Medical material tantalum coating PVD coating process

Abstract

The present application relates to a kind of medical material tantalum coating PVD coating process, comprising: S1, the medical material is carried out electron beam enhanced plasma cleaning modification, using argon ion bombardment medical material surface;S2, the medical material surface treated in S1 is bombarded with metal ion, and the charged metal ion generated by ionization source is accelerated by high negative bias and bombards the medical material surface;S3, transition layer and metal film layer are deposited on the medical material surface treated in S2, the transition layer is deposited by gradient by reaction gas, and the metal film layer uses tantalum as target material.The process can obtain strong binding force on medical material, dense plating layer, biocompatibility and have radiopaque metal film layer, form tantalum film layer by gradient reaction gas, negative bias, target current deposition to medical material surface, gradient coating reduces the stress generated in the process of tantalum metal stacking, increases the reliability of film layer, has excellent mechanical properties.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of medical devices, in particular to a PVD coating process of a medical material tantalum coating. BACKGROUND

[0002] PEEK, i.e. polyether ether ketone, is a biologically inert material. A large number of documents and clinical applications have proved that PEEK has no adverse reactions after being implanted into the human body. However, when the implanted product needs to have the function of bone integration, the chemical inertness and low surface energy of PEEK make the cell adhesion and protein absorption slow, which reduces the bone integration between the implant and the tissue and prolongs the bone fusion time. In order to solve the above problems, 3D printing PEEK material can be designed into a porous structure in advance, which to some extent increases the bone integration ability of PEEK, but the biological inertness of the material itself does not change. Therefore, the prior art improves the physicochemical properties of the surface of PEEK by depositing a biologically active metal tantalum on the surface of the PEEK material to form a tantalum coating, so as to enhance the bone integration ability of the surface thereof.

[0003] For example, the patent application CN115591018A discloses a PEEK bone implant material and a preparation method thereof. A photoresist is spin-coated on the surface of the PEEK material, and then the photoresist is subjected to exposure and development in sequence and etched to obtain a surface with the topological pattern. Then, a tantalum coating is deposited by using a magnetron sputtering. However, this scheme is complex and has high cost. The unmodified PEEK has weak adhesion of the coating deposited at a sputtering power of 150-250W. The patent application CN115429940A discloses a method for enhancing the stability of a biologically active coating. A microstructure composed of a plurality of microstructure units is directly formed on the PEEK by photolithography, micro-milling or laser to solve the problems of insufficient mechanical stability, easy damage, short service life and poor wear resistance of the biologically active coating in the actual use environment. However, the method for forming the microstructure has the problems of complex process and risk of coating falling off caused by micro-motion wear.

[0004] In addition, although titanium or titanium alloy has strong biocompatibility, compared with PEEK material, titanium, aluminum and vanadium ions are released, and there are problems such as residual of processing aids and large elastic modulus. Therefore, it has become a common method to use PEEK or modified PEEK to replace titanium-based band wire anchors and bone plates. However, PEEK or modified PEEK is an organic material and does not have radio-opacity. Therefore, there are problems such as inaccurate positioning, judgment of whether the bone plate is broken and whether the fracture line is healed in the radio-graphic examination. SUMMARY

[0005] The purpose of the present application is to solve the problem of poor adhesion of the coating formed on the medical material, and to provide a PVD coating process of a medical material tantalum coating.

[0006] To solve the above problems, the present invention deposits metallic tantalum on the surface of PEEK or CRF / PEEK material to form a tantalum coating with a strong radiation absorption coefficient, thereby increasing the radiopacity of the material.

[0007] PEEK is a material with high thermal stability. Its linear expansion coefficient is about 3.5ppm / ℃ at room temperature, while the linear expansion coefficient of tantalum is 7-8ppm / ℃ at room temperature. When tantalum coating is deposited on the surface of PEEK, due to the large difference in linear expansion coefficient and the fact that PEEK material is non-conductive and has poor thermal conductivity, the deposition process easily accumulates large stress, leading to coating failure. For metal carbon / nitride, since carbon / nitrogen atoms occupy a large space in the crystal lattice, the lattice spacing of metal carbon / nitride increases. When the temperature rises, the atomic vibration amplitude increases, and the lattice spacing further expands, resulting in the linear expansion coefficient of metal carbon / nitride being smaller than that of metal. Correspondingly, the linear expansion coefficient of tantalum nitride is about 5.5ppmppm / ℃. In combination with the above material properties, in order to solve the coating stress problem, the present invention utilizes gradient reaction gas, negative bias voltage, and target current to deposit onto the surface of PEEK material to form a tantalum metal carbon / nitride transition layer with decreasing carbon / nitrogen atom content, that is, increasing linear expansion coefficient. The gradient coating reduces the stress generated by the stacking of tantalum metal materials during the coating process and increases the reliability of the film layer.

