CN113210625A - 3D porous titanium alloy material with tantalum coating deposited on surface and preparation method thereof - Google Patents
3D porous titanium alloy material with tantalum coating deposited on surface and preparation method thereof Download PDFInfo
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- CN113210625A CN113210625A CN202110501750.7A CN202110501750A CN113210625A CN 113210625 A CN113210625 A CN 113210625A CN 202110501750 A CN202110501750 A CN 202110501750A CN 113210625 A CN113210625 A CN 113210625A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
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- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C14/00—Alloys based on titanium
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
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Abstract
The invention provides a 3D porous titanium alloy material with a tantalum coating deposited on the surface, which comprises the following components: the porous titanium alloy printed by 3D is used as a substrate, and metal tantalum is deposited on the surface of the substrate. The advantages are that: the specific structure can be customized as required, and the pore structure on the porous structure can be designed according to the size of the adjusting design unit and the thickness of the silk diameter so as to obtain a porous structure with different pore diameters, porosities and mechanical properties, thereby fully meeting the clinical requirements.
Description
Technical Field
The invention relates to the technical field of medical equipment, in particular to a 3D porous titanium alloy material with a tantalum coating deposited on the surface and a preparation method thereof.
Background
In medicine, the use of bone implant materials is more and more common, but the existing method for preparing the material has the problem of high cost investment, and meanwhile, the existing material has a plurality of defects in the preparation process, such as high deposition temperature and large energy consumption, and the existing material has poor mechanical properties of carbon nets, needs a large amount of metal tantalum to coat so as to improve the strength of metal tantalum bone trabeculae, and the mechanical properties of the existing material are also barely close to the metal tantalum and the like.
Disclosure of Invention
The invention provides a 3D porous titanium alloy material with a tantalum coating deposited on the surface and a preparation method thereof, which are close to the technical defects.
In order to achieve the above purpose, the invention provides the following technical scheme:
the invention provides a 3D porous titanium alloy material with a tantalum coating deposited on the surface, which comprises the following components: the porous titanium alloy printed by 3D is used as a substrate, and metal tantalum is deposited on the surface of the substrate.
Preferably, the base body is formed by stacking titanium alloy metal powder layer by layer in an electron beam melting mode according to an electron beam melting technology, and then is printed into a shape in a 3D mode according to design requirements.
Preferably, the pore structure on the substrate comprises a regular hexahedron, a face-centered cube, a rotating face-centered cube, a bionic bone trabecula, a rhombic dodecahedron structure and a curved surface porous structure.
The invention also provides a preparation method of the 3D porous titanium alloy material with the tantalum coating deposited on the surface, which comprises the following steps:
s1, stacking and forming titanium alloy metal powder layer by layer in an electron beam melting mode by using an electron beam melting technology, and forming a 3D porous titanium alloy by 3D printing according to shape requirements, wherein the porous titanium alloy is used as a base body for standby;
s2, placing the substrate obtained in the step S1 into a chemical vapor deposition chamber after acid washing, placing tantalum pentachloride powder into a quartz reaction chamber, carrying out continuous ultimate vacuum treatment on the quartz reaction chamber and the chemical vapor deposition chamber, introducing high-purity argon into the quartz reaction chamber and the chemical vapor deposition chamber every 8-12min, and repeatedly introducing the high-purity argon for 2-3 times;
s3, under the protection of high-purity argon, heating the quartz reaction chamber containing the tantalum pentachloride powder to 420-430K to generate tantalum pentachloride gas, closing the high-purity argon, and introducing high-purity hydrogen into the quartz reaction chamber; then, tantalum pentachloride gas is introduced into the chemical vapor deposition chamber to be reacted so as to replace tantalum metal to be deposited on the surface of the substrate;
and S4, repeating the step S3, so that the replaced tantalum metal is deposited on the same substrate surface every time, and finally obtaining the tantalum metal coating on the substrate surface.
Preferably, in step S2, the substrate obtained in step S1 is subjected to acid cleaning treatment using an etching solution.
Further, the etching solution is prepared from nitric acid, hydrofluoric acid and deionized water, and the volume ratio of the solution is 10:5: 85.
Preferably, in step S2, the acid washing time is 20min, and then the air is dried by dry nitrogen; the time for introducing high-purity argon each time is 20 min.
