A tantalum-silver coating modified bone implant and a method for preparing the same

By depositing a tantalum silver coating on a titanium alloy substrate, the problem of insufficient osseointegration capacity of bone implants was solved, the biocompatibility and antibacterial properties of bone implants were improved, and cell behavior and implant stability were optimized.

CN119685780BActive Publication Date: 2026-04-07XI AN JIAOTONG UNIV
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-12-26
Publication Date
2026-04-07

AI Technical Summary

Technical Problem

Existing bone implants have poor osseointegration capabilities, and traditional coating technologies suffer from problems such as difficulty in uniformly controlling thickness and insufficient bonding strength with the substrate.

Method used

Tantalum and silver were sequentially deposited on the surface of a titanium alloy substrate using magnetron sputtering and then heat-treated to prepare a tantalum-silver coating. By combining appropriate process parameters such as argon purity, target current, vacuum degree, bias voltage, and magnetic field strength, a dense and uniform coating was formed.

Benefits of technology

It improves the osseointegration capacity of bone implants, enhances biocompatibility and antibacterial properties, optimizes cell behavior, improves implant stability and durability, and reduces the risk of postoperative infection.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application discloses a tantalum-silver coating modified bone implant and a preparation method thereof. The method comprises the following steps: depositing tantalum and silver on the surface of a base metal in sequence under an argon atmosphere by using a magnetron sputtering method, and performing heat treatment on the base material after magnetron sputtering, so as to obtain the tantalum-silver coating modified bone implant. The tantalum-silver coating modified bone implant improves the bone integration ability of the implant, enhances the biocompatibility, optimizes the cell behavior, and improves the antibacterial performance.
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Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of surface modification of metal materials, and relates to a tantalum-silver coating modified bone implant and a preparation method thereof. BACKGROUND

[0002] Bone implants, as an important tool of modern medicine, are widely used in repairing jaw defects, installing dental implants, and performing joint replacement surgeries. In order to ensure that the implant can function long-term and stably in the human body, an ideal bone implant needs to have a series of key characteristics. First of all, biocompatibility is the basic requirement of bone implants. This means that the implant must be able to coexist peacefully with human tissues and not trigger immune reactions or rejection reactions. Secondly, good mechanical properties are also essential, because the implant needs to withstand various mechanical pressures from the inside of the human body. In addition, corrosion resistance is also an important indicator of the quality of bone implants, which determines the durability and stability of the implant in the human body. In addition to the above basic characteristics, an ideal bone implant should also have good bone integration ability and antibacterial ability. Bone integration ability refers to the ability of the implant to form a direct contact with the surrounding bone and tissue after being implanted into the body, and to form a bone union. Under an optical microscope, it can be seen that the newly formed bone tissue is directly attached to the metal surface without a fibrous connective tissue interface layer. That is, the implant can form a close bond with the surrounding bone tissue, thereby ensuring the stability and long-term effect of the implant. Bone integration is a direct structural and functional connection between bone tissue and the surface of the implant, which is a structural response of living bone tissue to the non-living implant. Bone integration is a complex dynamic process involving immune responses and related processes such as adhesion, proliferation, and osteogenic differentiation of precursor cells. When there is no progressive relative movement between the bone in direct contact with the implant, the implant is considered to have achieved bone integration. The antibacterial ability helps to reduce the risk of implant infection and improve the success rate of surgery.

[0003] Among the current bone implant materials, metal materials occupy a dominant position. Among them, pure titanium and titanium alloys have become the first choice for bone implant materials due to their excellent biocompatibility and mechanical properties. However, although pure titanium and titanium alloys have many advantages, their bone integration ability still needs to be improved, so modifying the surface of pure titanium and titanium alloys to enhance their bone integration ability has become a hot research topic. Traditional coating techniques can improve the performance of the implant to some extent, but they have defects such as difficulty in uniformly controlling the thickness and insufficient bonding force with the substrate. SUMMARY

[0004] In view of the problems in the prior art, the present application provides a tantalum-silver coating modified bone implant and a preparation method thereof, thereby solving the technical problem of poor bone integration ability of the bone implant in the prior art.