[0008] The specific plan is as follows:

[0009] A PVD coating process for a medical material tantalum coating comprises the following steps:

[0010] S1. The medical material is subjected to electron beam enhanced plasma cleaning and modification, and argon ions are used to bombard the surface of the medical material. The process control includes: vacuum degree at 1-5 Pa, cleaning time 10-120 min, negative bias voltage 50-300 V, arc current 50-250 A, and anode current 10-100 A. Under these conditions, a large number of argon ions are generated to bombard the surface of the medical material, which can enhance the bonding strength between the film layer subsequently formed on the surface and the material.

[0011] S2. The surface of the medical material treated in S1 is bombarded with metal ions. Charged metal ions generated by an ionization source are accelerated to bombard the surface of the medical material using a high negative bias. Preferably, the process control includes: a vacuum level of 0.1-1 Pa, a bombardment time of 10-120 minutes, a negative bias of 200-1000 V, and an ionization source current of 1-200 A. More preferably, the vacuum level is 0.2 Pa, the bombardment time is 20 minutes, the negative bias is 700 V, and the ionization source current is 1.8 A. Under these conditions, the surface energy of the PEEK is increased, thereby further improving the bonding strength, ensuring the stability of the film layer, and preventing it from falling off.

[0012] S3. Depositing a transition layer and a metal film layer on the surface of the medical material treated in S2. The transition layer is deposited using a reaction gas. The metal film layer uses tantalum as a target material. The transition layer and tantalum coating are formed on the medical material under a vacuum of 0.1-1 Pa, a coating time of 10-120 min, a negative bias voltage of 30-200 V, and a target current of 1-100 A. The transition layer is deposited on the surface of the PEEK material to form a tantalum metal film layer using a gradient reaction gas, negative bias voltage, and target current. The gradient coating reduces the stress generated during the stacking process of the tantalum coating and increases the reliability of the film layer.

[0013] Preferably, the medical material is a PEEK porous fusion device formed by 3D printing, or a wire anchor or bone plate made of PEEK or carbon fiber reinforced PEEK;

[0014] Preferably, for a PEEK porous fusion device formed by 3D printing, the thickness of the tantalum coating is 1-1500 nm, preferably 100-1000 nm, and more preferably 200-800 nm; for wire anchors and bone plates made of PEEK or carbon fiber reinforced PEEK, the thickness of the tantalum coating is 100-10000 nm, preferably 1000-6000 nm, and more preferably 3000-5000 nm;

[0015] Preferably, the bonding force of the tantalum coating is 30-50 MPa, preferably 37-45 MPa, and more preferably 40-46 MPa.

[0016] Furthermore, the electron beam generated by arc discharge in S1 excites and generates argon ions to bombard the surface of the medical material.

[0017] Furthermore, the arc discharge described in S1 utilizes a cathode arc discharge method. During the cathode arc source discharge process, a shield is used to prevent metal ions from depositing on the product surface, and an anode device is installed within the vacuum chamber. The shield blocks the metal ions, while only electrons can pass through the gaps on both sides of the shield. They are accelerated by the electric field of the anode device and then bombard the argon gas, producing a large number of argon ions. Under the action of a negative bias, the argon ions are accelerated to bombard the product surface, achieving a good surface treatment effect and facilitating the smooth progress of steps S2 and S3.

[0018] Furthermore, the cathode arc source in S1 is a cylindrical arc source, a planar arc source, or a circular arc source, preferably a cylindrical arc source. When a cylindrical arc source is used, the target material utilization rate is high, and the plasma is evenly distributed, which can better perform electron bombardment and obtain a better surface treatment effect.

