is connected to one end of the second water pipe 6 through the second connection joint 3; the other end of the second water pipe 6 is a water outlet;

[0045] One end of the first water outlet pipe 5 is connected to the flange 1, and the other end is connected to one end of the second water outlet pipe 20 through the third connecting joint 18; the other end of the second water outlet pipe 20 is the water inlet of the second water delivery pipe 6;

[0046] The hollow cathode target 8 is connected to the cathode tube 7, and the magnetic plug 9 is connected to the magnet 10 and is placed inside the cathode tube 7 and at the connection between the hollow cathode target 8 and the cathode tube 7; the magnetic plug 9 is sealed and connected to the cathode tube 7;

[0047] The slender tube member 12 is sleeved with a second water pipe 6, a cathode tube 7, a hollow cathode target 8, a magnetic plug 9, a magnet 10 and an anode tube 11; the second water pipe 6, the cathode tube 7, the hollow cathode target 8, the magnetic plug 9, the magnet 10, the anode tube 11 and the slender tube member 12 are coaxially arranged; the length of the cathode tube 7 and the anode tube 11 is longer than that of the slender tube member 12.

[0048] In this embodiment, the magnetic plug 9 is connected to the magnet 10 and placed inside the cathode tube 7 and located at the connection between the hollow cathode target 8 and the cathode tube 7 , so as to support the hollow cathode target 8 while sealing the cathode tube 7 .

[0049] Specific embodiment 2: This embodiment is different from specific embodiment 1 in that it also includes a first insulating support 14, a second insulating support 19 and a base 15; the first insulating support 14 is fixed on the base 15, and the first insulating support 14 supports the second water pipe 6 and the anode tube 11; the second insulating support 19 is fixed on the reciprocating mechanism 13, and the second insulating support 19 supports the slender tube member 12; the second insulating support 19 is pulled by the reciprocating mechanism 13 to drive the slender tube member 12 to reciprocate along the axial direction. The rest is the same as specific embodiment 1.

[0050] Specific embodiment 3: This embodiment is different from specific embodiment 1 in that the positive output end of the bias power supply 17 is connected to the anode tube 11 and grounded, and the negative output end is connected to the slender tube 12; the negative output end of the hollow cathode power supply 16 is connected to the hollow cathode target 8, and the positive output end is connected to the anode tube 11 and grounded. The rest is the same as specific embodiment 1.

[0051] Specific embodiment 4: This embodiment is different from the specific embodiment 1 in that the material of the hollow cathode target 8 is Cr, Ti, Ta, Cu, Ni, Zn, Nb, Sn, Al, Fe, Mg or Zr;

[0052] Or it can be nickel-chromium alloy, nickel-aluminum alloy, nickel-iron alloy, nickel-vanadium alloy, titanium-aluminum alloy, titanium-aluminum-silicon alloy, gold-tin alloy, gold-palladium alloy, molybdenum-niobium alloy, ruthenium-chromium alloy, boron-iron alloy or silicon-iron alloy. Others are the same as the first embodiment.

[0053] Specific embodiment 5: This embodiment is different from specific embodiment 1 in that the hollow cathode power supply 16 and the bias power supply 17 can be a DC power supply, a pulse power supply, a high voltage power supply, a radio frequency power supply, an intermediate frequency power supply or a high power pulse power supply. The rest is the same as specific embodiment 1.

[0054] In this embodiment, when the hollow cathode power supply 16 and the bias power supply 17 adopt pulse power supply, high voltage power supply, radio frequency power supply, medium frequency power supply or high power pulse power supply, the frequency is adjustable from 0.1 to 5000 Hz and the pulse width is adjustable from 0.1 to 5000 μs.