[0005] The present application is realized by the following technical solutions:

[0006] A preparation method of a tantalum-silver coating modified bone implant, comprising: depositing tantalum and silver on the surface of a base metal in sequence under an argon atmosphere by a magnetron sputtering method, and performing heat treatment on the base material after magnetron sputtering to obtain the tantalum-silver coating modified bone implant.

[0007] Preferably, the purity of the argon is greater than 99.999%, and the flow rate of the argon is 20-100 sccm.

[0008] Preferably, in the magnetron sputtering process, the target current is 1-3 A, and the magnetron sputtering time is 18-450 min.

[0009] Preferably, in the magnetron sputtering process, the vacuum degree is 10 -3 ~10 -5 Pa.

[0010] Preferably, in the magnetron sputtering process, a negative bias voltage is applied between the target material and the base material, and the bias voltage is -100 to -200 V.

[0011] Preferably, in the magnetron sputtering process, a magnetic field is applied between the target material and the base material, and the magnetic field strength is 200-500 G.

[0012] Preferably, the heat treatment temperature is 150-300℃, and the heat treatment time is 1-3 h.

[0013] Preferably, before the magnetron sputtering, the base material is pretreated, and the pretreatment comprises: sequentially placing the base material in acetone, alcohol and deionized water for ultrasonic cleaning, and then performing vacuum drying at 150-200℃, wherein the vacuum degree is 10 -3 ~ 10 -2 Pa.

[0014] A tantalum-silver coating modified bone implant is prepared by the above method; the bonding force between the tantalum-silver coating and the bone implant is 20-60 MPa, and the roughness is 15-100 nm.

[0015] Preferably, the thickness of the tantalum-silver coating is 200 nm-5 µm.

[0016] Compared with the prior art, the present application has the following beneficial technical effects:

[0017] The application discloses a preparation method of a tantalum-silver coating modified bone implant, and the tantalum-silver coating modified bone implant is formed by sequentially depositing tantalum and silver on the surface of a titanium alloy base, the coating can form an endogenous electric field with a cell membrane, and is helpful to promote the adhesion, proliferation and differentiation of cells on the surface of the implant, in particular, tantalum is a metal with good biocompatibility, the surface of which is easy to be recognized and combined by cells, and silver has certain antibacterial performance and can reduce the risk of post-implantation infection, thereby improving the bone integration ability together. The tantalum-silver coating not only improves the potential difference of the surface of the titanium alloy base, but also improves the overall biocompatibility, the compatibility of tantalum with human tissues is very good, and almost no rejection reaction is caused. Meanwhile, the addition of silver can further inhibit bacterial growth and reduce inflammatory reactions around the implant, which is beneficial to postoperative recovery; the formation of the endogenous electric field can guide the directional growth and arrangement of cells on the surface of the implant, thereby optimizing the cell behavior, which not only helps to form a more compact and firm bone-implant interface, but also improves the stability and durability of the implant; as a broad-spectrum antibacterial agent, silver can effectively kill or inhibit the growth of various bacteria, and the addition of the silver coating in the bone implant can significantly reduce the risk of postoperative infection and improve the success rate of surgery and the rehabilitation quality of patients. Therefore, the tantalum-silver coating modified bone implant improves the bone integration ability of the implant, enhances the biocompatibility, optimizes the cell behavior and improves the antibacterial performance.