[0019] Furthermore, the arc discharge anode device in S1 is a copper electrode, and the copper electrode is connected to the positive electrode of the anode power supply;

[0020] Preferably, the cylindrical copper electrode is installed in the middle of the vacuum chamber, so that the electrons generated by the cathode arc source can fly to the anode device after passing through the path of product rotation, and the electron bombardment can be more thorough.

[0021] Furthermore, the ionization source described in S2 is one or more of cathode arc, magnetron sputtering, or laser discharge, the target material used in the ionization source is tantalum or titanium target, preferably magnetron sputtering titanium target, and the power supply form is one or more of direct current, medium frequency, high frequency pulse power supply, radio frequency or pulse, preferably high frequency pulse power supply.

[0022] Preferably, the negative bias voltage decreases gradually from large to small, and more preferably, the gradient negative bias voltage is 120-150V, 80-100V, or 40-50V.

[0023] Preferably, the target current increases in a gradient from small to large, and more preferably, the gradient target current is 6-8, 7-9, or 8-10 A;

[0024] Preferably, each gradient coating time increases gradually, and more preferably, the coating time is 10-30, 15-45, or 20-60 min.

[0025] Furthermore, the purity of the target material is greater than 99.99 wt %, and argon gas is used to control the vacuum degree in the coating process, and the purity of the argon gas is greater than 99.99 wt %.

[0026] Beneficial effects:

[0027] In the present invention, electron beam-enhanced plasma bombardment (EBEP) in S1 uses arc discharge to generate a large number of argon ions, which bombard the surface of medical materials. This increases the surface energy of the medical material and strengthens the bonding strength between the film and the material. The device is integrated into the coating equipment, is simple to operate, and is suitable for large-scale production.

[0028] Furthermore, the charged metal ions generated by the S2 metal ion bombardment of the present invention through the ionization source are accelerated to bombard the surface of the medical material through a high negative bias voltage, so that a rough structure is produced on the PEEK surface. At the same time, the accelerated ions can better fuse with the PEEK surface, further improving the stability of the membrane layer.

[0029] Further, since the carbon / nitrogen atoms in the metal carbon / nitrogen compound occupy a large space in the metal carbon / nitrogen compound, the lattice spacing of the metal carbon / nitrogen compound is increased, the amplitude of atomic vibration in the metal carbon / nitrogen compound is increased when the temperature is increased, and the lattice spacing is further expanded, resulting in the characteristic that the linear expansion coefficient of the metal carbon / nitrogen compound is smaller than that of the metal. In S3 of the present application, the metal deposition is performed by gradient reaction gas, negative bias voltage and target current to deposit a tantalum metal carbon / nitrogen compound transition layer with decreasing carbon / nitrogen content and increasing linear expansion coefficient on the surface of the PEEK material. The gradient plating reduces the stress generated by the stacking of the tantalum metal material in the plating process, and increases the reliability of the film layer.

[0030] In summary, the present application uses the PVD plating process to deposit a layer of biologically active tantalum coating with strong adhesion, uniform and dense coating on medical materials, improves the surface characteristics of the PEEK biologically inert surface, and can completely retain the elastic modulus and 3D printing porous structure, and can enhance the radiopacity of the material, and the deposition temperature is lower than 100℃, and at the same time does not affect the original mechanical properties of the material, so as to play a role in enhancing the cell adhesion and bone bonding ability after the material is implanted.

[0031] Compared with the thermal spraying process, the thickness of the metal coating deposited by the present application can be controlled to be below 1000 nm, the porous structure and the low elastic modulus matching characteristics of the surface of the medical material can be better maintained, and the deposition temperature is controlled to be below 100℃, which does not affect the mechanical properties of the material. BRIEF DESCRIPTION OF DRAWINGS

[0032] In order to more clearly illustrate the technical solutions of the present application, the following will briefly introduce the drawings. Obviously, the drawings described below only relate to some embodiments of the present application, and are not a limitation on the present application.

[0033] Figure 1 is a product real photo provided by embodiment 1 of the present application.

[0034] Figure 2 is an SEM diagram of the tantalum coating on the surface of the product in embodiment 1 of the present application.

[0035] Figure 3 is an SEM diagram of the cross section of the tantalum coating in embodiment 1 of the present application.

[0036] Figure 4 is a coating adhesion test diagram of embodiment 1 in the present application.