[0055] Specific embodiment 6: This embodiment is a method for using a device for quickly and uniformly depositing a thin film on the inner wall of a hollow cathode elongated tube based on water cooling and magnetic confinement, which is implemented by the following steps:

[0056] 1. Self-glow cleaning of the inner wall of slender tubes:

[0057] The vacuum chamber is evacuated, and working gas is introduced into the vacuum chamber to maintain the vacuum chamber pressure of 1-50 Pa. The positive output end of the bias power supply 17 is connected to the anode tube 11 and grounded, and the negative output end is connected to the slender tube member 12. The voltage of the bias power supply 17 is controlled to be -50-2000V, and the duty cycle is 5%-100%. The plasma generated by the hollow cathode discharge effect is used to self-glow clean the inner surface of the slender tube member 12 to obtain the slender tube member after self-glow cleaning;

[0058] 2. Hollow cathode enhanced glow cleaning of the inner wall of slender tube parts:

[0059] The vacuum chamber pressure is maintained at 1-50 Pa, the negative output end of the hollow cathode power supply 16 is connected to the hollow cathode target 8, the positive output end is connected to the anode tube 11 and grounded, and the negative output end of the bias power supply 17 is connected to the slender tube after self-glow cleaning, and the positive output end is grounded. The voltage of the hollow cathode power supply 16 is controlled to be 400-2000V, the peak current is 0.1-100A, and the duty cycle is 0.1%-100%. The voltage of the bias power supply 17 is -50--2000V, and the duty cycle is 5%-100%. The hollow cathode enhanced glow cleaning is performed to obtain the slender tube after hollow cathode enhanced glow cleaning;

[0060] 3. Deposition on the inner wall of tube and barrel:

[0061] The negative output end of the hollow cathode power supply 16 is connected to the hollow cathode target 8, and the positive output end is connected to the anode tube 11. At the same time, the negative output end of the bias power supply 17 is connected to the slender tube after the hollow cathode enhanced glow cleaning, and the positive output end is grounded. The vacuum chamber pressure is maintained at 1-50Pa, and the voltage of the hollow cathode power supply 16 is controlled to be 400-2000V, the peak current is 0.1-100A, and the duty cycle is 0.1%-100%. The voltage of the bias power supply 17 is -0.1-500V, and the duty cycle is 5%-100%. Hollow cathode coating is carried out to complete the rapid and uniform deposition of a thin film on the inner wall of the slender tube, that is, the method for using the device is completed.

[0062] Specific embodiment 7: This embodiment is different from specific embodiment 6 in that the working gas in step 1 is argon (Ar), helium (He), neon (Ne), krypton (Kr), xenon (Xe), radon (Rn), oxygen (O 2 ), nitrogen (N 2 ), hydrogen (H 2 ), methane (CH4), hydrogen sulfide (H2S), ammonia (NH3), Ar+O 2 、Ar+N 2 、Ar+H 2 , O 2 +N 2 , O 2 +CH 4 , Ar+He or Ar+Xe; when the working gas is a mixed gas, the two are mixed in any ratio. Other steps and parameters are the same as those in the sixth embodiment.

[0063] Specific implementation example eight: This implementation example is different from specific implementation example six in that the time for self-glow cleaning in step one is 5 minutes to 700 minutes. The other steps and parameters are the same as those in specific implementation example six.

[0064] Specific embodiment 9: This embodiment is different from specific embodiment 6 in that the time of hollow cathode enhanced glow cleaning in step 2 is 5 minutes to 700 minutes. Other steps and parameters are the same as those in specific embodiment 6.

[0065] Specific embodiment 10: This embodiment is different from specific embodiment 6 in that the time of hollow cathode coating in step 3 is 10 minutes to 700 minutes. Other steps and parameters are the same as those in specific embodiment 6.

[0066] The beneficial effects of the present invention are verified by the following examples:

[0067] Example:

[0068] A method for using a device for quickly and uniformly depositing a thin film on the inner wall of a hollow cathode elongated tube based on water cooling and magnetic confinement is implemented by the following steps:

[0069] 1. Self-glow cleaning of the inner wall of slender tubes:

[0070] Evacuate the vacuum chamber to 5 × 10 -3 Pa, introduce working gas into the vacuum chamber, maintain the vacuum chamber pressure at 5Pa, connect the positive output end of the bias power supply 17 to the anode tube 11 and ground, connect the negative output end to the slender tube member 12, control the voltage of the bias power supply 17 to -800V, the duty cycle is 60%, and the Ar plasma generated by the hollow cathode discharge effect performs self-glow cleaning on the inner surface of the slender tube member 12 to obtain the slender tube member after self-glow cleaning;