[0018] Further, the purity of the argon is greater than 99.999%, and the flow rate of the argon is 20-100 sccm. The argon with a purity greater than 99.999% almost contains no impurities, so that additional contaminant substances are not introduced in the sputtering process, thereby ensuring the purity and quality of the coating. The high-purity argon can also provide a stable sputtering environment, reduce the sputtering instability caused by gas impurities, and improve the sputtering efficiency and uniformity of the coating. The flow rate of the argon is controlled in the range of 20-100 sccm, so as to ensure the flowability and uniformity of the gas in the sputtering area, which is beneficial to the effective sputtering and deposition of target atoms. The appropriate flow rate can also reduce the problems of sputtering efficiency reduction or coating quality instability caused by excessively large or small gas flow. The high-purity argon can effectively isolate oxygen in the air, and reduce the oxidation of the target material and the deposited coating in the sputtering process, which is crucial for preparing high-quality tantalum and silver coatings, because oxidation can reduce the conductivity, corrosion resistance and biocompatibility of the coating. Under the appropriate argon flow rate, the sputtered target atoms can be more effectively deposited and combined on the surface of the base to form a dense and uniform coating. The dense coating structure is helpful to improve the mechanical properties and durability of the coating, and is also beneficial to improve the biocompatibility and antibacterial performance of the coating.

[0019] Further, in the magnetron sputtering process, the target current is 1-3 A, and the magnetron sputtering time is 18-450 min. The size of the target current directly affects the sputtering rate. In the range of 1-3 A, the target current is moderate, which can not only ensure sufficient sputtering rate, but also avoid overheating of the target material, unstable sputtering or degradation of the coating quality caused by excessive current. Appropriate target current also helps to improve the energy of sputtered atoms, so that they can be more effectively deposited on the substrate surface to form a dense and uniform coating. The sputtering time in the range of 18-450 min can ensure that the coating reaches the required thickness and uniformity. Too short sputtering time may result in a thin or uneven coating, while too long sputtering time may increase production cost and energy consumption. In this time period, the sputtering process can be stable, which is conducive to the formation of high-quality coatings. Appropriate target current and sputtering time can reduce the introduction of impurities during sputtering, thereby improving the purity of the coating. High-purity coatings are beneficial to improve the electrical conductivity, corrosion resistance and biocompatibility of the coating. Under appropriate sputtering conditions, sputtered atoms can more effectively bond with the substrate surface to form a firm coating. This helps to improve the durability and stability of the coating.

[0020] Further, in the magnetron sputtering process, the vacuum degree is 10 -3 ~10 -5 Pa. In this vacuum degree range, the probability of interaction between evaporated substances and other gas molecules can be significantly reduced, thereby reducing the risk of possible "contamination". This helps to improve the purity and quality of the film layer and avoid the introduction of unnecessary impurities. Moderate vacuum degree helps evaporated materials to obtain better flying properties, so that they can be more uniformly deposited on the substrate surface. This helps to form a smooth and dense film, improving the overall quality of the coating. High vacuum degree can reduce the scattering of gas molecules on the film and reduce energy loss during sputtering, thereby improving sputtering efficiency. Low vacuum degree will cause unnecessary reactions between evaporated materials and residual gas molecules, introducing impurities or causing loose film structure. In this vacuum degree range, such situations can be avoided to ensure the stability and reliability of the film layer and improve the adhesion of the film layer.

[0021] Further, in the process of magnetron sputtering, a negative bias voltage is applied between the target material and the substrate, with a bias voltage of -100 to -200 V. The negative bias voltage can attract positive ions in the plasma to accelerate towards the substrate. These high-energy ions can transfer energy and promote the rearrangement of atoms on the substrate surface when bombarding the substrate surface, which helps to form a more dense and uniform coating. Appropriate negative bias voltage can reduce defects such as pores and cracks in the coating, improve the overall quality of the coating, and affect the microstructure of the coating, enhancing the surface roughness. Ion bombardment under negative bias voltage can enhance the interaction between coating atoms and substrate atoms, promoting chemical bonding between them, thereby improving the adhesion of the coating to the substrate. Strong adhesion helps to reduce the risk of coating peeling during use and improves the service life of the coating. Negative bias voltage can increase the energy of sputtered atoms, making them more easily sputtered from the target surface and more effectively deposited on the substrate. Under appropriate negative bias voltage, the sputtering rate can be optimized, thereby ensuring the quality of the coating while improving production efficiency.