Preferably, in step S2, before the chemical vapor deposition chamber and the quartz reaction chamber are subjected to the ultimate vacuum treatment, the degrees of vacuum in the chemical vapor deposition chamber and the quartz reaction chamber are greater than or equal to 1Pa and less than 8Pa, the average pore diameter of the porous titanium alloy is 500 ± 400 μm, the average wire diameter is 500 ± 200 μm, and the average porosity is 50% -85%.
Preferably, in step S3, tantalum pentachloride gas is introduced and then reacted for 7-10h under 1073.15-1273.15K to replace tantalum metal.
Preferably, in step S3, the tantalum metal is deposited on the surface of the substrate to a thickness of 5-12 μm.
The 3D porous titanium alloy material with the tantalum coating deposited on the surface and the preparation method thereof have the advantages that:
1. the medium 3D porous titanium alloy material provided by the invention takes a 3D printed porous titanium alloy as a substrate, can be prepared into a universal or special acetabulum filling block, a femur filling block, a tibia filling block, a limb bone filling block and the like, and the specific structure of the material can be customized according to the needs, and the pore structure on the material can be designed according to the size of a design unit and the thickness of a wire diameter, so that porous structures with different pore diameters, porosity and mechanical properties can be obtained, and the clinical requirements can be fully met; in addition, compared with the traditional method of using a porous carbon material as a matrix, the method can better ensure the high mechanical strength of the matrix material, has low requirement on the deposition amount of the metal tantalum, and has short preparation period and high generation efficiency;
2. the material protected by the invention realizes that the surface of the substrate which is a 3D printed porous titanium alloy is completely coated with the tantalum coating to form a firmly combined metal tantalum coating structure;
3. the structure of the material protected by the invention can be designed according to the needs, which is beneficial to the growth of different bone tissues and cell tissues, thereby realizing good osseointegration between the tantalum metal layer and the surrounding tissues; the porous structure in the prior art can only be fixed as a carbon net structure, and the prepared tantalum technology has the advantages of large coating thickness, low porosity and uneven and compact coating, and is not beneficial to the adhesion of small molecular substances on a substrate;
4. the material protected by the invention has the advantages of consistent mechanical property with a matrix, good biocompatibility and high strength, can match the mechanical property of the elastic modulus of human cancellous bone, and provides the effect of bone ingrowth;
5. the material prepared by the method of the invention ensures that the tantalum coating is uniform and compact, can be tightly attached to the substrate, has almost the same surface performance as the metallic tantalum performance, can meet the requirements of clinical application, promotes the regeneration and reconstruction of bone tissues, and is a good biological implantation material;
6. in the method, the tantalum coating and the substrate are combined in the high-temperature phase region of the tantalum coating and the substrate, so that the bonding strength is high and the interface is stable;
7. in the preparation method of the material, the personalized 3D printed porous titanium alloy substrate is adopted, the preparation time of the tantalum metal coating is shorter than that of a film formed on the porous carbon mesh substrate, the preparation temperature is low, and the energy consumption is low, so that the preparation method of the tantalum metal coating by using the 3D printed porous titanium alloy as the substrate has more advantages under the same process;
8. the invention relates to an advanced porous metal tantalum preparation technology, which can be used for preparing a novel porous tantalum filling block or a novel technology for uniformly depositing a tantalum coating on the surface of a porous material.