[0037] Figure 5 is a radiopacity diagram of the tantalum coating in embodiment 5 of the present application (from left to right, tantalum coating CFR / PEEK, CFR / PEEK, PEEK material), wherein CFR refers to carbon fiber reinforced polyether ether ketone. DETAILED DESCRIPTION

[0038] The preferred embodiments of the present application will be described in more detail below. Although the preferred embodiments of the present application are described below, it is to be understood that the present application can be carried out in various forms and should not be limited by the embodiments set forth herein. If no specific technique or condition is specified in the examples, the technique or condition described in the literature in the art or according to the product manual is used. If no manufacturer of the reagent or instrument is specified, it is a conventional product that can be commercially available. In the following examples, unless otherwise specified, "%" means weight percent, and "parts" means weight parts.

[0039] The test standards used in the present application are as follows:

[0040] The coating thickness test standard of the present application: the film thickness of the sample is tested according to "GB / T 31563-2015 Metal Coating Thickness Measurement Scanning Electron Microscope Method".

[0041] The test standard of the coating adhesion of the present application: the sample is tested according to "YY / T 0988.11 Surgical Implant Coating Part 11: Calcium Phosphate Coating and Metal Coating Tensile Test Method".

[0042] Example 1

[0043] Arc target installation in the coating machine Arc target installation in the coating machine Arc target installation in the coating machine The cleaned and dried PEEK porous fusion device and tensile sample are placed into the vacuum coating machine, and the initial temperature is 31℃. When the vacuum degree reaches 0.003pa, the coating begins. The process of S1 electron beam enhanced plasma bombardment has a vacuum degree of 2pa, a cleaning time of 15min, a negative bias of 150V, an arc current of 60A, and an anode current of 15A. The process of S2 metal ion bombardment uses magnetic target 1, has a vacuum degree of 0.1pa, a bombardment time of 30min, a negative bias of 500V, and a magnetron sputtering current of 1.8A. The process of S3 metal deposition has a vacuum degree of 0.5pa, an initial nitrogen flow of 200sccm, a nitrogen flow gradient reduction, a negative bias gradient of 120, 80, 40V, a magnetron sputtering current gradient of 7, 7.5, 8A, and a time gradient of 30, 45, 60min. The coating end temperature is 92℃. The specific process parameters are shown in Table 1.

[0044] After testing, the film thickness is about 900nm, and the coating adhesion is 46Mpa.

[0045] Figure 1 The physical picture after the coating is finished can be seen, the porous fusion device surface has dense holes, and after the coating, the hole structure is still uniform, which is the same as the sample without coating.Figure 2 This is an SEM image of the tantalum coating surface, with a magnification of 10,000 times. It can be seen that the tantalum coating is very dense. Figure 3 This is a cross-sectional SEM coating. It can be seen that the tantalum coating with a thickness of about 900nm is continuously adhered to the PEEK surface. Among them, the transition layer is the thin layer corresponding to the thin white horizontal line in the middle of the figure. Figure 4 It is a specimen that failed under tension, and its tensile strength is greater than 40 MPa.

[0046] Table 1 Process parameters of Example 1

[0047]

[0048]

[0049] Example 2

[0050] Arc target installation in coating machine Arc tantalum target, magnetron target 1 installation Cylindrical titanium target, magnetron target 2 installation A cylindrical tantalum target was used, and the magnetron power supply used a high-frequency pulse power supply. After cleaning and drying, the 3D-printed PEEK porous fusion device and tensile specimen were placed in the vacuum coating machine at an initial temperature of 27°C. Coating began when the vacuum reached 0.003 Pa. The S1 electron beam-enhanced plasma bombardment process had a vacuum of 1.8 Pa, a cleaning time of 15 minutes, a negative bias of 100 V, an arc current of 70 A, and an anode current of 20 A. The S2 metal ion bombardment process used magnetron target 2, a vacuum of 0.1 Pa, a bombardment time of 30 minutes, a negative bias of 700 V, a magnetron sputtering current of 1.8 A, and a high-frequency pulse power supply. The S3 metal deposition process had a vacuum of 0.5 Pa, an initial nitrogen flow rate of 250 sccm, and a decreasing nitrogen flow rate gradient. The negative bias voltage gradients were 120, 90, and 60 V, and the magnetron sputtering current gradients were 7, 7.5, and 8 A, with time gradients of 20, 30, and 40 minutes. The final coating temperature was 87°C. Specific process parameters are shown in Table 2.