[0022] Further, in the process of magnetron sputtering, a magnetic field is applied between the target material and the substrate, with a magnetic field strength of 200 to 500 G. The magnetic field can constrain and extend the motion trajectory of electrons, increasing the collision probability of electrons and working gas, thereby promoting ionization. The newly generated electrons also join the collision process, increasing the collision probability by several orders of magnitude and effectively utilizing the energy of electrons. Therefore, in the abnormal glow discharge that forms a high-density plasma, the plasma density increases, and the rate of sputtering target atoms also increases. The magnetic field can guide the motion trajectory of sputtered particles, making them more concentratedly bombard the substrate surface, thereby improving the sputtering efficiency. The magnetic field can constrain the movement of electrons near the target surface, reducing direct bombardment of the substrate by electrons, thereby reducing the temperature rise of the substrate. At the same time, the magnetic field can also make the sputtered particles more uniformly distributed on the substrate surface, thereby improving the uniformity of the coating. The magnetic field can reduce scattering during sputtering, reducing the probability of defects such as pores and cracks in the coating, thereby improving the overall quality of the coating. The magnetic field can accelerate the bombardment of positive ions towards the substrate, increasing the bombardment energy and density, thereby promoting the interaction and chemical bonding between coating atoms and substrate atoms, improving the adhesion of the coating to the substrate. The magnetic field can also affect the interface structure between the coating and the substrate, making it more compact and firm, further improving the adhesion of the coating to the substrate.

[0023] Further, the temperature of the heat treatment is 150-300℃, and the time is 1-3h. The heat treatment helps the metallurgical reaction between the coating and the substrate, and forms chemical bonding, thereby improving the adhesion of the coating. The appropriate temperature and time can ensure that the metallurgical reaction is fully carried out without causing excessive thermal damage to the coating or the substrate. During the heat treatment, the atoms in the coating are rearranged and diffused, which helps to eliminate pores and cracks in the coating, and improves the uniformity and density of the coating. Through the heat treatment, the grains in the coating can be refined, and the number of grain boundaries increases, thereby improving the hardness and wear resistance of the coating. The heat treatment can release the stress generated in the coating during sputtering, and reduce the risk of cracking of the coating due to excessive stress. At the same time, the heat treatment under this condition also improves the stability and adhesion of the coating.

[0024] Further, before the magnetron sputtering, the substrate is pretreated. The pretreatment is to sequentially place the substrate in acetone, alcohol and deionized water for ultrasonic cleaning, and then vacuum dry at 150-200℃, wherein the vacuum degree is 10 -3 ~ 10 -2 Pa, which can improve the cleanliness of the coating surface.

[0025] Placing the substrate in acetone, alcohol and deionized water for ultrasonic cleaning can effectively remove contaminants such as grease, dust and oxides on the surface of the substrate. If these contaminants remain on the surface of the substrate, they will affect the adhesion and deposition of particles during sputtering, thereby reducing the quality and performance of the film. Ultrasonic cleaning can penetrate into the small pores on the surface of the substrate through the oscillation of ultrasonic waves, and completely remove the difficult-to-remove contaminants, thereby improving the surface cleanliness of the substrate. A clean substrate surface is conducive to the formation of chemical bonding between the sputtering particles and the substrate, thereby improving the adhesion between the film and the substrate. In addition, vacuum drying at 150-200℃ can remove residual moisture on the surface and inside the substrate. If the moisture remains in the substrate, it may cause defects such as bubbles and cracks during sputtering, affecting the quality and stability of the film. During vacuum drying, the vacuum degree is controlled at 10 -3 ~ 10 -2In the range of Pa, air can be isolated to prevent the substrate from oxidation reaction during the drying process, which helps to maintain the original performance and structure of the substrate and provides a good foundation for the subsequent sputtering process. The surface of the substrate after vacuum drying is drier and cleaner, which is conducive to the uniform deposition and adhesion of sputtering particles on the substrate. This can improve the quality, uniformity and stability of the coating; the surface of the pretreated substrate is smoother and cleaner, which is conducive to the smooth progress of the sputtering process, which can improve the efficiency and quality of the coating. The pretreated substrate can significantly improve the adhesion, hardness and wear resistance between the coating and the substrate, which helps to prolong the service life of the coating and improve the reliability and stability of the product. BRIEF DESCRIPTION OF DRAWINGS