[0071] 2. Hollow cathode enhanced glow cleaning of the inner wall of slender tube parts:

[0072] The vacuum chamber pressure is maintained at 5 Pa, the negative output end of the hollow cathode power supply 16 is connected to the hollow cathode target (8), the positive output end is connected to the anode tube 11 and grounded, and the negative output end of the bias power supply 17 is connected to the slender tube member after self-glow cleaning, and the positive output end is grounded. The voltage of the hollow cathode power supply 16 is controlled to be 1200V, the peak current is 60A, and the duty cycle is 40%. The voltage of the bias power supply 17 is controlled to be -800V and the duty cycle is 60%. The hollow cathode enhanced glow cleaning is performed to obtain the slender tube member after hollow cathode enhanced glow cleaning;

[0073] 3. Deposition on the inner wall of tube and barrel:

[0074] The negative output end of the hollow cathode power supply 16 is connected to the hollow cathode target 8, and the positive output end is connected to the anode tube 11. At the same time, the negative output end of the bias power supply 17 is connected to the slender tube after the hollow cathode enhanced glow cleaning, and the positive output end is grounded. The vacuum chamber pressure is maintained at 5Pa, and the voltage of the hollow cathode power supply 16 is controlled to be 1200V, the peak current is 60A, and the duty cycle is 1.4%. The voltage of the bias power supply 17 is -200V and the duty cycle is 20%. The hollow cathode coating is performed to complete the rapid and uniform deposition of a thin film on the inner wall of the slender tube, that is, the use method of the device is completed;

[0075] The working gas in step 1 is argon.

[0076] The time for the self-glow cleaning in step 1 is 15 minutes.

[0077] The time for the hollow cathode enhanced glow cleaning in step 2 is 15 minutes.

[0078] The time for hollow cathode coating in step 3 is 12 minutes.

[0079] In this embodiment, the hollow cathode power supply 16 adopts a pulse power supply; the bias power supply 17 adopts a DC power supply.

[0080] The slender tube member described in step 1 of this embodiment is a 304 stainless steel tube member with an inner diameter of 6 mm and a length of 20 mm.

[0081] The hollow cathode target material in step three of this embodiment is pure Cr metal prepared by hot isostatic pressing.

[0082] In this embodiment, the hollow cathode target material inside the slender tube is used to discharge and ionize argon gas; the ionized argon plasma causes the entire hollow target tube surface to be uniformly ablated to obtain a rapidly deposited uniform large thickness film; and this method effectively reduces the temperature increase on the surface of the slender tube material, and meets the requirements of film thickness and uniformity while ensuring the mechanical properties of the material.

[0083] Figure 2 This is a cross-sectional electron microscope image of a metal Cr film deposited on the inner wall of a slender tube with an inner diameter of 6 mm in this embodiment; Figure 2 The upper middle part is the plated metal Cr film, and the lower part is the slender tube substrate. The metal Cr film is well bonded to the substrate and has a dense structure.

[0084] Figure 3 is the surface morphology of the metal Cr film plated in this embodiment; Figure 3 It can be seen that the surface of the plated metal Cr film is relatively smooth, no large particles or droplets are seen, and the surface uniformity is relatively excellent.

[0085] Figure 4 is the indentation morphology of the metal Cr film plated in this embodiment; Figure 4 It can be seen that the indentation of the plated metal Cr film is a complete circular indentation with a smooth and complete edge, without radial cracks and large areas of film removal, indicating that the structure of the metal Cr film and the substrate is dense and the connection is reliable.

[0086] Figure 5 The discharge voltage and current waveforms of the hollow cathode power supply used for thin film deposition on the inner wall of the elongated tube in this embodiment; Figure 5 It shows that during the film deposition process, the actual sputtering power supply pulse voltage is 1200V, the pulse peak current is 60A, the corresponding frequency is 900Hz, and the pulse width is 15μs.