[0051] After testing, the film thickness is about 610nm and the coating bonding strength is 32Mpa.

[0052] Table 2 Process parameters of Example 2

[0053]

[0054] Example 3

[0055] Arc target installation in coating machine Arc tantalum target, magnetron target 1 installation Cylindrical titanium target, magnetron target 2 installation A cylindrical tantalum target was used, and a high-frequency pulsed magnetron power supply was used. The cleaned and dried PEEK fuser and tensile specimen were placed in the vacuum coating machine, and coating began when the vacuum reached 0.003 Pa. The S1 electron beam-enhanced plasma bombardment process had a vacuum of 1.8 Pa, a cleaning time of 15 minutes, a negative bias of 100 V, an arc current of 70 A, and an anode current of 20 A. The S2 metal ion bombardment process used magnetron target 1, a vacuum of 0.1 Pa, a bombardment time of 30 minutes, a negative bias of 700 V, a magnetron sputtering current of 1.5 A, and a high-frequency pulsed power supply. The S3 metal deposition process had a vacuum of 0.5 Pa, an initial nitrogen flow rate of 200 sccm, a decreasing nitrogen flow rate gradient, negative bias voltage gradients of 120, 90, and 60 V, magnetron sputtering current gradients of 8, 8.5, and 9 A, and time gradients of 10, 15, and 20 minutes. The final coating temperature was 73°C. Specific process parameters are shown in Table 3.

[0056] After testing, the film thickness is about 300nm and the coating bonding strength is greater than 37Mpa.

[0057] Table 3 Process parameters of Example 3

[0058]

[0059] Example 4

[0060] Arc target installation in coating machine Arc tantalum target, magnetron target 1 installation Cylindrical titanium target, magnetron target 2 installation A cylindrical tantalum target was used, and the magnetron power supply used a high-frequency pulse power supply. The cleaned and dried PEEK wire anchor was placed in the vacuum coating machine, and coating began when the vacuum reached 0.003 Pa. The S1 electron beam-enhanced plasma bombardment process had a vacuum of 1.8 Pa, a cleaning time of 15 minutes, a negative bias of 100 V, an arc current of 70 A, and an anode current of 20 A. The S2 metal ion bombardment process used magnetron target 1, a vacuum of 0.1 Pa, a bombardment time of 20 minutes, a negative bias of 700 V, a magnetron sputtering current of 1.5 A, and a high-frequency pulse power supply. The S3 metal deposition process had a vacuum of 0.5 Pa, an initial nitrogen flow rate of 200 sccm, a decreasing nitrogen flow rate gradient, negative bias gradients of 120, 90, and 60 V, magnetron sputtering current gradients of 6, 7, and 7.2 A, and time gradients of 30, 45, and 60 minutes. The final coating temperature was 91°C. Specific process parameters are shown in Table 4.

[0061] After testing, the film thickness is about 1800nm ​​and the coating bonding strength is greater than 36Mpa.

[0062] Table 4 Process parameters of Example 4

[0063]

[0064] Example 5

[0065] Arc target installation in coating machine Arc tantalum target, magnetron target 1 installed Cylindrical titanium target, magnetron target 2 installed Cylindrical tantalum target, magnetron power supply uses high-frequency pulse power supply. After cleaning and drying, the CRF / PEEK bone plate is placed in the vacuum coating machine, and the vacuum degree is reached 0.003 pa. The process of S1 electron beam enhanced plasma bombardment is vacuum degree 1.8 pa, cleaning time 15 min, negative bias 100 V, arc current 70 A, anode current 20 A. The process of S2 metal ion bombardment uses magnetron target 1, vacuum degree 0.1 pa, bombardment time 20 min, negative bias 700 V, magnetron sputtering current 1.5 A, and high-frequency pulse power supply is used. The process of S3 metal deposition is vacuum degree 0.5 pa, nitrogen initial flow 300 sccm, nitrogen flow gradient reduction, negative bias gradient 120, 90, 60 V, magnetron sputtering current gradient 6, 7, 7.5 A, time gradient 60, 90, 120 min. The coating end temperature is 97℃. The specific process parameters are shown in Table 5.