[0026] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the following will briefly introduce the drawings needed to be used in the embodiments. It should be understood that the following drawings only show some embodiments of the present application, and therefore should not be regarded as a limitation on the scope. For those skilled in the art, other related drawings can also be obtained without creative labor on the basis of these drawings.

[0027] Figure 1 Micro-morphology diagram of the fracture of the tantalum-silver coating modified material prepared for Comparative Example 1 of the present application;

[0028] Figure 2 Surface potential difference and surface morphology diagram of the tantalum-silver coating modified material prepared for Comparative Example 1 of the present application;

[0029] Figure 3 Micro-morphology diagram of the fracture of the tantalum-silver coating modified material prepared for Comparative Example 2 of the present application;

[0030] Figure 4 Surface potential difference and surface morphology diagram of the tantalum-silver coating modified material prepared for Comparative Example 2 of the present application;

[0031] Figure 5 Micro-morphology diagram of the fracture of the tantalum-silver coating modified material prepared for Comparative Example 3 of the present application;

[0032] Figure 6 Surface potential difference and surface morphology diagram of the tantalum-silver coating modified material prepared for Comparative Example 4 of the present application;

[0033] Figure 7 Micro-morphology diagram of the fracture of the tantalum-silver coating modified material prepared for Example 1 of the present application;

[0034] Figure 8 Surface potential difference and surface morphology diagram of the tantalum-silver coating modified material prepared for Example 1 of the present application. DETAILED DESCRIPTION

[0035] To enable persons skilled in the art to understand the features and effects of the present application, the following is a general description and definition of the terms and phrases mentioned in the specification and claims. Unless otherwise specified, all technical and scientific words used herein are in the usual meaning understood by those skilled in the art of the present application, and in the event of conflict, the definition in the specification shall prevail.

[0036] Theories or mechanisms described and disclosed herein, whether correct or not, should not be considered limiting on the scope of the present application, that is, the present application can be implemented without regard to any particular theory or mechanism.

[0037] Herein, all features defined in the form of numerical ranges or percentage ranges, such as numerical values, amounts, contents and concentrations, are for the sake of brevity and convenience. Accordingly, the description of numerical ranges or percentage ranges should be considered to have encompassed and specifically disclosed all possible sub-ranges and individual numerical values within the range (including integers and fractions).

[0038] Herein, unless otherwise specified, "comprise", "include", "contain", "have", or similar words encompass the meaning of "consist of" and "consist essentially of", for example, "A comprises a" encompasses the meaning of "A comprises a and other" and "A comprises only a".

[0039] Herein, for the sake of brevity, all possible combinations of the technical features in each embodiment or example are not described. Therefore, as long as the combinations of the technical features do not conflict, the technical features in each embodiment or example can be combined arbitrarily, and all possible combinations should be considered as the scope of the present specification.

[0040] The present application provides a preparation method of a tantalum-silver coating modified bone implant, comprising sequentially depositing tantalum and silver on the surface of a base metal by magnetron sputtering method under an argon atmosphere, and heat treating the base material after magnetron sputtering to obtain the tantalum-silver coating modified bone implant.

[0041] The purity of the argon is greater than 99.999%, and the flow rate of the argon is 20-100 sccm.

[0042] In the magnetron sputtering process, the target current is 1-3 A, and the magnetron sputtering time is 18-450 min.