Drawings
The accompanying drawings are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention. In the drawings:
FIG. 1 is a schematic diagram of a thickness structure of a tantalum metal layer obtained on a surface of a substrate in step S3 according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of a thickness structure of a tantalum metal layer obtained on a surface of a substrate in step S3 according to an embodiment of the present invention;
FIG. 3 is a schematic diagram of the thickness structure of the tantalum metal layer obtained on the surface of the substrate in the three step S3 according to the embodiment of the present invention.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
The first embodiment is as follows:
the invention provides a preparation method of a 3D porous titanium alloy material with a tantalum coating deposited on the surface, which comprises the following steps:
s1, stacking and forming titanium alloy metal powder layer by layer in an electron beam melting mode by using an electron beam melting technology, wherein the electron beam power is 900W, the spot diameter is 100 microns, the thickness is 50 microns, and the scanning speed is 800mm/S, so as to prepare a porous filling block, and then forming the porous titanium alloy through 3D printing according to the shape requirement, so as to form the 3D porous titanium alloy which is used as a substrate for standby;
wherein: the 3D printed porous titanium alloy is suitable for filling various bone defects, and can be used for preparing universal or special acetabulum filling blocks, femur filling blocks, tibia filling blocks, limb bone filling blocks and the like; the filling porous structure printed in the step 3D is the matrix, different pore structures including a regular hexahedron, a face-centered cube, a rotating face-centered cube, a bionic bone trabecula, a rhombic dodecahedron structure, a curved surface porous structure and the like can be designed according to needs, and the porous structures with different pore diameters, porosity and mechanical properties can be obtained by adjusting the size of the designed unit and the thickness of the wire diameter, so that the clinical requirements are met;
the rhombic dodecahedron structure is formed by small beams which extend outwards from two opposite vertexes of twelve surfaces of the rhombic dodecahedron, and a pore is formed between every two adjacent small beams;
the curved surface porous structure can generate porous structures with different porosities by using different parameters, and has strong design degree;
the structure of the matrix can be designed according to the requirement, so that different bone tissues and cell tissues can grow in the matrix, and good osseointegration between the tantalum metal coating and the surrounding bone tissues can be realized; in addition, compared with the traditional porous carbon material substrate, the substrate material selected by the invention has high mechanical strength and low requirement on the deposition amount of metal tantalum;
s2, performing acid washing treatment on the substrate obtained in the step S1 for 20min by using corrosive liquid, drying the substrate by using dry nitrogen, placing the substrate into a chemical vapor deposition chamber, placing tantalum pentachloride powder into a quartz reaction chamber, and enabling the vacuum degree in the chemical vapor deposition chamber and the quartz reaction chamber to be 6Pa, the average pore diameter of the porous titanium alloy to be 450 microns, the average wire diameter to be 350 microns and the average porosity to be 66%;
then carrying out continuous ultimate vacuum treatment on the quartz reaction chamber and the chemical vapor deposition chamber, introducing high-purity argon into the quartz reaction chamber and the chemical vapor deposition chamber every 10min for 20min, and repeatedly introducing the high-purity argon for 2 times;
wherein the corrosive liquid is prepared from nitric acid, hydrofluoric acid and deionized water, and the volume ratio of the solution is 10:5: 85.
S3, under the protection of high-purity argon, heating the quartz reaction cavity containing the tantalum pentachloride powder to 423.15K to generate tantalum pentachloride gas, closing the high-purity argon, and introducing high-purity hydrogen into the quartz reaction cavity; then, introducing tantalum pentachloride gas into the chemical vapor deposition chamber, reacting for 9h under the condition of 1173.15K to replace the tantalum metal deposited on the surface of the substrate, wherein the thickness of the tantalum metal deposited on the surface of the substrate is 5 μm (shown in figure 1);
and S4, repeating the step S3, so that the replaced tantalum metal is deposited on the same substrate surface every time, and finally obtaining the tantalum metal coating on the substrate surface.
Example two:
the difference from the first embodiment is that: in step S2, the average pore diameter of the porous titanium alloy is 100 μm, the average wire diameter is 300 μm, and the average porosity is 85%; the vacuum degree is 7 Pa;
introducing high-purity argon into the quartz reaction chamber and the chemical vapor deposition chamber every 8min for 18 min; the thickness of the tantalum metal deposited on the surface of the substrate in the step S3 is 8 μm (shown in FIG. 2);
example three:
the difference from the first embodiment is that: in step S2, the average pore diameter of the porous titanium alloy is 900 μm, the average wire diameter is 700 μm, and the average porosity is 50%; the vacuum degree is 2 Pa;
introducing high-purity argon into the quartz reaction chamber and the chemical vapor deposition chamber every 12min for 25 min; the thickness of the tantalum metal deposited on the surface of the substrate in the step S3 is 12 μm (as shown in FIG. 3);
other parameters different from the first embodiment are shown in the following table:
steps, structures, devices, etc. that are not explicitly described herein are conventional in the art and, thus, will not be described in detail.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. The 3D porous titanium alloy material with the tantalum coating deposited on the surface is characterized in that: the porous titanium alloy printed by 3D is used as a substrate, and metal tantalum is deposited on the surface of the substrate.
2. The 3D porous titanium alloy material with the tantalum coating deposited on the surface according to claim 1, wherein the material comprises the following components in percentage by weight: the base body is formed by stacking titanium alloy metal powder layer by layer in an electron beam melting mode according to an electron beam melting technology, and then the base body is printed into a shape through 3D according to design requirements.