[0087] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments, or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A device for rapidly and uniformly depositing a thin film on the inner wall of a hollow cathode elongated tube based on water cooling and magnetic confinement, characterized in that It comprises a flange (1), a first connecting joint (2), a second connecting joint (3), a third connecting joint (18), a first water delivery pipe (4), a first water outlet pipe (5), a second water delivery pipe (6), a second water outlet pipe (20), a third water delivery pipe (21), a cathode tube (7), a hollow cathode target material (8), a magnetic plug (9), a magnet (10), an anode tube (11), a slender tube member (12), a reciprocating mechanism (13), a hollow cathode power supply (16) and a bias power supply (17); The first connecting joint (2), the second connecting joint (3), the third connecting joint (18), the first water pipe (4), the water outlet pipe (5), the second water pipe (6), the second water outlet pipe (20), the third water pipe (21), the cathode tube (7), the hollow cathode target material (8), the magnetic plug (9) and the magnet (10) together constitute a water cooling system of the device; One end of the first water pipe (4) is connected to the flange (1), and the other end is connected to one end of the third water pipe (21) via a first connecting joint (2); the other end of the third water pipe (21) is connected to one end of the second water pipe (6) via a second connecting joint (3); the other end of the second water pipe (6) is a water outlet; One end of the first water outlet pipe (5) is connected to the flange (1), and the other end is connected to one end of the second water outlet pipe (20) via a third connecting joint (18); the other end of the second water outlet pipe (20) is the water inlet of the second water delivery pipe (6); The hollow cathode target (8) is connected to the cathode tube (7); the magnetic plug (9) is connected to the magnet (10) and is placed inside the cathode tube (7) and at the connection between the hollow cathode target (8) and the cathode tube (7); the magnetic plug (9) and the cathode tube (7) are sealed; The slender tube member (12) is sleeved with a second water pipe (6), a cathode tube (7), a hollow cathode target material (8), a magnetic plug (9), a magnet (10) and an anode tube (11); the second water pipe (6), the cathode tube (7), the hollow cathode target material (8), the magnetic plug (9), the magnet (10), the anode tube (11) and the slender tube member (12) are coaxially arranged; the lengths of the cathode tube (7) and the anode tube (11) are longer than those of the slender tube member (12).

2. According to claim 1, a device for rapidly and uniformly depositing a thin film on the inner wall of a hollow cathode elongated tube based on water cooling and magnetic confinement, characterized in that It also comprises a first insulating support (14), a second insulating support (19) and a base (15); the first insulating support (14) is fixed on the base (15), and the first insulating support (14) supports the second water pipe (6) and the anode tube (11); the second insulating support (19) is fixed on the reciprocating mechanism (13), and the second insulating support (19) supports the slender tube member (12); the second insulating support (19) is pulled by the reciprocating mechanism (13) to drive the slender tube member (12) to reciprocate along the axial direction.

3. The device for rapidly and uniformly depositing a thin film on the inner wall of a hollow cathode elongated tube based on water cooling and magnetic confinement according to claim 1, characterized in that The positive output end of the bias power supply (17) is connected to the anode tube (11) and grounded, and the negative output end is connected to the slender tube member (12); the negative output end of the hollow cathode power supply (16) is connected to the hollow cathode target material (8), and the positive output end is connected to the anode tube (11) and grounded.

4. The device for rapidly and uniformly depositing a thin film on the inner wall of a hollow cathode elongated tube member based on water cooling and magnetic confinement according to claim 1, characterized in that The hollow cathode target (8) is made of Cr, Ti, Ta, Cu, Ni, Zn, Nb, Sn, Al, Fe, Mg or Zr; Alternatively, it may be a nickel-chromium alloy, a nickel-aluminum alloy, a nickel-iron alloy, a nickel-vanadium alloy, a titanium-aluminum alloy, a titanium-aluminum-silicon alloy, a gold-tin alloy, a gold-palladium alloy, a molybdenum-niobium alloy, a ruthenium-chromium alloy, a boron-iron alloy or a silicon-iron alloy.