[0043] In the magnetron sputtering process, the vacuum degree is 10 -3 ~10 -5 Pa.

[0044] In the magnetron sputtering process, a negative bias voltage is applied between the target and the substrate, and the bias voltage is -100-200V. At the same time, a magnetic field is applied between the target and the substrate during the magnetron sputtering process, and the magnetic field strength is 200-500G.

[0045] Preferably, the temperature of the heat treatment is 150-300℃, and the time is 1-3h.

[0046] Before the magnetron sputtering, the substrate is pretreated, that is, the substrate is sequentially placed in acetone, alcohol and deionized water for ultrasonic cleaning, and then vacuum drying is carried out at 150-200℃, wherein the vacuum degree is 10 -3 ~ 10 -2 Pa.

[0047] In addition, the application also discloses a tantalum-silver coating modified bone implant, which is prepared by the above method; the bonding force between the tantalum-silver coating and the bone implant is 20-60MPa, and the roughness is 15-100nm; the thickness of the tantalum-silver coating is 200nm-5µm.

[0048] By using the magnetron sputtering technology, the application can deposit a coating with controllable, uniform and stable thickness on a titanium or titanium alloy metal substrate. By changing the sputtering order of the target metal, the osteogenic ability and antibacterial ability of the bone implant are effectively improved, and the bone integration ability of the bone implant is further improved. Compared with the traditional coating technology, the coating thickness of the application is controlled between 200nm and 5µm, which not only ensures the stability and uniformity of the coating, but also avoids the adverse reactions that may be caused by the over-thick coating. By comparing different coating thicknesses and different sputtering orders of different target metals, the application aims to find the best composite metal coating in terms of bone integration ability. Through a series of verifications, it is found that the 500nm thick tantalum-silver coating has the best mechanical properties, and the 500nm thick tantalum-silver coating has the best osteogenic ability. At the same time, the tantalum and silver are deposited on the surface of the substrate metal in sequence, which has the best osteogenic and antibacterial ability, which provides a more flexible solution for different clinical needs.

[0049] The application will be further described in conjunction with specific examples. It should be understood that these examples are only used to illustrate the application and not to limit the scope of the application. In addition, it should be understood that those skilled in the art can make various modifications or changes to the application after reading the content taught by the application, and these equivalent forms also fall within the scope defined by the claims attached hereto.

[0050] The following examples use apparatus and equipment that are conventional in the art. The experimental methods in the following examples, unless otherwise specified, are generally conducted under conventional conditions, or under conditions recommended by the manufacturer. The following examples use various raw materials, unless otherwise specified, which are conventional commercially available products, and the specifications thereof are conventional in the art. In the specification of the present application and in the following examples, unless otherwise specified, "%" means "percent by weight", "parts" means "parts by weight", and the ratio means "ratio by weight".

[0051] Comparative Example 1

[0052] The base metal was cut into a suitable size of sheet or column, and ultrasonic cleaned in deionized water. Ultrasonic cleaning was performed in acetone, alcohol and deionized water, respectively, to ensure surface cleanliness. And dried in a vacuum environment at 200℃. In the environment of vacuum degree 10^-5 Pa, tantalum silver coating was deposited by magnetron sputtering equipment. The target current was set to 0.3A, the substrate temperature was kept at room temperature, and the argon flow was constant at 20 sccm. After sputtering coating, appropriate heat treatment (400℃ for 1 hour) can be performed to improve the adhesion and uniformity of the coating. The surface morphology of the coating was observed by scanning electron microscope (SEM), as shown in Figure 1 , indicating that the coating is uniform and dense.

[0053] Comparative Example 2

[0054] The difference between this example and Comparative Example 1 is that the thickness of the tantalum silver coating is 500nm.

[0055] Comparative Example 3

[0056] The difference between this example and Comparative Example 1 is that the thickness of the tantalum silver coating is 750nm.