[0066] Tested, the film thickness is about 3800 nm, and the coating adhesion is greater than 40 Mpa.

[0067] Table 5 Process parameters of Example 5

[0068]

[0069] Comparative Example 1

[0070] Referring to Example 1, arc target installation in coating machine Arc tantalum target, magnetron target 1 installed Cylindrical titanium target, magnetron target 2 installed Cylindrical tantalum target, magnetron power supply uses high-frequency pulse power supply. After cleaning and drying, the PEEK fusion device and the tensile sample are placed in the vacuum coating machine, and the vacuum degree is reached 0.003 pa.

[0071] This comparative example uses a conventional ion source cleaning method, uses a DZS1 glow cleaning process (DZS1 is shown in Table 6, which is a high-bias glow cleaning process used in conventional processes), high-bias glow discharge cleaning process, control conditions: vacuum degree 1.8 pa, cleaning time 15 min, negative bias 1000 V. Other steps are consistent with Example 1, and the coating end temperature is 89℃. The specific process parameters are shown in Table 6.

[0072] Tested, the film thickness is about 890 nm, and the coating adhesion is about 24 Mpa.

[0073] Table 6 Process parameters of Comparative Example 1

[0074]

[0075] Comparative Example 2

[0076] This comparative example refers to Example 1, and the gradient deposition is not performed in the S3 step, and other process parameters are consistent. The film coating end temperature is 113℃. The specific process parameters are shown in Table 7.

[0077] After testing, the film thickness is about 1120nm, and the coating adhesion is about 16Mpa.

[0078] Table 7 Process parameters of Comparative Example 2

[0079]

[0080] Comparative Example 3

[0081] This comparative example refers to Example 1, and the gas gradient deposition is not performed in the S3 step, and other process parameters are consistent. The film coating end temperature is 88℃. The specific process parameters are shown in Table 8.

[0082] After testing, the film thickness is about 840nm, and the coating adhesion is about 21Mpa.

[0083] Table 8 Process parameters of Comparative Example 3

[0084]

[0085] The preferred embodiments of the present application are described in detail above, but the present application is not limited to the specific details of the above-described embodiments. Within the technical concept of the present application, various simple modifications can be made to the technical solutions of the present application, and these simple modifications all belong to the protection scope of the present application.

[0086] In addition, it should be noted that each specific technical feature described in the above specific embodiments can be combined in any appropriate manner without contradiction. In order to avoid unnecessary repetition, various possible combinations are not described again by the present application.

[0087] In addition, various different embodiments of the present application can also be combined in any manner, as long as they do not deviate from the idea of the present application, and they should also be considered as disclosed by the present application.

Claims

1. A PVD coating process for tantalum coating of medical materials, characterized by: The following steps are involved: S1. Electron beam enhanced plasma cleaning and modification of the medical material is performed, wherein the electron beam generated by arc discharge excites argon ions to bombard the surface of the medical material. During the cathode arc source discharge process, a shield is used to prevent metal ions from depositing on the product surface, and an anode device is installed in a vacuum chamber; The process control includes: vacuum degree of 1-5 Pa, cleaning time of 10-120 min, negative bias voltage of 50-300 V, arc current of 50-250 A, and anode current of 10-100 A; S2, bombarding the surface of the medical material treated in S1 with metal ions, wherein charged metal ions generated by an ionization source are accelerated to bombard the surface of the medical material by a high negative bias voltage; S3. Depositing a transition layer and a metal film layer on the surface of the medical material treated by S2, the transition layer is deposited by a reaction gas, and the flow rate of the reaction gas changes gradiently from large to small; the metal film layer uses tantalum as a target material, and forms a transition layer and a tantalum coating on the medical material under the action of a vacuum degree of 0.1-1pa, a coating time of 10-120min, a negative bias voltage of 30-200V, and a target current of 1-100A. The negative bias voltage decreases gradiently from large to small, and the target current increases gradiently from small to large, and the coating time of each gradient increases gradiently.

2. The PVD coating process for medical material tantalum coating according to claim 1, characterized in that: The medical material has a porous structure.

3. The PVD coating process for tantalum coating of medical materials according to claim 2, characterized in that: The medical material is a PEEK porous fusion device formed by 3D printing.