5. The device for rapidly and uniformly depositing a thin film on the inner wall of a hollow cathode elongated tube based on water cooling and magnetic confinement according to claim 1, characterized in that The hollow cathode power supply (16) and the bias power supply (17) can both be a direct current power supply, a pulse power supply, a high voltage power supply, a radio frequency power supply, an intermediate frequency power supply or a high power pulse power supply.

6. A method for using the device for rapidly and uniformly depositing a thin film on the inner wall of a hollow cathode elongated tube based on water cooling and magnetic confinement as claimed in claim 1, characterized in that: It is implemented as follows:

1. Self-glow cleaning of the inner wall of slender tubes: The vacuum chamber is evacuated, and working gas is introduced into the vacuum chamber to maintain the vacuum chamber pressure at 1-50 Pa. The positive output end of the bias power supply (17) is connected to the anode tube (11) and grounded, and the negative output end is connected to the slender tube member (12). The voltage of the bias power supply (17) is controlled to be -50--2000V, and the duty cycle is 5%-100%. The inner surface of the slender tube member (12) is self-glowing and cleaned by plasma generated by the hollow cathode discharge effect, so as to obtain the slender tube member after self-glowing cleaning; 2. Hollow cathode enhanced glow cleaning of the inner wall of slender tube parts: The vacuum chamber pressure is maintained at 1-50 Pa, the negative output end of the hollow cathode power supply (16) is connected to the hollow cathode target (8), the positive output end is connected to the anode tube (11) and grounded, and the negative output end of the bias power supply (17) is connected to the slender tube after self-glow cleaning, and the positive output end is grounded. The voltage of the hollow cathode power supply (16) is controlled to be 400-2000V, the peak current is 0.1-100A, and the duty cycle is 0.1%-100%, and the voltage of the bias power supply (17) is -50--2000V, and the duty cycle is 5%-100%, and the hollow cathode enhanced glow cleaning is performed to obtain the slender tube after hollow cathode enhanced glow cleaning; 3. Deposition on the inner wall of tube and barrel: The negative output end of the hollow cathode power supply (16) is connected to the hollow cathode target material (8), and the positive output end is connected to the anode tube (11). At the same time, the negative output end of the bias power supply (17) is connected to the slender tube after the hollow cathode enhanced glow cleaning, and the positive output end is grounded. The vacuum chamber pressure is maintained at 1-50 Pa, and the voltage of the hollow cathode power supply (16) is controlled to be 400-2000V, the peak current is 0.1-100A, and the duty cycle is 0.1%-100%. The voltage of the bias power supply (17) is -0.1-500V, and the duty cycle is 5%-100%. Hollow cathode coating is performed to complete the rapid and uniform deposition of a thin film on the inner wall of the slender tube. This completes the method for using the device.

7. A method for using the device for rapidly and uniformly depositing a thin film on the inner wall of a hollow cathode elongated tube based on water cooling and magnetic confinement according to claim 6, characterized in that The working gas described in step 1 is argon, helium, neon, krypton, xenon, radon, oxygen, nitrogen, hydrogen, methane, hydrogen sulfide, ammonia, Ar+O2, Ar+N2, Ar+H2, O2+N2, O2+CH4, Ar+He or Ar+Xe; when the working gas is a mixed gas, the two are mixed in any ratio.

8. The method for using the device for rapidly and uniformly depositing a thin film on the inner wall of a hollow cathode elongated tube based on water cooling and magnetic confinement according to claim 6 is characterized in that The time of the self-glow cleaning in step 1 is 5 minutes to 700 minutes.

9. The method for using the device for rapidly and uniformly depositing a thin film on the inner wall of a hollow cathode elongated tube based on water cooling and magnetic confinement according to claim 6, characterized in that The time for the hollow cathode enhanced glow cleaning in step 2 is 5 minutes to 700 minutes.

10. The method for using the device for rapidly and uniformly depositing a thin film on the inner wall of a hollow cathode elongated tube based on water cooling and magnetic confinement according to claim 6, characterized in that The time for hollow cathode coating in step 3 is 10 min to 700 min.

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