[0057] Example 1

[0058] A method for preparing a tantalum silver coating modified bone implant, the base metal was cut into a suitable size of sheet or column, and ultrasonic cleaned in deionized water. Ultrasonic cleaning was performed in acetone, alcohol and deionized water, respectively, to ensure surface cleanliness. And dried in a vacuum environment at 200℃. In the environment of vacuum degree 10^-5 Pa, tantalum silver coating was deposited by magnetron sputtering equipment. The target current was set to 0.3A, the substrate temperature was kept at room temperature, and the argon flow was constant at 20 sccm. After sputtering coating, appropriate heat treatment (400℃ for 1 hour) can be performed to improve the adhesion and uniformity of the coating.

[0059] The prepared material was characterized by tomographic micro-morphology, surface potential difference of the material and surface morphology, specifically:

[0060] Figure 1The figure shows the microstructure of the tantalum silver coating modified material obtained in Comparative Example 1 of the present invention. As can be seen from the figure, the tantalum silver coating with a thickness of 250 nm is intact and unbroken.

[0061] Figure 2 The image shows the surface potential difference and surface morphology of the tantalum silver coating modified material prepared in Comparative Example 1 of the present invention. As can be seen from the image, the potential difference of the tantalum silver coating with a thickness of 250 nm is 160 mV, and the surface is relatively smooth.

[0062] Figure 3 The figure shows the microstructure of the tantalum-silver coating modified material obtained in Comparative Example 2 of the present invention. As can be seen from the figure, the tantalum-silver coating with a thickness of 500 nm is intact and unbroken.

[0063] Figure 4 The image shows the surface potential difference and surface morphology of the tantalum silver coating modified material prepared in Comparative Example 2 of the present invention. As can be seen from the image, the potential difference of the 500nm thick tantalum silver coating is 210mV, and the surface is significantly rougher.

[0064] Figure 5 The figure shows the microstructure of the tantalum-silver coating modified material obtained in Comparative Example 3 of the present invention. As can be seen from the figure, the tantalum-silver coating with a thickness of 750 nm is intact and unbroken.

[0065] Figure 6 The figures show the surface potential difference and surface morphology of the tantalum silver coating modified material prepared in Comparative Example 4 of the present invention. As can be seen from the figures, the potential difference of the 500nm thick tantalum silver coating is 170mV, and the surface roughness is also higher than that of the 250nm thick tantalum silver coating.

[0066] Figure 7 The figure shows the cross-sectional microstructure of the tantalum-silver coating modified material obtained in Example 1 of the present invention. As can be seen from the figure, the tantalum-silver coating is intact and unbroken.

[0067] Figure 8 The image shows the surface potential difference and surface morphology of the tantalum-silver coating modified material prepared in Example 1 of the present invention. As can be seen from the image, the surface potential difference of the tantalum-silver coating is 380mV. The high potential difference can affect the cell membrane potential and form an endogenous electric field, thereby promoting bone integration. The surface roughness is also significantly higher than that of the simple tantalum-silver coating.

[0068] Example 2

[0069] A method for preparing a tantalum silver-coated modified bone implant includes the following steps:

[0070] S1: Pretreatment of the substrate, wherein the pretreatment involves ultrasonically cleaning the substrate sequentially with acetone, alcohol, and deionized water, followed by vacuum drying at 150°C, wherein the vacuum degree is 10. -2Pa;

[0071] S2: Tantalum and silver are sequentially deposited on the pretreated substrate metal surface by magnetron sputtering under an argon atmosphere with a purity greater than 99.999% and a flow rate of 20 sccm. The magnetron sputtered substrate is then heat-treated at 150°C for 3 hours to obtain the tantalum-silver coated modified bone implant.

[0072] During the magnetron sputtering process, the target current was 1A, the sputtering time was 18 minutes, and the vacuum level was 10. -5 Pa. In addition, during magnetron sputtering, a negative bias voltage of -200V is applied between the target and the substrate. Simultaneously, during magnetron sputtering, a magnetic field of 200G is applied between the target and the substrate.