4. The PVD coating process for tantalum coating of medical materials according to claim 2, characterized in that: The thickness of the tantalum coating is 1-1500 nm.

5. The PVD coating process for medical material tantalum coating according to claim 4, characterized in that: The thickness of the tantalum coating is 100-1000 nm.

6. The PVD coating process for tantalum coating of medical materials according to claim 5, characterized in that: The thickness of the tantalum coating is 200-800 nm.

7. The PVD coating process for tantalum coating of medical materials according to claim 1, characterized in that: The medical material is PEEK material or carbon fiber reinforced PEEK material.

8. The PVD coating process for tantalum coating of medical materials according to claim 7, characterized in that: The medical material is PEEK or carbon fiber reinforced PEEK with wire anchors and bone plates.

9. The PVD coating process for tantalum coating of medical materials according to claim 7, characterized in that: The thickness of the tantalum coating is 100-10000 nm.

10. The PVD coating process for medical material tantalum coating according to claim 9, characterized in that: The thickness of the tantalum coating is 1000-6000 nm.

11. The PVD coating process for medical material tantalum coating according to claim 10, characterized in that: The thickness of the tantalum coating is 3000-5000 nm.

12. The PVD coating process for medical material tantalum coating according to claim 7, characterized in that: The bonding strength of the tantalum coating is 30-50 MPa.

13. The PVD coating process for medical material tantalum coating according to claim 12, characterized in that: The bonding strength of the tantalum coating is 37-45 MPa.

14. The PVD coating process for medical material tantalum coating according to claim 13, characterized in that: The bonding strength of the tantalum coating is 40-46 MPa.

15. The PVD coating process for medical material tantalum coating according to claim 1, characterized in that: The cathode arc source in S1 is a cylindrical arc source, a plane arc source, or a circular arc source.

16. The PVD coating process for medical material tantalum coating according to claim 15, characterized in that: The cathode arc source in S1 is a cylindrical arc source.

17. The PVD coating process for medical material tantalum coating according to claim 15, characterized in that: The anode device of the arc discharge in S1 is a copper electrode, and the copper electrode is connected to the positive electrode of the anode power supply.

18. The PVD coating process for medical material tantalum coating according to claim 17, characterized in that: The copper electrode is a cylindrical copper electrode and is installed in the middle of the vacuum chamber.

19. The PVD coating process for medical material tantalum coating according to any one of claims 1 to 18, characterized in that: The ionization source in S2 is one or more of cathode arc, magnetron sputtering, or laser discharge.

20. The PVD coating process for medical material tantalum coating according to claim 19, characterized in that: The ionization source in S2 is magnetron sputtering, and the power supply is one or more of direct current, medium frequency, high frequency pulse power, radio frequency or pulse.

21. The PVD coating process for tantalum coating of medical material according to claim 20, characterized in that: The power supply is in the form of high-frequency pulse power supply.

22. The PVD coating process for medical material tantalum coating according to claim 19, characterized in that: The process control in S2 includes: vacuum degree of 0.1-1 Pa, bombardment time of 10-120 min, negative bias voltage of 200-1000 V, and ionization source current of 1-200 A.

23. The PVD coating process for medical material tantalum coating according to any one of claims 1 to 18, characterized in that: In S3, the reaction gas is nitrogen, acetylene, or methane, and the flow gradient is 2-10 gradients.

24. The PVD coating process for tantalum coating of medical material according to claim 23, characterized in that: The reaction gas is nitrogen, and the initial flow rate of nitrogen is 300 sccm, which is reduced by 1 sccm every 25 seconds.

25. The PVD coating process for medical material tantalum coating according to claim 23, characterized in that: The negative bias voltage gradient varies from 120-150V, 80-100V, and 40-50V.

26. The PVD coating process for medical material tantalum coating according to claim 23, characterized in that: The target current gradient changes are 6-8, 7-9, and 8-10A.

27. The PVD coating process for medical material tantalum coating according to claim 23, characterized in that: The coating time is 10-30, 15-45, or 20-60 minutes.

28. The PVD coating process for medical material tantalum coating according to any one of claims 1 to 18, characterized in that: The purity of the target material is greater than 99.99 wt %. Argon is used to control the vacuum degree in the coating process, and the purity of the argon is greater than 99.99 wt %.

Images