3. The 3D porous titanium alloy material with the tantalum coating deposited on the surface according to claim 1, wherein the material comprises the following components in percentage by weight: the pore structure on the substrate comprises a regular hexahedron, a face-centered cube, a rotary face-centered cube, a bionic bone trabecula, a rhombic dodecahedron structure and a curved surface porous structure.
4. The preparation method of the 3D porous titanium alloy material with the tantalum coating deposited on the surface is characterized by comprising the following steps of: the method comprises the following steps:
s1, stacking and forming titanium alloy metal powder layer by layer in an electron beam melting mode by using an electron beam melting technology, and forming a 3D porous titanium alloy by 3D printing according to shape requirements, wherein the porous titanium alloy is used as a base body for standby;
s2, placing the substrate obtained in the step S1 into a chemical vapor deposition chamber after acid washing, placing tantalum pentachloride powder into a quartz reaction chamber, carrying out continuous ultimate vacuum treatment on the quartz reaction chamber and the chemical vapor deposition chamber, introducing high-purity argon into the quartz reaction chamber and the chemical vapor deposition chamber every 8-12min, and repeatedly introducing the high-purity argon for 2-3 times;
s3, under the protection of high-purity argon, heating the quartz reaction chamber containing the tantalum pentachloride powder to 420-430K to generate tantalum pentachloride gas, closing the high-purity argon, and introducing high-purity hydrogen into the quartz reaction chamber; then, tantalum pentachloride gas is introduced into the chemical vapor deposition chamber to be reacted so as to replace tantalum metal to be deposited on the surface of the substrate;
and S4, repeating the step S3, so that the replaced tantalum metal is deposited on the same substrate surface every time, and finally obtaining the tantalum metal coating on the substrate surface.
5. The method of claim 4, further comprising: in step S2, the substrate obtained in step S1 is subjected to acid washing treatment using an etching solution.
6. The method of claim 5, further comprising: the corrosive liquid is prepared from nitric acid, hydrofluoric acid and deionized water, and the volume ratio of the solution is 10:5: 85.
7. The method of claim 4, further comprising: in step S2, the pickling time is 20min, and then the steel plate is dried by dry nitrogen; introducing high-purity argon for 18-25min each time.
8. The method of claim 4, further comprising: in step S2, before the chemical vapor deposition chamber and the quartz reaction chamber are subjected to the ultimate vacuum processing, the vacuum degrees in the chemical vapor deposition chamber and the quartz reaction chamber are greater than or equal to 1Pa and less than 8Pa, the average pore diameter of the porous titanium alloy is 500 ± 400 μm, the average wire diameter is 500 ± 200 μm, and the average porosity is 50% -85%.
9. The method of claim 4, further comprising: in step S3, tantalum pentachloride gas is introduced and then reacted for 7-10h under 1073.15-1273.15K to replace tantalum metal.
10. The method of claim 4, further comprising: in step S3, the tantalum metal is deposited on the surface of the substrate to a thickness of 5-12 μm.
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Cited By (3)
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| CN113563114A (en) * | 2021-08-12 | 2021-10-29 | 昆明理工大学 | Porous tantalum coating carbon fiber/carbon composite material and preparation method thereof |
| CN114540789A (en) * | 2022-02-25 | 2022-05-27 | 王虎跃 | Preparation method of titanium alloy surface corrosion-resistant coating |
| CN115120783A (en) * | 2022-06-29 | 2022-09-30 | 湖南华翔医疗科技有限公司 | Porous titanium-based antibacterial active material, and preparation method and application thereof |
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| CN113563114A (en) * | 2021-08-12 | 2021-10-29 | 昆明理工大学 | Porous tantalum coating carbon fiber/carbon composite material and preparation method thereof |
| CN114540789A (en) * | 2022-02-25 | 2022-05-27 | 王虎跃 | Preparation method of titanium alloy surface corrosion-resistant coating |
| CN114540789B (en) * | 2022-02-25 | 2024-04-19 | 中国科学院金属研究所 | Preparation method of corrosion-resistant coating on surface of titanium alloy |
| CN115120783A (en) * | 2022-06-29 | 2022-09-30 | 湖南华翔医疗科技有限公司 | Porous titanium-based antibacterial active material, and preparation method and application thereof |
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