[0073] The thickness of the tantalum silver coating is 200 nm.

[0074] Example 3

[0075] A method for preparing a tantalum silver-coated modified bone implant includes the following steps:

[0076] S1: Pretreatment of the substrate, wherein the pretreatment involves ultrasonically cleaning the substrate sequentially with acetone, alcohol, and deionized water, followed by vacuum drying at 300°C, wherein the vacuum degree is 10. -3 Pa;

[0077] S2: Tantalum and silver are sequentially deposited on the pretreated substrate metal surface by magnetron sputtering under an argon atmosphere with a purity greater than 99.999% and a flow rate of 100 sccm. The magnetron sputtered substrate is then heat-treated at 150°C for 3 hours to obtain the tantalum-silver coated modified bone implant.

[0078] During the magnetron sputtering process, the target current was 3A, the sputtering time was 450 minutes, and the vacuum level was 10. -3 Pa. In addition, during magnetron sputtering, a negative bias voltage of -150V is applied between the target and the substrate. Simultaneously, during magnetron sputtering, a magnetic field with a strength of 500G is applied between the target and the substrate.

[0079] The thickness of the tantalum silver coating is 5µm.

[0080] Example 4

[0081] A method for preparing a tantalum silver-coated modified bone implant includes the following steps:

[0082] S1: Pretreatment of the substrate, wherein the pretreatment involves ultrasonically cleaning the substrate sequentially with acetone, alcohol, and deionized water, followed by vacuum drying at 200°C, wherein the vacuum degree is 10. -3 Pa;

[0083] S2: Tantalum and silver are sequentially deposited on the pretreated substrate metal surface by magnetron sputtering under an argon atmosphere with a purity greater than 99.999% and a flow rate of 50 sccm. The magnetron sputtered substrate is then heat-treated at 300°C for 2 hours to obtain the tantalum-silver coated modified bone implant.

[0084] During the magnetron sputtering process, the target current was 2A, the sputtering time was 90 minutes, and the vacuum level was 10. -4 Pa. In addition, during magnetron sputtering, a negative bias voltage of -100V is applied between the target and the substrate. Simultaneously, during magnetron sputtering, a magnetic field with a strength of 300G is applied between the target and the substrate.

[0085] The thickness of the tantalum silver coating is 1µm.

[0086] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

[0087] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the essence and scope of the technical solutions of the present invention.

Claims

1. A method for preparing a tantalum silver-coated modified bone implant, characterized in that, The method includes depositing tantalum and silver sequentially on the surface of a base metal by magnetron sputtering under an argon atmosphere, and then heat-treating the substrate after magnetron sputtering to obtain the tantalum-silver coated modified bone implant. The argon gas has a purity greater than 99.999% and a flow rate of 20~100 sccm; Before magnetron sputtering, the substrate undergoes pretreatment, which involves ultrasonic cleaning of the substrate sequentially in acetone, alcohol, and deionized water, followed by vacuum drying at 150-200°C with a vacuum degree of 10. -3 ~ 10 -2 Pa; The heat treatment temperature is 150~300℃, and the time is 1~3h; During the magnetron sputtering process, the target current is 1~3A, the magnetron sputtering time is 18~450min, and the vacuum degree is 10. -3 ~10 -5 Pa; apply a negative bias voltage between the target and the substrate, with a bias voltage of -100~-200V; apply a magnetic field between the target and the substrate, with a magnetic field strength of 200~500G.

2. A tantalum silver-coated modified bone implant, characterized in that, The tantalum silver coating is prepared by the method described in claim 1; the bonding strength between the coating and the bone implant is 20~60MPa, and the roughness is 15~100nm.

3. The tantalum silver-coated modified bone implant according to claim 2, characterized in that, The thickness of the tantalum-silver coating is 200 nm to 5 µm.

Citation Information

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